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CN113861442A - Organic silicon emulsion and preparation method thereof - Google Patents

Organic silicon emulsion and preparation method thereof Download PDF

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Publication number
CN113861442A
CN113861442A CN202010607315.8A CN202010607315A CN113861442A CN 113861442 A CN113861442 A CN 113861442A CN 202010607315 A CN202010607315 A CN 202010607315A CN 113861442 A CN113861442 A CN 113861442A
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emulsion
fatty acid
active substance
catalyst
organic silicon
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黄伟
苏芳
曹添
胡佳新
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Yangzhou Sixin New Material Technology Co ltd
Jiangsu Sixin Scientific Technological Application Research Institute Co ltd
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Yangzhou Sixin New Material Technology Co ltd
Jiangsu Sixin Scientific Technological Application Research Institute Co ltd
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Priority to CN202010607315.8A priority Critical patent/CN113861442A/en
Priority to PCT/CN2021/098240 priority patent/WO2022001575A1/en
Publication of CN113861442A publication Critical patent/CN113861442A/en
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    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
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    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
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    • C08L33/26—Homopolymers or copolymers of acrylamide or methacrylamide
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    • C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04—Polysiloxanes
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/10—Block- or graft-copolymers containing polysiloxane sequences
    • C08L83/12—Block- or graft-copolymers containing polysiloxane sequences containing polyether sequences
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    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L87/00—Compositions of unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
    • C08J2383/10—Block- or graft-copolymers containing polysiloxane sequences
    • C08J2383/12—Block- or graft-copolymers containing polysiloxane sequences containing polyether sequences
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C—CHEMISTRY; METALLURGY
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    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
    • C08J2433/24—Homopolymers or copolymers of amides or imides
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
    • C08J2483/10—Block- or graft-copolymers containing polysiloxane sequences
    • C08J2483/12—Block- or graft-copolymers containing polysiloxane sequences containing polyether sequences
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2487/00—Characterised by the use of unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/10—Esters; Ether-esters
    • C08K5/101—Esters; Ether-esters of monocarboxylic acids
    • C08K5/103—Esters; Ether-esters of monocarboxylic acids with polyalcohols

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Abstract

The invention aims to provide an organic silicon emulsion and a preparation method thereof, wherein firstly, hydrogen-containing polysiloxane and hydrophobic particles react under the action of a catalyst to prepare an active substance, preferably polyether modified polysiloxane and glycerin fatty acid ester are compounded to emulsify the active substance, the glycerin fatty acid ester not only has emulsifying property, but also has certain anti-corrosion property, and the finally prepared organic silicon emulsion is stable and has excellent performance.

