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Method of preparing small molecule polyol from carbohydrate under near-critical or supercritical conditions

A technology of carbohydrates and supercritical water, which is applied in the preparation of hydroxyl compounds, organic compounds, chemical instruments and methods, etc., to achieve the effects of high space-time conversion rate, simple preparation process, and convenient use

Active Publication Date: 2013-12-04
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction time is greater than 0.1s and less than 60min

Method used

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  • Method of preparing small molecule polyol from carbohydrate under near-critical or supercritical conditions
  • Method of preparing small molecule polyol from carbohydrate under near-critical or supercritical conditions
  • Method of preparing small molecule polyol from carbohydrate under near-critical or supercritical conditions

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Metal catalyst Ni / AC,Ni / SiO 2 ,Pt / AC,Ru / AC,Ir / TiO 2 Preparation: impregnate nickel nitrate, chloroplatinic acid, ruthenium trichloride, and chloroiridic acid aqueous solution on the carrier, dry at 120°C for 12h, and then reduce it in a hydrogen atmosphere at 450°C for 1h to obtain the catalyst Ni / AC (5wt%Ni), Ni / MC(5wt%Ni), Pt / AC(0.5wt%Pt), Ru / AC(5wt%Ru), Ni / SiO 2 (15wt%Ni), Ir / TiO 2 (2wt%Ir) catalyst.

Embodiment 2

[0024] Preparation of bimetallic catalyst composed of noble metal and nickel:

[0025] Co-impregnation or step-by-step impregnation is used. Taking co-impregnation as an example, the specific operation steps are: take 1.0g of mesoporous carbon (MC) and add it to a chloride solution containing 1% Ir (Ru, Pt, Pd, Rh are all available, Ir is used as an example here) and In the 5ml aqueous solution of 0.259g nickel nitrate, stand by room temperature for 12 hours, then dry in the oven of 60 ℃ and 120 ℃ respectively for 12 hours. The as-prepared precursors were reduced at 450 °C for 1 h under a hydrogen atmosphere. The theoretical loading amount of nickel in the prepared catalyst is 5wt%, and the theoretical loading amount of noble metal is 1%. The final prepared catalyst is labeled as 1%Ir-5%Ni / MC.

Embodiment 3

[0027] Catalytic conversion experiment: Add 0.5g of carbohydrates, 0.2g of catalyst and 50ml of water into a 100ml reactor, pass through hydrogen to replace the gas three times, fill it with hydrogen to 4MPa, place it in a tin bath at 355°C, and react for 5min. After the reaction is finished, cool down to room temperature, take the centrifuged supernatant, separate it on a high-performance liquid chromatography calcium-type ion-exchange column and detect it with a differential refraction detector. Ethylene glycol, propylene glycol, and hexahydric alcohols (including sorbitol, mannitol) are calculated in the product yield, and the gaseous product is CO 2 , CH 4 , C 2 h 6 Wait for the gas to calculate.

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Abstract

The method provides a method of preparing small molecule polyol such as glycol and propylene glycol from Cn(H2O)m compounds such as straw, paper pulp, waste paper, cellulose, starch, semi-cellulose, cane sugar, glucose, fructose, fructosan, xylose, and soluble xylo oligosaccharide under the near-critical or supercritical conditions. In the method, carbohydrate is taken as the raw material, the 8, 9 and 10 groups of transition metals, namely iron, cobalt, nickel, ruthenium, rhodium, palladium, iridium, and platinum, are taken as the catalytic active components, one-step catalytic conversion process is carried out under the near-critical and supercritical water conditions: temperature of 300 to 450 DEG C, hydrogen pressure of 1 to 10 MPa, and total pressure of 10 to 35 MPa, and high efficient, high selective, and high yield preparation of small molecule polyol such as glycol and propylene glycol is achieved. The reaction provided by the invention has the prominent advantages of recyclable raw material and high atom economy, and the preparation of the catalyst has the advantages of simple and easy process and low cost. Furthermore, compared to other technologies, which prepare polyol from biomass, the method has the advantages of simple reaction process, high space time yield, and convenience for industrial production.

Description

technical field [0001] The present invention relates to the preparation method of ethylene glycol, propylene glycol and other small molecular alcohols, specifically the reaction process of carbohydrates undergoing one-step catalytic hydrogenation degradation to produce ethylene glycol, propylene glycol and other small molecular alcohols under near-critical or supercritical water conditions . Background technique [0002] Small molecule alcohols such as ethylene glycol and propylene glycol are important energy liquid fuels, and are also very important raw materials for polyester synthesis, for example, for polyethylene terephthalate (PET), polyethylene naphthalate ( PEN), can also be used as antifreeze, lubricant, plasticizer, surfactant, etc., and is a widely used organic chemical raw material. [0003] At present, the industrial production of small molecule alcohols such as ethylene glycol and propylene glycol is mainly obtained from petroleum raw materials (Document 1: Cu...

Claims

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Application Information

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IPC IPC(8): C07C29/00
CPCY02P20/54
Inventor 庞纪峰张涛郑明远姜宇王爱琴
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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