CN106633103A - Preparation method of high-internal-phase-viscosity polysiloxane emulsion - Google Patents
Preparation method of high-internal-phase-viscosity polysiloxane emulsion Download PDFInfo
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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
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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
- C08L83/04—Polysiloxanes
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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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- C08L83/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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- 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
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- 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
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- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
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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
- C08J2483/04—Polysiloxanes
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Abstract
The invention discloses a method of preparing high-internal-phase-viscosity polysiloxane emulsion through a high-effective shear emulsifying mechanical device. The method is simple and high-effective and is convenient to carry out. The polysiloxane emulsion has excellent stability and excellent application performance. The emulsion can be used in the fields of household and personal care, and is free of roll sticking, demulsification and oil floating during a post-finishing process of fabrics and leather.
Description
Technical field
The present invention relates to a kind of preparation method of the polysiloxane emulsion of high internal phase viscosities, belongs to chemical products field.
Background technology
Organopolysiloxane due to fabulous chemical stability, heat resistance, hydrophobicity and relatively low surface tension with
And good biocompatibility so that it is widely used.But due to the hydrophobicity of silicone oil it is very strong, it is difficult to be dispersed in water
In system.And the appearance of organic silicon emulsion solves this problem, it is widely used in the form of an emulsion spinning more than current silicone oil
The sides such as weaver's industry, plastic processing, papermaking, finishing agent, defoamer, releasing agent, building surface waterproofing, cosmetics and ink formulations
Face.
Using Mechanical Method prepare organic silicon emulsion be silicone oil is dispersed under strong mechanical shearing effect it is tiny micro-
Grain is used as dispersion phase, and emulsifying agent forms one layer of molecular interface film with certain mechanical strength on the interface of water and oil, with
Enable that oil phase particulate is stable to be dispersed in water phase, be difficult aggregation and become big and be layered, so as to obtain water oil uniformly emulsion.For many years
Come, have been used up high pressure homogenizer, colloid mill and high-efficient homogeneous vacuum emulsifying machine next life galactopoiesis liquid.Patent US2755194,
US4784844, US530028 to be referred to and can be readily available the relatively low emulsion of internal phase viscosities by the said equipment.But but it is difficult water
In being added to viscous silicone fluid, and while give emulsion of enough emulsification pretreatments into high stability.
It is silicon rubber that patent CN100500742C is mentioned by preparing interior phase with double screw extruder, silane elastomer,
The oil-in-water emulsions such as organic siliconresin.But this kind of method can only prepare the emulsion that interior phase is silane elastomer class.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the polysiloxane emulsion of high internal phase viscosities, by a kind of machinery
The method of conversion is prepared for the organic silicon emulsion of high internal phase viscosities, compared with other conventional arts, organosilicon prepared by the method
Emulsion has more high stability, there is provided the interior phase organosiloxane of higher molecular weight, and the more excellent property of product is imparted in application
Energy.
A kind of preparation method of the polysiloxane emulsion of high internal phase viscosities, concretely comprises the following steps：
（1）The component of following parts by weight is added in high-efficient shear emulsifying equipment at 20-30 DEG C of temperature and normal pressure：
The silicone oil of 30-80 parts, the emulsifying agent of 1-10 parts, the purified water of 0.5-20 parts, after mixing in high-efficient shear emulsifying equipment
Mixture is applied shearing force 60-300min to emulsify；
（2）Add purified water, assistant for emulsifying agent, bactericide, PH conditioning agents and finally give oil-in-water emulsion.
The step（1）In silicone oil represent for following structural formula：
Wherein, R2For methyl, R1For methyl or hydroxyl, R3For methyl, aminoethylaminopropyl, phenyl, alkyl or silicon hydrogen, m and n is each
From for positive integer or 0.
The step（1）In silicon oil viscosity be from 5000mpa s to 1000000mpa s.
The step（1）In silicone oil be made up of one or more silicone oil, such as various, need first be well mixed oil phase
Afterwards, then next step operation is carried out.
The step（1）In silicone oil be preferably polydimethyl siloxane fluid, hydroxyl polydimethyl siloxane fluid, amido silicon oil.
The step（1）In emulsifying agent be anion, cation, nonionic, amphoteric surfactant in one kind or
Several, in the C8-C15 alkylation APEOs of preferred nonionic compounds of one or more.
The step（1）The homogeneous oil phase viscosity obtained after emulsification is from 50000mpa s to 1000000mpa s.
Described step（2）In assistant for emulsifying agent be anion surfactant, cationic surfactant, nonionic table
One or more in the activating agent of face, preferably anionic emulsifier.
