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Preparation method of 2-pentylthiuram hexasulfide

A technology based on thiuram VI and sulfide, applied in the direction of organic chemistry, can solve the problems of direct discarding of waste liquid, inability to use water directly, and high corrosion of metals, etc., and achieve the effect of improving product yield

Active Publication Date: 2022-07-05
HEBI YUANHAO CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, piperidine, sulfur and water are generally mixed uniformly, and then carbon disulfide and hydrogen peroxide are added dropwise to prepare secondary amylthiuram hexasulfide. The violent reaction is not easy to control, resulting in low yield, low purity, high free sulfur, and water cannot be used directly, which brings great pressure to environmental protection, and the rubber and plastic products produced are relatively corrosive to metals.
[0004] Patent CN1944504A records the production method of rubber vulcanization accelerator dipentamethylenethiuram tetrasulfide, adopts piperidine, sulfur, carbon disulfide, hydrogen peroxide in non-reactive medium Carry out the reaction to obtain bispentamethylenethiuram tetrasulfide. The product yield obtained by this method is low, the reaction is difficult to carry out and the waste liquid is directly discarded, which pollutes the environment; a rubber vulcanization accelerator recorded in the patent CN100558707C The preparation method of bispentamethylenethiuram tetrasulfide is to use water as the reaction medium, and piperidine, sulfur, carbon disulfide and hydrogen peroxide react in the medium to prepare bispentamethylenethiuram tetrasulfide. The product yield that obtains is low, and waste water is difficult to handle, and brings great pressure to environmental protection; The preparation method of the rubber vulcanization accelerator DPTT-6 that patent CN108148018A records, is to be reaction medium with low-carbon chain alcohol, piperidine, sulfur, Carbon disulfide and hydrogen peroxide react in the medium to produce accelerator DPTT-6. The product produced by this method has solvent residues, and VOC cannot reach the standard in the production process, so it is difficult to realize industrialized continuous production; a kind of Qiulan disclosed in patent US5015752A The production process of mudosulfide is to react in an autoclave with oxygen or oxygen-containing gas in an organic solvent such as methanol, piperidine, sulfur, and carbon disulfide under the action of manganese acetate and triethylamine, at 50°C Synthesize secondary pentylthiuram hexasulfide at a temperature of 60°C. The free sulfur content of the product produced by this method is less than 1%, but there are solvent and catalyst residues in the product, and the requirements for equipment are high, and the three wastes are polluted Serious, not suitable for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] At room temperature, first add 24.58g carbon disulfide and 19.34g sulfur into a 500ml flask and mix evenly, then add 0.13g sodium octadecyl sulfate and 100g water, and stir evenly; secondly, control the temperature to 20-30°C and dropwise add 25g piperidine and 50g The mixture of water was added dropwise for 3 hours; then 24.29 g of hydrogen peroxide was slowly added dropwise at 10 to 15 °C for 6 hours; after the dropwise addition, the temperature was raised to 75 to 95 °C, and the reaction was kept for 4 hours; The circulating water was cooled to 30℃~40℃, and the solid-liquid separation, drying and pulverization were carried out to obtain 64.12g of diamylthiuram hexasulfide;

[0021] The chromatographic detection showed that the product yield was 97.82%, the purity was 98.94%, the initial melting point was 115.9°C, and the free S% was 0.41%.

Embodiment 2

[0023] At room temperature, first add 34.41g of carbon disulfide and 27.08g of sulfur into a 500ml flask and mix evenly, then add 0.18g of sodium octadecyl sulfate and 140g of mother liquor, and stir evenly; secondly, control the temperature to 20-30°C and dropwise add 35g of piperidine and 70g of The mixture of water was added dropwise for 3 hours; then 34.01 g of hydrogen peroxide was slowly added dropwise at 10 to 15 °C for 6 hours; after the dropwise addition, the temperature was raised to 75 to 95 °C, and the reaction was kept for 4 hours; The circulating water was cooled to 30℃~40℃, and the solid-liquid separation, drying and pulverization were carried out to obtain 89.96g of diamylthiuram hexasulfide;

[0024] The chromatographic detection showed that the product yield was 98.03%, the purity was 98.69%, the initial melting point was 116.2°C, and the free sulfur was 0.48%.

Embodiment 3

[0026] At room temperature, first add 49.15g carbon disulfide and 38.68g sulfur into a 1000ml flask and mix evenly, then add 0.25g sodium octadecyl sulfate and 200g water, and stir well; then control the temperature to 20-30°C and add dropwise 50g piperidine and 100g The mixture of water was added dropwise for 3 hours; then 48.57 g of hydrogen peroxide was slowly added dropwise at 10 to 15 °C for 6 hours; after the dropwise addition, the temperature was raised to 75 to 95 °C, and the reaction was kept for 4 hours; The circulating water was cooled to 30℃~40℃, and the solid-liquid separation, drying and pulverization were carried out to obtain 129.88g of diamylthiuram hexasulfide;

[0027] After chromatographic detection, the product yield was 98.67%, the purity was 99.13%, the initial melting point was 116.8°C, and the free sulfur content was 0.46%.

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Abstract

The invention provides a preparation method of secondary amylthiuram hexapulfide, which comprises the following steps: uniformly mixing carbon disulfide, sulfur, water and a surfactant, controlling the temperature to be 20-30 DEG C, dropwise adding a mixture of piperidine and water, slowly dropwise adding hydrogen peroxide at 10-15 DEG C, controlling the temperature to be 75-95 DEG C after dropwise adding is finished, reacting for 3-5 hours, and after the reaction is finished, filtering, washing and drying to obtain the secondary amylthiuram hexapulfide. Carrying out solid-liquid separation, drying and crushing to obtain secondary amyl thiuram hexasulfide; the preparation method takes water as a medium, has the advantages of high operation safety, no organic solvent residue in the product, high yield, high purity, low free sulfur content, recycling of mother liquor and the like, and can realize clean preparation of the secondary amylthiuram hexasulfide without emission of three wastes.

Description

technical field [0001] The invention belongs to the field of rubber-plastic foaming material auxiliaries synthesis, in particular to a preparation method of diamylthiuram hexasulfide. Background technique [0002] The emergence of rubber-plastic foam materials has solved the industrial pursuit of lightweight and high performance of rubber materials. Rubber-plastic foam materials have excellent chemical stability, good electrical insulation performance, aging resistance and waterproof performance. , Widely used in sporting goods, various types of construction and refrigeration, air conditioning, auto parts, medicine, military equipment and other fields. Therefore, rubber and plastic foaming materials have become indispensable fine chemicals; diamylthiuram hexasulfide is widely used as a vulcanization accelerator in the field of rubber and plastic foaming materials, because it can be used in a wide range of temperature. Use, it is easy to vulcanize and shape the rubber, and t...

Claims

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Application Information

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IPC IPC(8): C07D295/21
CPCC07D295/21Y02E60/10
Inventor 李合平赵小锋杨瑞朝侯万喜马晓光宋士杰董海娜焦瑞艳杨利琴
Owner HEBI YUANHAO CHEM CO LTD