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Catalyst for synthesizing ethylene glycol by oxalate hydrogenation, and preparation method and application method of catalyst

A catalyst and ethylene glycol technology, applied in the direction of catalyst activation/preparation, carboxylate preparation, chemical instruments and methods, etc., can solve the problems of increased production cost, no breakthrough development, high performance requirements, etc., and achieve inhibition of agglomeration , shorten the pretreatment time, solve the effect of high temperature and easy sintering

Active Publication Date: 2017-04-19
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in practical applications, too high hydrogen-ester ratio also requires high performance of the circulating compressor, which will greatly increase the production cost.
[0005] At present, the research on the modification of additives has achieved certain results, and indeed the performance of catalyst hydrogenation has been greatly improved, but no breakthrough has been achieved.

Method used

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  • Catalyst for synthesizing ethylene glycol by oxalate hydrogenation, and preparation method and application method of catalyst
  • Catalyst for synthesizing ethylene glycol by oxalate hydrogenation, and preparation method and application method of catalyst
  • Catalyst for synthesizing ethylene glycol by oxalate hydrogenation, and preparation method and application method of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Catalyst preparation

[0023] A. Dissolve 10.6g of copper nitrate and 0.5g of mannitol in 100g of distilled water. After fully dissolving, put them in an ultrasonic instrument for 20 minutes of ultrasonic oscillation with an ultrasonic frequency of 25kHz.

[0024] B. Add 5.0g of urea to the above solution and stir to dissolve, then add 20ml of ammonia water and stir for 30min,

[0025] C. Finally add 21g SiO drop by drop 2 For the alkaline silica sol with a content of 40%, the mixed solution was mechanically stirred and placed in a water bath at 80° C. for 3 to 6 hours, and then stopped heating until the pH value of the solution was close to 7. The filter cake was obtained by filtration, and the filter cake was washed several times with distilled water, and the resulting filter cake was dried in air at 120°C for 24 hours to obtain Cu / SiO 2 catalyst precursors.

[0026] Cu / SiO 2 The precursor of the catalyst was pressed into tablets and sieved to obtain particles wit...

Embodiment 2

[0030] In Example 1, the mannitol in the catalyst preparation step was changed to 2.0 g of citric acid, namely the cost example.

[0031] The performance evaluation conditions are the same as in Example 1, and the results of selective hydrogenation of dimethyl oxalate to ethylene glycol after 24 hours are shown in Table 1.

Embodiment 3

[0033] In Example 1, the mannitol in the catalyst preparation step was changed to 1.0 g of glucose, which is the cost example.

[0034] The performance evaluation conditions are the same as in Example 1, and the results of selective hydrogenation of dimethyl oxalate to ethylene glycol after 24 hours are shown in Table 1.

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Abstract

The invention provides a catalyst for synthesizing ethylene glycol by oxalate hydrogenation, and a preparation method and an application method of the catalyst. The preparation method comprises the steps of taking copper nitrate and copper acetate as copper sources, taking alkaline silica gel as a silicon source, and taking urea and ammonia water as a precipitant; adding a multi-hydroxyl organic matter; and preparing a Cu / SiO2 catalyst with a deposition-precipitation method. According to the method, the dimension and dispersity of copper species are adjusted and controlled by adding the multi-hydroxyl organic matter in the preparation process, and the aggregation of the copper species is inhibited by utilizing carbon deposition, so that the problem of easy sintering of the copper species at a high temperature is better solved. The application method for applying the catalyst to the synthesis of ethylene glycol by oxalate hydrogenation comprises the steps of firstly enabling the organic matter on the catalyst to form the carbon deposition at a relatively high temperature in an inert atmosphere; secondly switching inert gas to hydrogen in a cooling process after carbon deposition formation; and finally when the temperature is reduced to a reaction temperature, performing subsequent hydrogenation synthesis. The method has the characteristics that the catalyst does not need to be pre-roasted before use, and hydrogen pre-reduction does not need to be carried out for a long time, so that the preparation and use costs of the catalyst can be reduced.

Description

technical field [0001] The invention relates to the preparation of a catalyst for synthesizing ethylene glycol through the hydrogenation of lower oxalate. In particular, it relates to a preparation method of a catalyst for hydrogenation of dimethyl oxalate to synthesize ethylene glycol. Background technique [0002] Ethylene glycol (EG) is an important organic chemical raw material, which can be used in the production of polyester fibers, plastics, rubber, antifreeze, unsaturated polyester resins, lubricants and explosives, and has a wide range of uses. At present, the main method of industrial synthesis of ethylene glycol is the traditional petroleum route, that is, the oxidation of ethylene to ethylene oxide (EO), and then the hydration of ethylene oxide to ethylene glycol. Syngas hydrogenation of oxalate to ethylene glycol is an emerging route for the synthesis of bulk chemicals by non-petroleum routes. Glycols, especially synthesis gas hydrogenation of oxalate to ethyl...

Claims

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Application Information

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IPC IPC(8): B01J23/72C07C29/149C07C31/20C07C67/31C07C69/675
CPCY02P20/52B01J23/72B01J37/086C07C29/149C07C67/31C07C31/202C07C69/675
Inventor 姚元根林凌叶闰平李斌孙明玲杨锦霞周张锋覃业燕
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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