CN104356159A - Method for preparing silsesquioxane by virtue of hydrolysis of methyl trichlorosilane - Google Patents
Method for preparing silsesquioxane by virtue of hydrolysis of methyl trichlorosilane Download PDFInfo
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- CN104356159A CN104356159A CN201410682816.7A CN201410682816A CN104356159A CN 104356159 A CN104356159 A CN 104356159A CN 201410682816 A CN201410682816 A CN 201410682816A CN 104356159 A CN104356159 A CN 104356159A
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- Prior art keywords
- methyl
- silsesquioxane
- trichloro silane
- water
- methyl trichloro
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Abstract
The invention relates to a preparation of a compound and particularly relates to a method for preparing silsesquioxane by virtue of hydrolysis of methyl trichlorosilane. An organic phase and water form a two-phase solution, according to the characteristics that methyl-CH3 on the methyl trichlorosilane is easily dissolved in an organic solvent while a silicon-chlorine bond is dissolved in water, methyl trichlorosilane forms a reaction layer between a water layer and an organic layer, the hydrolysis of methyl trichlorosilane is mostly carried out on the same layer between the water layer and the organic layer, the generated nCH3SiO3/2 forms a net-shaped microstructure; by controlling the hydrolytic condensation speed, product particles are smaller and the structure of the condensation product is changed so that the reaction for preparing a downstream product methyl sodium silicate is more easily performed. The by-product generated in the method can be recycled, no emission of three wastes is fundamentally caused, a circular economy system is formed and the method has good social, economic and eco-environmental benefits.
Description
Technical field
The present invention relates to the preparation of a kind of compound, be specially the method that silsesquioxane is prepared in METHYL TRICHLORO SILANE hydrolysis.
Background technology
Silsesquioxane, the both at home and abroad main method adopting the directly synthesis under copper catalyst effect of methyl chloride and silica flour.The method is except generating target product (CH
3)
2siCl
2outward, along with generating portion by product: CH
3siCl
3(3 ~ 15%), (CH
3)
3siCl (3%), CH
3hSiCl
2(1 ~ 3%), (CH
3)
2hSiCl (0.5%), (CH
3)
4si (0.1%), SiCl
4high boiling material (1 ~ 6%).Wherein CH
3siCl
3ratio is maximum.At present, CH
3siCl
3do not obtain fully developing causing a large amount of accumulation.Due to CH
3siCl
3facile hydrolysis produces HCl in atmosphere, brings immense pressure to environment.So CH
3siCl
3process not only become with application bottleneck restrict organosilicon industry development, also certainly will become the key of guiding whole piece industrial chain Sustainable development.By CH
3siCl
3catalytic disproportionation is converted into (CH
3)
2siCl
2have many research, but correlation technique is still immature.By CH
3siCl
3though prepare the industrialization of nano-gas-phase white carbon black, Technology is mainly monopolized by external Ji Jia major company.Also there are some to prepare methyl silicon resin, silane coupling agent, prepare sodium methyl silicate (potassium) as water-resisting agent and oil drilling stablizer and the research preparing the aspects such as polymethyl siloxane hydrophober.The exploitation of major part product needs METHYL TRICHLORO SILANE to be converted into solid-state silsesquioxane, and " the utilizing METHYL TRICHLORO SILANE to be hydrolyzed the method preparing methyl siliconic acid and technical hydrochloric acid " of CN 101906111 invention can only obtain larger cotton-shaped poly-methyl siliconic acid (i.e. silsesquioxane) crude product of particle.Adopt monomethyl trichlorosilane directly react with water, the methyl siliconic acid reacting generation carries out from condensation, the CH of formation
3siO
3/2do not have solid form, may be that dimerization, four is gathered, six gather, eight cage structures such as poly-, the situation namely shown in Fig. 1.The hydrolysis-condensation reaction shown is too violent, bad control.Because cotton-shaped poly-methyl siliconic acid (i.e. silsesquioxane) crude product cage structure is not easily opened, and density is very little, swims in fluid surface be unfavorable for abundant reaction when preparing derived product.
