Preparation method for increasing synthetic yield of 1,1,3-trichloroacetone

A technology of trichloroacetone and acetone, which is applied in the field of preparation to improve the synthesis yield of 1,1,3-trichloroacetone, can solve the problems of poor selectivity, low yield, long reaction cycle, etc., and achieve firm loading and high chemical properties Stable, easy-to-storage effect

Active Publication Date: 2017-01-11
山东聚强绿洲生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Aiming at many technical problems such as long reaction period, poor selectivity and low yield in the existing 1,1,3-trichloroacetone synthesis process, the present invention provides a method for improving the synthesis yield of 1,1,3-trichloroacetone preparation method

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  • Preparation method for increasing synthetic yield of 1,1,3-trichloroacetone

Examples

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Effect test

Embodiment 1

[0025] Example 1: Add 232.0g (4.0mol) of ultra-pure acetone to a 1000mL reaction flask, slowly add 11.6g of loaded polyamine catalysts under stirring, stir evenly and raise the temperature with a water bath, and wait for the reaction flask to When the temperature is stable at 25°C, start to pass chlorine gas into the reaction bottle for chlorination reaction. The speed of chlorine gas flow is 6.0L / h in the first 1~2h of the reaction, and the speed of 2~6h in the middle stage is 30.0L / h. In the later period of 6-20h, the rate of chlorine gas flow is 6.0L / h. After the chlorine reaction is completed, keep the temperature in the reaction bottle constant and continue to stir for 1-2 hours. After the heat preservation reaction, keep the temperature in the reaction bottle constant, add a certain amount of special solvent into the reaction bottle, and keep stirring for 1 hour. After the stirring was completed, the temperature of the obtained mixture was lowered to 10° C. with ice wat...

Embodiment 2

[0026] Example 2: Add 232.0 g (4.0 mol) of ultra-pure acetone to a 1000 mL reaction flask, slowly add 14.0 g of loaded polyamine catalysts under stirring, stir evenly, and raise the temperature with a water bath, and wait for the reaction flask to When the temperature is stable at 30°C, start to pass chlorine gas into the reaction bottle for chlorination reaction. The speed of chlorine gas flow is 6.0L / h in the first 1~2h of the reaction, and the speed of 2~6h in the middle stage is 32.0L / h. In the later period of 6-18h, the rate of chlorine gas flow is 6.0L / h. After the chlorine reaction is completed, keep the temperature in the reaction bottle constant and continue to stir for 1-2 hours. After the heat preservation reaction, keep the temperature in the reaction bottle constant, add a certain amount of special solvent into the reaction bottle, and keep stirring for 1 hour. After the stirring was completed, the temperature of the obtained mixture was lowered to 10° C. with ic...

Embodiment 3

[0027] Example 3: Add 232.0 g (4.0 mol) of ultra-pure acetone to a 1000 mL reaction flask, slowly add 21.0 g of loaded polyamine catalysts under stirring, stir evenly and raise the temperature with a water bath, and wait for the reaction flask to When the temperature is stable at 30°C, start to pass chlorine gas into the reaction bottle for chlorination reaction. The speed of chlorine gas flow is 8.0L / h in the first 1~2h of the reaction, and the speed of chlorine gas flow in 2~6h in the middle stage is 28.0L / h. In the later period of 6-18 hours, the rate of chlorine gas flow is 8.0L / h. After the chlorine reaction is completed, keep the temperature in the reaction bottle constant and continue to stir for 1-2 hours. After the heat preservation reaction, keep the temperature in the reaction bottle constant, add a certain amount of special solvent into the reaction bottle, and keep stirring for 1 hour. After the stirring was completed, the temperature of the obtained mixture was ...

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Abstract

The invention discloses a preparation method for increasing the synthetic yield of 1,1,3-trichloroacetone, and belongs to the technical field of organic synthesis. The method comprises the steps that a load type amine catalyst is prepared, a certain amount of ultra pure acetone is added into a reactor, the load type amine catalyst is slowly added in a stirring state, after the load type amine catalyst and ultra pure acetone are fully mixed to be uniform, temperature is increased, the temperature inside the reactor is controlled to be at 25 DEG C to 30 DGE C, chlorine starts to be introduced into the reactor under the stirring condition, after chlorine introduction is finished, the reaction temperature is controlled to be constant, stirring and thermal reacting continue to be conducted for 2 h, and then 1,1,3-trichloroacetone is obtained. According to the preparation method, the load type amine catalyst is used, the contact area with reactant is increased, the selectivity of 1,1,3-trichloroacetone is improved, and the yield of 1,1,3-trichloroacetone is further increased. According to the load type amine catalyst, load in a covalent bond connection mode is firm, and the catalyst can be recycled multiple times.

Description

[0001] Technical field: [0002] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method for improving the synthesis yield of 1,1,3-trichloroacetone. [0003] Background technique: [0004] 1,1,3-Trichloroacetone is an important intermediate in the production of folic acid. Folic acid is also called vitamin B9. It is a water-soluble vitamin. essential substance. There are many foods containing folic acid, but because the natural folic acid is extremely unstable and easily oxidized by sunlight, temperature and other factors, the human body can not really obtain much folic acid from food; while the synthetic folic acid can remain stable for a long time , is easily absorbed by the body and has a high degree of utilization. [0005] At present, the main method of domestic production of 1,1,3-trichloroacetone is the direct chlorination of acetone. The production process of this method does not need to add catalysts, but ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/63C07C49/16B01J31/02
CPCY02P20/584C07C45/63B01J31/0275C07C49/16
Inventor 张千峰陈向莹马森贾爱铨
Owner 山东聚强绿洲生物科技有限公司
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