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Caprolactamyl silane and preparation method thereof

A caprolactam-based silane technology, applied in the field of caprolactam-based silane and its preparation, can solve the problems of poor compatibility, low strength and the like, and achieve the effects of low cost, fast dispersion and good compatibility

Pending Publication Date: 2016-05-04
GBXF SILICONES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the problems of low product strength and poor compatibility in the prior art, the invention provides a caprolactam-based silane and a preparation method thereof, which have the advantages of high resin product strength and good compatibility with polyamide resins

Method used

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  • Caprolactamyl silane and preparation method thereof
  • Caprolactamyl silane and preparation method thereof
  • Caprolactamyl silane and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] In order to maintain the activity of the substance and have good compatibility in polyamide, a caprolactam-based silane has been developed in this program. The caprolactam group in the silane has a good synergistic effect with the structure in polyamide, which is beneficial to The increase in strength of polyamide resins is superior to that of conventional aminosilanes.

[0031] The specific steps of making the required caprolactam-based silane are as follows:

[0032] (1) Add 56 grams of caprolactam, 90 grams of methanol solution of 30% mass fraction sodium methoxide, and 220 grams of benzene in a three-necked flask with a stirring device, stir and heat up, keep warm at 50° C. for 24 hours, and cool to room temperature. After filtering and stirring the reaction, the temperature of the reaction liquid is lowered and cooled, and finally the solid salt is obtained by filtration, and the solid salt is dried to obtain caprolactam sodium salt, which is set aside.

[0033] (...

Embodiment 2

[0043] (1) Add 75 grams of caprolactam, 120 grams of methanol solution of 30% mass fraction sodium methoxide, and 310 grams of benzene in a three-necked flask with a stirring device, stir and heat up, keep warm at 90° C. for 2 hours, and cool to room temperature. After filtering and stirring the reaction, the temperature of the reaction liquid is lowered and cooled, and finally the solid salt is obtained by filtration, and the solid salt is dried to obtain caprolactam sodium salt, which is set aside.

[0044] (2) Put 68 grams of caprolactam sodium salt prepared above into a three-necked flask with a reflux device, chloropropyl silane adopts 115 grams of chloropropyl triethoxysilane, and the phase transfer catalyst is trimethylbenzyl ammonium chloride 1.8 grams, the organic solvent here is 190 grams of N,N-dimethylacetamide, start to stir and heat up, keep the temperature at 150°C for 1 hour, and cool down to room temperature after the reaction;

[0045] (3) filter, can produce...

Embodiment 3

[0048] (1) Add 70 grams of caprolactam, 110 grams of methanol solution of 30% mass fraction sodium methoxide, and 280 grams of benzene in a three-necked flask with a stirring device, stir and heat up, keep warm at 70° C. for 12 hours, and cool to room temperature. After filtering and stirring the reaction, the temperature of the reaction liquid is lowered and cooled, and finally the solid salt is obtained by filtration, and the solid salt is dried to obtain caprolactam sodium salt, which is set aside.

[0049](2) Put 50 grams of caprolactam sodium salt prepared above into a three-necked flask with a reflux device, chloropropyl silane adopts 80 grams of chloropropyl triisopropoxysilane, and the phase transfer catalyst is trioctylmethyl chloride 1.6 grams of ammonium, the organic solvent here is 170 grams of dimethyl sulfoxide, start to stir and heat up, keep warm at 120 ° C for 2 hours, and cool down to room temperature after the reaction;

[0050] (3) filter, can produce by-pr...

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Abstract

The invention discloses caprolactamyl silane and a preparation method thereof. The invention relates to the technical field of organic synthesis. According to the invention, caprolactam, a methanol solution and benzene are added into a three-necked flask with a stirring device; stirring and heating are carried out, and a reaction is allowed; an obtained material is cooled to room temperature; filtering is carried out; after a stirring reaction, solid salt is dried, such that caprolactam sodium salt is obtained; the prepared caprolactam sodium salt, chloropropyl silane, a phase transfer catalyst, and an organic solvent are added into a three-necked flask with a reflux device; stirring and heating are carried out, and a reaction is allowed; the temperature is maintained; after the reaction, the temperature is reduced to room temperature; filtering is carried out, such that a byproduct is removed, and a filtrate is extracted; the filtrate is subjected to reduced-pressure distillation; and the solvent is removed through vacuum heat preservation, such that caprolactamyl silane is obtained. The caprolactamyl silane provided by the invention has good compatibility with polyamide resin. The method has high reaction efficiency. When in use, caprolactamyl silane has good stability. When polyamide resin is combined with polyamide resin, a strength increase is higher than 20%. The cost is low, and strength increase is high.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a caprolactam-based silane and a preparation method thereof. Background technique [0002] Silane is widely used in the microelectronics and optoelectronics industries for the manufacture of solar cells, flat panel displays, glass and steel coatings, and is the only intermediate product of large-scale production of granular high-purity silicon in the world so far. The high-tech applications of silane are still emerging, including the use in the manufacture of advanced ceramics, composite materials, functional materials, biological materials, high-energy materials, etc., and become the basis of many new technologies, new materials, and new devices. [0003] Polyamide is commonly known as nylon (Nylon), and its English name is PolyamideP. It is a general term for polymers containing amide groups in the repeating unit of the macromolecular main chain. Polyamides can be pr...

Claims

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Application Information

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IPC IPC(8): C07F7/18C07F7/10C08K5/544C08L77/00
CPCC07F7/0812C07F7/083C07F7/1804C08K5/544C08L77/00
Inventor 席日勇
Owner GBXF SILICONES CO LTD
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