Preparation method of thiofide TiBTM (Tetraisobutylethiuram Monosulfide)

A technology of tetraisobutylthiuram and rubber vulcanization, which is applied in the direction of organic chemistry, can solve the problems of non-compliance with national environmental protection policies and energy-saving production requirements, difficulty in achieving "green and clean" production, and difficulty in meeting high-end requirements, and achieve reduction Fixed asset investment, superior vulcanization performance, and short vulcanization time

Active Publication Date: 2011-04-27
WILLING NEW MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the production process of this process, the synthesis process is lengthy, the operation is complicated, the amount of waste gas and waste water produced is large, the equipment is severely corroded, the energy consumption of the reaction is high, and what is more serious is the safety hazard, which brings great difficulties to environmental protection. , it is difficult to achieve "green and clean" production, does not meet the national environmental protection policy and energy-saving production requirements, and the product has a low melting point, dull appearance, and low yield, which is difficult to meet the high-end requirements of domestic and foreign sales markets

Method used

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  • Preparation method of thiofide TiBTM (Tetraisobutylethiuram Monosulfide)

Examples

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Embodiment 1

[0027] The used raw material of the present invention is diisobutylamine, carbon disulfide, hydrogen peroxide, sodium cyanide; The stoichiometric molar ratio of raw material is: diisobutylamine: carbon disulfide: hydrogen peroxide: sodium cyanide=1: 1.1: 0.52: 0.50

[0028] The process is as follows: add a certain amount of diisobutylamine to the reaction kettle containing 100ml of methanol with a mass percentage of 70%, and the stirrer rotates at a speed of 400 rpm; control the temperature at 15°C, and add carbon disulfide dropwise at a uniform speed Liquid and hydrogen peroxide, in which carbon disulfide drops slightly earlier than hydrogen peroxide, carry out condensation reaction and oxidation reaction, control the reaction time for 4 hours; react to pH value 7, put in NaCN, control the reaction temperature 40 ℃, after the reaction is complete, keep warm for 0.5 h, solid-liquid centrifugal separation; solid drying, crushing, sieving, and packaging. It was determined that t...

Embodiment 2

[0030] The used raw material of the present invention is diisobutylamine, carbon disulfide, hydrogen peroxide, sodium cyanide; The stoichiometric molar ratio of raw material is: diisobutylamine: carbon disulfide: hydrogen peroxide: sodium cyanide=1: 1.3: 0.60: 0.60

[0031] The process is as follows: add a certain amount of diisobutylamine to the reaction kettle containing 150ml of ethanol with a mass percentage of 72%, and the stirrer rotates at 800 rpm; control the temperature at 35°C, and dropwise add The required carbon disulfide liquid and hydrogen peroxide, in which carbon disulfide is dropped slightly earlier than hydrogen peroxide, carry out condensation and oxidation reactions, and control the reaction time for 6 hours; react to a pH value of 8, put in NaCN, control the reaction temperature at 50 ° C, after the reaction is complete , keep warm for 1.5h, and carry out solid-liquid centrifugation; solid drying, crushing, sieving, and packaging. After determination, the ...

Embodiment 3

[0033] The used raw material of the present invention is diisobutylamine, carbon disulfide, hydrogen peroxide, sodium cyanide; The stoichiometric molar ratio of raw material is: diisobutylamine: carbon disulfide: hydrogen peroxide: sodium cyanide=1: 1.2: 0.56: 0.52

[0034]The process is as follows: add a certain amount of diisobutylamine sequentially to a reaction kettle filled with 180ml of isopropanol with a mass percentage of 75%, and the stirrer rotates at 1200 rpm; control the temperature at 28°C, and drop Add the required carbon disulfide liquid and hydrogen peroxide, wherein the carbon disulfide drops slightly earlier than the hydrogen peroxide, carry out the condensation and oxidation reaction, control the reaction time for 5 hours; react to a pH value of 7.6, put in NaCN, control the reaction temperature at 45°C, and the reaction is complete Afterwards, keep warm for 1.0h, and carry out solid-liquid centrifugation; the solid can be dried, pulverized, sieved, and packa...

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Abstract

The invention relates to a preparation method of thiofide TiBTM (Tetraisobutylethiuram Monosulfide). The raw materials include diisobutylamine, carbon disulfide, hydrogen peroxide and sodium cyanide; the raw materials contain the following components according to stoichiometric molar ratio: 1 diisobutylamine, 1.1-1.3 carbon disulfide, 0.50-0.60 hydrogen peroxide and 0.60 sodium cyanide. The specific technique of the preparation method comprises the following steps of sequentially adding an amount of diisobutylamine liquid to a reaction kettle containing 100-200 ml alcohol (methanol, ethanol, isopropyl alcohol and the like) with the mass percentage of 70-80% under the condition that the rotation speed of a stirring device is 200-1200rpm; controlling the temperature within 10-35 DEG C, synchronously dripping the needed carbon disulfide liquid and the hydrogen peroxide, wherein the dripping of the hydrogen peroxide is a little earlier than that of the hydrogen peroxide to carry out condensation and oxidation reactions, and controlling the time of the reactions within 4-6h; reacting till a pH value is within 7 to 8, adding NaCN, and controlling the reaction temperature within 40-50 DEG C; after the reactions are finished, holding the temperature for 0.5-1.5h, and carrying out the solid-liquid centrifugal separation; and drying, crushing, sieving and packing the solid to obtain thethiofide TiBTM.

Description

1. Technical field: [0001] The invention belongs to a preparation method of a rubber vulcanization accelerator, in particular to a production method of a rubber vulcanization accelerator-vulcanized tetraisobutylthiuram. 2. Background technology: [0002] Since the 1980s, my country's rubber additives industry has developed continuously, stably and healthily, and its annual output has increased from 12,000 tons in 1980 to 620,000 tons in 2009, especially during the "Eleventh Five-Year Plan" period. , The rapid development of the domestic automobile industry and communication industry has driven the accelerated growth of the rubber processing industry and provided an unprecedented good opportunity for the development of the rubber additives industry. However, although the production of rubber accelerators in my country has been greatly improved, compared with developed countries in the world, there is still a big gap in product intrinsic quality and "green" environmental protec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C333/20
Inventor 王志强郭同新王平生岳法亮史宗浩徐治松王飞
Owner WILLING NEW MATERIALS TECH CO LTD
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