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A kind of preparation method of isopropyl mercaptan

A technology of isopropyl mercaptan and propylene, which is applied in the field of preparation of isopropyl mercaptan, can solve the problems of high equipment requirements, low yield of isopropyl mercaptan, difficult processing, etc., and achieve comprehensive utilization of resources and easy industrial transformation , the effect of preventing environmental pollution

Active Publication Date: 2016-07-20
SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0004] 1) The alcoholic solution of sodium hydrosulfide (potassium) reacts with 2-bromopropane, and this method easily has by-product isopropyl sulfide to generate;
[0005] 2) 2-bromopropane reacted with thiourea in ethanol solution for 4 hours, and distilled off the ethanol to obtain S-isopropyl isothiourea salt. The salt was hydrolyzed in alkali solution, and then acidified to obtain isopropyl mercaptan , the method is complicated to operate;
[0006] Above two kinds of methods all adopt intermittent operation, and mercaptan volatilizes in the air during operation, and smell is unpleasant, pollutes environment, is the method for laboratory preparation a small amount of isopropyl mercaptans, is difficult to realize suitability for industrialization, simultaneously the isopropyl mercaptan of these two kinds of methods The yield of propanethiol is not high (about 81%)
[0007] 3) Isopropyl alcohol and hydrogen sulfide are catalyzed to synthesize isopropyl mercaptan with modified alumina as a catalyst. During the reaction process, water is generated, and the generated water and unreacted hydrogen sulfide form a strong corrosive fluid, which has extremely high requirements for equipment anti-corrosion. High, at the same time generate wastewater containing mercaptans and sulfides, which is difficult to treat
[0008] 4) Propylene and hydrogen sulfide use plasma method to prepare isopropyl mercaptan. Relevant patents point out that propylene and hydrogen sulfide can be used to prepare isopropyl mercaptan in a plasma reaction chamber. This reaction process requires the use of special equipment such as a plasma reaction chamber , while using the plasma electric field to generate high-energy state electrons, which is difficult to industrialize
"Synthesis of isopropyl mercaptan by sodium hydrosulfide method and basic theoretical research" mentioned that "at present, the industrial methods for synthesizing isopropyl mercaptan in foreign countries mainly include the substitution reaction of isopropanol with hydrogen sulfide under the action of a solid catalyst; the reaction of propylene under the action of a catalyst Addition reaction with hydrogen sulfide, but the water and hydrogen sulfide generated by this method form a strong corrosive fluid, which requires high equipment, difficult process and high cost
In addition, the related patents also mentioned the report on the synthesis of isopropyl mercaptan from propylene and hydrogen sulfide. The method used in this technology is the plasma method, which requires the use of special equipment such as a plasma reaction chamber, and at the same time uses the plasma electric field Generate high-energy state electrons, which are difficult to industrialize

Method used

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  • A kind of preparation method of isopropyl mercaptan
  • A kind of preparation method of isopropyl mercaptan
  • A kind of preparation method of isopropyl mercaptan

Examples

Experimental program
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Embodiment 1

[0053] Hydrogen sulfide and propylene are fully mixed at a molar ratio of 1:1, pressurized to 0.2MPa by a compressor, and heated to 160°C by a heating furnace, according to the propylene volume space velocity of 400h -1 , into an adiabatic fixed-bed reactor equipped with a solid acid catalyst for reaction, the catalyst used is composed of 1% molybdenum oxide, 1% cobalt oxide, 5% ZSM-5 molecular sieve, and the rest is alumina carrier , the ZSM-5 molecular sieve has a silicon-aluminum molar ratio of 10, a grain size of 5 μm, a pore volume of 0.4ml / g, and a specific surface area of ​​137m 2 / g. The reaction effluent is cooled to 25°C by heat exchange, the gas phase is returned to the hydrogen sulfide feed, and the liquid phase is fractionated to obtain four products, isopropyl mercaptan, n-propylene mercaptan, isopropyl sulfide and n-propyl sulfide. Among them, the single-pass conversion rate of propylene is 80.2%, the selectivity of isopropyl mercaptan is 89.4%, and the total y...

