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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

Inactive Publication Date: 2018-04-03
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the ionic liquid oxidative desulfurization process can greatly improve the desulfurization rate compared with the traditional desulfurization process, there are still many unavoidable problems in the actual use process, such as: high cost, easy loss and deactivation of the catalyst, fuel quality indicators (such as olefin content, octane number, etc.) are susceptible to adverse effects, etc.

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  • Hydroxyl functionalized heteropolyacid catalyst as well as preparation method and application thereof
  • Hydroxyl functionalized heteropolyacid catalyst as well as preparation method and application thereof
  • Hydroxyl functionalized heteropolyacid catalyst as well as preparation method and application thereof

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preparation example Construction

[0039] The preparation method of the hydroxyl-functionalized heteropolyacid catalyst provided by the embodiment of the present invention comprises: reacting a haloalkane with a hydroxyl tertiary amine to generate a quaternary ammonium salt intermediate, and then making the quaternary ammonium salt intermediate and the heteropolyacid in a liquid phase system Mixing reaction in medium to prepare the hydroxy-functionalized heteropolyacid catalyst.

[0040] In some embodiments, the preparation method comprises:

[0041] Mix the hydroxyl tertiary amine and halogenated alkanes in the solvent, and react at 50-90°C for 2-6h, then cool and separate to obtain the quaternary ammonium salt intermediate;

[0042] The quaternary ammonium salt intermediate and the heteropoly acid are prepared into aqueous solutions respectively, and the aqueous solution of the quaternary ammonium salt intermediate and the heteropoly acid are mixed and reacted at 10-30°C for 1-3h, and then the obtained solid ...

Embodiment 1

[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] Bromoctadecane (166.71g, 0.5mol) and N,N-dimethylethanolamine (44.56g, 0.5mol) were placed in a 1L round bottom flask, added to 400mL ethyl acetate, heated to reflux for 4h, then cooled To room temperature, separate out solid, filter to obtain 188.25g intermediate product [(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 deionized water, and phosphotungstic acid (38.16g, 13.3mmol) was dissolved in 100mL deionized water, and the two aqueous solutions were mixed and stirred for 2 hours, and the system produced a white precipitate , filtered, and the solid product was washed three times with 20 mL of deionized water, and dried in vacuum at 40° C. to obtain 50.14 g of a white solid, with a yield of 93.0%. 1 H NMR(400MHz...

Embodiment 2

[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 ethyl acetate, heated to reflux for 4h, and then cooled to room temperature. Separate out 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), dissolve it in 100mL deionized water, dissolve silicotungstic acid (71.98g, 25mmol) in 150mL deionized water, mix and stir the two aqueous solutions for 2h, the system produces white precipitate, filter, 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 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(m, 14H), 0.89(t,3H).

...

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Abstract

The invention discloses a hydroxyl functionalized heteropolyacid catalyst as well as a preparation method and an application thereof. The cationic structure of the hydroxyl functionalized heteropolyacid catalyst contains hydroxyl. Preferably, the hydroxyl functionalized heteropolyacid catalyst has the structure shown in the description, wherein R1 is C2-C45 alkyl, R2, R3 and R4 are selected from C1-C25 alkyl or hydroxyalkyl, at least one of R2, R3 and R4 contains hydroxyl, Zn- is heteropolyacid radical, and n is any integer of 1-8. The hydroxyl functionalized heteropolyacid catalyst can be used in the oxidative desulfurization process, for example, the sulfur content of fuel can be decreased to 70% or below at the normal temperature while the quality indexes such as olefin content, octanenumber and the like of fuel are not affected, besides, and the hydroxyl functionalized heteropolyacid catalyst can still keep 50% desulfurization efficiency or above after being recycled.

Description

technical field [0001] The invention specifically relates to a hydroxyl-functionalized heteropolyacid catalyst, its preparation method and application, such as the application in oxidation extraction desulfurization, and belongs to the field of gasoline and diesel desulfurization and chemical catalysis in petroleum refining process. Background technique [0002] In recent years, the problems of smog and acid rain have become the main problems of air pollution, and the SOx produced by the combustion of sulfide in fuel oil is the main source of acid rain and air pollution. In order to reduce environmental pollution, countries have successively issued policies on the sulfide content standards in fuel oil, which has prompted domestic and foreign oil companies to actively study corresponding clean gasoline production technologies. Currently, hydrodesulfurization technology is widely used in industry. However, due to the large steric hindrance of dibenzothiophene and its derivati...

Claims

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Application Information

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IPC IPC(8): B01J31/18B01J27/188B01J27/19C10G27/04
CPCB01J23/30B01J27/188B01J27/19C07C2527/188C10G27/04C10G2300/305C10G2300/70
Inventor 童丁毅赵云星曾红玲刘丹孙俪文蔡涛刘升高栾波姚刚王耀伟
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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