CN112607813A - Method for synergistically extracting nickel from nickel plating wastewater - Google Patents

Method for synergistically extracting nickel from nickel plating wastewater Download PDF

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CN112607813A
CN112607813A CN202110001595.2A CN202110001595A CN112607813A CN 112607813 A CN112607813 A CN 112607813A CN 202110001595 A CN202110001595 A CN 202110001595A CN 112607813 A CN112607813 A CN 112607813A
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solution
nickel
d2ehpa
stirring
nickel plating
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CN112607813B (en
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周磊
张捷菲
计枫斌
刘哲
陈建
刘香宁
王志凌
谢雨
邱慧恬
熊沁宇
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Nanchang Hangkong University
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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
    • C02F1/26—Treatment of water, waste water, or sewage by extraction
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/04—Obtaining nickel or cobalt by wet processes
    • C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Organic Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Manufacturing & Machinery (AREA)
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  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Water Supply & Treatment (AREA)
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  • Physical Water Treatments (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Removal Of Specific Substances (AREA)

Abstract

The invention discloses a method for synergistically extracting nickel from nickel plating wastewater, which relates to the technical field of wastewater treatment and comprises the following steps: s1, preparing a D2EHPA solution, adding alkali liquor into the D2EHPA solution, stirring to ensure that the saponification rate of the D2EHPA is 30-70%, and layering the reaction liquid to obtain an upper layer reaction liquid; s2, adding a diluent into the upper layer reaction solution; s3, continuously adding methyl isobutyl ketone to obtain an extracting agent; s4, adding an extracting agent into the nickel plating wastewater, stirring and mixing uniformly to stratify the reacted solution, and taking the upper solution; and S5, adding an acid solution into the upper solution for back extraction to obtain a nickel-containing recovered material. The method has the beneficial effects that the D2EHPA solution and the methyl isobutyl ketone solution are used for extracting the nickel ions in the nickel plating waste liquid cooperatively, so that the concentration of the residual nickel ions in the nickel plating waste liquid meets the national standard discharge requirement, and the acid solution is used for back extraction of the extraction liquid, so that the nickel ions in the extraction liquid are recovered.

Description

Method for synergistically extracting nickel from nickel plating wastewater
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to a method for synergistically extracting nickel from nickel plating wastewater.
Background
With the development of economy, the industrial development is more and more rapid, and the industrial production processes of electroplating, batteries and the like can generate a large amount of industrial wastewater. About 4 hundred million tons of heavy metal wastewater, 5 multiplied by 10, is discharged every year in the electroplating industry of China4t electroplating sludge and 3X 107m3An acid gas. 35 urban underground waters exceed the standard in China, the exceeding rate is 3% -80%, and drinking water in thousands of wells is scrapped due to the exceeding standard of heavy metals. Although the total amount of the electroplating sludge is not much than that of the wastewater, the electroplating sludge is a typical solid waste, is mainly a precipitate formed after treatment by a chemical precipitation method, and heavy metals contained in the electroplating sludge are difficult to degrade, and become a potential environmental pollution source if the electroplating sludge is not treated properly or is not treated, so that the electroplating sludge has great harm to human health and environment. Heavy metal ions have great harm to the earth environment and human health, and nickel ions are common heavy metal ions. Nickel is a metal ion, and the toxicity of nickel and nickel salt is relatively low, so if too much nickel ion is ingested or nickel poisoning occurs, certain harm can be caused to human bodies.
The current common methods for treating nickel-containing wastewater include: chemical precipitation, electrolysis, ion exchange, adsorption and redox processes using hydroxides or sulfides as precipitants. Although the above methods have good effect of removing nickel ions, they all have the problems of high treatment cost, easy secondary pollution, etc., and the nickel ions in the wastewater are often transferred to solid wastes after treatment, and cannot be recycled.
Disclosure of Invention
The invention aims to at least solve one of the technical problems in the prior art and provides a method for synergistically extracting nickel from nickel plating wastewater, which is simple to operate, low in cost and high in efficiency, and the concentration of residual nickel ions meets the emission requirement of industrial pollution sources of copper, cobalt and nickel specified in national standard GB 25467-2010.
