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Method for directly preparing glycols from biological cellulosan

A bio-fiber and polysaccharide technology, applied in the chemical industry, can solve the problems of low diol selectivity and achieve the effects of high yield, improved stability and less investment

Inactive Publication Date: 2012-05-09
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the selectivity to diols in this process is very low (below 15%) [Liu Haichao, Luo Chen. Utilize the method for producing sorbitol and mannitol from cellulose, Chinese Patent Publication No. CN101058531A, 2007; Chen Luo, Shuai Wang and HaichaoLiu , "Cellulose conversion into polyols catalyzed by reversibly formed acids and supported ruthenium clusters in hot water", Angew.Chem.Int.Ed., 2007, 46, 7636-7639.]

Method used

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  • Method for directly preparing glycols from biological cellulosan
  • Method for directly preparing glycols from biological cellulosan
  • Method for directly preparing glycols from biological cellulosan

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Preparation of Cu-ZnO, Ni-Cu-ZnO, Ni-ZnO catalysts:

[0028] A series of Ni-Cu-Zn catalysts with different metal ratios were prepared by co-current precipitation method. The preparation process is:

[0029] ① Make the precursor metal salt of the catalyst into a 1mol / L solution (change the ratio of the metal salt, but keep the total concentration of M2+ at 1mol / L);

[0030] ②Under full stirring, add the metal salt solution and 1.2mol / L sodium carbonate solution dropwise into 400mL deionized water preheated to 70°C at the same time, adjust the dropping speed so that the pH is about 8.0, and keep Keep the temperature constant, pH=8.0, continue to stir for 3h;

[0031] ③Washing: Let the formed emulsion stand still, cool to room temperature, add 800mL 50°C deionized water, stir evenly, let stand, pour out the supernatant, and then fully wash with suction;

[0032] ④ Drying and roasting: drying in a blast drying oven at 120°C for 12 hours, and roasting at 350°C for 4 hours...

Embodiment 2

[0036] ZrO with high surface area 2 (Precipitation-hydrothermal method preparation, BET specific surface area up to 223m 2 / g) and commercial catalyst supports, such as activated carbon, microsphere silica gel, titanium dioxide, diatomaceous earth, alumina, etc. to prepare supported Ni-based, Ni-Cu-based catalysts. Activated carbon, microsphere silica gel, white carbon black, ZnO and other carriers are pretreated by drying, roasting, etc., and then measure their volumetric water absorption, and then prepare supported catalysts by equal volume impregnation method and stepwise equal volume impregnation method. The metal loading is 2wt%-20wt%, and the catalyst is expressed as xNiyCu / carrier, where x and y represent the loadings of the two metals respectively.

[0037] Table 1: Conditions for preparation of supported Ni and Ni-Cu catalysts by impregnation method

[0038]

Embodiment 3

[0040] Cellulose conversion experiment: the evaluation of cellulose hydrolysis-hydrogenolysis reaction is carried out in a high-pressure reactor, intermittent reaction, using green and environmentally friendly high-temperature and high-pressure water as the reaction medium, the catalyst is evaluated under milder conditions, and it is connected to a computer for recording Reaction temperature and pressure changes. Add 0.5g of cellulose, 0.15g of catalyst and 50mL of water into a 100m stainless steel autoclave, replace the gas with hydrogen for three times, fill with hydrogen to 4MPa, stir at a speed of 500 rpm, and heat up to 245°C for 0.5 ~8h. After the reaction, cool down to room temperature, take the centrifuged supernatant, pass through a 0.22 μm filter membrane, and separate and detect on gas chromatography (GC) and high performance ion chromatography (HPAEC-PAD).

[0041] Qualitative analysis of low-boiling point products by gas chromatography-mass spectrometry (GC-MS) a...

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Abstract

The invention discloses a method for directly preparing glycols from biological cellulosan, comprising the following steps: using cellulose cellulose as a raw material and a polar solvent as a reaction solvent, adding a catalyst in the raw material solution, and reacting for 0.5-72 h at a temperature of 150-300 DEG C under the condition of hydrogenation to obtain a mixture of glycols and sugar alcohol, wherein, the catalyst is a supported nickel-based catalyst, copper-based catalyst, nickel-copper, copper-zinc, nickel-copper-zinc dual metal of poly metal catalyst. According to the invention, various glycols can be obtained simultaneously; the product can be used individually by separation, and can be directly used for producing unsaturated polyester resin, polyurethane, fuel additive, surfactant, emulsifier, motor vehicle antifreeze fluid and the like without deep separation.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a method for preparing diols, in particular to a method for preparing diols from plant cellopolysaccharides through hydrolysis coupled hydrogenation and hydrogenolysis. Background technique [0002] Glycol compounds are very important polyester macromolecular monomers. Ethylene glycol, propylene glycol, butanediol, etc. can be used to react with diacids to produce polyester materials with excellent performance, so the demand and output are huge. . At present, most of the industrial processes for preparing diols are based on petrochemical raw materials. However, with the depletion of fossil resources and the increasingly serious problem of environmental pollution, it has become an inevitable trend to use bio-renewable resources as raw materials to replace traditional petrochemical industrial processes with environmentally friendly green processes. . [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/00B01J23/755B01J23/80B01J23/72
Inventor 牟新东王喜成姚胜昔姜义军王晓燕
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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