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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

AI Technical Summary

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 occur on certain types of molecular sieves such as ZSM series, there are May increase the efficiency of the hydrogenation reaction

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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Embodiment 1

[0023] Weigh 6.84g of copper nitrate trihydrate, dissolve it in 100mL of deionized water, add 28wt% ammonia solution dropwise under stirring until the precipitate disappears, and obtain a transparent dark blue solution, which is transferred into a glass with 0.06g of HX molecular sieve In the container, in the state of strong mechanical stirring, slowly drop 10.35g of 40wt% silica sol and 20ml of 20wt% urea aqueous solution at a speed of about 1ml / min successively, raise the temperature to 60°C and stir at a speed of 500r / min for 8h, after cooling, After the precipitate was washed to neutral, it was dried at 120°C for 12 hours, placed in a muffle furnace at a rate of 4°C / min to 350°C, and calcined for 2 hours to obtain a catalyst precursor. Press the tablet and sieve out 40~60 mesh particles, put the catalyst into the reactor, under 5% H 2 30% Cu / SiO was obtained by reducing the temperature at 2°C / min to 350°C for 4 hours under / Ar atmosphere 2 -1% HX catalyst, ICP-MS quantit...

Embodiment 2

[0027] Weigh 6.84g copper nitrate trihydrate, dissolve it in 100mL deionized water, add 28wt% ammonia solution dropwise under stirring until the blue precipitate disappears, transfer it into a glass container equipped with 0.16g HY molecular sieve, and stir it vigorously 10.20g of 40wt% silicate and 30ml of 20wt% urea aqueous solution were slowly dropped at a speed of about 1ml / min, and the temperature of the water bath was raised to 70°C and stirred at a speed of 400r / min for 8h. After cooling, the precipitate After suction filtration and washing to neutrality, dry at 120°C for 12h, place in a muffle furnace to raise the temperature to 450°C at a rate of 4°C / min, and calcinate for 4h to obtain a catalyst precursor. Press the tablet and sieve out 40~60 mesh particles, put the catalyst into the reactor, under 5% H 2 30% Cu / SiO was obtained after reduction at 1°C / min to 320°C for 4 hours under Ar atmosphere 2 -3% HY catalyst, ICP-MS analysis results show that the copper content...

Embodiment 3

[0030] Weigh 6.59g copper acetate monohydrate, dissolve it in 120mL deionized water, add 28wt% ammonia solution dropwise under stirring until the blue precipitate disappears, and transfer it into ) in a glass container under strong mechanical stirring, slowly drop 9.47g of 40wt% silica sol and 30ml of 20wt% urea aqueous solution successively at a speed of about 1ml / min, and raise the temperature of the water bath to 70°C at a speed of 400r / min After stirring for 6 hours, after cooling, the precipitate was filtered and washed until neutral, dried at 120°C for 12 hours, placed in a muffle furnace at a rate of 4°C / min to 450°C, and calcined for 4 hours to obtain a catalyst precursor. Press the tablet and sieve out 40~60 mesh particles, put the catalyst into the reactor, under 5% H 2 35% Cu / SiO was obtained after reduction at 1°C / min to 320°C for 4 hours under Ar atmosphere 2 -5% HZSM-5 catalyst, ICP-MS analysis results show that the copper content is 32.7wt%; after nitrogen stat...

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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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