CN113214498A - Preparation method of emulsified silicone oil with high viscosity and good stability - Google Patents
Preparation method of emulsified silicone oil with high viscosity and good stability Download PDFInfo
- Publication number
- CN113214498A CN113214498A CN202110474181.1A CN202110474181A CN113214498A CN 113214498 A CN113214498 A CN 113214498A CN 202110474181 A CN202110474181 A CN 202110474181A CN 113214498 A CN113214498 A CN 113214498A
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- Prior art keywords
- silicone oil
- stirring
- preparation
- high viscosity
- good stability
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- 229920002545 silicone oil Polymers 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 18
- 238000004945 emulsification Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 5
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 5
- 238000010907 mechanical stirring Methods 0.000 claims abstract description 4
- 230000001804 emulsifying effect Effects 0.000 claims description 6
- -1 polyoxyethylene lauryl ether Polymers 0.000 claims description 4
- 229920000259 polyoxyethylene lauryl ether Polymers 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 2
- 238000010008 shearing Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000011112 process operation Methods 0.000 abstract 1
- 239000000839 emulsion Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000013517 stratification Methods 0.000 description 3
- 239000002671 adjuvant Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
Classifications
-
- 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
- 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
- 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
- C08J2383/04—Polysiloxanes
Abstract
The invention discloses a preparation method of emulsified silicone oil with high viscosity and good stability, which is characterized by comprising the following steps: taking 100 ten thousand centistokes dimethyl silicone oil as an oil phase and lauryl alcohol polyoxyethylene ether as an emulsifier, adopting a phase inversion emulsification method, uniformly stirring the dimethyl silicone oil and the emulsifier under mechanical stirring, slowly dripping warm water while stirring, quickly adding the rest water when the system is in phase inversion, and continuously stirring to obtain the emulsified silicone oil with high viscosity and good stability. The invention can realize the emulsification of the dimethyl silicone oil with high viscosity of 100 ten thousand centistokes by adopting the conventional mechanical stirring, and the process operation is simple and convenient. The investment of expensive equipment such as a shearing machine, a homogenizer and the like is avoided, and the production cost is reduced.
Description
Technical Field
The invention belongs to the technical field of preparation of surfactants, and particularly relates to a preparation method of emulsified silicone oil with high viscosity and good stability.
Background
An emulsion is a dispersion formed from two (or more) liquids that are completely immiscible (or partially miscible). The emulsified silicone oil (silicone oil emulsion) is an O/W type emulsion obtained by stirring silicone oil, an emulsifier and deionized water at a high speed according to a certain emulsifying formula and sequence.
So far, the problem of the research of the expert scholars is still that the emulsified silicone oil with excellent performance is still the problem of the research. Since silicone oil itself is not easily emulsified, the higher the viscosity of the emulsion, the more difficult it is to emulsify. Meanwhile, the silicone oil is a demulsifier and a defoaming agent, and the stability of the emulsion is deteriorated due to the addition of the silicone oil. Therefore, the silicone oil is better emulsified, the stability of the emulsified silicone oil is improved, and the problems which need to be solved by experts, scholars and enterprises are solved urgently.
The emulsification of the low-viscosity silicone oil is relatively easy, the proportion of the silicone oil, the emulsifier and the water is adjusted appropriately, and the stable emulsification can be obtained by stirring and emulsifying at the appropriate emulsification temperature (the preparation research of the emulsified silicone oil [ J ]. Zhejiang chemical industry, 2012(4):6-9 ], the preparation conditions research of the silicone oil emulsion for hair-shift, 2014, 33(2): 97-99.). However, no report is made that high viscosity silicone oil is emulsified into a silicone oil emulsion by conventional stirring.
Disclosure of Invention
The invention mainly aims to overcome the defects in the prior art and provide a preparation method of emulsified silicone oil with high viscosity and good stability. The invention takes dimethyl silicone oil with 100 ten thousand centistokes viscosity as oil phase, and lauryl alcohol polyoxyethylene ether as emulsifier, and adopts a kettle type stirring process to prepare emulsified silicone oil products with good stability.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme.
