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Method of preparing trialkoxysilanes isocyanic ester

A technology of trialkoxysilyl isocyanate and trialkoxysilyl propyl isocyanate, which is applied in the field of preparation of trialkoxysilyl isocyanate, can solve the problems of unsafe and reliable, weak operability, etc., and avoid Effect of phosgene, low price, and low production cost

Inactive Publication Date: 2009-07-29
常州胜杰生命科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The biggest disadvantage of this method is that it uses highly toxic phosgene to participate in the reaction, which is not safe and reliable, and the operability is not strong.

Method used

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  • Method of preparing trialkoxysilanes isocyanic ester
  • Method of preparing trialkoxysilanes isocyanic ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The present embodiment is the preparation method of triethoxysilyl propyl isocyanate, specifically comprises the following steps:

[0022] ① Put a 2L reaction device with a stirrer and a thermometer into an ice-salt bath, and control the temperature 3 Dissolve in 600ml of water, then add to the reaction device and stir, and control the temperature at 5°C to 0°C.

[0023] ②Dissolve 25.4g of triphosgene in 400ml of CH 2 Cl 2 in, and then added to the reaction device; 45.12 g of triethoxysilylpropylamine was dissolved in 400 ml of CH 2 Cl 2 Then add it to the reaction device, stir and react for 15 minutes, and control the temperature at -5°C to 10°C.

[0024] ③ Place the reacted solution to separate the phases into aqueous phase and organic phase, and use 100ml of CH for the aqueous phase 2 Cl 2 Extract twice, combine the organic phase obtained after extraction and the organic phase obtained during phase separation, then dry, filter with suction, and remove CH 2 Cl ...

Embodiment 2～ Embodiment 5

[0027] The preparation method of each embodiment is basically the same as that of Example 1, and the specific parameters of each embodiment are shown in Table 1, wherein the finished product obtained in Example 4 is trimethoxysilylpropyl isocyanate, and all the other are triethoxysilylpropyl isocyanate .

[0028] Example 1

Example 2

Example 3

Example 4

Example 5

Reactor volume

2L

5L

20L

2L

500L

Chlorine scavenger

60g

NaHCO 3

160g

NaHCO 3

700g

NaHCO 3

43.1g

NaHCO 3

14kg

NaHCO 3

Water in which chlorine scavenger is dissolved

600ml

2L

7L

600ml

140L

Triphosgene

25.4g

60g

250g

25.4g

5kg

dissolved triphosgene

CH 2 Cl 2

400ml

1000ml

3L

400ml

60L

Trialkoxysilylamine

45.12g

Triethoxy

silyl propyl...

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Abstract

The invention discloses a preparation method of trialkoxy siloyl isocyanate, comprising the following steps: (1) chlorine catching agent is dissolved in water and then is added into a reaction device to be stirred, wherein, the temperature is controlled at -5-0 DEG C; (2) triphosgene and trialkoxysilane amine are respectively dissolved in organic solvent and then respectively added into the reaction device and react by stirring for 10-20min, wherein, the temperature is controlled at -5-10 DEG C; (3) the phase separation is carried out on the reacted solution, the organic solvent is used for extracting water phase for 1-3 times, the drying is carried out after organic phases are annexed, and the organic solvent is extracted, filtered and removed; (4) after the vacuum distillation, the trialkoxy siloyl isocyanate is obtained. The chlorine catching agent used by the invention has the advantages of cheap price and low production cost. The used triphosgene has the advantages of no toxicity, safety and reliability.

Description

technical field [0001] The invention relates to a preparation method of an isocyanate compound, in particular to a preparation method of a trialkoxysilyl isocyanate. Background technique [0002] At present, the preparation method of trialkoxysilyl isocyanate mainly contains following two kinds: [0003] Japanese patent document JP5540592 discloses a high-temperature addition reaction of alkoxy silicon and allyl isocyanate under the catalysis of rhodium trichloride to obtain alkoxy silicon propyl isocyanate. The main problem of this method is the price of catalyst rhodium trichloride Expensive, high cost, and the reaction must be carried out at high temperature, under harsh conditions. [0004] U.S. patent document US4654428 discloses a kind of with alkoxysilyl propyl amine, phosgene and N, N-dimethylaniline reacts in toluene solution to generate trialkoxy silyl propyl isocyanate, after reaction, use stearic acid Wash with calcium acid to adjust the pH to neutral and then ...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 苏衡吴怡祖李海燕吴春明夏雨
Owner 常州胜杰生命科技股份有限公司
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