Preparation method of catalyst for producing 1,2-cyclohexane dicarboxylic ester through hydrogenation

A cyclohexanedicarboxylate and catalyst technology, applied in the field of catalysis, can solve the problems of complex catalyst preparation process, high reaction temperature, unfavorable reaction progress and the like

Inactive Publication Date: 2013-02-13
CHINA NAT OFFSHORE OIL CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the current technology has the disadvantages of high reaction temperature and low conversion rate or selectivity of the reaction.
Moreover, due to the limitation of the specific surface area of ​​the macroporous carrier (30-70 m 2 /g), making the active components of noble metals gather on the surface of the carrier, reducing the active specific surface area, which is not conducive to the reaction
Patent CN10...

Method used

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  • Preparation method of catalyst for producing 1,2-cyclohexane dicarboxylic ester through hydrogenation

Examples

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Embodiment 1

[0027] Take 100g of activated alumina spherical carrier (specific surface 190.34m 2 / g, pore diameter 10.5nm, pore volume 0.51ml / g, ball diameter 5mm), and dried at 110℃ for 12h for later use. RuCl containing 0.1g Ru elemental 3 Impregnate 100 g of the carrier with an equal volume of hydrochloric acid aqueous solution for 3 hours, dry at 110°C for 10 hours after impregnation, and heat up to 300°C for 3 hours. Soak the catalyst with 0.5wt% NaOH aqueous solution, slightly heat, boil and wash 3 times. The catalyst was washed with deionized water, dried in the air, and dried at 120° C. for 10 h. Prepare Ru / Al with 0.1% Ru elemental mass fraction 2 o 3 catalyst.

Embodiment 2

[0029] Take 100g of activated alumina spherical carrier (specific surface 190.34m 2 / g, pore diameter 10.5nm, pore volume 0.51ml / g, ball diameter 5mm), and dried at 110℃ for 12h for later use. RuCl containing 0.5g Ru elemental 3 Impregnate 100 g of the carrier with an equal volume of hydrochloric acid aqueous solution for 5 hours, dry at 110°C for 10 hours after impregnation, and heat up to 300°C for 3 hours. Soak the catalyst with 0.5wt% NaOH aqueous solution, heat slightly, boil and wash 6 times. The catalyst was washed with deionized water, dried in the air, and dried at 120° C. for 10 h. Prepare Ru / Al with 0.5% Ru mass fraction 2 o 3 catalyst.

Embodiment 3

[0031] Take 100g of activated alumina spherical carrier (specific surface 190.34m 2 / g, pore diameter 10.5nm, pore volume 0.51ml / g, ball diameter 5mm), and dried at 110℃ for 12h for later use. Ru(NO 3 ) 3 Impregnate 100 g of the carrier with an equal volume of hydrochloric acid aqueous solution for 8 hours, dry at 110°C for 10 hours after impregnation, and heat up to 300°C for 3 hours. Soak the catalyst with 2.0wt% NaOH aqueous solution, heat slightly, boil and wash 3 times. The catalyst was washed with deionized water, dried in the air, and dried at 120° C. for 10 h. Prepare Ru / Al with 2.0% Ru mass fraction 2 o 3 catalyst.

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Abstract

The invention discloses a preparation method of catalyst for producing 1,2-cyclohexane dicarboxylic ester through hydrogenation. The preparation method is characterized in that the catalyst comprises Ru and/or Pd as active components; Ru is 0.01-5.0% of the catalyst in percentage by mass, and Pd is 0.01-3% of the catalyst in percentage by mass; and a carrier is a mesoporous oxide which is selected from aluminum oxide, amorphous silica-alumina or silicon dioxide. The preparation method is carried out by the following steps of: a, drying the mesoporous oxide carrier; b, diluting a hydrochloric acid aqueous solution of a calculated quantity of Ru compound and/or a hydrochloric acid aqueous solution of Pd compound with a certain amount of deionized water, and evenly mixing; c, dipping a noble metal solution on the mesoporous carrier through an equivalent-volume dipping method, wherein the impregnation time is 1-10h; d, drying the catalyst for 10h at a temperature of 110 DEG C after the dipping process, raising the temperature to 200-500 DEG C through programs and roasting for 3h; e, washing the catalyst for 1-10 times by using 0.1-5wt% of NaOH aqueous solution; and f, stoving the catalyst for 10h at 120 DEG C after the catalyst is dried.

Description

technical field [0001] The invention relates to the technical field of catalysis, and relates to a method for preparing a catalyst for hydrogenation to produce 1,2-cyclohexanedicarboxylate. Background technique [0002] The main products of international plasticizers are phthalates, of which dioctyl phthalate (DOP) and dibutyl phthalate (DBP) are the main products, especially dioctyl phthalate About 70% of China's total consumption. However, in recent years, the disadvantages of phthalate PVC plasticizers such as carcinogenicity, teratogenicity, accumulation in the human body, and poor biodegradability have been paid more and more attention. Since 2007, the European Union, the United States, and Japan have successively issued policies to prohibit the use of o-phthalic plasticizers in packaging, medical care, and children's toys. Therefore, the research and development of non-toxic green plasticizer products has become a current research hotspot. 1,2-Cyclohexanedicarboxyla...

Claims

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Application Information

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IPC IPC(8): B01J23/46B01J23/44B01J35/10C07C67/303C07C69/75
Inventor 李孝国费亚南于海滨孙国方李佳赵甲裴仁彦
Owner CHINA NAT OFFSHORE OIL CORP
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