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Preparation of levulinate from glucose by molecular screen catalytic hydrolysis

A technology of catalytic hydrolysis and levulinic acid, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as nonconformity, equipment corrosion, catalyst and raw materials and products are not easily separated, etc., and achieve mild reaction conditions. , the effect of high activity

Inactive Publication Date: 2005-10-12
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The above methods all use liquid acid as a catalyst, which will produce a large amount of waste liquid and residue, serious corrosion of equipment, and difficult separation of catalyst, raw materials and products, etc., which are not in line with the current development direction of global green chemistry.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0020] Add 8.25g of Hβ molecular sieve catalyst calcined at 550°C for 4h into a 1L closed autoclave, and then add 300ml of 55g / L glucose aqueous solution. After sealing the autoclave, nitrogen gas was introduced for 10 minutes to exhaust the air in the reactor. At a stirring speed of 500 rpm, the reaction temperature was rapidly raised to 180° C., and after reacting at a pressure of 1.7 Mpa for 8 hours, the material was rapidly cooled and discharged. After the product was filtered through a 0.45 μm microporous membrane, it was quantitatively analyzed by high performance liquid chromatography (HPLC). The obtained glucose conversion rate was 98.50%, and the yield of levulinic acid was 23.39%.

example 2

[0022] Add 1.5 g of ZRP molecular sieve catalyst calcined at 550° C. for 4 h into a 1 L closed autoclave, and then add 300 ml of 10 g / L glucose aqueous solution. After sealing the autoclave, nitrogen gas was introduced for 10 minutes to exhaust the air in the reactor. At a stirring speed of 300 rpm, the reaction temperature was rapidly raised to 160° C., and after reacting at a pressure of 1.4 Mpa for 4 hours, the material was rapidly cooled and discharged. After the product was filtered through a 0.45 μm microporous membrane, it was quantitatively analyzed by high performance liquid chromatography (HPLC). The obtained glucose conversion rate was 94.41%, and the yield of levulinic acid was 20.73%.

example 3

[0024] Add 3.75g of ZRP molecular sieve catalyst calcined at 550°C for 4h into a 1L closed autoclave, and then add 300ml of 25g / L glucose aqueous solution. After sealing the autoclave, nitrogen gas was introduced for 10 minutes to exhaust the air in the reactor. At a stirring speed of 300 rpm, the reaction temperature was rapidly raised to 180° C., and after reacting for 4 hours under a pressure of 1.7 Mpa, the material was rapidly cooled and discharged. After the product was filtered through a 0.45 μm microporous membrane, it was quantitatively analyzed by high performance liquid chromatography (HPLC). The obtained glucose conversion rate was 98.42%, and the yield of levulinic acid was 29.53%.

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Abstract

Production of acetylpropionic acid by molecular sieve catalytic hydrolyzing glucose is carried out by: 1) calcining molecular sieve catalyst at 500-900deg.C; 2) adding calcined molecular sieve catalyst and glucose solution with concentration 5-100g / L into closed high-pressure reactor with weight ratio of glucose and catalyst 6-0.5; 3) inducing nitrogen into reactor, discharging air from reactor, raising temperature to 120-220deg.C, and reacting for 2-20hrs at 0.1-2Mpa. Its advantages include moderate reaction, high catalyst activity, no corrosion, and easy separation of catalyst, material and product.

Description

technical field [0001] The invention relates to a method for preparing levulinic acid, in particular to a method for preparing levulinic acid by catalytically hydrolyzing glucose with molecular sieves. Background technique [0002] Levulinic acid, also known as 4-oxopentanoic acid, levulonic acid or penteroic acid, is a widely used chemical raw material, which can be processed through esterification, halogenation, hydrogenation, oxidative dehydrogenation, condensation and other chemical reactions Preparation of various products; its 4-position carbonyl is a latent chiral group, which can obtain chiral compounds through asymmetric reduction; meanwhile, levulinic acid is also an intermediate of pesticides and fuels. Therefore it is expected to be a new platform compound. [0003] At present, there are two methods for producing levulinic acid: catalytic hydrolysis of furfuryl alcohol and direct hydrolysis of biomass. Among them, the direct biomass hydrolysis method directly u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/00C07C59/185
Inventor 陈丰秋危春玲詹晓力张欢欢
Owner ZHEJIANG UNIV
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