Hydroxyl functionalized heteropolyacid catalyst as well as preparation method and application thereof
A heteropolyacid and functionalized technology, which is applied in the direction of carbon compound catalysts, physical/chemical process catalysts, catalysts, etc., can solve the problems of bad influence on fuel quality indicators, catalyst loss, high cost, etc., and achieve excellent recovery utilization rate and desulfurization conditions Gentle, problem-solving effect on recycling
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[0039] The preparation method of the hydroxyl-functionalized heteropolyacid catalyst provided in the embodiment of the present invention includes: reacting a halogenated alkane with a tertiary hydroxyamine to form a quaternary ammonium salt intermediate, and then allowing the quaternary ammonium salt intermediate and the heteropolyacid in a liquid phase system mixed reaction in the middle to prepare the hydroxyl-functionalized heteropolyacid catalyst.
[0040] In some embodiments, the preparation method comprises:
[0041] The hydroxyl tertiary amine and the halogenated alkane are mixed in a solvent and reacted at 50-90 ° C for 2-6 h, then cooled and separated to obtain the quaternary ammonium salt intermediate;
[0042] The quaternary ammonium salt intermediate and the heteropoly acid are respectively prepared into aqueous solutions, the aqueous solution of the quaternary ammonium salt intermediate and the aqueous solution of the heteropoly acid are mixed and reacted at 10-30...
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[0077] Embodiment 1 [(C 18 H 37 )N + (CH 3 ) 2 (C 2 H 4 OH)] 3 PW 12 O 40
[0078] 1) Catalyst synthesis (see figure 1 )
[0079] Bromooctadecane (166.71g, 0.5mol) and N,N-dimethylethanolamine (44.56g, 0.5mol) were placed in a 1L round-bottomed flask, added to 400mL of ethyl acetate, heated to reflux for 4h, and then cooled to room temperature, a solid was precipitated, and 188.25 g of intermediate product were obtained by filtration [(C 18 H 37 )N + (CH 3 ) 2 (C 2 H 4 OH)]Br; take the intermediate product [(C 18 H 37 )N + (CH 3 ) 2 (C 2 H 4 OH)]Br (16.80g, 39.8mmol) was dissolved in 100mL of deionized water, phosphotungstic acid (38.16g, 13.3mmol) was dissolved in 100mL of deionized water, the two aqueous solutions were mixed and stirred for 2h, the system produced a white precipitate , filtered, the solid product was washed three times with 20 mL of deionized water, and dried under vacuum at 40° C. to obtain 50.14 g of a white solid with a yield of 9...
Example Embodiment
[0086] Embodiment 2 [(C 10 H 21 )N + (CH 3 )(C 2 H 4 OH) 2 ] 4 SiW 12 O 40
[0087] Bromodecane (110.54g, 0.5mol) and N-methyldiethanolamine (59.68g, 0.5mol) were placed in a 1L round-bottom flask, added to 400mL of ethyl acetate, heated under reflux for 4h, and then cooled to room temperature, Precipitate solid, filter to obtain 139.56g intermediate product [(C 10 H 21 )N + (CH 3 )(C 2 H 4 OH) 2 ]Br; take the intermediate product [(C 10 H 21 )N + (CH 3 )(C 2 H 4 OH) 2 ]Br (34.04g, 100mmol) was dissolved in 100mL deionized water, silicotungstic acid (71.98g, 25mmol) was dissolved in 150mL deionized water, the two aqueous solutions were mixed and stirred for 2h, the system produced a white precipitate, filtered, solid The product was washed three times with 20 mL of deionized water, and dried under vacuum at 40° C. to obtain 95.45 g of a white solid with a yield of 90.1%. 1 H NMR(400MHz,DMSO-d6)δ4.12(m,4H),3.73(m,4H),3.50(m,2H),3.31(s,3H),1.77(m,2H),1.26...
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