CN110592561B - Treatment method of chemical nickel plating waste liquid - Google Patents

Treatment method of chemical nickel plating waste liquid Download PDF

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Publication number
CN110592561B
CN110592561B CN201910955178.4A CN201910955178A CN110592561B CN 110592561 B CN110592561 B CN 110592561B CN 201910955178 A CN201910955178 A CN 201910955178A CN 110592561 B CN110592561 B CN 110592561B
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waste liquid
nickel plating
solution
chemical nickel
plating waste
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CN110592561A (en
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刘万民
秦牡兰
王伟刚
申斌
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Hunan Institute of Engineering
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601—Process or apparatus
    • C23C18/1617—Purification and regeneration of coating baths
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/31—Coating with metals
    • C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/101—Sulfur compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/105—Phosphorus compounds

Abstract

The invention discloses a treatment method of chemical nickel plating waste liquid, and relates to the field of resource utilization of the chemical nickel plating waste liquid. The method comprises the steps of adding soluble barium salt into the chemical nickel plating waste liquid to obtain barium sulfate, recycling sulfur elements, continuously adding sodium hydroxide to obtain spherical nickel hydroxide, recycling nickel elements, and finally taking the obtained solution as a raw material for synthesizing sodium vanadium phosphate of a sodium ion battery material. The method almost realizes the proliferation and regeneration utilization of all elements in the chemical nickel plating waste liquid, can provide a practical and effective solution for the chemical nickel plating waste liquid which is a chronic disease in the environment for many years, realizes the change of waste into valuable, and accords with the concept of green economic development.

