Preparation method of 3-isocyanate propyltriethoxysilane

A technology of ester propyl triethoxy silane and chloropropyl triethoxy silane is applied in the field of fine chemical synthesis, can solve the problems of large operating coefficient, unsafe, low yield and the like, and achieves simple process, Simple equipment and simple operation

Active Publication Date: 2019-11-12
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

Method used

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  • Preparation method of 3-isocyanate propyltriethoxysilane
  • Preparation method of 3-isocyanate propyltriethoxysilane
  • Preparation method of 3-isocyanate propyltriethoxysilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-6

[0031] Embodiment 1-6 (the influence of different solvents on synthetic 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 a polar solvent needs to be added. Traditionally, polar solvents such as N,N-dimethylformamide (DMF) and N-methylpyrrolidone (NMP) are used. Sexual 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-propylpyrrolidinium chloride and ionic liquid N,N'-dialkylimidazolium cyanate.

[0033] Embodiment 1-6 prepares the specific steps of 3-isocyanatopropyltriethoxysilane as follows: in the reaction flask of 3L, install mechanical stirring and tempera...

Embodiment 7-11

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

[0038] Embodiment 7-11 prepares the specific steps of 3-isocyanatopropyltriethoxysilane as follows: in the reaction flask of 3L, install mechanical stirring and temperature device, 162.2g (2mol) potassium cyanate dissolves in a certain amount of ion Liquid N-methyl-N-propylpyrrolidine cyanate, then add 9.65g catalyst, pass N 2 System replacement was carried out, and 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 kept for 11 hours. The reacted liquid was transferred to a rectification tower, and rectification under reduced pressure was carried out 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 impact of different catalyst types on synthetic effect)

[0043] Embodiment 12-15 prepares the specific steps of 3-isocyanatopropyltriethoxysilane as follows: in the reaction flask of 3L, install mechanical stirring and temperature device, 162.2g (2mol) potassium cyanate and 1300g ionic liquid N- Methyl-N propylpyrrolidine cyanate, add 9.65g catalyst again, pass N 2 System replacement was carried out, and 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 kept for 11 hours. The reacted liquid was transferred to a rectification tower, and rectification under reduced pressure was carried out 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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PUM

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Abstract

The invention relates to a preparation method of 3-isocyanate propyltriethoxysilane, belonging to the field of fine chemical synthesis. The method comprises synthesizing the 3-isocyanate propyltriethoxysilane from chloropropyltriethoxysilane and potassium cyanate through one-step synthesis in an ionic liquid adopted as a solvent under a catalysis function. An isocyanate process is adopted, and aiming at disadvantages, of the process, that reaction raw materials are difficult to dissolve and yields are low, the preparation method of the 3-isocyanate propyltriethoxysilane based on the ionic liquid is provided.

Description

technical field [0001] The invention relates to a preparation method of 3-isocyanatopropyl triethoxysilane, which belongs to the field of fine chemical synthesis. Background technique [0002] 3-Isocyanatopropyltriethoxysilane is a silane coupling agent containing isocyanate-based active groups, and its function is to promote the bonding performance between inorganic materials and organic materials. It is widely used in high-grade polyurethane sealants and modified polyurethane resins, and can also be used as a tackifier for room temperature vulcanized silicone rubber and a component of varnish resins. [0003] Common preparation methods of isocyanatosilane mainly include the following: [0004] Phosgene method: [0005] Patent CN104203910 describes the preparation of isocyanate compounds by reacting phosgene and amine in an inert solvent. The disadvantage of this method is that phosgene is a colorless, odorless and highly toxic gas. During the production process, phosgene...

Claims

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Application Information

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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
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