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A kind of temperature-sensitive polyoxometalate composite catalyst and its synthesis method

A technology of polyoxometalates and composite catalysts, applied in the direction of metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., capable of solving two-phase The mass transfer and heat transfer of the system are hindered, and the catalytic effect is reduced, so as to achieve the effect of repeated utilization

Active Publication Date: 2021-12-28
NANYANG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In order to realize this system, in the final analysis, it is still a matter of catalyst design, because in this type of reaction system, the organic matter is hydrophobic, and if water is used as the solvent, the mass transfer and heat transfer of the two-phase system will be hindered, and the catalytic effect will be greatly reduced.

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  • A kind of temperature-sensitive polyoxometalate composite catalyst and its synthesis method

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Embodiment 1

[0029] A kind of synthetic method of temperature-sensitive polyoxometalate composite catalyst, comprises the following steps:

[0030] (1) Add N-isopropylacrylamide and diallyldimethylammonium chloride with a molar ratio of (2.5-3.5):1 into water, stir to dissolve, and pass non-reactive gas to remove oxygen for more than 30 minutes, so Said non-reactive gas is nitrogen or inert gas;

[0031] (2) Add an initiator, the initiator is potassium persulfate-FeCl 2 4H 2 O or 2-hydroxyl-4'-(2-hydroxyethoxy)-2-methylpropiophenone, the quality of the initiator is 1-2% of the N-isopropylacrylamide quality, stirred until the solution consists of Colorless and viscous, stop stirring, crystallize with saturated sodium chloride solution, and dry at 30-50°C to obtain a temperature-sensitive cationic polymer;

[0032] (3) The temperature-sensitive cationic polymer with a mass ratio of (3-5): 1 and K 8 [BW 11 o 39 H]·13H 2O is made into the temperature-sensitive cationic polymer aqueous s...

Embodiment 2

[0035] A kind of synthetic method of temperature-sensitive polyoxometalate composite catalyst, comprises the following steps:

[0036] (1) Weigh 2.1g of N-isopropylacrylamide (molecular weight 113.16) and 1.0g of diallyldimethylammonium chloride (molecular weight 161.67) into a 25mL round bottom flask, add 15mL of water, Stir to dissolve, and deoxygenate with nitrogen for 30 minutes;

[0037] (2) Weigh 0.016g of potassium persulfate and 0.016g of FeCl 2 4H 2 Dissolve O in 0.5mL water, pour it into a round bottom flask with a syringe, stir in an ice-water bath until the solution becomes viscous, stop stirring, add saturated sodium chloride solution to precipitate a white solid, and dry the white solid at 40°C Dry thermosensitive cationic polymer;

[0038] (3) Weigh 2g of temperature-sensitive cationic polymer and dissolve it in 38mL of water to make an aqueous solution of cationic polymer with a mass fraction of 5%, and weigh 0.5g of K 8 [BW 11 o 39 H]·13H 2 O was dissol...

Embodiment 3

[0041] A kind of synthetic method of temperature-sensitive polyoxometalate composite catalyst, comprises the following steps:

[0042] (1) Weigh 1.75g ​​of N-isopropylacrylamide and 1.0g of diallyldimethylammonium chloride into a 25mL round-bottomed flask, add 15mL of water, stir to dissolve, and argon to remove oxygen 40min;

[0043] (2) Weigh 0.018g of 2-hydroxy-4'-(2-hydroxyethoxy)-2-methylpropiophenone and dissolve it in 0.6mL of water, put it into a round bottom flask with a syringe, and put it under the irradiation of ultraviolet light Stir until the solution becomes viscous, stop stirring, add saturated sodium chloride solution to precipitate a white solid, and dry the white solid at 35°C to obtain a temperature-sensitive cationic polymer;

[0044] (3) Weigh 1.5g of temperature-sensitive cationic polymer and dissolve it in 23.5mL of water to make an aqueous solution of cationic polymer with a mass fraction of 6%, and weigh 0.5g of K 8 [BW 11 o 39 H]·13H 2 O was dis...

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Abstract

A synthesis method of a temperature-sensitive polyoxometalate composite catalyst provided by the present invention comprises the following steps: (1) N-isopropylacrylamide and diallyl with a molar ratio of (2.5-3.5): 1 Add dimethyl ammonium chloride into water, stir to dissolve, and remove oxygen for 30 minutes; (2) Add initiator, stir until the solution becomes viscous, crystallize, and dry to obtain a temperature-sensitive cationic polymer; (3 ) The temperature-sensitive cationic polymer with a mass ratio of (3‑5): 1 and K 8 [BW 11 o 39 H]·13H 2 O was formulated into thermosensitive cationic polymer aqueous solution and K respectively 8 [BW 11 o 39 H]·13H 2 O aqueous solution, the K 8 [BW 11 o 39 H]·13H 2 O aqueous solution was added dropwise to the temperature-sensitive cationic polymer aqueous solution under stirring to obtain a white precipitate, which was washed and dried. The polyoxometalate composite catalyst synthesized by this synthesis method is hydrophilic at room temperature and can be dissolved in the water phase. When the temperature rises to 35-65°C, it becomes hydrophobic and lipophilic, and enters the organic phase for catalysis. reaction.

Description

technical field [0001] The invention relates to the technical field of synthesis of polyoxometalate composite catalysts, in particular to a temperature-sensitive polyoxometalate composite catalyst and a synthesis method thereof. Background technique [0002] The development of polyoxometalate chemistry has a history of nearly 200 years, and its related research and application fields involve structural chemistry, material science, food chemistry, supramolecular chemistry, host-guest chemistry, analytical chemistry, surface chemistry, pharmaceuticals, Electrochemistry, photochemistry and catalytic chemistry, etc. Although the research history of polyoxometalate chemistry is very long, its special structure and excellent performance still make it an important research field at present, and new polyoxometalate structures and special properties are constantly being discovered and promoted. developed. Among the many properties and research fields of polyoxometalates, the most e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/16B01J31/06B01J23/30
CPCB01J23/30B01J27/188B01J31/06
Inventor 赵伟杨春霞汤鑫悦李彪王亚萍焦杰郭琳
Owner NANYANG NORMAL UNIV