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A kind of organic polysulfide mixed vulcanizing agent and its synthesis method

A synthesis method and vulcanizing agent technology, applied in organic chemistry, hydrogenated polysulfide/polysulfide preparation, refining to remove heteroatoms, etc., can solve problems such as high production cost, low sulfur content, and low safety, and achieve Reduce the cost of pre-vulcanization, high sulfur content, avoid the effect of concentrated heat release

Active Publication Date: 2015-09-09
XI'AN PETROLEUM UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] A technical problem to be solved by the present invention is to overcome the problems of existing organic polysulfide vulcanizing agents such as high toxicity, high production cost, low safety, difficult transportation, low sulfur content, etc. Broad, oil-soluble organic polysulfide mixed vulcanizing agent

Method used

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  • A kind of organic polysulfide mixed vulcanizing agent and its synthesis method
  • A kind of organic polysulfide mixed vulcanizing agent and its synthesis method
  • A kind of organic polysulfide mixed vulcanizing agent and its synthesis method

Examples

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Effect test

Embodiment 1

[0028] Taking the synthesis of diethyl polysulfide mixed vulcanizing agent as an example, its synthesis method is as follows:

[0029] 1. Add 18g (0.075mol) sodium sulfide nonahydrate, 9.6g (0.3mol) sulfur, and 90mL distilled water into a 250mL flask and mix evenly, place in a water bath with a magnetic heating stirrer, and react at 50°C for 30 minutes, then Naturally cool to room temperature, filter, separate unreacted sulfur, and obtain an intermediate containing sodium polysulfide.

[0030] 2. Add 16.5g (0.15mol) ethyl bromide and 1.0g (0.003mol) tetrabutylammonium bromide to the intermediate containing sodium polysulfide obtained in step 1, react at room temperature for 2 hours, then transfer the reaction solution into a separate Stand in a liquid funnel for liquid separation, and remove the lower light yellow transparent organic layer to obtain the diethyl polysulfide mixed vulcanizing agent.

[0031] The obtained product was analyzed by gas chromatography-ion trap mass ...

Embodiment 2

[0036] Taking the synthesis of diisobutyl polysulfide mixed vulcanizing agent as an example, its synthesis method is as follows:

[0037] In embodiment 1, the bromoethane used is replaced with chloroisobutane of equal substance amount, other steps are the same as embodiment 1, obtain diisobutyl disulfide, diisobutyl trisulfide, diisobutyl disulfide A mixed vulcanizing agent of butyl tetrasulfide and diisobutyl pentasulfide, wherein the mass fraction of sulfur is 55.46%, and its decomposition temperature ranges from 55 to 250°C.

Embodiment 3

[0039] Taking the synthesis of dihexyl polysulfide mixed vulcanizing agent as an example, its synthesis method is as follows:

[0040] In embodiment 1, bromoethane used is replaced with bromo-n-hexane of the same amount of substance, other steps are the same as embodiment 1, obtain dihexyl disulfide, dihexyl trisulfide, dihexyl tetrasulfide, dihexyl tetrasulfide, Mixed vulcanizing agent of hexyl pentasulfide and dihexyl hexasulfide, in which the mass fraction of sulfur is 50.19%, and its decomposition temperature ranges from 60 to 260°C.

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Abstract

The invention discloses an organic polythioether mixing vulcanizing agent and a synthetic method thereof. The general formula of the mixing vulcanizing agent is R-Sx-R, wherein R represents n-alkyl or iso-alkyl, x is selected from more than two of integers of 2-6, and the mass percentage of sulfur in the mixing vulcanizing agent is 50-70%. The synthetic method for the vulcanizing agent is environment-friendly by using easily available and harmless haloalkane as a raw material, the reaction conditions are mild, and the reaction time is relatively short; the synthetic product is high in sulfur content, wide in decomposition temperature range and good in oil solubility; when the vulcanizing agent is used for pre-vulcanizing treatment of a hydrogenation catalyst, the sulfur holding rate of the catalyst is high, and the pre-vulcanizing cost can be effectively reduced; moreover, the vulcanizing agent has a relatively large heat absorption effect in the process of introducing H2 to prepare H2S, and can counteract part of heat released in the subsequent vulcanizing process of the catalyst, thus realizing alleviated heat release in the pre-vulcanizing process of the hydrogenation catalyst, avoiding the phenomenon of centralized heat release during pre-vulcanizing treatment of the hydrogenation catalyst and achieving broad industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of vulcanizing agents, and in particular relates to an organic polysulfide mixed vulcanizing agent used for catalytic hydrogenation catalyst presulfurization and a synthesis method thereof. Background technique [0002] The quality of oil products is closely related to the environment, and now crude oil is generally heavy, which contains a large amount of nitrogen, sulfur, oxygen and metals. In addition, most of the oil products in my country come from catalytic cracking and have high olefin content, which will inevitably affect the environment. If there are relatively large adverse effects, the use of catalytic hydrogenation technology can effectively reduce these hazards. Most industrial hydrogenation catalysts use molybdenum, cobalt, nickel, tungsten and other elements as active components, and they are attached to the carrier in an oxidized state. However, the catalysts in the oxidized state are not only ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C10G45/04C07C319/22C07C321/14
Inventor 徐海升许世业
Owner XI'AN PETROLEUM UNIVERSITY
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