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Catalyst for CO2 synthesized acetylenic acid and preparation method and application thereof

A catalyst and alkyne technology, which is applied in the direction of carboxylate preparation, organic compound preparation, organic compound/hydride/coordination complex catalyst, etc., can solve the problems of large amount of catalyst, reduced catalyst practicability, sensitivity, etc. Achieving high application potential

Active Publication Date: 2018-10-02
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the research, it was found that the conditions used to realize the reaction were either high temperature and high pressure, or the recycling of the catalyst could not be realized in a homogeneous system
Although Cheng Peng et al. of Nankai University reported a metal-organic framework complex catalyst Ag@MIL-101 loaded with silver nanoparticles (Angew. ) can catalyze the reaction under mild conditions (50 °C, 1 atm) and can be recycled 5 times, but the preparation process of the Ag@MIL-101 catalyst requires additional reducing agents, such as sodium borohydride, and metal-organic framework complexes Sensitive to air, the catalyst needs to be stored in an inert gas
In addition, the catalyzer has a large amount of catalyst in practical application, and the conversion number (TON) of its phenylpropylic acid product is only 36, which greatly reduces the practicability of the catalyzer

Method used

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  • Catalyst for CO2 synthesized acetylenic acid and preparation method and application thereof
  • Catalyst for CO2 synthesized acetylenic acid and preparation method and application thereof
  • Catalyst for CO2 synthesized acetylenic acid and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Ag(1.17wt%) / SiO 2 - Preparation of Schiff catalyst:

[0027] First, measure 1 mL of 3-aminopropyltriethoxysilane and dissolve it in 450 mL of deionized water, and add 2.5 mL of formaldehyde solution with a mass fraction of 37% at 25° C., and continue stirring for 12 h. The resulting white precipitate was filtered, washed with deionized water, and dried at 120 °C for 2 h to obtain the carrier SiO 2 -Schiff. Weigh 200mg SiO 2 -Schiff support, added to 40mL of methanol, and ultrasonically dispersed at room temperature. Then 2 mL of silver nitrate (10 mg) solution was added and sonication was continued for 5 min. After the suspension was separated and washed, the solid product was dried in an oven to obtain the Ag(1.17wt%) / SiO modified by Schiff base. 2 -Schiff catalyst.

Embodiment 2

[0029] Ag(1.36wt%) / SiO 2 - Preparation of Schiff catalyst

[0030] First, measure 1 mL of 3-aminopropyltriethoxysilane and dissolve it in 450 mL of deionized water, and add 2.5 mL of formaldehyde solution with a mass fraction of 37% at 25° C., and continue stirring for 12 h. The resulting white precipitate was filtered, washed with deionized water, and dried at 120 °C for 2 h to obtain the carrier SiO 2 -Schiff. Weigh 200mg SiO 2 -Schiff support, added to 40mL of methanol, and ultrasonically dispersed at room temperature. Then 2 mL of silver nitrate (15 mg) solution was added and sonication was continued for 5 min. After the above-mentioned suspension is separated and washed, the solid product is placed in an oven and dried to obtain the Schiff base-modified Ag (1.36wt%) / SiO 2 -Schiff catalyst.

Embodiment 3

[0032] Ag(1.45wt%) / SiO 2 - Preparation of Schiff catalyst:

[0033] First, measure 1 mL of 3-aminopropyltriethoxysilane and dissolve it in 450 mL of deionized water, and add 2.5 mL of formaldehyde solution with a mass fraction of 37% at 25° C., and continue stirring for 12 h. The resulting white precipitate was filtered, washed with deionized water, and dried at 120 °C for 2 h to obtain the carrier SiO 2 -Schiff. Weigh 200mg SiO 2 -Schiff support, added to 40mL of methanol, and ultrasonically dispersed at room temperature. Then 2 mL of silver nitrate (20 mg) solution was added and sonication was continued for 5 min. After the above-mentioned suspension is separated and washed, the solid product is placed in an oven and dried to obtain the Schiff base-modified Ag (1.45wt%) / SiO 2 -Schiff catalyst.

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Abstract

The invention relates to a preparation method of a Schiff base modified nano-silver based catalyst and application of the catalyst in reaction of CO2 synthesized acetylenic acid. The catalyst uses Schiff base modified silicon oxide as a carrier and uses nanoscale Ag as an active component, and the mass content of the catalyst is 0.1%-10.0%. The catalyst can efficiently catalyze reaction of CO2 andalkyne and convert the CO2 into acetylenic acid under the mild condition. The catalyst has the advantages of easy preparation, high activity and high stability, the yield of phenylpropiolic acid is as high as 99%, the turn over number (TON) of the phenylpropiolic acid is as high as 720, and the method is provided for preparation of the catalyst for efficient synthesis of acetylenic acid and has avery good application prospect.

Description

technical field [0001] The present invention relates to a CO 2 A catalyst for synthesizing alkynoic acid, specifically a preparation method and application of a Schiff base-modified nanometer silver-based catalyst. Background technique [0002] CO 2 The reaction of alkynes to synthesize alkynes has once again aroused widespread interest, not only because alkynes can be used as an important intermediate in medicinal chemistry and organic synthesis, but more importantly, the reduction of greenhouse gases can be achieved through this technology. emission, and realize resource utilization of carbon dioxide. If the technical problem of efficient fixation of carbon dioxide under mild conditions can be overcome, alkynes can be obtained from renewable energy sources (wind, solar, biomass, etc.) on a large scale, which will further increase the CO 2 Economic and technical feasibility of reactions with alkynes for the synthesis of alkynoic acids. Therefore, it is very important to...

Claims

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Application Information

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IPC IPC(8): B01J31/02C07C51/15C07C57/42
CPCB01J31/0275C07C51/15C07C57/42
Inventor 黄延强吴志连杨小峰刘清港樊斯斯张涛
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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