CN105001423A - Organosilicon softening finishing agent with ice-cold feeling and preparation method of organosilicon softening finishing agent - Google Patents
Organosilicon softening finishing agent with ice-cold feeling and preparation method of organosilicon softening finishing agent Download PDFInfo
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Abstract
The invention relates to the technical field of printing and dyeing auxiliaries, particularly to an organosilicon softening finishing agent with ice-cold feeling and a preparation method of the organosilicon softening finishing agent. The organosilicon softening finishing agent consists of the following raw materials in parts by weight: 10-60 parts of hydrophilic ternary copolymerized organosilicon, 0.1-30 parts of microcapsule ice-cold particles, 0.4-2.4 parts of glacial acetic acid and 20-70 parts of water. The preparation method comprises the following steps: adding hydrophilic ternary copolymerized organosilicon into an emulsifying machine, turning on the emulsifying machine, adding glacial acetic acid, then gradually adding distilled water for emulsification, after silicone oil is changed into a uniform emulsifiable solution, gradually adding the microcapsule ice-cold particles which are 0.1-30 in parts by weight into the emulsifiable solution, and when the microcapsule ice-cold particles are fully dissolved, turning off the emulsifying machine so as to obtain the organosilicon softening finishing agent. The organosilicon softening finishing agent has excellent hydrophilicity, excellent yellowing resistance and excellent launderability, and has the ice-cold feeling that common silicone oil cannot compare.
Description
Technical field
The present invention relates to dyeing and printing auxiliary technical field, be specifically related to a kind of organosilicon flexible finishing composition with coolness and preparation method thereof.
Background technology
Along with improving constantly of standard of living, people just do not rest on soft feel aspect to the demand of silicone softening agent, improve requirement gradually, require to have the sliding sensation of cool silk simultaneously to feel for the absorbing sweat of clothes, water vapour permeability.This just allows the development of organosilicon flexible finishing composition gradually towards the future development of diversification.Organosilicon flexible finishing composition should be allowed to retain higher softness, fluffy, level and smooth feel, and the fabric requirement after arranging it again has hydrophilic water vapour permeability and surperficial coolness.
Although traditional amido silicon oil has excellent softness, but the wetting ability of fabric is poor after arranging, this makes the fabric moisture after arranging perspiration wicking poor, summer easily produces feeling of oppression and heat, and amido silicon oil due to the content of primary amine group on molecular chain higher, easy generation " yellowing " phenomenon, makes fabric affect the quality appearance of fabric taking in process to turn yellow gradually.In addition amino silicon oil emulsion stability is poor, because fabric can with alkaline agent in dyeing course, if these alkaline agents are not thoroughly cleaned, dressing liquid can be entered in Final finishing process, the pH value of dressing liquid is uprised, thus amino silicon oil emulsion can be made to occur demulsifying phenomenon, produce at fabric face " the silicon spot " that be difficult to clean, this allows the use of amido silicon oil be restricted.
Market being applied general hydrophilic silicone oil is the product adopting containing hydrogen silicone oil and glycidyl allyl ether addition reaction, although adopt this hydrophilic silicone oil finish fabric, can increase to the wetting ability of fabric, but due to this type of silicone molecule chain not containing the stronger group (such as amino, secondary amino group etc.) of polarity, so arrange after fabric feeling and washing fastness all poor, repeatedly washed by fabric after arranging, its softness significantly declines.
Also do not have a kind of silicone softening agent to possess hydrophilic water vapour permeability, yellowing resistance and ice-cold feel in the market, silicone oil on the market just has feature mostly in one aspect simultaneously.Therefore, be necessary to develop the organosilicon flexible finishing composition that a kind of hydrophilic water vapour permeability is excellent, yellowing resistance is good, feel ice is refreshing.
Summary of the invention
In order to overcome the shortcoming and defect existed in prior art, the object of the present invention is to provide a kind of organosilicon flexible finishing composition with coolness, this organosilicon flexible finishing composition has the washing resistance performance of splendid wetting ability, yellowing resistance and excellence, and has the ice-cold feel that common silicone oil cannot match in excellence or beauty.
Another object of the present invention is to provide a kind of preparation method with the organosilicon flexible finishing composition of coolness, this preparation method's technique is simple, and convenient operation and control, steady quality, production efficiency is high, can large-scale industrial production.
Object of the present invention is achieved through the following technical solutions: a kind of organosilicon flexible finishing composition with coolness, and described organosilicon flexible finishing composition is made up of the raw material of following weight part:
Hydrophilic terpolymer organosilicon 10 ~ 60 parts
Microcapsule ice is felt well 0.1 ~ 30 part, particle
0.4 ~ 2.4 part, Glacial acetic acid
20 ~ 70 parts, water.
Preferably, the organosilyl preparation method of described hydrophilic terpolymer comprises the steps:
A, amino-polyether and Virahol to be added in reactor, and be warmed up to certain temperature, then add epoxy silicon oil, the reaction some time, obtained terpolymer silicone oil; The reaction of both-end epoxy silicon oil and double-end amino polyethers belongs to the opening of epoxy group(ing).
B, then under certain temperature condition, then add hydrophilic modifying agent in above-mentioned terpolymer silicone oil, the reaction some time, obtained hydrophilic silicone oil; What the secondary amine in the middle of the primary amine groups at the epoxy group(ing) in hydrophilic modifying agent and terpolymer silicone macromolecule two ends and molecular chain was carried out is also opening.
C, treat that hydrophilic silicone oil cools to 40 DEG C with bottom discharge, obtained hydrophilic terpolymer organosilicon.
Preferably, in described steps A, the molecular weight of epoxy silicon oil is 4000 ~ 10000; The molecular weight of amino-polyether is 600 ~ 2200; The mass ratio of epoxy silicon oil and amino-polyether is 1.11 ~ 1.66:1.
