Method for preparing nano-nickel/carbon fiber (Ni/CF) catalyst from chemical nickel-plating waste liquid

Abstract

The invention provides a method for preparing a nano-nickel / carbon fiber (Ni / CF) catalyst from a chemical nickel-plating waste liquid. The method comprises the following steps: on the basis of taking a conductive CF as a matrix material, and covalent-grafting ethylenediamine (EDA) on the conductive CF by a potentiostatic method so as to obtain an EDA / CF composite material; then grafting ethylenediamine tetra-oxaloacetic acid on the EDA / CF composite material by virtue of amido reaction, and then adding tripolycyanamide and formaldehyde so as to obtain chelate resin / EDA / CF by virtue of polymerization reaction; and placing the obtained chelate resin / EDA / CF in the chemical nickel-plating waste liquid to adsorb nickel ions, and reducing the nickel ions in situ by an electrochemical process so as to finally obtain the nano-Ni / CF catalyst. The method provided by the invention has the advantages of lowering the energy consumption, simplifying the processing steps, improving the added value ofa product and establishing a new approach for effective resource utilization of the chemical nickel-plating waste liquid, thus having higher economic value and higher environmental protection value.

Description

1. Technical field

[0001] The invention relates to the recovery and reuse of electroless nickel plating waste liquid, in particular to a method for preparing nano-nickel / carbon fiber (Ni / CF) catalyst by utilizing the electroless nickel plating waste liquid. 2. Background technology

[0002] Electroless nickel plating technology is widely used in industries such as abrasive tools, corrosion and protection. During the plating process, nickel ions and hypophosphite are gradually consumed, and the by-product phosphite is continuously accumulated, which eventually leads to the failure of the plating solution and the generation of waste solution. Since nickel is a carcinogenic substance and is a rare and precious metal resource, the recovery of nickel in the electroless nickel plating waste solution has both environmental protection and economic significance.

[0003] There are two main directions for the treatment of electroless nickel plating waste solution. One is to regenera...

Examples

preparation example Construction

[0037] 2. Preparation of ethylenediamine / carbon fiber composites

[0038] Carboxylated carbon fibers were placed in absolute ethanol and twice distilled water for ultrasonic cleaning for 5 minutes, and then dried naturally in the air after cleaning, and then placed in an acetonitrile solution of ethylenediamine and lithium perchlorate, in which ethylenediamine The concentration is 1-10mmol·L -1 , the concentration of lithium perchlorate is 0.1mol L -1 At room temperature, a conventional electrochemical three-electrode system (carbon fiber as the working electrode, silver wire as the reference electrode, and platinum wire as the auxiliary electrode) is used at a constant potential of 1.2-1.8V for 1.5-4.5 hours to make ethylenediamine covalently modified On the surface of carbon fiber, then take it out and place it in an aqueous ethanol solution of potassium chloride, and keep the electrodes constant at -0.7 to -1.4V for 1-3 hours of constant potential reduction to aminate the ...

Embodiment 1

[0049] Prepare according to the above-mentioned embodiment, wherein:

[0050] In step 2, the carboxylated carbon fibers were put into absolute ethanol and twice-distilled water for ultrasonic cleaning for 5 minutes respectively, and after cleaning, they were naturally dried in the air, and then placed in an acetonitrile solution of ethylenediamine and lithium perchlorate, wherein The concentration of ethylenediamine is 1mmol L -1 , the concentration of lithium perchlorate is 0.1mol L -1 At room temperature, a conventional electrochemical three-electrode system (carbon fiber as the working electrode, silver wire as the reference electrode, and platinum wire as the auxiliary electrode) was used at a constant potential of 1.5V for 3 hours to covalently modify the surface of the carbon fiber with ethylenediamine. Then take it out and put it in the ethanol aqueous solution of potassium chloride, each electrode is constant potential reduction at -1.4V for 1 hour, the carbon fiber s...

