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Method for preparing isopropyl mercaptan

A technology of isopropyl mercaptan and isothiourea salt, which is applied in the directions of mercaptan preparation, chemical instruments and methods, organic compound/hydride/coordination complex catalyst, etc., can solve the problem of high product cost, complicated operation, unsuitable industrial-scale production applications, etc., to achieve the effects of industrialized production, mild reaction conditions, and excellent mechanical strength

Inactive Publication Date: 2010-05-12
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is in short supply of propylene raw materials, and has poor selectivity to isopropyl mercaptan, high product cost, low yield, and pollutes the environment; (2) acetone reacts with CoS and hydrogen under the action of a catalyst to generate isopropyl mercaptan, with a yield of 58% %[Journal of Industrial and Engineering Chemistry[Washington, D.C., 1950, 42, 2547-9]; (3) 2-bromopropane and hydrogen sulfide undergo a heterogeneous catalytic substitution reaction in ethanol under high pressure, high temperature and catalyst conditions, isopropyl mercaptan
[0003] In comparison, the gas phase method is limited to its own defects, such as high pressure requirements, strict requirements on equipment materials, difficult process, high cost, low yield, and environmental pollution.
The liquid phase method, or the required raw materials are expensive, or the operation is complicated, or the product yield is low, and it is not suitable for industrial scale production applications.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] In the reaction system, add 2-bromopropane 0.2mol, thiourea 0.24mol, the molar ratio of the two is 1: 1.2, add 2.46g supported CTAB / MCM-41 catalyst, the mass percent of 2-bromopropane and catalyst is 100: 10. Triethylene glycol 25mL, under normal pressure, reaction temperature 50°C, react for 7h, then pass nitrogen gas to remove unreacted 2-bromopropane, then add 18.93mL tetraethylenepentamine with a boiling point of 340°C for cracking, and at the same time Distillation in isopropyl mercaptan. The yield of isopropyl mercaptan can reach 85%, and the purity reaches 99.4%. The mother liquor is filtered to separate the catalyst, and the filtrate is distilled under reduced pressure to separate the organic solvent triethylene glycol, and the solvent and the catalyst are recycled; the non-volatile guanidinium salt is used as a product through further separation and purification, or as a product by adding ammonia water. Nitrogen fertilization.

Embodiment 2

[0023] In the reaction system, add 1mol of 2-bromopropane, 1.1mol of thiourea, the molar ratio of the two is 1:1.1, add 9.84g of supported CTAB / MCM-41 catalyst, the mass percentage of 2-bromopropane and catalyst is 100:8 , diethylene glycol 250mL, under normal pressure, reaction temperature 65°C, react for 5h, then pass nitrogen gas to remove unreacted 2-bromopropane, then add tetraethylenepentamine 94.65mL with a boiling point of 340°C for cracking, normal pressure Distillation in isopropyl mercaptan. Isopropyl mercaptan yield can reach 82%, and purity reaches 99.6%, and other is with embodiment 1.

Embodiment 3

[0025] In the reaction system, add 2-bromopropane 0.2mol, thiourea 0.26mol, the molar ratio of the two is 1: 1.3, add 1.48g supported CTAB / MCM-41 catalyst, the mass percent of 2-bromopropane and catalyst is 100: 6. Ethylene glycol 30mL, under normal pressure, reaction temperature 60°C, react for 6h, then blow nitrogen to remove unreacted 2-bromopropane, then add 21.62mL of diethylenetriamine with a boiling point of 206.7°C for cracking, and distill under normal pressure to obtain Isopropylthiol. Isopropyl mercaptan yield can reach 79%, and purity reaches 99.2%, and others are with embodiment 1.

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Abstract

The invention relates to the technical field of fine chemical synthesis and discloses a novel isopropyl mercaptan synthesizing method. 2-bromine propane and thiourea are taken as main raw materials, and a mesoporous molecular sieve material is taken as a carrier, is subjected to surface chemical modification and is loaded with proper quaternary ammonium salt with a chain group structure serving as a phase transfer catalyst, and the method comprises the following steps of: reacting main raw materials in the presence of the catalyst for 3 to 10 hours in an organic solvent at the temperature between 30 and 70 DEG C under normal pressure to generate an intermediate S-alkyl isothiourea salt; then introducing nitrogen to remove the unreacted 2-bromine propane; carrying out cracking reaction on high boiling point organic amine and the intermediate S-alkyl isothiourea salt; and carrying out distillation under normal pressure to obtain the isopropyl mercaptan. Compared with the current method,the novel method has the advantages of accessible raw materials, mild reaction conditions, simple technological process, short process flow, high catalyst activity, good selectivity, easy recovery from a reaction system and recycling, high product purity, high yield, easy separation of products and the like, is favorable for saving energy, reducing investment, lightening pollution and the like and has better application prospect.

Description

technical field [0001] The invention belongs to the technical field of synthesis of fine chemicals, and relates to a synthesis method of mercaptan compounds, in particular to a preparation method of low-carbon isopropyl mercaptan. Background technique [0002] At present, the synthesis methods of isopropyl mercaptan mainly include liquid phase method and gas phase method. (1) Liquid-phase method: the platinum-manganese compound of ethylene sulfide is reacted with HCl in toluene to generate isopropyl mercaptan, and the yield is 72% [Journal of the American Chemical Society, 2000, 122(1): 170-171] , but the raw material of this reaction is relatively rare and expensive, and can only be obtained in a specific reaction process, and the reaction condition requirements are high, and the reaction process is complicated; 1987, 1(3), 274-279], but this kind of method is because raw material is rare, and no one uses now; (3) 2-bromopropane reacts with sodium and sodium sulfide in sul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C321/04C07C319/02B01J31/02
Inventor 李华章亚东郭峰朱江赵蕾
Owner ZHENGZHOU UNIV