CN1328321C - Method for preparing micropowder of organic silicone - Google Patents
Method for preparing micropowder of organic silicone Download PDFInfo
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- CN1328321C CN1328321C CNB2005100496277A CN200510049627A CN1328321C CN 1328321 C CN1328321 C CN 1328321C CN B2005100496277 A CNB2005100496277 A CN B2005100496277A CN 200510049627 A CN200510049627 A CN 200510049627A CN 1328321 C CN1328321 C CN 1328321C
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- micropowder
- preparation
- organic silicone
- dispersion liquid
- silicone oil
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Abstract
The present invention discloses a method for preparing the micropowder of organic silicone. The method prepares the micropowder of organic silicone by the procedures of dispersing liquid preparation, active silicon oil dispersion and crosslinking, crosslinking organic silicon particle curing, etc. The method of the present invention has the advantages of various product source, low cost and simple operation, and can prepare organic silicon powder with different grain diameters by the dosage of dispersing agents, and shearing and mixing speed control. The prepared organic silicon powder has good dispersivity.
Description
Technical field
The present invention relates to field of fine chemical, especially, relate to a kind of preparation method of micropowder of organic silicone.
Background technology
One of application of micropowder of organic silicone is the function weighting agent as the energy that has specific characteristics, because its peculiar oilness, hydrophobic nature, non-viscosity, flame retardant resistance, snappiness, wear resistance, therefore the application at aspects such as plastics, coating, printing ink, rubber and makeup can make product performance be improved, and this is that leading hi-tech, high profit economy has certain meaning from the extensive economy to science and technology to China's industry.Before this, famous organosilicon such as Dow corning company, Japan XINYUE, eastern beautiful organosilicon company, the fertile gram of Germany company succeeds in developing the high performance organo-silicon micropowder of median size at the various compositions of 0.1-50 mu m range in succession, these micro mists succeed in developing the update that has greatly promoted various chemical materialss.
The organosilyl output of China is very big, and meticulous organosilicon product is fewer, and the production of micropowder of organic silicone is still blank.
It seems from the situation of development, though external product mainly is to be used for high-grade paint in China's sale at present, to obtain the extremely smooth inferior light coating of silk shape; But along with growth in the living standard, using the characteristic such as lubricious, nontoxic, tasteless, comfortable can give full play to the organosilicon micro mist in makeup, is traditional stopping composition such as SiO
2/ CaCO
3Etc. incomparable, and makeup added value height.Can be used for plastics industry on the other hand.According to external new type chemical material report, the application of organosilicon micro mist has fundamentally solved organosilicon and has been difficult to blended problem mutually with plastics, for example in the fused polymeric amide, sneak into 5% organosilicon micro mist and can reduce the kinetic friction coefficient of product significantly, improve processibility, release property, wear resistance, oilness etc., so the organosilicon micro mist reduces cost on the basis that enlarges output, also is expected to be applied aspect plastics.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of preparation method of micropowder of organic silicone is provided.
The objective of the invention is to be achieved through the following technical solutions: a kind of preparation method of micropowder of organic silicone may further comprise the steps:
(1) preparation dispersion liquid: under the room temperature condition, in water, add fatty alcohol-polyoxyethylene ether, polyoxyethylene nonylphenol ether and sodium lauryl sulphate, make dispersion liquid;
(2) decentralized crosslinking of active silicone oil: active silicone oil and mixture of catalysts are added in the above-mentioned dispersion liquid, and static the depositing in back stirs;
(3) crosslinked organosilicon particle slaking: what will make contains the stirring of crosslinked organosilicon dispersion of particles liquid, filtration, washing, drying, thus the preparation micropowder of organic silicone.
Further, described step (1) is specially: under the room temperature condition, add fatty alcohol-polyoxyethylene ether 5～30 grams, polyoxyethylene nonylphenol ether 1～10 gram, sodium lauryl sulphate 1～10 gram in 100～500 gram water, thorough mixing is even; Regulate PH to 7～9, make dispersion liquid.
Further, described active silicone oil is containing hydrogen silicone oil, hydroxy silicon oil or their mixture, and described catalyzer is dibutyl tin laurate or stannous octoate.Described step (2) is specially: mixture 25～250 grams of getting containing hydrogen silicone oil or containing hydrogen silicone oil and hydroxy silicon oil, be added dropwise to stannous octoate or dibutyl tin laurate 0.01～1 gram, thorough mixing is even in 1～10 minute, this mixture is added in the described dispersion liquid, stir static at ambient temperature then depositing more than 24 hours.
Further, described step (3) is specially: the described static dispersion liquid of depositing is stirred with high-shear emulsion machine, the particle of a small amount of reunion is spread out, filter, wash, remove remaining catalyzer and tensio-active agent, under 70～90 ℃ of temperature, be dried to micropowder of organic silicone.