The invention provides a preparation method of emulsified silicone oil with high viscosity and good stability, which comprises the following steps:
taking 100 ten thousand centistokes dimethyl silicone oil as an oil phase and lauryl alcohol polyoxyethylene ether as an emulsifier, adopting a phase inversion emulsification method, uniformly stirring the dimethyl silicone oil and the emulsifier under mechanical stirring, slowly dripping warm water while stirring, quickly adding the rest water when the system is in phase inversion, and continuously stirring to obtain the emulsified silicone oil with high viscosity and good stability.
Preferably, the polyoxyethylene lauryl ether is selected from any one of AEO-3 and L-23.
Preferably, the polyoxyethylene lauryl ether is a mixture of AEO-3 and L-23, and the mass of the AEO-3 and the L-23 is 1: 3-6: 1.
Preferably, the stirring speed is 100-800 r/min.
Preferably, the emulsifying temperature is 70-90 ℃.
Preferably, the emulsifying time is 20-60 min.
Preferably, the mass ratio of the dimethyl silicone oil to the emulsifier is (50-60): (5-15).
By the technical scheme, the invention at least has the following advantages: the invention provides a method for preparing emulsified silicone oil with high viscosity and good stability, which has simple process and low cost. The invention takes dimethyl silicone oil with 100 ten thousand centistokes viscosity as oil phase, and lauryl alcohol polyoxyethylene ether as emulsifier, and adopts a kettle type stirring process to prepare emulsified silicone oil products with good stability. The method provided by the invention abandons shearing and homogenizing equipment required by the traditional high-viscosity silicone oil emulsification, and has the advantages of simple process and low cost.
In summary, the preparation method of the present invention has the advantages and practical values described above, and similar designs are not published or used in similar products, but rather are innovative, and it has great improvements in product components or functions, great progress in technology, good and practical effects, and multiple enhanced effects compared with the existing preparation methods, thereby being more practical, having industrial wide utilization value, and being a novel, advanced and practical new design.
The foregoing is a summary of the present invention, and in order to provide a clear understanding of the technical means of the present invention and to be implemented in accordance with the present specification, the following is a detailed description of the preferred embodiments of the present invention.
Specific embodiments of the present invention are given in detail by the following examples.
Detailed Description
To further illustrate the technical means and effects of the present invention for achieving the predetermined objects, the following detailed description of the embodiments, methods and effects of the adjuvant and the herbal water-aqua according to the present invention will be given with reference to the preferred embodiments.
Example 1
Dimethyl silicone oil with the viscosity of 100 ten thousand centistokes is used as a raw material, AEO-3 and L-23 are used as compound emulsifiers, the proportion of the silicone oil, the emulsifiers and water is kept at 60:5:35, a phase inversion emulsification method is adopted, the emulsification temperature is 70 ℃, the stirring speed is 800r/min, the AEO-3: L-23=1:3, and emulsification is carried out for 30min, so that the emulsified silicone oil product is obtained. After the prepared emulsified silicone oil product is centrifuged at 3000r/min for 30min at high speed, the phenomenon of water-oil stratification does not occur, and the emulsion is stable.
Example 2
Dimethyl silicone oil with the viscosity of 100 ten thousand centistokes is used as a raw material, AEO-3 and L-23 are used as compound emulsifiers, the proportion of the silicone oil, the emulsifiers and water is kept at 50:15:35, a phase inversion emulsification method is adopted, the emulsification temperature is 80 ℃, the stirring speed is 100 r/min, the AEO-3: L-23=3:1, and the emulsification is carried out for 60min, so that the emulsified silicone oil product is obtained. After the prepared emulsified silicone oil product is centrifuged at 3000r/min for 30min at high speed, the phenomenon of water-oil stratification does not occur, and the emulsion is stable.