Description

Organic silicon emulsion and preparation method thereof
Technical Field
The invention relates to an organic silicon emulsion and a preparation method thereof, belonging to the technical field of fine chemical preparations.
Background
The organic silicon emulsion is one of important organic silicon products, has been widely applied to industry due to the unique temperature resistance and high hydrophobicity and is widely applied to the industrial fields of paper making, textile, slurry, coating, building, leather, medicine, cosmetics and the like.
The organosilicon emulsion used in the industrial process is mainly oil-in-water type, and the preparation method comprises a conventional emulsion polymer method, a phase inversion emulsion polymerization method and an ultrasonic emulsification method; evaluating a silicone emulsion, which generally has a close relationship between its function and stability, the emulsifier, a key component of the silicone emulsion, is primarily used to disperse the active; a large number of experimental experiences show that the main functions of the organic silicon emulsion are influenced by excessive emulsifier; the emulsifier is too little, and the obtained organic silicon emulsion is very unstable and can cause loss; on the other hand, the organic silicon emulsion contains a large amount of water, the common organic silicon emulsion is prevented from deteriorating by adding the preservative, and the stability of the performance of the emulsion is ensured, but with the continuous perfection of chemical safety regulations and the wider application range of the organic silicon emulsion, the limitation requirement of the organic silicon emulsion on the preservative is higher and higher, and the application of the organic silicon emulsion is finally limited.
Disclosure of Invention
The invention aims to provide an organic silicon emulsion and a preparation method thereof, wherein firstly, hydrogen-containing polysiloxane and hydrophobic particles react under the action of a catalyst to prepare an active substance, preferably polyether modified polysiloxane and glycerin fatty acid ester are compounded to emulsify the active substance, the glycerin fatty acid ester not only has emulsifying property, but also has certain anti-corrosion property, and the finally prepared organic silicon emulsion is stable and has excellent performance.
The organic silicon emulsion is characterized by comprising the following components:
A. active substance:
the active substance is a reaction product of hydrogen-containing polyorganosiloxane and hydrophobic particles under the action of a catalyst.
(1) The hydrogen-containing polyorganosiloxane has the following structural general formula:
H c Me c3-SiO(MeHSiO) a (Me 2SiO) b SiMe c3-H c
Meis methyl, subscriptcIs a number of 0, 1 or 2,ais an integer of 2 to 100, and,bis an integer of 20 to 300, and has at least 2 silicon-bonded hydrogen atoms per molecule in an amount of 90 to 95% of the total mass of the active material.
(2) The hydrophobic particles are hydrophobic silicon dioxide, and the specific surface area is 150-250 m2The dosage of the active substance is 4-8% of the total mass of the active substance.
(3) The catalyst is selected from LiOH, CsOH, NaOH, KOH and Me4And (3) NOH, NaOH is preferably selected in the invention, and the dosage of the catalyst is 1-3% of the total mass of the active substances.
The preparation process of the active substance comprises the following steps: the polyorganosiloxane and the hydrophobic particles are first mixed homogeneously at room temperature to maintain sufficient contact. And then heating to 80-250 ℃, adding a catalyst for reaction for 2-8 h, and cooling to room temperature after the reaction is finished to obtain an active substance, wherein the using amount of the active substance accounts for 10-30% of the total mass of the organosilicon emulsion.
B. Glycerin fatty acid ester
The glycerin fatty acid ester is obtained by esterifying glycerin and fatty acid serving as raw materials under the condition of an alkaline catalyst; the fatty acid is selected from one or more of propionic acid, caprylic acid, capric acid and lauric acid; the catalyst is selected from sodium bicarbonate, potassium hydroxide, sodium hydroxide and potassium bicarbonate; the mass ratio of the glycerol to the fatty acid to the alkaline catalyst is glycerol: fatty acid: the alkaline catalyst is 20-100:25-300: 0.3-3.0;
the preparation method of the glycerin fatty acid ester is characterized in that glycerin and fatty acid are used as raw materials and are subjected to esterification for 40-90min at the temperature of 200-250 ℃ in the presence of a basic catalyst; the content of glycerin fatty acid ester accounts for 2-8% of the total weight of the silicone emulsion.
C. Polyether modified polysiloxane
The structural formula of the polyether modified polysiloxane is as follows:
Figure 572460DEST_PATH_GDA0002700466490000021
wherein the letter R2Is methyl, ethyl, propyl, butyl or benzeneA group; r3Is hydrogen atom, methyl, ethyl, propyl or butyl; subscriptr，sIs the degree of polymerization of the silicon units,sis an integer of 1 to 50, and,ris an integer of 1 to 200; subscripteAndfthe degrees of polymerization of Ethylene Oxide (EO) and Propylene Oxide (PO), respectively,eandfare integers of 1 to 50; subscripttis-CH2The polymerization degree of (a) is an integer of 1-6, and the dosage of the polyether modified polysiloxane accounts for 5-15% of the total mass of the organosilicon emulsion.
D. Thickening agent
The thickener is selected from polyacrylamide, carbomer, xanthan gum, polyacrylate and cellulose ether, and the amount of the thickener accounts for 0.5-3% of the total mass of the silicone emulsion.
E. Water (W)
The amount of water accounts for 50-80% of the total mass of the silicone emulsion.
The preparation method of the organic silicon emulsion comprises the following steps:
