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Synthesizer for high-purity 3-isocyanate propyltriethoxysilane and synthetic method thereof

An ester propyl triethoxy silane and a synthesis device technology are applied in the field of synthesis devices of high-purity 3-isocyanatopropyl triethoxy silane, and can solve the problem of consuming large vacuum pump oil or mineral oil, raw material residues, etc. problem, to achieve the effect of easy operation and simple process

Pending Publication Date: 2018-03-06
INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The purpose of the present invention is to solve problems such as the residue of raw materials and the consumption of a large amount of vacuum pump oil or mineral oil in the process of synthesizing 3-isocyanatopropyltriethoxysilane with diethyl carbonate two-step method, and provides a A kind of synthetic device and synthetic method of high-purity 3-isocyanatopropyl triethoxysilane

Method used

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  • Synthesizer for high-purity 3-isocyanate propyltriethoxysilane and synthetic method thereof
  • Synthesizer for high-purity 3-isocyanate propyltriethoxysilane and synthetic method thereof
  • Synthesizer for high-purity 3-isocyanate propyltriethoxysilane and synthetic method thereof

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specific Embodiment approach 1

[0036]A kind of synthetic device of high-purity 3-isocyanatopropyl triethoxysilane, the synthetic device of described high-purity 3-isocyanatopropyl triethoxysilane comprises fixed bed reactor 1, described fixed bed Reactor is installed in heating furnace 5, and solid support 18 is housed in the described fixed-bed reactor, and the top of described fixed-bed reactor is provided with feeding port 17, protective gas inlet 16, and described fixed-bed reaction The feed port of the reactor is connected to the metering pump 12 through the pipeline, and the metering pump is connected to the feed box 14 through the pipeline, and the protective gas inlet of the fixed bed reactor is connected to the pressure reducing valve 2 through the pipeline. The pressure reducing valve is connected to the cylinder 3 through a pipeline, and the bottom of the fixed bed reactor is provided with a discharge port 19, and the discharge port is connected to the inlet of the first condenser 6 through a pipe...

specific Embodiment approach 2

[0040] According to the synthetic method of the high-purity 3-isocyanatopropyl triethoxysilane described in specific embodiment one, comprises the steps:

[0041] Step 1. Check the airtightness of the synthesis device of the high-purity 3-isocyanatopropyltriethoxysilane, heat the fixed-bed reactor to 350° C. and keep the temperature for use;

[0042] Step 2. Adjust the pressure reducing valve to pass protective gas into the fixed-bed reactor. After passing the protective gas for 10 minutes, use a metering pump to pass the raw material [3-(triethoxysilyl)propyl] ethyl carbamate into the A fixed-bed reactor for thermal cracking reaction, the reaction time is 2h;

[0043] Step 3, the reacted mixture in step 2 is cooled by the first condenser, and the first condenser is cooled by 80°C hot water, and the cooled mixture enters the gas-liquid separator for separation, and the separated liquid enters the The product receiving tank, the separated gas enters the second condenser, the s...

specific Embodiment approach 3

[0055] According to the synthetic method of the high-purity 3-isocyanatopropyl triethoxysilane described in specific embodiment one, comprises the steps:

[0056] Step 1. Check the airtightness of the synthesis device of the high-purity 3-isocyanatopropyltriethoxysilane, heat the fixed-bed reactor to 370°C and keep the temperature for use;

[0057] Step 2. Adjust the pressure reducing valve to pass protective gas into the fixed-bed reactor. After passing the protective gas for 10 minutes, use a metering pump to pass the raw material [3-(triethoxysilyl)propyl] ethyl carbamate into the A fixed-bed reactor for thermal cracking reaction, the reaction time is 2h;

[0058] Step 3, the reacted mixture in step 2 is cooled by the first condenser, and the first condenser is cooled by 80°C hot water, and the cooled mixture enters the gas-liquid separator for separation, and the separated liquid enters the The product receiving tank, the separated gas enters the second condenser, the sec...

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Abstract

The invention discloses a synthesizer for high-purity 3-isocyanate propyltriethoxysilane and a synthetic method thereof and belongs to the field of chemical synthesis. The synthetic method disclosed by the invention comprises the following steps: heating a fixed bed reactor to 350-400 DEG C, and maintaining the temperature for later use; regulating a reducing valve to introduce protective gases into the fixed bed reactor, introducing a raw material [3-(triethoxysilicyl)propyl]ethyl carbamate by a metering pump within 3-30 minutes introducing after the protective gases, and carrying out a thermal cracking reaction for 2-4 hours; cooling the mixture reacted in the step 2 by a first condenser, cooling the first condenser by adopting hot water at the temperature of 80 DEG C, enabling the cooled mixture to enter a gas-liquid separator to be separated, and enabling the separated liquid to enter a product collection tank by virtue of a cooler. According to the method disclosed by the invention, 97.5g of the high-purity 3-isocyanate propyltriethoxysilane is obtained, the yield is 81.3%, and the gas chromatographic detection purity is 99.19%. The production process is safe, the process is simple, the product is easy to separate, and reactive raw materials are completely converted.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a high-purity 3-isocyanatopropyltriethoxysilane synthesis device and a synthesis method thereof. Background technique [0002] Silane coupling agent is a kind of low molecular organosilicon compound with special structure, its general formula is RSiX 3 , where R represents groups such as amino, mercaptovinyl, epoxy, chloropropyl, cyano and methacryloxy groups, these groups have strong reactivity with different matrix resins, and x represents Groups capable of hydrolysis, such as halogen, alkoxy, acyloxy, etc. [0003] The silane coupling agent is made of trichlorosilane (HSiCl 3 ) and unsaturated olefins with reactive groups are added under the catalysis of platinum acid, followed by alcoholysis. Silane coupling agents can interact with both the hydroxyl groups in inorganic substances and the long molecular chains in organic polymers, coupling two materials with d...

Claims

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Application Information

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IPC IPC(8): C07F7/18
CPCC07F7/1804C07F7/1892
Inventor 徐虹李淑辉李猛吕宏飞白雪峰吴绵园杨杰梅立鑫王艳华刘洋单雯妍
Owner INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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