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Novel process method for preparing trimethyl borate through continuous reactive distillation

A technology of trimethyl borate and reactive distillation, which is applied in the field of continuous reactive distillation to prepare trimethyl borate, can solve the problems of low primary conversion rate, easy plugging of main equipment, and large loss of boric acid, etc., to reduce overall cost, The effect of saving energy consumption and equipment investment and reducing investment

Active Publication Date: 2014-06-04
TIANJIN PULAI CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] It is not difficult to find that the primary conversion rate of the reaction raw materials in the above method is low; the loss of boric acid is large; It is easy to gamble; the discharge of waste liquid pollutes the environment because it contains saturated boric acid

Method used

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  • Novel process method for preparing trimethyl borate through continuous reactive distillation

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Massage methanol and boric acid with a ratio of 10:1, enter the evaporator after preliminary reaction in the reactor, and enter the reactive distillation tower after evaporation. Water is extracted from the bottom of the distillation tower, and the extracted product from the top of the tower enters the azeotropic distillation tower, and the azeotrope of trimethyl borate and methanol is collected from the top of the azeotropic distillation tower. Trimethyl borate can be obtained after the azeotrope separation of trimethyl ester and methanol, and the specific parameters are as follows:

[0030] ⑴. The top temperature of the reactive distillation tower is 61-63°C, and the bottom temperature is 100-101°C

[0031] ⑵. The reflux ratio of the reactive distillation column is controlled to be 3

[0032] (3) The temperature at the top of the azeotropic distillation tower is 53.5-54.5°C, and the temperature at the bottom of the tower is 64-66°C

[0033] ⑷. The reflux ratio of th...

Embodiment 2

[0036] Massage methanol and boric acid with a ratio of 8:1, enter the evaporator after a preliminary reaction in the reactor, enter the reactive distillation tower after evaporation, and extract trimethyl borate and methanol from the top of the reactive distillation tower. Water is extracted from the bottom of the distillation tower, and the extracted product from the top of the tower enters the azeotropic distillation tower, and the azeotrope of trimethyl borate and methanol is collected from the top of the azeotropic distillation tower. Trimethyl borate can be obtained after the azeotrope separation of trimethyl ester and methanol, and the specific parameters are as follows:

[0037] ⑴. The top temperature of the reactive distillation tower is 61-63°C, and the bottom temperature is 100-101°C

[0038] ⑵. The reflux ratio of the reactive distillation column is controlled at 2

[0039] (3) The temperature at the top of the azeotropic distillation tower is 53.5-54.5°C, and the ...

Embodiment 3

[0043] Massage methanol and boric acid with a ratio of 6:1, enter the evaporator after a preliminary reaction in the reactor, and enter the reactive distillation tower after evaporation. Trimethyl borate and methanol are extracted from the top of the reactive distillation tower, and the reaction essence Water is extracted from the bottom of the distillation tower, and the extracted product from the top of the tower enters the azeotropic distillation tower, and the azeotrope of trimethyl borate and methanol is collected from the top of the azeotropic distillation tower. Trimethyl borate can be obtained after the azeotrope separation of trimethyl ester and methanol, and the specific parameters are as follows:

[0044] ⑴. The top temperature of the reactive distillation tower is 61-63°C, and the bottom temperature is 100-101°C

[0045] ⑵. The reflux ratio of the reactive distillation column is controlled at 2

[0046] (3) The temperature at the top of the azeotropic distillation...

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Abstract

The invention provides a novel process method for preparing trimethyl borate through continuous reactive distillation. The process method comprises the following steps of: (1) continuously feeding methyl alcohol and boric acid into a reaction kettle based on ratio to realize initial reaction; (2) continuously feeding reaction liquid into a rough evaporating kettle to evaporate; transferring methyl alcohol, trimethyl borate and water into a reactive distillation tower in form of mixed gas by a evaporating manner; continuously draining water produced in the reaction of methyl alcohol and trimethyl borate from the bottom of the tower; carrying out reaction for producing trimethyl borate after the water is drained until boric acid is completely reacted, so as to improve the one-time conversion rate of boric acid to be more than 99.5% as well as reduce the mixing ratio of methyl alcohol, wherein the energy consumption in preparation of trimethyl borate is greatly lowered down, all discharges from the bottom of the tower are the water produced in the reaction, and little boric acid and methyl alcohol are left; and (3) transferring trimethyl borate output from the reactive distillation tower by an evaporating manner into an azeotropic distillation tower together with methyl alcohol, lowering down the temperature of absolute methanol at the bottom part of the zeotropic distillation tower and recovering the absolute methanol, recovering azeotrope of trimethyl borate and methyl alcohol from the top of the tower, and then separating the azeotrope to obtain trimethyl borate.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, in particular to a new process for preparing trimethyl borate through continuous reactive distillation. Background technique [0002] Trimethyl borate is mainly used in the synthesis of organic borides and the preparation of high-purity boron, and can also be used as organic solvents, dehydrating agents, plasticizers, catalysts, welding fluxes and flame retardants, and can also be used as polymers stabilizer. [0003] At present, the preparation of advanced borates is mainly carried out by the transesterification method of lower borates and higher alcohols. With the development and application of domestic advanced borates and the rise of high-energy fuels, trimethyl borate as the representative The demand for lower borates will increase sharply, so it is of great significance to develop and research new methods for the preparation of trimethyl borate. [0004] The reactio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/04
CPCY02P20/10
Inventor 徐仁萍孙晓宁刘翠茹赤俊祥
Owner TIANJIN PULAI CHEM TECH
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