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Catalyst used for preparing glycol from hydrogenation of oxalates and preparation method thereof

A catalyst, ethylene glycol technology, applied in chemical instruments and methods, hydroxyl compound preparation, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of unmentioned catalyst stability, decrease in copper active surface area, The problem of catalyst activity decline, etc., to achieve excellent low-temperature catalytic activity, easy industrial scale production, and improved performance.

Inactive Publication Date: 2010-06-30
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because copper-based catalysts are prone to copper aggregation and sintering under reaction conditions, the active surface area of ​​copper decreases, resulting in a decrease in catalyst activity.
From literature result, although the oxalate hydrogenation copper catalyst of silicon oxide base is better in activity, stability is not as good as copper chromium base catalyst (U.S. Patent US 4,112,245; ), most of the literature did not mention the catalyst stability

Method used

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  • Catalyst used for preparing glycol from hydrogenation of oxalates and preparation method thereof
  • Catalyst used for preparing glycol from hydrogenation of oxalates and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1: Weighing pipe diameter is 20~40nm, purity 98%, length 1~2μm, specific surface area 180m 2 8.0 g of multi-walled carbon nanotubes / g was put into a round-bottomed flask, and 250 mL of concentrated nitric acid was added, stirred at 90°C for 12 hours, cooled to room temperature, washed with deionized water until neutral, and dried at 120°C Backup.

[0027] Weigh 4.57g of copper nitrate trihydrate, dissolve it in 50mL of deionized water, add 28wt% ammonia solution dropwise under stirring until the precipitate disappears, and obtain a transparent dark blue copper ammonia complex solution, which is transferred into a prepacked 0.30g 11.25g of 40wt% silica sol and 10mL of 20wt% urea aqueous solution were slowly dropped into the glass container of the treated multi-walled carbon nanotubes under strong mechanical stirring at a rate of about 1mL / min, and the temperature was raised to above 60°C. Stir at a speed of 500r / min for 8h, after cooling, wash the precipitate...

Embodiment 2

[0029] Embodiment 2: The specification and pretreatment method of carbon nanotubes are the same as in Embodiment 1.

[0030] The preparation method of the carbon nanotube-promoted copper-silicon-based catalyst is the same as in Example 1, but the addition of multi-walled carbon nanotubes and 40wt% silica sol is changed to 0.6g and 10.5g, and the other compositions are unchanged, and a carbon nanotube-promoted type is obtained. Copper-silicon-based catalyst 20Cu / SiO 2 -10CNTs_12-A, ICP-MS analysis results show that the copper content is 17.7wt%. The activity evaluation and product analysis conditions of the catalyst for the hydrogenation of dimethyl oxalate to ethylene glycol are the same as in Example 1, and the results are shown in Table 1.

Embodiment 3

[0031] Embodiment 3: The specification and pretreatment method of carbon nanotubes are the same as in Embodiment 1.

[0032] The preparation method of the carbon nanotube-promoted copper-silicon-based catalyst is the same as in Example 1, but the addition of multi-walled carbon nanotubes and 40wt% silica sol is changed to 0.9g and 9.8g, and the other compositions are unchanged, so that the carbon nanotube-promoted Copper-silicon-based catalyst, denoted as 20Cu / SiO 2 -15CNTs_12-A, ICP-MS analysis results show that the copper content is 19.1wt%; after nitrogen static adsorption test, the specific surface area is 323.0m 2 / g, the pore volume (the range of pore diameter is 1.7~300nm) is 0.95ml / g, and the average pore diameter is 11.1nm; figure 1 . The activity evaluation and product analysis conditions of the catalyst for the hydrogenation of dimethyl oxalate to ethylene glycol are the same as in Example 1, and the results are shown in Table 1.

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Abstract

The invention relates to a catalyst used for preparing glycol from hydrogenation of oxalates and a preparation method thereof. The invention is characterized in that carbon nano tubes are added in hydrogenation of oxalates catalyst for preparing efficient carbon nano tube glycol copper-silicon based catalyst with promoting effect for hydrogenation of oxalates, which has environmentally friendly features, high activity and high selectivity. The catalyst contains copper, silicon dioxide and carbon nano tubes. The chemical formula of the catalyst is xCu / SiO2-yCNTs, wherein x% indicates that the mass percent of copper in the catalyst is x%, y% indicates that the mass percent of the carbon nano tubes in the catalyst is y%, and CNTs indicates multi-wall carbon nano tubes. The catalyst contains the ingredients in mass percent: 5-60 of Cu, 0.5-30 of CNTs and balance of SiO2. The catalyst is prepared in a method of coprecipitation, and is obtained after oven-drying, furnacing and reduction.

Description

technical field [0001] The invention relates to a catalyst, in particular to a catalyst for hydrogenating oxalate to ethylene glycol and a preparation method thereof. Background technique [0002] Ethylene glycol (EG) is an important organic chemical raw material, mainly used in the production of polyester, antifreeze, adhesives, paint solvents, cold-resistant lubricants, non-ionic surfactants, explosives and plasticizers, etc., especially polyester. At present, the industrial production of ethylene glycol mainly adopts the petroleum route of ethylene oxide hydration method, ethylene is the direct raw material, and naphtha is the indirect raw material. However, with the decline of petroleum resources, it is necessary to explore non-petroleum routes for energy and chemical production. appear more important. From the perspective of existing technology, the promising non-petroleum route of ethylene glycol synthesis mainly includes coal-to-ethylene glycol and biomass-to-ethyle...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72B01J21/18C07C31/20C07C29/149
CPCY02P20/52
Inventor 林海强何萍何喆袁友珠
Owner XIAMEN UNIV
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