Embodiment 2

[0058] Hydrogen sulfide and propylene are fully mixed at a molar ratio of 2:1, pressurized to 0.2MPa by a compressor, and heated to 180°C by a heating furnace, according to the propylene volume space velocity of 300h -1 , into an adiabatic fixed-bed reactor equipped with a solid acid catalyst for reaction, the catalyst used is composed of 5% molybdenum oxide, 2% nickel oxide, 2% phosphorus pentoxide, 5% ZSM-5 molecular sieve, and the rest is alumina carrier , the ZSM-5 molecular sieve has a silicon-aluminum ratio of 20, a grain size of 5 μm, a pore volume of 0.3ml / g, and a specific surface area of ​​141m 2 / g. The reaction effluent is cooled to 20°C by heat exchange, the gas phase is returned to the hydrogen sulfide feed, and the liquid phase is subjected to fractional distillation to obtain four products, isopropyl mercaptan, n-propylene mercaptan, isopropyl sulfide and n-propyl sulfide. Wherein the single-pass conversion rate of propylene is 86.3%, the selectivity of isopro...

Embodiment 3

[0063] Hydrogen sulfide and propylene are fully mixed at a molar ratio of 3:1, pressurized to 0.25MPa by a compressor, and heated to 200°C by a heating furnace, according to the propylene volume space velocity of 300h -1 , into an adiabatic fixed-bed reactor equipped with a solid acid catalyst for reaction, the catalyst used is composed of 8% molybdenum oxide, 5% nickel oxide, 4% phosphorus pentoxide, 8% ZSM-5 molecular sieve, and the rest is alumina carrier , the ZSM-5 molecular sieve has a silicon-aluminum ratio of 25, a grain size of 3 μm, a pore volume of 0.5ml / g, and a specific surface area of ​​168m 2 / g. The reaction effluent is cooled to 15°C by heat exchange, the gas phase is returned to the hydrogen sulfide feed, and the liquid phase is subjected to fractional distillation to obtain four products, namely, isopropyl mercaptan, n-propylene mercaptan, isopropyl sulfide and n-propyl sulfide. Wherein the single-pass conversion rate of propylene is 91.8%, the selectivity ...

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Abstract

The invention discloses a method for synthesizing isopropyl mercaptan from propylene and hydrogen sulfide. According to the method, a heat insulation type fixed bed reactor is used and isopropyl mercaptan is synthesized of hydrogen sulfide and propylene in the presence of a solid acid catalyst according to a continuous production process. The method disclosed by the invention has the advantages that the reaction conditions are easy to control, the yield is high, the process is simple, and the environmental pollution is reduced.

Description

technical field [0001] The invention belongs to the field of chemical industry, in particular to a preparation method of isopropyl mercaptan. Background technique [0002] Isopropyl mercaptan is one of the important varieties of low-carbon mercaptan series. It is an important chemical raw material and intermediate. It occupies an important position in the field of synthetic pesticides. The market demand is increasing year by year. At present, my country's isopropyl mercaptan mainly relies on imports. [0003] The synthesis of isopropyl mercaptan can take the following methods: [0004] 1) The alcoholic solution of sodium hydrosulfide (potassium) reacts with 2-bromopropane, and this method easily has by-product isopropyl sulfide to generate; [0005] 2) 2-bromopropane reacted with thiourea in ethanol solution for 4 hours, and distilled off the ethanol to obtain S-isopropyl isothiourea salt. The salt was hydrolyzed in alkali solution, and then acidified to obtain isopropyl me...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C319/04C07C321/04B01J29/48
Inventor 郭振莲姜雪丽李寿丽马欢栾立霞牟庆平张建林
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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