Nothing Special   »   [go: up one dir, main page]

CN103547665A - Process for manufacturing group of detergent granules - Google Patents

Process for manufacturing group of detergent granules Download PDF

Info

Publication number
CN103547665A
CN103547665A CN201280023908.3A CN201280023908A CN103547665A CN 103547665 A CN103547665 A CN 103547665A CN 201280023908 A CN201280023908 A CN 201280023908A CN 103547665 A CN103547665 A CN 103547665A
Authority
CN
China
Prior art keywords
foam
anionic surfactant
detergent
surfactant compositions
manufacture method
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201280023908.3A
Other languages
Chinese (zh)
Other versions
CN103547665B (en
Inventor
中山高志
割田浩章
今泉义信
山口将宽
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kao Corp
Original Assignee
Kao Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Kao Corp filed Critical Kao Corp
Publication of CN103547665A publication Critical patent/CN103547665A/en
Application granted granted Critical
Publication of CN103547665B publication Critical patent/CN103547665B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/12Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/14Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
    • C11D1/146Sulfuric acid esters
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/12Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/22Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/12Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/29Sulfates of polyoxyalkylene ethers
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00Special methods for preparing compositions containing mixtures of detergents
    • C11D11/0082Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
    • C11D11/0088Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads the liquefied ingredients being sprayed or adsorbed onto solid particles

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Detergent Compositions (AREA)
  • Glanulating (AREA)

Abstract

A process for manufacturing a group of detergent granules which includes a step of granulating powdery raw materials for a detergent in a rotating mixer, wherein the granulation of the powdery raw materials is conducted with a foamed anionic surfactant composition sprayed in the rotating mixer through a multi-fluid nozzle. By this process, a group of detergent granules having a medium or low bulk density can be obtained in a high yield. The group of detergent granules thus obtained exhibits high solubility.

