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A kind of synthetic method of trimethyl boron

A technology of trimethyl boron and synthesis method, which is applied in the field of organic chemical synthesis, can solve the problems of complex synthesis process steps, high cost, and low yield, and achieve the goal of improving light energy conversion rate, low production cost, and reducing production cost Effect

Active Publication Date: 2019-07-30
TAIHE GAS JINGZHOU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims to solve the problems of complex synthesis process steps, high cost and low yield in the prior art, and provides a new synthesis method of trimethyl boron

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A kind of synthetic method of trimethyl boron, the steps are as follows:

[0027] Under the protective condition of dry helium, add 0.01mol of p-chlorobenzonitrile and 1mol of boric acid to the reaction kettle in sequence, vacuumize until the pressure is -0.04Mpa, and keep the temperature of the reaction kettle at -60~-50℃ and feed 3mol of methyl chloride , After the addition of methyl chloride was completed, the reaction was incubated at -40 to -30°C for 1 h.

[0028] Pass the reaction kettle gas through an adsorption column equipped with an adsorbent, keep the temperature of the adsorption column at -15 to -10°C, and collect it with a cooled collection tank to obtain trimethyl boron with a purity of 99.99%.

[0029] In this example, the adsorbent is 5A molecular sieve.

Embodiment 2

[0031] A kind of synthetic method of trimethyl boron, the steps are as follows:

[0032] Under the protection of dry helium, add 0.02 mol of p-chlorobenzonitrile and 1 mol of boric acid to the reaction kettle in sequence, vacuumize until the pressure is -0.04Mpa, and keep the temperature of the reaction kettle at -50~-45°C and feed 3.3 mol of methyl chloride , After the addition of methyl chloride was completed, the reaction was incubated at -30 to -25°C for 1 h.

[0033] Pass the reaction kettle gas through an adsorption column equipped with an adsorbent, keep the temperature of the adsorption column at -15 to -10°C, and collect it with a liquid nitrogen-cooled collection tank to obtain trimethyl boron with a purity of 99.99%.

[0034] In this example, the adsorbent is 5A molecular sieve.

Embodiment 3

[0036] A kind of synthetic method of trimethyl boron, the steps are as follows:

[0037] Under the protection of dry helium, add 0.03 mol of m-chlorobenzonitrile and 1 mol of boric acid in turn to the reactor, vacuumize until the pressure is -0.05Mpa, keep the temperature of the reactor at -50~-40°C, and feed 4 mol of methyl chloride, After the addition of methyl chloride was completed, the reaction was kept at -40 to -30°C for 2 hours.

[0038] Pass the reaction kettle gas through an adsorption column equipped with an adsorbent, keep the temperature of the adsorption column at -10-0° C., and collect it with a liquid nitrogen-cooled collection tank to obtain trimethyl boron with a purity of 99.99%.

[0039] In this example, the adsorbent is 5A molecular sieve.

[0040] Example 3

[0041] A kind of synthetic method of trimethyl boron, the steps are as follows:

[0042] Under the protection of dry helium, add 0.03 mol of m-chlorobenzonitrile and 1 mol of boric acid in turn to...

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PUM

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Abstract

The invention discloses a synthesis method of trimethylboron, and belongs to the technical field of organic chemical synthesis. The synthesis method comprises the following steps: A, synthesizing: adding a catalyst and boric acid into a reaction kettle under the protection of inert gas, inflating chloromethane at the pressure of -0.04Mpa to -0.06Mpa and the temperature of -60 DEG C to -40 DEG C, and then reacting for 1-2h at the temperature of -40 DEG C to -20 DEG C; B, adsorbing: passing gas synthesized in the step A through an adsorption column at the adsorption temperature of -15 DEG C to 0DEG C, and then collecting gas left after adsorption of the adsorption column by using a collection tank to obtain the trimethylboron. The synthesis method invention has the advantages of simpleness,high purity and yield of the trimethylboron and low cost.

Description

technical field [0001] The invention relates to a synthesis method of trimethyl boron, which belongs to the technical field of organic chemical synthesis. Background technique [0002] Amorphous silicon solar cells have the characteristics of low manufacturing cost and easy mass production. They have been widely used in recent years and have attracted widespread attention. The quality of P-type window materials has an important impact on the performance of solar cells, and improving the properties of P-type materials is an effective way to improve the performance of solar cells. At present, the production line of amorphous silicon solar cells mainly uses diborane or trimethyl boron as dopant. When diborane is used as a dopant, the mutual restriction between the dark conductivity and the optical band gap of the material is more serious, mainly because there are B-B bonds and B-H bonds in the molecular structure of diborane. During the vapor deposition process, these bonds T...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/02
CPCC07F5/027
Inventor 吴平修汪正宏阳辉曾令军何西平徐诗飞
Owner TAIHE GAS JINGZHOU
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