fully mixing the active substance, the glycerin fatty acid ester and the silicon polyether for 10-50 min under stirring at room temperature to form a mixture M; mixing the thickening agent and water, and fully stirring to obtain a mixture N; and raising the temperature of the mixture M to 55-85 ℃ to keep the system temperature, slowly adding the mixture N, increasing the stirring speed to change the water-in-oil emulsion into the oil-in-water emulsion, and further emulsifying the crude emulsion by a colloid mill to obtain the organic silicon emulsion.
The specific implementation mode is as follows:
preparation of active substance:
the active material was prepared according to the aforementioned method for preparing active material using the reaction raw materials and conditions in the following table
Figure DEST_PATH_IMAGE004
Preparation of glycerin fatty acid ester
The glycerin fatty acid ester was prepared according to the aforementioned method for preparing glycerin fatty acid ester using the reaction raw materials and conditions shown in the following table
Figure DEST_PATH_IMAGE006
Example values for silicon polyethers
Figure DEST_PATH_IMAGE008
Preparation of the silicone emulsion:
example 1:
mixing 10g of active substance A-1, 8g of glycerin fatty acid ester B-1 and 15g of silicon polyether E-1 at room temperature under stirring for 10min to obtain mixture M1; 3g of thickening agent polyacrylamide and 64g of water are mixed and fully stirred to obtain a mixture N1; then raising the temperature of the mixture M1 to 55 ℃ to keep the system temperature, slowly adding the mixture N1, increasing the stirring speed to change the water-in-oil emulsion into the oil-in-water emulsion, and further emulsifying the crude emulsion by a colloid mill to obtain the organic silicon emulsion.
Example 2:
mixing 30g of active substance A-2, 2g of glycerin fatty acid ester B-2 and 5g of silicon polyether E-2 at room temperature under stirring for 20min to obtain mixture M2; mixing 0.5g of thickening agent carbomer and 62.5g of water, and fully stirring to obtain a mixture N2; then raising the temperature of the mixture M2 to 85 ℃ to keep the system temperature, slowly adding the mixture N2, increasing the stirring speed to change the mixture from water-in-oil emulsion to oil-in-water emulsion, and further emulsifying the crude emulsion by a colloid mill to obtain the organic silicon emulsion.
Example 3:
mixing 30g of active substance A-3, 6g of glycerin fatty acid ester B-3 and 12g of silicon polyether E-3 at room temperature under stirring for 30min to obtain mixture M3; 2g of thickener xanthan gum and 50g of water are mixed and fully stirred to obtain a mixture N3; then raising the temperature of the mixture M3 to 60 ℃ to keep the system temperature, slowly adding the mixture N3, increasing the stirring speed to change the mixture from water-in-oil emulsion to oil-in-water emulsion, and further emulsifying the crude emulsion by a colloid mill to obtain the organic silicon emulsion.
Example 4:
mixing active substance A-4 12.5g, glycerin fatty acid ester B-4 2g, and silicon polyether E-4 5g at room temperature under stirring for 45min to obtain mixture M4; 0.5g of thickening agent polyacrylate and 80g of water are mixed and fully stirred to obtain a mixture N4; then raising the temperature of the mixture M4 to 70 ℃ to keep the system temperature, slowly adding the mixture N4, increasing the stirring speed to change the mixture from water-in-oil emulsion to oil-in-water emulsion, and further emulsifying the crude emulsion by a colloid mill to obtain the organic silicon emulsion.
Example 5
Mixing 20g of active substance A-5, 4g of glycerin fatty acid ester B-5 and 8g of silicon polyether E-5 at room temperature under stirring for 50min to obtain mixture M5; 1g of thickener carboxymethyl cellulose and 67g of water are mixed and fully stirred to obtain a mixture N5; then raising the temperature of the mixture M5 to 75 ℃ to keep the system temperature, slowly adding the mixture N5, increasing the stirring speed to change the mixture from water-in-oil emulsion to oil-in-water emulsion, and further emulsifying the crude emulsion by a colloid mill to obtain the organic silicon emulsion.
Comparative example 1:
mixing 10g of active substance A-1 and 23g of silicon polyether E-1 at room temperature under stirring for 10min to form a mixture M6; 3g of thickening agent polyacrylamide and 64g of water are mixed and fully stirred to obtain a mixture N1; then raising the temperature of the mixture M6 to 55 ℃ to keep the system temperature, slowly adding the mixture N1, increasing the stirring speed to change the water-in-oil emulsion into the oil-in-water emulsion, and further emulsifying the crude emulsion by a colloid mill to obtain the organic silicon emulsion.
Wherein the letter R2Is methyl, ethyl, propyl, butyl or phenyl; r3Is hydrogen atom, methyl, ethyl, propyl or butyl; subscript r, s is the polymerization degree of the silicon chain link, s is an integer of 1-50, and r is an integer of 1-200; subscripts e and f are polymerization degrees of Ethylene Oxide (EO) and Propylene Oxide (PO) respectively, and both e and f are integers of 1-50; subscript t is-CH2The polymerization degree of (a) is an integer of 1-6, and the dosage of the polyether modified polysiloxane accounts for 5-15% of the total mass of the organosilicon emulsion.
The test method comprises the following steps:
the performance of the high viscosity silicone composition emulsion prepared by the method of the present invention is evaluated mainly from the following aspects:
(1) oil temperature of the emulsion:
adding 1% of organic silicon emulsion into 99% of water, heating, and observing the liquid level condition of the water diluent, wherein the emulsion is more stable when the temperature of the floating oil is higher.
(2) The corrosion resistance of the emulsion is as follows:
the silicone emulsion was tested for total colony count with reference to GB4799.2-2016 (determination of total food microbial colony count).
And (3) testing results:
Figure DEST_PATH_IMAGE010
from the above data, it can be seen that the introduction of the glycerin fatty acid ester can improve the stability and the preservative property of the emulsion.