Summary of the invention
For above-mentioned technical problem, the object of this invention is to provide a kind of method preparing ultra-fine silsesquioxane.
Concrete technical scheme is: the method for silsesquioxane is prepared in METHYL TRICHLORO SILANE hydrolysis, is prepared in mass ratio, deionized water: organic solvent: METHYL TRICHLORO SILANE is 2 ~ 2.5: 1 ~ 1.2: 1 ~ 1.2 by following raw material; Machine solvent is decane or dodecane;
Comprise the following steps:
(1) first add deionized water in a kettle., then add organic solvent, control at 25 ~ 40 DEG C, stir and form organic-water two phase liquid;
(2) in reactor, drip METHYL TRICHLORO SILANE, control to dropwise for 30 ~ 50 minutes, dropwise rear continuation reaction 45 minutes;
(3) reaction slurry released and proceed to filter decompress filter, precipitating 2 ~ 3 times with water wash;
(4) throw out proceeds in 100 DEG C of constant temperature drying rooms and dries, and obtains dry silsesquioxane pressed powder.
Preferred version is, deionized water: organic solvent: METHYL TRICHLORO SILANE is that 2: 1: 1 temperature keep 25 DEG C.
The mixing filtrate of suction filtration pumps into reactor recycling, and when in filtrate, aqueous phase hydrogen cloride concentration reaches about 30%, static lower floor's aqueous phase of isolating stores sale as industrial concentrated hydrochloric acid.To add in organic phase mixing by initial proportion as aqueous phase and pump into reactor and recycle after wash filtrate water isolates concentrated hydrochloric acid.
The hydrogen chloride gas that reaction produces is got back to organosilane monomer beginning of production by reactor collected overhead and is prepared methyl chloride, or is separately used as him.
The reaction formula that the method for silsesquioxane is prepared in METHYL TRICHLORO SILANE hydrolysis of the present invention is:
CH
3SiCl
3+3H
2O＝CH
3Si(OH)
3
nCH
3Si(OH)
3→nCH
3SiO
3/2+H
2O
The method of silsesquioxane is prepared in METHYL TRICHLORO SILANE hydrolysis provided by the invention, adopts organic phase and water to form two phase liquid, utilizes the methyl (-CH in METHYL TRICHLORO SILANE
3) be soluble in organic solvent and silicon chlorine key is dissolved in the characteristic of water layer, and similar dissolve mutually theory namely, make METHYL TRICHLORO SILANE between water layer and organic layer, define a responding layer, as shown in Figure 2, the hydrolysis reaction that METHYL TRICHLORO SILANE occurs only carries out at phase interface.The hydrolysis of METHYL TRICHLORO SILANE almost all between water layer and organic layer same layer carry out, so self-condensation reaction is also all mutually carry out by between the methyl siliconic acid being in same layer, so just make the nCH of generation
3siO
3/2form a kind of reticulated microstructure instead of the cage structure as Fig. 1.This not only controls hydrolytic condensation speed, makes product grain less, and changes condensation product structure, and the reaction of preparation derived product sodium methyl silicate etc. is more easily carried out.By product of the present invention all can be recycled, basic three-waste free discharge, forms Recycling Economy System, has good society, economy and ecological environment benefit.
Accompanying drawing explanation
Fig. 1 is the (CH of prior art
3siO
3/2)
ncage structure;
Fig. 2 is the responding layer of METHYL TRICHLORO SILANE hydrolysis.
Embodiment
The specific embodiment of the present invention is described in conjunction with the embodiments.
Embodiment 1
The method of silsesquioxane is prepared in METHYL TRICHLORO SILANE hydrolysis, is prepared in mass ratio, deionized water: organic solvent: METHYL TRICHLORO SILANE is 2.5: 1.2: 1.2 by following raw material;
Comprise the following steps:
(1) first add deionized water in a kettle., then add organic solvent, control at 40 DEG C, stir and form organic-water two phase liquid,
(2) in reactor, drip METHYL TRICHLORO SILANE, control to dropwise for 50 minutes, dropwise rear continuation reaction 45 minutes;
(3) reaction slurry released and proceed to filter decompress filter, precipitating 2 ~ 3 times with water wash;
(4) throw out proceeds in 100 DEG C of constant temperature drying rooms and dries, and obtains dry silsesquioxane pressed powder.
