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A method for selectively producing dichloro-p-xylene

A technique for the ratio of p-xylene and dichloride, which is applied in the field of preparation of dichloro-p-xylene, can solve the problems of easy carbon deposition, deactivation, and coking of catalysts, and achieve improved selectivity, process safety, high production efficiency, The effect of simple process

Active Publication Date: 2020-12-18
JIANGSU YANGNONG CHEM GROUP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are disadvantages such as poor chlorination selectivity and low yield
[0006] (2) Elemental catalysts: such as sulfur, iodine, lead, etc., which have no practical application in the synthesis of dichloro-p-xylene
[0012] (3) Molecular sieve catalyst: the positioning effect is better, but the catalyst is easy to deactivate due to carbon deposition and coking
[0014] So far, there has been no report on using p-xylene as a raw material to continuously catalyze the synthesis of dichloro-p-xylene using a combined catalyst

Method used

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  • A method for selectively producing dichloro-p-xylene
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The effective reaction volume of the tank reactor is 500L. Feed 180 kg of p-xylene into the reactor through a metering pump, add 5wt% ferrous sulfide and 0.5wt% 2-chloro-phenyl methyl sulfide to the kettle, and adopt secondary absorption for tail gas absorption: primary water Absorption, secondary alkali absorption. Chlorine flow rate is 5m 3 / h, control reaction temperature 15~30℃, reaction pressure -0.002MPa, react for 10h, pass chlorine gas for about 50m 3 When the temperature rises to 50-60°C, continue to pass chlorine gas, and stop the reaction when the basic reaction of monochlorine is complete. The ratio of 2,5-dichloro to 2,6-dichloro in the chlorinated solution is 8.9, and the utilization rate of chlorine gas is 98.5%.

Embodiment 2

[0043] Two-stage tank type reactor in series, each tank has an effective reaction volume of 30L, and the total effective reaction volume is 60L. Add 1kg ferrous sulfide respectively in the first-level and second-level kettles, and enter the p-xylene containing 2-chloro-phenyl methyl sulfide (auxiliary dose is 0.5wt% of p-xylene) to the first-level reactor by metering pump , the feed flow rate is 8L / h, and the chlorine gas flow rate in the primary and secondary kettles is 1.5m respectively 3 / h, 1m 3 / h, control the reaction temperature of the primary and secondary kettles to be 20-30°C and 50-60°C respectively. The reaction solution overflows from the top of the first-stage reactor to the second-stage reactor, and the reaction residence time is about 8 hours. The ratio of 2,5-dichloro to 2,6-dichloro in the chlorinated solution is 8.61, and the utilization rate of chlorine gas is 98%.

Embodiment 3

[0045] Three-stage tank-type series reactor, the effective reaction volume of each tank is 30L, and the total effective reaction volume is 90L. Add 1kg of ferrous sulfide respectively in the first-level, second-level and third-level kettles, and enter the p-xylene containing 2-chloro-phenyl methyl sulfide into the first-level reaction kettle by metering pump (the auxiliary dose is 0.5% of p-xylene). wt%), the feed flow rate is 8L / h, and the chlorine gas flow rate in the primary, secondary, and tertiary kettles is respectively 1.5m 3 / h, 1m 3 / h, 1m 3 / h, control the reaction temperatures of the primary, secondary, and tertiary kettles to be 15-20°C, 40-50°C, and 55-65°C, respectively. The reaction solution overflows from the top of the first-stage reactor to the next-stage reactor in sequence, and the reaction residence time is about 11 hours. The ratio of 2,5-dichloro to 2,6-dichloro in the chlorinated liquid is 10.5, and the utilization rate of chlorine gas is 99.5%.

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Abstract

The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method of dichloro-p-xylene. According to the method, p-xylene or 2-chloro-p-xylene servesas the raw material, a continuous chlorination reaction is carried out by selecting different catalytic systems and reaction process conditions, and the proportion of 2,5-dichloro-p-xylene to 2,6-dichloro-p-xylene can be selectively controlled to better meet requirements of the market and customers. The method has relatively high economic value.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of dichloro-p-xylene. The present invention uses p-xylene or 2-chloro-p-xylene as raw material, and can selectively control 2,5-dichloro-p-xylene (abbreviated as 2, The ratio of 5-dichloro) to 2,6-dichloro-p-xylene (abbreviated as 2,6-dichloro) better adapts to the needs of the market and customers, and has higher economic value. Background technique [0002] 2,5-dichloro is a white solid with a melting point of 69-70°C, and 2,6-dichloro is a colorless liquid with a melting point of 15°C. Both substances contain active groups that can undergo substitution and addition reactions. It is mainly used in the preparation of pesticides and pharmaceutical intermediates, such as the preparation of dichloroterephthalonitrile and dichloroterephthalic acid. When p-xylene or 2-chloro-p-xylene is used as raw material for chlorination, the chlorinat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/12C07C25/125B01J31/28B01J23/745
CPCB01J23/002B01J23/745B01J31/28C07C17/12C07C25/125
Inventor 周颖华王怡明丁克鸿徐林严绘黄杰军赵慧卞辰超
Owner JIANGSU YANGNONG CHEM GROUP