Claims (2)

1. An organic silicon emulsion and a preparation method thereof are characterized in that the organic silicon emulsion consists of the following components:
A. active substance:
the active substance is a reaction product of hydrogen-containing polysiloxane and hydrophobic particles under the action of a catalyst;
(1) the hydrogen-containing polyorganosiloxane has the following structural general formula:
Hc Me 3-cSiO(MeHSiO)a(Me 2SiO)bSiMe 3-cHc
Methe subscript c is 0, 1 or 2, a is an integer of 2 to 100, b is an integer of 20 to 300, each molecule has at least 2 silicon-bonded hydrogen atoms, and the amount is 90 to 95% of the total mass of the active material;
(2) the hydrophobic particles are hydrophobic silicon dioxide, and the specific surface area is 150-250 m2The dosage of the active substance is 4-8 percent of the total mass of the active substance；
(3) The catalyst is selected from LiOH, CsOH, NaOH, KOH and Me4NOH, wherein the dosage of the catalyst is 1-3% of the total mass of the active substances;
the preparation process of the active substance comprises the following steps: the polyorganosiloxane and the hydrophobic particles are first mixed homogeneously at room temperature to maintain sufficient contact. Heating to 80-250 ℃, adding a catalyst for reaction for 2-8 h, and cooling to room temperature after the reaction is finished to obtain an active substance, wherein the using amount of the active substance accounts for 10-30% of the total mass of the organic silicon emulsion;
B. glycerin fatty acid ester
The glycerin fatty acid ester is obtained by esterifying glycerin and fatty acid serving as raw materials under the condition of an alkaline catalyst; the fatty acid is selected from one or more of propionic acid, caprylic acid, capric acid and lauric acid; the catalyst is selected from sodium bicarbonate, potassium hydroxide, sodium hydroxide and potassium bicarbonate; the mass ratio of the glycerol to the fatty acid to the alkaline catalyst is glycerol: fatty acid: the alkaline catalyst is 20-100:25-300: 0.3-3.0;
the preparation method of the glycerin fatty acid ester is characterized in that glycerin and fatty acid are used as raw materials and are subjected to esterification for 40-90min at the temperature of 200-250 ℃ in the presence of a basic catalyst; the content of glycerin fatty acid ester accounts for 2-8% of the total weight of the silicone emulsion.
C. Polyether modified polysiloxane
The structural formula of the polyether modified polysiloxane is as follows:
Figure RE-FDA0002700466480000011
wherein the letter R2Is methyl, ethyl, propyl, butyl or phenyl; r3Is hydrogen atom, methyl, ethyl, propyl or butyl; subscript r, s is the polymerization degree of the silicon chain link, s is an integer of 1-50, and r is an integer of 1-200; subscripts e and f are polymerization degrees of Ethylene Oxide (EO) and Propylene Oxide (PO) respectively, and both e and f are integers of 1-50; subscript t is-CH2The polymerization degree of (a) is an integer of 1-6, and the amount of the polyether modified polysiloxane accounts for the total mass of the organosilicon emulsion5-15％；
D. Thickening agent
The thickening agent is selected from polyacrylamide, carbomer, xanthan gum, polyacrylate and cellulose ether, and the amount of the thickening agent accounts for 0.5-3% of the total mass of the silicone emulsion;
E. water (W)
The using amount of the water accounts for 50-80% of the total mass of the organic silicon emulsion;
the preparation method of the organic silicon emulsion comprises the following steps:
fully mixing the active substance, the glycerin fatty acid ester and the silicon polyether for 10-50 min under stirring at room temperature to form a mixture M; mixing the thickening agent and water, and fully stirring to obtain a mixture N; and raising the temperature of the mixture M to 55-85 ℃ to keep the system temperature, slowly adding the mixture N, increasing the stirring speed to change the water-in-oil emulsion into the oil-in-water emulsion, and further emulsifying the crude emulsion by a colloid mill to obtain the organic silicon emulsion.
2. The silicone emulsion and process of claim 1 wherein the catalyst in the process of preparing the active material is preferably sodium hydroxide.
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