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Method for preparing rubber peptizing agent, namely 2,2'-dibenzamido diphenyl disulfide compound

A technology of dibenzamidodiphenyl disulfide compound and diphenylamino disulfide, applied in hydrogenated polysulfide/polysulfide preparation, organic chemistry, etc., can solve the problem of dibenzamidodiphenyl disulfide There are few reports on sulfur synthesis and other problems, and the effects of improving the fluidity in the mold, high product purity and fast reaction speed are achieved.

Inactive Publication Date: 2012-01-04
LIAOCHENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there are few reports on the synthesis of dibenzamidodiphenyl disulfide at home and abroad.

Method used

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  • Method for preparing rubber peptizing agent, namely 2,2'-dibenzamido diphenyl disulfide compound
  • Method for preparing rubber peptizing agent, namely 2,2'-dibenzamido diphenyl disulfide compound
  • Method for preparing rubber peptizing agent, namely 2,2'-dibenzamido diphenyl disulfide compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 1.0mmol of diphenylamino disulfide and 5ml of diethyl ether into the reaction flask, stir on a magnetic stirrer, add 2.0mmol of triethylamine, dropwise add 2.0mmol of benzoyl chloride, a yellow precipitate is formed immediately, react for 10min, and filter with suction , drying, yield 83%. The product has a melting point of 134-136°C. The assessment index of gained dibenzamido diphenyl disulfide product is as follows:

[0026] Appearance: light yellow solid

[0027] Melting point (°C) 134-136

[0028] The nuclear magnetic data of gained product is as follows:

[0029] NMR data of dibenzamidodiphenyl disulfide:

[0030] 1 H NMR (400MHz, CDCl 3 , ppm), δ=8.93(b, 2H), 8.50-6.93(m, 18H), 4.24-3.59(m, 6H), 2.68-2.51(m, 2H), \1.78-1.35(m, 30H), 0.89-0.86(m, 3H).

[0031] 13 C NMR (CDCl 3 , 100M, ppm,): δ=164.89, 139.91, 136.71, 136.54, 134.29, 134.25, 132.34, 132.27, 131.99, 128.79, 127.97, 127.50, 124.29, 123.54, 123.51, 120.59,

[0032] Infrared analysis is a...

Embodiment 2

[0038] Add 1.0mmol of diphenylamino disulfide and 5ml of diethyl ether to the reaction flask, stir on a magnetic stirrer, add 2.2mmol of triethylamine, dropwise add 2.2mmol of benzoyl chloride, a yellow precipitate is formed immediately, react for 10min, and filter with suction , drying, yield 87%. The product has a melting point of 134-136°C.

Embodiment 3

[0040] Add 1.0mmol of diphenylamino disulfide and 5ml of diethyl ether into the reaction flask, stir on a magnetic stirrer, add 2.2mmol of triethylamine, dropwise add 2.4mmol of benzoyl chloride, a yellow precipitate is formed immediately, react for 10min, and filter with suction , drying, yield 91%. The product has a melting point of 134-136°C.

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Abstract

The invention relates to a method for preparing a rubber peptizing agent, namely a 2,2'-dibenzamido diphenyl disulfide compound. The method comprises the following steps of: putting diphenyl disulfide, a deacid reagent, namely triethylamine, and a solvent in a reactor, stirring at room temperature, and slowly dropping benzoyl chloride, wherein the reaction time is 15-30 min; and obtaining the product by filtering, washing and drying after reacting. The mol ratio of the diphenyl disulfide to the deacid reagent to the benzoyl chloride to diethyl ether is (1.0-1.2):(2.0-2.2):(2.0-2.4):(50-70). According to the method disclosed by the invention, the nitrochlorobenzene is used as a raw material; the diphenyl disulfide is synthesized; the reaction speed is rapid; the reaction process is simple;and the purity of the obtained product is high.

Description

technical field [0001] The invention relates to a method for preparing a rubber peptizer, in particular to a method for preparing a dibenzamidodiphenyl disulfide compound, and belongs to the technical field of chemical additives. Background technique [0002] Mastication is the first step in rubber processing. It depends on the strong mechanical shear force of the open mill or internal mixer to break the rubber molecular chain, thereby improving the plasticity of raw rubber. It is the basis of other processing steps. Plasticizing consumes a lot of energy, labor and time. Therefore, shortening the plasticizing time is an important part of improving production efficiency, and adding peptizers is an effective and simple way to save energy and time. It can accelerate the production process through chemical action. The breakage of molecules significantly improves the plasticizing effect. [0003] Dibenzamido diphenyl disulfide, English name, 2,2′-Dithiobisbenzanilide or 2,2′-Dib...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/42C07C319/22
Inventor 黄现强赵长秋赫庆鹏柳仁民李大成窦建民
Owner LIAOCHENG UNIV
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