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Method for preparing levulinic acid from hexabasic sugar catalyzed and hydrolyzed by fire resistant and highly acidic resin

A strong acid resin, catalytic hydrolysis technology, applied in chemical instruments and methods, preparation of carboxylate, preparation of organic compounds, etc., can solve the problems of corrosion, large pollution, poor water resistance, etc., and achieve mild reaction conditions and high yields , to avoid the effect of difficult recycling

Inactive Publication Date: 2007-12-26
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] As mentioned above, liquid inorganic acids (mainly sulfuric acid and hydrochloric acid) are currently used as catalysts in the preparation of levulinic acid. This process has the disadvantages of difficult catalyst recovery, large pollution, and serious corrosion in the process of inorganic acid catalysis.
ZL200510023259.9 proposes a method of using molecular sieves to catalyze the hydrolysis of glucose to produce levulinic acid. However, molecular sieve catalysts have the fatal disadvantage of poor water resistance. Therefore, in the process of using molecular sieves to catalyze the hydrolysis of glucose to produce levulinic acid, molecular sieve catalysts are difficult to reuse.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In the 500mL batch type autoclave, adding concentration is 10g / L glucose aqueous solution 300mL and 35w resin 0.3g (the water content of 35w resin is 50%, the mass ratio of glucose and high temperature resistant strong acid resin (dry basis) is 20: 1), after airtight, start stirring, heat up to boiling under normal pressure, open the exhaust valve for 2 minutes; continue to heat up to 120°C for hydrolysis for 16 hours; the hydrolyzate is cooled to obtain a hydrolyzate, and the hydrolyzate is sampled, and the sample is passed through a 0.45um microporous membrane After filtration, it was quantitatively analyzed by high performance liquid chromatography (HPLC). The conversion rate of glucose in the hydrolyzate was 62.2%, and the molar yield of levulinic acid was 12.6%.

Embodiment 2

[0020] In the 500mL batch type autoclave, adding concentration is 20g / L glucose aqueous solution 300mL and 35w resin 0.8g (the water content of 35w resin is 50%, the mass ratio of glucose and high temperature resistant strong acid resin (dry basis) is 15: 1), after airtight, start stirring, heat up to boiling under normal pressure, open the exhaust valve for 2 minutes; continue to heat up to 130°C for 16 hours of hydrolysis; the hydrolyzate is cooled to obtain a hydrolyzate, and the hydrolyzate is sampled, and the sample is passed through a 0.45um microporous membrane After filtration, it was quantitatively analyzed by high performance liquid chromatography (HPLC). The conversion rate of glucose in the hydrolyzate was 65.6%, and the molar yield of levulinic acid was 15.4%.

Embodiment 3

[0022] In the 500mL intermittent autoclave, adding concentration is 40g / L glucose aqueous solution 300mL and 35w resin 2.4g (the water content of 35w resin is 50%, the mass ratio of glucose and high temperature resistant strong acid resin (dry basis) is 10: 1), after airtight, start stirring, heat up to boiling under normal pressure, open the exhaust valve for 3 minutes; continue to heat up to 140°C for hydrolysis for 16 hours; the hydrolyzate is cooled to obtain a hydrolyzate, and the hydrolyzate is sampled, and the sample is passed through a 0.45um microporous membrane After filtration, it was quantitatively analyzed by high performance liquid chromatography (HPLC). The conversion rate of glucose in the hydrolyzate was 70.2%, and the molar yield of levulinic acid was 20.2%.

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Abstract

This invention discloses a method for preparing levulinic acid by hydrolyzing hexamylose catalyzed by heat-resistant strong-acidic resin. The method comprises: (1) adding 10-400 g / L hexamylose aqueous solution and heat-resistant strong-acidic resin at a weight ratio of (2-20):1 into a pressure reaction kettle, sealing, stirring, heating to boiling under normal pressure, and evacuating for 2-5 min; (2) heating to 120-180 deg.C, and hydrolyzing for 2-16 h; (3) cooling the hydrolysis product to obtain hydrolysis solution. The method utilizes heat-resistant strong-acidic resin as a substitute for liquid inorganic acid as the catalyst, and has such advantages as mild reaction conditions, easy separation of the catalyst, recoverable catalyst, high catalytic activity, and high levulinic acid yield. The method is environmentally friendly, and can avoid the problems of difficult recovery of catalyst, serious pollution and serious corrosion faced by the method utilizing inorganic acid catalyst.

Description

technical field [0001] The invention relates to a method for preparing levulinic acid by using a high-temperature resistant strong acid resin to catalyze and hydrolyze hexavalent sugar. Background technique [0002] Levulinic acid, also known as 4-oxopentanoic acid, levulonic acid or valeric acid, contains a carbonyl group, a carboxyl group and α-hydrogen in its molecule, and its activity is very high, and the hydrogen atoms on its different functional groups have different activities , so it has good reactivity, and can participate in the reaction as both carboxylic acid and ketone. Through esterification, halogenation, hydrogenation, oxidative dehydrogenation condensation and other chemical reactions, various useful compounds and new polymer materials can be prepared, including resins, medicines, pesticides, spices, solvents and inks; at the same time it The carbonyl group at position 4 is a latent chiral group, and chiral compounds can be obtained through asymmetric redu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/185C07C51/00B01J31/06
Inventor 吕秀阳荆琪
Owner ZHEJIANG UNIV
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