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A kind of preparation method of 3-isocyanatopropyl triethoxysilane

A technology of ester group propyltriethoxysilane and chloropropyl triethoxysilane, which is applied in the field of fine chemical synthesis, can solve the problems of large operation coefficient, unsafety, and low yield, and achieve simple process, The effect of simple equipment and simple operation

Active Publication Date: 2022-05-24
ZHEJIANG HUANGMA TECH +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] Aiming at the shortcomings of unsafe factors, low yield and large operating coefficient in the existing synthetic method of 3-isocyanatopropyltriethoxysilane

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1-6

[0031] Embodiment 1-6 (the influence of different solvent on synthesis effect)

[0032] Based on the presence of a large amount of salt in the reaction system, the viscosity of the system increases; the reaction is a nucleophilic reaction, and polar solvents need to be added. Traditionally, polar solvents such as N,N-dimethylformamide (DMF) and N-methylpyrrolidone (NMP) are used. It is a natural solvent, but its solubility for inorganic salts is weak. Therefore, a solvent with better solubility such as ionic liquid is used. Such as ionic liquid N-methyl-N-propylpyrrolidine cyanate, ionic liquid N,N'-dialkylimidazolium cyanate, ionic liquid quaternary ammonium cyanate, ionic liquid quaternary ammonium chloride, ionic liquid N -Methyl-N-propylpyrrolidine chloride and ionic liquid N,N'-dialkylimidazolium cyanate.

[0033] The concrete steps of embodiment 1-6 preparing 3-isocyanatopropyl triethoxysilane are as follows: mechanical stirring and temperature device are installed in ...

Embodiment 7-11

[0037] Embodiment 7-11 (the influence of different ratio of solvent on synthesis effect)

[0038] Embodiment 7-11 The concrete steps of preparing 3-isocyanatopropyl triethoxysilane are as follows: mechanical stirring and temperature device are installed in a 3L reaction flask, 162.2g (2mol) potassium cyanate is dissolved in a certain amount of ions Liquid N-methyl-N propyl pyrrolidine cyanate, then add 9.65g catalyst, pass N 2 System replacement was performed, 481.6 g (2 mol) of chloropropyltriethoxysilane was added dropwise, stirring was started, and stirring was performed while adding dropwise. The reaction temperature was controlled at 100 °C, and the reaction was maintained for 11 h. The reacted liquid was transferred to a rectifying tower, and rectified under reduced pressure at a temperature of 170° C., and the collected fractions were analyzed by gas chromatography, and Table 2 was obtained.

[0039] Table 2

[0040]

[0041]

Embodiment 12-15

[0042] Embodiment 12-15 (the influence of different catalyst types on synthesis effect)

[0043] The specific steps for preparing 3-isocyanatopropyltriethoxysilane in Example 12-15 are as follows: a 3L reaction flask is equipped with a mechanical stirring and a temperature device, 162.2g (2mol) potassium cyanate and 1300g ionic liquid N- Methyl-N propyl pyrrolidine cyanate, then add 9.65g catalyst, pass N 2 System replacement was performed, 481.6 g (2 mol) of chloropropyltriethoxysilane was added dropwise, stirring was started, and stirring was performed while adding dropwise. The reaction temperature was controlled at 100 °C, and the reaction was maintained for 11 h. The reacted liquid was transferred to a rectifying tower, and rectified under reduced pressure at a temperature of 170° C., and the collected fractions were analyzed by gas chromatography, and Table 3 was obtained.

[0044] table 3

[0045]

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Abstract

The invention relates to a preparation method of 3-isocyanatopropyl triethoxysilane, which belongs to the field of fine chemical synthesis. A kind of preparation method of 3-isocyanatopropyl triethoxysilane of the present invention comprises the following steps: take chloropropyl triethoxysilane and potassium cyanate as reaction raw materials, use ionic liquid as solvent, under catalysis , One-step synthesis of 3‑isocyanatopropyltriethoxysilane. The present invention selects the isocyanate method, and its reaction raw materials are difficult to dissolve, and the yield is low, and proposes a method for preparing 3-isocyanatopropyl triethoxysilane based on ionic liquid.

Description

technical field [0001] The invention relates to a preparation method of 3-isocyanatopropyltriethoxysilane, which belongs to the field of fine chemical synthesis. Background technique [0002] 3-Isocyanatopropyltriethoxysilane is a silane coupling agent containing reactive groups of isocyanate groups, and its function is to promote the bonding properties between inorganic materials and organic materials. It is widely used in high-grade polyurethane sealant and modified polyurethane resin, and can also be used as a tackifier for room temperature vulcanized silicone rubber, a component of varnish resin, etc. [0003] Common preparation methods of isocyanatosilanes mainly include the following: [0004] Phosgene method: [0005] Patent CN104203910 describes the use of phosgene and amine to react in an inert solvent to prepare isocyanate compounds. The disadvantage of this method is that phosgene is a colorless and odorless highly toxic gas, and phosgene is easily leaked in the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18
CPCC07F7/1804C07F7/1892Y02P20/54
Inventor 张玉桥余江金一丰余渊荣叶达峰
Owner ZHEJIANG HUANGMA TECH