Synthesis technique of sulfide isobutene by one-step method

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

Inactive Publication Date: 2008-01-02
HOLITECH TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 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

[0020] 1) Raw material and dosage: sulfur 32Kg, 10% sodium carbonate solution 28Kg, sulfurized isobutylene 56Kg, water 22.5Kg;

[0021] 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%.

[0022] The specification parameter of making sulfurized isobutylene is as follows:

[0023] Sulfur content (W / W, %) 38

[0024] Viscosity (mm 2 / s, 10...

Embodiment 2

[0030] 1) Raw materials and dosage: 71.5Kg of sulfur, 112Kg of 10% sodium bicarbonate solution, 56Kg of sulfurized isobutylene, and 21.6Kg of water;

[0031] 2) Preparation process: add elemental sulfur and catalyst into the autoclave, heat up to 250°C, stir and react for 0.5h, slowly add isobutene into the autoclave, increase the pressure to 2Mpa after the addition, react for 8h, then cool to 70°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 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.

[0032] The specification parameter of making sulfurized isobutylene is as follows:

[0033] Sulfur content (W / W, %) 46...

Embodiment 3

[0040] 1) Raw materials and dosage: 40Kg of sulfur, 56Kg of 10% sodium carbonate solution, 56Kg of sulfurized isobutylene, and 15Kg of water;

[0041] 2) Preparation process: add elemental sulfur and catalyst into the autoclave, heat up to 200°C, stir and react for 0.5h, slowly add isobutylene into the autoclave, increase the pressure to 8Mpa after the addition, react for 5h, then cool to 70°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%.

[0042] The specification parameter of making sulfurized isobutylene is as follows:

[0043] Sulfur content (W / W, %) 42

[0044] Viscosity (mm 2 / s, 10...

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Abstract

The invention discloses a synthetic technology of vulcanizing isobutene with one-step method in the sulfide technique field of acyclic unsaturated carbon skeleton, which comprises the following steps: adding the elemental sulfur and accelerant in autoclave; heating to 150-250Deg. C; mixing for 0.5 hours; adding isobutene in the autoclave slowly; increasing the pressure to 2-10MPa for 1-8 hours; cooling less than 80Deg. C; extruding the mixture from the high-pressure autoclave with the rest pressure; separating the organic phase after stewing and layering; distilling; filtering; getting the vulcanized isobutene product( the accelerant is inorganic weak base material). The invention is provided the high efficient, the low cost and the clean reaction, which solves the prior technique problem.

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. [0003] The synthesis of traditional sulfurized isobutylene mainly uses sulfur monochloride (S 2 Cl 2 ) and alkali metal (or alkaline earth metal sulfide) and isobutene through addition reaction, sulfuration dechlorination reaction, and refined finished 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; su...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C321/18C07C319/22
Inventor 段会伟李继文李德军亓即道魏峰李芝光
Owner HOLITECH TECH CO LTD
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