The technical solution of the invention is as follows:
a method for synergistically extracting nickel from nickel plating wastewater comprises the following steps:
s1, preparing a D2EHPA solution, adding alkali liquor into the D2EHPA solution, stirring to ensure that the saponification rate of the D2EHPA is 30-70%, layering reaction liquid after stirring, and taking upper-layer reaction liquid;
s2, adding a diluent into the upper layer reaction liquid in the step S1, and stirring, wherein the reaction temperature is controlled to be 15-35 ℃;
s3, continuously adding methyl isobutyl ketone into the upper layer reaction liquid in the step S1, stirring, and controlling the reaction temperature at 15-35 ℃ to obtain an extracting agent;
s4, adding an extracting agent into the nickel plating wastewater, uniformly stirring and mixing, layering the reacted solution after stirring, and taking the upper layer solution;
s5, adding an acid solution into the upper solution in the step S4 for back extraction, and obtaining a nickel-containing reclaimed material.
In one embodiment of the invention, in the step S1, the concentration of the D2EHPA solution is 0.5 to 15mol/L, preferably 0.5 to 1mol/L, and more preferably 0.8mol/L, and the stirring is performed for 15 to 40 min.
In one embodiment of the present invention, in step S1, the saponification rate of D2EHPA is 55%.
In a specific embodiment of the invention, in the step S2, the diluent is sulfonated kerosene, and the volume ratio of the D2EHPA solution to the diluent is 1: 2-4.
In one embodiment of the present invention, in step S3, the volume of the methylisobutylketone added is 15 to 50% of the volume of the D2EHPA solution, and more preferably 30%.
In one embodiment of the present invention, the reaction temperature is controlled at 25 ℃ in the steps S2 and S3.
In a specific embodiment of the invention, in the step S4, the volume ratio of the nickel plating wastewater to the extracting agent is 1: 0.6-1.02, and the stirring is performed for 15-40 min.
In a specific embodiment of the invention, in the step S4, the volume ratio of the nickel plating wastewater to the extracting agent is 1:1, and the stirring is performed for 30 min.
In a specific embodiment of the present invention, in the step S5, the volume ratio of the acid solution to the upper solution is 1: 0.8-1.5.
In one embodiment of the present invention, in step S5, the acid solution is one or more of sulfuric acid, hydrochloric acid and nitric acid.
The invention has at least one of the following beneficial effects:
according to the invention, the D2EHPA solution and the methyl isobutyl ketone solution are used as extracting agents to extract nickel ions in the nickel plating waste liquid in a synergistic manner, so that the nickel ions in the nickel plating waste liquid are extracted efficiently, the concentration of the residual nickel ions in the nickel plating waste liquid meets the discharge requirement of industrial pollution sources specified in the national standard GB25467-2010, and the environment is not polluted. Then the invention further carries out back extraction on the nickel ions in the extraction liquid by adopting an acid solution, so that the nickel ions in the extraction liquid are recovered, and a nickel-containing recovered material is obtained. The extraction rate of the invention to nickel ions can reach more than 93 percent, the invention well solves the problem of recycling nickel ions in sewage, and greatly reduces the environmental hazard caused by direct discharge of sewage.
Detailed Description
The present invention will be described in further detail with reference to the following examples, but the present invention is not limited to the following examples.
Reagent D2EHPA is referred to herein as di (2-ethylhexyl) phosphoric acid.
The reagent MIBK is known by its chinese name methyl isobutyl ketone.
The following reagents were all commercially available.