Preferably, in described steps A, the consumption of Virahol is identical with the total mass of epoxy silicon oil, amino-polyether; Warming temperature is 60 ~ 90 DEG C, and the reaction times is 10 ~ 16h.
Preferably, in described step B, hydrophilic modifying agent is 2,3-epoxypropyltrimethylchloride chloride, molecular weight be 500 epoxy group(ing) polyethers or molecular weight be 900 epoxy group(ing) polyethers; The quality of hydrophilic modifying agent is 3% ~ 15% of terpolymer silicone oil total mass; Temperature of reaction is 60 ~ 90 DEG C, and the reaction times is 10 ~ 18h.
Preferably, the feel well preparation method of particle of described microcapsule ice comprises the steps:
A, take a certain amount of gelatin and add in hot water under certain agitation condition, get a certain amount of ice composition of feeling well and add in aqueous gelatin solution;
B, in above-mentioned system, add a certain amount of gum arabic solution, under keeping the constant condition of temperature, stirring velocity, drip the pH value that massfraction is 5% ~ 15% acetum, regulator solution;
C, the solution obtained by step b are cooled to less than 10 DEG C, drip the pH value that massfraction is the NaOH solution of 5% ~ 15%, regulator solution subsequently; Finally adding a certain amount of massfraction is 20% ~ 30% glutaraldehyde solution, stirs certain hour, is warming up to certain temperature and completes solidification;
D, centrifugal by carrying out under gained solution normal temperature, then leave standstill and be precipitated thing, obtain microcapsule ice after drying and to feel well particle.
Preferably, in described step a, the quality of gelatin accounts for hot water quality's 2% ~ 15%, and mixing speed is 200 ~ 700r/min; Hot water temperature is 40 ~ 60 DEG C; Ice composition of feeling well is menthol and/or Xylitol; The feel well quality of composition of ice accounts for 20% ~ 70% of gelatin quality.
Preferably, in described step b, the massfraction of gum arabic solution is 3% ~ 10%; The mass ratio of the aqueous gelatin solution in the quality of gum arabic solution and step 1 is 0.6 ~ 1.3:1; The pH value of regulator solution is to 3 ~ 5.
Preferably, in described step c, the pH value of regulator solution is to 8 ~ 11; The add-on of glutaraldehyde solution is 2-10mL, stirs 5 ~ 25min; Solidification value is 40 ~ 70 DEG C.
A kind of preparation method with the organosilicon flexible finishing composition of coolness, comprise the steps: that the hydrophilic terpolymer organosilicon getting above-mentioned weight part adds in mulser, open mulser, add the Glacial acetic acid of above-mentioned weight part, then the distilled water of above-mentioned weight part is added gradually, carry out emulsification, by the time after silicone oil becomes uniform emulsion, the microcapsule ice adding above-mentioned weight part again in this emulsion is gradually felt well particle, until all dissolve, close mulser, obtained described organosilicon flexible finishing composition.
Beneficial effect of the present invention is: 1, the present invention is by adopting hydrophilic terpolymer organosilicon as hydrophilic silicone oil main body, and it is terpolymer silicone macromolecule, all has suitability for multiple fiber.First linear terpolymer silicone macromolecule compound with regular structure has good avidity for synthon; In addition the hydroxyl on the amino on terpolymer silicone macromolecule, secondary amino group energy and cellulosic fibre, amino, carboxyl etc. on protein fibre form hydrogen bond, so and also have stronger bonding force between these two kinds of fibers.
2, the present invention is by adopting hydrophilic terpolymer organosilicon, amino-polyether segment on terpolymer silicone backbone can and water molecules between formed " hydrogen bond ", terpolymer silicone molecules is made to have certain wetting ability, do not need to add emulsifying agent and just can carry out emulsification, and alkaline-resisting, acidproof, the dewatering ability of emulsion all show excellence, can meet the environment for use of various harshness.By the further hydrophilic modifying of above-mentioned terpolymer silicone macromolecule, the fabric after arranging can be allowed on the one hand to improve further in wetting ability, even can reach " moment is hydrophilic ".No longer containing primary amine groups on terpolymer silicone macromolecule after hydrophilic modifying, fundamentally solve " xanthochromia " problem.
3, the present invention to feel well particle by adopting micro encapsulation ice, its capsule heart composition is menthol and/or Xylitol, these two kinds of alcohol slowly release in microcapsule, touch people and know from experience and make human feeling arrive refrigerant sensation, meet summer people and to feel well to ice the requirement of feel.
4, the present invention to feel well particle by adopting micro encapsulation ice, composition in microcapsule has multiple pharmacological function, can anti-inflammatory analgesic and antipruriticly to calm the nerves, for diseases such as common cold due to wind-heat, rheumatism, headache, hot eyes, larynx numbness, swelling and pain in the throat, ulceration on the oral mucosa and the tongue, toothache, the fabric arranged through organosilicon flexible finishing composition of the present invention is made to have health-care effect.
6, organosilicon flexible finishing composition of the present invention is not containing the objectionable constituent of contaminate environment, not containing the composition that the countries such as APEO forbid strictly.
7, organosilicon flexible finishing composition of the present invention has the washing resistance performance of splendid wetting ability, yellowing resistance and excellence, and has the ice-cold feel that common silicone oil cannot match in excellence or beauty.
8, preparation method's technique of the present invention is simple, and convenient operation and control, steady quality, production efficiency is high, can large-scale industrial production.
Embodiment
For the ease of the understanding of those skilled in the art, below in conjunction with embodiment, the present invention is further illustrated, and the content that embodiment is mentioned not is limitation of the invention.
