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Preparation method of dibasic ester aromatic ring saturation catalyst containing benzene ring

A catalyst, a technology of benzene dibasic acid, which is applied in the field of preparation of dibasic ester aromatic ring saturated catalysts, can solve the problem of deactivation of active components, and achieve the effect of improving reaction efficiency and precious metal utilization

Inactive Publication Date: 2016-02-17
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, it is well known that the presence of halogen elements can easily cause the deactivation of active components

Method used

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  • Preparation method of dibasic ester aromatic ring saturation catalyst containing benzene ring

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Take amorphous silica-alumina powder and macroporous silica gel and mix appropriate amount of alumina binder to extrude into strips. After drying and roasting, the specific surface area of ​​the carrier is 105cm 2 / g, the total pore volume is 2.0ml / g. Take an appropriate amount of ruthenium acetate powder, dissolve it in an appropriate amount of acetic acid solution, slowly add dilute ammonia solution dropwise until the pH of the solution reaches 9.5, impregnate an appropriate amount of carrier in it, after saturated adsorption, immediately put it in an oven to dry at 80°C for 18h, and then roast at 300°C for 3h. The results of X-ray fluorescence analysis show that the content of elemental Ru accounts for 0.3%wt of the catalyst, and the content of Cl element is less than 0.02%wt.

Embodiment 2

[0021] Take an appropriate amount of macroporous alumina dry powder (dry basis accounts for 90%) and alumina binder (dry basis accounts for 10%) to extrude into strips, and after drying and roasting, the specific surface area of ​​the carrier is 193cm 2 / g, the total pore volume is 1.31ml / g. Take an appropriate amount of ruthenium acetate powder, dissolve it in an appropriate amount of ethanol solution, slowly add dilute ammonia solution dropwise until the pH of the solution reaches 8.5, impregnate an appropriate amount of carrier in it, after saturated adsorption, immediately put it in an oven for drying at 60°C for 18 hours, and roast at 300°C for 3 hours. The results of X-ray fluorescence analysis show that the content of elemental Ru accounts for 0.8%wt of the catalyst, and the content of Cl element is less than 0.02%wt.

Embodiment 3

[0023] Take macroporous alumina powder (30% on dry basis) and alumina A101 powder (70% on dry basis) to extrude into strips, after drying and roasting, the specific surface area of ​​the carrier is 218cm 2 / g, the total pore volume is 0.79ml / g. Take an appropriate amount of ruthenium acetate powder, dissolve it in an appropriate amount of ethanol solution, slowly add dilute ammonia solution dropwise until the pH of the solution reaches 8.0, impregnate an appropriate amount of carrier in it, after saturated adsorption, immediately put it in an oven for drying at 60°C for 18 hours, and then roast at 300°C for 3 hours. The results of X-ray fluorescence analysis show that the content of elemental Ru accounts for 0.8%wt of the catalyst, and the content of Cl element is less than 0.02%wt.

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Abstract

The invention discloses a preparation method of a dibasic ester aromatic ring saturation catalyst containing a benzene ring. According to the preparation method, a carrier with a specific macroporous structure and a halogen-free noble metal precursor are adopted, a Ru-containing catalyst is prepared through a special impregnation method, and the catalyst with the total pore volume ranging from 0.7 mg / g to 2.5 ml / g is prepared after low-temperature drying and calcination are conducted, wherein the proportion of pores with the pore volume larger than 15 nm is not lower than 55%, and the specific surface area ranges from 90 cm<2> / g to 240 cm<2> / g; the active component is the noble metal Ru, and the content of the simple substance Ru ranges from 0.02 wt% to 1.3 wt%; the chlorine content of the catalyst is smaller than or equal to 0.05 wt% of the total weight of the catalyst, the active component is distributed on the catalyst in an eggshell or egg white mode, and the content of the active component in the carrier is not larger than 0.01 wt%. According to the preparation method, the use ratio of the noble metal and the activity of the catalyst can be increased; meanwhile, the intoxicating phenomenon of the active component is restrained, the catalyst can be applied to the hydrogenation process of terephthalic acid dibasic ester or isophthalic acid dibasic ester and the hydrogenation process of o-benzene dibasic ester or p-benzene dibasic ester or m-benzene dibasic ester, and the conversion rate of reactants and the selectivity both reach 99 percent or above.

Description

technical field [0001] The invention belongs to the technical field of chemical catalysts, and in particular relates to a preparation method of a dibasic ester aromatic ring saturation catalyst containing a benzene ring. Background technique [0002] In the plastic industry, the negative impact of phthalic plasticizers on the human body and the environment has attracted more and more attention. Many countries are researching and developing non-toxic green plasticizer products. Cyclohexanedicarboxylic acid dibasic ester is a kind of A new environmentally friendly plasticizer product. Its preparation process is simple, and it can be prepared in one step from phthalic acid dicarboxylate through benzene ring hydrogenation reaction. [0003] U.S. Patent No. 6,284,917 and U.S. No. 6,248,924 disclose the preparation method of hydrogenation method to produce cyclohexane dicarboxylate, adopt the catalyst of the medium-macroporous carrier of loading Group VIII metal, adopt batch reac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/46B01J35/10C07C69/75C07C67/303
Inventor 费亚南于海斌孙国方赵甲李孝国高鹏郑修新刘有鹏臧甲忠隋芝宇张永惠
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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