Described step（2）In bactericide be preferably methylisothiozoline, methyl chloride isothiazoline or diformazan hydantoins.
Described step（2）In PH conditioning agents be weak acid or weak base, preferably triethanolamine or acetic acid.
Described high-efficient shear emulsifying equipment can be EKATO KOAX equipment.
It is an advantage of the current invention that：The emulsion prepared by this kind of method not only has excellent stability, size tunable,
Narrowly distributing, and preparation process is simple, reproducible, easy to operate, quick, the oil-in-water emulsion of preparation has compared with stiff stability,
Room temperature storage is more than 12 months, and 50 DEG C are more than 30 days.The silicone oil good film-forming property of high internal phase viscosities, while giving smooth soft hand
Sense, this product is all widely used in personal care product, coating products, household care products or leather product.
The difference of the present invention and other patented methods
| This patent | Screw extruder technique | Super-pressure emulsion polymerization technique | Anionic polymerization process | |
| Pressure | Normal pressure | Micro-vacuum | >1Mpa | Normal pressure |
| Temperature | 20-30℃ | 60℃ | 10-50℃ | 85℃ |
| Particle diameter | >5um | 0.3 um | 0.4 um | <0.5 um |
| Internal phase viscosities | 50,000-1,000,000 mpa•s | 1,000,000,000 mpa•s | 300,000 mpa•s | 113,000 mpa•s |
As can be seen from the above table, at the present invention is using temperature 20-30 DEG C and condition of normal pressure, it is possible to prepare the emulsion and produce
Product, and additive method must react under high temperature or condition of high voltage, it is seen that present invention reaction is gentle, the oil-in-water emulsion of preparation
Also have compared with stiff stability.
Specific embodiment
To more fully understand the present invention, technical scheme is described in detail with specific embodiment below, but this
Invention is not limited to this.
Embodiment 1
The hydroxy silicon oil of 45 parts of 550,000mpas, 4 parts of alkylation APEOs, 2 parts of purified waters are added into efficiently shearing breast
In change equipment, temperature is 20～300C, under normal pressure after stirring and emulsifying 150min, adds 1 part of lauryl sodium sulfate, methyl chloride different
Final product emulsion is obtained after thiazolinone, acetic acid and 48 parts of purified waters.
Embodiment 2
High-efficient shear emulsifying is added to set the dimethicone of 5 parts of 5000mpas, the hydroxy silicon oil of 40 parts of 550,000mpas
In standby, whole system is well mixed after uniform stirring, adds 4 parts of alkylation APEOs, 2 parts of purified waters, and temperature is 20～
300C, under normal pressure after stirring and emulsifying 120min, 1 part of lauryl sodium sulfate of addition, methylchloroisothiazandnone, acetic acid and 48 parts
Final product emulsion is obtained after purified water.
Embodiment 3
The dimethicone of 45 parts of 60,000mpas is added in high-efficient shear emulsifying equipment, 4 parts of alkylation polyoxy second are added
Alkene ether and 2 parts of purified waters, temperature is 20～300C, stirs after 180min under normal pressure, adds 1 part of lauryl sodium sulfate, methyl
Final emulsion is obtained after OIT, acetic acid and 48 parts of purified water.
Embodiment 4
45 parts of 80,000mpas hydroxy silicon oils are added in high-efficient shear emulsifying equipment, 4 parts of emulsifying agents of addition, 2 parts of purified waters,
Temperature is 20～300C, stirs after 180min under normal pressure, adds 1 part of sldium lauryl sulfate, methylisothiazolinone, acetic acid and 38
Final emulsion is obtained after the purified water of part.
If table 1 below is the test result of organic silicon emulsion
The present invention is as follows to the method for testing of every physicochemical property of the organic silicon emulsion for preparing：
Dewatering ability：Emulsion 20ml, a is added to be put into centrifuge in 20ml centrifuge tubes, 3000rpm rotation speed operations 30min
Afterwards, sample is observed without layering, belong to steady quality.
Heat endurance：Emulsion is put into vial with cover, 50 are put into0In the constant temperature oven of C after 30 days, sample without point
Layer, without demulsifying phenomenon, belong to steady quality.
Storage stability：By emulsion（It is with cover）After placing 12 months at room temperature, without breakdown of emulsion, without lamination, belong to quality
It is stable.
Stability towards electrolytes：By 15g emulsions, 20gNaCl, 80g H2O is added in beaker, 500rpm rotation speed operations
10min, after standing 24h, sample breakdown of emulsion, without lamination belongs to steady quality.