Embodiment 1
Have an organosilicon flexible finishing composition for coolness, described organosilicon flexible finishing composition is made up of the raw material of following weight part:
Hydrophilic terpolymer organosilicon 30 parts
Microcapsule ice is felt well 5 parts, particle
1.2 parts, Glacial acetic acid
63.8 parts, water.
Described hydrophilic terpolymer is organosilyl preparation method comprise the steps:
A, by 450.45kg molecular weight be 2003 amino-polyether and 950.45kg Virahol add in reactor and stir, and be warmed up to 80 DEG C, and then in reactor, add the epoxy silicon oil reaction 14h that 500kg molecular weight is 8000, obtained terpolymer silicone oil;
B, then under 80 DEG C of conditions, then add the epoxy group(ing) polyethers that 133.06kg molecular weight is 500 in above-mentioned terpolymer silicone oil, reaction 14h, prepares hydrophilic silicone oil;
C, treat that hydrophilic silicone oil cools to 40 DEG C with bottom discharge, obtained hydrophilic terpolymer organosilicon.
The feel well preparation method of particle comprises the steps: described microcapsule ice
A, take 5 kilograms of gelatin, add under 400r/min agitation condition in 100 kilograms of 40 DEG C of hot water, get 1 kilogram of menthol and add in aqueous gelatin solution;
B, in above-mentioned system, add 106 kilograms of gum arabic solutions, keep temperature, the constant dropping massfraction of stirring velocity is 10% acetum, the pH value of regulator solution is to 3.5;
C, the solution obtained by step b are cooled to less than 10 DEG C, and dripping massfraction is subsequently the NaOH solution of 10%, and the pH value of regulator solution is to 8; Finally adding 1 kilogram of massfraction is 25% glutaraldehyde solution, stirs 15min, is warming up to 50 DEG C and completes solidification;
D, centrifugal by carrying out under gained solution normal temperature, then leave standstill and be precipitated thing, obtain microcapsule ice after drying and to feel well particle.
A kind of preparation method with the organosilicon flexible finishing composition of coolness, comprise the steps: that the hydrophilic terpolymer organosilicon of taking-up 30 parts adds in mulser, open mulser, add 1.2 parts of Glacial acetic acid wherein, then add 63.8 parts of distilled water gradually, carry out emulsification, by the time after silicone oil becomes uniform emulsion, then the microcapsule ice adding 5 parts in this emulsion is gradually felt well particle, until all dissolve, close mulser, obtained described organosilicon flexible finishing composition.
Embodiment 2
Have an organosilicon flexible finishing composition for coolness, described organosilicon flexible finishing composition is made up of the raw material of following weight part:
Hydrophilic terpolymer organosilicon 32 parts
Microcapsule ice is felt well 6 parts, particle
1.28 parts, Glacial acetic acid
60.72 parts, water.
Described hydrophilic terpolymer is organosilyl preparation method comprise the steps:
A, by 357.14kg molecular weight be 900 amino-polyether and 857.14kg Virahol add in reactor and stir, and be warmed up to 80 DEG C, and then in reactor, add the epoxy silicon oil reaction 14h that 500kg molecular weight is 6000, obtained terpolymer silicone oil;
B, then under 80 DEG C of conditions, then add the epoxy group(ing) polyethers that 111.43kg molecular weight is 900 in above-mentioned terpolymer silicone oil, reaction 15h, prepares hydrophilic silicone oil;
C, treat that hydrophilic silicone oil cools to 40 DEG C with bottom discharge, obtained hydrophilic terpolymer organosilicon.
The feel well preparation method of particle comprises the steps: described microcapsule ice
A, take 6 kilograms of gelatin, add under 500r/min agitation condition in 100 kilograms of 50 DEG C of hot water, get 1 kilogram of menthol and add in aqueous gelatin solution;
B, in above-mentioned system, add 107 kilograms of gum arabic solutions, keep temperature, the constant dropping massfraction of stirring velocity is 10% acetum, the pH value of regulator solution is to 4;
C, the solution obtained by step b are cooled to less than 10 DEG C, and dripping massfraction is subsequently the NaOH solution of 10%, and the pH value of regulator solution is to 9; Finally adding 1 kilogram of massfraction is 25% glutaraldehyde solution, stirs 20min, is warming up to 60 DEG C and completes solidification;
D, centrifugal by carrying out under gained solution normal temperature, then leave standstill and be precipitated thing, obtain microcapsule ice after drying and to feel well particle.
A kind of preparation method with the organosilicon flexible finishing composition of coolness, comprise the steps: that the hydrophilic terpolymer organosilicon of taking-up 32 parts adds in mulser, open mulser, add 1.28 parts of Glacial acetic acid wherein, then add 60.72 parts of distilled water gradually, carry out emulsification, by the time after silicone oil becomes uniform emulsion, then the microcapsule ice adding 6 parts in this emulsion is gradually felt well particle, until all dissolve, close mulser, obtained described organosilicon flexible finishing composition.
Embodiment 3
Have an organosilicon flexible finishing composition for coolness, described organosilicon flexible finishing composition is made up of the raw material of following weight part:
Hydrophilic terpolymer organosilicon 34 parts
Microcapsule ice is felt well 6.4 parts, particle
1.36 parts, Glacial acetic acid
58.24 parts, water.
Described hydrophilic terpolymer is organosilyl preparation method comprise the steps:
A, by 301.20kg molecular weight be 600 amino-polyether and 801.20kg Virahol add in reactor and stir, and be warmed up to 80 DEG C, and then in reactor, add the epoxy silicon oil reaction 14h that 500kg molecular weight is 4000, obtained terpolymer silicone oil;
B, then under 80 DEG C of conditions, then add 48.07kg 2,3-epoxypropyltrimethylchloride chloride in above-mentioned terpolymer silicone oil, reaction 13h, prepares hydrophilic silicone oil;
C, treat that hydrophilic silicone oil cools to 40 DEG C with bottom discharge, obtained hydrophilic terpolymer organosilicon.
