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Synthesis method of hydroxy-acetone using vanadium-based catalyst

A technology of hydroxyacetone and catalyst, which is applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of high energy consumption for separation and low conversion rate of cellulose, and achieve low energy consumption for separation and excellent preparation process The effect of simplicity and good application prospects

Active Publication Date: 2019-06-18
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the conversion rate of cellulose is low
Moreover, the reaction is carried out in water, and the boiling point of hydroxyacetone is higher than that of water, so the water needs to be evaporated and removed first in the product separation process, and the separation energy consumption is high
[0007] Chinese patents CN200910309282 and CN201110056529 both mentioned the method of producing hydroxyacetone from glycerin. The raw material glycerin can be derived from carbohydrates such as biomass. It is not as simple and direct as the process of directly producing hydroxyacetone from carbohydrates, and the raw material is limited to glycerol, so the application has limitations.

Method used

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  • Synthesis method of hydroxy-acetone using vanadium-based catalyst
  • Synthesis method of hydroxy-acetone using vanadium-based catalyst
  • Synthesis method of hydroxy-acetone using vanadium-based catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Beta molecular sieve dealumination: Weigh 20g of Hβ molecular sieve, 200mL of 12mol / L concentrated nitric acid, place in a 500mL three-neck flask, stir and reflux in a water bath at 80°C, dealuminate for 12h, wash until neutral, dry at 110°C for 24h, Raise the temperature to 550°C at a rate of ℃ / min, cool to room temperature after calcination for 4 hours, and obtain Hβ-deAl molecular sieves. V in the catalyst V / Hβ-deAl in the examples represents V 2 o 5 .

[0026] Catalyst Preparation: 1% V / Hβ-deAl Catalyst Preparation:

[0027] Dissolve 0.034g of vanadyl trichloride in 2ml of ethanol, add 1g of Hβ-deAl molecular sieve, stir well, dry at 80°C overnight, and then roast at 600°C for 3 hours to obtain 1% V / Hβ-deAl catalyst.

[0028] Prepare 0.5% V / Hβ-deAl, 2% V / Hβ-deAl, 4% V / Hβ-deAl catalysts by the same method.

[0029] 1%Ru / AC catalyst preparation:

[0030] 0.103g RuCl 3 Dissolve in 10ml of water, add 5g of activated carbon, stir and impregnate, dry at 80°C overnigh...

Embodiment 2

[0032] Glucose catalytic conversion experiment: add 45ml methanol, vanadium-based catalyst containing 0.012g vanadium, 0.30g 1% Ru / AC into a 100ml reactor, pass through nitrogen for three times, then pass through hydrogen for three times, fill the hydrogen to 3MPa, Raise the temperature to 220°C, inject 5ml of 50wt% glucose aqueous solution with a high-pressure constant-flow pump at a flow rate of 1ml / min, and continue the reaction for 30min after the injection. After the reaction, cool to room temperature, release the pressure and open the kettle. After the reaction solution is filtered, the yield of hydroxyacetone is analyzed on gas chromatography, and the conversion rate of glucose and the yield of sorbitol are analyzed on liquid chromatography.

[0033]

[0034] The product yields in the table are all carbon yields, and the product carbon yield=the number of carbon moles in the product / the number of carbon moles in carbohydrates×100%.

[0035] 1%Ru / AC-4%V / Hβ-deAl and 1%...

Embodiment 3

[0037]Glucose catalytic conversion experiment: Add 45ml of methanol, 4% V / Hβ-deAl catalyst containing 0.012g of vanadium, 0.30g of 1%Ru / AC into a 100ml reactor, pass through nitrogen for three times, and then pass through hydrogen for three times. Inflate hydrogen to 3MPa, heat up to the reaction temperature, inject 5ml of 50wt% glucose aqueous solution with a high-pressure constant-flow pump, flow rate is 1ml / min, and continue to react for 30min after the injection is completed. After the reaction, cool to room temperature, release the pressure and open the kettle. After the reaction solution is filtered, the yield of hydroxyacetone is analyzed on gas chromatography, and the conversion rate of glucose and the yield of sorbitol are analyzed on liquid chromatography.

[0038]

[0039] As can be seen from the data in the table, the highest yield of hydroxyacetone was obtained at 220°C.

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Abstract

The invention provides a synthesis method of hydroxy-acetone using a vanadium-based catalyst. The method realizes the process of producing hydroxy-acetone through carbohydrate by a one-step catalyticconversion process under the condition that the carbohydrate is taken as a reaction raw material, vanadium pentoxide and hydrogenation active metal as catalysts, methyl alcohol, ethyl alcohol and water as solvents, the temperature is 150-280 DEG C, and the hydrogen pressure is 0.1-10 MPa. According to the synthesis method of hydroxy-acetone using the vanadium-base catalyst, the product selectivityis good, the raw material carbohydrate can be of a biomass origin, the advantages of environmental protection, reproducible property and the like are realized, the used supported catalyst is easy tobe separated, and the molecular sieve-loaded vanadium-based catalyst is not easy to be lost in the reaction process.

Description

technical field [0001] The invention relates to a method for synthesizing hydroxyacetone with a vanadium-based catalyst, in particular to a reaction process in which carbohydrates are degraded into hydroxyacetone through one-step catalytic conversion under the action of the vanadium-based catalyst. Background technique [0002] Hydroxyacetone is mainly used in the synthesis of 4-methylimidazole, 2-aminopropanol, 4-hydroxymethylimidazole, vitamin H, acetonate, 1,2-propanediol and other fine chemicals, and can also be used as biochemical reagents and food Additives etc. It is mainly produced by oxidation of 1,2-propanediol and esterification and alcoholysis of bromoacetone / monochloroacetone. Among them, the reaction conditions of the oxidation method are harsh and the equipment requirements are high; the raw materials used in the alcoholysis method are poisonous and the price is relatively high. In addition, these two methods both use petroleum-based products as raw material...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/60C07C49/17B01J29/78B01J23/46
Inventor 郑明远乔比塞巴斯蒂安姜宇张涛
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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