Preparation method of ethyltriethoxysilane

A technology of ethyltriethoxysilane and triethoxysilane, which is applied in the field of preparation of intermediate ethyltriethoxysilane, can solve the problems of large investment in reaction equipment, large environmental hazards, and high cost of industrial production. Achieve the effect of low price, good effect and saving operation cost

Active Publication Date: 2015-04-22
XINYAQIANG SILICON CHEM JIANGSU
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0010] In order to solve the problems that the highly toxic solvent benzene is used as the reaction medium in the current preparation process of ethyl triethoxysilane, the present invention is harmful to the environment, the investment in reaction equipment is large, and the industrial production cost is high. The present invention proposes an ethyl triethoxysilane The preparation method of triethoxysilane, the present invention does not need to add additional solvent, and process and equipment are simple, and catalyst consumption and cost are reduced, and synthetic yield and selectivity of reaction are improved, make target product ethyl triethoxysilane easy separate

Method used

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  • Preparation method of ethyltriethoxysilane
  • Preparation method of ethyltriethoxysilane

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Add 1597.7 g (9.726 mol) of raw material triethoxysilane, catalyst RuCl 3 ·xH 2 0.0201g (8.514×10 -5 mol), cocatalyst CuCl 0.0064 g (6.465×10 -5 mol);

[0028] (2) After stirring, the temperature of the reaction system was raised to 65-75°C and maintained for 32 minutes, and 0.35MPa ethylene gas was introduced into the synthesis kettle from the gas bottom pipe. After the reaction was initiated, the reaction temperature was maintained at 65-75°C and stirred for reaction;

[0029] (3) When the ethylene inlet valve is closed and the pressure in the synthesis kettle no longer decreases, the reaction is stopped, the materials in the kettle are lowered to room temperature and collected, and the samples are analyzed by gas chromatography GC (HP-5 chromatographic column, column temperature 120°C, vaporization chamber 200°C, sampling chamber 200°C, FID detector), the content of ethyltriethoxysilane is 97.29%, and the content of tetraethoxysilane is 2.52%. Calculate th...

Embodiment 2

[0034] (1) Add 382.4 g (2.328 mol) of raw material triethoxysilane, catalyst RuCl 3 ·xH 2 O 0.0387g (1.639×10 -4 mol), cocatalyst CuCl 0.1475 g (1.490×10 -3 mol);

[0035] (2) Heat up the temperature of the reaction system to 75-80°C with stirring and maintain it for 30 minutes, then feed 0.25MPa ethylene gas into the synthesis kettle from the gas bottom pipe, after the reaction is initiated, keep the reaction temperature at 75-85°C and stir for reaction;

[0036] (3) When the ethylene inlet valve is closed and the pressure in the synthesis kettle no longer decreases, the reaction is stopped, the materials in the kettle are lowered to room temperature and collected, and the samples are analyzed by gas chromatography GC (HP-5 chromatographic column, column temperature 120°C, vaporization chamber 200°C, sampling chamber 200°C, FID detector), the content of ethyltriethoxysilane is 97.63%, and the content of tetraethoxysilane is 2.20%. Calculate the content of ethyltriethoxys...

Embodiment 3

[0039] (1) Add 300.4 g (1.829 mol) of raw material triethoxysilane, catalyst RuCl 3 ·xH 2 O 0.0557g (2.359×10 -4 mol), cocatalyst CuCl 0.1454 g (1.469×10 -3 mol);

[0040] (2) After stirring, raise the temperature of the reaction system to 55-65°C and maintain it for 14 minutes, then pass 0.35MPa ethylene gas into the synthesis kettle from the gas bottom pipe, after the reaction is initiated, keep the reaction temperature at 55-65°C and stir the reaction;

[0041] (3) When the ethylene inlet valve is closed and the pressure in the synthesis kettle no longer decreases, the reaction is stopped, the materials in the kettle are lowered to room temperature and collected, and the samples are analyzed by gas chromatography GC (HP-5 chromatographic column, column temperature 120°C, vaporization chamber 200°C, sampling chamber 200°C, FID detector), the content of ethyltriethoxysilane is 97.83%, and the content of tetraethoxysilane is 1.91%. Calculate the content of ethyltriethoxys...

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Abstract

The invention relates to the field of organic chemistry and discloses a preparation method of ethyltriethoxysilane. The preparation method solves the problem that the existing ethyltriethoxysilane preparation method utilizes a high-toxicity benzene solvent as a reaction medium so that environmental pollution is large; a reaction equipment investment is high; and an industrial production cost is high. The preparation method comprises the following steps that triethoxysilane, a catalyst and a cocatalyst are added into a pressure-resistant reactor, then are heated to a temperature of 15 to 90 DEG C with stirring, and then are added with ethylene; the mixture undergoes a reaction until the pressure in the reactor is not reduced after ethylene feeding is stopped, so that a ethyltriethoxysilane synthesis product is obtained; and the ethyltriethoxysilane synthesis product is separated and purified to form ethyltriethoxysilane. The preparation method does not utilize an additional solvent, adopts simple equipment and processes, utilizes a small amount of a catalyst, reduces a cost, improves a synthesis yield and reaction selectivity, and realizes easy separation of a desired product ethyltriethoxysilane.

Description

technical field [0001] The invention relates to the field of organic chemistry, in particular to a preparation method of ethyltriethoxysilane, an intermediate commonly used in the preparation of resins, crosslinking agents and coupling agents. technical background [0002] Ethyltriethoxysilane is an important organosilicon chemical reagent. It can be used as a crosslinking agent in the preparation of silicone rubber, as a raw material in the preparation of silicone resin, and as a silane coupling agent. In addition, It also has important applications in the preparation of dielectric materials and insulating materials. [0003] At present, ethyltriethoxysilane is mainly prepared by triethoxysilane and ethylene through the hydrosilylation process or the reduction reaction of tetraethoxysilane under high temperature conditions. The chemical reaction equations are as formula (1) and Formula (2). [0004] [0005] [0006] Russian Journal of General Chemistry (2006, 76(2)...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18
Inventor 伍川刘玲董红蒋剑雄彭家建厉嘉云白赢
Owner XINYAQIANG SILICON CHEM JIANGSU
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