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Preparation of carbon-loaded cobalt heterogeneous catalyst and application of carbon-loaded cobalt heterogeneous catalyst in catalysis of olefin hydroformylation reaction

A heterogeneous catalyst, cobalt catalyst technology, applied in the field of catalysts and composite materials, to achieve the effects of enhanced interaction, good catalytic activity and selectivity, and low cost

Inactive Publication Date: 2020-05-05
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the application of cobalt-based catalysts supported by carbon materials obtained through alkali activation and carbonization of phenolic resins in hydroformylation reactions has not been reported yet.

Method used

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  • Preparation of carbon-loaded cobalt heterogeneous catalyst and application of carbon-loaded cobalt heterogeneous catalyst in catalysis of olefin hydroformylation reaction
  • Preparation of carbon-loaded cobalt heterogeneous catalyst and application of carbon-loaded cobalt heterogeneous catalyst in catalysis of olefin hydroformylation reaction

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Experimental program
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Effect test

Embodiment 1

[0021] Weigh 2.20 g (20 mmol) resorcinol and 22 mg Na 2 CO 3 Dissolve in 9 ml of water, then add 3.246 g (40 mmol) formaldehyde aqueous solution and stir evenly, put it into a 100 mL polytetrafluoroethylene stainless steel hydrothermal reaction kettle, seal it and place it in an oven at 80°C for 24 hours. The cured wet gel was taken out, ground and dried in vacuum at 130 °C for 3 h. Take 1.5 g of the obtained material and KOH at a mass ratio of 1:1, mix and grind, mix evenly, place in a tube furnace at 800 °C, and carbonize for 5 h under nitrogen; the carbonized material is washed with deionized water until neutral, and then Dry at 80°C for 12 hours to obtain 750 mg of carbon material, which is designated as C-1.

[0022] Weigh 0.5 g of C-1 and add it to 25 mL of deionized water, then add 1 mL of cobalt chloride solution with a cobalt concentration of 5 mg / mL, and stir for 3.0 h; then add NaOH solution dropwise to the above solution to adjust the pH of the solution value to...

Embodiment 2

[0024] Weigh 2.20 g (20 mmol) resorcinol and 11 mg K 2 CO 3 Dissolve in 12 ml water, then add 1.623 g (20 mmol) formaldehyde aqueous solution and stir evenly, put it into a 100 mL polytetrafluoroethylene stainless steel hydrothermal reaction kettle, seal it and place it in an oven at 80°C for 24 hours; The wet gel was taken out and dried under vacuum at 100° C. for 5 h after grinding. 1.5 g of the obtained material was mixed and ground with NaOH at a mass ratio of 1:1.5, mixed evenly, placed in a tube furnace at 900 °C, and carbonized for 4 h under nitrogen. The carbonized material was washed with deionized water until neutral, and dried at 80 °C for 12 h. Finally, 750 mg of carbon material was obtained, denoted as C-2.

[0025] Weigh 0.5 g of C-2 and add it to 25 mL of deionized water, then add 1 mL of cobalt nitrate solution with a cobalt concentration of 0.5 mg / mL, and continue stirring for 2.0 h. Then ammonia solution was added dropwise to the above solution to adjust ...

Embodiment 3

[0027] Weigh 2.20 g (20 mmol) resorcinol and 22 mg Na 2 CO 3 Dissolve in 20 ml of water, then add 4.869 g (60 mmol) of formaldehyde in aqueous solution and stir evenly, put it into a 100 mL polytetrafluoroethylene stainless steel hydrothermal reaction kettle, seal it and place it in a 120°C oven for 24 hours. After the cured wet gel was taken out, it was ground and dried in vacuum at 150 °C for 1 h. 1.5 g of the obtained material was mixed and ground with LiOH at a mass ratio of 1:1, mixed evenly, placed in a tube furnace at 1000 °C, and carbonized for 1 h under nitrogen. The carbonized material was washed with deionized water until neutral, and dried at 80 °C for 12 h. Finally, 750 mg of carbon material was obtained, denoted as C-3.

[0028] Weigh 1.0 g of C-3 into 25 mL of deionized water, and then add 1 mL of CoCl with a cobalt concentration of 0.5 mg / mL 2 The solution was stirred for 3.5h. Then KOH solution was added dropwise to the above solution to adjust the pH val...

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Abstract

The invention provides a preparation method of a carbon material loaded cobalt-based catalyst for olefin hydroformylation reaction. The preparation method of the catalyst comprises the following steps: performing alkali activation treatment and high-temperature carbonization on phenolic resin xerogel prepared by a gel-sol method to obtain an activated carbon material; using activated carbon as a carrier, carrying out deposition precipitation, reduction, water washing and drying so as to obtain the heterogeneous catalyst. The catalyst shows good catalytic activity and selectivity in the reaction of preparing aldehyde through hydroformylation of various olefins, and can synthesize aldehyde compounds with high yield. The catalyst has the advantages of being good in catalytic performance, simple in preparation method, high in stability, good in controllability, low in cost and high in practicability, the catalyst is easy to separate and reusable, and a new industrial technology is providedfor production of aldehyde compounds.

Description

technical field [0001] The invention relates to a preparation method of a carbon-loaded cobalt heterogeneous catalyst, which is mainly used for catalyzing olefin hydroformylation, and belongs to the technical field of composite materials and catalysts. Background technique [0002] Olefin hydroformylation refers to the reaction of raw material olefin and synthesis gas (CO / H 2 ) reaction to form an aldehyde with one more carbon atom than the starting olefin. Since the reaction was discovered in 1938, it has become one of the most important reactions in homogeneous catalysis. The product aldehyde of hydroformylation reaction is the key raw material for preparing various solvents, plasticizers and surfactants and other chemical products. In addition, it is also an important synthetic intermediate for the synthesis of organic compounds such as carboxylic acids, esters and amines. [0003] Homogeneous catalyst systems are mainly used in the hydroformylation reaction of olefins...

Claims

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Application Information

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IPC IPC(8): B01J23/75C07C45/50C07C47/02C07C47/228C07C47/277C07C47/24
CPCB01J23/75C07C45/505C07C47/02C07C47/228C07C47/277C07C47/24
Inventor 石峰柳淑娟王红利袁航空
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI