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A metal-organic framework-based copper-silicon catalyst and its preparation and application

A technology of metal-organic frameworks and catalysts, applied in catalyst activation/preparation, preparation of organic compounds, preparation of hydroxyl compounds, etc., can solve the problems of copper agglomeration, poor thermal stability, easy sintering and decomposition, etc., and achieve small particle size and high stability Good, excellent physical properties

Active Publication Date: 2021-07-16
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the poor thermal stability of MOFs, it is easy to sinter and decompose under high temperature conditions, resulting in copper agglomeration, so it is necessary to further load MOFs onto SiO 2 on other carriers

Method used

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  • A metal-organic framework-based copper-silicon catalyst and its preparation and application
  • A metal-organic framework-based copper-silicon catalyst and its preparation and application
  • A metal-organic framework-based copper-silicon catalyst and its preparation and application

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Embodiment 1: Prepare Cu / SiO with copper acetate as copper source 2 -1 catalyst

[0029] A. Dissolve 1.5g of copper acetate monohydrate and 1.05g of trimesic acid in 8mL of absolute ethanol, stir for 20min, then sonicate for 30min, then react at 65°C for 48h, cool and filter, and wash with absolute ethanol several times filter cake, place the filter cake in a 50°C oven and dry for 5 hours to obtain a metal-organic framework [Cu 3 (BTC) 2 ]. 5.0 g [Cu 3 (BTC) 2 ] was added to a mixed solution of 22.0g distilled water, 37.0g absolute ethanol and 28.5g tetraethyl orthosilicate, stirred at a constant temperature in a water bath at 65°C for 1 to 3 hours to form a sol-gel; aged at room temperature for 24 hours , and then carry out programmed temperature-controlled drying in an oven. The drying program is to dry at 65°C for 7h, at 70°C for 7h, at 100°C for 40h, and then at 120°C for 4h to obtain the dried [Cu 3 (BTC) 2 ] / SiO 2 -1 sample.

[0030] B. Combine the above ...

Embodiment 2

[0039] Embodiment 2: Prepare Cu / SiO with copper nitrate as copper source 2 -2 Catalyst

[0040] Cu / SiO 2 -2 The preparation steps of the catalyst are as follows: Dissolve 2.34g of copper nitrate trihydrate in 50mL of absolute ethanol at 60°C, then add 50mL of N,N-dimethylformamide containing 1.35g of trimesic acid solution, and continuously After stirring for 20 minutes, put it in an ultrasonic instrument for 60 minutes of ultrasonic oscillation, then transfer it to a reaction kettle at 85 ° C for 12 hours and then filter it. The cake was dried in an oven at 60°C for 6 hours to obtain a metal-organic framework [Cu 3 (BTC) 2 ]. 4.0g [Cu 3 (BTC) 2 ] was added to a mixed solution of 17.6g of distilled water, 29.6g of absolute ethanol and 22.8g of tetraethyl orthosilicate, stirred at a constant temperature in a water bath at 70°C for 1 to 3 hours to form a sol-gel; it was aged at room temperature for 24 hours , and then carry out programmed temperature-controlled drying in ...

Embodiment 3

[0042] Embodiment 3: increase calcination temperature and time to prepare Cu / SiO 2 -3 Catalyst

[0043] Cu / SiO 2 The preparation steps of -3 catalyst are as follows: prepare [Cu by embodiment 1 step A 3 (BTC) 2 ] / SiO 2 -3 samples, and then placed in a muffle furnace at 500 ° C for 8 h, and then in a pure hydrogen atmosphere of 200 mL / min, the temperature was raised to 300 ° C for 4 h reduction, and the prepared catalyst was expressed as Cu / SiO 2 -3. Among them, the Cu loading is 8.27%; the specific surface area of ​​the catalyst is 406.8m 2 g -1 .

[0044] According to the evaluation conditions of Example 1, the hydrogenation reaction activity of dimethyl oxalate was evaluated, and the results are shown in Table 1.

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Abstract

The invention provides a metal-organic framework-based copper-silicon catalyst as well as its preparation and application. The preparation method of the catalyst is to prepare metal-organic framework-containing [Cu 3 (BTC) 2 ] / SiO 2 sample, and then roast the sample at high temperature to degrade the organic components and activate the active components with hydrogen reduction to obtain Cu / SiO 2 catalyst. The metal-organic framework-based copper-silicon catalyst, including SiO as a support 2 Cu, Cu with catalytic active sites and different valence composition + ‑O‑Si and Cu 2 O composite particles, wherein the active component Cu accounts for 4-25% of the mass of the carrier, preferably 6-18%; the particle size of the Cu particles on the surface is 3.5-9nm, and the specific surface of the catalyst is 100-500m 2 / g, the conversion rate of dimethyl oxalate when the catalyst is used in the hydrogenation reaction of dimethyl oxalate is 98.5-99.9%, the selectivity of ethylene glycol is 92.7-98.6%, and the service life is more than 500h.

Description

technical field [0001] The invention relates to a nanometer catalyst and a preparation method thereof, in particular to a novel catalyst based on a metal organic framework material and its application in the hydrogenation reaction of dimethyl oxalate. Background technique [0002] After more than 30 years of exploration, the world's first 200,000 tons / year coal-to-ethylene glycol (EG) project jointly developed by the Fujian Institute of Material Structure of the Chinese Academy of Sciences, Jiangsu Danhua Group and Shanghai Jinmei Chemical New Technology Co., Ltd. was launched in 2011 Tongliao, Inner Mongolia, was successfully put into operation in December 2019, and then coal-to-ethylene glycol projects were rapidly rolled out across the country. However, judging from the current operation of domestic coal-to-ethylene glycol projects, there are still several problems. One of the problems is that the stability of copper-based catalysts in the hydrogenation process of oxalate...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/72B01J35/10B01J37/03B01J37/08B01J37/18C07C31/20C07C29/149
CPCY02P20/52
Inventor 姚元根叶闰平林凌覃业燕孙明玲杨锦霞张鑫陈冲冲
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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