The feel well preparation method of particle comprises the steps: described microcapsule ice
A, take 7 kilograms of gelatin, add under 600r/min agitation condition in 100 kilograms of 60 DEG C of hot water, get 1.2 kilograms of menthols and add in aqueous gelatin solution;
B, in above-mentioned system, add 108.2 kilograms of gum arabic solutions, keep temperature, the constant dropping massfraction of stirring velocity is 10% acetum, the pH value of regulator solution is to 4.5;
C, the solution obtained by step b are cooled to less than 10 DEG C, and dripping massfraction is subsequently the NaOH solution of 10%, and the pH value of regulator solution is to 10; Finally adding 1 kilogram of massfraction is 25% glutaraldehyde solution, stirs 20min, is warming up to 60 DEG C and completes solidification;
D, centrifugal by carrying out under gained solution normal temperature, then leave standstill and be precipitated thing, obtain microcapsule ice after drying and to feel well particle.
A kind of preparation method with the organosilicon flexible finishing composition of coolness, comprise the steps: that the hydrophilic terpolymer organosilicon of taking-up 34 parts adds in mulser, open mulser, add 1.36 parts of Glacial acetic acid wherein, then add 58.24 parts of distilled water gradually, carry out emulsification, by the time after silicone oil becomes uniform emulsion, then the microcapsule ice adding 6.4 parts in this emulsion is gradually felt well particle, until all dissolve, close mulser, obtained described organosilicon flexible finishing composition.
Embodiment 4
Have an organosilicon flexible finishing composition for coolness, described organosilicon flexible finishing composition is made up of the raw material of following weight part:
Hydrophilic terpolymer organosilicon 10 parts
Microcapsule ice is felt well 0.1 part, particle
0.4 part, Glacial acetic acid
20 parts, water.
Described hydrophilic terpolymer is organosilyl preparation method comprise the steps:
A, amino-polyether and Virahol to be added in reactor, and be warmed up to certain temperature, then add epoxy silicon oil, the reaction some time, obtained terpolymer silicone oil;
B, then under certain temperature condition, then add hydrophilic modifying agent in above-mentioned terpolymer silicone oil, the reaction some time, obtained hydrophilic silicone oil;
C, treat that hydrophilic silicone oil cools to 40 DEG C with bottom discharge, obtained hydrophilic terpolymer organosilicon.
In described steps A, the molecular weight of epoxy silicon oil is 4000; The molecular weight of amino-polyether is 600; The mass ratio of epoxy silicon oil and amino-polyether is 1.11:1.
In described steps A, the consumption of Virahol is identical with the total mass of epoxy silicon oil, amino-polyether; Warming temperature is 60 DEG C, and the reaction times is 16h.
In described step B, hydrophilic modifying agent to be molecular weight be 500 epoxy group(ing) polyethers; The quality of hydrophilic modifying agent is 3% of terpolymer silicone oil total mass; Temperature of reaction is 60 DEG C, and the reaction times is 18h.
The feel well preparation method of particle comprises the steps: described microcapsule ice
A, take a certain amount of gelatin and add in hot water under certain agitation condition, get a certain amount of ice composition of feeling well and add in aqueous gelatin solution;
B, in above-mentioned system, add a certain amount of gum arabic solution, under keeping the constant condition of temperature, stirring velocity, drip the pH value that massfraction is 5% acetum, regulator solution;
C, the solution obtained by step b are cooled to less than 10 DEG C, drip the pH value that massfraction is the NaOH solution of 5%, regulator solution subsequently; Finally adding a certain amount of massfraction is 20% glutaraldehyde solution, stirs certain hour, is warming up to certain temperature and completes solidification;
D, centrifugal by carrying out under gained solution normal temperature, then leave standstill and be precipitated thing, obtain microcapsule ice after drying and to feel well particle.
In described step a, the quality of gelatin accounts for hot water quality's 2%, and mixing speed is 200r/min; Hot water temperature is 40 DEG C; Ice composition of feeling well is menthol; The feel well quality of composition of ice accounts for 20% of gelatin quality.
In described step b, the massfraction of gum arabic solution is 3%; The mass ratio of the aqueous gelatin solution in the quality of gum arabic solution and step 1 is 0.6:1; The pH value of regulator solution is to 3.
In described step c, the pH value of regulator solution is to 8; The add-on of glutaraldehyde solution is 2mL, stirs 5min; Solidification value is 70 DEG C.
A kind of preparation method with the organosilicon flexible finishing composition of coolness, comprise the steps: that the hydrophilic terpolymer organosilicon getting above-mentioned weight part adds in mulser, open mulser, add the Glacial acetic acid of above-mentioned weight part, then the distilled water of above-mentioned weight part is added gradually, carry out emulsification, by the time after silicone oil becomes uniform emulsion, the microcapsule ice adding above-mentioned weight part again in this emulsion is gradually felt well particle, until all dissolve, close mulser, obtained described organosilicon flexible finishing composition.
Embodiment 5
Have an organosilicon flexible finishing composition for coolness, described organosilicon flexible finishing composition is made up of the raw material of following weight part:
Hydrophilic terpolymer organosilicon 20 parts
Microcapsule ice is felt well 8 parts, particle
1 part, Glacial acetic acid
30 parts, water.
