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Method for preparing methyl levulinate by means of simultaneous conversion, catalyzed by molecular sieve, of five-member sugar and six-member sugar as well as enhancement of polyformaldehyde in near critical methanol

A technology of methyl levulinate and paraformaldehyde, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate and other directions, can solve the problems of excess capacity, low utilization rate of raw materials, and high separation cost

Active Publication Date: 2018-03-23
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Aiming at the problems of low raw material utilization rate, high separation cost and expensive catalyst, the present invention proposes a method for preparing methyl levulinate by strengthening paraformaldehyde in near-critical methanol, and simultaneously transforming pentavalent sugar and hexavalent sugar through molecular sieve catalysis. Polyoxymethylene is a white solid that is easily soluble in water and organic solvents. It is derived from methanol and downstream products of methanol, which helps to solve the current situation of methanol overcapacity

Method used

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  • Method for preparing methyl levulinate by means of simultaneous conversion, catalyzed by molecular sieve, of five-member sugar and six-member sugar as well as enhancement of polyformaldehyde in near critical methanol
  • Method for preparing methyl levulinate by means of simultaneous conversion, catalyzed by molecular sieve, of five-member sugar and six-member sugar as well as enhancement of polyformaldehyde in near critical methanol
  • Method for preparing methyl levulinate by means of simultaneous conversion, catalyzed by molecular sieve, of five-member sugar and six-member sugar as well as enhancement of polyformaldehyde in near critical methanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 300mL methyl alcohol in 500mL band agitated high-temperature high-pressure reactor, then add 1.5g glucose, 1.5g xylose, 6g paraformaldehyde (n=3) and 3g Hβ-25 molecular sieve, the total mass concentration of glucose and xylose is 10g / L, the mass ratio of the total mass of glucose and xylose to paraformaldehyde (n=3) is 1:2, and the mass ratio of the total mass of glucose and xylose to Hβ-25 is 1:1; Stirring is started, Stirring speed is 500rpm, heat up to 150°C, react in near-critical methanol for 15h; after the reaction, cool to room temperature and filter, the filtrate is sampled and analyzed by GC-FID, the molar yield of methyl levulinate is 49.32% , to obtain methyl levulinate product and methanol (reuse) after rectification at the same time; the filter residue is reused after being regenerated by the catalyst.

Embodiment 2

[0034] Add 300mL methyl alcohol in 500mL band stirred high-temperature high-pressure reactor, then add 4.5g glucose, 4.5g xylose, 18g paraformaldehyde (n=3) and 9g Hβ-25 molecular sieve, the total mass concentration of glucose and xylose is 30g / L, the mass ratio of the total mass of glucose and xylose to paraformaldehyde (n=3) is 1:2, and the mass ratio of the total mass of glucose and xylose to Hβ-25 is 1:1; Stirring is started, Stirring speed is 500rpm, heat up to 160°C, react in near-critical methanol for 12h; after the reaction, cool to room temperature and filter, the filtrate is sampled and analyzed by GC-FID, the molar yield of methyl levulinate is 49.67% , to obtain methyl levulinate product and methanol (reuse) after rectification at the same time; the filter residue is reused after being regenerated by the catalyst.

Embodiment 3

[0036]Add 300mL methyl alcohol in 500mL band agitated high-temperature high-pressure reactor, then add 7.5g glucose, 7.5g xylose, 30g paraformaldehyde (n=3) and 15g Hβ-25 molecular sieve, the total mass concentration of glucose and xylose is 50g / L, the mass ratio of the total mass of glucose and xylose to paraformaldehyde (n=3) is 1:2, and the mass ratio of the total mass of glucose and xylose to Hβ-25 is 1:1; Stirring is started, Stirring speed is 500rpm, heat up to 160°C, react in near-critical methanol for 12h; after the reaction, cool to room temperature and filter, the filtrate is sampled and analyzed by GC-FID, the molar yield of methyl levulinate is 48.09% , to obtain methyl levulinate product and methanol (reuse) after rectification at the same time; the filter residue is reused after being regenerated by the catalyst.

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Abstract

The invention discloses a method for preparing methyl levulinate by means of simultaneous conversion, catalyzed by a molecular sieve, of five-member sugar and six-member sugar as well as enhancement of polyformaldehyde in near critical methanol. The method comprises the following steps: (1) adding methanol into a high-temperature and high-pressure reaction kettle with a stirring function, and thenadding the five-member sugar, the six-member sugar, the polyformaldehyde and a molecular sieve based catalyst; (2) stirring, heating up to 130-230 DEG C, and carrying out a reaction for 10min-30h inthe near critical methanol; (3) after the reaction is finished, cooling to room temperature and then filtering, and carrying out rectification on filtrate, thus obtaining a methyl levulinate product at the bottom of a tower, and obtaining recyclable methanol on the top of the tower; carrying out catalyst regeneration on filter residue, and then recycling. The method proves that that the polyformaldehyde can greatly improve the yield of the methyl levulinate prepared by means of the simultaneous conversion, catalyzed by the molecular sieve, of the five-member sugar and the six-member sugar in the near critical methanol; the method has the advantages of environment friendliness, simple process, low cost and no need of high-energy density hydrogen, thus having good industrial application prospect.

Description

technical field [0001] The invention relates to a method for preparing methyl levulinate by strengthening paraformaldehyde in near-critical methanol and simultaneously converting pentasaccharides and hexasaccharides catalyzed by molecular sieves. Background technique [0002] With the depletion of fossil resources and the seriousness of the greenhouse effect, biomass resources have become a research hotspot. Biomass resources are abundant and renewable on the earth, and a series of high value-added products and biofuels can be obtained from biomass. Methyl levulinate is an important platform compound derived from biomass. [0003] Methyl levulinate (Methyl levulinate, CAS number: 624-45-3), the structural formula is shown in the following formula. [0004] Methyl levulinate structure [0005] Methyl levulinate is a colorless and transparent liquid with aromatic odor, miscible with water, soluble in methanol, ethanol and other organic solvents. Methyl levulinate can be ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/00C07C69/716
CPCC07C67/00C07C69/716Y02P20/584
Inventor 吕秀阳吕喜蕾徐玲王俊成王夏蕾
Owner ZHEJIANG UNIV