Method for preparing methyl lactate through supported nickel oxide catalyzed monosaccharide conversion in near critical methanol medium

A methyl lactate, supported technology, applied in the field of methyl lactate prepared from supported nickel oxide catalyzed conversion of monosaccharides in near-critical methanol medium, can solve the problems of difficult industrialization, difficult loading of nano-nickel oxide, long preparation cycle, etc.

Active Publication Date: 2016-09-21
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, in terms of catalyst selection, nano-nickel oxide is not easy to load in a fixed-bed reactor, and it is difficult to realize industrialization; the preparation cycle of Sn-β molecular sieve and Zr-SBA-15 is too long

Method used

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  • Method for preparing methyl lactate through supported nickel oxide catalyzed monosaccharide conversion in near critical methanol medium
  • Method for preparing methyl lactate through supported nickel oxide catalyzed monosaccharide conversion in near critical methanol medium
  • Method for preparing methyl lactate through supported nickel oxide catalyzed monosaccharide conversion in near critical methanol medium

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] First add 1.5g glucose and 1.5g xylose to a 500mL stirred high temperature and high pressure reactor, then add 300mL methanol, the total mass concentration of glucose and xylose is 10g / L, and finally add 0.75gNiO / ZrO 2 , the total mass of glucose and xylose and NiO / ZrO 2 The mass ratio is 4:1; start stirring, heat up to 160°C, and the reaction time is 12h; after the reaction, cool down to room temperature, filter, and filtrate (the mass yield of methyl lactate is 38.27% by GC analysis after sampling) The methyl lactate product is obtained after rectification, and the methanol is reused; the filter residue is obtained as a supported nickel oxide catalyst, which is washed with methanol, dried, and reused.

Embodiment 2

[0036]First add 4.5g glucose and 4.5g xylose to a 500mL stirred high-temperature and high-pressure reactor, then add 300mL methanol, the total mass concentration of glucose and xylose is 30g / L, and finally add 2.25gNiO / ZrO 2 , the total mass of glucose and xylose and NiO / ZrO 2 The mass ratio is 4:1; start stirring, heat up to 160°C, and the reaction time is 12h; after the reaction, cool down to room temperature, filter, and filtrate (after sampling, the mass yield of methyl lactate is 38.66% by GC analysis) The methyl lactate product is obtained after rectification, and the methanol is reused; the filter residue is obtained as a supported nickel oxide catalyst, which is washed with methanol, dried, and reused.

Embodiment 3

[0038] First add 7.5g glucose and 7.5g xylose to a 500mL stirred high-temperature and high-pressure reactor, then add 300mL methanol, the total mass concentration of glucose and xylose is 50g / L, and finally add 3.75gNiO / ZrO 2 , the total mass of glucose and xylose and NiO / ZrO 2 The mass ratio is 4:1; start stirring, heat up to 160°C, and the reaction time is 12h; after the reaction is completed, cool down to room temperature, filter, and filtrate (the mass yield of methyl lactate is 37.05% by GC analysis after sampling) The methyl lactate product is obtained after rectification, and the methanol is reused; the filter residue is obtained as a supported nickel oxide catalyst, which is washed with methanol, dried, and reused.

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Abstract

The invention discloses a method for preparing methyl lactate through supported nickel oxide catalyzed monosaccharide conversion in a near critical methanol medium. The method comprises the following steps: 1, adding monosaccharide, methanol and a supported nickel oxide catalyst to a high-temperature and high-pressure reaction kettle with a stirring function, wherein the monosaccharide is five-membered sugar, six-membered sugar or a five-membered sugar and six-membered sugar mixture; 2, starting stirring, heating above added materials to 140-240DEG C, and reacting the materials for 1-12h; and 3, cooling a material obtained after the reaction ends to room temperature, filtering the cooled material, rectifying the obtained filtrate to obtain a methyl lactate product and methanol for reuse, washing filter residues containing the catalyst with methanol, and drying the catalyst for reuse. The method for preparing methyl lactate through monosaccharide conversion has the advantages of high raw material utilization rate, high methyl lactate yield, and great reduction of the separation cost, low price and good reusability of the catalyst supported nickel oxide, good mass transfer performance of the near critical methanol used as a solvent and a reactant, greenness and good industrial application prospect.

Description

technical field [0001] The invention relates to a method for preparing methyl lactate by catalyzing supported nickel oxide in a near-critical methanol medium by transforming monosaccharides into methyl lactate. The monosaccharides in the invention refer to pentasaccharides, hexasaccharides or mixtures thereof. Background technique [0002] The chemical products obtained through petroleum refining are the basis of the modern chemical industry, but with the depletion of petrochemical resources, the development of the modern chemical industry is restricted, and it is imminent to seek alternative resources. Biomass is generally regarded as a good alternative resource. The preparation of fuels and chemicals from sugars is an important way to utilize biomass resources. Monosaccharides are renewable green resources that come from biomass and are rich in content. Converting them into high value-added chemicals through chemical methods is sustainable for human beings. development is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/00C07C69/68B01J23/755
CPCB01J23/002B01J23/755C07C67/00C07C69/68
Inventor 吕秀阳吕喜蕾王立新阮厚航
Owner ZHEJIANG UNIV
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