Method for preparing low carbon polyol by internal circulating catalysis and conversion of carbohydrate

A carbohydrate and catalytic conversion technology, applied in the preparation of hydroxyl compounds, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of decreased reaction selectivity, catalyst poisoning, affecting the yield of target products and catalyst life, etc. Life, avoid direct contact, improve the effect of target product yield

Active Publication Date: 2012-10-17
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] On the other hand, when the method of literature 7-9 is used for the conversion of relatively high concentration (greater than 5wt%) cellulose to prepare ethylene glycol and propylene glycol, due to a certai

Method used

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  • Method for preparing low carbon polyol by internal circulating catalysis and conversion of carbohydrate
  • Method for preparing low carbon polyol by internal circulating catalysis and conversion of carbohydrate
  • Method for preparing low carbon polyol by internal circulating catalysis and conversion of carbohydrate

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Embodiment 1

[0034] Metal catalyst Ni / AC,Ni / TiO 2 , the preparation of Pt / AC, Ru / AC: impregnated activated carbon support with nickel nitrate, chloroplatinic acid, and ruthenium trichloride aqueous solution respectively, after drying at 120°C for 12h, and reducing it in a hydrogen atmosphere at 450°C for 1h to obtain Catalysts Ni / AC(50wt%Ni), Pt / AC(0.5wt%Pt), Ru / AC(5wt%Ru). Replace the activated carbon support with SiO 2 , the same method can prepare Ni / TiO 2 (15wt%Ni) catalyst.

Embodiment 2

[0036] References Angew.Chem.Int.Ed.2008,47,8510–8513, Preparation of Ni-W 2 C / AC catalyst: Make a mixed solution of ammonium metatungstate and nickel nitrate according to the weight ratio of tungsten / nickel of 6:1, wherein the mass concentration of ammonium metatungstate is 0.4g / ml. Then, the mixed solution was impregnated with activated carbon support (AC). After oven drying at 120°C for 12 h, the catalyst precursor was placed in H 2 A temperature-programmed carbothermal reaction was carried out in the atmosphere. The specific reaction process was: 1.0g of the precursor was heated from room temperature to 400°C in a quartz reaction tube for 1h, then raised to 700°C at 1°C / min and kept for 1h for carbonization. The hydrogen flow rate was 60ml / min. Obtain Ni-W with 30wt% tungsten loading and 5wt% nickel loading 2 C / AC catalyst, expressed as Ni-W 2 C / AC (5wt%Ni-30wt%W 2 C).

Embodiment 3

[0038] Catalytic conversion experiment: 10.0g cellulose, 0.1g Ru / AC (5wt%Ru) catalyst, 0.03g tungstic acid catalyst and 100ml water were added to a 200ml reactor, 0.2g Ru / AC (5wt%Ru) catalyst was added to In the filter hanging basket, after replacing the gas with hydrogen for three times, fill it with hydrogen to 5MPa, raise the temperature to 240°C, and reflux the reaction solution through a high-pressure liquid pump at a flow rate of 10ml / min. The reaction time is 60min. After the reaction, 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. In the product yield, only the target products ethylene glycol, propylene glycol and hexahydric alcohols (including sorbitol and mannitol) are calculated, and other liquid products include butylene glycol, ethanol, unknown components, and gas products (CO 2 , CH 4 , C 2 h 6 etc.) ...

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Abstract

The present invention relates to a reaction apparatus for preparing a low carbon polyol by catalysis and conversion of a carbohydrate, and a reaction process thereof. The reaction process adopts a high pressure reactor, wherein a catalyst filtering gondola is positioned inside the high pressure reactor, the position of the gondola is higher than the liquid level of the reactant inside the reactor, and the reaction is carried out under a high temperature hydrothermal condition. During the reaction, reactant slurry of the carbohydrate (comprising one or more than two materials selected from cellulose, hemicellulose, sucrose, glucose, fructose, xylose, soluble xylooligosaccharide and starch) flows from the bottom of the reactor, is driven to flow back to the reactor by a high pressure liquid pump, then is injected into the gondola to perform a catalytic reaction with the catalyst inside the gondola, and flows and accumulates on the bottom of the reactor, and the reaction is circulated. With the process, catalyst poisoning and deactivation can be effectively reduced, such that the reaction selectivity and the catalyst life can be improved.

Description

technical field [0001] The invention relates to a preparation method for selective preparation of ethylene glycol or propylene glycol, in particular to a device and a reaction process for the selective one-step catalytic hydrogenation degradation reaction of carbohydrate internal circulation to prepare ethylene glycol or propylene glycol. Background technique [0002] Ethylene glycol and propylene glycol are important energy liquid fuels, and are also very important raw materials for polyester synthesis. For example, ethylene glycol can be used in polyethylene terephthalate (PET), polyethylene naphthalate (PEN ), can also be used as antifreeze, lubricant, plasticizer, surfactant, etc.; 1,2-propanediol can be used to produce unsaturated polyester, epoxy resin, polyurethane resin, and also in the food, pharmaceutical and cosmetic industries Widely used as moisture absorbent, antifreeze, lubricant and solvent. They are widely used organic chemical raw materials. [0003] At p...

Claims

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Application Information

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IPC IPC(8): C07C31/20C07C29/00
CPCY02P20/52
Inventor 郑明远张涛庞纪峰姜宇王爱琴
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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