Description

Detergent particles group's manufacture method
Technical field
The present invention relates to use the detergent particles group's of container rotary mixing machine, the foam of anionic surfactant compositions, many fluid tips manufacture method.
Background technology
Now in commercially available washing composition, rough classification has high volume density type washing composition (being greater than 690g/L), middle volume density type washing composition (400~690g/L), low volume density type washing composition (250g/L above and be less than 400g/L), liquid washing agent etc.For example in Japan, use high volume density type washing composition, but in areas such as asia and ocenia or Europe, the demand of the low volume density type of centering washing composition is also many more.
From the viewpoint of economy, environmental response, as not using spray-dired manufacture method, disclose the manufacture method of using the detergent composition of aniorfic surfactant by non-spray-drying process.In patent documentation 1, disclose by surfactant paste and for dried detergent materials high-speed mixer/middling speed mixing machine/drying machine manufacture continuously the method for detergent composition.In patent documentation 2, while disclose, in high-speed mixer/middling speed mixing machine/setting device, make particulate recirculation manufacture continuously the method for detergent composition surfactant paste and dried detergent raw material.
Yet, in the method for making of patent documentation 1, be difficult to regulate granularity, in addition, in the method for making of patent documentation 2, in order to carry out the adjusting of granularity, use the method for making of particulate recirculation, from but the low manufacture method of productivity.Therefore, seek the method for making that yield more simply obtains the detergent particles group of necessary granularity well.Further, these patent documentations are all to provide the method for the volume density that increases detergent particles group, the detergent particles group's of low volume density manufacture method in being not suitable as.
In addition, in patent documentation 3, as reducing spray-dired use or not using spray-dired manufacture method, disclose by the foam of tensio-active agent being imported to the manufacture method of the surfactant granules in mixing machine.
Yet, in the manufacture method of patent documentation 3, be not enough to as obtain detergent particles group's method for making with good yield.
Prior art document
Patent documentation
Patent documentation 1: the flat 10-500716 communique of Japanese Unexamined Patent Application Publication
Patent documentation 2: the flat 10-506141 communique of Japanese Unexamined Patent Application Publication
Patent documentation 3: Japanese Unexamined Patent Application Publication 2002-525420 communique
Summary of the invention
The present invention relates to a kind of detergent particles group's manufacture method, described detergent particles group's manufacture method has the container of use rotary mixing machine by the operation of detergent use powder raw material granulation, and described detergent particles group's manufacture method for carrying out by multithread body nozzle spray the foam of anionic surfactant compositions the granulation of this detergent use powder raw material in this container rotary mixing machine.
Embodiment
The present invention relates to provide with do not use spray-dired method with good yield manufacture contain anion surfactant in detergent particles group's the method for low volume density.
By detergent particles group's of the present invention manufacture method, can produce the effect of the detergent particles group of low volume density in can obtaining with good yield.In obtaining like this, the detergent particles group of low volume density also has the high deliquescent effect of demonstration.
One of the present invention is characterised in that, uses container rotary mixing machine to carry out the granulation of detergent use powder raw material.
In general, while using container rotary mixing machine to carry out granulation, can make powder flow equably, in addition, due to the mixed organization that takes up and cause landing to fall due to deadweight with cause particle due to rotation, thereby suppressed to put on the shearing force on powder.Therefore, can say and use the prilling process that the prilling process of described mixing machine is non-densification.In addition, if just can not carry out granulation by force owing to adding anionic surfactant compositions in the described mixing machine tackiness when contacting with powder to, therefore, need to when contacting with powder, show tackiness.If such anionic surfactant compositions is used as to single fluid nozzle or the pipe arrangement of common supply method, be supplied to container rotary mixing machine, can find to be difficult to make in mixing machine the liquid component of supplying with to disperse equably, due to the large liquid piece of part generation, easily form the tendency of thick particle.
At this, many fluid tips of use two-fluid spray nozzle etc., the foam that shows adhesive anionic surfactant compositions by spraying when contact with powder is supplied in container rotary mixing machine, is surprised to find that the also granulation equably of formation that can suppress big particle.This is considered to due to by using many fluid tips to make in advance the foam of such anionic surfactant compositions become fine drop, even if thereby in container rotary mixing machine, also can reach the high dispersive of the foam of anionic surfactant compositions, can not produce the large liquid piece that forms big particle.Therefore, by using many fluid tips to adding the foam that shows adhesive anionic surfactant compositions while contacting with powder in container rotary mixing machine, can be with good yield manufacture detergent particles group.
Further, one of feature of the present invention is for being used the foam of multithread body nozzle spray anionic surfactant compositions.
Anionic surfactant compositions, by producing foamed body, not only shows tackiness when contacting with powder, and proportion also reduces.If use the such foam of multithread body nozzle spray, can generate the fine drop that proportion reduces, its number also increases.Its result, with the granulation of detergent use powder raw material in, anionic surfactant compositions shared volume in each detergent particles increases, and because this anionic surfactant compositions becomes foam, proportion reduces, therefore, with the situation of this anionic surfactant compositions producing foamed body is not compared, because the density of every 1 detergent particles reduces, therefore, the detergent particles group of low volume density in accessing.
Like this, in the present invention, by combination, adopt container rotary mixing machine and many fluid tips, further use the foam of anionic surfactant compositions, thereby can play in the situation that using separately respectively the detergent particles group's of low volume density effect in unforeseeable can obtaining with good yield.
Embodiment as the granulation in manufacture method of the present invention, so long as use container rotary mixing machine agitator treating agent powder raw material, and use many fluid tips by the foam of anionic surfactant compositions be sprayed to embodiment in this detergent use powder raw material just without particular limitation of.Below, the embodiment for an example as manufacture method of the present invention illustrates in greater detail.
In the present invention, detergent particles is the particle that contains tensio-active agent and washing assistant etc., and detergent particles group refers to its aggregate.Detergent composition refers to and contains detergent particles group, and the composition of the detergent ingredients except detergent particles group (for example, lotion-aid particle, fluorescence dye, enzyme, spices, defoamer, SYNTHETIC OPTICAL WHITNER, bleach-activating agent etc.) adding in addition containing with good grounds hope.
In this manual, water-solublely refer to that the solubleness of the water with respect to 25 ℃ is more than 0.5g/100g, water-insoluble refers to that the solubleness of the water with respect to 25 ℃ is less than 0.5g/100g.
A. detergent particles group
Detergent particles group of the present invention is for coordinating the foam of (1) detergent use powder raw material, (2) anionic surfactant compositions to form.Detergent particles group of the present invention further also can be contained (3) other powder composition and/or (4) other liquid component.
(1) detergent use powder raw material
As detergent use powder raw material, can enumerate water-soluble solid alkali inorganic substance and/or water-soluble inorganic salt.
(1-1) water-soluble solid alkali inorganic substance
Water-soluble solid alkali inorganic substance are that under normal temperature, (20 ℃) are the alkali inorganic substance of solid state, as these water-soluble solid alkali inorganic substance, are not particularly specified, such as enumerating sodium carbonate, sodium bicarbonate, salt of wormwood, water glass etc.Wherein, preferably as the sodium carbonate that shows the alkaline agent of suitable pH buffering range in washings.These water-soluble solid alkali inorganic substance can be used separately, also can mix two or more uses.
As sodium carbonate, can use any in Soda ash light (gently ash), dense soda ash (heavy ash).
In addition, the median size of water-soluble solid alkali inorganic substance without particular limitation of, in the situation that coordinate the tensio-active agent of high-content, from improving the viewpoint of yield, also can be crushed to 1~50 μ m and use.In addition, the median size of water-soluble solid alkali inorganic substance is calculated with dimension criteria, for example, is to use laser diffraction granularity measure of spread device: the value of the manufacture of LA-920(hole field Co., Ltd. of making institute) measuring.
(1-2) water-soluble inorganic salt
In order to improve the ionic strength of washings, the effect of raising sebum soil cleaning etc., is preferably used water-soluble inorganic salt as detergent use powder raw material.As this water-soluble inorganic salt, sodium sulfate, sodium-chlor, S-WAT, vitriolate of tartar that preference is as high in ionic dissociation degree.In addition, from improving the viewpoint of dissolution rate, and also effective with sal epsom.
In addition, the median size of water-soluble inorganic salt without particular limitation of, but high-content coordinate anion surfactant in the situation that, from improving the viewpoint of detergent particles group's yield, also can be crushed to 1~50 μ m and use.In addition, the median size of water-soluble inorganic salt is calculated with dimension criteria, for example, is to use laser diffraction granularity measure of spread device: the value of the manufacture of LA-920(hole field Co., Ltd. of making institute) measuring.
As detergent use powder raw material, in water-soluble solid alkali inorganic substance, water-soluble inorganic salt, can use separately cited raw material, also can mix two or more use.As detergent use powder raw material, be preferably sodium carbonate and/or sodium sulfate, more preferably light ash.
The content of the detergent use powder raw material in detergent particles group, the content of preferably water dissolubility solid alkali inorganic substance and water-soluble inorganic salt, from improving the viewpoint of clean power, more than being preferably 10 quality %, more preferably more than 20 quality %.In addition, from reducing the viewpoint of detergent particles group's volume density, be preferably below 80 quality %.From these viewpoints, in detergent particles group, the content of detergent use powder raw material, the content of preferably water dissolubility solid alkali inorganic substance and water-soluble inorganic salt, is preferably 10~80 quality %, more preferably 20~80 quality %.
(2) foam of anionic surfactant compositions
(2-1) anionic surfactant compositions
From obtaining the detergent particles group's of sharp-pointed size-grade distribution viewpoint, as the anionic surfactant compositions using in the present invention, be preferably surfactant paste, further preferably contain following a) composition and b) surfactant paste of composition.
A) be selected from a kind of above anion surfactant in the salt of the salt of linear alkyl benzene sulphonic acid, the salt of alkylsurfuric acid and polyxyethylated sulfuric acid.
B) the above-mentioned a) composition with respect to 100 mass parts is the water of 25~70 mass parts.
As the salt of linear alkyl benzene sulphonic acid, the carbonatoms of preferred alkyl is 10~18, the salt of the linear alkyl benzene sulphonic acid that further preferably carbonatoms is 12~16.In addition, as salt, can enumerate sodium salt, sylvite, ammonium salt or amine salt.As the salt of alkylsurfuric acid, preferably the carbonatoms of carbochain is 10~18, the alkyl that further preferably carbonatoms is 12~16 or the material of thiazolinyl.In addition, as salt, can enumerate sodium salt, sylvite, ammonium salt or amine salt.
As the salt of polyxyethylated sulfuric acid, preferably the carbonatoms of carbochain is 10~18, the salt of the alkyl that further preferably carbonatoms is 12~16 or the polyxyethylated sulfuric acid of thiazolinyl.In addition, as polyoxyethylated average addition mole number, be preferably 0.1~3.0.Further, as salt, can enumerate sodium salt, sylvite, ammonium salt or amine salt.
Wherein, from obtaining the detergent particles group's of sharp-pointed size-grade distribution viewpoint, the salt of preferred alkyl sulfuric acid.
