CN103665395B - A kind of preparation method of silicone oil - Google Patents
A kind of preparation method of silicone oil Download PDFInfo
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- CN103665395B CN103665395B CN201310641248.1A CN201310641248A CN103665395B CN 103665395 B CN103665395 B CN 103665395B CN 201310641248 A CN201310641248 A CN 201310641248A CN 103665395 B CN103665395 B CN 103665395B
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Abstract
The invention discloses a kind of preparation method of silicone oil, by be the dimethyl silicone oil of 2000pa.s by viscosity, emulsifying agent, water, smoke suppressor, oxidation inhibitor, sanitas, water allocates in proportion and forms.The method has prepared uniform particle diameter, stable silicone oil emulsion.
Description
Technical field
The present invention relates to silicone oil preparing technical field, particularly relate to a kind of preparation method of silicone oil.
Background technology
Silicone oil is a kind of organopolysiloxane of different polymerization degree chain-like structure, is generally colourless (or faint yellow), tasteless, nontoxic, not volatile liquid.Silicone oil not only has remarkable thermotolerance, electrical insulating property, weathering resistance, hydrophobicity, radiation resistance, physiological inertia and less surface tension, has low temperature coefficient of viscosity in addition, higher resistance to compression, has good application prospect.
Current silicone oil oneself become important component or the auxiliary agent of many makeup.Dimethyl silicone oil is one of wherein the most frequently used silicone oil, and simethicone emulsion can be applicable to the industries such as makeup, weaving, the demoulding, leather.Therefore, the silicone oil emulsion preparing good stability has become the key point of silicone oil application.Traditional method preparing silicone oil emulsion mainly contains mechanical stirring, ultrasonic emulsification, colloidal film emulsification, homogenizing emulsifying method, the common shortcoming of these preparation methods is that the size distribution of obtained emulsion is wider, this is mainly because the shearing force that emulsion is suffered in preparation process is uneven, be difficult to the drop generating uniform particle diameter, finally cause instability and and then the layering of emulsion.Thus be very restricted in actual applications.Therefore, find and a kind ofly the method for emulsion of homogeneous, the good stability of preparation size can have very important realistic meaning.
The present invention is directed to defect and the deficiency of traditional silicon fat liquor preparation method, by changing the formula of silicone oil emulsification agent, finally having prepared uniform particle diameter, stable silicone oil emulsion, for solid basis is established in the application after it in shampoo and hair conditioner.
Summary of the invention
Object of the present invention is exactly defect for above-mentioned existence and provides a kind of preparation method of silicone oil emulsion.The method has prepared uniform particle diameter, stable silicone oil emulsion.
Preparation method's technical scheme of a kind of silicone oil of the present invention is, by be the dimethyl silicone oil of 2000pa.s by viscosity, emulsifying agent, water, smoke suppressor, oxidation inhibitor, sanitas, water allocates in proportion and forms.
Comprise following composition by weight:
45-65 part dimethyl silicone oil;
10-20 part emulsifying agent;
0.2-1 part smoke suppressor;
1.2-2 part oxidation inhibitor;
1-5 part sanitas;
10-15 part water.
Emulsifying agent is at least one in Span60, Tween60, Span80, Tween80, OP-10.
Smoke suppressor is at least one in ferrocene, molybdic oxide, eight molybdic acids, aluminium hydroxide.
Oxidation inhibitor is at least one in phosphoric acid salt, phosphate derivative, and sanitas is barium sulfonate.
Concrete steps are as follows:
(1) by dimethyl silicone oil, OP-10, water adds in container in proportion, mixes;
(2) transfer in autoclave pressure by the emulsion mixed in step (1), then add ferrocene, sodium phosphate, barium sulfonate, closing presure still carries out being uniformly mixed 2-4h, can obtain the silicone oil emulsion had good stability.
In step (1), mixing condition is 70 DEG C, 200rpm uniform stirring 1 hour.
In step (2), autoclave pressure internal pressure is 2 normal atmosphere, and temperature is 80 DEG C, and stirring velocity is 200rp.
