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Reaction for preparing hydroxyacetone by selectively dewatering natural glycerol and catalyst

A technology of natural glycerol and hydroxyacetone, applied in physical/chemical process catalyst, metal/metal oxide/metal hydroxide catalyst, preparation of carbon-based compounds, etc., can solve problems such as easy curing and deactivation

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, the catalyst is easily solidified and deactivated during the reaction.

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

[0014] 20g of silicon dioxide was calcined at 600°C for 6 hours, cooled to room temperature, pressed into tablets and granulated, and the catalyst of 20-30 meshes was screened for use.

[0015] A proper amount of catalyst is filled in the quartz reaction tube of the fixed bed reactor, and 20-30 mesh quartz sand is filled in the upper part of the catalyst bed and the lower part of the reactor space. Hydrogen gas was introduced into the reactor, and the catalyst was reduced for 6 hours under the conditions of a pressure of 0.01 MPa and a temperature of 300°C. After the reaction tube is cooled to room temperature, 40% glycerol aqueous solution is fed into the reactor with a constant flow pump to carry out selective dehydration of glycerin, and the LHSV is 0.1h -1 , The dehydration reaction temperature is 310°C. The result of the reaction is as follows:

[0016] Glycerin conversion rate is 10.50%; Product molar selectivity is: hydroxyacetone 3.33%, 1,2-propanediol 2.35%, acetald...

Embodiment 2

[0018] Weigh 5g of copper nitrate trihydrate, 15g of silicon dioxide and 50g of deionized water in a beaker and mix evenly, stir at room temperature for 6 hours, remove the liquid and dry at 120°C, bake at 600°C for 6 hours, cool to room temperature, repeat the above Cu / SiO with 20% CuO content was prepared by impregnation loading and firing process 3 times 2 catalyst. The catalyst is tableted and granulated, and the granules with 20-30 meshes are screened for the reaction of glycerin dehydration to produce hydroxyacetone.

[0019] Reaction process condition is with embodiment 1. The result of the reaction is as follows:

[0020] Glycerin conversion rate is 51.64%; Product molar selectivity is: hydroxyacetone 38.18%, 1,2-propanediol 1.69%, acetaldehyde 6.78%, and other components (mainly acetic acid, dihydrofuran, dihydroxyfuran, glycerol acetate esters, etc.) 53.35%.

Embodiment 3

[0022] Weigh 9g of ferric chloride hexahydrate, 15g of silicon dioxide and 50g of deionized water in a beaker and mix evenly, stir at room temperature for 6 hours, remove the liquid and dry at 120°C overnight, roast at 600°C for 6 hours, and cool to room temperature , repeat the above impregnation loading and roasting process twice to obtain Fe 2 o 3 28% Fe / SiO 2 catalyst. Tablet granulation, screening of 20-30 mesh catalysts for use.

[0023] Reaction process condition is with embodiment 1. The result of the reaction is as follows:

[0024]Glycerin conversion rate is 16.90%; Product molar selectivity is: hydroxyacetone 1.92%, 1,2-propanediol 1.71%, acetaldehyde 7.10%, and other components (mainly acetic acid, dihydrofuran, dihydroxyfuran, glycerol acetate esters, etc.) 89.27%.

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Abstract

The invention relates to a reaction technology for manufacturing hydroxyacetone through selective dehydration of natural glycerin, and a corresponding catalyst. The catalyst is composed of low-activity carriers such as SiO2, etc. and active metal components of 20 to 90wt percent, and is prepared by adopting an insuccation loading method. The active metal components which are used are IB group elements, or the combination of IB and VIB group elements, or the combination of IB, VIB and light rare earth elements. The reaction for manufacturing the hydroxyacetone through selective dehydration of the natural glycerin is performed in a fixed bed flowing-type reactor; the glycerin conversion rate can reach up to 99.89 percent, and the molar selectivity of the hydroxyacetone can reach up to 89.74 percent under the conditions that the material concentration can reach 10 to 100 percent, the normal atmosphere is provided, the temperature ranges from 200 to 400 DEG C, and the liquid hourly space velocity (LHSV) satisfies 0.01 to 0.60h<-1>. The catalyst has simple preparation technology and low price, and the concentration of the reaction material that is glycerin water solution and the liquid hourly space velocity has wide range.

Description

technical field [0001] The invention relates to the selective dehydration reaction of natural glycerin to prepare hydroxyacetone and a catalyst. Background technique [0002] Hydroxyacetone is mainly used to synthesize H in the digestive system 2 The intermediate 4-methylimidazole of the blocking drug cimetidine, the intermediate of the quinolone antibacterial drug levofloxacin (s)-(+)-2-aminopropanol, the intermediate of racemic histidine 4-Hydroxymethylimidazole, vitamin H, antipyretic and analgesic aspirin acetonate without ulcer side effects, chiral intermediate (1)-(-)-1,2-propanediol and other fine chemicals. Used as biochemical reagents and food additives, etc. [0003] Hydroxyacetone is currently mainly produced by the esterification / alcoholysis of bromoacetone and the oxidation of 1,2-propanediol. Relatively speaking, the former reaction conditions are milder, the production equipment is simpler, and the product yield and purity are higher. However, there are pr...

Claims

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Application Information

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IPC IPC(8): B01J23/70B01J23/83C07C49/17C07C45/52
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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