A method for synergistically extracting nickel from nickel plating wastewater comprises the following specific steps:
s1, preparing a D2EHPA solution with the concentration of 0.5-15 mol/L, adding alkali liquor into the D2EHPA solution, stirring for 15-40 min to allow saponification reaction to occur, wherein the addition amount of the alkali liquor is such that the saponification rate of the D2EHPA is 30-70%, layering the reaction solution after stirring is finished, and taking an upper layer reaction solution; preferably, the concentration of the D2EHPA solution is 0.8mol/L, the alkali liquor is a sodium hydroxide solution with the mass percent concentration of 50%, and the saponification rate of the D2EHPA is 55%;
s2, adding a diluent sulfonated kerosene into the upper layer reaction liquid in the step S1, and stirring, wherein the temperature is controlled to be 15-35 ℃;
s3, continuously adding methyl isobutyl ketone into the upper layer reaction liquid in the step S1, wherein the adding amount of the methyl isobutyl ketone is 15-50% of that of the oil phase, and more preferably 30%, stirring, and controlling the temperature to be 15-35 ℃ to obtain an extracting agent;
s4, adding an extracting agent into the nickel plating wastewater, wherein the volume ratio of the nickel plating wastewater to the extracting agent is 1: 0.6-1.02, preferably 1:1, stirring for 15-40 min, preferably 25min, uniformly mixing, layering the reacted solution after stirring, and taking the upper layer solution;
s5, adding an acid solution into the upper layer solution in the step S4 for back extraction, wherein the acid solution is one or more of sulfuric acid, hydrochloric acid and nitric acid, and the volume ratio of the acid solution to the upper layer solution is 1: 0.8-1.5, so that a nickel-containing recovered material is obtained.
Example 1
S1, preparing a D2EHPA solution with the concentration of 5 mol/L. 5ml of D2EHPA solution was added to 5ml of an aqueous NAOH solution (mNaOH. RTM. 0.3591g) to adjust the saponification rate of the D2EHPA solution to 60%. Mechanically stirring for 20min, standing for liquid separation, and collecting the upper organic phase solution.
S2, adding 15ml sulfonated kerosene to the organic phase solution for dilution with mechanical stirring, and controlling the reaction temperature at 22 ℃.
S3, adding 2.2ml of MIBK solution into the organic phase solution, and keeping the reaction temperature in the step S2 unchanged to obtain the extractant.
S4, adding an extracting agent into 15mL of nickel plating waste liquid (pH 4.8) with the nickel ion concentration of 3.373g/L, mechanically stirring for 30min, and separating by using a separating funnel after stirring to obtain an upper layer solution for later use; simultaneously taking the lower layer solution (water phase), measuring and analyzing the Ni ion concentration by using an atomic absorption spectrophotometer (AAS, conttra A700, AnalytikJena), and obtaining the Ni ion concentration according to the formula
Figure BDA0002881551430000031
Wherein, CiIs the nickel ion concentration (ppm), C, in the feed water phaseaqThe extraction rate of nickel ions was calculated from the concentration (ppm) of nickel ions in the aqueous phase after extraction.
S5, adding 22ml of 1mol/L sulfuric acid solution into the upper layer solution obtained in the step S4, and carrying out steam stripping to obtain a nickel-containing recovered substance; at the same time, according to the formula
Figure BDA0002881551430000041
Wherein, CsIs the concentration of nickel ions in the aqueous phase after back extraction, wherein, CorgThe concentration of the nickel ions in the organic phase is calculated, and the back extraction rate of the nickel ions is calculated.
Example 2
S1, preparing a D2EHPA solution with the concentration of 2.5 mol/L. 2.5ml of the D2EHPA solution was added to 2.5ml of an aqueous NAOH solution (mNaOH. RTM. 0.1496g) to adjust the saponification rate of the solution to 50%. Mechanically stirring for 20min, standing for liquid separation, and collecting the upper organic phase solution.
S2, adding 10ml sulfonated kerosene to the organic phase solution for dilution with mechanical stirring, and controlling the reaction temperature at 24 ℃.
S3, adding 1.8ml of MIBK solution into the organic phase solution, and keeping the reaction temperature in the step S2 unchanged to obtain the extractant.
S4, adding an extracting agent into 15mL of nickel plating waste liquid (pH 4.8) with the nickel ion concentration of 3.373g/L, mechanically stirring for 30min, and separating by using a separating funnel after stirring to obtain an upper layer solution for later use; taking the lower layer (water) at the same timePhase) Ni ion concentration was measured and analyzed using atomic absorption spectrophotometer (AAS, contrAA700, Analytik Jena), according to the formula
Figure BDA0002881551430000042
Wherein, CiIs the nickel ion concentration (ppm), C, in the feed water phaseaqThe nickel ion concentration (ppm) in the aqueous phase after extraction was calculated as the extraction rate of nickel ions.
