CN102286203A - Method for improving stability of organic silicone emulsion - Google Patents
Method for improving stability of organic silicone emulsion Download PDFInfo
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- CN102286203A CN102286203A CN 201110178485 CN201110178485A CN102286203A CN 102286203 A CN102286203 A CN 102286203A CN 201110178485 CN201110178485 CN 201110178485 CN 201110178485 A CN201110178485 A CN 201110178485A CN 102286203 A CN102286203 A CN 102286203A
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Abstract
The invention provides a method for improving the stability of organic silicone emulsion. A silicone polyether emulsifying agent prepared by utilizing two types of propenol polyether to modify hydrogen-containing polysiloxane has higher emulsifying efficiency than a silicone polyether emulsifying agent prepared by utilizing one type of propenol polyether to modify the hydrogen-containing polysiloxane. The organic silicone emulsion prepared from the emulsifying agent has excellent stability and shearing resistance, and the application range of the organic silicone emulsion is widened.
Description
Technical field
The present invention relates to a kind of organic silicon emulsion, the present invention relates to a kind of method that improves organic silicon emulsion stability more precisely, it relates to the preparation of fine chemicals additive, therefore is under the jurisdiction of technical field of fine chemical preparations.
Technical background
The basic structural unit of organosilicon product is made of silicon-oxygen chain link, and side chain then links to each other by the various organic groups of Siliciumatom and other.Therefore, both contained in the structure of organosilicon product " organic group ", and contained " inorganic structure " again, this special composition and molecular structure make it integrate the function of organic characteristic and inorganics.Compare with other macromolecular materials, the outstanding properties of organosilicon product is: heatproof characteristic, weathering resistance, electrical insulation properties, biological nature, low surface tension and low surface energy, so its range of application is very extensive.
Organic silicon emulsion is one of important organosilicon product, is made up of organosilicon, water and tensio-active agent etc., because its special performance and characteristics are widely used industrial, wherein, the organic silicon emulsion that is used for textile industry accounts for 1/5th of total amount.Organic silicon emulsion is divided into nonactive organic silicon emulsion, active organosilicon emulsion, modified organic silicon emulsion and organosilicon composite emulsion, be divided into cation type organic silicon emulsion, anionic organic silicon emulsion, non-ionic type organic silicon emulsion and compound ion type organic silicon emulsion again, also be divided into oil-in-water-type organic silicon emulsion and water-in-oil-type organic silicon emulsion.
The method for preparing organic silicon emulsion is a lot, but will prepare stable organic silicon emulsion, and it is played a role when being applied to corresponding field, will propose many requirements to emulsion preparation.Wherein, the stability requirement of emulsion is ubiquitous.So it is very important selecting suitable emulsifying agent and emulsification method at organosilicon material.About the document for preparing organic silicon emulsion has much: patent CN1807512 and CN101298027 have introduced by adding some auxiliary substances full-bodied organosilicon mixture have been scattered in the water, are prepared into more stable organic silicon emulsion; Patent CN102002242A has introduced a kind of method that the high fatty alcohol polyethers improves stability of emulsion of introducing; Patent CN101003008 has introduced by the pfpe molecule that contains hydroxyl as emulsifying agent being carried out chemical modification and has handled, and generates new end capped polyether, then it is used for emulsion preparation, thereby makes stable emulsion.
Above-mentioned patent mostly is and adopts common silicon polyethers as emulsifying agent, prepares organic silicon emulsion.The inventor finds by a large amount of experiments, with the common a kind of hydrogen containing siloxane W of modification of two kinds of vinylcarbinol polyethers (A and B), obtain the silicon polyethers and be designated as W-AB, than using vinylcarbinol polyethers A and vinylcarbinol polyethers B modification hydrogen containing siloxane W respectively, the silicon polyethers W-A that obtains, the emulsifying power height of W-B separately.The organic silicon emulsion that uses this class emulsifying agent to make has advantages of excellent stability and anti-shear performance, and has widened the range of application of organic silicon emulsion.
Summary of the invention
The purpose of this invention is to provide the new silicon polyethers emulsifying agent of a class, use the organic silicon emulsion of its preparation to have advantages of excellent stability, increased its applicable scope.