Surfactant paste at least contains as the above-mentioned a) anion surfactant shown in composition with as above-mentioned b) water shown in composition.The viscosity of described lotion at 60 ℃ is preferably below 100Pas.
This surfactant paste is because its water ratio viscosity occurs to change significantly.For example, can, by the acid precursor of a) composition with in alkali cpd and this surfactant paste of modulation, now preferably regulate the amount of moisture of the alkali cpd using, modulation tool water ratio likely, the i.e. surfactant paste of tool viscosity likely.Conventionally in the time of known this anion surfactant contains 25~70 mass parts with respect to this anion surfactants of 100 mass parts water, can become the anion surfactant of the paste of reduced viscosity, operation can become easily, preferably uses the moisture of anion surfactant is adjusted to the surfactant paste within the scope of this in the present invention.
Scope as the amount of the water in surfactant paste, viewpoint from operability, preferably a) the composition with respect to 100 mass parts is 25~70 mass parts, more preferably 30~65 mass parts, are more preferably 35~65 mass parts, the amount of moisture in surfactant paste, viewpoint from operability, be preferably 20~41 quality %, more preferably 23~39 quality %, are more preferably 26~39 quality %.
In addition, the viewpoint of the operability from manufacturing, the viscosity of surfactant paste preferably, in the use temperature region of this surfactant paste, is preferably below 10Pas, more preferably below 5Pas, in addition, more than being similarly preferably 0.5Pas, more preferably more than 1Pas, from these viewpoints, be preferably 0.5~10Pas, more preferably 1~5Pas.As above-mentioned use temperature scope, the viewpoint from the stability of surfactant paste, is preferably 20~70 ℃, more preferably 20~60 ℃.At this, viscosity be rotational viscosimeter by coaxial dual round tube type (HAAKE manufactures, sensor: be SV-DIN) 50[1/s in velocity of shear] lower mensuration try to achieve.
The modulator approach of surfactant paste, without particular limitation of, known method can be used.The labile material of very unstable appearance in the acid precursor of this anion surfactant, preferably modulates can suppress the mode of its decomposition.For example, can use loop reactor (loop reactor), by heat exchanger etc., remove neutralization heat, while notice that the temperature of this acid precursor and surfactant paste manufactures.Temperature range during as manufacture, is preferably 30~60 ℃, as the storage temperature range after manufacturing, is preferably below 60 ℃.In addition, during use, can heat up as required, use surfactant paste.
The surfactant paste obtaining, the viewpoint from suppressing to decompose, preferably has excessive basicity.
The pH buffer reagent that can add when the saltcake of the by product in the time of also can containing unreacted alcohol while manufacturing acid precursor or unreacted Voranol EP 2001, neutralization reaction in this tensio-active agent, neutralization reaction, discoloring agent etc.
In this surfactant paste, as tensio-active agent, can use separately more than one that are formed by a) composition, also can be used together following tensio-active agent and use.And use in the situation that, can be in advance with contain a) surfactant paste of composition and mix use, also can add respectively.In addition, also with following tensio-active agent in the situation that, following tensio-active agent is preferably 1~70 mass parts with respect to a) composition of 100 mass parts, and more preferably 2~50 mass parts, are more preferably 3~30 mass parts.As described tensio-active agent, can enumerate alpha-sulfo fatty acid ester salt or secondary paraffin sulfonate.
(2-2) foam
In the present invention, use the foam of above-mentioned anionic surfactant compositions.Foam contains gaseous media (air, nitrogen, carbonic acid gas etc.) and forms in this anionic surfactant compositions.As gaseous media, from productive viewpoint, preferred air.
Described foam, for example, can obtain by entrained gas medium in anionic surfactant compositions.As the more specifically modulator approach of this foam, can enumerate batch-type, continous way.As batch-type, be to drop into this anionic surfactant compositions in the normally used mixing rolls such as batch-type kneader, under gaseous media exists, by carrying out the mixing gaseous media that is involved in of specified time, the method for modulation foam.
As continous way, be by this surfactant composition of specified amount and gaseous media are imported in high-speed rotary transfer part continuously, blending dispersion gaseous media, the method for modulation foam.
From the stability of physical property or the easiness of modulator approach and the productive viewpoint of the proportion of this foam etc., the preferably modulator approach of continous way.As an example of foaming machine that carries out the modulator approach of such continous way, can enumerate MDF series (Pacific Machinery & Engineering Co., Ltd. manufacture), BM series (Yanagiya Machinery Co., Ltd. manufactures) etc.
In batch-wise modulator approach, can control by the mixing time of this surfactant composition the proportion of this foam.
In addition, in the modulator approach of continous way, by regulating the flow with respect to the gaseous media of this surfactant composition, can control the proportion of this foam.As the scope of the volumetric flow rate of gaseous media, for example, be preferably the scope of 0.2 times to 10 times of the volumetric flow rate of this surfactant composition.Gaseous media is sneaked in anion surfactant and is preferably used foaming machine to carry out.
The temperature of the anionic surfactant compositions when supplying with in foaming machine, the viewpoint from the stability of surfactant paste, is preferably 20~70 ℃, more preferably 20~60 ℃.
The proportion of the foam of this anionic surfactant compositions obtaining, from the yield with good obtains, the detergent particles group's of low volume density viewpoint, is preferably 0.1~0.9, and more preferably 0.1~0.8, be more preferably 0.1~0.7.
In addition, content as anion surfactant in the detergent particles group who obtains in the present invention, from cleaning capacity and with detergent use powder raw material, form the viewpoint of granules, more than being preferably 5 quality % in detergent particles group, more preferably more than 10 quality %.In addition, from suppressing the viewpoint of the generation of big particle, be preferably below 50 quality %, more preferably below 40 quality %, from these viewpoints, as the above-mentioned content in detergent particles group, be preferably 5~50 quality %, more preferably 10~50 quality %, are more preferably 10~40 quality %.
In the present invention, (2) foam of anionic surfactant compositions has the ability that forms granules in conjunction with detergent use powder raw material, described in above-mentioned paragraph, this anionic surfactant compositions shows the feature that tackiness is the application when contacting with detergent use powder raw material.
Infer that the foam of this anionic surfactant compositions is when being added in detergent use powder raw material, moisture in this anionic surfactant compositions is due to the hydration of detergent use powder raw material or dissolving and seized, or in the situation that the temperature of detergent use powder raw material is lower than the temperature of this anion surfactant, because the temperature of the foam of this anionic surfactant compositions is reduced near its fusing point or below fusing point, the foam of this anionic surfactant compositions solidifies, and shows thus tackiness.
Like this, foam by this anionic surfactant compositions shows the granulation that tackiness is carried out detergent use powder raw material while being contacted with detergent use powder raw material, benchmark as its tackiness performance, more than viscosity when the foam of this anionic surfactant compositions contacts with detergent use powder raw material is preferably 2Pas, more preferably more than 3Pas.In addition, the viscosity of foam during contact, can be by rotational viscosimeter (the HAAKE manufacture of coaxial dual round tube type, sensor: be SV-DIN) 50[1/s in velocity of shear] condition under, same mode while contacting with the foam of this anionic surfactant compositions and detergent use powder raw material to become, regulates its temperature or moisture value to measure.
(3) other powder composition
In container rotary mixing machine, also can add in the lump the known material in " detergent use powder raw material " field that is generally used for detergent composition in addition.The amount of other powder composition in detergent particles group is preferably 1~30 quality %, more preferably 1~20 quality %.
As described material, can enumerate powder polymkeric substance (carboxylic acid polyalcohol, carboxymethyl cellulose, Zulkovsky starch, carbohydrate, polyoxyethylene glycol), water-insoluble vehicle (clay compound of silicon-dioxide, silicate hydrate compound, perlite, wilkinite etc. etc.) or granular tensio-active agent (lipid acid or its salt, linear alkylbenzene sulfonate, alkyl-sulphate etc.) in sequestrant (tri-polyphosphate, orthophosphoric acid salt, pyrophosphate salt etc., alkali metal aluminosilicate), water-soluble polymers.
Above-mentioned substance can add before the foam that adds this anionic surfactant compositions together with detergent use powder raw material, also can after the foam that has added this anionic surfactant compositions, add.In the situation that adding alkali metal aluminosilicate, due to by using and can realize the raising of mobility, the raising of storage stability as surface-modifying agent, therefore preferably after the foam that has added this anion surfactant, add.
(4) other liquid component
In the present invention, also can further add other liquid component and manufacture detergent particles group.As other liquid component adding, can suitably select according to the detergent particles group's who wants to obtain composition.The interpolation time of liquid component without particular limitation of, for example can be pre-mixed in this anionic surfactant compositions, also can be before the foam that adds this anionic surfactant compositions or in its process, or after carry out, in the situation that adding surface-modifying agent, preferably before the interpolation of surface-modifying agent.
In the situation that add liquid component after the foam of this anionic surfactant compositions of interpolation; can in container rotary mixing machine, add this liquid component; also can be after by the detergent particles group amount discharge container rotary mixing machine obtaining by manufacture method of the present invention; the detergent particles group who obtains is dropped in other mixing machine/tablets press, add therein this liquid component.
As liquid component, such as enumerating the liquid component arbitrarily for common detergent composition such as nonionogenic tenside or lipid acid, water-soluble polymers (carboxylic acid polyalcohol, carboxymethyl cellulose, Zulkovsky starch, carbohydrate, polyoxyethylene glycol etc.).Liquid component can only be used a kind of composition, also can be used together two or more compositions.As liquid component, can at temperature more than fusing point, as liquid, add at it, or also can add with the form of the aqueous solution or dispersion liquid.As the amount of removing the actual liquid component after medium, from suppressing the viewpoint of detergent particles group's aggegation, be preferably below detergent particles group's the 15 quality % of final product, more preferably below 10 quality %.
As the nonionogenic tenside as liquid component, without particular limitation of, but from cleaning the viewpoint of power, for example, on the alcohol that is preferably 10~14 at carbonatoms, addition has the polyoxyalkylene alkyl of the olefin oxide of 6~22 moles.
As the addition means of these liquid components, do not rely on many fluid tips of recording in the present invention, can use nozzle arbitrarily to spray.
B. detergent particles group's manufacture method
In manufacture method of the present invention, have by using container rotary mixing machine that the foam of anionic surfactant compositions is sparged in this mixing machine, detergent use powder raw material is carried out to the operation of granulation.When adding the foam of this anionic surfactant compositions, can be by carrying out granulation by multithread body nozzle spray in this container rotary mixing machine.
As the amount of the foam of the anionic surfactant compositions of being sprayed, preferably the detergent use powder raw material with respect to 100 mass parts is 20~100 mass parts, more preferably 25~90 mass parts.Viewpoint from clean power, more than being preferably 20 mass parts, from granulation yield, deliquescent viewpoint, is preferably below 100 mass parts.
(1) container rotary mixing machine
As container rotary mixing machine, preferred drum mixer or pan mixer.As drum mixer; so long as the cylinder of drum type being just not particularly limited of rotating to process, except level or the drum mixer that tilts a little, can also use circular cone drum granulator (mixing machine), multistage circular cone drum granulator (mixing machine) etc.These devices can be used in the either method of batch-type, continous way.
