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Polyvinyl-imidazole-supported cobalt carbonyl catalyst, preparation method and application of catalyst

A polyvinyl imidazole, carbonyl cobalt catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, carbon monoxide or formate reaction preparation, etc., can solve the problems of loss of Co element, complicated operation, etc. high efficiency, simple preparation method and good catalytic reaction effect

Inactive Publication Date: 2017-11-17
南京大学扬州化学化工研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reason is (1) due to [Bmin][Co(CO) 4 ] The catalyst is combined in the form of ionic bonds. The addition of water and the presence of oxygen in the water during the separation process will inevitably lead to the decomposition of the catalyst and the loss of Co element; (2) After the reaction, the catalyst and the product are separated by water extraction , the operation is more complex

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] PVI containing 0.01mol imidazole group, 0.0025mol Co 2 (CO) 8 (n(Co) / n(N)=0.5), placed in an autoclave containing 5 mL tetrahydrofuran (THF) and 15 mL methanol, replaced by carbon monoxide (CO) 3 times, filled with CO to P co =2MPa, 75 o C for 24 h.

[0032] After the reaction was completed, the solid was collected by filtration and washed with THF (3×15 mL) to obtain a polyvinylimidazole-supported cobalt carbonyl catalyst.

[0033] After the filtrate was collected and diluted, the lost Co content was analyzed by plasma spectrometry (ICP). After calculation, the actual catalyst loading (calculated based on Co content) was 12.2 wt%.

Embodiment 2

[0035] PVI with 0.01 mol of imidazole groups, 0.008 mol of NaCo(CO) 4 (n(Co) / n(N)=0.8), placed in a high-pressure reactor containing 20 mL tetrahydrofuran (THF), replaced by carbon monoxide (CO) 3 times, filled with CO to P co =5 MPa, 90 o C under reaction for 12h.

[0036] After the reaction was completed, it was directly filtered and washed with THF (3×10 mL) to obtain a polyvinylimidazole-supported cobalt carbonyl catalyst.

[0037]The filtrate was collected and diluted to analyze the loss of Co content by ICP. After calculation, the actual catalyst loading (calculated based on Co content) was 17.9 wt%.

Embodiment 3

[0039] 2.2 g (0.050 mol) ethylene oxide, the catalyst synthesized in Example 1 (containing 0.002 mol of Co) (n(EO):n(Co)=100:4), 2.4 g methanol (0.075 mol), 15 mL THF , carbon monoxide (CO) displacement 3 times, P co =3 MPa, 75 o C for 15 h. After the reaction, centrifugation was carried out, and the filtrate was taken out and analyzed by gas chromatography, and the conversion rate of ethylene oxide (EO) and the selectivity of methyl 3-hydroxypropionate (3-MHP) were calculated respectively. (See Table 1 for the results)

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Abstract

The invention relates to a polyvinyl-imidazole-supported cobalt carbonyl catalyst, a preparation method and an application of the catalyst. The raw materials comprise a high-molecular compound containing imidazole groups and cobalt carbonyl, and the catalyst is used to catalyze an alkoxycarbonylation reaction of ethylene oxide to synthesize methyl 3-hydroxypropanoate. The method provided by the invention has the characteristics that the cobalt carbonyl which is used in the alkoxycarbonylation reaction of ethylene oxide is loaded on the PVI high-molecular compound containing imidazole groups through coordination, and the catalyst can be recycled and reused in the premise that the catalytic activity is not decreased. The polyvinyl-imidazole-supported cobalt carbonyl catalyst prepared by the method has the advantages of simple preparation method, high stability, easiness for separation recovery and cyclic utilization after the reaction, and stable catalytic performance after repeated use for multiple times.

Description

technical field [0001] The invention relates to a polyvinylimidazole-loaded cobalt carbonyl catalyst used for synthesizing methyl 3-hydroxypropionate through alkoxy-carbonylation reaction of ethylene oxide, a preparation method and application thereof. Background technique [0002] 1,3-Propanediol (1,3-PDO) is mainly used in the production of new polyester polytrimethylene terephthalate (PTT), and can also be used in the synthesis of various drugs, plasticizers, detergents, emulsifiers and other fine chemicals product. Because PTT not only has the chemical stability of polyethylene terephthalate (PET), but also has resilience and pollution resistance comparable to nylon 6 and nylon 66, it is a new type of polyester fiber with a very wide application prospect. , which makes 1,3-PDO have a very large market demand. At present, there are three main methods for the preparation of 1,3-PDO: biological fermentation, acrolein hydration hydrogenation, and ethylene oxide carbonylati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J31/18B01J31/20C07C69/675C07C67/37
CPCB01J31/1691B01J31/1815B01J31/20B01J2531/0233B01J2531/0238B01J2531/0258B01J2531/845C07C67/37C07C69/675Y02P20/584
Inventor 刘玉炳周军陆海孟许波连范以宁
Owner 南京大学扬州化学化工研究院
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