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Solid superacid catalyst as well as preparation method and application thereof

A solid superacid and catalyst technology, which is applied in the direction of catalyst activation/preparation, carboxylate preparation, chemical instruments and methods, etc., and can solve problems affecting catalytic activity, sintering of sulfated zirconia, etc.

Inactive Publication Date: 2021-06-08
BEIFANG UNIV OF NATITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most of the zirconium sources for the synthesis of sulfated zirconia are zirconium hydroxide, zirconium oxychloride, zirconium oxide and zirconium n-propoxide, etc., but the sulfated zirconia synthesized with these raw materials is prone to sintering, which affects the catalytic activity

Method used

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  • Solid superacid catalyst as well as preparation method and application thereof
  • Solid superacid catalyst as well as preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Synthesis of UiO-66: First, 1.16g (4.97mmol) of zirconium chloride and 0.825g (4.97mmol) of terephthalic acid (H 2 BDC) was dissolved in 60 mL of N,N-dimethylformamide (DMF) and 20 mL of acetic acid. Then ultrasonic treatment was used for 30 min to homogenize the solution, and after the ultrasonic treatment was completed, the reaction was carried out at 120° C. for 24 h. After the reaction, the mixture was centrifuged, washed three times with N,N-dimethylformamide (DMF) and methanol, and dried at 120° C. for 6 h to obtain UiO-66 nanocrystals.

Embodiment 2

[0052] Sulfated zirconia (SO 4 2- / ZrO 2 ) synthesis: UiO-66 was calcined at 500 °C for 3 h (heating rate 1 °C / min) to obtain ZrO 2 . According to the ratio of 1g:15mL ZrO at 30°C 2 Immersed in ammonium sulfate solution (3mol / L) for 1h, then filtered, dried at 100°C for 6h, then calcined at 500°C and kept for 3h (heating rate 1°C / min) to obtain SO 4 2- / ZrO 2 .

Embodiment 3

[0054] The solid superacid catalyst (SO 4 2- / ZrO 2 @Al 2 o 3 ) preparation method, as follows:

[0055] Dissolve 0.5 g of aluminum isopropoxide in 20 mL of ethanol and stir for 3 h to form a transparent solution for later use. Disperse 100mg UiO-66 nanocrystals in 30mL deionized water, sonicate for 10min, add 0.3g CTAB and stir for 5min. Then slowly add the aluminum isopropoxide solution into the UiO-66 dispersion, stir for 3 hours, filter under reduced pressure and wash with 95% ethanol and deionized water for 3 to 5 times, and dry at 100°C for 6 hours to obtain aluminum hydroxide-coated The product of UiO-66, denoted as UiO-66@Al(OH) 3 . UiO-66@Al(OH) 3 Calcined at 500°C for 3 hours to obtain calcined product of alumina-coated zirconia, denoted as ZrO 2 @Al 2 o 3 , and then placed in ammonium sulfate solution (1mol / L) at 30°C for 1h with stirring (dosage: 1g UiO-66: 15mL ammonium sulfate solution), then filtered and dried at 100°C for 6h. Calcined at 500 DEG C f...

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Abstract

The invention discloses a solid superacid catalyst as well as a preparation method and application thereof, which relates to the technical field of solid superacid catalysts. According to the preparation method, aluminum isopropoxide is used as an aluminum source, UiO-66 is used as a zirconium source, the solid superacid catalyst is prepared, the sintering phenomenon is avoided, and the prepared solid superacid catalyst is high in BET specific surface area, contains Bronsted acid sites and Lewis acid sites at the same time and has higher catalytic reaction efficiency.

Description

technical field [0001] The invention relates to the technical field of solid superacid catalysts, in particular to a solid superacid catalyst and its preparation method and application. Background technique [0002] As an important chemical intermediate, ethyl levulinate usually uses carbohydrates (cellulose, glucose and fructose) as raw materials, through acid-catalyzed alcoholysis of carbohydrate-derived levulinic esterification, furfural and its derivative furfuryl alcohol Alcoholysis conversion and other methods of synthesis. Compared with the corrosion of equipment and environmental pollution caused by the use of traditional inorganic liquid acids (such as sulfuric acid, hydrochloric acid, and phosphoric acid, etc.), solid superacids are more and more popular due to their low corrosion, environmental protection, and easy recycling. attention of many researchers. [0003] A solid superacid is an acid stronger than 100% sulfuric acid, that is, an acid with a Hammett fun...

Claims

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Application Information

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IPC IPC(8): B01J27/053B01J35/10B01J37/02B01J37/08C07C67/00C07C69/716
CPCB01J27/053B01J37/086B01J37/0201C07C67/00B01J35/615C07C69/716
Inventor 袁红张志黄志航
Owner BEIFANG UNIV OF NATITIES