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Preparation of 2,2-disulfo-dibenzopyrene by oxygen process based on 2-mercaptan benzothiazole ammonia salt

A technology of dithiodibenzothiazole and dithiodibenzothiazole, which is applied in the field of preparation 2, can solve problems such as high risk, high toxicity, and difficult control of the process, and achieve the effect of cost reduction

Inactive Publication Date: 2008-03-12
QINGDAO UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The object of the present invention is to overcome the disadvantages of high toxicity, serious environmental pollution, difficult process control, and high risk in the manufacturing process of the prior art, and provide a low toxicity, convenient source of raw materials, no pollution to the environment, and economical A new process method for large quantities of industrial water

Method used

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  • Preparation of 2,2-disulfo-dibenzopyrene by oxygen process based on 2-mercaptan benzothiazole ammonia salt
  • Preparation of 2,2-disulfo-dibenzopyrene by oxygen process based on 2-mercaptan benzothiazole ammonia salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] 1. Weigh 50 grams of refined 2-mercaptobenzothiazole and add it to the container, then add 200 grams of 25% ammonia water and 720 grams of water, heat the container to 70 ° C, and stir during the heating process to make 2- Mercaptobenzothiazole is fully dissolved in the solution;

[0014] 2. Put the obtained ammonium salt solution of 2-mercaptobenzothiazole at room temperature, filter it and add it to the reactor, add 0.45 g of copper sulfate catalyst, and feed oxygen to make the raw material undergo oxidation-reduction reaction, and keep the temperature of the reactor at 50°C ; Pressure 1.0mMPa, reaction time 120min;

[0015] 3. After the reaction time is over, open the reaction kettle, and suction filter the solution; obtain a filter cake; wash the filter cake with water, dry, and pulverize to obtain 43.45 grams of the target product 2,2'-dithiodibenzothiazole.

[0016] 5. Tested by the GB11408-89 method, the purity is >90%, and the yield is 86.9%.

Embodiment 2

[0018] 1. Weigh 50 grams of crude 2-mercaptobenzothiazole and add it to a four-necked flask, add 45 grams of liquid ammonia and 470 grams of water, heat the container to 40°C, and stir during the heating process to make the 2-mercaptan The base benzothiazole is fully dissolved in the solution;

[0019] 2. Put the ammonium salt solution of 2-mercaptobenzothiazole at room temperature, filter it and add it to the reaction kettle, add 0.45 g of catalyst copper acetate catalyst; when the ammonium salt solution is 70-75°C, air is introduced to oxidize the raw material For reaction, keep the container pressure at 0.6MPa, and the reaction time is 100min;

[0020] 3. After the reaction is over, open the reaction kettle and filter the solution with suction; obtain a filter cake;

[0021] 4. The filter cake was washed with water, dried and pulverized to obtain 35.75 g of 2,2'-dithiodibenzothiazole.

[0022] 5. Tested by GB11408-89 method, the purity is >90%, and the yield is 71.5.5%. ...

Embodiment 3

[0024] 1. Weigh 50 grams of crude 2-mercaptobenzothiazole and add it to the container, add 450 grams of 40% ammonia and 500 grams of water, heat the container to 55 ° C, and stir during the heating process to make the 2-thiol The base benzothiazole is fully dissolved in the solution;

[0025] 2. After the ammonium salt solution of 2-mercaptobenzothiazole is left to stand at room temperature, it is filtered and added to the reactor, and 1.95 grams of catalyst manganese acetate is added in a ratio of 0.15% by weight, and air is introduced to make the raw material undergo redox reaction. Keep the container pressure at 0.8MPa, the reaction temperature of the reactor is 80°C; the reaction time is 60min,

[0026] 3. After the reaction, the reaction kettle was opened, and the solution was suction-filtered; the filter cake was obtained, which was washed, dried, and pulverized to obtain 29.85 grams of the target product 2,2'-dithiodibenzothiazole.

[0027] 4. Tested by the GB11408-89 ...

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Abstract

A method of preparing the 2, 2'-dithiocarbamate dibenzo thiazole based on the oxygen method of the 2-mercaptan benzothiazole ammonia salt is characterized in that the 2-mercaptan benzothiazole is added with ammonia or a compound for the dissolution reaction; the compound can produce the ammonia with the existence of water; in the dissolution process, the solution is heated and stirred; the solution of the ammonia salt is filtered after the dissolution; the catalyst is added; the air or oxygen is added under the condition with a certain temperature and pressure for the reaction of a certain period; the suspension produced after the reaction is pumped and filtered to get the filter cake; the filter cake is washes by water, dried and cracked to get the product 2, 2'-dithiocarbamate dibenzo thiazole; the filtered solution after being pumped and filtered and water for the washing process can return to the container to be used as the solvent for the cycling use after being supplemented with ammonia. The method has no wastewater and exhaust emission in the whole production process.

Description

Technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a new process for preparing 2,2'-dithiodibenzothiazole by an oxygen method using 2-mercaptobenzothiazole as a raw material. Background technique [0002] 2,2′-Dithiodibenzothiazole is used as an accelerator in a wide range of industrial production at present, and its production methods are also varied, and most of the commonly used production methods are divided into two steps. The first step: first refine the crude product 2-mercaptobenzothiazole as a raw material. The second step: reacting refined 2-mercaptobenzothiazole with an oxidizing agent to synthesize 2,2'-dithiodibenzothiazole. At present, the preparation of 2-mercaptobenzothiazole in industrial production generally adopts aniline, CS 2 , Sulfur as raw material, in the direct reaction under high pressure. This method produces 2-mercaptobenzothiazole with a purity of about 85%. In order to improve its puri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D333/62
Inventor 黎振球徐程秋潘鹏勇吕桂中赵新远沙德昌殷树梅宋鑫宋玉叶黄彩霞李敬华
Owner QINGDAO UNIV OF SCI & TECH
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