Production method of 1,1,3-trichloroacetone

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...

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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 solvent and low yield

However, organic amines are often used as catalysts to catalyze chlorination synthesis, and the reaction speed is relatively slow. However, the direct chlorination method of acetone not only takes a long time to react, but also has poor selectivity and difficulty in separation of 1,1,3-trichloroacetone, resulting in low product purity.

In actual production, 1,1,3-trichloroacetone is extracted and purified by water and organic solvents, and the process produces more waste water. Using organic solvents for recrystallization is not only complicated in process, but also high in cost.

These factors all lead to problems such as high production cost of domestic folic acid and difficulty in improving the purity.

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