The organic silicon emulsion of the present invention's preparation is characterized in that comprising following several component:
1, silicon polyethers
Described silicon polyethers is by hydrogen containing siloxane and unsaturated polyether addition reaction to take place under the effect of catalyzer to prepare, and concrete preparation method can consult on the professional technique document and learn.The kinematic viscosity of described silicon polyethers in the time of 25 ℃ is 10～50, and 000mPas is preferably 50～20,000mPas.The structural formula of silicon polyethers is represented with following general formula:
(CH
3)
3SiO{(CH
3)
2SiO)
x(CH
3GSiO)
y}(CH
3)
3 ①
Wherein, G is a polyether group, represents with following general structure:
-(CH
2)
z(EO)
g(PO)
hR ②
In the said structure formula, R is-H or-CH
3Or-COCH
3Subscript x, y, z, g, h are the polymerization degree, x is 10～500 integer; Y is 1～50 integer; Z is 2～6 integer; G is 1～40 integer; H is 1～60 integer.
Structural formula 1. in, if G is identical vinylcarbinol polyether group, then this silicon polyethers is single polyethers synthetic silicon polyethers (being above-mentioned W-A and W-B); If G is different vinylcarbinol polyether group, then this silicon polyethers is a multiple polyethers synthetic silicon polyethers (being W-AB).
Patent of the present invention is to replace W-A and W-B oil in water emulsion phase component with W-AB.In whole organic silicon emulsion is 100% quality, and the consumption of silicon polyethers is 4～30%.
2, oil phase component
Oil phase component of the present invention is a silicone grease, is to be prepared from by organopolysiloxane and silicon-dioxide, and this treatment process can be inquired about on general professional technique data and obtain.The organopolysiloxane that relates in the oil phase component comprises polydimethylsiloxane, poly-di-ethyl siloxane, alkyl-modified polydimethylsiloxane, poly-methyl trifluoro propyl siloxanes, preferred polydimethylsiloxane, its kinematic viscosity in the time of 25 ℃ is 50～200,000mPas.
In whole organic silicon emulsion is 100% quality, and the consumption of oil phase component is 8～50%.
3, assistant for emulsifying agent
Assistant for emulsifying agent among the present invention, it comprises nonionogenic tenside, anion surfactant, cats product and amphoterics.
Preferred nonionic surfactants of the present invention specifically is selected from polyoxyethylene nonylphenol ether, polyoxyethylene octylphenol ether, lauric acid Soxylat A 25-7, oleic acid polyoxyethylene, sorbitan monostearate, sorbitan monooleate, anhydrous sorbitol tristearate, Witconol AL 69-66, anhydrous sorbitol Stearinsaeure polyoxyethylene ether-ester, anhydrous sorbitol list oleic acid polyoxyethylene ester, anhydrous sorbitol three stearic acid polyoxyethylene ether esters, castor oil polyoxyethylene ether, alkylphenol polyoxyethylene.
In whole organic silicon emulsion is 100% quality, and the consumption of assistant for emulsifying agent is 0.5～10%.
4, water
In whole organic silicon emulsion is 100% quality, and the consumption of water is 50～80%.
According to requirement to emulsion viscosity, can add thickening material, thickening material comprises polyacrylamide, carbomer, xanthan gum, polyacrylic ester, cellulose ethers, the dosage of thickening material is adjusted according to the viscosity of emulsion.Need add sterilant and sanitas during standing storage, as clorox, potassium sorbate, s-triazine, triumphant pine etc.
The preparation method of organic silicon emulsion is as follows among the present invention: under the room temperature, and with oil phase component, assistant for emulsifying agent, silicon polyethers thorough mixing 10～40min under agitation, preferred 15min～30min; The temperature of above-mentioned system is increased to 55 ℃～85 ℃, then, keeps system temperature, add entry lentamente, improve stirring velocity and make it become the emulsion oil-in-water phase inversion, continue to add water to needed mass concentration by water-in-oil emulsion, be generally 40%～70%, be preferably 50%～65%; Thick emulsion is by the further emulsification of colloidal mill; Be diluted to needed emulsion concentration with viscous water at last.
