Preparation method of methyl tris-methylethylketoxime silane

A technology of methyltributanone oxime and butanone oxime is applied in chemical instruments and methods, compounds of elements of Group 4/14 of the periodic table, organic chemistry, etc. Many other problems, to achieve the effect of high purity and low consumption

Active Publication Date: 2011-06-01
湖北新蓝天新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] (1) The reaction is intermittent production, with low efficiency, small output and unstable quality
[0004] (2) The reaction is an intermittent operation, and there are many opportunities to contact air, resulting in hydrolysis of the product, so the product quality is poor
[0005] (3) The finished product dissolved in the lower sediment during the reaction process cannot be recovered, resulting in product waste and low yield
[0006] (4) The production cost is high. It needs

Method used

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  • Preparation method of methyl tris-methylethylketoxime silane
  • Preparation method of methyl tris-methylethylketoxime silane

Examples

Experimental program
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Effect test

Embodiment 1

[0024] First, put 1.8t of butanone oxime and 0.5t of 120# solvent gasoline into the reactor, turn on the stirring, start the circulation pump for full reflux, turn on the A feed pump to inject 1t / h into the reactor, turn on the circulation pump and cool down Keep the temperature at 30°C. After reacting for 30 minutes, turn on the butanone oxime feed pump to inject the butanone oxime into the reactor at a flow rate of 3.6t / h, and turn on the solvent feed pump to inject the solvent at a flow rate of 1t / h. into the reaction kettle, and open the extraction valve of the pump at the same time, keep the circulation flow rate of the pump at 20m3 / h, and the output flow rate at 5.6t / h; The feed flow rate of the bottom solvent is controlled at 0.85m3 / h, and the solvent extracted from the product is pumped back to the reactor for recycling. Butanone oxime is recovered, the ammonium chloride solution in the lower layer is crystallized and dried in a crystallizer to obtain pure ammonium chl...

Embodiment 2

[0026] First, put 1.8t of butanone oxime and 0.5t of 120# solvent gasoline into the reactor, turn on the stirring, start the circulation pump for full reflux, turn on the A feed pump to inject 1t / h into the reactor, turn on the circulation pump and cool down Keep the temperature at 40°C. After 30 minutes of reaction, turn on the butanone oxime feed pump to inject the butanone oxime into the reactor at a flow rate of 3.6t / h, and turn on the solvent feed pump to inject the solvent at a flow rate of 1t / h. into the reaction kettle, and open the extraction valve of the pump at the same time, keep the circulation flow rate of the pump at 30m3 / h, and the output flow rate at 5.6t / h; The feed flow rate of the bottom solvent is controlled at 1.25m3 / h. The solvent extracted from the product is pumped back to the reactor for recycling. After the bottom sediment and solvent of the extraction tower are neutralized by the neutralizer, the crude product of butanone oxime in the upper layer is ...

Embodiment 3

[0028]First, put 1.8t of butanone oxime and 0.5t of 120# solvent gasoline into the reactor, turn on the stirring, start the circulation pump for full reflux, turn on the A feed pump to inject 1t / h into the reactor, turn on the circulation pump and cool down Keep the temperature at 35°C. After reacting for 30 minutes, turn on the butanone oxime feed pump to inject the butanone oxime into the reactor at a flow rate of 3.55t / h, and turn on the solvent feed pump to inject the solvent at a flow rate of 1t / h. into the reaction kettle, and open the extraction valve of the pump at the same time, keep the circulation flow rate of the pump at 30m3 / h, and the extraction flow rate at 5.55t / h; The feed flow rate of the bottom solvent is controlled at 1.0m3 / h, and the solvent extracted from the product is pumped back to the reactor for recycling. After the bottom sediment and solvent of the extraction tower are neutralized by the neutralizer, the crude butanone oxime in the upper layer is re...

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Abstract

The invention discloses a preparation method of methyl tris-methylethylketoxime silane, comprising the following steps of: a, respectively and continuously pumping monomethyl trichlorosilane, diacetylmonoxime and a solvent No. 120 into a kettle type stirring reactor by a feeding pump via a flowmeter, circulating one part of discharged reaction materials to the kettle type reactor, and recovering the other part of discharged reaction materials, precipitating and separating the recovered materials through a two-phase separator for demixing to obtain a solvent, as well as crude products of methyl tris-methylethylketoxime silane, unreacted diacetylmonoxime and a little included diacetylmonoxime hydrochloride in the upper layer, and a diacetylmonoxime hydrochloride precipitate in the lower layer; and b, neutralizing the crude products in the upper layer with ammonia gas in a neutralizer to obtain solid ammonium chloride, filtering, distilling a filtered crude solution through a film evaporator, and circulating the distilled solvent to an extraction tower for use, wherein a finished product of the high-purity methyl tris-methylethylketoxime silane can be obtained at the bottom in the film evaporator. The method can be used for realizing the continuous production of the methyl tris-methylethylketoxime silane and has the advantages of high reaction conversion rate, high product recover rate and no pollution to the environment, wherein the obtained product yield reaches 95% and the content of the methyl tris-methylethylketoxime silane exceeds 97%.

Description

technical field [0001] The invention relates to a preparation method of a silane crosslinking agent, in particular to a preparation method of methyl tributylketoxime silane. Background technique [0002] Methyl tributyl ketoxime silane is mainly used as a crosslinking agent for room temperature vulcanized silicone rubber. The existing preparation method of methyl tributanone oxime silane is: put butanone oxime and solvent into the reaction kettle, slowly add methyl trichlorosilane dropwise through the head tank; layer; the upper layer material is neutralized and the solvent is evaporated to obtain the finished product, and the lower layer material is used to recover butanone oxime. There is following shortcoming in above-mentioned technique: [0003] (1) The reaction is intermittent production with low efficiency, small output and unstable quality. [0004] (2) The reaction is an intermittent operation, and there are many opportunities to contact air, which causes the pro...

Claims

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Application Information

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IPC IPC(8): C07F7/10
Inventor 肖俊平
Owner 湖北新蓝天新材料股份有限公司
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