Preparation method of organic vulcanizing agent for hydrogenation catalyst pre-vulcanizing

Abstract

The present invention discloses a preparation method of an organic vulcanizing agent for hydrogenation catalyst pre-vulcanizing. According to the present invention, in the presence of a catalyst, isobutylene, 1-butene or 2-butene, or a mixture comprising two or three selected from isobutylene, 1-butene and 2-butene reacts with sulphur to produce the required additive product; the consumption of the catalyst used in the method is low, the catalyst can be dissolved in the product, the performance of the product during the subsequent use process is not affected, and the catalyst is not required to be separated from the product; and the preparation method has characteristics of simple process, high yield, low production cost and no production of dust, wastewater and waste residue, belongs to the environmentally friendly green process technology, and is easily subjected to industrialization promotion.

Description

technical field

[0001] The invention belongs to the technical field of refining aids in fine chemical industry, in particular relates to a method for synthesizing an organic vulcanizing agent presulfurized by a hydrogenation catalyst, in particular to a method for preparing sulfide butene. It also belongs to the technical field of sulfides of acyclic unsaturated carbon frame. Background technique

[0002] Hydrogenation catalysts are composed of active components in an oxidized state and a carrier. During use, the active components in an oxidized state can only be converted into sulfide forms to have higher activity. Therefore, the hydrogenation catalyst must be presulfurized with a presulfidation agent before use. The vulcanizing agent is easy to decompose during the pre-sulfurization process, and can provide sufficient sulfur to convert the metal oxides in the catalyst into metal sulfides. There are many types of vulcanizing agents, but the most common ones are some organ...

Examples

Embodiment 1

[0014] Add 1200g of sulfur and 5g of catalyst into the autoclave, heat up to 160°C, stir at constant temperature for 1 hour, then pump 1,000g of isobutene into the autoclave with a metering pump, and the pressure of the autoclave rises rapidly after the isobutene is introduced, and the temperature rises to 160°C When it reaches above 3MPa, control the feed rate of isobutylene to ensure that the reaction pressure is between 3-6MPa, stir and react at 160-170°C for 2 hours, then lower the temperature, release the pressure, and filter to obtain 2200g of the additive product.

Embodiment 2

[0016] Add 1200g of sulfur and 5g of catalyst into the autoclave, heat up to 160°C, stir at constant temperature for 1 hour, then, as in Example 1, inject 1000g of 1-butene into the autoclave with a metering pump, and control the reaction pressure to 3 ~6MPa, 160~170°C stirring and reacting for 2 hours, then cooling down, depressurizing and filtering to obtain 2200g of the additive product.

Embodiment 3

[0018] Add 1200g of sulfur and 5g of catalyst into the autoclave, heat up to 160°C, stir at constant temperature for 1 hour, then, as in Example 1, inject 1000g of 2-butene into the autoclave with a metering pump, and control the reaction pressure to 3 ~6MPa, 160~170°C stirring and reacting for 2 hours, then cooling down, depressurizing and filtering to obtain 2200g of the additive product.

technical field

[0001] The invention belongs to the technical field of refining aids in fine chemical industry, in particular relates to a method for synthesizing an organic vulcanizing agent presulfurized by a hydrogenation catalyst, in particular to a method for preparing sulfide butene. It also belongs to the technical field of sulfides of acyclic unsaturated carbon frame. Background technique

[0002] Hydrogenation catalysts are composed of active components in an oxidized state and a carrier. During use, the active components in an oxidized state can only be converted into sulfide forms to have higher activity. Therefore, the hydrogenation catalyst must be presulfurized with a presulfidation agent before use. The vulcanizing agent is easy to decompose during the pre-sulfurization process, and can provide sufficient sulfur to convert the metal oxides in the catalyst into metal sulfides. There are many types of vulcanizing agents, but the most common ones are some organ...

Examples

Embodiment 1

[0014] Add 1200g of sulfur and 5g of catalyst into the autoclave, heat up to 160°C, stir at constant temperature for 1 hour, then pump 1,000g of isobutene into the autoclave with a metering pump, and the pressure of the autoclave rises rapidly after the isobutene is introduced, and the temperature rises to 160°C When it reaches above 3MPa, control the feed rate of isobutylene to ensure that the reaction pressure is between 3-6MPa, stir and react at 160-170°C for 2 hours, then lower the temperature, release the pressure, and filter to obtain 2200g of the additive product.

Embodiment 2

[0016] Add 1200g of sulfur and 5g of catalyst into the autoclave, heat up to 160°C, stir at constant temperature for 1 hour, then, as in Example 1, inject 1000g of 1-butene into the autoclave with a metering pump, and control the reaction pressure to 3 ~6MPa, 160~170°C stirring and reacting for 2 hours, then cooling down, depressurizing and filtering to obtain 2200g of the additive product.

Embodiment 3

[0018] Add 1200g of sulfur and 5g of catalyst into the autoclave, heat up to 160°C, stir at constant temperature for 1 hour, then, as in Example 1, inject 1000g of 2-butene into the autoclave with a metering pump, and control the reaction pressure to 3 ~6MPa, 160~170°C stirring and reacting for 2 hours, then cooling down, depressurizing and filtering to obtain 2200g of the additive product.

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