Preparation method of silane coupling agent with imide cycle structural unit

A monosilane coupling agent and imide ring-containing technology, which is applied in the field of silane coupling agent and preparation, can solve the problems of high cost and expensive desiccant, and achieve the effect of easy product, low cost and high yield

Inactive Publication Date: 2014-03-26
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In detail, add cyclic anhydride and aminosilane into an organic solvent, stir to dissolve, add acetic anhydride and triethylamine, after the reaction is complete, remove the low boiling point components under reduced pressure to obtain the product, in order to prevent the hydrolysis of silane, the reaction produces The water must be removed, usually by adding chemical desiccants, such as: hexamethyldisilazane, trimethylsilyl nitride, but these desiccants are very expensive, and the cost of application is too high (Ben Patel, Niskayuna. Process for preparing unsaturated imidoalkoxysilanes. US 2007101-23728, 2007-05-30)

Method used

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  • Preparation method of silane coupling agent with imide cycle structural unit
  • Preparation method of silane coupling agent with imide cycle structural unit
  • Preparation method of silane coupling agent with imide cycle structural unit

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The method for preparing silane coupling agent with phthalic anhydride, allylamine and triethoxysilane as raw material:

[0020] 1) Preparation of platinum-containing catalyst

[0021] Take 1g of chloroplatinic acid and dissolve it in anhydrous isopropanol, and make it constant in a 50ml volumetric flask, and the molar concentration is 0.0386mol / l.

[0022] 2) Preparation of imidization products

[0023] In a dry 500ml three-necked flask, add 14.8g (0.1mol) phthalic anhydride and 180ml glacial acetic acid, stir and dissolve, add 5.7g (0.1mol) allylamine, react at room temperature for 1h, heat to reflux for 4h, cool to After room temperature, add 170ml of water, heat to boil, cool to room temperature, a white solid precipitates out, filter with suction, wash with water, and recrystallize the solid with chloroform to obtain 17.2g of product with a yield of 92%, m.p.: 69~71 o c.

[0024] 3) Preparation of the final product

[0025] In a dry 250ml three-necked flask, ad...

Embodiment 2

[0027] The method for preparing silane coupling agent with norbornene monoanhydride, allylamine and triethoxysilane as raw material:

[0028] 1) Preparation of platinum-containing catalysts.

[0029] Take 1g of chloroplatinic acid and dissolve it in anhydrous isopropanol, and make it constant in a 50ml volumetric flask, and the molar concentration is 0.0386mol / l.

[0030] 2) Preparation of imidization products.

[0031] In a dry 500ml three-neck flask, add 16.4g (0.1mol) norbornene monoanhydride and 180ml glacial acetic acid, stir and dissolve, add 5.7g (0.1mol) allylamine, react at room temperature for 1h, heat to reflux for 24h, and cool to After room temperature, 170ml of water was added, heated to boiling, cooled to room temperature, a light yellow solid precipitated out, suction filtered, washed with water, and the solid was recrystallized with petroleum ether to obtain 8.1g of the product with a yield of 40%.

[0032] 3) Preparation of the final product.

[0033] In a...

Embodiment 3

[0035] 1) Preparation of platinum-containing catalysts.

[0036] Take 1g of chloroplatinic acid and dissolve it in anhydrous isopropanol, and make it constant in a 50ml volumetric flask, and the molar concentration is 0.0386mol / l.

[0037] 2) Preparation of imidization products.

[0038] In a dry 500ml three-neck flask, add 14.7g (0.05mol) biphenyltetraic dianhydride and 300ml glacial acetic acid, stir and dissolve, add 5.7g (0.1mol) allylamine, react at room temperature for 1h, heat to reflux for 4h, cool After reaching room temperature, 300ml of water was added, heated to boiling, cooled to room temperature, a white solid precipitated out, suction filtered, washed with water, and the solid was recrystallized with chloroform / acetone to obtain 16.7g of the product with a yield of 90%.

[0039] 3) Preparation of the final product.

[0040] In a dry 500ml three-necked flask, add 1.86g (0.005mol) of imidization product and 300ml of benzene, stir and add 0.12ml of platinum-conta...

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PUM

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Abstract

The invention discloses a preparation method of a silane coupling agent with an imide cycle structural unit. The preparation method comprises the following steps: (1) dissolving cyclic anhydride into glacial acetic acid, adding allylamine according to the mole ratio (1:1 or 2:1) of cyclic anhydride to allylamine, refluxing for 2-36h while stirring, adding water, filtering and drying to obtain an imidization product; (2) dissolving the imidization product into benzene or methylbenzene, adding trialkoxysilane with the molar concentration of 0.01-0.05mol/l, reacting at the temperature of 50-90 DEG C for 2-10h, and removing fractions with low boiling points through reduced pressure distillation to obtain the silane coupling agent with the imide cycle structural unit, wherein the trialkoxysilane contains a platinum catalyst, and the mole ratio of trialkoxysilane to the imidization product is 1:1 or 2:1. According to the invention, the silane coupling agent with the imide cycle structural unit is synthesized by taking cyclic anhydride, allylamine and trialkoxysilane as reactants through a two-step method, and an expensive chemical drying agent is not needed to be added in the process, so that the cost is low; moreover, the preparation method is simple in synthesis process and high in yield, and the silane coupling agent with the imide cycle structural unit is easy to purify.

Description

technical field [0001] The invention belongs to the field of silane coupling agent and its preparation. Background technique [0002] As the four major branches of the silicone industry, silane coupling agents are mainly used as tackifiers for surface treatment, inorganic filler-filled plastics, sealants, adhesives and coatings. General silane coupling agent at lower temperature (200 o C) It has good application performance. At high temperature, the silane coupling agent will decompose and lose its application value. As a very important material additive, the silane coupling agent has a great influence on the heat resistance of the entire material. thermal performance. [0003] The imide ring has a planar symmetrical ring structure, and the bond length and bond angle are in the normal state, which makes it have high thermal stability; at the same time, the imide ring has strong polarity, which can be mixed with the material The surface has a certain strength of interactio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 刘峰张余宝李夫
Owner NANCHANG UNIV
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