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Alkoxy silane continuous atomizing, neutralizing and purifying method and alkoxy silane continuous atomizing, neutralizing and purifying system

The technology of alkoxysilane and the alkoxysilane is applied in the field of continuous atomization, neutralization, purification and system of alkoxysilane, and can solve the problem of complicated quantification of neutralizer, high nitrogen content of alkoxysilane and high acid value. question

Active Publication Date: 2014-08-20
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The present invention aims to solve the technical problems of high acid value after synthesizing alkoxysilane by traditional esterification method, tedious quantification of neutralizing agent, excessive addition of neutralizing agent, poor neutralization depth and high nitrogen content in alkoxysilane; and provides alkoxysilane Oxysilane continuous atomization neutralization purification method and system

Method used

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  • Alkoxy silane continuous atomizing, neutralizing and purifying method and alkoxy silane continuous atomizing, neutralizing and purifying system

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specific Embodiment approach 1

[0020] Specific embodiment one: in this embodiment, the alkoxysilane continuous atomization neutralization and purification method is carried out according to the following steps: the acidic alkoxysilane containing HCl is atomized with ammonia gas in the atomization and in the chamber, In the purification tower, it is atomized with high-pressure hydrogen gas (the pressure of hydrogen gas is 0.2-1.0MPa), and then neutralized by an organic base, and then treated with a mixed layer of calcium chloride and strong alkali ion resin, and a layer of corrugated plate structured packing. , then condensed and collected; that is, complete the continuous atomization of alkoxysilane and purification; wherein, the mass ratio of calcium chloride and strong base ion resin in the mixed layer of calcium chloride and strong base ion resin is (1~ 100):1.

specific Embodiment approach 2

[0021] Embodiment 2: This embodiment is different from Embodiment 1: the organic base is ethylenediamine, tetramethylenediamine, decylamine, dodecylamine, hexadecylamine or octadecylamine. Others are the same as in the first embodiment.

[0022] The salt formed after the reaction of this type of organic base and hydrogen chloride will form a precipitate, which will not dissolve into the alkoxysilane and introduce impurities. At the same time, neutralize the heat release and the system assists in raising the temperature, so that the solid organic base reaches the melting point and melts. Under reduced pressure, the alkoxysilane atomized at a lower temperature passes through the viscous solid organic base in gaseous form. , through the gas-liquid neutralization reaction, so that the internal hydrogen chloride is completely neutralized, and the product does not contain excess organic alkali; the second layer of filler layer is CaCl 2Mixed layer with strong base ion resin. There...

specific Embodiment approach 3

[0023] Embodiment 3: This embodiment differs from Embodiment 1 or Embodiment 2 in that: the strong base ion resin is an ion exchange resin with quaternary amino bases. Other steps and parameters are the same as those in Embodiment 1 or Embodiment 2.

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Abstract

The invention discloses an alkoxy silane continuous atomizing, neutralizing and purifying method and an alkoxy silane continuous atomizing, neutralizing and purifying system, which belong to an alkoxy silane neutralizing and purifying method and an alkoxy silane neutralizing and purifying system and solve the technical problems that acid value is high, quantifying of neutralizer is complicated, the neutralizer is easy to be excessively added, neutralizing depth is small after alkoxy silane is synthetized by the conventional esterifying method, nitrogen gas content in the alkoxy silane is high and the like. The alkoxy silane continuous atomizing, neutralizing and purifying method includes: atomizing alkoxy silane containing HCl by ammonia gas first and then by high-pressure hydrogen gas, neutralizing the same by organic alkali before the alkoxy silane is treated through a calcium chloride and strong-alkali ionic resin mixed layer and a structured packing layer of a corrugated plate, and condensing and collecting. An acidic alkoxy silane feeding valve is respectively connected with an acidic alkoxy silane feeding pipe, a high-pressure ammonia gas atomizer feeding valve and an acidic alkoxy silane atomizing nozzle, and the other end of the high-pressure ammonia atomizer feeding valve is communicated with a liquid ammonia gasifying jacket. The content of hydrogen chloride of the alkoxy silane is lower than 10ppm, the content of the nitrogen gas is lower than 10ppm, and product purity can be up to 99%.

Description

technical field [0001] The invention relates to a method and system for neutralizing and purifying alkoxysilane. Background technique [0002] Trialkoxysilane is an important intermediate in the silicone industry, and its general chemical formula is HSi(OR) 3 Scholars in the United States and Germany tend to believe that R is a straight-chain alkyl group containing less than 6 carbon atoms, and Japanese scholars believe that R is generally a straight-chain alkyl group with less than 4 carbon atoms. Among them, trimethoxysilane and triethoxysilane are the most important. They can be used to synthesize a variety of silane coupling agents through hydrosilation reactions, or to prepare high-purity silane gases through disproportionation reactions, and can also be used to prepare organic-inorganic hybrids. materials etc. [0003] Silane and polysilicon materials are ultra-high-purity electronic materials obtained by purifying metal silicon through a series of physical and chemi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/02
Inventor 杨春晖张磊李季
Owner HARBIN INST OF TECH