Production method of 1,1,3-trichloroacetone

A technology of trichloroacetone and dichloroacetone, applied in chemical instruments and methods, preparation of organic compounds, separation/purification of carbonyl compounds, etc., can solve the problems of high folic acid production cost, complicated process, and low product purity, and achieve Improving product competitiveness, avoiding separation operations, and making the process green and environmentally friendly

Active Publication Date: 2021-10-26
常州新东化工发展有限公司
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  • Abstract
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Problems solved by technology

CN105461529A chlorinated acetone in methanol to first generate 1,3-dichloroacetone dimethyl acetal and then deprotected it, and then obtained 1,1,3-trichloroacetone after chlorination, with a yield of 73.9%, but the process was relatively complicated
CN1047853A prepares 1,1,3-trichloroacetone by catalyzing the reaction of acetone and chlorine with triethylamine and diethylamine, but the reaction needs 10-20 hours and the reaction rate is relatively slow
CN101768066A discloses a method for refining 1,1,3-trichloroacetone, which uses two different solvents in a two-step process to refine trichloroacetone with a purity of about 50% to obtain relatively high-purity 1,1,3- - Trichloroacetone, but large amount of solve...

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  • Production method of 1,1,3-trichloroacetone

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Effect test

Embodiment 1

[0039] (1) Add the solvent chloroform and acetone into a 5L photochlorination circulation reactor in a mass ratio of 1:1.02, control the liquid level in the reactor at 65%, and preheat the material to 44.8°C under stirring ;

[0040] (2) Turn on the 457nm blue-green light source (rated power 50W), turn on the chlorine gas into the equipment, and gradually adjust the flow of chlorine gas to 0-60L / h to generate a reaction liquid, and control the chlorination reaction by adjusting the flow of cooling water The temperature is -10°C;

[0041] (3) In the reaction process, take the reaction solution in the step (2) every 15min to remove the solvent chloroform as the detection solution, and use the gas chromatography area normalization method to analyze the detection solution composition. After the solvent peak is deducted from the detection solution chromatogram The content of 1,1,3-trichloroacetone in the spectrum reaches 34.5%, the chlorine flow is stopped, and the reaction is con...

Embodiment 2

[0046] (1) Add the solvent chloroform and acetone into a 5L photochlorination circulation reactor in a mass ratio of 1:1.98, control the liquid level in the reactor at 70%, and preheat the material to 44.9°C under stirring ;

[0047] (2) Turn on the 403nm purple light source (rated power 50W), turn on the chlorine gas feeding equipment, and gradually adjust the flow rate of chlorine gas to 0-80L / h to generate a reaction liquid, and at the same time control the chlorination reaction at 15.5 by adjusting the cooling water flow rate ℃;

[0048] (3) In the reaction process, take the reaction solution in the step (2) every 15min to remove the solvent chloroform as the detection solution, and use the gas chromatography area normalization method to analyze the detection solution composition. After the solvent peak is deducted from the detection solution chromatogram The content of 1,1,3-trichloroacetone in the spectrum reaches 33.9%, stop the chlorine flow, and continue the reaction...

Embodiment 3

[0053] (1) Add the solvent chloroform and acetone into a 5L photochlorination circulation reactor in a mass ratio of 1:2.99, control the liquid level in the reactor at 80%, and preheat the material to 44.7°C under stirring ;

[0054] (2) Turn on the 354nm purple light source (rated power 50W), turn on the chlorine gas feeding equipment, and gradually adjust the flow rate of chlorine gas to 0-90L / h to generate a reaction liquid, and at the same time control the chlorination reaction at 43.6 by adjusting the cooling water flow rate ℃;

[0055] (3) In the reaction process, take the reaction solution in the step (2) every 15min to remove the solvent chloroform as the detection solution, and use the gas chromatography area normalization method to analyze the detection solution composition. After the solvent peak is deducted from the detection solution chromatogram The content of 1,1,3-trichloroacetone in the spectrum reaches 33.5%, the chlorine flow is stopped, and after the react...

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Abstract

The invention discloses a method for producing 1,1,3-trichloroacetone, belonging to the technical field of chemical product preparation. The method comprises the following steps: with acetone as a raw material, synthesizing 1,1,3-trichloroacetone in an inert solvent through photocatalytic chlorination, recovering a solvent, acetone, monochloroacetone, 1,1-dichloroacetone and other light components from a chlorination solution in a rectification manner, separating the intermediate component 1,3-dichloroacetone from 1,1,3-trichloroacetone in a simulated moving bed filled with an adsorbent to obtain 1,1,3-trichloroacetone, conducting eluting with a desorption agent to obtain a desorption solution containing 1,3-dichloroacetone and 1,1,3-trichloroacetone, distilling the desorption solution to remove the solvent, and then returning the desorption solution to a chlorination kettle for indiscriminate application. The method has the characteristics of mild reaction conditions, high reaction rate, high selectivity of 1,1,3-trichloroacetone, low wastewater discharge amount, environment-friendly process and the like.

Description

technical field [0001] The invention relates to a production method of 1,1,3-trichloroacetone, belonging to the technical field of chemical product preparation. Background technique [0002] 1,1,3-Trichloroacetone is a colorless, transparent liquid with a strong pungent odor. It is mainly used as an important intermediate for the synthesis of folic acid, and is also widely used in medicine, pesticides, spices and dyes. At present, the main methods for preparing 1,1,3-trichloroacetone include acetone direct chlorination method, acetone indirect chlorination method and acetone catalytic chlorination method. [0003] For example, in CN106542979A, acetone is reacted with 2-alkylaniline to form an imine, and then chlorinated to obtain 1,1,3-trichloroacetone with a yield of 80%, but the reaction process needs to use a large amount of sodium hydroxide to adjust the pH, resulting in More salty wastewater. CN105461529A chlorinated acetone in methanol to first generate 1,3-dichloroa...

Claims

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Application Information

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IPC IPC(8): C07C45/63C07C45/82C07C45/79C07C49/16
CPCC07C45/63C07C45/82C07C45/79C07C49/16
Inventor 董亮陶文平王顺利孙运林张驰吴发明马凯
Owner 常州新东化工发展有限公司
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