The invention has the beneficial effects as follows:
(1) desired raw material mainly is the bigger containing hydrogen silicone oil of output in domestic, hydroxy silicon oil and common tensio-active agent; Rule of origin is abundant, and cost is low;
(2) simple to operate;
(3) organic silica flour that consumption that can be by dispersion agent and controlling shear stirring velocity are prepared different grain warps;
(4) good dispersity of Zhi Bei organic silica flour.
Embodiment
Describe the present invention below in detail.
Raw material of the present invention mainly contains active silicone oil, tensio-active agent, catalyzer.Active silicone oil can be that containing hydrogen silicone oil, hydroxy silicon oil etc., tensio-active agent can be that sodium alkyl benzene sulfonate, polyoxyethylene nonylphenol ether, fatty alcohol-polyoxyethylene ether, sodium lauryl sulphate etc., catalyzer can be dibutyl tin laurate, stannous octoate etc.Preparation process is divided into following steps:
One, preparation dispersion liquid
Under the room temperature condition, in water, add tensio-active agent, make dispersion liquid.Be specially: under the room temperature condition, in 100～500 gram water, add fatty alcohol-polyoxyethylene ether 5～30 grams; Polyoxyethylene nonylphenol ether 1～10 gram; Sodium lauryl sulphate 1～10 gram thorough mixing is even; Regulate PH to 7～9, make dispersion liquid.
Two, the decentralized crosslinking of active silicone oil
Active silicone oil and mixture of catalysts are added in the above-mentioned dispersion liquid, and static the depositing in back stirs.Be specially: get containing hydrogen silicone oil or blended containing hydrogen silicone oil and hydroxy silicon oil 25～250 grams by a certain percentage, be added dropwise to stannous octoate or dibutyl tin laurate 0.01～1 gram, thorough mixing is even in 1～10 minute, there is a small amount of gas to produce in the mixing process, mainly be hydrogen, this mixture is added in the above-mentioned dispersion liquid, use the high-shear emulsion machine dispersed with stirring after 5～20 minutes, stirred 1～4 hour static at ambient temperature then depositing more than 24 hours more at a slow speed with common stirrer.There is bubble to produce in the process static depositing, impels active silicone oil crosslinking curing in aqueous systems simultaneously, obtain the dispersive organosilicon particle of slaking.Require the hydrogen of timely emptying output in the entire operation process.
Three, crosslinked organosilicon particle slaking
Contain the stirring of crosslinked organosilicon dispersion of particles liquid, filtration, washing, drying with what make, thus the preparation micropowder of organic silicone.Be specially: with containing of above-mentioned slaking crosslinked organosilicon dispersion of particles liquid stir with high-shear emulsion machine again, the particle of a small amount of reunion is spread out, catalyzer and the tensio-active agent filter, remnants removed in washing, obtain the meal of white, under 70～90 ℃ of situations, be dried to easy dispersed crosslinked organic silicone particle micro mist.
Can prepare the micropowder of organic silicone of smooth, transparent, 5～35 microns of proper spheres, good dispersity with method of the present invention.
Embodiment 1
Under the room temperature condition, water 1400 grams, polyoxyethylene nonylphenol ether 10 grams, fatty alcohol-polyoxyethylene ether 82 grams, sodium lauryl sulphate 10 grams are mixed, get dispersion liquid.
Get containing hydrogen silicone oil 500 grams and add stannous octoate 2 grams, thorough mixing is even in 2 minutes, in the mixing process, the bubble that has small quantity of hydrogen to produce, this mixture is added in the above-mentioned dispersion liquid, and the high-shear dispersed with stirring stirred at a slow speed after 10 minutes 2 hours, static depositing more than 24 hours.
With containing of above-mentioned slaking crosslinked organosilicon dispersion of particles liquid stir with high-shear emulsion machine again, a small amount of aggregate is spread out, the tensio-active agent of filter, remnants being removed in washing for three times, obtain the meal of white, be dried to easy dispersed crosslinked organic silicone particle micro mist under 70～90 ℃ of situations, grain is through 5～35 μ M.
Embodiment 2
Containing hydrogen silicone oil 500 grams are got among the embodiment 1 second step operation changed into containing hydrogen silicone oil 140 grams, hydroxy silicon oil 360 grams, other is constant.
The foregoing description is used for the present invention that explains, rather than limits the invention, and in the protection domain of spirit of the present invention and claim, any modification and change to the present invention makes all fall into protection scope of the present invention.
