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A montmorillonite-based solid acid catalyst and its application to catalyze the selective dehydration of glycerol to prepare acrolein

A solid acid catalyst, montmorillonite-based technology, applied in the preparation of carbon-based compounds, preparation of organic compounds, physical/chemical process catalysts, etc., can solve the problem of uneven distribution of metal oxides, large particle size, affecting catalytic activity, etc. problem, to achieve the effect of simple preparation process, uniform distribution and good stability

Active Publication Date: 2017-09-26
菏泽建数智能科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The metal oxides loaded in the montmorillonite-based solid acid catalyst prepared by the traditional physical impregnation method are unevenly distributed and have large particle sizes, which affect the catalytic activity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] In the reactor equipped with condensation reflux device, add 15g calcium-based montmorillonite, 29.6g ethanol, 11.2g chloroform and 1.56g dichloro titanocene (titanium accounts for 2wt% of montmorillonite quality, ethanol and chloroform and montmorillonite The mass ratio of destoned is 2.0:0.7:1.0), under argon protection, react at 45°C, stir for 8h, cool to room temperature, then add 50.0g of 10wt% acetic acid solution (deionized water and acetic acid and montmorillonite The mass ratio of stone is 3.0:0.3:1.0), after stirring evenly, let it stand for 4 hours, filter, wash with deionized water, and suction filter, extrude the filter cake with extruder, dry at 110°C under air atmosphere, 450 The catalyst was prepared by calcining at ℃ for 4h. The catalyst is used for glycerin gas phase dehydration reaction: 12g of the catalyst is loaded into a tubular reactor, and glycerol is vaporized at 180°C by a 15% glycerin aqueous solution at a flow rate of 0.25ml / (min·g catalyst)....

Embodiment 2

[0033] In a reactor equipped with a condensation reflux device, add 15g of sodium montmorillonite, 37.9g ​​of ethanol, 17.9g of chloroform, 3.12g of titanocene dichloride and 0.72g zirconocene dichloride (titanium and zirconium account for montmorillonite respectively 4% and 1.5% of the mass of montmorillonite, the mass ratio of ethanol to chloroform to montmorillonite is 2.5:1.2:1.0), under the protection of argon, react at 60°C, after stirring for 12h, cool to room temperature, and then add 25wt % phosphoric acid solution 70.0g (mass ratio of deionized water to phosphoric acid to montmorillonite is 3.5:1.2:1.0), after stirring evenly, let it stand for 6h, after filtering, washing and suction filtration, the filter cake is extruded by extruder Molded, dried at 100°C in an air atmosphere, and calcined at 500°C for 4 hours to obtain a catalyst. The catalyst is used for glycerin gas phase dehydration reaction: 12g of the catalyst is loaded into a tubular reactor, and glycerin is...

Embodiment 3

[0035]In a reactor equipped with a condensation reflux device, add 15g of sodium montmorillonite, 50.9g of ethanol, 15.6g of chloroform, 0.78g of titanocene dichloride and 0.96g of zirconocene dichloride (titanium and zirconium account for montmorillonite respectively 1% and 2% of the mass of montmorillonite, the mass ratio of ethanol to chloroform to montmorillonite is 3.4:1.0:1.0), under the protection of argon, react at 45°C, stir for 10h, cool to room temperature, and then add 20wt % phosphoric acid solution 56.3g (mass ratio of deionized water to phosphoric acid to montmorillonite is 3.0:0.8:1.0), after stirring evenly, let stand for 5h, filter, wash, suction filter, and extrude the filter cake with extruder Shaped, dried at 120°C under air atmosphere, and calcined at 450°C for 4 hours to obtain the catalyst. The catalyst is used for glycerin gas phase dehydration reaction: 12g of the catalyst is loaded into a tubular reactor, and glycerol is vaporized at 190°C by a 15% g...

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Abstract

The invention discloses a montmorillonite-based solid acid catalyst, which is prepared according to the following method: adding a metallocene compound and a montmorillonite into a mixed solvent of chloroform and ethanol, the metallocene compound being metallocene titanium, metallocene A mixture of one or two of metal zirconium and metallocene molybdenum, stirred and reacted at 30-80°C under the protection of argon, cooled to room temperature, added phosphoric acid or acetic acid aqueous solution, stirred evenly, let stand, filtered, filtered The cake is washed, dried, and calcined at 400-550° C. for 3-6 hours to obtain the montmorillonite-based solid acid catalyst. The catalyst provided by the invention can be used to catalyze the selective dehydration of glycerin in the gas phase to produce acrolein, the conversion rate of glycerin is 60-100%, the selectivity of acrolein is 74-95%, and it can run for up to 120 hours. The preparation process of the catalyst is simple and the catalytic performance is high. ,long life.

Description

(1) Technical field [0001] The invention relates to a preparation method of a montmorillonite-based solid acid catalyst and its application in the selective dehydration of glycerol to produce acrolein. (2) Background technology [0002] With the expansion of biofuel production scale and rapid growth in application, the conversion and utilization of crude glycerol, the main by-product, has become an urgent problem to be solved. Researchers at home and abroad have conducted a lot of research on the conversion and utilization of crude glycerol, mainly focusing on selective dehydration, selective hydrogenation, and selective oxidation. The selective dehydration of glycerol to produce acrolein has potential market competitiveness. On the one hand, acrolein is an important organic chemical intermediate, which has a wide range of uses in drug synthesis, coatings, papermaking, oil fields, organic synthesis industries, etc., and has a large market capacity; on the other hand, the cu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22C07C47/22C07C45/52
Inventor 周春晖俞卫华童东绅
Owner 菏泽建数智能科技有限公司
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