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One-step synthesis method of sulfurized isobutylene

A technology of sulfurized isobutylene and synthesis process, applied in the direction of organic chemistry, can solve the problems of difficult processing, low conversion rate of raw materials, high price, etc., and achieve the effect of simple process control, high conversion rate of raw materials and stable product quality

Inactive Publication Date: 2017-05-24
QINGDAO SENMEIKE CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The disadvantages of the traditional process method mainly lie in: 1) the production process is long, the process control is difficult, the product will have trace chlorine, which is difficult to remove, the conversion rate of raw materials is low, the production cost is high, and the price is expensive; 2) the dechlorination and refining process produce A large amount of waste water, waste residue, heavy pollution, difficult to handle, unfavorable to the environment; 3) Sulfurized olefin has a strong pungent smell

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] 1) Raw material and dosage: sulfur 32Kg, 10% sodium carbonate solution 28Kg, sulfurized isobutylene 56Kg, water 22.5Kg;

[0013] 2) Preparation process: Add elemental sulfur and catalyst into the autoclave, raise the temperature to 150°C, stir and react for 0.5h, slowly add isobutylene into the autoclave, increase the pressure to 10Mpa after the addition, react for 1h, then cool to 80°C, Using residual pressure, the reaction mixture is pressed out of the autoclave, the organic phase is separated after standing and stratified, and then the product sulfurized isobutylene is obtained after distillation and filtration. After analyzing the concentration of sodium carbonate in the inorganic phase, add a calculated amount of new sodium carbonate to recycle the concentration of sodium carbonate in the inorganic phase to 10%.

[0014] The specification parameter of making sulfurized isobutylene is as follows:

[0015] Sulfur content (W / W, %)38

[0016] Viscosity (mm2 / s, 100℃)1...

Embodiment 2

[0022] 1) Raw materials and dosage: 71.5Kg of sulfur, 112Kg of 10% sodium bicarbonate solution, 56Kg of sulfurized isobutylene, and 21.6Kg of water;

[0023] 2) Preparation process: Add elemental sulfur and catalyst into the autoclave, raise the temperature to 250°C, stir and react for 0.5h, slowly add isobutene into the autoclave, increase the pressure to 2Mpa to react for 8h after the addition, then cool to 70°C, use Extrude the reaction mixture out of the autoclave, separate the organic phase after standing and stratifying, and then obtain the product sulfurized isobutylene after distillation and filtration. After analyzing the concentration of sodium bicarbonate in the inorganic phase, add a calculated amount of new sodium bicarbonate to make the concentration of sodium bicarbonate in the inorganic phase reach 10% again before recycling.

[0024] The specification parameter of making sulfurized isobutylene is as follows:

[0025] Sulfur content (W / W, %)46

[0026] Viscos...

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Abstract

The invention discloses a one-step synthesis method of sulfurized isobutylene, and belongs to the technical field of sulfide of acyclic unsaturated carbon skeletons. The one-step synthesis method comprises following steps: elemental sulfur and a catalyst are delivered into an autoclave, temperature is increased to 150 to 250 DEG C, stirring reaction is carried out for 0.5h, isobutylene is added into the autoclave slowly, pressure is increased to 2 to 10MPa, reaction is carried out for 1 to 8h, the temperature of an obtained product reduced to be lower than 80 DEG C via cooling, an obtained reaction mixture is taken out from the autoclave via pumping under the action of left pressure, is allowed to stand, and is subjected to layering so as to obtain an organic phase, and the organic phase is subjected to distillation and filtering so as to obtain finished product sulfurized isobutylene. The catalyst is an inorganic weak alkaline substance. The one-step synthesis method is high in yield, and low in cost; reaction is clean; and the problems in the prior art are solved.

Description

technical field [0001] The invention belongs to the technical field of sulfides of acyclic unsaturated carbon frame, and in particular relates to a synthesis process of one-step sulfurized isobutylene. Background technique [0002] Sulfurized isobutylene is an organic sulfur extreme pressure and anti-wear additive for lubricating oils. Due to its high sulfur content, extreme pressure and anti-wear properties, and good oil solubility, it is widely used in gear oils, metal additives and greases. The traditional synthesis of sulfurized isobutylene is mainly obtained by addition reaction of sulfur monochloride (S 2 Cl 2 ) and alkali metal (or alkaline earth metal sulfide) and isobutylene, sulfuration dechlorination reaction, and refined product. Addition reaction is the reaction of isobutene and sulfur monochloride in the presence of a catalyst at normal pressure and 0-50°C to obtain sulfur-chlorinated isobutylene adducts. The catalyst can be Lewis acid-methanol; sulfur dechlori...

Claims

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Application Information

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IPC IPC(8): C07D341/00
CPCC07D341/00
Inventor 李春梅
Owner QINGDAO SENMEIKE CHEM TECH CO LTD
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