Production technology of boron trifluoride complex

A boron trifluoride, production process technology, applied in the chemical industry, can solve the problems of high toxicity, low boiling point, high drying cost, etc., and achieve the effect of low cost, no pollution, and easy control

Active Publication Date: 2011-12-14
RUNTAI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, the production technologies in Japan and the United States all use boron trifluoride to react with acetonitrile liquid, petroleum ether liquid, monoethylamine liquid or ethyl acetate liquid, and dry it with a magnesium drum to obtain a flaky boron trifluoride complex. This reaction has the following disadvantages:

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The production process of boron trifluoride complex includes the following steps:

[0017] a. Gas generation steps:

[0018] Slowly add acetonitrile dropwise to the caustic soda kettle, absorb water to generate acetonitrile vapor, introduce the acetonitrile vapor into the complexing device, and at the same time introduce boron trifluoride gas for complexation reaction, according to the mass ratio of acetonitrile to boron trifluoride gas 1:2 reaction, temperature control between 30°, reaction time 2 hours;

[0019] b. Crystallization steps:

[0020] After the above reaction is completed, stir for 1 hour, centrifuge at 15°C, and collect the centrifuged liquid before applying;

[0021] c. Decompression drying steps:

[0022] The above centrifuged crystals are put into a double cone dryer, the temperature is controlled at 35°, and dried for 3 hours to obtain boron trifluoride acetonitrile.

Embodiment 2

[0024] The production process of boron trifluoride complex includes the following steps:

[0025] a. Gas generation steps:

[0026] Slowly add petroleum ether dropwise to the caustic soda kettle, absorb water to generate petroleum ether vapor, introduce petroleum ether vapor into the complexing device, and at the same time introduce boron trifluoride gas for complexation reaction, press petroleum ether and boron trifluoride gas The mass ratio is 1:2.5 for reaction, the temperature is controlled between 40°, and the reaction time is 3.5 hours;

[0027] b. Crystallization steps:

[0028] After the above reaction is completed, stir for 1.5 hours, the temperature is lowered to 18° and centrifuge, and the centrifuged liquid is collected and applied;

[0029] c. Decompression drying steps:

[0030] The above centrifuged crystals are put into a double cone dryer, the temperature is controlled at 40°, and dried for 5 hours to obtain boron trifluoride petroleum ether.

Embodiment 3

[0032] The production process of boron trifluoride complex includes the following steps:

[0033] a. Gas generation steps:

[0034] Slowly add monoethylamine dropwise to the caustic cauldron, absorb water to generate monoethylamine vapor, introduce monoethylamine vapor into the complexing device, and at the same time introduce boron trifluoride gas for complexation reaction, press monoethylamine and triethylamine The mass ratio of boron fluoride gas is 1:4 for reaction, the temperature is controlled between 50°, and the reaction time is 5 hours;

[0035] b. Crystallization steps:

[0036] After the above reaction is completed, stir for 2 hours, centrifuge at 20°C, and collect the centrifuged liquid before applying;

[0037] c. Decompression drying steps:

[0038] The above centrifuged crystals are put into a double cone dryer, the temperature is controlled at 45°, and dried for 5 hours to obtain boron trifluoride monoethylamine.

[0039] This process adopts an aqueous solution and has a ...

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PUM

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Abstract

The invention relates to a process for producing a boron trifluoride complex. The process comprises the following steps of: a, making gas, namely slowly dripping an organic solvent into a caustic soda flake kettle and absorbing water to generate an organic solvent with vapor, leading the organic solvent with the vapor into a complexing device, leading boron trifluoride gas and performing a complexing reaction, and controlling the temperature to 30 to 50 DEG C and the reaction time to 2 to 5 hours; b, crystallizing, namely after the reaction is finished, stirring for 1 to 2 hours, reducing the temperature to 15 to 20 DEG C, centrifuging, collecting centrifugate and applying; and c, drying under reduced pressure, namely allowing crystals obtained after centrifugation to enter a double cone dryer, controlling the temperature to 35 to 45 DEG C, and drying for 3 to 5 hours to obtain the boron trifluoride complex. The process has the characteristics that: aqueous solution is adopted, the cost is low, liquid caustic soda generated after water is absorbed by using caustic soda flakes can be used for other working sections, and the pollution is avoided; and the reaction temperature is normal temperature or a little higher than the normal temperature and is easy to control, the vacuum drying is adopted, the cost for the application of the centrifugate is low and the like.

Description

Technical field [0001] The invention relates to a production process of a boron trifluoride complex and belongs to the field of chemical industry. Background technique [0002] At present, the production technology in Japan and the United States is to use boron trifluoride and acetonitrile liquid, petroleum ether liquid, monoethylamine liquid or ethyl acetate liquid to react, and use magnesium drum to dry to obtain flake boron trifluoride complex. This reaction has the following shortcomings: for example, boron trifluoride monoethylamine, the reaction needs to use higher purity liquid monoethylamine, monoethylamine is a low boiling point, highly toxic liquid, and the boiling point is only 16.6°. The reaction is exothermic The reaction must be controlled under low temperature conditions, and the product drying cost is high. Therefore, it is necessary to provide a new production process to solve the above-mentioned problems. Summary of the invention [0003] The purpose of the pre...

Claims

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Application Information

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IPC IPC(8): C07F5/02
Inventor 张洪飞陈灵军冯建峰
Owner RUNTAI CHEM CO LTD
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