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Method for continuously synthesizing trichloracetic aldehyde and device thereof

A technology of trichloroacetaldehyde and chlorine gas, which is applied in the direction of oxidative preparation of carbonyl compounds, etc., can solve the problems of increasing the solubility of hydrogen chloride, difficulty in industrialization, and increasing the difficulty of separating catalysts and products, so as to reduce side reactions, increase yield, and reduce The effect of the concentration of hydrochloric acid

Inactive Publication Date: 2012-11-07
XIANGTAN UNIV
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  • Abstract
  • Description
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Problems solved by technology

Adding water at one time increases the solubility of hydrogen chloride in the reaction solution, and also causes the generation of by-products
Chinese patent CN1388108A discloses a method for catalyzing the production of chloral, which uses sulfuric acid and its sodium salt as a catalyst to improve the product yield, but increases the difficulty of separating the catalyst from the product, making it difficult to realize industrialization

Method used

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  • Method for continuously synthesizing trichloracetic aldehyde and device thereof

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Comparison scheme
Effect test

Embodiment 11

[0023]Example 11 mol / h of ethanol is continuously added to the first-stage reactor 5 through the pipeline, and 0.2mol / h of water, 0.2mol / h of water, and 0.5mol / h of water are continuously added into the fourth-stage reactor through the pipeline respectively 8 (packed reactor) upper, middle and lower parts. The chlorine of 0.35mol / h is continuously added to the second stage reactor 6, the chlorine of 0.4mol / h is continuously added to the third stage reactor 7, and the chlorine of 2.75mol / h is continuously added to the fourth stage reactor 8 (packing reaction device). The 2nd stage reactor 6, the tail chlorine of the 3rd stage reactor 7 and the 4th stage reactor 8 (filler reactor) continue to enter the 1st stage reactor 5, the tail gas of the 1st stage reactor 5 is from condenser 4 The input port enters the condenser 4 for condensation, and the condensate returns to the first-stage reactor 5 through the pipeline from the output port of the condenser 4, and the uncondensed tail ...

Embodiment 21

[0024] Example 21 The ethanol of 1mol / h is continuously added to the first-stage reactor 5 by the pipeline, the water of 0.3mol / h, the water of 0.4mol / h, and the water of 0.5mol / h are continuously added to the fourth-stage reactor by the pipeline respectively In the upper, middle and lower parts of 8 (plate reactor), 0.5 mol / h of chlorine gas is continuously added to the second-stage reactor 6, and 1.0 mol / h of chlorine gas is continuously added to the third-stage reactor 7, and 2.5 mol / h of chlorine gas is continuously added to the third-stage reactor 7. Chlorine gas is continuously fed into the fourth-stage reactor 8 (plate reactor). The tail chlorine of the second-stage reactor 6, the third-stage reactor 7 and the fourth-stage reactor 8 continues to enter the first-stage reactor 5 for reaction, and the tail gas of the first-stage reactor 5 enters from the inlet of the condenser 4 After condensing in the condenser 4, the condensate returns to the first-stage reactor 5 throug...

Embodiment 31

[0025] Example 31 mol / h of ethanol is continuously fed into the first-stage reactor 5 through the pipeline, 0.3mol / h of water, 0.1mol / h of water, and 0.9mol / h of water are continuously added into the fourth-stage reactor through the pipeline respectively 8 (plate reactor) upper, middle and lower parts. The chlorine of 0.8mol / h is continuously added to the second stage reactor 6, the chlorine of 1.0mol / h is continuously added to the third stage reactor 7, and the chlorine of 2.7mol / h is continuously added to the fourth stage reactor 8. The tail chlorine of the 2nd stage reactor 6, the 3rd stage reactor 7 and the 4th stage reactor 8 continues to enter the 1st stage reactor 5, and the tail gas of the 1st stage reactor 5 enters from the inlet of condenser 4 The condenser 4 is condensed, and the condensate is returned to the first-stage reactor 5 through the pipeline from the outlet of the condenser 4, and the uncondensed tail gas is discharged through the pipeline to recover hydro...

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Abstract

The invention discloses a method for continuously synthesizing trichloracetic aldehyde and a device thereof. Ethanol and chlorine gas react through countercurrent contact, a reaction vessel consists of three stages of loop reaction vessels and one stage of filling material reaction vessel or a plate type reaction vessel, the mol ratio of the chlorine gas to the ethanol is 3.5 to 4.5 / 1, and the mol ratio of water to the ethanol is 0.6 to 1.5 / 1. The first stage of the reaction vessel has the temperature between 10 and 30 DEG C, the second stage of the reaction vessel has the temperature between50 and 75 DEG C, the third stage of the reaction vessel has the temperature between 80 and 95 DEG C, and the third stage of the reaction vessel has the temperature between 80 and 110 DEG C. The chlorine gas is introduced through the bottom of the second stage, the third stage and the fourth stage of the reaction vessels, tail chlorine of the second stage, the third stage and the fourth stage of the reaction vessels enters the first stage of the reaction vessel after being merged, the ethanol is added from the first stage of the reaction vessel, intermediate products of the reaction sequentially flow into a next stage of the reaction vessel, and the water is respectively added at different heights of the fourth stage of the reaction vessel. The method and the device have the advantages that the reaction yield and the equipment utilization rate are high, and the invention has good industrial application prospects.

Description

technical field [0001] The invention relates to a method and a device for continuously synthesizing chloral. Background technique [0002] Chloral is an important intermediate in the production of pesticides and medicines. Chlorination of ethanol involves the following equation: C 2 h 5 OH+Cl 2 →C 2 h 5 OCl+HCl (1)C 2 h 5 OCl+C 2 h 5 OH→CH 3 CH(OH)OC 2 h 5 +HCl (2)CH 3 CH(OH)OC 2 h 5 +3Cl 2 →CCl 3 CH(OH)OC 2 h 5 +3HCl (3)CCl 3 CH(OH)OC 2 h 5 +H 2 O→CCl 3 CH(OH) 2 +C 2 h 5 The total reaction equation of OH (4) is: C 2 h 5 OH+4Cl 2 +H 2 O→CCl 3 CH(OH) 2 +5HCl (5) The following side reactions have taken place in the chlorination process, and the equation is: CCl 3 CH(OH)OC 2 h 5 +HCl+H 2 O→C 2 h 5 Cl+Cl 3 CCH(OH)(6)C 2 h 5 OH+HCl→C 2 h 5 Cl+H 2 O (7) In addition to the above-mentioned side reactions, there are also a series of side reactions such as chlorination of chloral to generate trichloroacetic acid or carbon tetrachloride. [...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C47/16C07C45/29
Inventor 罗和安艾秋红黄荣辉李诚吴剑刘平乐熊鹰
Owner XIANGTAN UNIV
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