In addition, the wall friction coefficient between detergent particles group and the inwall of container rotary mixing machine is little, is difficult to detergent particles group to apply in the situation of sufficient upward movement power, and a plurality of baffle plates (baffle) can be installed on container inner wall.Can make thus particle swarm carry out upward movement, improve powder Combination and solid-liquid Combination.
Operating condition as container rotary mixing machine, so long as the condition of the composition in can stirring mixer is all not particularly limited, the operating condition that the defined Froude number of preferred following formula is 0.005~1.0, more preferably 0.01~0.6 operating condition.
Froude number: Fr=V 2/ (R * g)
V: circumferential speed [m/s]
R: the radius of the circumference from rotation center to whirl [m]
G: universal gravity constant [m/s 2]
(2) many fluid tips
In the present invention, the foam that uses many fluid tips to supply with this anionic surfactant compositions is a technical characterictic.By using described nozzle, even if the so higher flow composition of viscosity ratio of above-mentioned surfactant paste or its foam also can make it its drop miniaturization to disperse.Many fluid tips be by liquid and for micronize gas (air, nitrogen etc.) by stream independently, make it to be circulated near the nozzle that carries out hybrid fine particles nozzle tip end, can use two-fluid spray nozzle or three fluid tips, four fluid tips etc.In these many fluid tips, from the viewpoint of the easiness operating or the easiness obtaining, preferably two-fluid spray nozzle.
In the present invention, preferably the foam of this anionic surfactant compositions and micronize are mixed with gas, make it micronize.Type as the foam of this anionic surfactant compositions and micronize with the mixing position of gas can be the internal mix type of mixing in nozzle tip end or any in the external mix type of mixing outside nozzle tip end.
As so many fluid tips, can enumerate Spraying Systems Japan K.K. manufacture, Kyoritsu Gokin Co., Ltd.'s manufacture, H.IKEUCHI CO., LTD. internal mix type two-fluid spray nozzle, the Spraying Systems Japan K.K. manufacturing etc. manufactures, Kyoritsu Gokin Co., Ltd. manufactures, ATOMAX Co., the external mix type two-fluid spray nozzle that Ltd. manufactures etc., external mix type four fluid tips that Fujisaki Electric Co., Ltd. manufactures etc.
In addition, the droplet dia about the drop of the foam of this anionic surfactant compositions, can regulate by the balance of the flow of gas by changing its flow and micronize.That is, with respect to the foam of this anionic surfactant compositions of certain certain flow, more increase the flow of gas for micronize, it is less that droplet dia becomes.Further, with respect to the micronize of certain certain flow, more reduce the flow of the foam of this anionic surfactant compositions with gas, droplet dia is less.Droplet dia is less,, more increases the flow of gas for micronize that is, owing to can being reduced coarse grain by the drop of miniaturization, that is, can improve yield.
On the other hand, this foam is subject to by the shearing force that is supplied to the micronize use γ-ray emission in many fluid tips, and this foam bubble burst easily causes the rising of the proportion of this foam.Therefore, preferably can suppress the mode of rising of the proportion of this foam, regulate the flow of gas for the micronize that is supplied in many fluid tips.That is, in the present invention, in order to take into account the rising of the proportion that reduces coarse grain and suppress this foam, there is the flow of gas for applicable micronize.
Applicable micronize with the flow of gas according to the kind of the many fluid tips that use and difference, at the consideration [volumetric flow rate (cm of the foam of anionic surfactant compositions 3in the situation of the parameter of/min)]/[flow (L/min) of gas for micronize], from the yield with good obtains, the detergent particles group's of low volume density viewpoint, is preferably 0.5~30cm 3/ L, more preferably 1~20cm 3/ L.Using ATOMAX Co., in the situation of the two-fluid spray nozzle BN90 that Ltd. manufactures, preferred above-mentioned scope.
As the droplet dia of using the foam of this anionic surfactant compositions after multithread body nozzle spray, preferably median size is 10~500 μ m.
In addition, the median size of the droplet dia of the foam of this anionic surfactant compositions is calculated based on dimension criteria, is to use laser diffraction formula particle size distribution device: the value of the manufacture of Spraytec(Malvern company) measuring.
Proportion with the foam of this anionic surfactant compositions after multithread body nozzle spray, the detergent particles group's of low volume density viewpoint from yield obtains well, be preferably 0.1~0.95, more preferably 0.2~0.95, be more preferably 0.2~0.85.
In addition, in the situation that hope improves the interpolation speed of the foam of this anionic surfactant compositions, use a plurality of these many fluid tips, maintain the miniaturization of drop and improve interpolation speed also effective.
By using the method for the foam of such container rotary mixing machine, anion surfactant and multithread body nozzles combine, even also can disperse equably in the foam of anionic surfactant compositions, obtain that yield improved in the detergent particles group of low volume density.
C. the detergent composition and the manufacture method thereof that contain detergent particles group
The detergent particles group who manufactures according to the method described above can directly be used as detergent composition, also can be by the composition that is further added with desirable composition as detergent composition.That is, detergent composition of the present invention is at least to contain the detergent particles group who obtains by manufacture method of the present invention to form.
As the composition adding, such as enumerating lotion-aid particle, fluorescence dye, enzyme, spices, defoamer, SYNTHETIC OPTICAL WHITNER, bleach-activating agent etc.Described composition can make an addition in container rotary mixing machine after having added this anionic surfactant compositions, or also can, by after in the detergent particles group amount discharge container rotary mixing machine being obtained by manufacture method of the present invention, use other mixing machine to add.
D. physical property and evaluation
As detergent particles group's who obtains by the present invention etc. physical property, can enumerate volume density or mobility, median size.In addition, as the physical property that becomes productive index, can enumerate granulation yield.In addition, as the physical property that becomes deliquescent index, can enumerate 60 seconds dissolution rates and granular sensation extinction time.As detergent particles group's volume density, from the viewpoint of 60 seconds dissolution rates and granular sensation extinction time excellence, in low volume density be preferably 250~690g/L, more preferably 250~650g/L, is more preferably 300~600g/L.As detergent particles group's median size, from improving the viewpoint of the granulation yield of detergent particles, be preferably 200~800 μ m, more preferably 200~600 μ m.As detergent particles group's mobility, the viewpoint from the operability excellence of detergent particles, is preferably 4~12 seconds, more preferably 4~10 seconds, is more preferably 4~8 seconds.As granulation yield, be preferably the degree that more approaches 100%, for example, be preferably 80~100%, more preferably 90~100%.
To the measuring method of detergent particles group's etc. physical property as described below.
The measuring method > of < physical property
1. volume density
Volume density is measured by the method for recording as apparent density in JIS K3362:2008.In addition, volume density is measured with residual particle after removing the particle on the sieve that residues in 2000 μ m.
2. mobility
Mobility is that the powder of 100mL flows out the needed time from the funnel (hopper) of the apparent density mensuration use of JIS K3362:2008 record.In funnel due to bridge joint etc. cause powder at 60 seconds with interior do not flow out in the situation that, mobility is decided to be 60<.In addition, mobility use the particle remove on the sieve that residues in 2000 μ m after remaining particle measure.
3. median size
About median size, after the metal-made mesh screen (order footpath 2000~45 μ m) that uses JIS Z8801-1:2006 to record carries out vibration in 5 minutes, by the massfraction of the size of mesh, calculate median particle diameter.Say in further detail, using order footpath is 45 μ m, 63 μ m, 90 μ m, 125 μ m, 180 μ m, 250 μ m, 355 μ m, 500 μ m, 710 μ m, 1000 μ m, 1410 μ m, the sieve of 12 grades of 2000 μ m and connect dish, connecing on dish according to starting lamination successively from the little sieve in order footpath, from the sieve of 2000 μ m of topmost, add the particle of 100g, cover lid, (HEIKO makes manufacturing to be installed on Ro-Tap type sieve shaker, knock 156 beats/min, rock 290 beats/min), after vibrating 5 minutes, mensuration residues in each sieve and connects the quality of this particle on dish, calculate the mass ratio (%) of this particle on each sieve.From connecing dish, add up in order the mass ratio of this particle the little sieve in order footpath, will add up to 50% particle diameter as median size.
Further, when the mensuration of above-mentioned detergent particles group's median size, the value that the ratio that represents to residue in the detergent particles group on each sieve that order footpath is 1000 μ m, 1410 μ m and 2000 μ m with quality % is obtained is tried to achieve as coarse grain (1000 μ mON) rate.Similarly, using representing to residue in quality %, to connect dish and order footpath be that the value that the ratio of the detergent particles group on each sieve of 45 μ m, 63 μ m, 90 μ m obtains is tried to achieve as micro mist (125 μ mPASS) rate.
4. granulation yield
Granulation yield in the present invention means the ratio of the quality of the particle below 2000 μ m in the detergent particles group who makes.
5.60 second dissolution rate
For 60 seconds dissolution rates, by following method, calculate.
The hardness of 1L is equivalent to 71.2mgCaCO 3/ L is also adjusted to the hard water (Ca/Mg mol ratio is 7/3) of 10 ℃ and fills beaker in 1L (internal diameter is 105mm, it is highly the round shape of 150mm, for example, the 1L glass beaker that Yan Cheng nitre Subsidiary Company manufactures), the water temperature of 10 ℃ is being kept with water-bath under certain state, with stirrer, (length is 35mm, diameter is 8mm, model for example: ADVANTEC company manufactures, TEFLON(registered trademark) the circular thin type of SA()) with the degree of depth of whirlpool, with respect to the depth of water, being about 1/3 rotating speed (800r/m) stirs.The detergent particles group who under agitation division weighing is become to 1.0000 ± 0.0010g drops into and is scattered in water, continues to stir.After input starts 60 seconds, the detergent particles group dispersion liquid in beaker is filtered with the metal-made mesh screen (diameter is 100mm) that the order footpath that the known JIS Z8801-1:2006 of quality records is 74 μ m, the detergent particles group who residues in the saturation state on sieve is recovered in the known open container of quality together with sieve.In addition, will be decided to be 10 ± 2 seconds from filtering the operating time starting to reclaiming sieve.By dry 1 hour of the electric drying apparatus that is heated to 105 ℃ for the detergent particles group's of recovery dissolution residual substance, afterwards, the moisture eliminator of silica gel (25 ℃) is housed in, maintenance 30 minutes is cooling.After cooling, measure the total quality of dissolution residual substance, sieve and the returnable of dried washing composition, through type (1) is calculated detergent particles group's dissolution rate (%).
60 seconds dissolution rates (%)=1-(T/S) } * 100 ... (1)
S: detergent particles group's input quality (g)
T: when the aqueous solution obtaining being supplied in to above-mentioned sieve under above-mentioned agitation condition, residue in the dry mass (g) of the dissolution residual substance of the detergent particles group on sieve
6. granular sensation extinction time
Granular sensation extinction time is measured by following method.
Packing the water of 3L20 ℃ into diameter is in 35cm, the degree of depth washbowl that is 12cm, after 15g detergent particles group is made an addition in washbowl gently, the time (second) disappearing for the granular sensation of the detergent particles group with the speed friction washbowl bottom surface of 1 time per second time with palm.
The measuring method > of the proportion of the foam of < anionic surfactant compositions
The proportion of the foam of the anionic surfactant compositions obtaining by foaming machine, by using in advance the aquametry of 20 ℃ arbitrarily after the volume of container, on one side the foam of the anionic surfactant compositions of discharging from foaming machine outlet is slowly made an addition to this container and repeats to knock on one side, not produce the mode in space between foam and foam, do not fill, volume by the quality of the foam obtaining divided by this container, the lower mensuration of the temperature when foaming (being to be supplied to the temperature in foaming machine in the situation that using foaming machine).The proportion of the foam of the anionic surfactant compositions after spraying, by the anionic surfactant compositions after spraying is reclaimed with containers such as polyethylene sack or buckets, is used with above-mentioned same method and is measured at the temperature when spraying.In addition, as long as do not record in addition in this specification sheets, proportion is the proportion of the density of the water with respect to 20 ℃.
About above-mentioned embodiment, the present invention is open following manufacture method further.
A <1> detergent particles group's manufacture method, wherein, described detergent particles group's manufacture method has the container of use rotary mixing machine and detergent use powder raw material is carried out to the operation of granulation, the foam of anionic surfactant compositions is carried out in this container rotary mixing machine to the granulation of this detergent use powder raw material by multithread body nozzle spray.
The manufacture method of <2> as described in above-mentioned <1>, wherein, with the proportion of the foam of this anionic surfactant compositions after multithread body nozzle spray, be 0.1~0.95, be preferably 0.2~0.95, be more preferably 0.2~0.85.
The manufacture method of <3> as described in above-mentioned <1> or <2>, wherein, the foam of anionic surfactant compositions obtains by entrained gas medium in anionic surfactant compositions.
The manufacture method of <4> as described in above-mentioned <3>, wherein, is used foaming machine to carry out to entrained gas medium in anionic surfactant compositions.
The manufacture method of <5> as described in above-mentioned <3> or <4>, wherein, gaseous media is air.
The manufacture method of <6> as described in any one in above-mentioned <1>~<5>, wherein, many fluid tips are two-fluid spray nozzle.
The manufacture method of <7> as described in any one in above-mentioned <1>~<6>, wherein, anion surfactant is to contain following a) composition and b) surfactant paste of composition.
A) be selected from a kind of above anion surfactant in the salt of the salt of linear alkyl benzene sulphonic acid, the salt of alkylsurfuric acid and polyxyethylated sulfuric acid,
B) the above-mentioned a) composition with respect to 100 mass parts is 25~70 mass parts, is preferably 30~65 mass parts, more preferably the water of 35~65 mass parts.
The manufacture method of <8> as described in any one in above-mentioned <1>~<7>, wherein, spraying is 20~100 mass parts with respect to the detergent use powder raw material of 100 mass parts, is preferably the foam of the anionic surfactant compositions of 25~90 mass parts.
The manufacture method of <9> as described in any one in above-mentioned <1>~<8>, wherein, detergent use powder raw material is water-soluble solid alkali inorganic substance and/or water-soluble inorganic salt.
The manufacture method of <10> as described in any one in above-mentioned <1>~<9>, wherein, in detergent particles group, the content of detergent use powder raw material is more than 10 quality %, more than being preferably 20 quality %, be preferably below 80 quality %, be preferably 10~80 quality %, more preferably 20~80 quality %.
The manufacture method of <11> as described in any one in above-mentioned <1>~<10>, wherein, detergent use powder raw material is sodium carbonate and/or sodium sulfate, is preferably light ash.
The manufacture method of <12> as described in any one in above-mentioned <7>~<11>, wherein, the anion surfactant of above-mentioned a) composition is 10~18 for being selected from carbonatoms, the salt of the linear alkyl benzene sulphonic acid that preferably carbonatoms is 12~16, carbonatoms is 10~18, salt and the carbonatoms of the alkylsurfuric acid that preferably carbonatoms is 12~16 are 10~18, in the salt of the polyxyethylated sulfuric acid that preferably carbonatoms is 12~16 more than a kind.
The manufacture method of <13> as described in any one in above-mentioned <1>~<12>, wherein, the content of the anion surfactant in detergent particles group is more than 5 quality %, more than being preferably 10 quality %, be preferably below 50 quality %, more preferably below 40 quality %, be preferably 5~50 quality %, more preferably 10~50 quality %, are more preferably 10~40 quality %.
The manufacture method of <14> as described in any one in above-mentioned <1>~<13>, wherein, container rotary mixing machine is drum mixer or pan mixer.
The manufacture method of <15> as described in any one in above-mentioned <1>~<14>, wherein, the proportion of the foam of anionic surfactant compositions is 0.1~0.9, be preferably 0.1~0.8, be more preferably 0.1~0.7.
The manufacture method of <16> as described in any one in above-mentioned <1>~<15>; wherein; many fluid tips are the nozzle that the foam of anionic surfactant compositions and micronize are mixed with gas, the [volumetric flow rate (cm of the foam of anionic surfactant compositions 3the scope of the value of/min)]/[flow (L/min) of gas for micronize] is 0.5~30cm 3/ L, is preferably 1~20cm 3/ L.
The manufacture method of <17> as described in any one in above-mentioned <1>~<16>, wherein, the detergent particles group's who obtains volume density is 250~690g/L, be preferably 250~650g/L, more preferably 300~600g/L.
The manufacture method of <18> as described in any one in above-mentioned <1>~<17>, wherein, container rotary mixing machine to pass through the Froude number that following formula tries to achieve be 0.005~1.0, be preferably the granulation of carrying out detergent use powder raw material under 0.01~0.6 operating condition.
Froude number: Fr=V 2/ (R * g)
V: circumferential speed [m/s]
R: the radius of the circumference from rotation center to whirl [m]
G: universal gravity constant [m/s 2]
Embodiment
Below, based on embodiment, wait the present invention is described in further detail, but the present invention is not only limited to described embodiment.
In following embodiment, as long as no special record, just use following raw material.In addition, the % of the composition in table represents quality %.
Polyxyethylated sodium sulfate (purity 70%, excess water; The carbonatoms of alkyl is C12/C14=70/30), flower king manufactures " EMAL270J "
Sodium alkyl sulfate (purity 66%, excess water; The carbonatoms of alkyl is C12/C14/C16=64/24/12(quality %))
Sodium dodecylbenzene sulfonate (purity 65%, excess water), flower king manufactures " NEOPELEX G-65 "
Light ash: median size is 100 μ m, Central Glass Co., Ltd. manufactures
Pulverize light ash: (by above-mentioned light ash pulverize for median size be the material after 10 μ m)
Sodium sulfate: median size is 200 μ m, " the neutral thenardite " that Shikoku Chem manufactures
Pulverize sodium sulfate: above-mentioned sodium sulfate is crushed to the material that median size is 22 μ m
Zeolite: median size is 3.5 μ m, ZEOBUILDER company manufactures
Sodium polyacrylate: Kao Corp manufactures, the material of weight-average molecular weight 10000 (purity 40%)
Polyoxyethylene glycol: Kao Corp manufactures, the material that weight-average molecular weight is 13000 (purity 60%)
In following embodiment etc., as container rotary mixing machine, will there is the 75L drum mixer (φ 40cm * L60cm) of baffle plate, the mode that becomes downside with the bottom of mixing machine is from 14 ° of uses of horizontal tilt.As many fluid tips, (ATOMAX Co., Ltd. manufactures, model: BN90) to use a two-fluid spray nozzle.The temperature of the foam of the anion surfactant while being supplied to two-fluid spray nozzle is decided to be 60 ℃.In addition, the foam of anionic surfactant compositions is used the foaming machine MDFO(Pacific Machinery & Engineering Co. of continous way, and Ltd. manufactures) modulate.When being supplied in foaming machine, the temperature of said composition is decided to be 60 ℃.
Embodiment 1(detergent particles group's modulation)
The Sodium dodecylbenzene sulfonate of 60 ℃ of the sodium alkyl sulfate of 60 ℃ of 100 mass parts and 135 mass parts is mixed to modulation anionic surfactant compositions.The surfactant paste that the anionic surfactant compositions making is the water that contains 52.8 mass parts with respect to the anion surfactant of 100 mass parts.In addition, the viscosity of this lotion at 60 ℃ is 1.7Pas.
The light ash of 1.81kg, 3.42kg are pulverized to sodium sulfate and make an addition in drum mixer as detergent use powder raw material, are to stir 30 seconds for 0.2 time at Froude number.Continue afterwards to stir, the foam of the anionic surfactant compositions that 1.55kg is modulated by above-mentioned MDFO is that the volumetric flow rate/micronize of 80L/min(foam is 5.3cm with the flow of gas with gas in 17 minutes interpolation time, micronize 3/ L) under spray condition, with two-fluid spray nozzle, add, after adding, stir 1 minute.That is, at 60 ℃, spraying is this foam of 29.6 mass parts with respect to the detergent use powder raw material of 100 mass parts.Stop afterwards stirring, add 0.22kg zeolite, under condition same as described above, carry out the stirring of 1 minute, the granules obtaining is discharged as detergent particles group from drum mixer.
In addition, the flow of the mixed gas in foaming machine is 0.50L/min, and the proportion of the foam of the anionic surfactant compositions obtaining by foaming machine is 0.20.In addition, the proportion of the foam of the anionic surfactant compositions after spraying by two-fluid spray nozzle, by the shearing force lather collapse with γ-ray emission by micronize, is 0.85.The detergent particles group's who obtains composition and physical property are shown in Table 1.
Embodiment 2
Sodium alkyl sulfate is adjusted to 60 ℃, as anionic surfactant compositions.The surfactant paste that the anionic surfactant compositions making is the water that contains 51.52 mass parts with respect to the anion surfactant of 100 mass parts.In addition, the viscosity of this lotion at 60 ℃ is 1.4Pas.
4.20kg being pulverized to sodium sulfate and as detergent use powder raw material, make an addition in drum mixer, is to stir 30 seconds for 0.2 time at Froude number.Afterwards, continuing to stir, is 33 minutes by the foam of the anionic surfactant compositions of 2.80kg modulation in the interpolation time, and micronize is that the volumetric flow rate/micronize of 80L/min(foam is 5.3cm with the flow of gas with gas 3/ L) under spray condition, with two-fluid spray nozzle, add, after adding, stir 1 minute.That is, at 60 ℃, spraying is this foam of 66.7 mass parts with respect to the detergent use powder raw material of 100 mass parts.Stop afterwards stirring, the granules obtaining is discharged as detergent particles group from drum mixer.
In addition, the flow of the mixed gas in foaming machine is 0.50L/min, and the proportion of the foam of the anionic surfactant compositions obtaining by foaming machine is 0.20.In addition, by the spray proportion of foam of the anionic surfactant compositions that obtains of two-fluid spray nozzle, by micronize, using the shearing force lather collapse of γ-ray emission is 0.85.The detergent particles group's who obtains composition and physical property are shown in Table 1.
Embodiment 3
Except making micronize, by volumetric flow rate/micronize that the flow of gas is 42L/min(foam, with the flow of gas, be 10.0cm 3/ L), outside, under condition similarly to Example 2, carry out granulation.By the spray proportion of foam of the anionic surfactant compositions that obtains of two-fluid spray nozzle, be 0.68.The detergent particles group's who obtains composition and physical property are shown in Table 1.
Embodiment 4
Sodium alkyl sulfate is adjusted to 60 ℃, as anionic surfactant compositions.
The light ash of 4.20kg is made an addition in drum mixer as detergent use powder raw material, is to stir 30 seconds for 0.2 time at Froude number.Afterwards, continuing to stir, is 33 minutes by the foam of the anionic surfactant compositions of 2.80kg modulation in the interpolation time, and micronize is that the volumetric flow rate/micronize of 80L/min(foam is 5.3cm with the flow of gas with gas 3/ L) under spray condition, with two-fluid spray nozzle, add, after adding, stir 1 minute.That is, at 60 ℃, spraying is this foam of 66.7 mass parts with respect to the detergent use powder raw material of 100 mass parts.Stop afterwards stirring, the granules obtaining is discharged as detergent particles group from drum mixer.
In addition, the flow of the mixed gas in foaming machine is 0.50L/min, and the proportion of the foam of the anionic surfactant compositions obtaining by foaming machine is 0.20.In addition, by the spray proportion of foam of the anionic surfactant compositions that obtains of two-fluid spray nozzle, by micronize, using the shearing force lather collapse of γ-ray emission is 0.85.The detergent particles group's who obtains composition and physical property are shown in Table 1.
Embodiment 5
Except making the amount of the mixed gas in foaming machine, be 0.10L/min, the proportion of the foam of the anionic surfactant compositions obtaining by foaming machine is that the volumetric flow rate/micronize of 0.58(foam is 1.8cm with the flow of gas 3/ L) in addition, under condition similarly to Example 4, carry out granulation.By the spray proportion of foam of the anionic surfactant compositions that obtains of two-fluid spray nozzle, with same method lather collapse, be 0.85.The detergent particles group's who obtains composition and physical property are shown in Table 1.
Embodiment 6
Sodium alkyl sulfate is adjusted to 60 ℃, as anionic surfactant compositions.The surfactant paste that the anionic surfactant compositions of modulation is the water that contains 51.52 mass parts with respect to the anion surfactant of 100 mass parts.In addition, the viscosity of this lotion at 60 ℃ is 1.4Pas.
4.20kg being pulverized to sodium sulfate and as detergent use powder raw material, make an addition in drum mixer, is to stir 30 seconds for 0.2 time at Froude number.Afterwards, continuing to stir, is 34.6 minutes by the foam of the anionic surfactant compositions of 2.80kg modulation in the interpolation time, and micronize is that the volumetric flow rate/micronize of 32L/min(foam is 12.6cm with the flow of gas with gas 3/ L) under spray condition, with two-fluid spray nozzle, add, after adding, stir 1 minute.That is, at 60 ℃, spraying is this foam of 66.7 mass parts with respect to the detergent use powder raw material of 100 mass parts.Stop afterwards stirring, the granules obtaining is discharged as detergent particles group from drum mixer.
In addition, the flow of the mixed gas in foaming machine is 0.50L/min, and the proportion of the foam of the anionic surfactant compositions obtaining by foaming machine is 0.20.In addition, by the spray proportion of foam of the anionic surfactant compositions that obtains of two-fluid spray nozzle, using the shearing force lather collapse of γ-ray emission by micronize, is 0.44.The detergent particles group's who obtains composition and physical property are shown in Table 1.
Embodiment 7
Sodium alkyl sulfate is adjusted to 60 ℃, as anionic surfactant compositions.The surfactant paste that the anionic surfactant compositions of modulation is the water that contains 51.52 mass parts with respect to the anion surfactant of 100 mass parts.In addition, the viscosity of this lotion at 60 ℃ is 1.4Pas.
0.93kg being pulverized to gently ash, 4.07kg and pulverize sodium sulfate and make an addition in drum mixer as detergent use powder raw material, is to stir 30 seconds for 0.2 time at Froude number.Afterwards, continue to stir, the interpolation time by the foam of the anionic surfactant compositions of 2.01kg modulation with 22.6 minutes is that the volumetric flow rate/micronize of 29L/min(foam is 15.2cm with the flow of gas with gas in micronize 3/ L) under spray condition, with two-fluid spray nozzle, add, after adding, stir 1 minute.That is, at 60 ℃, spraying is this foam of 40.2 mass parts with respect to the detergent use powder raw material of 100 mass parts.Stop afterwards stirring, the granules obtaining is discharged as detergent particles group from drum mixer.
In addition, the flow of the mixed gas in foaming machine is 0.50L/min, and the proportion of the foam of the anionic surfactant compositions obtaining by foaming machine is 0.20.In addition, by the spray proportion of foam of the anionic surfactant compositions that obtains of two-fluid spray nozzle, using the shearing force lather collapse of γ-ray emission by micronize, is 0.39.The detergent particles group's who obtains composition and physical property are shown in Table 1.
Embodiment 8
Sodium alkyl sulfate is adjusted to 60 ℃, as anionic surfactant compositions.The surfactant paste that the anionic surfactant compositions of modulation is the water that contains 51.52 mass parts with respect to the anion surfactant of 100 mass parts.In addition, the viscosity of this lotion at 60 ℃ is 1.4Pas.
2.00kg being pulverized to gently ash, 2.03kg and pulverize sodium sulfate and make an addition in drum mixer as detergent use powder raw material, is to stir 30 seconds for 0.2 time at Froude number.Continue afterwards to stir, the interpolation time by the foam of the anionic surfactant compositions of 2.24kg modulation with 26.4 minutes is that the volumetric flow rate/micronize of 28L/min(foam is 15.1cm with the flow of gas with gas in micronize 3/ L) under spray condition, with two-fluid spray nozzle, add, after adding, stir 1 minute.That is, at 60 ℃, spraying is this foam of 55.7 mass parts with respect to the detergent use powder raw material of 100 mass parts.
Next; the polyoxyethylene glycol of the sodium polyacrylate of 0.19kg60 ℃ and 0.025kg60 ℃ is made an addition to pressure to be carried with kettle (jacketed; jacket temperature is 60 ℃) in; in kettle, by air, apply 0.1MPa pressure; the opening degree of the control valve of kettle outlet is only opened to 90 degree; pressure is carried; in drum mixer, use two-fluid spray nozzle (ATOMAX Co.; Ltd. manufacture; BN90) take spray time as 2.0 minutes; at micronize gas, be to add under 80L/min, after adding, stir 1 minute.Stop afterwards stirring, add the zeolite of 0.19kg, with above-mentioned same condition under carry out the stirring of 1 minute, the granules obtaining is discharged as detergent particles group from drum mixer.
In addition, the flow of the mixed gas in foaming machine is 0.50L/min, and the proportion of the foam of the anionic surfactant compositions obtaining by foaming machine is 0.20.In addition, by the spray proportion of foam of the anionic surfactant compositions that obtains of two-fluid spray nozzle, be 0.36 use the shearing force lather collapse of γ-ray emission by micronize after.The detergent particles group's who obtains composition and physical property are shown in Table 1.
Embodiment 9
Polyxyethylated sodium sulfate is adjusted to 60 ℃, as anionic surfactant compositions.The surfactant paste that the anionic surfactant compositions of modulation is the water that contains 42.86 mass parts with respect to the anion surfactant of 100 mass parts.In addition, the viscosity of this lotion at 60 ℃ is 1.9Pas.
The light ash of 4.67kg is made an addition in drum mixer as detergent use powder raw material, is to stir 30 seconds for 0.2 time at Froude number.Continue afterwards to stir, the interpolation time by the foam of the anionic surfactant compositions of 2.00kg modulation with 15.3 minutes is that the volumetric flow rate/micronize of 30L/min(foam is 13.6cm with the flow of gas with gas in micronize 3/ L) under spray condition, with two-fluid spray nozzle, add, after adding, stir 1 minute.That is, at 60 ℃, spraying is this foam of 42.83 mass parts with respect to the detergent use powder raw material of 100 mass parts.Stop afterwards stirring, add 0.33kg zeolite, in condition same as described above, carry out the stirring of 1 minute, the granules obtaining is discharged as detergent particles group from drum mixer.
In addition, the flow of the mixed gas in foaming machine is 0.29L/min, and the proportion of the foam of the anionic surfactant compositions obtaining by foaming machine is 0.32.In addition, by the spray proportion of foam of the anionic surfactant compositions that obtains of two-fluid spray nozzle, by micronize, using after the shearing force lather collapse of γ-ray emission is 0.67.The detergent particles group's who obtains composition and physical property are shown in Table 1.
Comparative example 1
The Sodium dodecylbenzene sulfonate of 60 ℃ of the sodium alkyl sulfate of 60 ℃ of 100 mass parts and 135 mass parts is mixed to modulation anionic surfactant compositions.
The light ash of 1.81kg, 3.42kg are pulverized to sodium sulfate and make an addition in drum mixer as detergent use powder raw material, are to stir 30 seconds for 0.2 time at Froude number.Continuing afterwards to stir, the anionic surfactant compositions of 1.55kg modulation be take to the interpolation time as 17 minutes, is that the volumetric flow rate/micronize of 80L/min(said composition is 1.1cm with the flow of gas with gas in micronize 3/ L) under spray condition, with two-fluid spray nozzle, add, after adding, stir 1 minute.That is, at 60 ℃, spraying is the said composition of 29.64 mass parts with respect to the detergent use powder raw material of 100 mass parts.Stop afterwards stirring, add 0.22kg zeolite, with above-mentioned same condition under carry out the stirring of 1 minute, from drum mixer, discharge the granules obtaining, as detergent particles group.
In addition, the proportion of this surfactant composition is 1.0, and the proportion after spraying by two-fluid spray nozzle is also 1.0.The detergent particles group's who obtains composition and physical property are shown in Table 1.
Comparative example 2
Sodium alkyl sulfate is adjusted to 60 ℃, as anionic surfactant compositions.
4.20kg being pulverized to sodium sulfate and as detergent use powder raw material, make an addition in drum mixer, is to stir 30 seconds for 0.2 time at Froude number.Afterwards, continuing to stir, the anionic surfactant compositions of 2.80kg modulation be take to the interpolation time as 33 minutes, is that the volumetric flow rate/micronize of 80L/min(said composition is 1.1cm with the flow of gas with gas in micronize 3/ L) under spray condition, with two-fluid spray nozzle, add, after adding, stir 1 minute.That is, at 60 ℃, spraying is the said composition of 66.7 mass parts with respect to the detergent use powder raw material of 100 mass parts.Stop afterwards stirring, the granules obtaining is discharged from drum mixer, as detergent particles group.
In addition, the proportion of this surfactant composition is 1.0, and the proportion after spraying by two-fluid spray nozzle is also 1.0.The detergent particles group's who obtains composition and physical property are shown in Table 1.
Comparative example 3
Sodium alkyl sulfate is adjusted to 60 ℃, as anionic surfactant compositions.
4.20kg being pulverized to sodium sulfate and as detergent use powder raw material, make an addition in drum mixer, is to stir 30 seconds for 0.2 time at Froude number.Afterwards, continue to stir, the foam of the anionic surfactant compositions of 2.80kg modulation be take to the interpolation time as 33 minutes, under the spray condition that is 0L/min with gas in micronize, with two-fluid spray nozzle, add, after adding, stir 1 minute.That is, at 60 ℃, spraying is this foam of 66.7 mass parts with respect to the detergent use powder raw material of 100 mass parts.Stop afterwards stirring, the granules obtaining is discharged from drum mixer, as detergent particles group.
In addition, the flow of the mixed gas in foaming machine is 0.50L/min, and the proportion of the foam of the anionic surfactant compositions obtaining by foaming machine is 0.20.The proportion of the foam of the anionic surfactant compositions adding by two-fluid spray nozzle in addition, is 0.20.This is considered to owing to not following the supply of gas for micronize, thereby there is no the result of the lather collapse that generation causes by the shearing force of this γ-ray emission.The detergent particles group's who obtains composition and physical property are shown in Table 1.
Comparative example 4
Polyxyethylated sodium sulfate is adjusted to 60 ℃, as anionic surfactant compositions.The light ash of 4.33kg is made an addition in drum mixer as detergent use powder raw material, is to stir 30 seconds for 0.2 time at Froude number.Afterwards, continuing to stir, is 18 minutes by the anionic surfactant compositions of 2.33kg modulation in the interpolation time, and micronize is that the volumetric flow rate/micronize of 80L/min(said composition is 1.5cm with the flow of gas with gas 3/ L) under spray condition, with two-fluid spray nozzle, add, after adding, stir 1 minute.That is, at 60 ℃, spraying is the said composition of 53.8 mass parts with respect to the detergent use powder raw material of 100 mass parts.Stop afterwards stirring, add 0.66kg zeolite, with above-mentioned same condition under carry out the stirring of 1 minute, from drum mixer, discharge the granules obtaining, as detergent particles group.
In addition, the proportion of this surfactant composition is 1.08, and the proportion after spraying by two-fluid spray nozzle is also 1.08.The detergent particles group's who obtains composition and physical property are shown in Table 1.
[table 1]
The detergent particles group's who obtains in embodiment 1~9 volume density is 444~682g/L.In addition, granulation yield is more than 96%, the detergent particles group of low volume density in can yield obtaining well.Further, even if fall into the detergent particles group that composition that the sodium sulfate of heavy kind is many also can yield obtains low volume density well in detergent use powder raw material.
On the other hand, for comparative example 1,2 and 4, become than the detergent particles group of embodiment high volume density (more than 715g/L).This is considered to, due to the foam that does not use anionic surfactant compositions, can not give to consist of low-gravity anionic surfactant compositions the effect of the foam of particle.
For comparative example 3, than embodiment granulation yield, reduce (60.6%).Although this thinks due to the foam that has used anionic surfactant compositions; but micronize gas is 0L/min; in fact by the single fluid nozzle foam of spraying; can not reach the high dispersive of foam thus, there is the formation of big particle in the tackiness having due to foam.Further, for comparative example 3, become than the detergent particles group of embodiment high volume density (743g/L).This is considered to foam due to anionic surfactant compositions becomes large liquid piece and supplies with, its result is with the contacting of detergent use powder raw material, the hydration of detergent use powder raw material or dissolve institute's time spent and compare increase with the situation of fine droplets by the cooling time of detergent use powder raw material, foam is difficult to solidify, and more easily causes the lather collapse of foam in granulation.
Further, if relatively form identical embodiment 1 and comparative example 1,60 seconds dissolution rates improve, and granular sensation extinction time also shortens.This also can judge from embodiment 1 compares volume density step-down with comparative example 1, be considered to due to by using foam, thereby intragranular space increase, easily dissolve.Further, as shown in the value of coarse grain rate and micro mist rate, size distribution becomes sharply, and mobility also improves.
The possibility of utilizing in industry
By the present invention, with the detergent particles group who does not use spray-dired method with low volume density in good yield manufacture.Such detergent particles group can be used as the detergent composition that dress material such as uses at the various uses, or preferably as a kind of composition of such detergent composition, uses.