Described hydrophilic terpolymer is organosilyl preparation method comprise the steps:
A, amino-polyether and Virahol to be added in reactor, and be warmed up to certain temperature, then add epoxy silicon oil, the reaction some time, obtained terpolymer silicone oil;
B, then under certain temperature condition, then add hydrophilic modifying agent in above-mentioned terpolymer silicone oil, the reaction some time, obtained hydrophilic silicone oil;
C, treat that hydrophilic silicone oil cools to 40 DEG C with bottom discharge, obtained hydrophilic terpolymer organosilicon.
In described steps A, the molecular weight of epoxy silicon oil is 60000; The molecular weight of amino-polyether is 900; The mass ratio of epoxy silicon oil and amino-polyether is 1.25:1.
In described steps A, the consumption of Virahol is identical with the total mass of epoxy silicon oil, amino-polyether; Warming temperature is 70 DEG C, and the reaction times is 15h.
In described step B, hydrophilic modifying agent to be molecular weight be 900 epoxy group(ing) polyethers; The quality of hydrophilic modifying agent is 6% of terpolymer silicone oil total mass; Temperature of reaction is 70 DEG C, and the reaction times is 16h.
The feel well preparation method of particle comprises the steps: described microcapsule ice
A, take a certain amount of gelatin and add in hot water under certain agitation condition, get a certain amount of ice composition of feeling well and add in aqueous gelatin solution;
B, in above-mentioned system, add a certain amount of gum arabic solution, under keeping the constant condition of temperature, stirring velocity, drip the pH value that massfraction is 8% acetum, regulator solution;
C, the solution obtained by step b are cooled to less than 10 DEG C, drip the pH value that massfraction is the NaOH solution of 8%, regulator solution subsequently; Finally adding a certain amount of massfraction is 22% glutaraldehyde solution, stirs certain hour, is warming up to certain temperature and completes solidification;
D, centrifugal by carrying out under gained solution normal temperature, then leave standstill and be precipitated thing, obtain microcapsule ice after drying and to feel well particle.
In described step a, the quality of gelatin accounts for hot water quality's 5%, and mixing speed is 300r/min; Hot water temperature is 45 DEG C; Ice composition of feeling well is Xylitol; The feel well quality of composition of ice accounts for 30% of gelatin quality.
In described step b, the massfraction of gum arabic solution is 5%; The mass ratio of the aqueous gelatin solution in the quality of gum arabic solution and step 1 is 0.8:1; The pH value of regulator solution is to 3.5.
In described step c, the pH value of regulator solution is to 9; The add-on of glutaraldehyde solution is 4mL, stirs 10min; Solidification value is 50 DEG C.
A kind of preparation method with the organosilicon flexible finishing composition of coolness, comprise the steps: that the hydrophilic terpolymer organosilicon getting above-mentioned weight part adds in mulser, open mulser, add the Glacial acetic acid of above-mentioned weight part, then the distilled water of above-mentioned weight part is added gradually, carry out emulsification, by the time after silicone oil becomes uniform emulsion, the microcapsule ice adding above-mentioned weight part again in this emulsion is gradually felt well particle, until all dissolve, close mulser, obtained described organosilicon flexible finishing composition.
Embodiment 6
Have an organosilicon flexible finishing composition for coolness, described organosilicon flexible finishing composition is made up of the raw material of following weight part:
Hydrophilic terpolymer organosilicon 35 parts
Microcapsule ice is felt well 15 parts, particle
1.4 parts, Glacial acetic acid
45 parts, water.
Described hydrophilic terpolymer is organosilyl preparation method comprise the steps:
A, amino-polyether and Virahol to be added in reactor, and be warmed up to certain temperature, then add epoxy silicon oil, the reaction some time, obtained terpolymer silicone oil;
B, then under certain temperature condition, then add hydrophilic modifying agent in above-mentioned terpolymer silicone oil, the reaction some time, obtained hydrophilic silicone oil;
C, treat that hydrophilic silicone oil cools to 40 DEG C with bottom discharge, obtained hydrophilic terpolymer organosilicon.
In described steps A, the molecular weight of epoxy silicon oil is 7000; The molecular weight of amino-polyether is 2003; The mass ratio of epoxy silicon oil and amino-polyether is 1.35:1.
In described steps A, the consumption of Virahol is identical with the total mass of epoxy silicon oil, amino-polyether; Warming temperature is 75 DEG C, and the reaction times is 13h.
In described step B, hydrophilic modifying agent is molecular weight is 2,3-epoxypropyltrimethylchloride chloride; The quality of hydrophilic modifying agent is 9% of terpolymer silicone oil total mass; Temperature of reaction is 75 DEG C, and the reaction times is 14h.
The feel well preparation method of particle comprises the steps: described microcapsule ice
A, take a certain amount of gelatin and add in hot water under certain agitation condition, get a certain amount of ice composition of feeling well and add in aqueous gelatin solution;
B, in above-mentioned system, add a certain amount of gum arabic solution, under keeping the constant condition of temperature, stirring velocity, drip the pH value that massfraction is 10% acetum, regulator solution;
C, the solution obtained by step b are cooled to less than 10 DEG C, drip the pH value that massfraction is the NaOH solution of 10%, regulator solution subsequently; Finally adding a certain amount of massfraction is 25% glutaraldehyde solution, stirs certain hour, is warming up to certain temperature and completes solidification;
D, centrifugal by carrying out under gained solution normal temperature, then leave standstill and be precipitated thing, obtain microcapsule ice after drying and to feel well particle.
In described step a, the quality of gelatin accounts for hot water quality's 8%, and mixing speed is 450r/min; Hot water temperature is 50 DEG C; Ice composition of feeling well is menthol and Xylitol; The feel well quality of composition of ice accounts for 45% of gelatin quality.
In described step b, the massfraction of gum arabic solution is 6%; The mass ratio of the aqueous gelatin solution in the quality of gum arabic solution and step 1 is 0.9:1; The pH value of regulator solution is to 4.
