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Mild removal method of surfactant in nano-catalyst

A technology of nano-catalysts and surfactants, applied in chemical instruments and methods, catalyst activation/preparation, physical/chemical process catalysts, etc., can solve problems such as hindering catalytic reactions, particles are prone to agglomeration, and active area reduction, etc., to achieve Small damage to the microstructure, simple operation, and high catalytic activity

Inactive Publication Date: 2021-06-18
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

However, the size and shape of the nano-particles after high-temperature heat treatment change, and the particles are prone to agglomeration, resulting in a sharp decrease in the active area, thereby affecting the catalytic activity.
In addition, the carbon-containing organic macromolecule surfactant may generate some organic fragments after degradation, which will continue to be adsorbed on the surface of nanoparticles, occupy the active sites on the surface of nanocatalysts, and hinder the catalytic reaction.

Method used

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  • Mild removal method of surfactant in nano-catalyst
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  • Mild removal method of surfactant in nano-catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Adopt oleylamine method to prepare Pt / C catalyst, concrete steps are as follows: Weigh 94.4mg Pt(acac) 2 and dissolved in a mixed solution (50 mL) containing tetralin (40 mL) and oleylamine (OAm) (10 mL). Weighed 189.8 mg of carbon carrier (VulcanXC-72R) into the above solution and stirred ultrasonically for 10 min. 4.0 mL of oleylamine, 88.8 mg of borane-tert-butylamine complex (TBAB) and 36.0 mL of tetralin were mixed, vigorously stirred for 10 minutes, and then quickly injected into the Pt precursor solution. Raise the temperature to 200°C and keep it for 6 hours. After the reaction is completed and cooled at room temperature, add 50mL of ethanol to make the Pt / C nanoparticles settle at the bottom of the container, remove the supernatant, and store the obtained solid sample in a vacuum drying oven. Dry overnight at 60°C and record it as Pt / C-OAm. Disperse 100mg of Pt / C-OAm ground into powder in 100ml of acetone-water (volume ratio: 6:4) mixed solution, and ultrasoni...

Embodiment 2

[0031] Adopt ethylene glycol method to prepare Pt / C catalyst, concrete steps are as follows: weigh H 2 PtCl 6 6H 2O (270 mg) was dissolved in an ethylene glycol solution (100 mL) containing PVP (55000 molecular weight, 500 mg). Weigh 150 mg of carbon carrier (VulcanXC-72R) and add it to the above solution, and ultrasonically disperse for 30 minutes to make the carbon evenly dispersed. The mixed solution was heated to 130°C and maintained for 6 hours. After the reaction was completed and cooled at room temperature, it was filtered and washed, and the obtained solid sample was dried overnight at 60°C in a vacuum oven and recorded as Pt / C-PVP . Disperse 500 mg of Pt / C-PVP ground into powder in 100 ml of acetone-water (volume ratio 9:1) mixed solution. After ultrasonic dispersion, heat up and react in a water bath at 80 °C for 10 h under magnetic stirring conditions. The above Centrifuge the mixed solution for solid-liquid separation, the speed is 8000rpm, and the time is 5 m...

Embodiment 3

[0033] Adopt ethylene glycol method to prepare Pt / C catalyst, concrete steps are as follows: weigh H 2 PtCl 6 6H 2 O (270 mg) was dissolved in ethylene glycol solution (100 mL) containing CTAB (200 mg). Weigh 150 mg of carbon carrier (Vulcan XC-72R) into the above solution, and ultrasonically disperse for 30 minutes to make the carbon evenly dispersed. The mixed solution was heated to 130°C and maintained for 6 hours. After the reaction was completed and cooled at room temperature, it was filtered and washed, and the obtained solid sample was dried overnight at 60°C in a vacuum oven and recorded as Pt / C-CTAB . Disperse 1000mg of Pt / C-PVP ground into powder in 100ml of acetone-water (volume ratio 9:1) mixed solution, after ultrasonic dispersion, heat up and react in a water bath at 60°C for 10h under magnetic stirring conditions, and mix the above Centrifuge the mixed solution for solid-liquid separation, the speed is 8000rpm, and the time is 5 minutes. After 4 consecutive...

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Abstract

The invention relates to a mild removal method of a surfactant in a nano-catalyst, which comprises the following steps of: 1) dispersing the nano-catalyst with the surfactant adsorbed on the surface into acetone or an acetone-water mixed solution, and ultrasonically dispersing uniformly; (2) heating and reacting for 4-10 hours under a stirring condition; (3) cooling, centrifuging and removing supernate; 4) continuously dispersing the centrifuged solid in acetone or an acetone-water mixed solution, and centrifuging to remove supernate; repeating for more than one time (preferably 2-4 times), drying the obtained solid catalyst in a drying oven, and grinding to obtain catalyst powder. According to the method, acetone is used as a removing agent of a surfactant, operation is easy, reaction conditions are mild, and damage to the microstructure of the nano-catalyst is small. The surface of the obtained nano-catalyst is clean, the residual quantity of the surfactant is less than 0.5 wt%, and the catalytic reaction activity is high.

Description

technical field [0001] The invention relates to a method for removing a nano-catalyst surfactant, and the nano-catalyst can be used in the fields of fuel cell, petrochemical industry, chemical pharmacy, automobile tail gas purification and the like. Background technique [0002] By reducing the size of the material to the nanoscale range, the proportion of surface-exposed atoms can be increased by as much as 50-80% compared to bulk materials. Since the valence and electronic states of surface atoms are significantly different from those inside particles, the surface effect brought about by the regulation of nanometer size can make nanomaterials have high reactivity. In the catalytic reaction process, when the size of the catalyst active component is reduced to the nanometer range and loaded on some carrier materials, the huge surface area of ​​the catalyst particle and the existence of a large number of low-coordination surface atoms make the nanocatalyst present Very high ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J37/00B01J37/34B01J35/00B01J23/42
CPCB01J37/009B01J37/343B01J23/42B01J35/396B01J35/393
Inventor 王素力李焕巧孙公权
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI