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.

Table 2 lists a set of test data.

Table 2 Effects of pass-chlorine velocity on product selectivity

Test^condition:]Petri dish 1 acetone,catalyst:composite class 0.6go

The experiment found that the fluchlorine was early(12 hours)and later(8 24 h),most chlorine escape that the reaction was slow and the medium(28 h)was fast.When the chlorine gas is stopped,the product selectivity and yield are significantly reduced.The results showed that 1,1,3 produced much slower than

1,1-dichloroacetone.During the reaction with

chloride,chloride,acetone,1,1,4003000,

CICH2CCH3

　　o.

that is_II.chlorination on submethyl group was much

faster than on methyl group.Therefore,the

author believes that the acetone chloride generation process reaction process is:

The reaction is conducted with V1 1 2-5 as the main process.

According to the Table 2 data,the reaction velocity order of each step is

　　V2^”3^1 2 5>V4

Depending on the reaction speed of each step,

It can be seen from the data of Table 3 that,due to the small boiling point difference between 1,1,3.trichloroacetone and by-products,it is generally difficult to separate water extraction and separation is a simple means.Although most I products can be removed,the purity is difficult

we control the pass chlorine speed at each stage,

to achieve the purpose of reducing the pass chlorine time and inhibiting the selectivity of increasing the secondary reaction speed by 1,1,3 trichloroacetone..

1. Hydrated crystal purification According to the literature,usually the

acetone chloride liquid is extracted or refined by water to increase the content of 1,1,3-trichloroacetone,and the author used 1,1,3-trichloroacetone to crystallization from other by-products.

Table 3 lists the product purity obtained by the various separation methods.

Table 3.Product purity obtained from the different separation methods

to further improve.Product purity reaches over 99%,and the yield is also the highest in several methods,up to 45%o.1 The method requires a 1,1,3-trichloroacetone content of K more than 50%in the chloride solutiono.

Select appropriate compound amine catalyst,control slow chlorine blocking in early and late at 10~30°C,can make 1,1,3-trichloroacetone chloride,purified by special solvent crystallization,obtain crystalline product with no less than 99.0%,with yield of 45%,but 1,1,3-trichloroacetone in chloride solution must be greater than 50%o.Athena CEO

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