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Preparation method of methyl ketone oxime methoxy silane

A technology of methylketoximomethoxysilane and methyltrichlorosilane, which is applied in the field of silane crosslinking agent synthesis, can solve the problem that the technical inspiration of methylketoximomethoxysilane is not given and the conversion rate is not high , high color of the product and other problems, to achieve the effect of good cost advantage, good cohesiveness and high yield

Active Publication Date: 2013-12-25
ZHEJIANG QUZHOU GUIBAO CHEM
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  • Abstract
  • Description
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Problems solved by technology

The patent does not give any technical inspiration on how to prepare methylketoximomethoxysilane
In addition, the reaction of methyltrimethoxysilane and 2-butanone oxime to prepare methylketoximomethoxysilane has the disadvantages of slow reaction, difficult handling of by-product methanol, low conversion rate, and high chroma of the obtained product.

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  • Preparation method of methyl ketone oxime methoxy silane
  • Preparation method of methyl ketone oxime methoxy silane
  • Preparation method of methyl ketone oxime methoxy silane

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preparation example Construction

[0024] A kind of preparation method of methyl ketoximino methoxy silane, technological process is as figure 1 Shown, preparation method step is as follows:

[0025] (1) Add butanone oxime, methanol and No. 120 solvent oil into a stirred reactor, then drop methyltrichlorosilane into the reactor, adjust the drop rate of methyltrichlorosilane, and control the reaction temperature at 30-60°C; the molar ratio of methyltrichlorosilane: butanone oxime: methanol is 1: (5-5.5): 1, and the amount of No. 120 solvent oil is 1-2 times the weight of methyltrichlorosilane.

[0026] (2) After the dropwise addition, let it stand for stratification, and the upper product enters the first neutralization tank, and passes through ammonia gas for neutralization (the temperature of the first neutralization tank is controlled at 70-80°C during the period), and after the pH is greater than 7 Stop, then filter, after ammonium chloride is separated, the semi-finished product of methyl ketoxime methoxys...

Embodiment 1

[0030] In a 3000L reactor with stirring and circulating water cooling, put 1168kg of butanone oxime, 85.6kg of methanol, and 400kg of 120# solvent oil into it. While stirring, add 400kg of methyltrichlorosilane dropwise, adjust the rate of addition, and control The reaction temperature was 30°C. After the dropwise addition was completed, the temperature was kept at 30°C and the reaction was continued for 2 hours. Then let it sit and layer. The upper layer is a mixture of product and solvent oil, which enters the first neutralization tank, and then enters ammonia gas for neutralization. The neutralization temperature is 70°C. Stop when the pH is greater than 7, and then filter. After separating ammonium chloride, it enters the first membrane The evaporator distills off the solvent under the conditions of 100°C and vacuum degree of -0.098Mpa to obtain the methylketoximomethoxysilane product. The lower layer is butanone oxime hydrochloride, enter the second neutralization tank, ...

Embodiment 2

[0033] In a 3000L reactor with stirring and circulating water cooling, put 1238kg of butanone oxime, 85.6kg of methanol, and 400kg of 120# solvent oil into it. While stirring, add 400kg of methyltrichlorosilane dropwise to adjust the rate of addition. The reaction temperature was 40°C. After the dropwise addition was completed, the temperature was kept at 40°C and the reaction was continued for 2 hours. Then let it sit and layer. The upper layer is a mixture of product and solvent oil, which enters the first neutralization tank, and then enters ammonia gas for neutralization. The neutralization temperature is 75°C. Stop when the pH is greater than 7, and then filter. After ammonium chloride is separated, it enters the first membrane. Evaporator, under the conditions of 110°C and vacuum degree of -0.098Mpa, the solvent is distilled off to obtain the methyl ketoximomethoxysilane product. The lower layer is butanone oxime hydrochloride, enter the second neutralization tank, add ...

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Abstract

The invention discloses a preparation method of methyl ketone oxime methoxy silane. The method comprises the following steps: (1), adding butanone oxime, methanol and miscella No. 120 into a reaction kettle with a stirring function, then dripping methyl trichlorosilane into the reaction kettle, adjusting dripping speed of the methyl trichlorosilane, and controlling the reaction temperature between 30 DEG C and 60 DEG C; (2), after the dripping is completed, performing still standing for layering, adding an upper-layer product into a first neutralization kettle, pumping ammonia gas for neutralization, then filtering, separating ammonium chloride, and distilling out miscella to obtain a product; adding a lower-layer product into a second neutralization kettle, adding the miscella, pumping ammonia gas for neutralization, then filtering, separating ammonium chloride, and distilling out the No. 120 miscella to obtain the butanone oxime. The method provided by the invention is simple, feasible, suitable for industrial production, high in product yield and low in manufacturing cost; the prepared product has excellent activation, can be used for preparing RTV silicone rubber which meets fast surface dry requirements, and has low possibility of discoloration during storage.

Description

technical field [0001] The invention relates to the field of synthesis of silane crosslinking agents, in particular to a preparation method of methylketoximomethoxysilane. Background technique [0002] Preparation of room temperature curing silicone rubber The traditional crosslinking agent uses methyl tributyl ketoxime silane and vinyl tributyl ketoxime silane. Methyl tributylketoxime silane has low activity, and the prepared RTV silicone rubber has the disadvantages of slow surface drying and easy cracking. The above-mentioned disadvantages of methyl tributanone silane can be avoided by using vinyl tributyl ketoxime silane, but its price is high, resulting in an increase in cost, and vinyl tributyl ketoxime silane is very easy to turn yellow during storage. It will be affected when preparing transparent RTV silicone rubber. [0003] The invention of CN 102093721 A discloses a crosslinking agent for room temperature vulcanized silicone rubber. In the absence of a catalys...

Claims

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Application Information

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IPC IPC(8): C07F7/18C07F7/10C08L83/04C08K5/5419C08K5/5465
Inventor 李冲合王继良洪璞王伟洪根王燕锋
Owner ZHEJIANG QUZHOU GUIBAO CHEM
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