CN101362777B - Preparation method of hexamethyl disiloxane - Google Patents
Preparation method of hexamethyl disiloxane Download PDFInfo
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- CN101362777B CN101362777B CN2008101562284A CN200810156228A CN101362777B CN 101362777 B CN101362777 B CN 101362777B CN 2008101562284 A CN2008101562284 A CN 2008101562284A CN 200810156228 A CN200810156228 A CN 200810156228A CN 101362777 B CN101362777 B CN 101362777B
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- hexamethyldisiloxane
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- methyl
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Abstract
The invention relates to the field of organic chemistry, in particular to a preparation method for hexamethyldisiloxane, which is characterized in that: non-toxic and harmless carbonate is taken as a solid state reactant, trimethyl chloro silicane is taken as a liquid state reactant and hexamethyldisiloxane is taken as a reaction solvent; and the hexamethyldisiloxane is synthesized by liquid-solid reaction. The preparation method is simple and can react under mild conditions that only require normal temperature and normal pressure; reaction products can be obtained by simple solid-liquid separation.
Description
Technical field
The present invention relates to organic chemistry filed, be specifically related to a kind of preparation method of hexamethyldisiloxane.
Background technology
Hexamethyldisiloxane is mainly used in the production of organic chemical industry and medication chemistry, is used as closure agent, clean-out system, releasing agent etc. in recent years mostly.The main at present producing hydrolysis process that adopts of hexamethyldisiloxane, be about to the tri-methyl-chlorosilane reaction that under acidic conditions, is hydrolyzed, generate hexamethyldisiloxane and dilute hydrochloric acid, this method production efficiency is low, the yield of product is low, of poor quality, simultaneously the acid concentration that produces in the production process is lower and contain a small amount of organic waste water, therefore product separation is relatively more difficult, and environmental pollution is also relatively more serious, thereby has limited further developing of producing.
Summary of the invention
The invention discloses a kind of new preparation method of hexamethyldisiloxane, the present invention is a solid-phase reactant with nontoxic carbonate, with the tri-methyl-chlorosilane is the liquid phase reaction thing, is reaction solvent with the hexamethyldisiloxane, by the synthetic hexamethyldisiloxane of liquid-solid reaction.Preparation method of the present invention is simple, and the reaction conditions gentleness only needs to get final product at normal temperatures and pressures, and reaction product only needs simple solid-liquid separation promptly.In addition, contain a spot of reaction product in the solid, also only need to obtain reclaiming with baking steaming, condensation.Therefore, product yield height of the present invention, product purity are also high.
Be concrete technical scheme of the present invention below:
The preparation method of hexamethyldisiloxane of the present invention is a solvent with the hexamethyldisiloxane, with tri-methyl-chlorosilane and carbonate reaction promptly.Reaction stops the back solid-liquid separation, and liquid portion is a product, and solid-liquid separation is the means that those skilled in the art use always.The present invention is owing to directly make solvent with hexamethyldisiloxane, reaction efficiency height so not only, and do not have other impurity in the liquid reactants, the product purity height.
The ratio of weight and number of tri-methyl-chlorosilane, carbonate, hexamethyldisiloxane three components is preferably 100:48-100:20-200 in the above-mentioned reaction.
The preferred yellow soda ash of carbonate described in the present invention, sodium bicarbonate, salt of wormwood or saleratus etc. can react in independent a kind of participation, also can severally use simultaneously.
Among the preparation method of the present invention, tri-methyl-chlorosilane preferably splashes in the hexamethyldisiloxane of sneaking into carbonate in advance in the dropping mode.Preferred stirring while dripping.
Gas does not produce preferred reaction of the present invention and the pH value is 6.0～8.0 o'clock stopped reaction to having, and at this time reacts completely.
Reaction solution is after solid-liquid separation, and liquid portion is a desired product, and the product purity height is greater than 99%.Also residual a spot of hexamethyldisiloxane in the solid part, this part hexamethyldisiloxane can be steamed by baking, and the gas that steams is through condensation, recovery, and gained hexamethyldisiloxane purity is also very high, greater than 99%.