Description

Treatment method of chemical nickel plating waste liquid
Technical Field
The invention relates to treatment of industrial wastewater, in particular to a treatment method of chemical nickel plating waste liquid.
Background
The chemical nickel plating technology has the advantages of uniform plating layer, high hardness, good wear resistance, no limitation of the size and shape of parts during plating, and the like, and is widely applied to various industries such as machinery, chemical engineering, electronics, information and the like. With the increasing application range and production scale of electroless nickel plating technology, the environmental problems caused by the technology are more serious. After the chemical nickel plating solution works for a certain time, no matter how precise management and online regeneration are carried out, the performance of the plating solution is finally reduced due to the accumulation of by-products such as phosphite and the like, and the chemical nickel plating waste liquid is formed. The waste liquid has complex components, and contains 2-7 g/L nickel ions, 10-200 g/L phosphorus, more than 80 g/L sodium sulfate, more than 200g/L Chemical Oxygen Demand (COD) and trace impurity metal ions. Nickel is a relatively expensive metal element and has carcinogenic and sensitizing effects; phosphorus is one of the main pollution factors causing the eutrophication of water bodies; organic matters can not be spontaneously degraded under natural environmental conditions. Therefore, if the chemical nickel plating waste liquid is not effectively treated, not only the environment is seriously polluted, but also the resource waste is caused.
Aiming at nickel and phosphorus elements in chemical nickel plating waste liquid, people generally adopt treatment methods of recovering nickel through electrolysis, removing residual nickel through precipitation, treating phosphorus through oxidation precipitation, treating residual nickel and phosphorus through precipitation or catalytic reduction treatment, oxidizing complex breaking-precipitation treatment, recovering nickel, precipitating phosphorus and the like. The nickel element is finally recovered and utilized in the form of metallic nickel, nickel-phosphorus alloy, nickel hydroxide, nickel sulfate, or the like, and the phosphorus element is finally recovered and utilized in the form of nickel-phosphorus alloy, calcium phosphite, calcium phosphate, iron phosphate, or aluminum phosphate, or the like. However, no report is found about the recycling of sodium, sulfur and carbon in the electroless nickel plating waste liquid. Therefore, it is necessary to develop a treatment method capable of simultaneously realizing the proliferation and regeneration of main elements such as nickel, phosphorus, sodium, sulfur, carbon and the like in the chemical nickel plating waste liquid.
The invention content is as follows:
the invention aims to provide a method for treating chemical nickel plating waste liquid.
The purpose of the invention is realized by the following technical scheme:
a treatment method of chemical nickel plating waste liquid comprises the following steps:
(1) carrying out full analysis on the chemical nickel plating waste liquid, and determining the contents of nickel, phosphorus, sodium, sulfur, carbon and other elements in the waste liquid;
(2) adding 0.1-5 mol/L soluble barium salt into the chemical nickel plating waste liquid in the step (1) according to a stoichiometric ratio, stirring and reacting for 1-10 h at 25-100 ℃, and filtering to obtain barium sulfate and a solution A;
(3) adding the solution A and a sodium hydroxide solution with a stoichiometric ratio of 0.1-6.5 mol/L into a reaction kettle with a stirring device in a parallel flow manner, reacting for 5-36 h at a stirring speed of 300-700 rpm, a pH value of 8-13 and a temperature of 25-100 ℃, and filtering to obtain spherical nickel hydroxide and a solution B;
(4) adding 0.01-5 mol/L soluble sulfide into the solution B in a stoichiometric ratio, stirring and reacting at 25-100 ℃ for 1-10 h, and filtering to remove insoluble sulfide precipitate to obtain a solution C.
Further, the soluble barium salt is one or a mixture of more than two of barium nitrate, barium acetate and barium chloride.
Further, the soluble sulfide is one or a mixture of more than two of hydrogen sulfide, sodium hydrosulfide and ammonium sulfide.
The solution C is used for preparing a raw material of carbon-coated vanadium sodium phosphate of a sodium-ion battery material, a vanadium source with a metering ratio is added into the solution C, a sodium source or a phosphorus source with insufficient content is supplemented, and the carbon-coated vanadium sodium phosphate of the sodium-ion battery material is synthesized by roasting under the protection of inert gases such as nitrogen or argon, so that the recovery of phosphorus elements, sodium elements and carbon elements is realized; the method comprises the following specific steps:
(a) carrying out full analysis on the chemical nickel plating waste liquid after the sulfur and nickel removal and the vulcanization treatment to measure the contents of phosphorus, sodium, carbon and other elements in the waste liquid;
(b) adding a vanadium source, a phosphorus source or a sodium source into the waste liquid obtained in the step (a) to ensure that the molar ratio of Na (V + M) to P =3:2:3, namely the stoichiometric ratio, completely dissolving or uniformly mixing, and then drying and ball-milling to obtain a precursor;
(c) and (c) roasting the precursor obtained in the step (b), cooling the precursor to room temperature along with a furnace, and crushing and grading to obtain the carbon-coated sodium vanadium phosphate battery material.
It is to be noted that the above-mentioned stoichiometric ratio is determined by the product, for example, in step (1), the stoichiometric ratio is determined by the product barium sulfate, i.e., the amount of barium salt added is calculated based on the sulfur content of barium sulfate that can react with soluble barium salt in the waste liquid.
Compared with the prior art, the invention has the beneficial effects that:
(1) the method for treating the chemical nickel plating waste liquid does not relate to the recycling of the sulfur element, and the method adopts a precipitation method to convert the sulfur element in the chemical nickel plating waste liquid into barium sulfate with high added value.
(2) The conventional treatment method of nickel element in the chemical nickel plating waste liquid comprises the following steps: the nickel hydroxide is converted into nickel hydroxide with small value and no specific morphology by an oxidation breaking-precipitation method, or further converted into nickel sulfate. The invention utilizes the complexing action of the complexing agent existing in the chemical nickel-plating waste liquid on nickel ions, and adopts the crystallization control technology to convert nickel elements in the chemical nickel-plating waste liquid into spherical nickel hydroxide with high added value (with specific morphology), and the spherical nickel hydroxide can be widely applied to the fields of nickel-hydrogen batteries, lithium ion batteries and the like.
(3) The invention discloses a method for treating chemical nickel plating waste liquid, which is characterized in that phosphorus is converted into calcium phosphite, calcium phosphate, iron phosphate or aluminum phosphate, and the like, and sodium and carbon are not recycled.
In a word, the method disclosed by the invention is low in cost, short in flow, clean and environment-friendly, can realize the proliferation and regeneration utilization of main elements such as nickel, phosphorus, sodium, sulfur, carbon and the like in the chemical nickel plating waste liquid, realizes the resource utilization of the main elements, has high additional value of products, obviously improves the economic benefit, and accords with the green economic development concept.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the present invention is not limited thereto.
Example 1
1.0L of chemical nickel plating waste liquid in a certain factory is taken, and analyzed, the chemical nickel plating waste liquid comprises the following components: na 0.28 mol/L, P0.3 mol/L, Ni 0.13 mol/L, C1.02.02 mol/L, SO4 2- 0.15 mol/L、Ca 0.1×10-3 mol/L、Fe 0.03×10-3 mol/L、Mg 0.16×10-3 mol/L. Adding 300 ml of 0.5 mol/L barium nitrate into the waste liquid, stirring and reacting for 3 hours at 80 ℃, and filtering to obtain barium sulfate and a solution A. Adding the solution A and 2.6 liters of 0.1 mol/L sodium hydroxide into a reaction kettle with a stirring device in a concurrent flow manner, reacting for 15 hours under the conditions of stirring speed of 300rpm, pH value of 10 and temperature of 70 ℃, and filtering to obtain spherical nickel hydroxide and a solution B. Adding 30 ml of 0.01 mol/L sodium sulfide into the solution B, stirring and reacting for 2h at 75 ℃, filtering to remove insoluble sulfide precipitate to obtainAnd (5) solution C. And after full analysis, the solution C is used for preparing the carbon-coated vanadium sodium phosphate of the sodium-ion battery material.
Example 2
1.0L of chemical nickel plating waste liquid in a certain factory is taken, and analyzed, the chemical nickel plating waste liquid comprises the following components: na 0.28 mol/L, P0.3 mol/L, Ni 0.13 mol/L, C1.02.02 mol/L, SO4 2- 0.15 mol/L、Ca 0.1×10-3 mol/L、Fe 0.03×10-3 mol/L、Mg 0.16×10-3 mol/L. Adding 200 ml of 0.75 mol/L barium acetate into the waste liquid, stirring and reacting for 5 hours at the temperature of 60 ℃, and filtering to obtain barium sulfate and a solution A. Adding the solution A and 1.04L of 0.25 mol/L sodium hydroxide into a reaction kettle with a stirring device in a concurrent flow manner, reacting for 20 hours under the conditions of stirring speed of 400rpm, pH value of 10.5 and temperature of 60 ℃, and filtering to obtain spherical nickel hydroxide and a solution B. 15 ml of 0.02 mol/L sodium sulfide was added to the solution B, and the mixture was stirred at 55 ℃ for 4 hours to react, and then insoluble sulfide precipitate was removed by filtration to obtain a solution C. And after full analysis, the solution C is used for preparing the carbon-coated vanadium sodium phosphate of the sodium-ion battery material.
Example 3
1.0L of chemical nickel plating waste liquid in a certain factory is taken, and analyzed, the chemical nickel plating waste liquid comprises the following components: na 0.28 mol/L, P0.3 mol/L, Ni 0.13 mol/L, C1.02.02 mol/L, SO4 2- 0.15 mol/L、Ca 0.1×10-3 mol/L、Fe 0.03×10-3 mol/L、Mg 0.16×10-3 mol/L. 100 ml of 1.5 mol/L barium chloride is added into the waste liquid, stirred and reacted for 6 hours at the temperature of 50 ℃, and filtered to obtain barium sulfate and a solution A. Adding the solution A and 0.52L of 0.5 mol/L sodium hydroxide into a reaction kettle with a stirring device in a concurrent flow manner, reacting for 24 hours under the conditions of stirring speed of 500rpm, pH value of 11 and temperature of 50 ℃, and filtering to obtain spherical nickel hydroxide and a solution B. 10 ml of 0.03 mol/L sodium sulfide was added to the solution B, and the mixture was stirred at 45 ℃ for reaction for 6 hours, and then insoluble sulfide precipitate was removed by filtration to obtain a solution C. And after full analysis, the solution C is used for preparing the carbon-coated vanadium sodium phosphate of the sodium-ion battery material.
Finally, it should be noted that the above-mentioned list is only a specific embodiment of the present invention. It is obvious that the invention is not limited to the above embodiments, but that many variations are possible. In all respects, the above-described embodiments of the invention are to be considered illustrative of the invention and not restrictive. Therefore, the present invention is not limited to the specific embodiments disclosed and described above, and some modifications and variations of the present invention should fall within the scope of the claims of the present invention.