Embodiment 2

[0055] Prepare according to the above-mentioned embodiment, wherein:

[0056] In step 2, the carboxylated carbon fibers were put into absolute ethanol and twice-distilled water for ultrasonic cleaning for 5 minutes respectively, and after cleaning, they were naturally dried in the air, and then placed in an acetonitrile solution of ethylenediamine and lithium perchlorate, wherein The concentration of ethylenediamine is 10mmol L -1 , the concentration of lithium perchlorate is 0.1mol L -1 At room temperature, a conventional electrochemical three-electrode system (carbon fiber as the working electrode, silver wire as the reference electrode, and platinum wire as the auxiliary electrode) was used at a constant potential of 1.8V for 1.5 hours to covalently modify the surface of the carbon fiber with ethylenediamine. Then take it out and put it in the aqueous ethanol solution of potassium chloride, and keep the electrodes unchanged at -0.7V for 3 hours of constant potential reduct...

1. Technical field

[0001] The invention relates to the recovery and reuse of electroless nickel plating waste liquid, in particular to a method for preparing nano-nickel / carbon fiber (Ni / CF) catalyst by utilizing the electroless nickel plating waste liquid. 2. Background technology

[0002] Electroless nickel plating technology is widely used in industries such as abrasive tools, corrosion and protection. During the plating process, nickel ions and hypophosphite are gradually consumed, and the by-product phosphite is continuously accumulated, which eventually leads to the failure of the plating solution and the generation of waste solution. Since nickel is a carcinogenic substance and is a rare and precious metal resource, the recovery of nickel in the electroless nickel plating waste solution has both environmental protection and economic significance.

[0003] There are two main directions for the treatment of electroless nickel plating waste solution. One is to regenera...

Examples

preparation example Construction

[0037] 2. Preparation of ethylenediamine / carbon fiber composites

[0038] Carboxylated carbon fibers were placed in absolute ethanol and twice distilled water for ultrasonic cleaning for 5 minutes, and then dried naturally in the air after cleaning, and then placed in an acetonitrile solution of ethylenediamine and lithium perchlorate, in which ethylenediamine The concentration is 1-10mmol·L -1 , the concentration of lithium perchlorate is 0.1mol L -1 At room temperature, a conventional electrochemical three-electrode system (carbon fiber as the working electrode, silver wire as the reference electrode, and platinum wire as the auxiliary electrode) is used at a constant potential of 1.2-1.8V for 1.5-4.5 hours to make ethylenediamine covalently modified On the surface of carbon fiber, then take it out and place it in an aqueous ethanol solution of potassium chloride, and keep the electrodes constant at -0.7 to -1.4V for 1-3 hours of constant potential reduction to aminate the ...

Embodiment 1

[0049] Prepare according to the above-mentioned embodiment, wherein:

[0050] In step 2, the carboxylated carbon fibers were put into absolute ethanol and twice-distilled water for ultrasonic cleaning for 5 minutes respectively, and after cleaning, they were naturally dried in the air, and then placed in an acetonitrile solution of ethylenediamine and lithium perchlorate, wherein The concentration of ethylenediamine is 1mmol L -1 , the concentration of lithium perchlorate is 0.1mol L -1 At room temperature, a conventional electrochemical three-electrode system (carbon fiber as the working electrode, silver wire as the reference electrode, and platinum wire as the auxiliary electrode) was used at a constant potential of 1.5V for 3 hours to covalently modify the surface of the carbon fiber with ethylenediamine. Then take it out and put it in the ethanol aqueous solution of potassium chloride, each electrode is constant potential reduction at -1.4V for 1 hour, the carbon fiber s...

Embodiment 2

[0055] Prepare according to the above-mentioned embodiment, wherein:

[0056] In step 2, the carboxylated carbon fibers were put into absolute ethanol and twice-distilled water for ultrasonic cleaning for 5 minutes respectively, and after cleaning, they were naturally dried in the air, and then placed in an acetonitrile solution of ethylenediamine and lithium perchlorate, wherein The concentration of ethylenediamine is 10mmol L -1 , the concentration of lithium perchlorate is 0.1mol L -1 At room temperature, a conventional electrochemical three-electrode system (carbon fiber as the working electrode, silver wire as the reference electrode, and platinum wire as the auxiliary electrode) was used at a constant potential of 1.8V for 1.5 hours to covalently modify the surface of the carbon fiber with ethylenediamine. Then take it out and put it in the aqueous ethanol solution of potassium chloride, and keep the electrodes unchanged at -0.7V for 3 hours of constant potential reduct...

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