Method for producing tetramethylthiuram disulfide (TMTD) by methanol method

A methanol method and methanol technology, applied in the field of methanol production of TMTD, can solve the problems of poor product quality, environmental pollution, short shelf life, etc., and achieve the effects of low cost, no raw material loss, and long shelf life.

Inactive Publication Date: 2013-06-26
DONGGANG LONGXIANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The production of existing TMTD is usually liquid caustic soda method, with low purity, low melting point, poor product quality; short shelf life; using liquid caustic soda as reaction raw material, which pollutes the environment; high cost

Method used

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  • Method for producing tetramethylthiuram disulfide (TMTD) by methanol method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In a pressure reactor (autoclave), put 150 kg of methanol, 550 kg of dimethylamine aqueous solution with a mass concentration of 40% and 350 kg of carbon disulfide, and oxygen at room temperature to a gauge pressure of 0.08Mpa, and react at 25-28℃6 Hours; cooling to below 26℃, discharge the materials in the reaction kettle, suction filtration or centrifugation, the solid is vibrated and dried at 80℃, and discharged in about 60 seconds to obtain a white or off-white product with a yield of 92-96% and a purity of 98.5% Above, the melting point is 142-145.7; the filtrate is distilled to separate methanol for recycling in the next production.

Embodiment 2

[0020] In a pressure reactor (autoclave), put 300 kg of methanol, 1100 kg of dimethylamine aqueous solution with a mass concentration of 40% and 700 kg of carbon disulfide, and oxygen at 50°C to a gauge pressure of 0.1Mpa, and react at 25-28°C 6 hours; cooling to below 26℃, discharge the materials in the reactor, suction filtration or centrifugation, shake and dry the solid at 80℃, discharge in about 60 seconds, obtain a white or off-white product, yield 92-96%, purity 98.5 % Above, the melting point is 142-145.7; the filtrate is distilled to separate methanol for recycling in the next production.

Embodiment 3

[0022] In a pressure reactor (autoclave), put 150 kg of methanol, 500 kg of dimethylamine aqueous solution with a mass concentration of 40% and 300 kg of carbon disulfide, and oxygen at 50°C to a gauge pressure of 0.2Mpa, and react at 25-28°C 5 hours; cooling to below 26℃, discharge the materials in the reaction kettle, suction filtration or centrifugation, the solid is vibrated and dried at 80℃, and discharged in about 60 seconds, a white or off-white product is obtained, the yield is 92-96%, the purity is 98.5 % Above, the melting point is 142-145.7; the filtrate is distilled to separate methanol for recycling in the next production.

[0023] Benefits:

[0024] The product produced by the present invention meets the national inspection standards, and the indicators of the product in Example 1 are

[0025]

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PUM

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Abstract

The invention relates to production of tetramethylthiuram disulfide (TMTD), and particularly relates to a method for producing TMTD by a methanol method. Methanol is used as the solvent without pollution discharge, the solvent of methanol can be recycled, residue can be used as a fuel to be applied to a distillation and drying process, materials are fully utilized, a liquid caustic soda process is not used, the energy consumption, the cost are low, material loss is avoided, and the purity, the melting point and the quality of the product are high; and the guarantee period is long, the purity declines by only 0.2% after TMTD is stored for 2 years at normal temperature, while the purity of TMTD produced by a liquid caustic soda method declines by 2%.

Description

Technical field [0001] The invention relates to the production of TMTD, in particular to a method for producing TMTD by methanol method. Background technique [0002] Rubber accelerator (vulcanization accelerator) TMTD, as a super accelerator for natural rubber, synthetic rubber and latex, is the representative of thiuram vulcanization accelerator, chemical name: tetramethylthiuram disulfide, C6H12N2S4; white to off-white Powder (granule) with a relative density of 1.29. It is soluble in benzene, acetone, chloroform, carbon disulfide, slightly soluble in ethanol, ether, carbon tetrachloride, and insoluble in water, gasoline or dilute alkali. Heated with water to generate dimethylamine And carbon disulfide. Irritating to respiratory tract and skin. Used as a super-vulcanization accelerator in the rubber industry, it is often used in combination with thiazole accelerators, and it can also be used in combination with other accelerators as an accelerator for continuous rubber compo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C333/32
Inventor 黄炳琛黄树生韩淑琴李喜荣潘凤楼
Owner DONGGANG LONGXIANG CHEM
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