Prevulcanizing method for hydrogenating catalyst

A hydrogenation catalyst and pre-sulfurization technology, which is applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as catalyst sulfur loss, toxic additives, and environmental pollution. Achieve the effects of easy implementation, high sulfur retention and high catalytic activity

Inactive Publication Date: 2006-08-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The additives used are organic additives commonly used in rubber vulcanization, such as tetramethylthiuram disulfide, tetraethylthiuram disulfide, tetramethylthiuram monosulfide, tetramethylthiuram tetrasulfide, etc. These additives are toxic and will pollute the environment
The vulcanizing agent used in this method is elemental sulfur, which still has the disadvantage of easy loss
In addition, this patent uses acetone extraction method to test the retention of sulfur on the catalyst, which can only explain the process of dissolving sulfur in a static solvent, but cannot reflect the real sulfur loss of the catalyst in a dynamic reaction state

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] The catalyst is presulfided according to the method provided by the invention.

[0041] (1) 87g dodecene (1-Dodecene, boiling point 213-215°C, d 4 20 0.758) and 22g of di-tert-nonyl polysulfide (n=5), and 1.5g of a mixture of di(phenylisopropyl) diphenylamine and phenylisopropyl dianiline (wherein di(phenylisopropyl) ) diphenylamine is 95wt% by weight) mixed, and the mixture is heated at 180° C. for 2 hours to obtain a liquid product containing sulfurized olefins, and the sulfur content in the product is 9.8wt% (wherein the sulfur content is determined by microcoulometry);

[0042] (2) Take 180ml of the sulfurized olefin-containing product obtained in (1) and impregnate 80g of the hydrogenation catalyst TF-1 in a dry oxidation state, and heat the solid-liquid mixture at 160°C for 1 hour and dry it in the shade;

[0043] (3) After immersing the above product with 200ml of light diesel oil with a distillation range of 235-335°C at 25°C for 4 hours, evaporate the hydroca...

Embodiment 2

[0045] The catalyst is presulfided according to the method provided by the invention.

[0046] (1) 128g dodecene (1-Dodecene, boiling point 213~215°C, d 4 20 0.758) and 32.4g of di-tert-dodecyl polysulfide (n=5) and 2g of a mixture of di(phenylisopropyl) diphenylamine and phenylisopropyl dianiline (wherein di(phenylisopropyl) Base) diphenylamine accounted for 95wt% by weight) mixed, the above mixture was heated at 160 ° C for 1.5 hours to obtain a liquid product containing sulfurized olefins, the sulfur content in the product was 10.95wt% (wherein the sulfur content was measured by microcoulometry).

[0047] (2) Take 200ml of the sulfurized olefin-containing product obtained in (1) and impregnate 90g of dry oxidized hydrogenation catalyst TF-1, and heat the solid-liquid mixture at 150°C for 3 hours and dry it in the shade;

[0048] (3) The above product was impregnated with 220ml of gasoline with a distillation range of 150-250°C at 80°C for 6 hours, and then evaporated to d...

Embodiment 3

[0050] The catalyst is presulfided according to the method provided by the invention.

[0051] (1) 100g decene (containing α-C 10 Olefin 98%) and 25.3g di-tert-nonyl polysulfide (n=5), and the mixture of 1.69g bis(phenylisopropyl) diphenylamine and phenylisopropyl diphenylamine (wherein di(phenylisopropyl) Propyl) diphenylamine accounted for 98% by weight) mixed, heated the mixture at 160°C for 2 hours to obtain a liquid product containing sulfurized olefins, and the sulfur content in the product was 12.2wt% (wherein the sulfur content was measured by microcoulometry) .

[0052] (2) Take 150ml of the sulfurized olefin-containing product obtained in (1) and impregnate 68g of dry oxidized hydrogenation catalyst TF-1, and heat the solid-liquid mixture at 150°C for 2 hours and dry it in the shade;

[0053] (3) After immersing the above product with 186ml of light diesel oil with a distillation range of 235-335°C at 50°C for 9 hours, the hydrocarbon oil was evaporated to obtain t...

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Abstract

This invention opens one prevulcanization method of hydrogenated catalyst, which contains mixing one component of alkene, organic polysulfide and accessory ingredient, immersing hydrogenated catalyst in oxidation state after being heated; then immersing by hydrocarbon oil, after re-evaporation to dryness, hydrogenated catalyst being vulcanized can be produced. The method is simple and convenient and thus this invention can be easily carried out. By this method, the hydrogenated catalyst after prevulcanization can maintain higher rate of remaining sulphur, and possesses higher catalytical activity at the same time; it is especially applicable in backflow reactor, for it can solve the practical problem that the catalyst decreases its activity because of losing sulphur.

Description

technical field [0001] The invention relates to a presulfurization method of a hydrogenation catalyst, in particular to a presulfurization method of a distillate oil hydrogenation catalyst. Background technique [0002] The method of presulfurization of hydrogenation catalyst is generally divided into two categories, namely, internal presulfurization method and external presulfurization method. In-vehicle pre-vulcanization method is a traditional pre-vulcanization method. Its disadvantages are high cost, long vulcanization time, use of flammable and toxic sulfides, and pollution to the environment. In addition, the presulfurization in the device also brings problems such as long catalyst start-up time, high start-up cost, and high risk. [0003] The external presulfurization method means that the hydrogenation catalyst is combined with the vulcanizing agent before loading into the reactor, and then loaded into the reactor. When starting up, only hydrogen or hydrogen and oil...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J37/20C10G45/50C10G45/44
Inventor 刘雪玲兰玲蒋广安廖杰峰
Owner CHINA PETROLEUM & CHEM CORP
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