Ordered structure catalyst for hydrogenation of oxalic ester for preparing ethylene glycol and preparation method thereof

A regular structure and catalyst technology, which is applied in the direction of catalyst activation/preparation, chemical instruments and methods, preparation of hydroxyl compounds, etc., can solve the constraints on the industrialization process of oxalate hydrogenation to ethylene glycol technology, increase the particle size of particle catalysts, Catalyst overheating side reactions and other problems, to achieve the effect of shortening the internal diffusion path, increasing the effective contact area, and reducing bed resistance

Active Publication Date: 2010-11-10
TIANJIN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The current research on oxalate hydrogenation to diol catalysts has made some progress, but there are still some problems in further engineering scale-up
Since the hydrogenation of oxalate to ethylene glycol is a very temperature-sensitive reaction, the use of a catalyst bed with a larger aspect ratio is beneficial to control the uniform temperature field of the bed; and the increase of the aspect ratio leads to a decrease in the bed resistance. Increasing the particle size of the particulate catalyst will easily lead to local overheating of the catalyst and aggravation of side reactions
These factors seriously restrict the industrialization process of oxalate hydrogenation to ethylene glycol technology

Method used

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  • Ordered structure catalyst for hydrogenation of oxalic ester for preparing ethylene glycol and preparation method thereof
  • Ordered structure catalyst for hydrogenation of oxalic ester for preparing ethylene glycol and preparation method thereof
  • Ordered structure catalyst for hydrogenation of oxalic ester for preparing ethylene glycol and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Structured Catalyst Preparation

[0046] Weigh 15.5g of copper nitrate pentahydrate and dissolve it in 150ml of water, slowly add 52ml of 25wt.% ammonia water to dissolve it and mix well. 45ml of 30wt.% silica sol was added dropwise to the solution, and after the dropwise addition was completed, it was aged for 4 hours under stirring. Then heat up to 95°C to precipitate copper and silicon oxide. The precipitate was filtered, washed three times with deionized water, dried at 120°C for 12 hours, and calcined at 450°C for 4 hours to form a copper content of 20wt.%, SiO 2 80wt.% Cu / SiO 2 Catalyst raw powder.

[0047] Part of the above Cu / SiO 2 The raw catalyst powder is extruded and sieved into 40-60 mesh, and then 8.0g of the formed Cu / SiO is taken 2 Catalyst particles, 8.0gCu / SiO 2 Catalyst raw powder and 0.5 g of pseudo-boehmite were placed in a ball mill jar, 50 ml of water was added, and ball milled (planetary ball mill XQM-2L, Nanjing Sunco) at a speed of 200 rp...

Embodiment 2

[0052] Weighing 30g Zr(NO 3 ) 4 ·5H 2 O was added to a 200ml beaker, and 100ml of 70% nitric acid was added to dissolve it and adjust the Zr(NO 3 ) 4 The concentration is 2M. Under the stirring state, ammonia water was slowly added dropwise in the solution until the pH was 4.0-5.0, at this time Zr(NO 3 ) 4 The solution is transformed into a translucent zirconium sol, and deionized water is added to adjust the concentration of the zirconium sol to 1 mol / L, and then aged under air atmosphere for 24-48 hours with stirring.

[0053] In addition to adopting 127ml of the above zirconium sol instead of silica sol to prepare copper content of 20wt.%, ZrO 2 80wt.% Cu / ZrO 2 Catalyst former powder and prepare catalyst slurry with it, all the other are with embodiment 1, make the Cu / ZrO that coating weight is 20% of honeycomb carrier 2 / cordierite conformation catalyst.

[0054] The volumetric space velocity of dimethyl oxalate is 0.6h -1 In addition, the catalyst evaluation met...

Embodiment 3

[0056] Weigh 15.25g of copper nitrate pentahydrate dissolved in 120ml of water, slowly add 54.6g of NaHCO 3 Let it dissolve and mix well. 30wt.% silica sol and zirconium colloid prepared in Example 2 were added dropwise to the solution. The volumes of zirconium colloid and silica sol were 16ml and 39ml respectively. After the addition was completed, the mixture was aged for 4 hours under stirring. The temperature is then raised to 95°C to precipitate copper, silica and zirconia. The precipitate was filtered, washed 3 times with deionized water, dried at 120 degrees for 12 hours, and roasted at 450 degrees for 4 hours to form a copper content of 20wt.%, ZrO 2 10wt.% Cu / ZrO 2 -SiO 2 The raw catalyst powder is ready for use.

[0057] Part of the above Cu / ZrO 2 / SiO 2 The raw catalyst powder is extruded and sieved into 40-60 mesh, and then 15.0g of the formed Cu / ZrO 2 -SiO 2 Catalyst particles, 1.0g Cu / ZrO 2 -SiO 2 The raw catalyst powder and 0.5 g of pseudo-boehmite wer...

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PUM

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Abstract

The invention relates to an ordered structure catalyst for hydrogenation of oxalic ester for preparing ethylene glycol and a preparation method thereof. The ordered structure catalyst consists of a honeycomb carrier, an auxiliary agent and an active ingredient and is characterized in that: a ceramic honeycomb or a metal honeycomb is used as the carrier and is in an amount of 30 to 90 percent based on the total weight of the catalyst; oxide of one or more of main group elements of Al and Si, alkaline-earth metals of Ba and Ca, subgroup elements of Ti, Zr, Fe, Zn, Mn and V, and rare-earth metals of La and Ce is used as the auxiliary agent and is in an amount of 5 to 60 percent based on the weight of the honeycomb carrier; Cu is used as the main active ingredient and is in an amount of 1 to 25 percent based on the weight of the honeycomb carrier; the active ingredient copper and the auxiliary agent MOx is supported on the honeycomb carrier in a form of the coating; the coating is in an amount of 10 to 60 percent based on the weight of the honeycomb carrier; and the Cu is in an amount of 10 to 40 percent based on the total weight of the coating. The ordered structure catalyst has the advantages of high activity, high selectivity of the ethylene glycol, environmental friendliness, no pollution and adaptability to large-scale industrialized production.

Description

technical field [0001] The invention relates to a catalyst with a regular structure for oxalate hydrogenation to ethylene glycol and a preparation method thereof. The ceramic honeycomb or metal honeycomb is used as the carrier, copper is the main active component of the catalyst, and the auxiliary agent is composed of main group metals or transition metals. oxide composition. The catalyst can be used in a fixed-bed catalytic reactor to hydrogenate oxalate to produce ethylene glycol and obtain higher ethylene glycol selectivity and yield. Background technique [0002] Ethylene glycol is an important basic organic raw material. Ethylene glycol was first produced by Wurtz in 1859 by hydrolyzing ethylene glycol diacetate with potassium hydroxide. During the First World War, people used ethylene glycol dinitrate to lower the freezing point of glycerin to replace glycerin in the production of explosives. Subsequently, researchers developed a variety of feasible production proce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72B01J23/889B01J23/83B01J23/80C07C31/20C07C29/149
CPCB01J23/72B01J23/80C07C31/20C07C29/149B01J35/04B01J23/76B01J23/889B01J37/02B01J37/0215B01J23/83B01J23/8892Y02P20/52C07C31/202
Inventor 马新宾赵玉军岳海荣王胜平吕静王保伟李振花徐艳
Owner TIANJIN UNIV
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