Embodiment
Preparation oil phase component D
1, D
2, D
3, D
4:
Polysiloxane d
1: polydimethylsiloxane, kinematic viscosity: 5000mPas
Polysiloxane d
2: poly-di-ethyl siloxane, kinematic viscosity: 200mPas
Polysiloxane d
3: poly-ethylene methacrylic radical siloxane, kinematic viscosity: 60000mPas
Polysiloxane d
4: poly-methyl trifluoro propyl siloxanes, kinematic viscosity: 180000mPas
Earlier above-mentioned organopolysiloxane and hydrophobic particles are at room temperature mixed respectively, to keep abundant contact.Be warming up to 50～300 ℃ then, add a certain amount of catalyst reaction 2～8h then respectively.Reaction finishes and is cooled to room temperature and promptly gets oil phase component D
1, D
2, D
3, D
4
Preparation silicon polyethers:
Preparation silicon polyethers E
1, E
2, E
3, E
4, E
5, E
6, its general formula is:
(CH
3)
3SiO{(CH
3)
2SiO)
x(CH
3GSiO)
y}(CH
3)
3
G is a polyether group, represents with general structure:
-(CH
2)
z(EO)
g(PO)
hR
Wherein the value of x, y, z, g, h sees the following form 1 and table 2.
Table 1 silicon polyethers E
1, E
2, E
3And E
4
| The silicon polyethers | E 1 | E 2 | E 3 | E 4 |
| R | -CH 3 | -H | -COCH 3 | -CH 3 |
| x | 15 | 300 | 480 | 160 |
| y | 2 | 22 | 30 | 45 |
| z | 3 | 4 | 6 | 5 |
| g | 5 | 36 | 12 | 20 |
| h | 3 | 42 | 57 | 21 |
Annotate: G is identical vinylcarbinol polyether group.
Table 2 silicon polyethers E
5And E
6
Annotate: G is different vinylcarbinol polyether groups.
Embodiment 1
Under the room temperature, with oil phase component, assistant for emulsifying agent, silicon polyethers thorough mixing 35min under agitation, temperature with above-mentioned system after finishing is increased to 60 ℃, then, keeps system temperature, add entry lentamente, improving stirring velocity and make it become the emulsion oil-in-water phase inversion by water-in-oil emulsion, continue to add water to needed mass concentration, is 50%, thick emulsion is by the further emulsification of colloidal mill, and being diluted to solid content with the vinylformic acid viscous water at last is 25% emulsion H
1
Embodiment 2:
Under the room temperature, with oil phase component, assistant for emulsifying agent, silicon polyethers thorough mixing 40min under agitation, temperature with above-mentioned system after finishing is increased to 80 ℃, then, keeps system temperature, add entry lentamente, improving stirring velocity and make it become the emulsion oil-in-water phase inversion by water-in-oil emulsion, continue to add water to needed mass concentration, is 60%, thick emulsion is by the further emulsification of colloidal mill, and being diluted to solid content with the vinylformic acid viscous water at last is 40% emulsion H
2
Embodiment 3:
Under the room temperature, with oil phase component, assistant for emulsifying agent, silicon polyethers thorough mixing 25min under agitation, temperature with above-mentioned system after finishing is increased to 70 ℃, then, keeps system temperature, add entry lentamente, improving stirring velocity and make it become the emulsion oil-in-water phase inversion by water-in-oil emulsion, continue to add water to needed mass concentration, is 55%, thick emulsion is by the further emulsification of colloidal mill, and being diluted to solid content with the vinylformic acid viscous water at last is 20% emulsion H
3
Embodiment 4:
Under the room temperature, with oil phase component, assistant for emulsifying agent, silicon polyethers thorough mixing 30min under agitation, temperature with above-mentioned system after finishing is increased to 75 ℃, then, keeps system temperature, add entry lentamente, improving stirring velocity and make it become the emulsion oil-in-water phase inversion by water-in-oil emulsion, continue to add water to needed mass concentration, is 50%, thick emulsion is by the further emulsification of colloidal mill, and being diluted to solid content with the vinylformic acid viscous water at last is 30% emulsion H
4
Comparative Examples 1:
Under the room temperature, with oil phase component, assistant for emulsifying agent, silicon polyethers thorough mixing 35min under agitation, temperature with above-mentioned system after finishing is increased to 60 ℃, then, keeps system temperature, add entry lentamente, improving stirring velocity and make it become the emulsion oil-in-water phase inversion by water-in-oil emulsion, continue to add water to needed mass concentration, is 50%, thick emulsion is by the further emulsification of colloidal mill, and being diluted to solid content with the vinylformic acid viscous water at last is 25% emulsion T
1
Comparative Examples 2:
Under the room temperature, with oil phase component, assistant for emulsifying agent, silicon polyethers thorough mixing 40min under agitation, temperature with above-mentioned system after finishing is increased to 80 ℃, then, keeps system temperature, add entry lentamente, improving stirring velocity and make it become the emulsion oil-in-water phase inversion by water-in-oil emulsion, continue to add water to needed mass concentration, is 60%, thick emulsion is by the further emulsification of colloidal mill, and being diluted to solid content with the vinylformic acid viscous water at last is 40% emulsion T
2
Comparative Examples 3:
Under the room temperature, with oil phase component, assistant for emulsifying agent, silicon polyethers thorough mixing 25min under agitation, temperature with above-mentioned system after finishing is increased to 70 ℃, then, keeps system temperature, add entry lentamente, improving stirring velocity and make it become the emulsion oil-in-water phase inversion by water-in-oil emulsion, continue to add water to needed mass concentration, is 55%, thick emulsion is by the further emulsification of colloidal mill, and being diluted to solid content with the vinylformic acid viscous water at last is 20% emulsion T
3
Comparative Examples 4:
Under the room temperature, with oil phase component, assistant for emulsifying agent, silicon polyethers thorough mixing 30min under agitation, temperature with above-mentioned system after finishing is increased to 75 ℃, then, keeps system temperature, add entry lentamente, improving stirring velocity and make it become the emulsion oil-in-water phase inversion by water-in-oil emulsion, continue to add water to needed mass concentration, is 50%, thick emulsion is by the further emulsification of colloidal mill, and being diluted to solid content with the vinylformic acid viscous water at last is 30% emulsion T
4
According to the prescription in the foregoing description and the Comparative Examples, can draw each components contents, see the following form:
Each components contents in table 3 emulsion
Annotate: emulsifying power=oil phase component/(silicon polyethers+assistant for emulsifying agent), ratio is big more, and emulsifying power is high more.
Testing method:
The performance of the silicon composition emulsion of the inventive method preparation is mainly assessed from the following aspects:
(1) dilution stability of emulsion:
Organic silicon emulsion according to 1% joins in 99% the water, after being uniformly dispersed, observes the liquid level situation of water diluent.
(2) the floating oil temperature of emulsion:
Organic silicon emulsion according to 1% joins in 99% the water, the liquid level situation that water diluent is observed in the back of heating up.
(3) anti-shear performance of emulsion:
Under the normal temperature, emulsion stoste is placed on the hunting of frequency 30min of 100 times/min on the horizontal oscillator tube, according to the method for (1), comparative emulsion liquid level situation.
The performance test contrast of table 4 emulsion
From the result of table 3 and table 4 as can be seen, introduce containing hydrogen silicone oil and the two kinds of common synthetic silicon of polyethers polyethers after, the ratio between oil phase component/(the silicon polyethers+assistant for emulsifying agent) has all become greatly, thus the explanation emulsifying power has improved; After introducing containing hydrogen silicone oil and the two kinds of common synthetic silicon of polyethers polyethers, improved the stability of organic silicon emulsion to a greater extent.
Claims (7)
1. method that improves organic silicon emulsion stability, described organic silicon emulsion is made up of silicon polyethers, oil phase component, assistant for emulsifying agent and water, described oil phase component is a silicone grease, described assistant for emulsifying agent is a nonionogenic tenside, it is characterized in that described silicon polyethers is obtained by two kinds of a kind of hydrogen containing siloxanes of the common modification of vinylcarbinol polyethers.
2. a kind of method that improves organic silicon emulsion stability according to claim 1, wherein, the structural formula of silicon polyethers is: (CH
3)
3SiO{ (CH
3)
2SiO)
x(CH
3GSiO)
y(CH
3)
3, G is a polyether group, structural formula is :-(CH
2)
z(EO)
g(PO)
hR, wherein, R is-H or-CH
3Or-COCH
3Subscript x, y, z, g, h are the polymerization degree, x is 10～500 integer; Y is 1～50 integer; Z is 2～6 integer; G is 1～40 integer; H is 1～60 integer.
3. a kind of method that improves organic silicon emulsion stability according to claim 1, wherein, the kinematic viscosity of silicon polyethers in the time of 25 ℃ is 10～50,000mPas, the consumption of described silicon polyethers occupy 4～30% of machine silicon emulsion total mass.
4. a kind of method that improves organic silicon emulsion stability according to claim 1, wherein, the kinematic viscosity of silicon polyethers in the time of 25 ℃ is 50～20,000mPas.