Embodiment 2
The method of silsesquioxane is prepared in METHYL TRICHLORO SILANE hydrolysis, is prepared in mass ratio, deionized water: organic solvent: METHYL TRICHLORO SILANE is 2: 1: 1 machine solvents is dodecane by following raw material;
Comprise the following steps:
(1) first add deionized water in a kettle., then add organic solvent, control at 25 DEG C, stir and form organic-water two phase liquid,
(2) in reactor, drip METHYL TRICHLORO SILANE, control to dropwise for 30 minutes, dropwise rear continuation reaction 45 minutes;
(3) reaction slurry released and proceed to filter decompress filter, precipitating 2 ~ 3 times with water wash;
(4) throw out proceeds in 100 DEG C of constant temperature drying rooms and dries, and obtains dry silsesquioxane pressed powder.
Claims (3)
1. the method for silsesquioxane is prepared in METHYL TRICHLORO SILANE hydrolysis, it is characterized in that: prepared in mass ratio by following raw material, deionized water: organic solvent: METHYL TRICHLORO SILANE is 2 ~ 2.5: 1 ~ 1.2: 1 ~ 1.2;
Preparation method comprises the following steps:
(1) first add deionized water in a kettle., then add organic solvent, control at 25 ~ 40 DEG C, stir and form organic-water two phase liquid;
(2) in reactor, drip METHYL TRICHLORO SILANE, control to dropwise for 30 ~ 50 minutes, dropwise rear continuation reaction 45 minutes;
(3) reaction slurry released and proceed to filter decompress filter, precipitating 2 ~ 3 times with water wash;
(4) throw out proceeds in 100 DEG C of constant temperature drying rooms and dries, and obtains dry silsesquioxane pressed powder.
2. the method for silsesquioxane is prepared in METHYL TRICHLORO SILANE hydrolysis according to claim 1, it is characterized in that: deionized water: organic solvent: METHYL TRICHLORO SILANE is that 2: 1: 1 temperature keep 25 DEG C.
3. the method for silsesquioxane is prepared in METHYL TRICHLORO SILANE hydrolysis according to claim 1 and 2, it is characterized in that: described machine solvent is decane or dodecane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410682816.7A CN104356159A (en) | 2014-11-25 | 2014-11-25 | Method for preparing silsesquioxane by virtue of hydrolysis of methyl trichlorosilane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410682816.7A CN104356159A (en) | 2014-11-25 | 2014-11-25 | Method for preparing silsesquioxane by virtue of hydrolysis of methyl trichlorosilane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104356159A true CN104356159A (en) | 2015-02-18 |
Family
ID=52523490
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410682816.7A Pending CN104356159A (en) | 2014-11-25 | 2014-11-25 | Method for preparing silsesquioxane by virtue of hydrolysis of methyl trichlorosilane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104356159A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109705679A (en) * | 2019-01-10 | 2019-05-03 | 廊坊师范学院 | The preparation process of water nano metallic paint |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3435001A (en) * | 1964-10-01 | 1969-03-25 | Gen Electric | Method for hydrolyzing organochlorosilanes |
| CN101906111A (en) * | 2010-08-12 | 2010-12-08 | 胡竹林 | Method for preparing methyl silicic acid and industrial hydrochloric acid by using hydrolysis of methyl trichlorosilane |
-
2014
- 2014-11-25 CN CN201410682816.7A patent/CN104356159A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3435001A (en) * | 1964-10-01 | 1969-03-25 | Gen Electric | Method for hydrolyzing organochlorosilanes |
| CN101906111A (en) * | 2010-08-12 | 2010-12-08 | 胡竹林 | Method for preparing methyl silicic acid and industrial hydrochloric acid by using hydrolysis of methyl trichlorosilane |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109705679A (en) * | 2019-01-10 | 2019-05-03 | 廊坊师范学院 | The preparation process of water nano metallic paint |
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| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150218 |
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| RJ01 | Rejection of invention patent application after publication |