Preparation method of multi-walled carbon nanotube/nanoscale bimetallic zero-valent iron composite material

A technology of multi-wall carbon nanotubes and composite materials is applied in the field of preparation of multi-wall carbon nanotubes/nano-scale bimetallic zero-valent iron composite materials, and can solve the problems of uneven particle distribution, easy agglomeration, and difficulty in recycling. Achieve uniform particle size distribution, rapid response and convenient operation.

Active Publication Date: 2018-02-13
浙江聚盾科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the problems of uneven particle distribution, easy agglomeration and difficulty in recycling in the process of preparing nano-scale zero-valent iron bimetallic particles by ordinary liquid phase reduction method

Method used

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  • Preparation method of multi-walled carbon nanotube/nanoscale bimetallic zero-valent iron composite material
  • Preparation method of multi-walled carbon nanotube/nanoscale bimetallic zero-valent iron composite material

Examples

Experimental program
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Effect test

Embodiment 1

[0041] Under the action of ultrasonic (40KHz, 150W) and continuous stirring under nitrogen, the temperature of the water bath is 30°C, and the concentration of 200mL is 0.50mol L -1 NaBH 4 The aqueous solution was added dropwise within 10 minutes to a container with an equal volume of 0.25mol·L -1 FeSO 4 ·7H 2 In the 500mL three-neck flask of O aqueous solution, continue to react for 10min after the dropwise addition, and then add 26.8mL of 0.005mol·L -1 K 2 PdCl 6 The aqueous solution was reacted for 75 minutes (the color of the solution changed from reddish brown to light green), and nanoscale Pd / Fe particles were generated in the reaction system. 0.2g of MWCNTs with a diameter of 10-20nm was added to the nanoscale Pd / Fe system, and continued The reaction was stirred for 120 min, and the stabilized MWCNTs / nano-scale Pd / Fe composite particles were selected by magnetic separation, washed with anaerobic deionized water (50mL × 3), and then washed with absolute ethanol (50m...

Embodiment 2

[0046] Under the action of ultrasonic (40KHz, 150W) and continuous stirring under nitrogen, the temperature of the water bath is 30°C, and the concentration of 200mL is 0.50mol L -1 NaBH 4 The aqueous solution was added dropwise within 10 minutes to a container with an equal volume of 0.25mol·L -1 FeSO 4 ·7H 2 In the 500mL three-necked flask of O aqueous solution, continue to react for 10min after the dropwise addition, and then add 44.67mL of 0.003mol·L -1 K 2 PdCl 6 The aqueous solution was reacted for 75 minutes (the color of the solution changed from reddish brown to light green), and nanoscale Pd / Fe particles were generated in the reaction system. 0.2g of MWCNTs with a diameter of 10-20nm was added to the nanoscale Pd / Fe system, and continued The reaction was stirred for 120 min, and the stabilized MWCNTs / nano-scale Pd / Fe composite particles were selected by magnetic separation, washed with anaerobic deionized water (50mL × 3), and then washed with absolute ethanol (...

Embodiment 3

[0051] Under the action of ultrasonic (40KHz, 150W) and continuous stirring under nitrogen, the temperature of the water bath is 30°C, and the concentration of 200mL is 0.50mol L -1 NaBH 4 The aqueous solution was added dropwise within 10 minutes to a container with an equal volume of 0.25mol·L -1 FeSO 4 ·7H 2 In the 500mL three-neck flask of O aqueous solution, continue to react for 10min after the dropwise addition, and then add 37.5mL of 0.005mol·L -1 K 2 PdCl 6 The aqueous solution was reacted for 90 minutes (the color of the solution changed from reddish brown to light green), and nanoscale Pd / Fe particles were generated in the reaction system. 0.2g of MWCNTs with a diameter of 10-20nm was added to the nanoscale Pd / Fe system, and continued The reaction was stirred for 120 min, and the stabilized MWCNTs / nano-scale Pd / Fe composite particles were selected by magnetic separation, washed with anaerobic deionized water (50mL × 3), and then washed with absolute ethanol (50m...

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Abstract

The invention provides a method for preparing a multi-walled carbon nanotube / nano-scale bimetallic zero-valent iron composite material. The preparation method is as follows: under the conditions of nitrogen protection, ultrasonic wave action and continuous stirring, the reducing agent aqueous solution is gradually Add dropwise into the soluble ferrous salt aqueous solution, continue to react for 5-15 minutes after dropping, then add K2PdCl6 aqueous solution to react for 60-90 minutes, then add MWCNTs and stir for 90-150 minutes, and then use magnetic separation to separate the prepared polysaccharide from the reaction system The walled carbon nanotube / nano-scale bimetallic zero-valent iron composite material is stored in absolute ethanol or acetone after washing; the invention is based on an improved liquid phase reduction method, and utilizes an ultrasonic enhanced liquid phase reduction method to prepare particles with good dispersibility and The stabilized MWCNTs / nano-scale Pd / Fe composite particles are uniform, smaller in particle size, larger in specific surface area and easy to recover, and the method has rapid response, simple equipment and convenient operation.

Description

(1) Technical field [0001] The invention relates to a preparation method of a multi-walled carbon nanotube (MWCNTs) / nano-scale bimetallic zero-valent iron composite material. (2) Background technology [0002] Zero valent iron (Fe 0 , ZVI) research and application in the field of groundwater pollutant remediation began in the 1990s. At first, the granular ZVI was applied to the osmotic reaction grid (PRB). When the polluted groundwater passes through the PRB reaction grid, the pollutants Precipitation, adsorption and transformation on ZVI surface. From the early 1990s to the present, PRB technology has been widely used in actual groundwater remediation projects in the United States, and it has been proved that this technology is a relatively effective in-situ remediation technology, which is gradually replacing the traditional pumping treatment technology. Research hotspots of contaminated groundwater remediation (Puls R W, Paul C J, Powell RM. The application of in situ p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/24B22F1/00B82Y40/00
CPCB82Y40/00B22F9/24B22F1/07B22F1/0547
Inventor 赵德明付聪
Owner 浙江聚盾科技有限公司
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