Claims (11)

1. detergent particles group's a manufacture method, wherein,
Described detergent particles group's manufacture method has the container of use rotary mixing machine by the operation of detergent use powder raw material granulation,
Use many fluid tips the foam of anionic surfactant compositions to be sparged to the granulation of carrying out this detergent use powder raw material in this container rotary mixing machine.
2. manufacture method as claimed in claim 1, wherein,
With the proportion of the foam of this anionic surfactant compositions after multithread body nozzle spray, be 0.1~0.95.
3. manufacture method as claimed in claim 1 or 2, wherein,
The foam of anionic surfactant compositions is sneaked into gaseous media in anionic surfactant compositions and is obtained.
4. manufacture method as claimed in claim 3, wherein,
With foaming machine, carry out gaseous media sneaking into anionic surfactant compositions.
5. the manufacture method as described in claim 3 or 4, wherein,
Gaseous media is air.
6. the manufacture method as described in any one in claim 1~5, wherein,
Many fluid tips are two-fluid spray nozzle.
7. the manufacture method as described in any one in claim 1~6, wherein,
Anionic surfactant compositions is to contain following a) composition and b) surfactant paste of composition,
A) be selected from a kind of above anion surfactant in the salt of the salt of linear alkyl benzene sulphonic acid, the salt of alkylsurfuric acid and polyxyethylated sulfuric acid;
B) the above-mentioned a) composition with respect to 100 mass parts is the water of 25~70 mass parts.
8. the manufacture method as described in any one in claim 1~7, wherein,
Spraying is the foam of the anionic surfactant compositions of 20~100 mass parts with respect to the detergent use powder raw material of 100 mass parts.
9. the manufacture method as described in any one in claim 1~8, wherein,
The content of the anion surfactant in detergent particles group is 5~50 quality %.
10. the manufacture method as described in any one in claim 1~9, wherein,
In detergent particles group, the content of detergent use powder raw material is 10~80 quality %.
11. manufacture method as described in any one in claim 1~10, wherein,
Detergent use powder raw material is water-soluble solid alkali inorganic substance and/or water-soluble inorganic salt.
CN201280023908.3A 2011-05-18 2012-05-16 The manufacture method of detergent particles group Expired - Fee Related CN103547665B (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP2011-111867 2011-05-18
JP2011111867 2011-05-18
PCT/JP2012/062536 WO2012157681A1 (en) 2011-05-18 2012-05-16 Process for manufacturing group of detergent granules