In described step c, the pH value of regulator solution is to 9.5; The add-on of glutaraldehyde solution is 6mL, stirs 15min; Solidification value is 55 DEG C.
A kind of preparation method with the organosilicon flexible finishing composition of coolness, comprise the steps: that the hydrophilic terpolymer organosilicon getting above-mentioned weight part adds in mulser, open mulser, add the Glacial acetic acid of above-mentioned weight part, then the distilled water of above-mentioned weight part is added gradually, carry out emulsification, by the time after silicone oil becomes uniform emulsion, the microcapsule ice adding above-mentioned weight part again in this emulsion is gradually felt well particle, until all dissolve, close mulser, obtained described organosilicon flexible finishing composition.
Embodiment 7
Have an organosilicon flexible finishing composition for coolness, described organosilicon flexible finishing composition is made up of the raw material of following weight part:
Hydrophilic terpolymer organosilicon 50 parts
Microcapsule ice is felt well 25 parts, particle
2.0 parts, Glacial acetic acid
60 parts, water.
Described hydrophilic terpolymer is organosilyl preparation method comprise the steps:
A, amino-polyether and Virahol to be added in reactor, and be warmed up to certain temperature, then add epoxy silicon oil, the reaction some time, obtained terpolymer silicone oil;
B, then under certain temperature condition, then add hydrophilic modifying agent in above-mentioned terpolymer silicone oil, the reaction some time, obtained hydrophilic silicone oil;
C, treat that hydrophilic silicone oil cools to 40 DEG C with bottom discharge, obtained hydrophilic terpolymer organosilicon.
In described steps A, the molecular weight of epoxy silicon oil is 8000; The molecular weight of amino-polyether is 900; The mass ratio of epoxy silicon oil and amino-polyether is 1.45:1.
In described steps A, the consumption of Virahol is identical with the total mass of epoxy silicon oil, amino-polyether; Warming temperature is 80 DEG C, and the reaction times is 12h.
In described step B, hydrophilic modifying agent is molecular weight to be molecular weight be 900 epoxy group(ing) polyethers; The quality of hydrophilic modifying agent is 12% of terpolymer silicone oil total mass; Temperature of reaction is 80 DEG C, and the reaction times is 12h.
The feel well preparation method of particle comprises the steps: described microcapsule ice
A, take a certain amount of gelatin and add in hot water under certain agitation condition, get a certain amount of ice composition of feeling well and add in aqueous gelatin solution;
B, in above-mentioned system, add a certain amount of gum arabic solution, under keeping the constant condition of temperature, stirring velocity, drip the pH value that massfraction is 12% acetum, regulator solution;
C, the solution obtained by step b are cooled to less than 10 DEG C, drip the pH value that massfraction is the NaOH solution of 12%, regulator solution subsequently; Finally adding a certain amount of massfraction is 28% glutaraldehyde solution, stirs certain hour, is warming up to certain temperature and completes solidification;
D, centrifugal by carrying out under gained solution normal temperature, then leave standstill and be precipitated thing, obtain microcapsule ice after drying and to feel well particle.
In described step a, the quality of gelatin accounts for hot water quality's 12%, and mixing speed is 600r/min; Hot water temperature is 55 DEG C; Ice composition of feeling well is menthol and Xylitol; The feel well quality of composition of ice accounts for 60% of gelatin quality.
In described step b, the massfraction of gum arabic solution is 8%; The mass ratio of the aqueous gelatin solution in the quality of gum arabic solution and step 1 is 1.1:1; The pH value of regulator solution is to 4.5.
In described step c, the pH value of regulator solution is to 10; The add-on of glutaraldehyde solution is 8mL, stirs 20min; Solidification value is 60 DEG C.
A kind of preparation method with the organosilicon flexible finishing composition of coolness, comprise the steps: that the hydrophilic terpolymer organosilicon getting above-mentioned weight part adds in mulser, open mulser, add the Glacial acetic acid of above-mentioned weight part, then the distilled water of above-mentioned weight part is added gradually, carry out emulsification, by the time after silicone oil becomes uniform emulsion, the microcapsule ice adding above-mentioned weight part again in this emulsion is gradually felt well particle, until all dissolve, close mulser, obtained described organosilicon flexible finishing composition.
Embodiment 8
Have an organosilicon flexible finishing composition for coolness, described organosilicon flexible finishing composition is made up of the raw material of following weight part:
Hydrophilic terpolymer organosilicon 60 parts
Microcapsule ice is felt well 30 parts, particle
2.4 parts, Glacial acetic acid
70 parts, water.
Described hydrophilic terpolymer is organosilyl preparation method comprise the steps:
A, amino-polyether and Virahol to be added in reactor, and be warmed up to certain temperature, then add epoxy silicon oil, the reaction some time, obtained terpolymer silicone oil;
B, then under certain temperature condition, then add hydrophilic modifying agent in above-mentioned terpolymer silicone oil, the reaction some time, obtained hydrophilic silicone oil;
C, treat that hydrophilic silicone oil cools to 40 DEG C with bottom discharge, obtained hydrophilic terpolymer organosilicon.
In described steps A, the molecular weight of epoxy silicon oil is 10000; The molecular weight of amino-polyether is 2003; The mass ratio of epoxy silicon oil and amino-polyether is 1.66:1.
In described steps A, the consumption of Virahol is identical with the total mass of epoxy silicon oil, amino-polyether; Warming temperature is 90 DEG C, and the reaction times is 10h.
In described step B, hydrophilic modifying agent is 2,3-epoxypropyltrimethylchloride chloride; The quality of hydrophilic modifying agent is 15% of terpolymer silicone oil total mass; Temperature of reaction is 90 DEG C, and the reaction times is 10h.