Beneficial effect of the present invention is: the inventive method is simple to operation, the silicone oil emulsion uniform particle diameter of preparation, good stability.
embodiment:
In order to understand the present invention better, describe technical scheme of the present invention in detail with specific examples below, but the present invention is not limited thereto.
embodiment 1
Be the dimethyl silicone oil of 2000pa.s by 45 parts of (weight part) viscosity, 10 parts of (weight part) OP-10,10 parts of (weight part) water add in container, 70 DEG C, and 200rpm uniform stirring 1 hour, whole system mixes.The above-mentioned emulsion mixed is transferred in autoclave pressure, then add 0.2(weight part) ferrocene, 1.2(weight part) sodium phosphate, 1 part of (weight part) barium sulfonate, closing presure still carries out being uniformly mixed 2h, still internal pressure is kept to be external atmosphere pressure, temperature is 80 DEG C, and stirring velocity is 200rp.The silicone oil emulsion A had good stability can be obtained.
embodiment 2
Be the dimethyl silicone oil of 2000pa.s by 55 parts of (weight part) viscosity, 20 parts (weight part Tween60,10 parts of (weight part) tap water add in container, 70 DEG C, and 200rpm uniform stirring 1 hour, whole system mixes.The above-mentioned emulsion mixed is transferred in autoclave pressure, then add 0.4(weight part) ferrocene, 1.4(weight part) sodium phosphate, 2 parts of (weight part) barium sulfonates, closing presure still carries out being uniformly mixed 2.5h, still internal pressure is kept to be external atmosphere pressure, temperature is 80 DEG C, and stirring velocity is 200rp.The silicone oil emulsion had good stability can be obtained
b.
embodiment 3
Be the dimethyl silicone oil of 2000pa.s by 65 parts of (weight part) viscosity, 20 parts of (weight part) Span60,15 parts of (weight part) tap water add in container, 70 DEG C, and 200rpm uniform stirring 1 hour, whole system mixes.The above-mentioned emulsion mixed is transferred in autoclave pressure, then add 0.6(weight part) molybdic oxide, 1.6(weight part) sodium phosphate, 3 parts of (weight part) barium sulfonates, closing presure still carries out being uniformly mixed 3.0h, still internal pressure is kept to be external atmosphere pressure, temperature is 80 DEG C, and stirring velocity is 200rp.The silicone oil emulsion C had good stability can be obtained.
embodiment 4
Be the dimethyl silicone oil of 2000pa.s by 45 parts of (weight part) viscosity, 10 parts of (weight part) OP-10,10 parts of (weight part) tap water add in container, 70 DEG C, and 200rpm uniform stirring 1 hour, whole system mixes.The above-mentioned emulsion mixed is transferred in autoclave pressure, then add 0.8(weight part) ferrocene, 1.8(weight part) sodium phosphate, 4 parts of (weight part) barium sulfonates, closing presure still carries out being uniformly mixed 3.0h, still internal pressure is kept to be external atmosphere pressure, temperature is 80 DEG C, and stirring velocity is 200rp.The silicone oil emulsion D had good stability can be obtained.
embodiment 5
Be the dimethyl silicone oil of 2000pa.s by 45 parts of (weight part) viscosity, 10 parts of (weight part) OP-10,10 parts of (weight part) tap water add in container, 70 DEG C, and 200rpm uniform stirring 1 hour, whole system mixes.The above-mentioned emulsion mixed is transferred in autoclave pressure, then add 1.0(weight part) ferrocene, 2.0(weight part) sodium phosphate, 5 parts of (weight part) barium sulfonates, closing presure still carries out being uniformly mixed 3.5h, still internal pressure is kept to be external atmosphere pressure, temperature is 80 DEG C, and stirring velocity is 200rp.The silicone oil emulsion E had good stability can be obtained.
embodiment 6
The stability test of silicone oil emulsion: add samples of latex in centrifuge tube, puts into supercentrifuge, with the centrifugation 30min of 4000r/min.If samples of latex is not stratified, not oil spill, show emulsion-stabilizing.Stability grade is evaluated according to oil yield and water outlet.Not fuel-displaced, stability scoring is 10, and stable water outlet scoring is 0.