Claims (5)
1. the preparation method of a micropowder of organic silicone is characterized in that, may further comprise the steps:
(1) preparation dispersion liquid: under the room temperature condition, in water, add fatty alcohol-polyoxyethylene ether, polyoxyethylene nonylphenol ether and sodium lauryl sulphate, make dispersion liquid;
(2) decentralized crosslinking of active silicone oil: active silicone oil and mixture of catalysts are added in the above-mentioned dispersion liquid, and static the depositing in back stirs;
(3) crosslinked organosilicon particle slaking: what will make contains the stirring of crosslinked organosilicon dispersion of particles liquid, filtration, washing, drying, thus the preparation micropowder of organic silicone.
2. the preparation method of micropowder of organic silicone according to claim 1 is characterized in that, described step
(1) be specially: under the room temperature condition, add fatty alcohol-polyoxyethylene ether 5～30 grams, polyoxyethylene nonylphenol ether 1～10 gram, sodium lauryl sulphate 1～10 gram in 100～500 gram water, thorough mixing is even; Regulate PH to 7～9, make dispersion liquid.
3. the preparation method of micropowder of organic silicone according to claim 1 is characterized in that, described active silicone oil is containing hydrogen silicone oil, hydroxy silicon oil or their mixture, and described catalyzer is dibutyl tin laurate or stannous octoate.
4. the preparation method of micropowder of organic silicone according to claim 3, it is characterized in that, described step (2) is specially: mixture 25～250 grams of getting containing hydrogen silicone oil or containing hydrogen silicone oil and hydroxy silicon oil, be added dropwise to stannous octoate or dibutyl tin laurate 0.01～1 gram, thorough mixing is even in 1～10 minute, this mixture is added in the described dispersion liquid, stir static at ambient temperature then depositing more than 24 hours.
5. the preparation method of micropowder of organic silicone according to claim 1, it is characterized in that, described step (3) is specially: the described static dispersion liquid of depositing is stirred with high-shear emulsion machine, the particle of a small amount of reunion is spread out, filter, wash, remove remaining catalyzer and tensio-active agent, under 70～90 ℃ of temperature, be dried to micropowder of organic silicone.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100496277A CN1328321C (en) | 2005-04-22 | 2005-04-22 | Method for preparing micropowder of organic silicone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100496277A CN1328321C (en) | 2005-04-22 | 2005-04-22 | Method for preparing micropowder of organic silicone |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1687237A CN1687237A (en) | 2005-10-26 |
| CN1328321C true CN1328321C (en) | 2007-07-25 |
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ID=35305279
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100496277A Expired - Fee Related CN1328321C (en) | 2005-04-22 | 2005-04-22 | Method for preparing micropowder of organic silicone |
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| CN (1) | CN1328321C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011121752A1 (en) * | 2010-03-31 | 2011-10-06 | 竹本油脂株式会社 | Light-diffusing resin composition and light-diffusing molded body |
| CN103524822B (en) * | 2013-06-21 | 2015-10-21 | 杭州师范大学 | A kind of foaming silicone master batch and preparation method thereof and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62232448A (en) * | 1986-04-03 | 1987-10-12 | Mitsubishi Petrochem Co Ltd | Propylene copolymer film |
| JP2004189699A (en) * | 2002-12-13 | 2004-07-08 | Kao Corp | Powder cosmetic |
| CN1668701A (en) * | 2002-06-18 | 2005-09-14 | 罗狄亚化学公司 | Polyaddition-crosslinkable silicone composition useful as an antifriction varnish for making composite materials includes polyamide and silica powders |
-
2005
- 2005-04-22 CN CNB2005100496277A patent/CN1328321C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62232448A (en) * | 1986-04-03 | 1987-10-12 | Mitsubishi Petrochem Co Ltd | Propylene copolymer film |
| CN1668701A (en) * | 2002-06-18 | 2005-09-14 | 罗狄亚化学公司 | Polyaddition-crosslinkable silicone composition useful as an antifriction varnish for making composite materials includes polyamide and silica powders |
| JP2004189699A (en) * | 2002-12-13 | 2004-07-08 | Kao Corp | Powder cosmetic |
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| Publication number | Publication date |
|---|---|
| CN1687237A (en) | 2005-10-26 |
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| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Ningbo Kwung's Gift Co., Ltd. Assignor: Zhejiang University Contract fulfillment period: 2008.7.30 to 2013.7.30 contract change Contract record no.: 2008330001277 Denomination of invention: Method for preparing micropowder of organic silicone Granted publication date: 20070725 License type: Exclusive license Record date: 20081022 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2008.7.30 TO 2013.7.30; CHANGE OF CONTRACT Name of requester: NINGBO KUANGSHIZHIYUAN CRAFT DESIGN CO., LTD. Effective date: 20081022 |
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Granted publication date: 20070725 |