Catalyst for production of cyclohexylcarboxylate by phenylcarboxylate hydrogenation and its preparation method and use

A technology of cyclohexane carboxylate and benzene carboxylate, applied in the field of catalyst and its preparation

Active Publication Date: 2015-03-25
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The feature of the above-mentioned patents is that noble metals are often used as the active components of the catalyst, and they are loaded on macroporous carriers to realize the hydrogenation of benzenecarboxylates under relatively high hydrogen pressure. The conversion rate of raw materials and product selectivity also need to be improved.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Weigh 247.7g nickel nitrate hexahydrate, 123.5g cobalt nitrate hexahydrate, dissolve with deionized water, make a solution with total metal salt concentration of 2.0g / ml, stir and heat to 60 o C, after being completely dissolved, add 8g of polyethylene glycol and stir evenly. 925g α-alumina (specific surface area is 20m 2 / g, the pore volume is 0.2cm 3 / g, 80% pore size is 10-100nm) into the prepared solution, soaked for 1h, stirring constantly during the dipping process to keep the solution uniform. The impregnated catalyst was taken out and placed in an oven to dry for 24 hours at a temperature of 80 o c. Dry the catalyst at 180 oC for 10h, then at 500 o C under roasting 2h. Reductively activate the obtained catalyst, the conditions are: the hydrogen pressure is 0.5MPa, the volume space velocity is 4000h -1 , at 150 o C reduction for 10h, the temperature was raised to 500 o C reduced for 2h, the heating rate was 100 o C / h.

Embodiment 2

[0031] Take by weighing 2477.0g nickel nitrate, 4.6g manganese nitrate, dissolve with 800ml deionized water, be made into the solution that total metal salt concentration is 4.1g / ml, stir and heat to 80 o C, add 0.05g polyethylene glycol and stir evenly after being completely dissolved. 499g of γ-alumina (with a specific surface area of ​​150m 2 / g, the pore volume is 1.2cm 3 / g, 60% pore size is 10-100nm) into the prepared solution, soaked for 3 hours, stirring constantly during the dipping process to keep the solution uniform. Take out the impregnated catalyst, put it in an oven and dry it for 20h, the drying temperature is 120 o c. The dried catalyst was calcined at 250 for 5h, then at 400 o C under roasting 6h. Reductively activate the obtained catalyst, the conditions are: the hydrogen pressure is 1.5MPa, the volume space velocity is 3000h -1 , at 250 o Reduction at C for 2h, raise the temperature to 400 o C reduced for 6h, the heating rate was 60 o C / h.

Embodiment 3

[0033] Weigh 990.8g nickel nitrate hexahydrate, 57.1g barium nitrate, 36.8g ammonium heptamolybdate, 361.7g iron nitrate, dissolve with deionized water, make a solution with a total metal salt concentration of 2.6g / ml, stir and heat to 40 o C, add 20g of polyethylene glycol after completely dissolving and stir evenly. 700g of θ-alumina (with a specific surface area of ​​300m 2 / g, the pore volume is 0.8cm 3 / g, 30% pore size is 10-100nm) into the prepared solution, dipping for 6h, stirring constantly during the dipping process to keep the solution uniform. The impregnated catalyst was taken out and placed in an oven to dry for 5 hours at a temperature of 150 o c. Dry the catalyst at 200 o C for 1h, then at 251 o C under roasting 8h. Reductively activate the obtained catalyst, the conditions are: the hydrogen pressure is 5.0MPa, the volume space velocity is 2000h -1 , at 200 o C reduction for 5h, the temperature was raised to 300 o C reduced for 8h with a heating rate ...

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Abstract

The invention discloses a catalyst for production of cyclohexylcarboxylate by phenylcarboxylate hydrogenation and its preparation method and use. The catalyst comprises 5 to 50wt% of an active component Ni, 0.1 to 25wt% of at least one auxiliary agent and the balance a carrier. The catalyst has the advantages of low price and very high activity and selectivity.

Description

technical field [0001] The invention belongs to a catalyst and its preparation method and application, in particular to a catalyst for preparing cyclohexane carboxylate by hydrogenation of benzene carboxylate, its preparation method and application. Background technique [0002] Because benzenecarboxylate has excellent properties such as good ductility, plasticity, and light and heat stability, it is often used as a plasticizer to add to plastics such as PVC, such as for the manufacture of children's toys, medical equipment, beverage bottles, food packaging bags, etc. All plastics contain a certain amount of benzene carboxylate. Recent studies have shown that these compounds can seriously affect human health, especially women and children. Animal experiments have pointed out that phthalates can lead to the proliferation of peroxisomes, and long-term studies on mice and rats have found that they can lead to the occurrence of liver tumors. Many countries have introduced rele...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/755B01J23/889B01J23/887B01J23/83C07C67/303C07C69/75
Inventor 李学宽唐明兴杜明仙
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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