5. a kind of method that improves organic silicon emulsion stability according to claim 1, wherein, assistant for emulsifying agent is selected from polyoxyethylene nonylphenol ether, polyoxyethylene octylphenol ether, the lauric acid Soxylat A 25-7, oleic acid polyoxyethylene, sorbitan monostearate, sorbitan monooleate, the anhydrous sorbitol tristearate, Witconol AL 69-66, anhydrous sorbitol Stearinsaeure polyoxyethylene ether-ester, anhydrous sorbitol list oleic acid polyoxyethylene ester, anhydrous sorbitol three stearic acid polyoxyethylene ether esters, castor oil polyoxyethylene ether, alkylphenol polyoxyethylene, the consumption of described assistant for emulsifying agent are occupied 0.5～10% of machine silicon emulsion total mass.
6. a kind of method that improves organic silicon emulsion stability according to claim 1, wherein, the oil phase component silicone grease is to be prepared from by organopolysiloxane and silicon-dioxide, the preparation method is a known technology, described organopolysiloxane is a polydimethylsiloxane, its kinematic viscosity in the time of 25 ℃ is 50～200,000mPas, and described oil phase component consumption occupies 8～50% of machine silicon emulsion total mass.
7. a kind of method that improves organic silicon emulsion stability according to claim 1, wherein, the preparation method of organic silicon emulsion is:
1. under the room temperature, with oil phase component, assistant for emulsifying agent, silicon polyethers thorough mixing 10～40min under agitation;
2. the temperature with above-mentioned system is increased to 55 ℃～85 ℃, keeps system temperature then, adds entry lentamente, improves stirring velocity and makes phase reversal of emulsion, continues to add water to mass concentration 40%～70%;
3. thick emulsion is passed through the further emulsification of colloidal mill;
4. be diluted to needed emulsion concentration with viscous water at last, promptly.
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| CN106267914A (en) * | 2016-08-31 | 2017-01-04 | 湖北新四海化工股份有限公司 | A kind of efficient compound defoamer and preparation method thereof |
| CN106390529A (en) * | 2016-08-31 | 2017-02-15 | 湖北新四海化工股份有限公司 | High efficiency composite defoaming agent and preparation method thereof |
| CN107164001A (en) * | 2017-06-02 | 2017-09-15 | 汪建军 | A kind of compound emulsifying agent and preparation method thereof |
| CN107629214A (en) * | 2017-07-19 | 2018-01-26 | 合肥普庆新材料科技有限公司 | A kind of efficient wetting agent of organosilicon |
| CN107817316A (en) * | 2017-10-30 | 2018-03-20 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of detection method of titanium dioxide organic silicon emulsion ph stability |
| CN109233296A (en) * | 2018-08-23 | 2019-01-18 | 南京瑞思化学技术有限公司 | A method of improving stability of organic silicone emulsion |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106267914A (en) * | 2016-08-31 | 2017-01-04 | 湖北新四海化工股份有限公司 | A kind of efficient compound defoamer and preparation method thereof |
| CN106390529A (en) * | 2016-08-31 | 2017-02-15 | 湖北新四海化工股份有限公司 | High efficiency composite defoaming agent and preparation method thereof |
| CN107164001A (en) * | 2017-06-02 | 2017-09-15 | 汪建军 | A kind of compound emulsifying agent and preparation method thereof |
| CN107629214A (en) * | 2017-07-19 | 2018-01-26 | 合肥普庆新材料科技有限公司 | A kind of efficient wetting agent of organosilicon |
| CN107817316A (en) * | 2017-10-30 | 2018-03-20 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of detection method of titanium dioxide organic silicon emulsion ph stability |
| CN109233296A (en) * | 2018-08-23 | 2019-01-18 | 南京瑞思化学技术有限公司 | A method of improving stability of organic silicone emulsion |
| CN109929120A (en) * | 2019-01-03 | 2019-06-25 | 南京瑞思化学技术有限公司 | A kind of organic silicon emulsion |
| CN110370433A (en) * | 2019-07-03 | 2019-10-25 | 中建商品混凝土有限公司 | A kind of concrete multifunction surface optimization agent and preparation method thereof |
| CN110370433B (en) * | 2019-07-03 | 2021-07-30 | 中建商品混凝土有限公司 | Multifunctional surface optimizing agent for concrete and preparation method thereof |
| CN111713493A (en) * | 2020-07-23 | 2020-09-29 | 陕西农塔生物数据研究有限公司 | Synergistic insecticidal auxiliary agent |
| CN112185603A (en) * | 2020-10-12 | 2021-01-05 | 山东省分析测试中心 | Phosphorus fixing agent stable suspended oil-in-water high internal phase emulsion and preparation method and application thereof |
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