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A kind of preparation method of boron trichloride tertiary amine complex

A technology of boron trichloride and complexes, which is applied in the field of preparation of boron trichloride tertiary amine complexes, can solve the problems of poor product quality, poor binding force, easy decomposition, etc., and achieve high product yield and high efficiency High, simple and controllable process

Active Publication Date: 2019-10-15
江西瑞合特种材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The common synthetic technique of boron trichloride dimethyloctylamine complex is: the dimethyloctylamine (C 10 h 23 N) is pumped into the reactor, feeds boron trichloride (BCl3) gas at a molar ratio of 1:1, stirs, cools and reacts, and releases the product after the reaction is terminated. Although this process is simple to synthesize, the product quality is relatively poor. The content of tertiary amines in the raw material of octylamine is 97%, and the rest are impurity amines such as primary amines and secondary amines, and the binding force between impurity amines and boron trichloride is poor and easy to decompose, resulting in residual amines and chloride ions in the product. High content, high acidity, moisture and melting point indicators are not ideal, and the color is black, which affects the efficacy of the product. The indicators of this kind of one-time synthesis product are as follows:

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A kind of preparation method of boron trichloride tertiary amine complex, concrete steps are as follows:

[0029] Pump 465kg of dimethyloctylamine (octyl dimethyl tertiary amine) into a 2T enamel reaction kettle, stir and feed in -10°C refrigerated circulating water, and add 350kg of boron trichloride at 55kg / h The speed is passed into the reaction kettle under the liquid surface for exothermic reaction, so as to maintain the temperature in the reaction kettle not exceeding 42°C. After the reaction is completed, a synthetic product is obtained, and then 42°C constant temperature circulating water is introduced into the reaction kettle and fully stirred for 2 hours. To decompose the impurity amine complexes, and at the same time use the water ring vacuum pump to pump the residual and decomposed boron trichloride in the reactor into the sealed lye tank in front of the vacuum pump for absorption; then pump 480kg of methanol into the reactor, stir and dissolve , and then pa...

Embodiment 2

[0032] A kind of preparation method of boron trichloride tertiary amine complex, concrete steps are as follows:

[0033] Pump 465kg of dimethyloctylamine (octyl dimethyl tertiary amine) into a 2T enamel reaction kettle, stir and feed in -10°C refrigerated circulating water, and add 350kg of boron trichloride at 55kg / h The speed is passed into the reaction kettle under the liquid surface for exothermic reaction, so as to maintain the temperature in the reaction kettle not exceeding 42°C, and a synthetic product is obtained at the end of the reaction; then, the constant temperature circulating water of 42°C is passed into the reaction kettle, and it is fully stirred for 2 hours. To decompose the impurity amine complexes, and at the same time use the water ring vacuum pump to pump the residual and decomposed boron trichloride in the reactor into the sealed lye tank in front of the vacuum pump for absorption; then pump 500kg of methanol into the reactor and stir to dissolve , whil...

Embodiment 3

[0036] A kind of preparation method of boron trichloride tertiary amine complex, concrete steps are as follows:

[0037] Pump 465kg of dimethyloctylamine (octyl dimethyl tertiary amine) into a 2T enamel reaction kettle, stir and feed in -10°C refrigerated circulating water, and add 350kg of boron trichloride at 55kg / h The speed is passed into the reaction kettle under the liquid surface for exothermic reaction, so as to maintain the temperature in the reaction kettle not exceeding 42°C. After the reaction is completed, a synthetic product is obtained, and then 42°C constant temperature circulating water is introduced into the reaction kettle and fully stirred for 2 hours. To decompose the impurity amine complexes, and at the same time use the water ring vacuum pump to pump the residual and decomposed boron trichloride in the reactor into the sealed lye tank in front of the vacuum pump for absorption; then pump 450kg of methanol into the reactor and stir to dissolve At the same...

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Abstract

A preparation method of a highly-pure boron trichloride-tertiary amine complex comprises the following steps: pumping dimethyloctylamine into a reaction kettle, introducing excess boron trichloride according to a certain molar ratio while stirring and cooling, carrying out a reaction, carrying out constant temperature stirring after the above synthesis to decompose impurity amine complexes, adopting a methanol solvent to perform dissolving, performing cooling crystallization, spin-drying the obtained material through a centrifuge, and drying the material through adopting a bubbling and pressure reducing distillation technology to obtain a primarily crystallized and purified finished product; carrying out distilling concentration on a primary waste liquid obtained after the centrifugal spin-drying, and carrying out cooling crystallization, centrifuge spin-drying and bubbling and pressure reducing distillation to obtain a secondarily crystallized and purified finished product; and completely recovering the product residual in a secondary waste liquid through adopting a water extraction technology, and recycling the recovered product in the reaction kettle to make the final accumulated yield of the finished product reach 95% or above, wherein the recovered product is the primarily synthesized product. The purity of the prepared finished product reaches 99.5%. The preparation method has the advantages of simple process, high controllable efficiency, complete recycling and no discharging of a distilled and extracted methanol solution, environmental protection, no pollution, andhigh cumulated yield of the finished product.

Description

technical field [0001] The invention relates to the technical field of complex preparation, in particular to a preparation method of a boron trichloride tertiary amine complex. Background technique [0002] Boron trichloride is easy to form coordination covalent bonds with amine compounds with lone electron pairs due to the strong Lewis acid characteristics of its electron-deficient pair, thereby generating complexes, wherein boron trichloride dimethyloctylamine ( Octyl dimethyl tertiary amine) complex is an important organoboron intermediate, and boron trichloride dimethyl octylamine complex is mainly used in the preparation of advanced epoxy resin paints, curing agents and accelerators for coatings. agent. The common synthetic technique of boron trichloride dimethyloctylamine complex is: the dimethyloctylamine (C 10 h 23 N) is pumped into the reactor, feeds boron trichloride (BCl3) gas at a molar ratio of 1:1, stirs, cools and reacts, and releases the product after the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/02
Inventor 蔡杉蔡京陈永智
Owner 江西瑞合特种材料有限公司