Oxalic ester hydrogenated copper silicon catalyst and preparation method thereof

A technology of catalyst and oxalate, which is applied in molecular sieve catalysts, chemical instruments and methods, preparation of hydroxyl compounds, etc., to achieve the effects of easy large-scale production, high dispersion of copper, and simple preparation process

Inactive Publication Date: 2011-06-15
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, there are literatures (Chem.Eur.J.2007, 13, 6502-6507; Appl.Catal.A 2000, 202: 179-182) that hydrogen overflow can o

Method used

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  • Oxalic ester hydrogenated copper silicon catalyst and preparation method thereof
  • Oxalic ester hydrogenated copper silicon catalyst and preparation method thereof

Examples

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Example Embodiment

[0022] Example 1

[0023] Weigh 6.84g copper nitrate trihydrate, dissolve it in 100mL deionized water, add 28wt% ammonia solution dropwise under stirring until the precipitation disappears, and obtain a transparent dark blue solution, which is transferred to the glass containing 0.06g HX molecular sieve In the container, under strong mechanical stirring, slowly drop 10.35g of 40wt% silica sol and 20ml of 20wt% urea aqueous solution at a rate of about 1ml / min. The temperature is raised to 60°C and stirred at a rate of 500r / min for 8h. After cooling, After the precipitate was washed to neutrality, it was dried at 120°C for 12 hours, placed in a muffle furnace at a heating rate of 4°C / min to 350°C, and calcined for 2 hours to obtain a catalyst precursor. Tablets are sieved to obtain 40-60 mesh particles, and the catalyst is put into the reactor. 2 / Ar atmosphere, heat up at 2℃ / min to 350℃ and reduce for 4h to obtain 30%Cu / SiO 2 -1% HX catalyst, ICP-MS quantitative analysis results s...

Example Embodiment

[0026] Example 2

[0027] Weigh 6.84g copper nitrate trihydrate, dissolve it in 100mL deionized water, add dropwise 28wt% ammonia solution under stirring until the blue precipitate disappears, transfer it into a glass container containing 0.16g HY molecular sieve, and stir it under strong mechanical stirring. Under the state, slowly drop 10.20g of 40wt% silicate and 30ml of 20wt% urea aqueous solution at a speed of about 1ml / min. The water bath is heated to 70℃ and stirred at 400r / min for 8h. After cooling, the precipitate After suction filtration and washing to neutrality, drying at 120°C for 12h, placing it in a muffle furnace at a heating rate of 4°C / min to 450°C, calcining for 4h to obtain a catalyst precursor. Tablets are sieved to obtain 40-60 mesh particles, and the catalyst is put into the reactor. 2 / Ar atmosphere, heating up at 1℃ / min to 320℃ and reducing for 4h to obtain 30%Cu / SiO 2 -3% HY catalyst, ICP-MS analysis results show that the copper content is 29.1wt%; after...

Example Embodiment

[0029] Example 3

[0030] Weigh 6.59g of copper acetate monohydrate, dissolve it in 120mL of deionized water, add dropwise 28wt% aqueous ammonia solution under stirring until the blue precipitate disappears, and transfer it into a 0.3g H-type ZSM-5 molecular sieve (silica to aluminum ratio of 38 ) In a glass container under strong mechanical stirring, slowly drop 9.47g of 40wt% silica sol and 30ml of 20wt% urea aqueous solution at a rate of about 1ml / min. The water bath is heated to 70°C at a rate of 400r / min After stirring for 6 hours, after cooling, the precipitate was suction filtered and washed to neutrality, dried at 120°C for 12 hours, placed in a muffle furnace at a heating rate of 4°C / min to 450°C, and calcined for 4 hours to obtain a catalyst precursor. Tablets are sieved to obtain 40-60 mesh particles, and the catalyst is put into the reactor. 2 / Ar atmosphere, heating up at 1℃ / min to 320℃ and reducing for 4h, 35%Cu / SiO is obtained 2 -5% HZSM-5 catalyst, ICP-MS analysis...

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Abstract

The invention discloses an oxalic ester hydrogenated copper silicon catalyst and a preparation method thereof, and relates to a catalyst used in preparation of ethylene glycol by using oxalic ester hydrogenation. The invention provides the silicon-aluminum molecular sieve promoted oxalic ester hydrogenated copper silicon catalyst with environmental friendliness, high activity and high thermal stability for synthesizing the ethylene glycol by oxalic ester hydrogenation and a preparation method thereof. The catalyst comprises copper, silicon dioxide and silicon-aluminum molecular sieve, the composition of the catalyst is expressed as x%Cu/SiO2-y% silicon-aluminum molecular sieve, in the formula, x% expresses the mass percentage of the copper in the catalyst, and y% expresses the mass percentage of the silicon-aluminum molecular sieve in the catalyst. The catalyst comprises the following components in percentage by mass: 5 to 60 percent of Cu, 0.5 to 30 percent of silicon-aluminum molecular sieve, and the balance of SiO2. The preparation method comprises the following steps of: preparing a catalyst precursor, and reducing the catalyst precursor under hydrogen-containing atmosphere toobtain the oxalic ester hydrogenated copper silicon catalyst.

Description

technical field [0001] The invention relates to a catalyst for hydrogenating oxalate to prepare ethylene glycol. Background technique [0002] With the shortage of petroleum resources, it is of great strategic and economic significance to develop and utilize my country's relatively abundant coal and natural gas resources, and to develop carbon-one chemical industry. Among them, carbon-one chemical industry uses CO as raw material to prepare oxalate and its downstream products are carbon-one chemical industry important issues for development. Ethylene glycol (EG), also known as glycol and ethylene glycol, is an important organic chemical raw material. It is currently mainly used in the production of polyester, antifreeze, adhesives, paint solvents, cold-resistant lubricants, non- Ionic surfactants, explosives and plasticizers, etc. Among them, polyester is the main consumption area of ​​ethylene glycol and is the main factor driving the production and consumption of ethylene ...

Claims

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Application Information

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IPC IPC(8): B01J29/14B01J29/24B01J29/46B01J29/68B01J29/76C07C31/20C07C29/149
CPCY02P20/52
Inventor 林海强何喆段新平袁友珠
Owner XIAMEN UNIV
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