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Reaction for preparing hydroxyacetone by selectively dewatering natural glycerol and catalyst

A natural glycerin and catalyst technology, applied in the direction of molecular sieve catalysts, physical/chemical process catalysts, carbon-based compound preparation, etc., can solve the problems of easy muddy active components, easy loss, etc.

Inactive Publication Date: 2008-10-15
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, solid phosphoric acid catalysts have problems such as easy sliming and easy loss of active components.

Method used

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  • Reaction for preparing hydroxyacetone by selectively dewatering natural glycerol and catalyst
  • Reaction for preparing hydroxyacetone by selectively dewatering natural glycerol and catalyst
  • Reaction for preparing hydroxyacetone by selectively dewatering natural glycerol and catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～5

[0012]Weigh 15g of H-ZSM-5 raw powder with silicon-aluminum ratio of 25, 50, 75, 100 and 360, calcinate at 550°C for 3 hours, and cool to room temperature to prepare H-ZSM-5(X) catalyst. After tableting and granulation, it is used for the reaction of glycerol dehydration to acrolein.

[0013] Selective dehydration reaction of glycerol with 20% glycerol aqueous solution as raw material, LHSV is 0.15h -1 , The dehydration reaction temperature is 300°C. The reaction results are shown in Table 1.

[0014] The reaction result of table 1 embodiment 1~5

[0015]

[0016] a : Including by-products such as formaldehyde, acetaldehyde, acetic acid, benzene and phenol.

Embodiment 6～10

[0018] Weigh 10 g of H-ZSM-5 raw powder with a silicon-aluminum ratio of 75, and exchange it with 0.2 mol / L metal salt solution under acidic conditions for 3 times by boiling and refluxing, each time is 4 hours, and the amount of solution added each time is 80 mL. Afterwards, it was washed with deionized water, dried at 110°C, and then baked in a muffle furnace at 600°C for 3 hours to obtain M-ZSM-5(75). The content of the active metal component in the prepared catalyst was 1.0 wt%. After tableting and granulation, it is used for the reaction of glycerol dehydration to acrolein. Reaction technique and condition are with embodiment 1. The reaction results are shown in Table 2

[0019] The reaction result of table 2 embodiment 6~10

[0020]

[0021] a : Including by-products such as formaldehyde, acetaldehyde, acetic acid, benzene and phenol.

Embodiment 11～15

[0023] Accurately weigh 28.8g 33.3% silica sol, 12g NaOH particles, 6.6g Al 2 (SO 4 ) 3 18H 2 O powder and 192g H 2 O, move the silica sol into a three-necked flask, add NaOH solution, heat until clarified, then add Al 2 (SO 4 ) 3 solution, stirred at constant boiling for 2 hours, cooled to room temperature, and adjusted the pH value to 6.5 to obtain amorphous silica-alumina gel; weigh 10g of H-ZSM-5 raw powder with a silica-aluminum ratio of 75, and add 8g of amorphous silica-alumina gel After mixing, reflux and exchange with 0.2mol / L metal salt solution under boiling condition for 4 hours, add 100mL of solution, wash with deionized water after exchange, dry at 110°C, and put into 600°C muffle furnace The M-ZSM-5(75) / SA catalyst can be prepared by calcining for 3h. The content of amorphous silica-alumina in the prepared catalyst is 16wt%, and the content of metal is 1.5wt%.

[0024] Reaction technology and reaction condition are with embodiment 1. The reaction result...

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Abstract

The invention relates to a catalyst for selective dehydration and conversion of natural glycerin into acrolein and the corresponding reaction process. The catalyst is composed of an H-ZSM-5 molecular sieve and 0.05%-7% of an active metal component, or the H-ZSM-5 molecular sieve, 5%-30% of amorphous silicon aluminum gel and 0.05%-7% of the active metal component. The usage of the catalyst of the invention can realize the conversion of the glycerin into the acrolein with high conversion rate and high selectivity under the conditions of normal pressure, reaction temperature of 200 to 400 DEG C and liquid-space velocity (LHSV) of 0.01 to 0.60h, glycerin water solution with 10 to 60 percent is taken as the reaction raw material, and the reaction is directly carried out in a fixed bed flow reactor without the steps of preheating and gasification. The conversion rate of the glycerin is 100% and the selectivity of the acrolein is 75.2mol% under the optimized conditions. The catalyst and the reaction process of the invention are significantly characterized in that: the catalyst has high strength and difficult argillization; the activity and the selectivity of the catalyst are high; the concentration of the reaction raw material liquid and the range of the reaction liquid-space velocity are wide, the reaction temperature is lower, and the reaction process route is simple.

Description

technical field [0001] The invention relates to a reaction and a catalyst for preparing acrolein through selective dehydration of natural glycerin. Background technique [0002] Acrolein is an important organic chemical product and an important intermediate for the preparation of fine chemical products. In addition to being directly used as a biocidal agent, tissue fixative, and water treatment agent, it can also be used to produce D required for animal feed additives. L-methionine, folic acid, acrylic acid, glutaraldehyde, and pyrimidine drugs used to treat asthma are widely used in feed industry, oil exploration, papermaking, water treatment, and medical industries. [0003] The industrial production process of acrolein mainly includes: gas phase condensation of formaldehyde-acetaldehyde, pyrolysis of propylene ether and catalytic air oxidation of propylene. Among them, the formaldehyde-acetaldehyde gas phase condensation process was developed and industrialized by Deguss...

Claims

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Application Information

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IPC IPC(8): B01J29/40B01J29/42B01J29/46C07C47/22C07C45/52
Inventor 晁自胜周春姣章文贵凡美莲梁海军孙成高黄彩娟
Owner HUNAN UNIV
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