A kind of polyionic liquid-cerium oxide compound catalyst and its preparation method and application

A technology of polyionic liquid and oxygen compound, which is applied in the field of polyionic liquid-cerium oxygen compound catalyst and its preparation, can solve the problems of complicated urea process, etc., and achieves the improvement of conversion rate and selectivity, excellent catalytic performance, and good capture effect. Effect

Active Publication Date: 2021-01-19
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Taking 2-imidazolidinone with anti-tumor, anti-virus and anti-arrhythmic effects as an example, the traditional synthesis methods are mostly phosgene ([J].Synlett, 2001, 0900-0903) or urea ([J].Tetrahedronletters , 2004,45(39):7205-8) as a source of C=O, but phosgene is highly toxic and the urea process is cumbersome

Method used

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  • A kind of polyionic liquid-cerium oxide compound catalyst and its preparation method and application
  • A kind of polyionic liquid-cerium oxide compound catalyst and its preparation method and application
  • A kind of polyionic liquid-cerium oxide compound catalyst and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] After adding 200mmol 4-vinylbenzyl chloride and 50mmol TMPDA into the reactor to dissolve, N 2 Under protection, react at 70°C for 12 hours to prepare monomers, then add 0.8 g of azobisisobutyronitrile and stir to obtain polyionic liquid gel P[C 3 DVBTMA] [Cl]. Get 5mmol of this polyionic liquid and add 40mmol Ce(NO 3 ) 3 ·6H 2 O and H 2 O, then add Na 2 CO 3 Adjust the pH to 9, stir for 10h, filter the precipitate, wash, dry, and roast to obtain the polyionic liquid-cerium oxide catalyst P[C 3 DVBTMA][Cl]-Ce-8.

[0028] P[C 3 DVBTMA][Cl]-Ce-8, Ce 3+ The molar content accounts for 55.8% of the total amount of Ce elements, and the catalyst XPS figure is shown infigure 1 , according to Ce3 + / (Ce 3+ +Ce 4+ ) = area(u 1 , u 0 ,v 1 ,v 0 ) / total area for calculation, namely Ce 3+ corresponding u 1 , u 0 and v 1 , v 0 The ratio of the area of ​​the fitted peak to the sum of the areas of all fitted peaks; the catalyst XRD pattern is shown in figure 2 , w...

Embodiment 2

[0031] After adding 200mmol 4-vinylbenzyl chloride and 50mmol TMPDA into the reactor to dissolve, N 2 Under protection, react at 70°C for 12 hours to prepare monomers, then add 0.8 g of azobisisobutyronitrile and stir to obtain polyionic liquid gel P[C 3 DVBTMA] [Cl]. Get 5mmol of this polyionic liquid and add 20mmol Ce(NO 3 ) 3 ·6H 2 O and H 2 O, after adding NaHCO 3 Adjust the pH to 9, stir for 10h, filter the precipitate, wash, dry, and roast to obtain the polyionic liquid-cerium oxide catalyst P[C 3 DVBTMA][Cl]-Ce-4.

[0032] P[C 3 DVBTMA][Cl]-Ce-4, Ce 3+ The molar content of Ce accounts for 54.9% of the total amount of Ce elements, and its composition is CeO 2 and Ce 2 O(CO 3 ) 2 ·H 2 O.

[0033] Catalyst P[C 3 DVBTMA][Cl]-Ce-4 for CO 2 In the application of preparing 4-methylpropylene urea with 1,3-butanediamine, add 50mmol 1,3-butanediamine to the reactor, and then fill with 0.5MPa CO 2 , add 0.05g of catalyst, react at 140°C for 6h, the conversion rate...

Embodiment 3

[0035] After adding 200mmol 4-vinylbenzyl bromide and 50mmol TMPDA into the reactor to dissolve, N 2 Under protection, react at 70°C for 12 hours to prepare monomers, then add 1.0 g of azobisisobutyronitrile and stir to obtain polyionic liquid gel P[C 3 DVBTMA] [Br]. Take 5mmol of the polyionic liquid and add 20mmol Ce 2 (SO 4 ) 3 and H 2 O, then add K 2 CO 3 Adjust the pH to 9, stir for 10h, filter the precipitate, wash, dry, and roast to obtain the polyionic liquid-cerium oxide catalyst P[C 3 DVBTMA][Br]-Ce-4.

[0036] P[C 3 DVBTMA][Br]-Ce-4, Ce 3+ The molar content of Ce accounts for 46.4% of the total amount of Ce elements, and its composition is CeO 2 and Ce 2 O(CO 3 ) 2 ·H 2 O.

[0037] P[C 3 DVBTMA][Br]-Ce-4 for CO 2 In the application of preparing propylene urea with 1,3-propylenediamine, add 50mmol 1,3-propylenediamine to the reactor, and then fill it with 0.5MPa CO 2 , add catalyst 0.05g, react at 140°C for 6h, the conversion rate of 1,3-propanediam...

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Abstract

The invention discloses a polyionic liquid-cerium oxide catalyst, and a preparation method and an application thereof, and belong to the technical field of catalysts. A polyionic liquid is used as a carrier to load cerium oxide, and the cerium oxide comprises CeO2 and Ce2O(CO3)2.H2O, wherein the molar content of Ce<3+> is 30-60% of the total mole of the Ce element. The polyionic liquid / cerium oxide catalyst can be used in the preparation of cyclic urea compounds from CO2 and diamines, including the preparation of 2-imidazolidinone from CO2 and ethylene. The specific polyionic liquid is used asthe carrier, the cerium oxide is loaded on the carrier, so the proportions of Ce<3+> and Ce<4+> in the catalyst are effectively adjusted to make the proportion of the Ce<3+> in all the Ce element high, so the polyionic liquid-cerium oxide catalyst has the advantages of high oxygen vacancy concentration and many catalytic active sites.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a polyionic liquid-cerium oxide catalyst and its preparation method and application. Background technique [0002] Carbon dioxide is an abundant, low-cost, renewable carbon source that may provide an alternative production route for some organic compounds that are only available from fossil resources. Taking 2-imidazolidinone with anti-tumor, anti-virus and anti-arrhythmic effects as an example, the traditional synthesis methods are mostly phosgene ([J].Synlett, 2001, 0900-0903) or urea ([J].Tetrahedronletters , 2004,45(39):7205-8) as a source of C=O, but phosgene is highly toxic, and the urea process is cumbersome. [0003] Due to CO 2 The thermodynamic stability, if there is no catalyst, requires harsher reaction conditions. Based on this, many high-efficiency catalysts have been developed, such as Ph 3 SbO / P 4 S 10 ([J]. Journal of Molecular Catalysis A: Chemical, 2008...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/26C07D233/34C07D239/10C07D233/42C08F126/02C08F226/02C08F226/06C08F222/14C08F126/06
Inventor 李军李萌王焱良王宏涛洪燕珍
Owner XIAMEN UNIV
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