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Method for continuous production of sulphur chlorination isobutene

A technology for chlorinating isobutene and isobutene by sulfur, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry and other directions, can solve the problems of dark product color, complicated process and reduced yield, and saves process steps and processes. Simple process and light-colored product

Inactive Publication Date: 2009-06-24
陆晓
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] All above-mentioned methods all have following problems: 1, technological process is complicated, loaded down with trivial details; 2, adopt intermittent operation, product quality can not be guaranteed; 3, addition reaction is exothermic reaction, and reaction temperature should not be controlled, and temperature is too high, and product color is dark , the yield decreases

Method used

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  • Method for continuous production of sulphur chlorination isobutene

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The inner diameter of the cracking reactor is φ37mm, the height of the reaction catalyst bed is 1200mm, and 1600 milliliters of cracking catalyst is installed inside. The cracking catalyst is an acidic cation exchange resin (produced by Dandong Mingzhu Special Resin Co., Ltd., DWN).

[0027] The isobutylene recovery tower has an inner diameter of φ14mm, a packing of φ3mm inside, and a filling height of 35mm.

[0028] The sulfur chlorination reactor has an inner diameter of φ39mm, the reaction catalyst is Lewis acid, and the reactor is filled with 3500 grams of inert packing.

[0029] Firstly, the MTBE cracking reaction is carried out in the cracking reactor, and the reaction is carried out under the conditions of pressure 0.5MPa and temperature 155°C, and the MTBE feeding space velocity is 4h -1 The reacted mixture enters the isobutene recovery tower with an operating pressure of 0.4 MPa, a tower top temperature of 39° C. and a reflux ratio of 0.8. From the top of the ...

Embodiment 2

[0032] Operating equipment is the same as embodiment 1

[0033] Firstly, the MTBE cleavage reaction is carried out in the cleavage reactor. The reaction was carried out at a pressure of 0.30 MPa and a temperature of 180° C., and the MTBE feed rate was 5500 g / hour.

[0034] The reacted mixture enters the isobutene recovery tower with an operating pressure of 0.6 MPa, a tower top temperature of 40°C, and a reflux ratio of 1.8. 3445.1 grams of isobutene, 22.2 grams of MTBE and 31.0 grams of methanol can be obtained per hour from the top of the tower.

[0035] The obtained isobutylene enters from the bottom of the sulfur chlorination synthesis tower, and enters sulfur monochloride from the upper part of the synthesis tower at 3250 grams per hour. The reaction temperature was 40°C, and the obtained liquid mixture of sulfur-chlorinated isobutylene was 6062.3 g / hour, with a density of 1.16 and a sulfur content of 43.9%.

Embodiment 3

[0037] Operating equipment is the same as embodiment 1

[0038] Firstly, the MTBE cleavage reaction is carried out in the cleavage reactor. The reaction was carried out at a pressure of 0.60 MPa and a temperature of 120° C., and the feed rate of MTBE (96.88w%) was 6500 g / hour.

[0039] The reacted mixture enters the isobutene recovery tower with an operating pressure of 0.30 MPa, a tower top temperature of 40°C, and a reflux ratio of 1.6. 4075.5 grams of isobutene, 10.2 grams of MTBE and 19.7 grams of methanol can be obtained per hour from the top of the tower.

[0040] The obtained isobutylene enters from the bottom of the sulfur chlorination synthesis tower, and enters sulfur monochloride from the upper part of the synthesis tower at 3300 g / h. The reaction temperature was 40°C, and the obtained orange-yellow sulfur-chlorinated isobutylene liquid mixture was 6089.7 g / hour, with a density of 1.14 and a sulfur content of 42.2%.

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Abstract

The invention relates to a method for producing sulfur chloride isobutene continuously. Firstly, MTBE is cracked into isobutene and methanol substance under the action of acid catalyst; the reaction pressure is 0.1-1.0MPa, the temperature is 120-185 DEG C, and the feeding weight airspeed of the raw material MTBE is 1-10h<-1>; the generated isobutene is separated in a distilling tower to obtain isobutene mixture containing a little bit methanol by the separation; the operation pressure is 0.2-1.0Pa, and the reflux ratio is 0.3-3.0; the isobutene mixture enters into a sulfuration reactor to react with sulfur monochloride to generate the sulfur chloride isobutene at the temperature of 20-50 DEG C; the isobutene feeding volume airspeed is 0.5-5h<-1>; the feeding weight ratio of the isobutene and the sulfur monochloride is 1:0.8-1.2; and the technical steps are carried out continuously. The invention has simple technical process, saves the technical steps and ensures that the reaction is carried out continuously; and a product has light color, good quality and high yield.

Description

technical field [0001] The present invention relates to the preparation method of sulfur-chlorinated isobutylene, in particular to the process of preparing sulfur-chlorinated isobutylene by reacting methyl tert-butyl ether (MTBE) and sulfur monochloride. Background technique [0002] In order to improve the application performance of lubricating oil, it is often necessary to add additives with different functions to reduce friction and wear and prevent sintering. These additives are called extreme pressure antiwear agents. Sulfurized olefins are currently the most widely used extreme pressure and antiwear agents, and can be used as extreme pressure agents for cutting oils, gear oils, hydraulic oils, and metal processing oils. This kind of sulfide has good stability, high extreme pressure and light color, and has been widely used. [0003] Extreme pressure and antiwear agents are generally C 3 ~C 8 Sulfurized olefins can be prepared directly or indirectly under the action ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/00C07C319/00C10M135/22C10N30/06
Inventor 陆晓朱书魁刘中民许磊吕志辉孙新德
Owner 陆晓
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