Efficient synthesis method of 5-chlorobenzotriazole

A technology of chlorobenzotriazole and a synthetic method, which is applied in the preparation of sulfate/bisulfate, organic chemistry, etc., can solve the problems of low yield of process products, serious environmental pollution, and high production cost, and achieves high yield , the effect of high profit and low cost

Inactive Publication Date: 2018-07-27
肖志才
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process product yield is low, the production cost is high, the waste water is much, and the environmental pollution is serious

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1 A kind of high-efficiency synthetic method of 5-chlorobenzotriazole comprises the following steps:

[0019] ⑴Put 2-nitro-4-chloroaniline (red base 3GL), water, and catalyst Raney nickel into the reactor in sequence, and then vacuumize-inject nitrogen with a purity of 99.9%-vacuumize, repeat 3 times and then pump into High vacuum with a vacuum degree of 0.098MPa, and then inject hydrogen with a purity of 99.9%; start stirring and raise the temperature to 120°C, keep the pressure at 2MPa, and react for 4 hours until no hydrogen is absorbed, keep the hydrogen pressure for 2 hours, and then cool down To 80 ℃, empty, open the kettle, and get the completely reacted material through the climbing board test.

[0020] Wherein: the addition of water is 4 times of the weight of 2-nitro-4-chloroaniline; the addition of Raney nickel is 8% of the weight of 2-nitro-4-chloroaniline.

[0021] (2) The fully reacted material is left to stand for 2 hours and then filtered to ...

Embodiment 2

[0026] Embodiment 2 A high-efficiency synthesis method of 5-chlorobenzotriazole comprises the following steps:

[0027] ⑴Put 2-nitro-4-chloroaniline (red base 3GL), water, and catalyst Raney nickel into the reactor in sequence, and then vacuumize-inject nitrogen with a purity of 99.9%-vacuumize, repeat 3 times and then pump into High vacuum with a vacuum degree of 0.098MPa, and then inject hydrogen with a purity of 99.9%; start stirring and raise the temperature to 140°C, keep the pressure at 4MPa, and react for 3 hours until no hydrogen is absorbed, keep the hydrogen pressure for 2 hours, and then cool down To 80 ℃, empty, open the kettle, and get the completely reacted material through the climbing board test.

[0028] Wherein: the addition of water is 6 times of the weight of 2-nitro-4-chloroaniline; the addition of Raney nickel is 12% of the weight of 2-nitro-4-chloroaniline.

[0029] (2) The fully reacted material is left to stand for 2 hours and then filtered to obtain ...

Embodiment 3

[0034] Embodiment 3 A high-efficiency synthesis method of 5-chlorobenzotriazole comprises the following steps:

[0035] ⑴Put 2-nitro-4-chloroaniline (red base 3GL), water, and catalyst Raney nickel into the reaction kettle in sequence, and then vacuumize-inject nitrogen with a purity of 99.9%-vacuumize, repeat 3 times and then evacuate. High vacuum with a vacuum degree of 0.098MPa, and then inject hydrogen with a purity of 99.9%; start stirring and heat up to 130°C, keep the pressure at 3MPa, and react for 3.5 hours until no hydrogen is absorbed, keep the hydrogen pressure for 2 hours, and then cool down To 80 ℃, empty, open the kettle, and get the completely reacted material through the climbing board test.

[0036] Wherein: the addition of water is 5 times of the weight of 2-nitro-4-chloroaniline; the addition of Raney nickel is 10% of the weight of 2-nitro-4-chloroaniline.

[0037] (2) The fully reacted material is left to stand for 2 hours and then filtered to obtain an a...

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PUM

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Abstract

The invention relates to an efficient synthesis method of 5-chlorobenzotriazole. The method comprises the following steps of (1) adding 2-nitro-4-chloroaniline, water and catalysts of raney nickel into a reaction kettle for reaction; performing climbing plate detection to obtain completely reacted materials; (2) performing filtering and reduced pressure dewatering on the completely reacted materials to obtain 4-chloro-1,2-diaminobenzene materials and waste water A; (3) adding the 4-chloro-1,2-diaminobenzene materials and sodium nitrite into a medium pressure reaction kettle; adding water; performing heat release reaction to obtain a 5-chlorobenzotriazole sodium salt water solution; (5) dripping sulphuric acid into the 5-chlorobenzotriazole sodium salt water solution; performing filtering and spin drying to obtain a 5-chlorobenzotriazole coarse product and waste water B; (5) washing and drying the 5-chlorobenzotriazole coarse product to obtain washing water and a finished product of 5-chlorobenzotriazole with the content being higher than or equal to 99 percent; (6) mixing the waste water A, the waste water B and washing water; then, performing negative pressure distillation to obtain distilled water and waste slag; returning the distilled water into the step (1); dewatering the waste slag to obtain a byproduct of sodium sulfate with the content being higher than or equal to 96percent. The method has the advantages of low cost, low energy consumption and high earnings.

Description

technical field [0001] The invention relates to the technical field of compound synthesis, in particular to a high-efficiency synthesis method of 5-chlorobenzotriazole. Background technique [0002] 5-Chlorobenzotriazole is a white powder with the molecular formula C 6 h 4 ClN 3 , its melting point is 157~158°C, slightly soluble in water and soluble in organic solvents. It is widely used in water treatment, and mainly replaces benzotriazole to remove dirt in water circulation. 5-Chlorobenzotriazole is an efficient metal antirust agent, mainly used for vapor phase antirust of copper products, and the antirust effect is more than ten times higher than that of benzotriazole commonly used at home and abroad. [0003] The existing domestic method for producing 5-chlorobenzotriazole is to add hydrazine hydrate to reduce 2-nitro-4-chloroaniline to generate 4-chloro-o-phenylenediamine, which not only has low product yield, but also has a lot of waste water and hydrazine hydrate ...

Claims

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Application Information

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IPC IPC(8): C07D249/18C01D5/02
CPCC01D5/02C01P2006/80C07D249/18
Inventor 肖志才陈新
Owner 肖志才
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