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Synthetic technology for sulfurized isobutylene through vapor phase method and device thereof

A technology of sulfurized isobutylene and synthesis process, which is applied in the direction of organic chemistry, which can solve the problems of ineffective recycling of waste gas and waste residue, low reaction conversion rate, and serious environmental pollution, and achieve low production cost, good economic benefits, and high reaction rate. high effect

Inactive Publication Date: 2012-06-27
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since the catalyst of the liquid phase method is added to the reaction system in the form of an aqueous solution, the organic phase of sulfurized isobutylene needs to go through three steps of liquid separation, water washing and distillation dehydration, and the liquid phase method produces a large amount of inorganic phase waste liquid, which pollutes the environment. More serious, high processing costs
Since the liquid phase method is carried out in a tank reactor, there are technical defects such as low concentration of reactants, long reaction time and low production capacity
The reaction conversion rate of the liquid phase method is not high, the side reaction is severe, and a large amount of waste gas and waste residue generated during the reaction cannot be effectively recycled, and there are technical problems

Method used

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  • Synthetic technology for sulfurized isobutylene through vapor phase method and device thereof
  • Synthetic technology for sulfurized isobutylene through vapor phase method and device thereof
  • Synthetic technology for sulfurized isobutylene through vapor phase method and device thereof

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Experimental program
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Effect test

Embodiment 1

[0033] 1) 4 kg of sulfur (i.e. 125 mol of elemental sulfur) and 125 mol of ammonia gas were stirred and mixed for 20 minutes at 450 ° C and 3 MPa to obtain a mixed gas phase stream;

[0034] 2) Feed 100 mol of isobutene gas (the flow rate of isobutene gas is 60mL / min) and mix with the mixed gas phase stream obtained in step 1) to form a gas phase mixture and enter the reactor to react at 460°C and 2MPa for 15min to obtain a reaction product;

[0035] 3) Cool the reaction product obtained in step 2) to 30°C and perform gas-liquid separation. The liquid phase is filtered to obtain 8.1 kg of sulfurized isobutylene product; the gas phase is washed with tail gas to recover the catalyst, and the recovered catalyst is recycled to step 1) for reuse .

Embodiment 2

[0037] 1) Stir and mix 100 g of sulfur (3.125 mol of elemental sulfur) and 1.7 mol of diethylamine at 460° C. and 4 MPa for 10 minutes to obtain a mixed gas phase stream;

[0038] 2) Feed 5 mol of isobutene gas (the flow rate of isobutene gas is 1.5mL / min) and mix with the mixed gas phase stream obtained in step 1) to form a gas phase mixture and enter the reactor to react at 490°C and 3MPa for 12min to obtain the reaction product ;

[0039] 3) Cool the reaction product obtained in step 2) to 40° C. and then perform gas-liquid separation. The liquid phase is filtered to obtain 210 mL of sulfurized isobutylene product; the gas phase is washed with tail gas to recover the catalyst, and the recovered catalyst is recycled to step 1) for reuse.

Embodiment 3

[0041] 1) Stir and mix 100 g of sulfur (ie, 3.125 mol of elemental sulfur) and 3 mol of monomethylamine at 500° C. and 5 MPa for 15 minutes to obtain a mixed gas phase stream;

[0042] 2) Feed 5 mol of isobutene gas (the flow rate of isobutene gas is 1.5mL / min) and mix with the mixed gas phase stream obtained in step 1) to form a gas phase mixture and enter the reactor to react at 450°C and 4MPa for 15min to obtain the reaction product ;

[0043] 3) Cool the reaction product obtained in step 2) to 35° C. and then perform gas-liquid separation. The liquid phase is filtered to obtain 205 mL of sulfurized isobutylene product; the gas phase is washed with tail gas to recover the catalyst, and the recovered catalyst is recycled to step 1) for reuse.

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Abstract

The invention discloses a synthetic technology for sulfurized isobutylene through a vapor phase method. The technology comprises the following steps: 1, stir-mixing elemental sulfur and a catalyst for 10-20min under conditions that the temperature is 450-500DEG C and the pressure is 3-10MPa to obtain a mixed vapor phase material flow; 2, inletting an isobutene gas to mix the isobutene gas with the mixed vapor phase material flow to form a vapor phase mixture, allowing the vapor phase mixture to enter a reactor, and reacting for 10-20min under conditions that the temperature is 450-500DEG C and the pressure is 2-9MPa to obtain reaction products; and 3, cooling the reaction products, carrying out gas-liquid separation, and filtering the obtained liquid phase to obtain sulfurized isobutylene. The synthetic technology of the invention has the advantages of high reaction rate, high yield, simple process, low production cost, less pollution and the like. The invention provides a synthetic device for sulfurized isobutylene through the vapor phase method, the synthetic technology for sulfurized isobutylene through the vapor phase method is realized through the device, and the device whichhas the advantages of industrialized production benefiting and high production capacity has good economic benefits and a wide application prospect.

Description

technical field [0001] The invention relates to the field of preparation of sulfurized isobutylene, in particular to a synthesis process and device of gas-phase method sulfurized isobutylene. Background technique [0002] The industrial use of sulfurized isobutylene (referred to as sulfene) includes two aspects. On the one hand, it can be used as a pre-sulfurizing agent for hydrogenation catalysts, and sulfurized isobutylene can be used as an efficient organic vulcanizing agent to improve the activity and stability of hydrogenation catalysts; On the other hand, it can be used as lubricating oil additive, because sulfurized isobutylene has excellent anti-wear effect under extreme pressure, which can increase the performance of lubricating oil. In recent years, with the rapid development of industries such as catalysts and lubricating oils, the demand and production capacity of sulfurized isobutylene continue to increase worldwide. [0003] At present, the industrial producti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D341/00
Inventor 蒋斌波陈楠阳永荣王靖岱黄正梁廖祖维郑海俊王宇良赵伟浩
Owner ZHEJIANG UNIV
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