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Method of recovering tungsten-based catalyst from complex reaction substrate

A complex reaction and catalyst technology, applied in chemical instruments and methods, inorganic chemistry, tungsten compounds, etc., can solve the problems of complex process and low recovery efficiency, and achieve the effect of high recovery efficiency, simple recovery process and convenient economy

Active Publication Date: 2017-06-20
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

In the industry, the organic matter is usually removed by incineration to obtain tungsten oxide, which is then dissolved in alkali and recovered by ammoniation. The process is extremely complicated and the recovery efficiency of the product is low (Document 6: Research on Extracting Tungsten from Tungsten-containing Waste, China Mining Industry, 2008, 17:77-81)

Method used

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  • Method of recovering tungsten-based catalyst from complex reaction substrate
  • Method of recovering tungsten-based catalyst from complex reaction substrate
  • Method of recovering tungsten-based catalyst from complex reaction substrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The catalytic conversion of sugar-containing compounds to produce lower alcohols:

[0028] Add 1.0g of catalyst Ru / C and 50ml of water into a 300ml reactor. After nitrogen is introduced for three times to replace the gas, the temperature is programmed to 220°C. At this time, 40wt% glucose and ammonium metatungstate are pumped into the reactor. In, take the liquid at the same time, the mass space velocity is 2. During the reaction process, the product is taken out, separated on a high-performance liquid chromatography calcium ion exchange column and detected by a differential refractive index detector. Products such as propylene glycol, ethylene glycol and glycerin are calculated in the product yield. This reaction can be carried out in a fixed bed, the operation is similar, the sugar solution, space velocity and reaction temperature are adjustable.

[0029] Depending on the tungsten species, the tungsten catalyst can also be placed in the reaction vessel in advance.

Embodiment 2

[0031] Obtain complex substrates:

[0032] After the reaction, the solution is filtered to remove solid materials, distilled to remove water under reduced pressure, and rectified to obtain ethylene glycol and propylene glycol, and then a mixture of high boiling alcohol and tungsten salt remains.

Embodiment 3

[0034] Extraction experiment:

[0035] Mix the bottom product after rectification with ethanol at a temperature of 10°C and a mass ratio of 1:5, and stir quickly at a stirring speed of 600 rpm to make the bottom product evenly dispersed after rectification and stand for 12 hours. Then it was centrifuged and filtered at a speed of 1000 rpm, washed with ethanol solution 3 times, and dried to obtain a solid powder.

[0036] Mix the bottom product after rectification with ethanol and cyclohexane. The weight ratio of rectification substrate to solvent is 5:1, and the volume ratio of ethanol to cyclohexane is 1:1. Stir quickly at 600rpm. , Make the bottom product evenly dispersed after rectification, stand for 12 hours to separate. Then it was centrifuged and filtered at a speed of 1000 rpm, washed with ethanol solution 3 times, and dried to obtain a solid powder.

[0037] The reaction parameters can be changed according to different experiments to obtain high tungsten salt recovery.

[0...

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Abstract

In reaction for preparing low-carbon alcohol through catalytic conversion of a carbohydrate compound, a tungsten-based catalyst may be wholly or partly dissolved in a reaction substrate, and is difficult to recover, and the cost of the catalyst is increased. The invention provides a method of recovering the tungsten-based catalyst from a complex reaction substrate. The method is characterized in that the complex reaction substrate is a rectification residual product after the catalytic conversion of the carbohydrate compound, after reaction products are subjected to rectification for separation of glycol and propylene glycol, a kettle bottom residual product is obtained, a boiling point of the kettle bottom residual product is greater than or equal to 200 degrees, and the kettle bottom residual product contains tungsten salt; and through adding an organic solvent to the kettle bottom residual product, the tungsten salt is dissolved out and recovered, fusel having a high boiling point is obtained, and a mass recovery rate of the tungsten salt is greater than or equal to 90%. According to the method, a catalyst recovery process is simple, the catalyst recovery efficiency is high, and the cyclic activity of the tungsten-based catalyst is excellent. In addition, the overall process facilitates operation and industrialized production.

Description

Technical field [0001] The invention belongs to the field of catalysis in biomass chemical industry, and particularly relates to the recovery of tungsten salt catalysts, specifically a tungsten salt recovery method after product rectification in the catalytic conversion of sugar compounds. Background technique [0002] Low-carbon 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, they are used in polyethylene terephthalate (PET) and polyethylene naphthalate ( PEN), can also be used as antifreeze, lubricant, plasticizer, surface active agent, etc. It is an organic chemical raw material with a wide range of uses. [0003] At present, the production methods of ethylene glycol and 1,2-propylene glycol mainly include direct hydration and indirect hydration of ethylene oxide and propylene oxide. Although the technologies of various methods are relatively mature, there are...

Claims

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Application Information

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IPC IPC(8): C22B7/00C22B34/36C01G41/00
CPCC01G41/00C22B34/365Y02P10/20
Inventor 庞纪峰郑明远张涛王爱琴王晓东
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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