Technical process is as follows in the suitability for industrialized production:
Dried → condensation → reception → the detection of metering → mixing → dropping → reaction → cooling → centrifuging → force
Preparation method of the present invention compares with the hexamethyldisiloxane producing hydrolysis process, avoided waste water generation, environment is not had any pollution, human body is not had any injury yet, simultaneously the purity of liquid hexamethyldisiloxane reaches top grade product grade in the product, and advantage such as synthesis technique of the present invention has that production capacity is big, technological operation is simple, product yield high (in raw material METHYL TRICHLORO SILANE weight yield greater than 95%), production cost are low.Therefore hexamethyldisiloxane synthetic process of the present invention has the excellent popularization prospect.
Embodiment
Specification raw materials used in the present embodiment is as follows:
The yellow soda ash outward appearance: white powdery crystallization, total alkali content: 〉=99.2%,
Loss on ignition :≤0.80%;
The sodium bicarbonate total alkali content: 〉=99%, pH value (10g/L solution)≤8.6;
Salt of wormwood outward appearance: white powdery crystallization, total alkali content: 〉=99.0%
Saleratus outward appearance: white powdery crystallization, total alkali content: 〉=98%
Hexamethyldisiloxane density (25 ℃) g/cm
3: 0.762-0.770, content: 〉=99.0%, fusing point :-68 ℃,
Boiling point: 100 ℃, viscosity (25 ℃) 0.65mm
2/ s;
Tri-methyl-chlorosilane content: 〉=98.0%, density (25 ℃) g/cm
3: 0.8536,
Boiling point: 57-58 ℃, flash-point :-18 ℃.
Embodiment 1
Starting material
100 parts of tri-methyl-chlorosilane quality proportionings, weight 217g,
50 parts of yellow soda ash quality proportionings, weight 106g,
20 parts of hexamethyldisiloxane quality proportionings, weight 43.4g.
To add reactor through the 43g hexamethyldisiloxane and the 106g yellow soda ash of metering earlier, open and stir, to splash into reactor in the dropping mode through the 217g tri-methyl-chlorosilane of metering simultaneously, temperature of reaction is a normal temperature, changes according to temperature of reaction and adjusts the control rate of addition, has gas and emit in reaction, when after dropwising, continuing to be stirred to no gas and producing, stop to stir test material pH value, the pH value be 6.0～8.0 o'clock for reacting completely stopped reaction; Cooling, centrifuging (solid-liquid separation), 1200 rev/mins of centrifugal rotational speeds, gained liquid is the hexamethyldisiloxane finished product.
Solid heats evaporate to dryness again in flask, 105 ℃ of controlled temperature, and the gas that heating steams reclaims through condenser condenses, stops heating when dripless in the condenser produces, the cooling cooling.The liquid of condensation gained liquid and solid-liquid separation is merged, and getting the product hexamethyldisiloxane is 198.5g, and content is 99.0%, in raw material METHYL TRICHLORO SILANE weight yield 95.74%.
Embodiment 2
Starting material
100 parts of tri-methyl-chlorosilane quality proportionings, weight 217g,
100 parts of salt of wormwood quality proportionings, weight 217g,
200 parts of hexamethyldisiloxane quality proportionings, weight 434g.
1200 rev/mins of centrifuging centrifugal rotational speeds,
150 ℃ of the dry controlled temperature of baking evaporate to dryness.
When producing, to add reactor through the 434g hexamethyldisiloxane and the 217g salt of wormwood of metering earlier, open and stir, to splash into reactor in the dropping mode through the 217g tri-methyl-chlorosilane of metering simultaneously, temperature of reaction is a normal temperature, changes according to temperature of reaction and adjusts the control rate of addition, having gas in reaction emits, when after dropwising, continuing to be stirred to no gas and producing, stop to stir test material pH value, the pH value be 6.0～8.0 o'clock for reacting completely; Stopped reaction, centrifuging then, liquid is qualified hexamethyldisiloxane finished product.
Solid heats evaporate to dryness again in flask, 150 ℃ of temperature are steamed in baking., the gas that heating steams reclaims through condenser condenses, stops heating when dripless in the condenser produces, the cooling cooling.Final solid is a sodium-chlor.The liquid of condensation gained liquid and solid-liquid separation is merged, get product hexamethyldisiloxane 590.8g, content is 99.2%, in raw material METHYL TRICHLORO SILANE weight yield 96.8%.