The feel well preparation method of particle comprises the steps: described microcapsule ice
A, take a certain amount of gelatin and add in hot water under certain agitation condition, get a certain amount of ice composition of feeling well and add in aqueous gelatin solution;
B, in above-mentioned system, add a certain amount of gum arabic solution, under keeping the constant condition of temperature, stirring velocity, drip the pH value that massfraction is 15% acetum, regulator solution;
C, the solution obtained by step b are cooled to less than 10 DEG C, drip the pH value that massfraction is the NaOH solution of 15%, regulator solution subsequently; Finally adding a certain amount of massfraction is 30% glutaraldehyde solution, stirs certain hour, is warming up to certain temperature and completes solidification;
D, centrifugal by carrying out under gained solution normal temperature, then leave standstill and be precipitated thing, obtain microcapsule ice after drying and to feel well particle.
In described step a, the quality of gelatin accounts for hot water quality's 15%, and mixing speed is 700r/min; Hot water temperature is 60 DEG C; Ice composition of feeling well is menthol and Xylitol; The feel well quality of composition of ice accounts for 70% of gelatin quality.
In described step b, the massfraction of gum arabic solution is 10%; The mass ratio of the aqueous gelatin solution in the quality of gum arabic solution and step 1 is 1.3:1; The pH value of regulator solution is to 5.
In described step c, the pH value of regulator solution is to 11; The add-on of glutaraldehyde solution is 10mL, stirs 25min; Solidification value is 70 DEG C.
A kind of preparation method with the organosilicon flexible finishing composition of coolness, comprise the steps: that the hydrophilic terpolymer organosilicon getting above-mentioned weight part adds in mulser, open mulser, add the Glacial acetic acid of above-mentioned weight part, then the distilled water of above-mentioned weight part is added gradually, carry out emulsification, by the time after silicone oil becomes uniform emulsion, the microcapsule ice adding above-mentioned weight part again in this emulsion is gradually felt well particle, until all dissolve, close mulser, obtained described organosilicon flexible finishing composition.
Organosilicon flexible finishing composition obtained for embodiment 1 ~ 3 is carried out following performance test:
1, the test of alkali stability
Prepare the organosilicon flexible finishing composition that the embodiment 1 ~ 3 of 3 parts of 10g/L is obtained respectively, add 1g/L, 3g/L, 5g/L caustic soda respectively, leave standstill 24h, observe phenomena is as shown in table 1:
Table 1
| Concentration of caustic soda (g/L) | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| 1 | Transparent in floating oil | Transparent in floating oil | Transparent in floating oil |
| 3 | Transparent in floating oil | Transparent in floating oil | Transparent in floating oil |
| 6 | Transparent in floating oil | Transparent in floating oil | Transparent in floating oil |
As can be seen from Table 1, the organosilicon flexible finishing composition alkali stability that the present invention obtains is splendid, can meet dyeing and finishing and process various severe condition.
2, the test of heat-resistant stability
Prepare the organosilicon flexible finishing composition that the embodiment 1 ~ 3 of 3 parts of 10g/L is obtained respectively, increase the temperature to 80 DEG C, 90 DEG C, 100 DEG C respectively, and be incubated 2h, observe phenomena is as shown in table 2:
Table 2
| Temperature DEG C | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| 80 | Transparent in floating oil | Transparent in floating oil | Transparent in floating oil |
| 90 | Transparent in floating oil | Transparent in floating oil | Transparent in floating oil |
| 100 | Transparent in floating oil | Transparent in floating oil | Transparent in floating oil |
As can be seen from Table 2, the resistance to temperature stability of organosilicon flexible finishing composition that the present invention obtains is splendid, can meet dyeing and finishing and process various severe condition.
3, the application performance test of the organosilicon flexible finishing composition that embodiment 1 ~ 3 is obtained
Adopt padding method to arrange on cotton and terylene respectively by the organosilicon flexible finishing composition that above-mentioned traditional hydrophilic silicone oil and embodiment 1 ~ 3 obtain, finishing composition concentration all uses 30g/L, and a leaching one is rolled, preliminary drying temperature 90 DEG C, preliminary drying time 60 s, baking temperature 170 DEG C, bakes time 60s.Arrange complete evaluation feel, drip to fabric, survey the whiteness of infiltration time and fabric, its result data is as shown in table 3:
Table 3
As can be seen from Table 3, the organosilicon flexible finishing composition that the present invention obtains, after having arranged fabric, has had than traditional hydrophilic silicone oil and has significantly improved in wetting ability, and yellowing resistance aspect has and is improved greatly, the more important thing is and imparts the ice-cold feel of fabric.
Above-described embodiment is the present invention's preferably implementation, and in addition, the present invention can also realize by alternate manner, and any apparent replacement is all within protection scope of the present invention without departing from the inventive concept of the premise.
Claims (10)
1. there is an organosilicon flexible finishing composition for coolness, it is characterized in that: described organosilicon flexible finishing composition is made up of the raw material of following weight part:
Hydrophilic terpolymer organosilicon 10 ~ 60 parts
Microcapsule ice is felt well 0.1 ~ 30 part, particle
0.4 ~ 2.4 part, Glacial acetic acid
20 ~ 70 parts, water.
2. a kind of organosilicon flexible finishing composition with coolness according to claim 1, is characterized in that: described hydrophilic terpolymer is organosilyl preparation method comprise the steps:
A, amino-polyether and Virahol to be added in reactor, and be warmed up to certain temperature, then add epoxy silicon oil, the reaction some time, obtained terpolymer silicone oil;
B, then under certain temperature condition, then add hydrophilic modifying agent in above-mentioned terpolymer silicone oil, the reaction some time, obtained hydrophilic silicone oil;
C, treat that hydrophilic silicone oil cools to 40 DEG C with bottom discharge, obtained hydrophilic terpolymer organosilicon.
