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Vulcanizing agent preparing and deodorizing method for hydrogenation catalyst ex-situ pre-vulcanizing

An external presulfidation and hydrogenation catalyst technology, which is applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of development and research costs such as expensive products, and achieve high sulfur content, Low odor, high activity effect

Active Publication Date: 2015-08-19
JIANGSU KECHUANG PETROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional catalysts include organic bases such as amines and alkanolamines. The method of preparing polysulfides by the oxidation reaction of mercaptans and sulfur under alkaline conditions can obtain organic polysulfides with different sulfur crosslinking numbers, but the development of catalysts and research costs make the product expensive

Method used

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  • Vulcanizing agent preparing and deodorizing method for hydrogenation catalyst ex-situ pre-vulcanizing

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The synthesis of vulcanizing agent: sulfur (86.4g, 2.7mol) and ammoniacal liquor (concentration 25%, 153g, with NH 32.25mol in total) into the high-pressure reactor, heated to 170°C, stirred at constant temperature for 1 hour (during this period, the pressure of the reactor was about 2MPa), and reacted to generate ammonia polysulfides; then isobutylene (126g, 2.25mol) was pumped into In the reaction kettle, the pressure of the reaction kettle rises to above 3MPa after feeding isobutene, and the pressure is controlled not to exceed 9MPa. Stir and react at 170°C for 1 hour, then cool to room temperature, and separate the discharged material by natural sedimentation to obtain an organic phase and an inorganic phase. Phase filtration obtains thick vulcanizing agent product (184g); Carry out normal pressure distillation after inorganic phase filtration, absorb the ammonia gas and water that produce during distillation with 40g water, reclaim the ammoniacal liquor that obtains...

Embodiment 2

[0028] The synthesis of vulcanizing agent: sulfur (122.4g, 3.825mol) and ammoniacal liquor (concentration 25%, 153g, with NH 3 2.25mol) into the autoclave, heated up to 170°C, stirred at constant temperature for 1 hour, and reacted to generate ammonia polysulfides; Between ~9MPa, stir and react at 170°C for 1 hour, then cool to room temperature, and separate the discharged material by natural sedimentation to obtain an organic phase and an inorganic phase, and filter the organic phase to obtain a crude vulcanizing agent product (210g); the inorganic phase treatment is the same as in the example 1. Recover the isobutyramide with a concentration of 13% low-concentration ammonia and a purity of 99%.

[0029] Deodorization of vulcanizing agent: the crude vulcanizing agent product (210g) was stripped with nitrogen gas at normal temperature for 60min; 1% of the mass of the vulcanizing agent product), stirred at 60°C for 60 minutes, filtered to remove the precipitate produced by the...

Embodiment 3

[0031] The synthesis of vulcanizing agent: sulfur (86.4g, 2.7mol) and ammoniacal liquor (concentration 25%, 76.5g, with NH 3 1.125mol) into the autoclave, heated to 170°C, stirred at constant temperature for 1 hour, and reacted to generate ammonia polysulfide; Between ~9MPa, stir and react at 170°C for 1 hour, then cool to room temperature, and separate the discharged material by natural sedimentation to obtain an organic phase and an inorganic phase, and filter the organic phase to obtain a crude vulcanizing agent product (188g); Pressure distillation, use 30g of water to absorb the ammonia gas and water produced during the distillation, and recover the ammonia water with a concentration of 12%; the residue produced by the distillation is the by-product crude isobutyramide, and the crude isobutyramide and water are carried out according to the mass fraction of 1:2 For crystallization, heat to 80°C-90°C and stir to dissolve completely, then slowly cool down to room temperature...

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Abstract

The present invention discloses a vulcanizing agent preparing and deodorizing method for hydrogenation catalyst ex-situ pre-vulcanizing. The vulcanizing agent preparing and deodorizing method comprises vulcanizing agent synthesis and vulcanizing agent deodorizing, wherein excessive ammonia water is adopted as a catalyst, isobutene and sulphur are subjected to addition to produce the main product vulcanizing agent and concurrently produce the byproduct isobutyramide, and the physical method treatment technology of gas stripping and the chemical method treatment technology of hydrogen peroxide oxidation and ethylene carbonate treatment are used to carry out combined deodorizing on the vulcanizing agent. According to the present invention, the physical method treatment technology of the gas stripping and the chemical method treatment technology of the hydrogen peroxide oxidation and the ethylene carbonate treatment are used to carry out combined deodorizing, such that mercaptan, thioketone, thio thioketone and other odor components in the coarse vulcanizing agent product can be effectively removed so as to effectively reduce the odor; and after the reaction, the catalyst and the product are easily separated, the ammonia water can be recovered and recycled, the wastewater and the waste gas are not produced, only a small amount of the waste residue is produced during the filtering, and the isobutyramide product with the purity of more than 95% can be obtained by carrying out the crystallization purification treatment on the waste residue.

Description

technical field [0001] The invention relates to the synthesis and post-refining treatment of an oil refining auxiliary agent, in particular to a method for preparing and deodorizing a vulcanizing agent used for pre-sulfiding outside a hydrogenation catalyst. Background technique [0002] The external presulfurization of hydrodesulfurization catalyst has the characteristics of short curing time, high utilization rate of curing agent, and high catalyst activity after curing, and has become the main direction of presulfurization technology development. The vulcanizing agent for external pre-vulcanization is mainly organic polysulfide, which is a type of sulfur-containing compound with the general formula R-Sn-R1, n is generally 3 to 20, R and R1 can be the same or different, and each represents An organic group with 1 to 150 carbon atoms, this type of vulcanizing agent has the characteristics of low toxicity and wide decomposition temperature range, and is widely used in the pr...

Claims

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Application Information

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IPC IPC(8): B01J37/20
Inventor 顾齐欣郑来昌
Owner JIANGSU KECHUANG PETROCHEM
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