Method for preparing dichlorobenzene and trichlorobenzene and increasing para-ortho ratio

A technology of trichlorobenzene and dichlorobenzene, which is applied in the field of preparing dichlorobenzene and trichlorobenzene to improve the para-ortho ratio, can solve unsatisfactory para-selectivity, low conversion rate and para-selectivity, chlorination Problems such as low para-selectivity of the product, to achieve the effect of low cost of use on an industrial scale, low cost of use, and good selectivity

Inactive Publication Date: 2016-10-12
JIANGSU YANGNONG CHEM GROUP +2
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] (1) Lewis acids, such as FeCl 3 , AlCl 3 , ZnCl 2 , SbCl 5 etc., its main disadvantage is that the para-selectivity in the chlorinated product is low, about p / o=3, although many improvements have been made, the para-selectivity is still unsatisfactory
[0007] (2) Elemental catalysts, such as sulfur, iodine, lead, antimony powder, etc., have the advantage of being cheap and easy to obtain, but the problem is that the conversion rate and para-selectivity are low
[0011] At present, the market demand for p-dichlorobenzene is growing steadily, and there is a large backlog of o-dichlorobenzene. At the same time, due to the increase in the market use of the pesticide dicamba in 2014, the market has a relatively large increase in demand for 1,2,4-trichlorobenzene, reaching 1 10,000 tons / year, but 1,2,3-trichlorobenzene has no price and no market, and it is basically difficult to sell

Method used

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  • Method for preparing dichlorobenzene and trichlorobenzene and increasing para-ortho ratio
  • Method for preparing dichlorobenzene and trichlorobenzene and increasing para-ortho ratio
  • Method for preparing dichlorobenzene and trichlorobenzene and increasing para-ortho ratio

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Experimental program
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Effect test

Embodiment 1

[0037] The effective reaction volume of the tank reactor is 10L. Enter benzene 10L to reactor by metering pump, wherein add auxiliary agent 0.5wt% in the raw material benzene, add content and be 0.5kg of iron-copper bimetallic catalyst dry base of 60wt% in the system, wherein the weight ratio of iron and copper in the catalyzer is 15:1, control reaction temperature 65~70℃, reaction pressure -0.004MPa, chlorine gas flow rate 0.7m 3 / h, the reaction time is about 6hr. After the reaction is completed, the reaction liquid is delightened, rectified, and crystallized to obtain finished products of dichlorobenzene and trichlorobenzene. The content of p-dichlorobenzene and o-dichlorobenzene is greater than 99.9%, the content of 1,2,4-trichlorobenzene and 1,2,3-trichlorobenzene is greater than 99.5%, and the total yield is 95%.

[0038]

Embodiment 2

[0040] Three kettles are connected in series, and the effective volume of each kettle is 20L, 15L, and 15L respectively, and the total effective volume is 50L. Add 1.5kg of iron-copper bimetallic catalyst dry basis with a content of 60wt% respectively in the first-level, second-level, and third-level kettles, wherein the weight ratio of iron and copper in the catalyst is 15:1, and the reaction temperature is controlled at 65-70°C. The reaction pressure is -0.004Mpa, and the stirring speed is 200rpm. Benzene is fed into the first-stage reaction kettle through a metering pump, wherein 0.5wt% of additives are added to the raw material benzene, the feed flow rate is 8L / hr, and the chlorine gas flow rate of the first-stage, second-stage, and third-stage reactors is 1.5m 3 / h, 1m 3 / h, 1m 3 / h, the reaction solution overflows from the top of the first-stage reactor to the next-stage reactor successively, and the reaction residence time is about 6hr. The reaction solution from the ...

Embodiment 3

[0043] The volume of the ring chlorination reactor is 50L (including catalyst filtration and feed liquid extraction system). Add 2.5kg of iron-copper bimetallic catalyst with a content of 60wt% on a dry basis to the system, wherein the weight ratio of iron to copper in the catalyst is 15:1, control the reaction temperature at 65-70°C, and the reaction pressure -0.004MPa, through a metering pump Benzene is fed into the reactor, wherein 0.5wt% of additives are added to the raw material benzene, the feed flow rate is 8L / hr, and the chlorine gas flow rate is 3.5m 3 / h, the reaction residence time is about 6hr. The HCl generated by the reaction of the chlorination reaction material circulates in the loop reactor, and the reaction liquid containing additives passes through the ceramic filter, and the clear liquid is discharged through the overflow port, and the clear liquid is obtained after light removal, rectification, and crystallization Dichlorobenzene and trichlorobenzene prod...

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Abstract

The invention provides a method for preparing dichlorobenzene and trichlorobenzene and increasing the para-ortho ratio, and is characterized in that a chlorination reaction takes benzene or chlorobenzene as a raw material; a continuous chlorination reaction is carried out in the presence of a main catalyst and an auxiliary agent, through a ring type continuous chlorination reactor or a multi-stage series-connection kettle type reactor and under the conditions of the reaction temperature of 50-120 DEG C and the reaction pressure of -0.05-0.5 MPa; and a reaction liquid passes through a membrane filtration system, the main catalyst remains in the reactor for reaction, a dichlorobenzene clear liquid after filtration is subjected to light component removal, rectification and crystallization to obtain dichlorobenzene, orthodichlorobenzene, 1,2,3-trichlorobenzene and 1,2,4-trichlorobenzene finished products. Compared with a conventional dichlorobenzene preparation process, the method has the dichlorobenzene para-ortho ratio greatly increased to 8.5 and the trichlorobenzene para-ortho ratio greatly increased to 13.6, and has the advantages of low use cost of the catalyst auxiliary agent, continuous production realization, good product selectivity and the like.

Description

technical field [0001] The invention relates to a method for preparing dichlorobenzene and trichlorobenzene to improve the para-ortho ratio, especially adopting a method of using benzene or chlorobenzene as raw material, adding catalysts and additives to prepare dichlorobenzene and trichlorobenzene to improve the para-o-ratio Neighborhood method. Background technique [0002] P-dichlorobenzene has the characteristics of low toxicity, strong medicinal properties, easy volatilization, and no residue after sublimation. It is an excellent anti-mildew and anti-moth agent for household clothes and indoor deodorant. Since the carcinogenic effect of naphthalene was recognized by people, people tried to use it to replace naphthalene as an insecticide and disinfectant. Its outstanding advantages are that it will not damage clothes during use and leave no stains. The effect is better than naphthalene, but the toxicity is far away. lower than naphthalene. At the same time, p-dichlorob...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/12C07C25/08C07C25/10B01J31/02
CPCC07C17/12B01J27/02B01J31/02B01J35/0006C07C25/08C07C25/10
Inventor 王怡明申明稳丁克鸿邵波殷恒志严绘
Owner JIANGSU YANGNONG CHEM GROUP
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