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Method for efficiently preparing ex-situ presulfuration agent through medium-pressure solvothermal method

A solvothermal method and vulcanizing agent technology, applied in the preparation of sulfides, hydrogenated polysulfides/polysulfides, organic chemistry, etc., can solve the problems of high toxicity, low sulfur content and high cost of pre-vulcanizing agents, and avoid Concentrated exothermic phenomenon, high sulfur content, low pollution effect

Inactive Publication Date: 2016-02-10
定远县云森科技有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention aims to provide a method for the high-efficiency preparation of an external pre-vulcanizing agent by a medium-pressure solvothermal method. The technical problems to be solved are: 1. Overcome the existing pre-vulcanizing agent with high toxicity, high cost, low sulfur content, serious pollution, etc. Problem; 2. To provide a synthesis method with mild conditions, short reaction time, low equipment requirements and no "three wastes" problem. The mixed presulfiding agent can be directly applied to the presulfurization treatment of hydrogenation catalysts, and the reaction conditions are suitable at the same time. in industrial production

Method used

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  • Method for efficiently preparing ex-situ presulfuration agent through medium-pressure solvothermal method
  • Method for efficiently preparing ex-situ presulfuration agent through medium-pressure solvothermal method
  • Method for efficiently preparing ex-situ presulfuration agent through medium-pressure solvothermal method

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Effect test

Embodiment 1

[0026] Sulfurene ratio 2.5:1.

[0027] Add 17.86kg of elemental sulfur and 18.00kg of ammonia solvent with a mass fraction of 5% to the reactor, raise the temperature to 150°C, slowly add 12.50kg of isobutylene, and keep the pressure at 3.0-3.5MPa. Continue to react for 6h after adding, and then After cooling to 35°C, the mixture was forced out of the reaction vessel using residual pressure. The mixture was allowed to stand for liquid separation, and the organic phase was filtered, washed, and distilled to obtain the product of an external organic presulfurizing agent with a yield of 90%. After analyzing the ammonia concentration of the inorganic phase, add fresh ammonia water to make it reach the original concentration before recycling. The product obtained in this embodiment is compared and analyzed with the imported vulcanizing agent to obtain a total ion chromatogram (TIC) and a mass spectrogram (MS) (see figure 2 ), infrared spectrum (see image 3 ).

[0028] The spe...

Embodiment 2

[0031] Sulfurene ratio 2.5:1.

[0032] Add 17.86kg of elemental sulfur and 27.00kg of ammonia solvent with a mass fraction of 10% to the reactor, raise the temperature to 145°C, slowly add 12.50kg of isobutylene, and keep the pressure at 3.0-3.5MPa. Continue to react for 6 hours after adding, and then After cooling to 35°C, the mixture was forced out of the reaction vessel using residual pressure. The mixture was allowed to stand for liquid separation, and the organic phase was filtered, washed, and distilled to obtain the product of an external organic presulfurizing agent with a yield of 74%. After analyzing the ammonia concentration of the inorganic phase, add fresh ammonia water to make it reach the original concentration before recycling.

[0033] The specifications and parameters of the synthesized external organic prevulcanizing agent are as follows:

[0034]

Embodiment 3

[0036] Sulfurene ratio 2.0:1.

[0037] Add 14.29kg of elemental sulfur and 36.00kg of ammonia solvent with a mass fraction of 5% to the reactor, raise the temperature to 155°C, slowly add 12.5kg of isobutylene, and keep the pressure at 3.0-3.5MPa. Continue the reaction for 6 hours after the addition, and then After cooling to 35°C, the mixture was forced out of the reaction vessel using residual pressure. The mixture was allowed to stand for liquid separation, and the organic phase was filtered, washed, and distilled to obtain the product of an external organic presulfurizing agent with a yield of 81%. After analyzing the ammonia concentration of the inorganic phase, add fresh ammonia water to make it reach the original concentration before recycling.

[0038] The specifications and parameters of the synthesized external organic prevulcanizing agent are as follows:

[0039]

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Abstract

The invention discloses a method for efficiently preparing an ex-situ presulfuration agent through a medium-pressure solvothermal method, and belongs to the technical field of organic multi-sulfur-ether mixed vulcanizing agent synthesis of ring-free unsaturated carbon skeletons. The synthesis method includes the following steps of adding elemental sulfur and solvent into a reaction kettle, raising the temperature to be 145-160 DEG C, continuing to conduct stirring for 0.5 h, slowly adding isobutene into the reaction kettle, controlling the pressure at 3.0-3.5 MPa, conducting reacting for 3-6 h at a constant temperature, cooling to 35 DEG C after the reaction ends, and pressing the reaction mixture out of the reaction kettle through overbottom pressure. After standing and liquid distribution are conducted on the product, a certain amount of 120# gasoline or methylbenzene is added, filtering, washing, backflow and distillation are conducted on the organic phase, the ex-situ presulfuration agent is obtained, and fresh solvent can be compensated for till reaching the existing concentration to be recycled after the inorganic phase is analyzed. Ammonia water solutions of different concentrations serve as solvent. The method has the advantages of being low in cost, high in product yield, free of pollution, low in device requirement, and the like, solves the problems in the prior art, and breaks through technology monopoly for the ex-situ presulfuration agent at home and abroad.

Description

technical field [0001] The invention belongs to the technical field of synthesis of an organic polysulfide mixed vulcanizing agent with acyclic unsaturated carbon frame, and in particular relates to a method for efficiently preparing an external pre-vulcanizing agent by a medium-pressure solvothermal method. Background technique [0002] With the development of modern society, more and more attention is paid to the quality of oil products, which is not only related to the utilization rate of crude oil, but also closely related to the environment. Nowadays, heavy oil is generally used in the refining of crude oil, which contains a large amount of N , S, O and M (metal), since most of the oil products in my country come from catalytic cracking, and the olefin content is relatively high, it will inevitably have a large adverse impact on the environment. The use of catalytic hydrogenation technology can effectively reduce these hazards. Most industrial hydrogenation catalysts use...

Claims

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Application Information

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IPC IPC(8): C07C321/14C07C319/24C07C319/14
Inventor 潘文胜凌双英李平沈士兵
Owner 定远县云森科技有限公司
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