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A kind of preparation method of 1,1,1,2,3-pentachloropropane

The technology of pentachloropropane and tetrachloropropane is applied in the field of preparation of 1,1,1,2,3-pentachloropropane, and can solve the problems of complex reaction and purification system, coking and blackening of reaction solution, corrosion of production system, etc. , to achieve the effect of wide application prospects

Active Publication Date: 2021-10-01
JIANGXI TIANYU CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] In the existing preparation technology, in the presence of anhydrous ferric trichloride Lewis acid catalyst, the dehydrochlorination reaction of polychlorinated hydrocarbons, there are various side reactions such as polymerization and isomerization
Especially when 1,1,1,3-tetrachloropropane is dehydrochlorinated to produce 1,1,3-trichloropropene, due to the existence of 1,1,3-trichloropropene, in the presence of Lewis acid catalyst, it is very easy to Polymerization occurs, so that the entire reaction solution is coked and blackened, and the catalyst is deactivated, so that the yield of the key intermediate 1,1,1,2,3-pentachloropropane in the preparation of 1,1,2,3-tetrachloropropene is changed. Low, resulting in a reduction in the overall yield of 1,1,2,3-tetrachloropropene
[0013] In this field, in order to reduce the generation of polymer and tar, US 8877991 adds water to reduce the formation of high boiling matter, but adding water will cause corrosion of the production system
US 8889927 uses the high boilers generated in the previous step to reduce the formation of high boilers that deactivate the catalyst and complicate the reaction and purification system
US 8889928 discloses adding stabilizers or antioxidants to inhibit the generation of dimers or polymers, but adding stabilizers or antioxidants increases the cost of production and waste disposal

Method used

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  • A kind of preparation method of 1,1,1,2,3-pentachloropropane
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  • A kind of preparation method of 1,1,1,2,3-pentachloropropane

Examples

Experimental program
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Effect test

Embodiment 1

[0054] In this example, 1,1,1,2,3-pentachloropropane is prepared by batch reaction preparation method, and the reaction process is as follows:

[0055] Response one:

[0056] Response two:

[0057] Such as figure 1 Shown, reaction one and reaction two described in the present invention take place successively in the same intermittent reactor, and two-step reaction is carried out in the intermittent reactor with jacket of same 20L, and intermittent reactor is equipped with mechanical stirring , A condenser is installed above the reactor, and the tail gas pipe is connected to the top of the condenser, and the acid tail gas is emptied after being absorbed by liquid alkali with a concentration of 15%.

[0058] The first step reaction: dehydrochlorination of 1,1,1,3-tetrachloropropane to generate 1,1,3-trichloropropene.

[0059] Put 16.8kg of 1,1,1,3-tetrachloropropane, 4.5kg of 1,1,1,2,3-pentachloropropane, 0.021kg of anhydrous ferric chloride into the reactor in turn, star...

Embodiment 2

[0064] In this example, 1,1,1,2,3-pentachloropropane is prepared by batch reaction preparation method, and the reaction process is as follows:

[0065] Response one:

[0066] Response two:

[0067] Such as figure 1 As shown, the two-step reaction is carried out in the same 20L jacketed reactor with mechanical stirring. A condenser is installed on the reactor, and the tail gas pipe is connected to the top of the condenser. The acid tail gas is absorbed by 15% liquid alkali and then emptied. .

[0068] The first step reaction: dehydrochlorination of 1,1,1,3-tetrachloropropane to generate 1,1,3-trichloropropene.

[0069] 11.0kg of 1,1,1,3-tetrachloropropane, 11.0kg of 1,1,1,2,3-pentachloropropane, 0.033kg of anhydrous ferric chloride were put into the reactor in turn, and the stirring was started, and the jacket was passed through Heating with hot water, passing -20°C frozen brine through the condenser, and starting timing when the temperature of the reaction solution ris...

Embodiment 3

[0074] In this example, 1,1,1,2,3-pentachloropropane is prepared by batch reaction preparation method, and the reaction process is as follows:

[0075] Response one:

[0076] Response two:

[0077] A 500mL jacketed flask is equipped with a mechanical stirrer. A condenser is installed on the top of the reactor. The top of the condenser is connected to a tail gas pipe. The acid tail gas is absorbed by 15% liquid alkali and then emptied.

[0078]The first step reaction: dehydrochlorination of 1,1,1,3-tetrachloropropane to generate 1,1,3-trichloropropene. Put 100g of 1,1,1,3-tetrachloropropane, 400g of 1,1,1,2,3-pentachloropropane, 0.05g of anhydrous ferric chloride into the reactor in turn, start stirring, and heat the jacket with hot water , the condenser is fed with -15°C frozen brine, the temperature of the reaction solution is raised to 70°C and the timing is started, and the second batch of ferric chloride 0.18g is added after 2h, and the temperature is continued at 70...

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Abstract

The invention provides a preparation method of 1,1,1,2,3-pentachloropropane, the method uses 1,1,1,3-tetrachloropropane as raw material, 1,1,1,2,3- Pentachloropropane is used as a solvent, and dehydrochlorination reaction is carried out to obtain 1,1,3-trichloropropene, chlorine gas is introduced into the reaction system after the reaction, and chlorination reaction is carried out to obtain 1,1,1,2,3-pentachloropropane , in the present invention, 1,1,1,2,3-pentachloropropane is used as a solvent or diluent, and can be used as a solvent to prevent high boilers such as dimers, oligomers or polymers from being produced in the process of dehydrochlorination The inhibitor can increase the conversion rate of 1,1,1,3-tetrachloropropane and the yield of the final product 1,1,1,2,3-pentachloropropane. The preparation method of the invention can be used in the production mode of batch reaction, and can also be used in the production mode of continuous reaction, is suitable for industrial production, and has wide application prospects.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis and relates to a preparation method of 1,1,1,2,3-pentachloropropane. Background technique [0002] Chlorinated hydrocarbon compounds are often used as raw materials for the preparation of refrigerants, blowing agents, sprays, biopesticides and polymers. 1,1,2,3-Tetrachloropropene is one of the main intermediates for the preparation of the chemical herbicide tricamba, and it is also the main intermediate for the new generation of environmentally friendly refrigerant 2,3,3,3-tetrafluoropropene. The latest process for the preparation of 1,1,2,3-tetrachloropropene is obtained by dehydrochlorination of 1,1,1,2,3-pentachloropropane; the preparation of 1,1,1,2,3-pentachloropropene The main method of chloropropane is: use carbon tetrachloride and ethylene as raw materials to first produce 1,1,1,3-tetrachloropropane, then dehydrochloride to produce 1,1,3-trichloropropene, and then add chlorine ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/04C07C19/01
CPCC07C17/04C07C17/25C07C21/04C07C19/01C07C17/087C07C17/23
Inventor 周忠徐海朋余一鸣彭鹏赵亚玲王喜朝庞怀林岳晓日谢思勉田晓宏
Owner JIANGXI TIANYU CHEM CO LTD
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