Example 3
Dimethyl silicone oil with the viscosity of 100 ten thousand centistokes is used as a raw material, AEO-3 and L-23 are used as compound emulsifiers, the proportion of the silicone oil, the emulsifiers and water is kept at 55:10:35, a phase inversion emulsification method is adopted, the emulsification temperature is 90 ℃, the stirring speed is 400 r/min, the AEO-3: L-23=6:1, and the emulsification is carried out for 50min, so that the emulsified silicone oil product is obtained. After the prepared emulsified silicone oil product is centrifuged at 3000r/min for 30min at high speed, the phenomenon of water-oil stratification does not occur, and the emulsion is stable.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. The preparation method of the emulsified silicone oil with high viscosity and good stability is characterized by comprising the following steps:
taking 100 ten thousand centistokes dimethyl silicone oil as an oil phase and lauryl alcohol polyoxyethylene ether as an emulsifier, adopting a phase inversion emulsification method, uniformly stirring the dimethyl silicone oil and the emulsifier under mechanical stirring, slowly dripping warm water while stirring, quickly adding the rest water when the system is in phase inversion, and continuously stirring to obtain the emulsified silicone oil with high viscosity and good stability.
2. The method according to claim 1, wherein the polyoxyethylene lauryl ether is selected from any one of AEO-3 and L-23.
3. The preparation method of claim 1, wherein the polyoxyethylene lauryl ether is a mixture of AEO-3 and L-23, and the mass of the AEO-3 and the L-23 is 1: 3-6: 1.
4. The preparation method according to claim 1, wherein the stirring speed is 100 to 800 r/min.
5. The method according to claim 1, wherein the emulsifying temperature is 70 to 90 ℃.
6. The method according to claim 1, wherein the emulsifying time is 20 to 60 min.
7. The preparation method according to claim 1, wherein the mass ratio of the dimethyl silicone oil to the emulsifier is (50-60): (5-15).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110474181.1A CN113214498A (en) | 2021-04-29 | 2021-04-29 | Preparation method of emulsified silicone oil with high viscosity and good stability |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110474181.1A CN113214498A (en) | 2021-04-29 | 2021-04-29 | Preparation method of emulsified silicone oil with high viscosity and good stability |
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| CN113214498A true CN113214498A (en) | 2021-08-06 |
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| CN202110474181.1A Pending CN113214498A (en) | 2021-04-29 | 2021-04-29 | Preparation method of emulsified silicone oil with high viscosity and good stability |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106633103A (en) * | 2016-12-30 | 2017-05-10 | 江西蓝星星火有机硅有限公司 | Preparation method of high-internal-phase-viscosity polysiloxane emulsion |
| CN106700095A (en) * | 2016-12-30 | 2017-05-24 | 江西蓝星星火有机硅有限公司 | Preparation method of large-particle-size high-viscosity methyl silicon oil emulsion |
| CN109912814A (en) * | 2019-03-27 | 2019-06-21 | 江西蓝星星火有机硅有限公司 | A kind of preparation method and application of high viscosity silicon raw rubber lotion |
-
2021
- 2021-04-29 CN CN202110474181.1A patent/CN113214498A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106633103A (en) * | 2016-12-30 | 2017-05-10 | 江西蓝星星火有机硅有限公司 | Preparation method of high-internal-phase-viscosity polysiloxane emulsion |
| CN106700095A (en) * | 2016-12-30 | 2017-05-24 | 江西蓝星星火有机硅有限公司 | Preparation method of large-particle-size high-viscosity methyl silicon oil emulsion |
| CN109912814A (en) * | 2019-03-27 | 2019-06-21 | 江西蓝星星火有机硅有限公司 | A kind of preparation method and application of high viscosity silicon raw rubber lotion |
Non-Patent Citations (2)
| Title |
|---|
| 张存社;王前进;南蓉;李华杰;习娟;: "超高黏度聚二甲基硅氧烷大粒径乳液的制备", 应用化工, no. 10, pages 1887 - 1890 * |
| 王秋实;倪邦庆;范明明;刘华英;: "硅油乳状液制备新工艺研究", 应用化工, no. 08, pages 127 - 132 * |
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