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Catalyst for preparing ethylene glycol by dimethyl oxalate hydrogenation, and preparation and use thereof

A technology of dimethyl oxalate and catalyst, which is applied in the field of catalyst and its preparation for the hydrogenation of dimethyl oxalate to ethylene glycol, can solve the problems of low space-time yield, high pressure, high temperature, etc., to improve catalyst activity, The effect of reducing investment costs and mild reaction conditions

Active Publication Date: 2011-08-17
山东华鲁恒升集团德化设计研究有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Since the 1980s, countries all over the world have applied for a series of patents for oxalate-based ethylene glycol catalysts. The disadvantages are harsh reaction conditions (high temperature, high pressure), high energy and power consumption, and low conversion and selectivity of the reaction. Not very ideal, the space-time yield is not high; the dependence on metal chromium is large; the life of the catalyst is short, not suitable for industrial production

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  • Catalyst for preparing ethylene glycol by dimethyl oxalate hydrogenation, and preparation and use thereof

Examples

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preparation example Construction

[0039] The preparation method of catalyst provided by the invention is as follows:

[0040] Soluble salts of active metals (one or any combination of two or more of copper nitrate, copper halide, copper acetate and copper sulfate) and soluble salts of auxiliary metals (nitrate of zinc, magnesium, aluminum, silver, ruthenium or iridium) Salt, acetate or sulfate, one or any combination of two or more) are mixed and dissolved to prepare an aqueous solution, wherein the concentration of active metal ions and auxiliary metal ions is 0.1-1.5M, and the silicon source (silica sol) of the carrier Add to the mixed solution to form a mixed solution A, stir well. Dissolve the precipitating agent in water to prepare aqueous solution B with a concentration of 0.1-1.5M. Under the condition of stirring, slowly drop the mixed solution A into the precipitant aqueous solution B, keep the temperature at 50-90°C during the dropping process, adjust the pH value to 6-9, continue stirring for 2-4 ho...

Embodiment 1

[0043] Weigh 25 grams of copper nitrate, 5 grams of magnesium nitrate, and 3 grams of iridium nitrate and dissolve them in water to form an aqueous solution with a total metal ion concentration of 1.0 M, and add 60 mL of silica sol with a mass percentage concentration of 25% to prepare a mixed solution. Weigh 30 grams of sodium carbonate and dissolve it in 200ml of water, place in a 60°C water bath, under stirring, slowly add the mixture into the aqueous sodium carbonate solution, and adjust the pH value to about 7.5 with nitric acid or sulfuric acid. Continue to stir for 2 hours after mixing, filter, wash until the conductivity of the washing liquid is less than 500us / cm, dry at 100°C for 12 hours, heat up to 400°C at 10°C / h in a muffle furnace, and roast at this temperature After 4 hours, granulate in a micro granulator to obtain a catalyst precursor. 20ml of 40-60 mesh catalyst precursors are loaded into the reactor, and 10ml of 20-40 mesh inert ceramic balls are loaded on ...

Embodiment 2

[0049] Weigh 20 grams of copper sulfate, 5 grams of zinc sulfate, and 1 gram of ruthenium nitrate and dissolve them in water to form an aqueous solution with a total metal ion concentration of 0.5 M, and add 50 mL of silica sol with a concentration of 30% by mass to obtain a mixed solution. Weigh 30 grams of sodium bicarbonate and dissolve it in 200ml of water, put it in a water bath at 70°C, under stirring, slowly add the mixed solution into the aqueous sodium bicarbonate solution, and control the pH value of the mixed solution at about 8.5. After mixing, continue to stir for 2 hours, filter, wash until the conductivity of the washing liquid is less than 500us / cm, dry at 90°C for 12 hours, heat up to 450°C at 10°C / h in a muffle furnace, and roast at a constant temperature at this temperature After 4 hours, granulate in a micro granulator to obtain a catalyst precursor. 20ml of 40-60 mesh catalyst precursors are loaded into the reactor, and 10ml of 20-40 mesh inert ceramic bal...

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Abstract

The invention discloses a catalyst for preparing ethylene glycol by dimethyl oxalate hydrogenation, which is characterized by containing the following components by weight percent: 30 to 60% of active metal, 5 to 30% of metal additive and 20 to 60% of carrier, wherein the active metal is one or any combination of more than two of the group consisting of zinc, magnesium, aluminum, silver, ruthenium and iridium, and the carrier is silicon dioxide. The invention further discloses a preparation method of the catalyst, comprising the steps of: 1) mixing and dissolving soluble salts of the copper and soluble salts of the metal additive to prepare aqueous solution, adding a silicon source of the carrier to the aqueous solution to form a mixed liquid A; 2) dissolving precipitating agent in water,dropwise adding the mixed solution A to aqueous solution B under stir, and put the resultant solution on standing; 3) filtering; 4) drying; 5) calcining; 6) forming; and 7) reducing. The catalyst of the invention has the advantages of moderate reaction conditions, high activity, good stability, high selectivity, environmental friendliness and simple preparation process.

Description

technical field [0001] The invention relates to a catalyst for producing ethylene glycol by a coal-based method, in particular to a catalyst for synthesizing ethylene glycol by hydrogenation of dimethyl oxalate and a preparation method thereof. Background technique [0002] Ethylene glycol, commonly known as glycol, is an important organic chemical raw material. It can be mixed with water in any proportion. It has a high boiling point and a low freezing point. Ethylene glycol reacts with terephthalic acid to form polyethylene terephthalate , can be used as a raw material for polyester fiber and polyester plastic, widely used in lubricants, plasticizers, paints, adhesives, surfactants, explosives, etc., and can also be used to prepare antifreeze or directly as an organic solvent In addition, the dinitrate of ethylene glycol can also be used as explosives, and the steam generated after heating can be used as a stage smoke screen, and it is also indispensable for the production...

Claims

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Application Information

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IPC IPC(8): B01J23/80B01J23/72B01J23/89C07C31/20C07C29/149
CPCY02P20/52
Inventor 潘得胜于富红刘春丽
Owner 山东华鲁恒升集团德化设计研究有限公司
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