Publications (2)

Publication Number Publication Date
CN103547665A true CN103547665A (en) 2014-01-29
CN103547665B CN103547665B (en) 2016-04-13

Family

ID=47176998

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201280023908.3A Expired - Fee Related CN103547665B (en) 2011-05-18 2012-05-16 The manufacture method of detergent particles group

Country Status (3)

Country Link
JP (1) JP2012255145A (en)
CN (1) CN103547665B (en)
WO (1) WO2012157681A1 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116601274A (en) * 2021-01-07 2023-08-15 花王株式会社 Granular detergent composition

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6139994B2 (en) * 2012-06-20 2017-05-31 花王株式会社 Process for producing dentifrice granules
JP6350500B2 (en) 2015-12-04 2018-07-04 トヨタ自動車株式会社 Granule manufacturing apparatus and manufacturing method

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001181691A (en) * 1999-12-22 2001-07-03 Lion Corp Vessel rotary type mixing machine and method for producing granular detergent composition
WO2003054131A1 (en) * 2001-12-21 2003-07-03 Henkel Kommanditgesellschaft Auf Aktien Method for the production of surfactant granulates containing builders
JP2011001966A (en) * 2009-06-16 2011-01-06 Nippon Steel Corp Water sealed gas holder, internal dust collecting device for the same, and dust collecting method in water sealed gas holder

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS57192500A (en) * 1981-05-20 1982-11-26 Lion Corp Manufacture of granular detergent
JPH0827494A (en) * 1994-07-18 1996-01-30 Lion Corp Method for producing high bulk density detergent composition
JP2003105397A (en) * 2001-09-28 2003-04-09 Lion Corp Method for producing granular detergent composition having high bulk density
CN102015992B (en) * 2008-05-19 2012-07-11 花王株式会社 Surfactant-supporting granule cluster
CN102459555B (en) * 2009-06-30 2014-05-07 花王株式会社 Method for producing high bulk density detergent granules

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001181691A (en) * 1999-12-22 2001-07-03 Lion Corp Vessel rotary type mixing machine and method for producing granular detergent composition
WO2003054131A1 (en) * 2001-12-21 2003-07-03 Henkel Kommanditgesellschaft Auf Aktien Method for the production of surfactant granulates containing builders
JP2011001966A (en) * 2009-06-16 2011-01-06 Nippon Steel Corp Water sealed gas holder, internal dust collecting device for the same, and dust collecting method in water sealed gas holder

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116601274A (en) * 2021-01-07 2023-08-15 花王株式会社 Granular detergent composition
CN116601274B (en) * 2021-01-07 2024-07-16 花王株式会社 Granular detergent composition

Also Published As

Publication number Publication date
JP2012255145A (en) 2012-12-27
CN103547665B (en) 2016-04-13
WO2012157681A1 (en) 2012-11-22

Similar Documents

Publication Publication Date Title
JP5525755B2 (en) Surfactant-supporting granules
CN103547665B (en) The manufacture method of detergent particles group
CN103221527B (en) Method for producing detergent particle aggregates
CN103228776B (en) Method for producing detergent particle group
WO2000023560A1 (en) Process for producing detergent particles
CN102712884B (en) Method for producing detergent granules
CN102459555B (en) Method for producing high bulk density detergent granules
CN102712885B (en) Method for producing detergent granules
JP3875098B2 (en) Production method of mononuclear detergent particles
CN102666827B (en) Method for producing surfactant-supporting granule cluster
JP2936220B2 (en) Method for producing nonionic detergent particles
EP1550712B1 (en) Process for producing a granular anionic surfactant
JP3813674B2 (en) Method for producing crystalline alkali metal silicate granules
CN1883784B (en) Process for preparing granular anionic surfactant
JP2000186300A (en) Preparation of mononuclear detergent particle group
JP5971753B2 (en) Method for producing detergent particles
JP2022106336A (en) Granular detergent composition
JP2014125622A (en) Production method of detergent particle group
JP2000053999A (en) Continuous production of granular nonionic detergent composition
JP2014031450A (en) Production method of detergent particle group

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20160413

CF01 Termination of patent right due to non-payment of annual fee