Method for synthesizing silane coupler

A technology of silane coupling agent and monohalogenated alkane, which is applied in the field of synthesis of organosilicon monomers, can solve problems such as difficult separation, high price, and dangerous operation, and achieve simple separation and purification process, easy operation, and reduced side reactions Effect

Inactive Publication Date: 2006-06-21
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The traditional direct method uses copper as a catalyst, and the disadvantages are that the reaction temperature is high and separation is difficult (the product is a mixture containing multiple substances)
The Grignard reagent method combines magnesium and SiX 4 First add to the solvent, and then add the required organic halide to this solution to complete the reaction. The disadvantage of this method is that it is difficult to react with halocycloalkanes and Grignard reagents, and the product is also a mixture, which is difficult to separate.
In addition, the solvent used in the reaction is tetrahydrofuran, which is very easy to generate highly explosive peroxides after contacting with air, which brings certain dangers to the operation.
The hydrosilation reaction method uses the addition reaction of silicon hydrogen compounds and unsaturated olefins. The advantage of this method is that there are relatively few by-products, but there are many disadvantages, such as HSiCl 3 Strong volatility, high toxicity, harsh requirements on equipment, difficult to operate; the catalyst required for the reaction (H 2 PtCl 6 ·6H 2 O) the price is expensive (186 yuan / g), and the catalytic effect is not ideal

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1: the synthesis of cyclohexyltriethoxysilane

[0027] Tetraethoxysilane, chlorocyclohexane and iodine are dried with anhydrous calcium chloride and set aside; the magnesium powder is soaked with acetone to remove oil stains, poured out the acetone, and then soaked with 1-2% hydrochloric acid for 5- After 10 minutes, filter out the magnesium, wash with ethanol once more, dry quickly, and set aside.

[0028] Add 416 (2mol) tetraethoxysilane, 24g (1.2mol) magnesium and 2g (0.01mol) iodine into a 1000ml three-necked flask, stir (about 100r / min) and heat up under nitrogen protection. When the temperature reached 151±1°C, 118.5 g (1.0 mol) of chlorocyclohexane was added dropwise, and the addition was completed in about 1.5 hours. Subsequently, the reaction was continued at 150±1° C. for 2 h, and then the reaction was terminated. The generated magnesium salt was filtered off, and the filtrate was poured into a distillation flask to evaporate tetraethoxysilane and...

Embodiment 2

[0029] Embodiment 2: the synthesis of cyclohexyltriethoxysilane

[0030] The method pretreatment raw material by the embodiment 1, standby.

[0031] Add 312g (1.5mol) of tetraethoxysilane, 28.8g (1.2mol) of magnesium and 0.2g (0.001mol) of iodine into a 1000ml three-necked flask. Stir (approximately 100r / min) and heat up under nitrogen protection. When the temperature reached 180±1°C, 118.5 g (1.0 mol) of chlorocyclohexane began to be added dropwise, and the addition was completed in about 1.5 hours. Subsequently, the reaction was continued at 120±1° C. for 5 h, and then the reaction was terminated. The generated magnesium salt was filtered off, and the filtrate was poured into a distillation flask to evaporate tetraethoxysilane and iodine to obtain a crude product of cyclohexyltriethoxysilane. Then, the crude product was purified by rectification to obtain a colorless and transparent cyclohexyltriethoxysilane (boiling point: 253°C) with a yield of 97% and a purity of 99.5%...

Embodiment 3

[0032] Embodiment 3: the synthesis of cyclopentyltriethoxysilane

[0033] The method pretreatment raw material by the embodiment 1, standby.

[0034] Add 312g (1.5mol) of tetraethoxysilane, 26.4g (1.1mol) of magnesium and 0.2g (0.001mol) of iodine into a 1000ml three-necked flask. Stir (approximately 100r / min) and heat up under nitrogen protection. When the temperature reached 165±1°C, 105 g (1.0 mol) of chlorocyclopentane was added dropwise, and the addition was completed in about 1.5 hours. , about 1.5h dropwise completed. Subsequently, the reaction was continued at 130±1° C. for 3.5 h, and then the reaction was terminated. The generated magnesium salt was filtered off, and the filtrate was poured into a distillation flask to evaporate tetraethoxysilane and iodine to obtain a crude product of cyclohexyltriethoxysilane. Then, the crude product was purified by rectification to obtain a colorless and transparent cyclohexyltriethoxysilane (boiling point: 230°C) with a yield ...

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Abstract

The invention discloses a method for synthesizing silane coupling agent, comprising: feeding the pretreated tetraalkoxy silane 1.5-2.0 mol, magnesium 1.0-1.2 mol and initiating agent iodine 0.001-0.01 mol in the reactor, stirring and heating up; adding pretreated the first haloalkane 1 mol when the temperature is 150-180 Deg C, then cooling to 120-150 Deg C for continuous reaction for 2-5 hours; filtering the generated magnesium salt, distilling the filtering medium to remove dissolvent and initiating agent iodine; fractionating and purifying the got coarse product and getting the silane coupling agent with purity larger than 99%-alkyltrialkoxy silane; the reaction is carried out under protection of nitrogen. The process is characterized by the no usage of ethers solvant which is inflammable and high toxic, simple process, easy-to-control and operate, 95% of productivity and above 99% of purity. The unreacted raw material distilled out can be recovered for reuse.

Description

technical field [0001] The invention relates to the synthesis technology of organosilicon monomers, in particular to a method for synthesizing silane coupling agents. Background technique [0002] Silane coupling agent has a wide range of applications in the field of material science and technology, especially in polymer-based composite materials. The interfacial properties of composite materials can improve the comprehensive performance of materials. At the same time, it is also an important chemical intermediate, which can be used to synthesize a variety of new organosilicon compounds. The most striking thing is that starting from the trifunctional silane in this type of coupling agent, silsesquioxanes with different structures such as cages and trapezoids can be obtained through appropriate hydrolysis and polycondensation reactions. The obtained silsesquioxane compounds can be used as additives (crosslinking agents, thermal performance modifiers, viscosity regulators), ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 顾媛娟梁国正张增平卢婷利王结良
Owner ZHEJIANG UNIV
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