High-purity level of 1,1,3-trichloroacetone preparation

Abstract:acetone catalyzed chloride and produced by solvent crystallization at 1,1,3-trichloroacetone with high purity of no less than 99.0%,with a yield of 45%o Key words:1,1,3-trichloroacetone;synthesis;high purity

　　----------. Foreword

1,1,3■trichloroacetone is an important intermediate in the production of folic acid.At present,1,1,3.acetone trichloropacetone,long production cycle(48 hours),poor selectivity,low yield,1,1,3-trichloropacetone content is only about 17%,after water extraction,its content is only 51.9%.And the production cost is high,the product correction is low.These all lead to high domestic folic acid production costs,difficult to improve the content and other problems.The author read a large number of domestic and foreign documents. After many experiments and studies,we added catalyst and controlled fou chlorine speed,reducing the reaction time to 1,1,3-3 trichloropacetone in 24 hours, and 1,1,3-3 trichloropacetone crystallization with purity greater than 99%and the yield of more than 45%.

II. 　　Experimental part

1. reaction

0 0 0 0

1. II.

　　CHaCCHa+Cl:—ClCH.₂CCH.₃+Cl.₂CHCCH.₃+C1CH.₂CCH.₂C1+

1. Experimental steps

In a four-neck flask with a 500ml spherical condenser,a certain amount of acetone and catalyst were stirred and fed to chlorine at a reaction temperature of 10~30 W.Start timing,stop passing through chlorine several hours after the reaction,and continue stirring for 1 hour.A special solvent like material was added to the resulting mixture,stirred for 1 hour while cooled to 10°C crystallization,extracting 1,1,3-trichloroacetone.

1. 1,1,3.Selective determination of trichloroacetone purity

Varin 3700 gas chromatograph,QF・1 filling column and FID detector were used to selectively determine the purity profit of the product and chloride solution.

1. Results of the discussion
2. The influence of catalyst on chloride selectivity showed the selectivity of acetone chlorination

Big influence,Table 1 lists a set of experimental results.From Table 1,the minimum selectivity of 1,1,3-trichloroacetone is significantly increased(about 19.1%)without catalyst,and

　　compound amine catalyst is the best,up to 57.5%o.Test conditions: Innl acetone, 3nr) l chlorine,catalyst 0.6g,temperature 1030°C,

time 18 hours.Within 12 hours va:3.9 Cao h;2

〜7 hours,vq:27 Cao h;7〜18 hours,VQ:3.9 to h.Table 1.Effects of the catalyst on the product selectivity

1. Effect of the through-chlorine velocity on the reaction

The experiment found that uniform chlorine had poor product selectivity,significantly improving the product selectivity and yield.