Claims (3)

1. The method for treating the chemical nickel plating waste liquid is characterized by comprising the following steps of:
(1) carrying out total analysis on the chemical nickel plating waste liquid, and determining the contents of nickel, phosphorus, sodium, sulfur, carbon and other elements in the waste liquid, wherein a complexing agent exists in the chemical nickel plating waste liquid;
(2) adding 0.1-5 mol/L soluble barium salt into the chemical nickel plating waste liquid in the step (1) according to a stoichiometric ratio, stirring and reacting for 1-10 h at 25-100 ℃, and filtering to obtain barium sulfate and a solution A;
(3) adding the solution A and a sodium hydroxide solution with a stoichiometric ratio of 0.1-6.5 mol/L into a reaction kettle with a stirring device in a parallel flow manner, reacting for 5-36 h at a stirring speed of 300-700 rpm, a pH value of 8-13 and a temperature of 25-100 ℃, and filtering to obtain spherical nickel hydroxide and a solution B;
(4) and adding 0.01-5 mol/L of soluble sulfide in a stoichiometric ratio into the solution B, stirring and reacting at 25-100 ℃ for 1-10 h, filtering to remove insoluble sulfide precipitate to obtain a solution C, wherein the solution C is used for preparing the carbon-coated vanadium sodium phosphate of the sodium ion battery material.
2. The processing method according to claim 1, characterized in that: the soluble barium salt is one or a mixture of more than two of barium nitrate, barium acetate and barium chloride.
3. The processing method according to claim 1, characterized in that: the soluble sulfide is one or a mixture of more than two of hydrogen sulfide, sodium hydrosulfide and ammonium sulfide.
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CN114031103B (en) * 2021-11-22 2023-12-05 湖南工程学院 Method for preparing spherical barium sulfate from chemical nickel plating waste liquid

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