3. a kind of organosilicon flexible finishing composition with coolness according to claim 2, is characterized in that: in described steps A, and the molecular weight of epoxy silicon oil is 4000 ~ 10000; The molecular weight of amino-polyether is 600 ~ 2200; The mass ratio of epoxy silicon oil and amino-polyether is 1.11 ~ 1.66:1.
4. a kind of organosilicon flexible finishing composition with coolness according to claim 2, it is characterized in that: in described steps A, the consumption of Virahol is identical with the total mass of epoxy silicon oil, amino-polyether; Warming temperature is 60 ~ 90 DEG C, and the reaction times is 10 ~ 16h.
5. a kind of organosilicon flexible finishing composition with coolness according to claim 2, it is characterized in that: in described step B, hydrophilic modifying agent is 2,3-epoxypropyltrimethylchloride chloride, molecular weight be 500 epoxy group(ing) polyethers or molecular weight be 900 epoxy group(ing) polyethers; The quality of hydrophilic modifying agent is 3% ~ 15% of terpolymer silicone oil total mass; Temperature of reaction is 60 ~ 90 DEG C, and the reaction times is 10 ~ 18h.
6. a kind of organosilicon flexible finishing composition with coolness according to claim 1, is characterized in that: the feel well preparation method of particle comprises the steps: described microcapsule ice
A, take a certain amount of gelatin and add in hot water under certain agitation condition, get a certain amount of ice composition of feeling well and add in aqueous gelatin solution;
B, in above-mentioned system, add a certain amount of gum arabic solution, under keeping the constant condition of temperature, stirring velocity, drip the pH value that massfraction is 5% ~ 15% acetum, regulator solution;
C, the solution obtained by step b are cooled to less than 10 DEG C, drip the pH value that massfraction is the NaOH solution of 5% ~ 15%, regulator solution subsequently; Finally adding a certain amount of massfraction is 20% ~ 30% glutaraldehyde solution, stirs certain hour, is warming up to certain temperature and completes solidification;
D, centrifugal by carrying out under gained solution normal temperature, then leave standstill and be precipitated thing, obtain microcapsule ice after drying and to feel well particle.
7. a kind of organosilicon flexible finishing composition with coolness according to claim 6, it is characterized in that: in described step a, the quality of gelatin accounts for hot water quality's 2% ~ 15%, and mixing speed is 200 ~ 700r/min; Hot water temperature is 40 ~ 60 DEG C; Ice composition of feeling well is menthol and/or Xylitol; The feel well quality of composition of ice accounts for 20% ~ 70% of gelatin quality.
8. a kind of organosilicon flexible finishing composition with coolness according to claim 6, is characterized in that: in described step b, and the massfraction of gum arabic solution is 3% ~ 10%; The mass ratio of the aqueous gelatin solution in the quality of gum arabic solution and step 1 is 0.6 ~ 1.3:1; The pH value of regulator solution is to 3 ~ 5.
9. a kind of organosilicon flexible finishing composition with coolness according to claim 6, it is characterized in that: in described step c, the pH value of regulator solution is to 8 ~ 11; The add-on of glutaraldehyde solution is 2-10mL, stirs 5 ~ 25min; Solidification value is 40 ~ 70 DEG C.
10. a kind of preparation method with the organosilicon flexible finishing composition of coolness as described in any one of claim 1 ~ 9, it is characterized in that: comprise the steps: that the hydrophilic terpolymer organosilicon getting above-mentioned weight part adds in mulser, open mulser, add the Glacial acetic acid of above-mentioned weight part, then the distilled water of above-mentioned weight part is added gradually, carry out emulsification, by the time after silicone oil becomes uniform emulsion, the microcapsule ice adding above-mentioned weight part again in this emulsion is gradually felt well particle, until all dissolve, close mulser, obtained described organosilicon flexible finishing composition.
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| CN109137482A (en) * | 2018-08-02 | 2019-01-04 | 苏州市天翱特种织绣有限公司 | A kind of preparation method of air-permeable cool type finishing agent |
| CN109694783A (en) * | 2018-12-11 | 2019-04-30 | 深圳市科玺化工有限公司 | A kind of color protection soft liquid laundry detergent and preparation method thereof |
| CN109930392A (en) * | 2019-02-28 | 2019-06-25 | 上海驰纺材料科技有限公司 | A kind of preparation method of the water-fastness long acting containing cotton knitted fabric |
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| CN116043558A (en) * | 2023-01-05 | 2023-05-02 | 江苏新瑞贝科技股份有限公司 | Bio-based soft cool-feeling antibacterial finishing agent and preparation method and application thereof |
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| CN108219147A (en) * | 2018-01-04 | 2018-06-29 | 佛山市三水古闰纺织印染研究院有限公司 | A kind of preparation method of hydrophilic silicone oil |
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| CN109930392A (en) * | 2019-02-28 | 2019-06-25 | 上海驰纺材料科技有限公司 | A kind of preparation method of the water-fastness long acting containing cotton knitted fabric |
| CN110205822A (en) * | 2019-07-15 | 2019-09-06 | 广东湛丰精细化工有限公司 | Dustless elastic silicone oil emulsion of one kind and preparation method thereof |
| CN112853762A (en) * | 2021-02-20 | 2021-05-28 | 诸暨九丰纺织科技有限公司 | Novel fluffy soft polyester fabric finishing agent and production process thereof |
| CN116043558A (en) * | 2023-01-05 | 2023-05-02 | 江苏新瑞贝科技股份有限公司 | Bio-based soft cool-feeling antibacterial finishing agent and preparation method and application thereof |
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