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Preparation method of catalyst for hydrogenation of phthalic acid dicarboxylic ester

A technology of phthalic acid dicarboxylate and hydrogenation catalyst, applied in the field of catalysis, can solve the problems of low reaction conversion rate, difficult catalyst preparation process and the like

Inactive Publication Date: 2013-08-14
CHINA NAT OFFSHORE OIL CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The domestic CN101927166B patent introduces a co-precipitation method to prepare a highly active supported nickel catalyst for the hydrogenation of phthalic acid dibasic esters to produce cyclohexanedicarboxylic acid dibasic esters, but the reaction conversion rate is not high and the catalyst preparation process is not good. Easy to scale up industrially

Method used

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  • Preparation method of catalyst for hydrogenation of phthalic acid dicarboxylic ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Amorphous silicon aluminum powder (SiO 2 The content is 20%) 100g is mixed evenly with 130g of aluminum oxide powder of Shandong aluminum plant and 3.5g of celadon powder. Weigh Ni(NO 3 ) 2 .6H 2 The citric acid of O salt 34g and 3.5g is dissolved in the aqueous nitric acid solution of 4wt%. After dissolving, mix with the powder, knead for 20min, and extrude into four-leaf clover of Φ1.6. After air-drying, dry at 110°C for 12h, and bake at 550°C for 4h. SiO with a NiO content of 5% was obtained 2 -Al 2 o 3 Carrier (SiO 2 The content accounts for about 9% of the silica-alumina carrier).

[0032] Take 100g of the above-mentioned alumina-silica carrier, break the strips to 3-5mm, and dry at 110°C for 12h for later use. RuCl containing 1g Ru elemental 3 100g carrier was impregnated with an equal volume of aqueous solution, dried at 110°C after impregnated for 6h, and baked at 400°C for 3h. Prepare 1 %Ru-5%NiO / SiO 2 -Al 2 o 3 catalyst.

[0033] After the cat...

Embodiment 2

[0035] Amorphous silicon-aluminum powder (SiO 2 The content is 35%) 150g is mixed evenly with Shandong aluminum plant alumina powder 100g and 3.5g squash powder. Weigh Ni(NO 3 ) 2 .6H 2 O salt 100g and the citric acid of 3.5g, add the nitric acid aqueous solution of 180ml4wt%. After dissolving, mix with the powder, knead for 20min, and extrude into four-leaf clover of Φ1.6. After air-drying, dry at 110°C for 12h, and bake at 550°C for 4h. SiO with a NiO content of 15% was obtained 2 -Al 2 o 3 Carrier (SiO 2 The content accounts for about 15% of the silica-alumina carrier).

[0036] Take 100g of the above-mentioned alumina-silica carrier, break the strips to 3-5mm, test the water absorption and dry at 110°C for 12h for later use. RuCl containing 0.5g Ru elemental 3100g carrier was impregnated with an equal volume of aqueous solution, dried at 110°C after impregnated for 6h, and baked at 400°C for 3h. Prepared 0.5%Ru-15%NiO / SiO 2 -Al 2 o 3 catalyst.

[0037] Aft...

Embodiment 3

[0039] Amorphous silicon-aluminum powder (SiO 2 The content is 10%) 150g is mixed evenly with 100g of alumina powder of Shandong Aluminum Plant and 3.5g of scallop powder. Weigh Ni(NO 3 ) 2 .6H 2 O salt 170g and the citric acid of 3.5g, add the nitric acid aqueous solution of 185ml4wt%. After dissolving, mix with the powder, knead for 20min, and extrude into four-leaf clover of Φ1.6. After air-drying, dry at 110°C for 12h, and bake at 550°C for 4h. SiO with a NiO content of 25% was obtained 2 -Al 2 o 3 Carrier (SiO 2 The content accounts for about 6% of the silica-alumina carrier).

[0040] Take 100g of the above-mentioned alumina-silica carrier, break the strips to 3-5mm, test the water absorption and dry at 110°C for 12h for later use. RuCl containing 0.1g Ru elemental 3 100g carrier was impregnated with an equal volume of aqueous solution, dried at 110°C after impregnated for 6h, and baked at 400°C for 3h. Prepared 0.1%Ru-25%NiO / SiO 2 -Al 2 o 3 catalyst.

...

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Abstract

The invention discloses a preparation method of a catalyst for hydrogenation of phthalic acid dicarboxylic ester. According to the catalyst, an aluminum oxide-monox mixture carrier is adopted; a transitional metal Ni aid is added in the forming stage of the carrier; and noble metal active components Ru or / and Pd are loaded by an equivalent-volume impregnation method. Due to addition of the aid Ni, the activity of the catalyst can be improved, the conversion rate of the phthalic acid dicarboxylic ester and the selectivity of the products can reach over 99 percent, and the using amount of the noble metal can be reduced to a certain degree. The preparation method is simple in preparation process and easy in industrial production.

Description

technical field [0001] The invention relates to the technical field of catalysis, and relates to a preparation method of a phthalic acid dicarboxylate hydrogenation catalyst. technical background [0002] Phthalic acid long-chain esters represented by dioctyl phthalate (DOP) (dibutyl phthalate, diisononyl phthalate, butyl benzyl phthalate, phthalate Diisodecyl dicarboxylate, di-n-octyl phthalate) are important plasticizers that have been widely used for many years, but in view of the negative impact of phthalic plasticizers on the human body and the environment, many countries are studying And develop non-toxic green plasticizer products. [0003] German BASF company (US6248924, US7355084) first developed 1,2-cyclohexane diisononyl plasticizer (DINCH) as a substitute for DOP. The preparation route of this product is for dibasic phthalates The hydrogenation of benzene ring, the catalyst is the eggshell catalyst supported by Ru. Patent US6284917B1 and patent US7893295B2 int...

Claims

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Application Information

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IPC IPC(8): B01J23/89C07C69/753C07C67/303
Inventor 李孝国费亚南于海斌孙国方赵甲李佳
Owner CHINA NAT OFFSHORE OIL CORP
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