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Synthetic method of 2-mercaptobenzimidazole allyl sulfide

A technology of mercaptobenzimidazolene propylene sulfide and mercaptobenzimidazole, which is applied in the fields of iron and steel, petrochemical, electric power and construction, and petroleum, can solve the problems of high production cost and unfavorable industrialization, and achieve high yield and synthetic reaction The effect of mild conditions and simple process

Inactive Publication Date: 2014-03-12
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that a large amount of allyl alcohol is used as a solvent, which makes the production cost higher and is not conducive to industrialization.

Method used

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  • Synthetic method of 2-mercaptobenzimidazole allyl sulfide
  • Synthetic method of 2-mercaptobenzimidazole allyl sulfide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1) Under the protection of nitrogen, add 1 part (2.4g) of 2-mercaptobenzimidazole and 4 (9.6g) parts of acetone into the reaction kettle, and magnetically stir until 2-mercaptobenzimidazole Fully dissolve evenly.

[0023] 2) After dissolving evenly, add 5 parts (12g) of potassium hydroxide solution with a mass fraction of 26% into the reaction kettle, then quickly add 0.2 parts (0.48g) of tetrabutylammonium bromide, and stir magnetically to make it uniform.

[0024] 3) Add 1 part (2.4g) of allyl chloride dropwise and keep stirring at room temperature for 3h.

[0025] 4) Collect the product after filtration and drying, and further recrystallize and purify with acetone to obtain the product.

[0026] The prepared 2-mercaptobenzoallyl sulfide is a pale yellow solid crystal with a melting point between 125°C and 131°C.

Embodiment 2

[0028] 1) Under the protection of nitrogen, add 1 part (2.4g) of 2-mercaptobenzimidazole and 4 parts (9.6g) of tetrahydrofuran into the reaction kettle, and magnetically stir until 2-mercaptobenzimidazole Fully dissolve evenly.

[0029] 2) After dissolving evenly, add 5 parts (15g) of potassium hydroxide solution with a mass fraction of 26% into the reaction kettle, then quickly add 0.2 parts (0.48) of tetrabutylammonium hydroxide, and stir magnetically to make it uniform.

[0030] 3) Add 1 part (2.4g) of allyl bromide dropwise, and keep stirring at room temperature for 3h.

[0031] 4) Collect the product after filtration and drying, and further recrystallize and purify with acetone to obtain the product.

[0032] The prepared 2-mercaptobenzoallyl sulfide is a pale yellow solid crystal with a melting point between 125°C and 131°C.

Embodiment 3

[0034] 1) Under the protection of nitrogen, add 1.25 parts (3g) of 2-mercaptobenzimidazole and 5 parts (12g) of acetone into the reaction kettle, and stir magnetically until 2-mercaptobenzimidazole is fully dissolved uniform.

[0035] 2) After dissolving evenly, add 4 parts (9.6g) of potassium hydroxide solution with a mass fraction of 26% into the reaction kettle, then quickly add 0.1 part (0.24g) of tetrabutylammonium hydroxide, and stir magnetically to make it uniform.

[0036] 3) Add 2 parts (4.8g) of allyl chloride dropwise and keep stirring at room temperature for 3h.

[0037] 4) Collect the product after filtration and drying, and further recrystallize and purify with acetone to obtain the product.

[0038] The prepared 2-mercaptobenzoallyl sulfide is a pale yellow solid crystal with a melting point between 125°C and 131°C.

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Abstract

The invention relates to a synthetic method of 2-mercaptobenzimidazole allyl sulfide. The synthetic method comprises the following steps: adding 1-2 parts by mass of 2-mercaptobenzimidazole and 3-5 parts by mass of organic solvent to a reaction kettle under the protection of nitrogen, and magnetically stirring till the 2-mercaptobenzimidazole is fully and uniformly dissolved; then adding 4-5 parts by mass of 26% potassium hydroxide solution to the reaction kettle, afterwards, rapidly adding 0.1-0.2 part of phase transfer catalyst, and magnetically stirring so as to uniformize the phase transfer catalyst; dropwise adding 1-3 parts of halogenated hydrocarbon, stirring and reacting for 3 hours at a room temperature; and filtering, drying, collecting a product, further recrystallizing and purifying by using acetone so as to obtain the product. The synthetic method has the advantages that synthetic reaction conditions are relatively mild, the yield of the 2-mercaptobenzimidazole alkene thio-propenyl ether obtained by a phase transfer method is relatively high, the technology is simple, excessive aftertreatment is not needed, and the follow-up testing of the experiment is easily satisfied.

Description

technical field [0001] The invention relates to the fields of petroleum, petrochemical, steel, electric power, construction and the like, in particular to a synthesis method of a 2-mercaptobenzimidazolene propylene sulfide metal corrosion inhibitor. Background technique [0002] The contact between metal materials and equipment and acids in production is unavoidable. For example, acid leaching is required to remove iron scale and rust on the steel surface; pickling is required for descaling and rust removal of industrial equipment; in order to increase the speed of oil production, acid is injected into underground oil layers to dissolve rock formations; acid storage and transportation tools Wait. Corrosion inhibitors for acidic media are usually used to protect metal materials in contact with acid. However, hydrochloric acid has a corrosive effect on metal surfaces, and a corrosion inhibitor is a substance that can prevent or slow down the corrosion of metals in environmen...

Claims

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Application Information

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IPC IPC(8): C07D235/28
CPCC07D235/28
Inventor 黄定海宋丹
Owner TIANJIN UNIV
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