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Method for continuously producing 6-chloro-2, 4-dinitroaniline and diazonium salt thereof

A technology of dinitroaniline and diazotization, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of cumbersome operation steps and low production efficiency, so as to simplify the process flow and improve production efficiency , to achieve the effect of economic and environmental benefits

Pending Publication Date: 2021-12-21
ZHEJIANG DIBANG CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The product of the chlorination reaction needs to be washed, dried and ground before it can be used. The whole process operation steps are cumbersome and the production efficiency is low.

Method used

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  • Method for continuously producing 6-chloro-2, 4-dinitroaniline and diazonium salt thereof
  • Method for continuously producing 6-chloro-2, 4-dinitroaniline and diazonium salt thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0079] (continuous production of 6-chloro-2,4-dinitroaniline)

[0080] Such as figure 1 As shown, two series of high-gravity reactors B and C, three parallel stratified tanks F, G and H, and three parallel distillation tanks I, J and K are used. Among them, the volumes of the supergravity reactors B and C are both 500L, the chlorination reaction temperature is 40°C-45°C, the volumes of the layered tanks F, G, and H are all 1000L, and the volumes of the distillation tanks I, J, and K are all 1000L. is 1500L, the volume of hydrochloric acid recovery tank M is 1500L, the volume of condenser L is 500L, the volume of acid mixing tank N is 1000L, and the liquid level setting value of stratified tanks F, G and H is 90% of its volume. The liquid level setting value of distillation tank I, J and K is 50% of its volume.

[0081] In batching kettle A (volume 1500L), add 2,4-dinitroaniline and carbon tetrachloride continuously simultaneously, and the feeding speed of the two is respecti...

Embodiment 2

[0089] Repeat the method of Example 1 to obtain an organic phase comprising 6-chloro-2,4-dinitroaniline, followed by figure 2 As shown, the organic phase is not distilled, but is directly injected into the two-stage series high-gravity reactors b and c together with nitrosyl sulfuric acid with a mass concentration of 25% from the nitrosyl sulfuric acid storage tank a to carry out the diazotization reaction . Among them, the feed rates of the organic phase and nitrosyl sulfuric acid are 566.2kg / h and 254.2kg / h respectively, the volumes of the high-gravity reactors b and c are both 25L, and the diazotization reaction temperature is 18°C-25°C , the volume of stratified tanks h, g and f is 100L, the volume of diazonium salt solution storage tank k is 300L, and the liquid level setting value of stratified tanks h, g and f is 80% of its volume.

[0090] Wherein, a part of the material in the primary supergravity reactor b passes through the circulation pump (not shown) and then re...

Embodiment 3

[0094] (continuous production of 6-chloro-2,4-dinitroaniline)

[0095] Repeat the method of Example 1, except for the following steps, and the rest of the steps are the same as in Example 1.

[0096] Add 2,4-dinitroaniline and carbon tetrachloride continuously in batching kettle A (volume 500L) at the same time, and the feeding speeds of the two are respectively 110.02kg / h and 550.10kg / h; The carbon tetrachloride solution of nitroaniline is injected into the primary supergravity reactor B at a speed of 660.12kg / h. Simultaneously, mass concentration is that the hydrochloric acid of 16% is 547.5kg / h with feed rate, and chlorine is passed into the primary supergravity reactor B with the flow rate of 42.6kg / h. A part of the material in the primary supergravity reactor B passes through the circulating pump (not shown) and returns to the primary supergravity reactor B through the heat exchanger D, and the other part enters the secondary stage at a flow rate of 1250.22kg / h. Hypergr...

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Abstract

The invention relates to a method for continuously producing 6-chloro-2, 4-dinitroaniline and diazonium salt of 6-chloro-2, 4-dinitroaniline. A carbon tetrachloride solution in which 2, 4-dinitroaniline is dissolved, hydrochloric acid and chlorine are continuously injected into a first-stage supergravity reactor, and undergochlorination by adopting multiple stages of supergravity reactors connected in series, one part of the material in the first-stage supergravity reactor enters into the self reactor and undergo circular reaction, the other part of the material enters a second-stage supergravity reactor and undergoes chlorination, and in the whole process, one part of the material in the upper-stage supergravity reactor enters the reactor for circular reaction, and the other part of the material in the lower-stage supergravity reactor enters the next-stage supergravity reactor for chlorination reaction until the reaction is complete. And the material after complete reaction is separated to obtain an organic phase and hydrochloric acid, and the organic phase is distilled and separated to obtain 6-chloro-2, 4-dinitroaniline, carbon tetrachloride and hydrochloric acid for recycling. The organic phase can be used for the continuous production of 6-chloro-2, 4-dinitroaniline diazonium salt.

Description

technical field [0001] The invention belongs to the production field of dye intermediates, in particular to a method for continuous production of 6-chloro-2,4-dinitroaniline and its diazonium salt. Background technique [0002] 6-Chloro-2,4-dinitroaniline is an important intermediate of disperse dyes. Its production method is mainly obtained by chlorination reaction of 2,4-dinitroaniline as raw material. Common processes mainly include: [0003] (1) Sodium hypochlorite chlorination method: beat 2,4-dinitroaniline in hydrochloric acid, slowly add sodium hypochlorite solution to the beaten material to carry out chlorination reaction. The production process of this method is complicated, and by-products are generated during the reaction process, the product quality is poor, the color is deep, the time consumption is long, the production efficiency of the equipment is low, and the waste water contains more sodium chloride, and the post-treatment is relatively cumbersome. [0...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/74C07C209/86C07C211/52C07C245/20
CPCC07C209/74C07C209/86C07C245/20C07C211/52
Inventor 唐智勇罗勇刘泊良陈建峰冯彦博徐斌徐万福邹海魁初广文孙宝昌张亮亮
Owner ZHEJIANG DIBANG CHEM
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