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Preparation method and application method of a catalyst for selective oxidation of glycerol to dihydroxyacetone

A technology for oxidizing dihydroxyacetone and its application method, which is applied in the direction of oxidative preparation of carbonyl compounds, metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, etc., and can solve the problem of large profit margins and market demand, Low selectivity of dihydroxyacetone, unstable catalyst performance and other problems, to achieve the effect of good development prospects, long service life, catalytic activity and service life

Active Publication Date: 2017-01-04
ZHEJIANG COLLEGE OF ZHEJIANG UNIV OF TECHOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Dihydroxyacetone has a wide range of uses in pharmaceutical, cosmetic, food and chemical production, and is expensive, with great profit margins and market demand
Chinese patent (Application No. 200910309282.2) adopts impregnation method to support zinc, aluminum, magnesium, zirconium and titanium oxides on copper chromite powder, which is used to catalyze the oxidation of glycerin in the liquid phase. The conversion rate of glycerin is 78.4-94%. The selectivity of dihydroxyacetone is 50.4~88.9%, but the chromium ion of the heavy metal used is not friendly to the environment
Chinese patent (Application No. 201310181282.5) uses the impregnation method to load copper oxides on HZSM-5, and then reduce the copper oxides for liquid-phase catalytic oxidation of glycerin to produce dihydroxyacetone. The better result is that the conversion rate of glycerin is 92.1%. Dihydroxyacetone is less selective at 12.4%
At present, there is no industrial report on the production of dihydroxyacetone from glycerol gas-phase catalytic oxidation. The main reason is that the catalyst is easily deactivated and the catalyst performance is unstable.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] 5% Cu / Mt catalyst: Add 2.84g Cu(NO 3 ) 2 ·3H 2 0, it is 71.9g / l impregnation solution that is mixed with transparent concentration, and the impregnation solution prepared is added in the 15g montmorillonite (the quality of copper accounts for 5% of montmorillonite quality, and the mass ratio of water and montmorillonite is 2.0:1), after impregnating at room temperature for 3 hours, drying at 80°C for 3 hours in an air atmosphere, and obtaining a solid substance after cooling. Add 50g of ethylene glycol (the mass of ethylene glycol is 3.3 times the mass of montmorillonite) to the solid matter, then reflux at 195°C for 4h under the protection of argon, vacuumize at 200°C for 3h, and roast at 450°C for 4h, Prepare the montmorillonite supported by copper oxide, and then press it into 2-3 mm. Load 12g of copper oxide-supported montmorillonite into the tubular reactor, the temperature of the catalyst bed is programmed from room temperature to 350°C at 2°C / min, and at the s...

Embodiment 2

[0017] 10% Cu / Mt catalyst: Add 5.67g Cu(NO 3 ) 2 ·3H 2 0, it is 140.9g / l impregnation solution that is mixed with transparent concentration, and the impregnation solution prepared is added in 15g montmorillonite (the quality of copper accounts for 10% of montmorillonite quality, and the mass ratio of water and montmorillonite is 2.0:1), soaked at 30°C for 4h, dried at 100°C for 4h in air atmosphere, and obtained a solid substance after cooling. Add 66.6g of ethylene glycol (the mass of ethylene glycol is 4.4 times the mass of montmorillonite) to the solid matter, then reflux at 195°C for 4h under the protection of argon, vacuumize at 200°C for 4h, and roast at 500°C for 4h , to prepare montmorillonite supported by copper oxide, and then press it into 2-3 mm. 12g of copper oxide-supported montmorillonite is loaded into the tubular reactor, the temperature of the catalyst bed is programmed from room temperature to 400°C at 1.5°C / min, and 10% hydrogen and 90% nitrogen are fed ...

Embodiment 3

[0019] 15% Cu / Mt catalyst: Add 8.51g Cu(NO 3 ) 2 ·3H 2 0, it is 167.8g / l impregnation solution that is mixed with transparent concentration, and the impregnation solution prepared is added in 15g montmorillonite (the quality of copper accounts for 15% of montmorillonite quality, and the mass ratio of water and montmorillonite is 2.5:1), after impregnating at 50°C for 5h, drying at 80°C for 4h under air atmosphere, and obtaining a solid substance after cooling. Add 66.6g of ethylene glycol (the mass of ethylene glycol is 4.4 times the mass of montmorillonite) to the solid matter, then reflux at 195°C for 5h under the protection of argon, vacuumize at 220°C for 3h, and roast at 450°C for 5h , to prepare montmorillonite supported by copper oxide, and then press it into 2-3 mm. 12g of copper oxide-loaded montmorillonite is loaded into the tubular reactor, and the temperature of the catalyst bed is programmed to rise from room temperature to 380°C at 2.5°C / min, while feeding 10%...

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PUM

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Abstract

The invention discloses a preparation method of a catalyst for preparing dihydroxy acetone by selective oxidation of glycerinum and an application method thereof. The preparation method comprises the following steps: respectively adopting Cu(NO3)2.3H2O or Cu(CH2COO)2.H2O as a solute to dissolve in water, heating and stirring to prepare into transparent copper-salt aqueous solution, adding the prepared copper-salt aqueous solution into montmorillonite as impregnation liquid, cooling and then obtaining solid powder; carrying out heterogeneous nucleation on the solid powder, and adding a reducing agent (ethylene glycol) into the solid powder, wherein the mass of the ethylene glycol is 3-6 times of that of the montmorillonite; and then returning for 4-6 hours at the temperature of 195 DEG C under the protection of argon, successively vacuumizing for 3-6 hours at the temperature of 200-250 DEG C, calcining for 4-6 hours at the temperature of 450-550 DEG C, and thus preparing the montmorillonite loaded with copper oxides. The preparation method and the application method disclosed by the invention have the advantages that the catalyst is high in catalytic activity, stable in property and long in service life, and the catalyst is used for preparing the dihydroxy acetone by selective gas-phase oxidation of the glycerinum and has good development prospect.

Description

technical field [0001] The invention relates to a preparation method of a catalyst and an application method thereof, more specifically, it relates to a preparation method of a catalyst for the selective oxidation of glycerin to dihydroxyacetone and an application method thereof. Background technique [0002] Dihydroxyacetone is widely used in pharmaceutical, cosmetic, food and chemical production, and it is expensive, with great profit margin and market demand. At present, dihydroxyacetone is produced by microbial fermentation method, monobromoacetone esterification / alcoholysis method and propylene glycol oxidation method based on petroleum-based products. The former has low yield of fermentation and high cost of separation and purification; the latter also has There are many reaction steps, low yield, serious pollution and other problems. At the same time, the shortage of petroleum resources brings about the increase of raw material costs. However, with the rapid growth o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/72C07C45/29C07C49/17
Inventor 俞卫华周春晖童东绅刘彬彬
Owner ZHEJIANG COLLEGE OF ZHEJIANG UNIV OF TECHOLOGY
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