The dispersiveness of silicone oil emulsion measures, and with reference to the measuring method of agriculture breast, be divided into Pyatyi evaluation, order of excellence is: one-level ﹥ secondary ﹥ tri-grades of ﹥ level Four ﹥ Pyatyis.
The stability data of table 1 silicone oil emulsion
| Silicone oil | Stability of emulsion | Emulsion dispersibility |
| A | 8 | Secondary |
| B | 9 | Secondary |
| C | 8 | Secondary |
| D | 9 | Secondary |
| E | 9 | Secondary |
Claims (4)
1. a preparation method for silicone oil, is characterized in that, by be the dimethyl silicone oil of 2000pa.s by viscosity, emulsifying agent, smoke suppressor, oxidation inhibitor, sanitas, water allocates in proportion and forms;
Comprise following composition by weight:
45-65 part dimethyl silicone oil;
10-20 part emulsifying agent;
0.2-1 part smoke suppressor;
1.2-2 part oxidation inhibitor;
1-5 part sanitas;
10-15 part water;
Emulsifying agent is at least one in Span60, Tween60, Span80, Tween80, OP-10;
Smoke suppressor is at least one in ferrocene, molybdic oxide, eight molybdic acids, aluminium hydroxide;
Oxidation inhibitor is at least one in phosphoric acid salt, phosphate derivative, and sanitas is barium sulfonate.
2. the preparation method of a kind of silicone oil according to claim 1, it is characterized in that, concrete steps are as follows:
(1) by dimethyl silicone oil, OP-10, water adds in container in proportion, mixes;
(2) transfer in autoclave pressure by the emulsion mixed in step (1), then add ferrocene, sodium phosphate, barium sulfonate, closing presure still carries out being uniformly mixed 2-4h, can obtain the silicone oil emulsion had good stability.
3. the preparation method of a kind of silicone oil according to claim 2, is characterized in that, in step (1), mixing condition is 70 DEG C, 200rpm uniform stirring 1 hour.
4. the preparation method of a kind of silicone oil according to claim 2, is characterized in that, in step (2), autoclave pressure internal pressure is 2 normal atmosphere, and temperature is 80 DEG C, and stirring velocity is 200rpm.
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| CN108250454A (en) * | 2018-01-05 | 2018-07-06 | 芜湖维软新材料有限公司 | A kind of preparation method of silicone oil emulsion |
| CN109578511A (en) * | 2018-11-06 | 2019-04-05 | 宁波赛德森减振系统有限公司 | A kind of silicone oil for internal combustion engine torsional vibration damper |
| CN111320874A (en) * | 2019-12-25 | 2020-06-23 | 南通恒光大聚氨酯材料有限公司 | Medium-high density hydrogen-containing silicone oil and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1942509A (en) * | 2004-04-15 | 2007-04-04 | 瓦克化学有限公司 | Process for the continuous preparation of silicone emulsions |
| CN101541889A (en) * | 2006-11-29 | 2009-09-23 | 陶氏康宁公司 | Aqueous emulsions of silicone resins |
| CN102718978A (en) * | 2012-07-12 | 2012-10-10 | 南京四新科技应用研究所有限公司 | Method for reducing viscosity of organic silicone emulsion |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1942509A (en) * | 2004-04-15 | 2007-04-04 | 瓦克化学有限公司 | Process for the continuous preparation of silicone emulsions |
| CN101541889A (en) * | 2006-11-29 | 2009-09-23 | 陶氏康宁公司 | Aqueous emulsions of silicone resins |
| CN102718978A (en) * | 2012-07-12 | 2012-10-10 | 南京四新科技应用研究所有限公司 | Method for reducing viscosity of organic silicone emulsion |
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Effective date of registration: 20170526 Address after: 528000, No. 2 Li Feng South Road, Ronggui Li Rong Industrial Zone, Shunde District, Guangdong, Foshan Patentee after: FOSHAN SHUNDE RONGWEI SYNTHETIC MATERIAL CO.,LTD. Address before: North Qilihe Road, Licheng District, Shandong city of Ji'nan Province, 250000 No. 2 Building No. 11 Patentee before: JINAN DEVELOPMENT ZONE XINGHUO SCIENCE AND TECHNOLOGY Research Institute |
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