Embodiment 3
Starting material
100 parts of tri-methyl-chlorosilane quality proportionings, weight 217g,
75 parts of salt of wormwood quality proportionings, weight 162.8g,
100 parts of hexamethyldisiloxane quality proportionings, weight 217g.
1200 rev/mins of centrifuging centrifugal rotational speeds,
150 ℃ of the dry controlled temperature of baking evaporate to dryness.
When producing, to add reactor through the 217g hexamethyldisiloxane and the 162.8g salt of wormwood of metering earlier, open and stir, to splash into reactor in the dropping mode through the 217g tri-methyl-chlorosilane of metering simultaneously, temperature of reaction is a normal temperature, changes according to temperature of reaction and adjusts the control rate of addition, having gas in reaction emits, when after dropwising, continuing to be stirred to no gas and producing, stop to stir test material pH value, the pH value be 6.0～8.0 o'clock for reacting completely; Stopped reaction, centrifuging then, liquid is qualified hexamethyldisiloxane finished product.
Solid heats evaporate to dryness again in flask, 150 ℃ of temperature are steamed in baking.The gas that heating steams reclaims through condenser condenses, stops heating when dripless in the condenser produces, the cooling cooling.Final solid is a sodium-chlor.The liquid of condensation gained liquid and solid-liquid separation is merged, get product hexamethyldisiloxane 374.2g, content is 99.2%, in raw material METHYL TRICHLORO SILANE weight yield 97.0%.
Claims (6)
1. the preparation method of a hexamethyldisiloxane, it is characterized in that: be solvent with the hexamethyldisiloxane, with tri-methyl-chlorosilane and carbonate reaction promptly, wherein the ratio of weight and number of tri-methyl-chlorosilane, carbonate, hexamethyldisiloxane is 100: 48-100: 20-200.
2. the preparation method of claim 1, wherein carbonate is selected from one or more in yellow soda ash, sodium bicarbonate, salt of wormwood, the saleratus.
3. the preparation method of claim 1, it is characterized in that: tri-methyl-chlorosilane splashes in the hexamethyldisiloxane of sneaking into carbonate in advance in the dropping mode.
4. the preparation method of claim 1 is characterized in that reacting and under agitation carries out.
5. the preparation method of claim 1, it is characterized in that when reaction to not having that gas produces and pH value stopped reaction when being 6.0～8.0, solid-liquid separation, liquid portion is a hexamethyldisiloxane.
6. the preparation method of claim 5 is characterized in that getting separating obtained solid part baking and steams, and the gas that steams gets hexamethyldisiloxane through condensation, recovery.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008101562284A CN101362777B (en) | 2008-09-25 | 2008-09-25 | Preparation method of hexamethyl disiloxane |
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| CN2008101562284A CN101362777B (en) | 2008-09-25 | 2008-09-25 | Preparation method of hexamethyl disiloxane |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101935327B (en) * | 2010-07-28 | 2012-10-24 | 杭州师范大学 | Preparation method of disiloxane |
| CN102617625B (en) * | 2012-03-09 | 2015-02-18 | 山东东岳有机硅材料有限公司 | Preparation method for high-quality hexamethyldisiloxane |
| CN102731559A (en) * | 2012-06-11 | 2012-10-17 | 西南科技大学 | Alkyl-substituted disiloxane and preparation method thereof |
| CN102924493A (en) * | 2012-11-05 | 2013-02-13 | 安徽九天硅业有限公司 | Method for preparing hexamethyldisiloxane through separation of organosilicon azeotrope |
| CN103951692B (en) * | 2014-04-30 | 2016-04-06 | 浙江中天氟硅材料有限公司 | A kind of preparation method of high-purity high-quality hexamethyldisiloxane |
| CN114210292A (en) * | 2021-12-08 | 2022-03-22 | 浙江胡涂硅有限公司 | Preparation method and equipment of electronic-grade hexamethyldisilazane |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4675425A (en) * | 1985-03-08 | 1987-06-23 | Wacker Chemie Gmbh | Method for preparing organosilyl carbonates |
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2008
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4675425A (en) * | 1985-03-08 | 1987-06-23 | Wacker Chemie Gmbh | Method for preparing organosilyl carbonates |
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