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Method for producing boron-amine compound and its special apparatus

A technology of compound, boron amine, which is applied in the field of preparation of boron amine compounds, can solve problems such as complex production process, unfavorable environmental protection, energy loss, etc., and achieve the effect of increasing reaction yield, overcoming the biggest disadvantage, and reducing equipment loss

Active Publication Date: 2007-09-05
DALIAN NETCHEM CHIRAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Both this method and the reaction equipment have great defects: for example, the freezing and liquefaction of gas requires a large amount of cooling capacity, and the rectification process requires a lot of heat, which determines the need to switch between cold and heat during the reaction process, and a large amount of energy is lost
In addition, due to the particularity of the reaction, it is necessary to consider the amount of solvent used. If the amount is small, it will be difficult to stir and the yield will decrease.
If the amount is too large, a large amount of waste liquid will be generated, which is not conducive to environmental protection and will increase the cost
These kinds of problems all show that the conventional reaction method has complex production process, low yield, and the restriction effect of the reaction kettle on this type of reaction in terms of equipment.

Method used

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  • Method for producing boron-amine compound and its special apparatus

Examples

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Comparison scheme
Effect test

Embodiment 1

[0016] As shown in Figure 1, a 200-liter rake dryer is converted into a special equipment for the reaction of boron amine compounds, that is, two air inlets 2 are opened on the body 1, and a return device 3 and a gas outlet on the body are added. 4 connected.

[0017] Using the above-mentioned special equipment, put 38.5kg of dimethylamine and 80kg of sulfolane at -20°C, feed 25kg of boron trichloride under stirring, adjust the ventilation rate, and control the reaction temperature -20°C-80°C. After aeration, keep stirring for half an hour. Heat the system to 90°C to ensure that the system is clear and transparent, and distill off the solvent and the product bis(dimethylamino)boron chloride under a vacuum of -0.095Mpa. The separation yield reached 85.3%, and the reaction kettle residue was released in the form of solvent.

Embodiment 2

[0019] Using the same reaction device as in Example 1, 38.5kg of dimethylamine and 60kg of toluene were put into the mixture at -20°C, and 25kg of boron trichloride was introduced under stirring, the ventilation rate was adjusted, and the reaction temperature was controlled to be less than 80°C. After aeration, keep stirring for half an hour. Heat the system to 90°C, and distill off the solvent toluene and the product bis(dimethylamino)boron chloride under a vacuum of -0.095Mpa. The separation yield reached 70%, and the residue was released in solid form, mostly the hydrochloride of dimethylamine.

Embodiment 3

[0021] Using the same reaction device as Example 1, 38.5kg of dimethylamine was dropped in at -20°C, and 16.68kg of boron trichloride was introduced under stirring, the ventilation rate was adjusted, and the reaction temperature was controlled to be less than 80°C. After aeration, keep stirring for half an hour. Heat the system to 90°C, and distill the product tris(dimethylamino)boron under vacuum -0.098Mpa, and the separation yield reaches 90%.

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Abstract

A process for preparing boron amide compounds includes such steps as proportionally mixing dimethylamine with solvent, cooling to -20 deg.C,stirring while filling BCl3 at -20-80 deg.C, stirring for 0.5 hr, and vacuum distilling to obtain high-purity product. Its dedicated apparatus is also disclosed.

Description

Technical field: [0001] The present invention relates to the preparation method of boron amine compound, also relates to its reaction equipment. Background technique: [0002] For industrial production, the reaction of gas and gas is quite difficult. The preparation of boron amine compounds such as bis(dimethylamino)boron chloride and tris(dimethylamino)borane is the reaction of gas and gas. The usual way is to first freeze and dissolve the raw material dimethylamine in the solvent, then feed boron trichloride into the reaction kettle under low-temperature stirring, and then rectify to obtain high-purity bis(dimethylamino)boron chloride and tri( Dimethylamino) borane products. Both this method and the reaction equipment have great defects: for example, the freezing and liquefaction of gas requires a large amount of cooling capacity, and the rectification process requires a lot of heat, which determines the need to switch between cold and heat during the reaction process, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/02
Inventor 曹辉远唐义君张学龙毕重辉石作武
Owner DALIAN NETCHEM CHIRAL TECH
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