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Synthesizing method of sulfurized-chloridized isobutylene

A technology of sulfochlorination of isobutylene and synthesis method, which is applied in the preparation of hydrogenated polysulfides/polysulfides, organic chemistry, etc., and can solve the problem of increased by-products, difficulty in effectively controlling the amount of air intake, and decomposition of sulfur monochloride, etc. question

Inactive Publication Date: 2018-08-17
SHANDONG HIMILE CHEM TECH
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

The existing gas / vapor-liquid contact reaction will make isobutylene unable to fully react with sulfur monochloride and be discharged into the cavity of the reaction vessel, resulting in a large amount of gas retention, which will not only increase the pressure in the reaction vessel and affect the reaction, but also cause Affect the reaction efficiency and waste a lot of raw materials
Moreover, the reaction process between sulfur monochloride and isobutylene is extremely violent, and a large amount of heat is released during the reaction process. If the air intake cannot be well controlled, the temperature in the reaction vessel will be too high, and the reaction temperature is difficult to be effectively controlled; Sulfur decomposes, the amount of by-products increases, the yield is reduced, and the production cost is increased
In addition, the intake amount of isobutene is difficult to be effectively controlled, which will lead to excessive local temperature in the reaction solution and increase of by-products

Method used

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  • Synthesizing method of sulfurized-chloridized isobutylene

Examples

Experimental program
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Embodiment 1

[0045] A tubular reactor is adopted, the length of the reactor is 1-15m, the inner diameter is 1-6mm, and the temperature is controlled by a cooling and heating machine at 15-30°C. The outlet back pressure of the reaction system is ≥0.3MPa. Isobutene and sulfur monochloride are fed separately through the plunger pump, the feed rate is 5mL / min-3L / min, the molar ratio of isobutene to sulfur monochloride is 1.8:1~2.2:1, and the feed rate is controlled by controlling the pump. The reaction residence time is 0.5-2 hours. Crude chlorinated isobutene sulfide with a content of more than 95% is obtained.

Embodiment 2

[0047] A tubular reactor is adopted, the length of the reactor is 10-80m, the inner diameter is 2-8mm, the temperature is controlled at 20-35°C, the back pressure at the outlet of the reaction system is ≥0.5MPa, isobutylene and sulfur monochloride are respectively fed in liquid state through a plunger pump, and the The feed rate is 5mL / min-5L / min, the molar ratio of isobutene to sulfur monochloride is 1.8:1~2.2:1, and the reaction residence time is 1.0-5 hours. Crude chlorinated isobutene sulfide with a content of more than 95% is obtained.

Embodiment 3

[0049] A microchannel reactor is adopted, and the cross-sectional area of ​​the reactor is the shortest 0.3-2 mm. In this example, the Himile Chemical umbrella microchannel reactor is used. The length of the single-chip channel is 0.5-5 m, and the liquid holding capacity is 1-500 mL. The device has a temperature control device. The temperature of the reaction system is controlled by the temperature control device to be 15-35°C. The back pressure of the reaction system outlet is ≥0.3MPa. minutes to 300mL / min, the molar ratio of isobutene to sulfur monochloride is 1.8:1 to 2.2:1, and the reaction residence time is 10 to 300 seconds. Crude chlorinated isobutene sulfide with a content of more than 95% is obtained.

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Abstract

Disclosed is a synthesizing method of sulfurized-chloridized isobutylene. The synthesizing method of sulfurized-chloridized isobutylene comprises inletting isobutylene and sulfur monochloride into a reactor, both of which are fluids. The invention also discloses application of the synthesizing method of sulfurized-chloridized isobutylene to synthesizing sulfurized isobutylene.

Description

technical field [0001] The present invention relates to a kind of synthetic method of sulfur olefin compound, specifically, the present invention relates to the method for utilizing sulfur monochloride and isobutylene to synthesize sulfurized isobutylene intermediate sulfur chloride isobutylene. technical background [0002] Organic sulfur extreme pressure agent is a kind of additive used in a large amount at present, which includes structures such as thioester, sulfane, thioaryl, thiobenzyl, thioterpene, thioketone, and thioene. Various organic sulfur extreme pressure agents with different sulfur contents are widely used in industrial production. Among them, due to the high sulfur content of sulfurized isobutylene, strong extreme pressure and wear resistance, good oil solubility, low copper corrosion, low toxicity, light color, and less dosage, it is especially suitable for adjusting the sulfur index of extreme pressure agents in production. It can produce sulfurized isobu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/24C07C323/03
CPCC07C319/24C07C323/03
Inventor 丁全有李日翔李宁杨安明张海波肖淑焕
Owner SHANDONG HIMILE CHEM TECH
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