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Synthesis of organic polysulfide

A polysulfide and synthesis method technology, applied in the field of additives, can solve the problems of low cost of sulfurized olefins, insufficient product purity, environmental pollution, etc., and achieve the effects of being conducive to environmental protection, simple synthesis process route, and wide decomposition temperature range

Inactive Publication Date: 2009-07-08
大庆高新技术产业开发区南天实业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of these catalysts are: or the yield is not high, or the product purity is not enough, or the cost is high
The sulfurized olefin prepared by this method has low cost and simple process, but the product has high viscosity and poor fluidity, and needs to be diluted with solvent before use.
The additives used are one or more commonly used additives for rubber vulcanization. These additives are very expensive and most of them pollute the environment.

Method used

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  • Synthesis of organic polysulfide
  • Synthesis of organic polysulfide
  • Synthesis of organic polysulfide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1, adopt the atmospheric distillation method to cut the FCC gasoline cut of 70~140 ℃ (FCC gasoline is obtained by catalytic cracking process of straight-run vacuum residue), get 20.0g of this cut as reaction raw material, add 16.7g of elemental sulfur and 1.0g catalyst triethylamine, the three are mixed and placed in a 150ml stainless steel high-pressure reactor, the air in the reactor is replaced with nitrogen, and then the reactor is sealed. React at 170°C for 3 hours, distill triethylamine from the obtained product at 90°C, then place the mixture containing organic polysulfur and elemental sulfur in an ice-water mixture at about 0°C for 30 minutes, decant, and take the upper liquid as organic polysulfides. The obtained polysulfide was supported on alumina, and the sulfur content of the product was determined to be 24.35% by combustion neutralization titration. The synthesized organic polysulfide has a wide decomposition temperature range, high sulfur cont...

Embodiment 2

[0017] Embodiment 2, prepare organic polysulfide by the method for embodiment 1, difference is that distillate used is the FCC gasoline fraction of 60~120 ℃, and catalyst adopts the mixture of triethylamine and sodium hydroxide, and its mol ratio is 1.5: 1. The total mass added is 5% of the gasoline fraction mass, and the reaction time is 6h. The purified organic polysulfides have a sulfur content of 24.54%.

Embodiment 3

[0018] Embodiment 3, prepare organic polysulfide by the method for embodiment 1, difference is that distillate oil used is the FCC gasoline fraction of 60~140 ℃, and catalyst is the mixture of triethylamine, aniline and sodium carbonate, three molar ratios The ratio is 1:1:0.1, and the total amount added is 5% of the mass of the gasoline fraction. Purified by washing with organic polysulfides. The obtained polysulfide was supported on alumina, and the sulfur content of the product was determined to be 20.22% by combustion neutralization titration.

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Abstract

The invention discloses a synthesis method of an organic polysulfide used as a vulcanizing agent. In this method, the FCC distillate oil rich in olefins is used as a raw material. Under the action of a basic catalyst, the sulfur and the double bonds in the olefins undergo an addition reaction to form an adduct, and the unreacted elemental sulfur is separated by purification to obtain A mixture of relatively pure organic polysulfides. The organic polysulfide is mainly used as a vulcanizing agent for pre-sulfurization outside the hydrogenation catalyst. Its raw material has a wide range of sources and low cost, which can solve the problem of high production cost of the current organic vulcanizing agent; due to the use of mixed olefins as raw materials, the vulcanizing agent During application, the problem of excessively concentrated heat release can be alleviated; the process also has the advantages of simple preparation method and high sulfur content in the product, and has broad application prospects in the presulfurization process outside the hydrogenation catalyst.

Description

Technical field: [0001] The invention relates to an auxiliary agent used in the oil refining field, in particular to a method for synthesizing an organic polysulfide of a hydrogenation catalyst presulfiding agent. Background technique: [0002] Organopolysulfides are generally prepared by reacting mercaptans with elemental sulfur in the presence of basic catalysts. Traditional catalysts are amines, alkanolamines, inorganic bases, mercaptans or alcoholates. The shortcoming of these catalysts is: or yield is not high, or product purity is not enough, or cost is high. Therefore, the improvement of this synthetic route is mainly the research and improvement of the catalyst used. Adopt a kind of general formula in CN87108064A to be RSH x (C m h 2m O) The composition of yMOH is used as a catalyst, wherein R is an alkyl group of C6~C18, x is 4~12, C m h 2m O is a C2-C4 alkylene oxide, M is an alkali metal atom, and y is 0.1-0.5. Using this catalyst to prepare organic polysul...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C319/24B01J37/20
Inventor 董群王鉴于春梅陈慧娟邴国强邹丹杨春亮王德秋
Owner 大庆高新技术产业开发区南天实业有限公司
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