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Synthesis method of benzotriazole

A technology of benzotriazole and a synthesis method, which is applied in the field of organic synthesis, can solve the problems of high price, restricted application and the like, and achieves the effects of short reaction time, little pollution and high yield

Inactive Publication Date: 2016-01-13
NANTONG BOTAO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because benzimidazolone is prepared by the reaction of o-phenylenediamine and urea, it is expensive, which restricts the application of this synthetic method.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The synthesis method of benzotriazole in this embodiment is to synthesize benzotriazole in one step through the pressurization method of o-phenylenediamine, and the specific steps are as follows:

[0022] (1) Feeding: Put 100g o-phenylenediamine, 110g sodium nitrite and 1000g water into a 3000L stainless steel reactor;

[0023] (2) Heating and pressurizing: Turn on stirring, raise the temperature, raise the temperature to 240°C, control the pressure between 3.0MPa, and keep warm for 3 hours;

[0024] (3) Transfer to the acidification kettle: cool down to 120°C, and transfer the reaction product to the acidification kettle;

[0025] (4) pH adjustment and stratification: adjust the pH value from 11.7 to 5.0 with concentrated sulfuric acid, and stratify;

[0026] (5) Purification and collection: The stratified oil layer enters the rectification kettle for purification under reduced pressure, and collects the 202°C / 15mmHg distillate product.

Embodiment 2

[0028] The synthesis method of benzotriazole in this embodiment is to synthesize benzotriazole in one step through the pressurization method of o-phenylenediamine, and the specific steps are as follows:

[0029] (1) Feeding: Put 100g o-phenylenediamine, 120g sodium nitrite and 1500g water into a 3000L stainless steel reactor;

[0030] (2) Heating and pressurizing: Turn on stirring, raise the temperature, raise the temperature to 260°C, control the pressure between 4.0MPa, and keep warm for 3.5 hours;

[0031] (3) Transfer to the acidification kettle: cool down to 130°C, and transfer the reaction product to the acidification kettle;

[0032] (4) pH adjustment and stratification: adjust the pH value from 11.7 to 5.0 with concentrated sulfuric acid, and stratify;

[0033] (5) Purification and collection: The stratified oil layer enters the rectification kettle for purification under reduced pressure, and collects 204°C / 15mmHg distillate products.

Embodiment 3

[0035] The synthesis method of benzotriazole in this embodiment is to synthesize benzotriazole in one step through the pressurization method of o-phenylenediamine, and the specific steps are as follows:

[0036] (1) Feeding: Put 100g o-phenylenediamine, 115g sodium nitrite and 1250g water into a 3000L stainless steel reactor;

[0037] (2) Heating and pressurizing: Turn on stirring, raise the temperature, raise the temperature to 250°C, control the pressure between 3.5MPa, and keep warm for 3.2 hours;

[0038] (3) Transfer to the acidification kettle: cool down to 125°C, and transfer the reaction product to the acidification kettle;

[0039] (4) pH adjustment and stratification: adjust the pH value from 11.7 to 5.0 with concentrated sulfuric acid, and stratify;

[0040] (5) Purification and collection: The stratified oil layer enters the rectification kettle for purification under reduced pressure, and collects 203°C / 15mmHg distillate products.

[0041] The following table is...

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Abstract

The invention relates to a synthesis method of benzotriazole. The benzotriazole is synthesized in one step through an o-phenylenediamine pressurization method. The synthesis method particularly comprises the following steps that 1, material feeding is conducted, wherein o-phenylenediamine, sodium nitrite and water are added into a stainless steel reaction kettle according to the proportion of 1 to 1.1-1.2 to 10-15; 2, heating and pressurization are conducted, wherein stirring is started, the temperature is increased to range from 240 DEG C to 260 DEG C, the pressure is controlled to range from 3.0 MPa to 4.0 MPa, and heat preservation reaction is conducted for 3-3.5 h; 3, the reacted mixture is transferred to an acidification kettle, wherein the temperature is decreased to range from 120 DEG C to 130 DEG C, and a reaction product is transferred to the acidification kettle; 4, pH adjustment and delamination are conducted, the PH value is adjusted from 11.7 to 5.0 through concentrated sulfuric acid, and delamination is conducted; 5, purification and collection are conducted, wherein the delaminated oil layer enters a rectifying kettle for decompression purification, and distillate products at 202-204 DEG C / 15 mmHg are collected. The synthesis method of the benzotriazole has the advantages that acetic acid is not needed, side reactions are few, pollution is less, the yield is high, the reaction time is short, and continuous production can be achieved.

Description

technical field [0001] The invention relates to the field of organic compound synthesis, in particular to a synthetic method of benzotriazole [0002] Law. Background technique [0003] Benzotriazole (English name Benzotriazole, referred to as BTA; also known as benzotriazole, benzotriazole, benzotriazole, benzotriazole, triazine) is an important fine chemical product . [0004] Benzotriazole has a wide range of uses, mainly used as corrosion inhibitors for copper and copper alloys, metal rust inhibitors, photographic antifogging agents and organic synthesis intermediates; it is also widely used as preservatives for coating additives and synthetic detergents , anticoagulant, lubricating oil additive, synthetic dye intermediate, polymer material stabilizer, plant growth regulator, anti-tarnish agent, gas phase corrosion inhibitor and ultraviolet light absorber. Benzotriazole can be used in combination with various corrosion inhibitors to improve the corrosion inhibition ef...

Claims

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Application Information

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IPC IPC(8): C07D249/18
CPCC07D249/18
Inventor 黄海涛王宏李桂萍
Owner NANTONG BOTAO CHEM
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