Claims (10)
1. a kind of preparation method of the polysiloxane emulsion of high internal phase viscosities, it is characterized by：Concretely comprise the following steps：
（1）The component of following parts by weight is added in high-efficient shear emulsifying equipment at 20-30 DEG C of temperature and normal pressure：
The silicone oil of 30-80 parts, the emulsifying agent of 1-10 parts, the purified water of 0.5-20 parts, after mixing in high-efficient shear emulsifying equipment
Mixture is applied shearing force 60-300min to emulsify；
（2）Add purified water, assistant for emulsifying agent, bactericide, PH conditioning agents and finally give oil-in-water emulsion.
2. a kind of preparation method of the polysiloxane emulsion of high internal phase viscosities as claimed in claim 1, it is characterized by：Step
（1）In silicone oil represent for following structural formula：
Wherein, R2For methyl, R1For methyl or hydroxyl, R3For methyl, aminoethylaminopropyl, phenyl, alkyl or silicon hydrogen, m and n is each
From for positive integer or 0.
3. a kind of preparation method of the polysiloxane emulsion of high internal phase viscosities as claimed in claim 1, it is characterized by：The step
Suddenly（1）In silicon oil viscosity be from 5000mpa s to 1000000mpa s.
4. a kind of preparation method of the polysiloxane emulsion of high internal phase viscosities as claimed in claim 1, it is characterized by：The step
Suddenly（1）In silicone oil be made up of one or more silicone oil, such as various, after needing first be well mixed oil phase, then carry out next step
Operation.
5. a kind of preparation method of the polysiloxane emulsion of high internal phase viscosities as claimed in claim 1, it is characterized by：The step
Suddenly（1）In silicone oil be preferably polydimethyl siloxane fluid, hydroxyl polydimethyl siloxane fluid, amido silicon oil.
6. a kind of preparation method of the polysiloxane emulsion of high internal phase viscosities as claimed in claim 1, it is characterized by：The step
Suddenly（1）In emulsifying agent be anion, cation, nonionic, amphoteric surfactant in one or more, preferred nonionic
The compound of one or more in the C8-C15 alkylation APEOs of type.
7. a kind of preparation method of the polysiloxane emulsion of high internal phase viscosities as claimed in claim 1, it is characterized by：The step
Suddenly（1）The homogeneous oil phase viscosity obtained after emulsification is from 50000mpa s to 1000000mpa s.
8. a kind of preparation method of the polysiloxane emulsion of high internal phase viscosities as claimed in claim 1, it is characterized by：Described
Step（2）In assistant for emulsifying agent be anion surfactant, cationic surfactant, nonionic surfactant in one
Plant or several, preferably anionic emulsifier.
9. a kind of preparation method of the polysiloxane emulsion of high internal phase viscosities as claimed in claim 1, it is characterized by：Described
Step（2）In bactericide be preferably methylisothiozoline, methyl chloride isothiazoline or diformazan hydantoins.
10. a kind of preparation method of the polysiloxane emulsion of high internal phase viscosities as claimed in claim 1, it is characterized by：It is described
The step of（2）In PH conditioning agents be weak acid or weak base, preferably triethanolamine or acetic acid.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110403853A (en) * | 2019-09-06 | 2019-11-05 | 广州宏翼新材料有限公司 | A kind of novel polymeric silicone oil emulsion and preparation method |
| CN110922891A (en) * | 2019-12-17 | 2020-03-27 | 山东易石环保新材料有限公司 | Emulsion type silicone paper machine drying cylinder stripping agent and preparation method thereof |
| CN110964436A (en) * | 2019-12-17 | 2020-04-07 | 山东易石环保新材料有限公司 | Organic silicon emulsion type paper machine dry net stripping agent and preparation method thereof |
| CN113214498A (en) * | 2021-04-29 | 2021-08-06 | 南京威尔生物科技有限公司 | Preparation method of emulsified silicone oil with high viscosity and good stability |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110403853A (en) * | 2019-09-06 | 2019-11-05 | 广州宏翼新材料有限公司 | A kind of novel polymeric silicone oil emulsion and preparation method |
| CN110922891A (en) * | 2019-12-17 | 2020-03-27 | 山东易石环保新材料有限公司 | Emulsion type silicone paper machine drying cylinder stripping agent and preparation method thereof |
| CN110964436A (en) * | 2019-12-17 | 2020-04-07 | 山东易石环保新材料有限公司 | Organic silicon emulsion type paper machine dry net stripping agent and preparation method thereof |
| CN113214498A (en) * | 2021-04-29 | 2021-08-06 | 南京威尔生物科技有限公司 | Preparation method of emulsified silicone oil with high viscosity and good stability |
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