A kind of synthetic device and method of bis(trichloromethyl)carbonate

A technology of trichloromethyl group and synthesis device, which is applied in the field of dicarbonate synthesis device, can solve the problems of high environmental pollution pressure, high storage and transportation pressure, increased consumption of sodium hydroxide and water, etc., so as to improve product yield. efficiency and conversion of dimethyl carbonate, reducing storage and environmental pressures, and increasing reaction safety

Active Publication Date: 2020-04-21
SHANDONG DEPU CHEM IND SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the process of this method is backward, the amount of by-product hydrochloric acid is large, and the pressure of environmental pollution is great, which affects the development and growth of the industry, and specifically has the following disadvantages:
[0004] ②In addition to being absorbed by water to become hydrochloric acid, the multi-purpose chlorine gas is absorbed by sodium hydroxide to become sodium hypochlorite, which increases the production of hydrochloric acid and sodium hypochlorite, increases the consumption of sodium hydroxide and water, and increases environmental pollution pressure
[0005] ③Although hydrochloric acid and sodium hypochlorite are the most basic chemicals, the units of use are limited, and the storage and transportation pressure is very high. If the industry does not match, due to the pressure of hydrochloric acid inventory, it may lead to equipment reduction or even shutdown
[0006] ④The reaction time is long, and a reaction cycle takes at least 5 hours, generally 5 to 7 hours, and continuous production cannot be realized
[0007] ⑤ The chlorination reaction adopts fragile glass equipment, and the gasket adopts polytetrafluoroethylene mat, which is easy to leak

Method used

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  • A kind of synthetic device and method of bis(trichloromethyl)carbonate
  • A kind of synthetic device and method of bis(trichloromethyl)carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Embodiment 1 Utilize the synthetic device of above-mentioned two (trichloromethyl) carbonates to synthesize two (trichloromethyl) carbonates

[0036] The steps are as follows (process flow chart as figure 2 shown):

[0037] (1) Water vapor and dimethyl carbonate are passed into dimethyl carbonate vaporizer (solvent 15m 3 ), the dimethyl carbonate is vaporized, and the temperature is controlled at 90-93° C.; the liquid chlorine is passed into the liquid chlorine vaporizer, and the liquid chlorine is gasified into chlorine gas;

[0038] (2) Chlorine and vaporized dimethyl carbonate enter the heat exchanger in a molar ratio of 6:1. After heat exchange, a mixed gas phase is obtained, and the temperature of the mixed gas phase is controlled at 90-93° C.;

[0039] (3) The mixed gas phase is sprayed from the top into a column-and-tube reactor (capacity 6m) that is vertically filled with a solid catalyst (ceramics as a carrier, and the catalyst is a mixture of copper chlorid...

Embodiment 2

[0042] Embodiment 2 Utilize the synthetic device of above-mentioned bis(trichloromethyl)carbonate to synthesize bis(trichloromethyl)carbonate

[0043] Proceed as follows:

[0044] (1) Water vapor and dimethyl carbonate are passed into dimethyl carbonate vaporizer (solvent 15m 3 ), the dimethyl carbonate is vaporized, and the temperature is controlled at 93 to 95° C.; the liquid chlorine is passed into the liquid chlorine vaporizer, and the liquid chlorine is gasified into chlorine gas;

[0045] (2) Chlorine and vaporized dimethyl carbonate enter the heat exchanger in a molar ratio of 6:1, and a mixed gas phase is obtained after heat exchange, and the temperature of the mixed gas phase is controlled at 93 to 95°C;

[0046] (3) The mixed gas phase is sprayed from the top into a column-and-tube reactor (capacity 6m) that is vertically filled with a solid catalyst (ceramics as a carrier, and the catalyst is a mixture of copper chloride and zinc chloride) through a mixed gas phase...

Embodiment 3

[0050] Embodiment 3 Utilize the synthetic device of above-mentioned bis(trichloromethyl)carbonate to synthesize bis(trichloromethyl)carbonate

[0051] Proceed as follows:

[0052] (1) Water vapor and dimethyl carbonate are passed into dimethyl carbonate vaporizer (solvent 15m 3 ), the dimethyl carbonate is vaporized, and the temperature is controlled at 95 to 98° C.; the liquid chlorine is passed into the liquid chlorine vaporizer, and the liquid chlorine is gasified into chlorine gas;

[0053] (2) Chlorine and vaporized dimethyl carbonate enter the heat exchanger in a molar ratio of 6:1, and a mixed gas phase is obtained after heat exchange, and the temperature of the mixed gas phase is controlled at 95-98°C;

[0054] (3) The mixed gas phase is sprayed from the top into a column-and-tube reactor (capacity 6m) that is vertically filled with a solid catalyst (ceramics as a carrier, and the catalyst is a mixture of copper chloride and zinc chloride) through a mixed gas phase di...

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PUM

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Abstract

The invention discloses a device for synthesizing bi(trichloromethyl) carbonic ester. The device comprises a liquid chlorine gasifier, a dimethyl carbonate gasifier, a heat exchanger, a tubular reactor, a gas storage tank, a stirring kettle, a flaker and the like. The invention further discloses a method for synthesizing the bi(trichloromethyl) carbonic ester. The method comprises the following steps: mixing chlorine with gasified dimethyl carbonate in a mole ratio of (5-7):1, performing heat exchange so as to obtain mixed gas phase, feeding the mixed gas phase into the tubular reactor filled with a solid catalyst, keeping reaction temperature to be 90-100 DEG C and the pressure to be 0.1-0.15Mpa, and performing reaction for 5-10 minutes; recycling unreacted chlorine for circulation use; performing flash evaporation, and performing flaking molding, so as to obtain the bi(trichloromethyl) carbonic ester. By adopting the method for synthesizing the bi(trichloromethyl) carbonic ester, the use amount of the chlorine can be reduced, the reaction time can be shortened, the equipment security can be improved, the reaction efficiency is high, continuous reaction can be achieved, the product yield can be greatly increased, and the dimethyl carbonate conversion rate can be greatly increased.

Description

technical field [0001] The invention relates to a synthesis device and method of bis(trichloromethyl)carbonate, which belongs to the technical field of chemical industry. Background technique [0002] The traditional synthetic method of bis(trichloromethyl)carbonate mainly contains two kinds of solvent method and bulk method, because the used solvent of solvent method is the CCL that has destructive effect to ozone layer 4 , has been phased out. Bulk method is exactly dimethyl carbonate / chlorine gas chlorination method, and this method is to be raw material with dimethyl carbonate and chlorine gas, under light, heat or initiator trigger, synthesize bis (trichloromethyl) carbonate by chlorination reaction, This chlorination reaction is carried out in a free radical chain reaction distribution. The whole process of the reaction is divided into three stages of low, medium and high temperature, and the obtained product is almost pure. The process is to add a certain amount of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/96C07C68/06
CPCC07C68/06C07C69/96
Inventor 卢伟张淑娟王安华卢建行刘长峰
Owner SHANDONG DEPU CHEM IND SCI & TECH
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