S5, adding 18ml of 1mol/L nitric acid solution into the upper layer solution obtained in the step S4, and carrying out steam stripping to obtain a nickel-containing recovered substance; at the same time, according to the formula
Figure BDA0002881551430000043
Wherein, CsIs the concentration of nickel ions in the aqueous phase after back extraction, CorgThe concentration of the nickel ions in the organic phase is calculated, and the back extraction rate of the nickel ions is calculated.
Example 3
S1, preparing an EHPA solution with the concentration of 7.5mol/L D2. 5ml of D2EHPA solution was added to 5ml of an aqueous NAOH solution (m NaOH. RTM. 0.4040g) to adjust the saponification rate to 45%. Mechanically stirring for 20min, standing for liquid separation, and collecting the upper organic phase solution.
S2, adding 20ml sulfonated kerosene to the organic phase solution for dilution with mechanical stirring, and controlling the reaction temperature at 25 ℃.
S3, adding 2.8ml of MIBK solution into the organic phase solution, and keeping the reaction temperature in the step S2 unchanged to obtain the extractant.
S4, adding an extracting agent into 15ml of nickel plating waste liquid (pH 4.8) with the nickel ion concentration of 3.373g/L, mechanically stirring for 30min, and separating by using a separating funnel after stirring to obtain an upper layer solution for later use; simultaneously taking the lower layer (water phase), measuring and analyzing the Ni ion concentration by using an atomic absorption spectrophotometer (AAS, contrAA700, Analytik Jena), and obtaining the Ni ion concentration according to a formula
Figure BDA0002881551430000051
Wherein, CiIs the nickel ion concentration (ppm), C, in the feed water phaseaqIs the nickel ion concentration (ppm) in the water phase after extraction, and the extraction of the nickel ions is calculatedAnd (4) taking the rate.
S5, adding 22ml of 1mol/L hydrochloric acid solution into the upper layer solution obtained in the step S4 for steam stripping to obtain a nickel-containing recovered substance; at the same time, according to the formula
Figure BDA0002881551430000052
Wherein, CsIs the concentration of nickel ions in the aqueous phase after back extraction, CorgThe concentration of the nickel ions in the organic phase is calculated, and the back extraction rate of the nickel ions is calculated.
Comparative example 1
The difference from example 1 is that: the steps S2 and S3 are eliminated, and the saponification reaction of the D2EHPA solution in the step S1 is not carried out, i.e. the D2EHPA solution with the concentration of 5mol/L in the step S1 is directly added into the nickel plating waste liquid in the step S4 as an extracting agent, and the rest is the same as the example 1.
Comparative example 2
The difference from example 1 is that: the same procedure as in example 1 was repeated except that the D2EHPA reagent in step S1 was replaced with the P507 reagent.
Specific values of the extraction rate and the back extraction rate of nickel ions in examples 1 to 3 are shown in the following table:
TABLE 1 extraction and stripping rates of nickel ions according to examples of the present invention
Example 1 Example 2 Example 3 Comparative example 1 Comparative example 2
Ni2+Extraction rate 93.6％ 97.25％ 95.17％ 53.56％ 92.33％
Ni2+Back extraction rate 95.4％ 100％ 97.6％ 84.97％ 93.71％
As can be seen from Table 1, the nickel plating wastewater treated by the methods of examples 1 to 3 was treated with Ni2+The extraction rate can reach more than 93.6 percent and can reach 97.25 percent at most, and the back extraction rate can reach more than 95.4 percent and can reach 100 percent at most. Comparing examples 1-3 with comparative examples 1-2, it can be seen that the extraction rate of examples 1-3 is significantly higher than that of comparative example 1 (only using D2EHPA solution as the extractant) and comparative example 2 (using P507 reagent instead of D2EHPA reagent), thus demonstrating that the invention realizes Ni-based Ni alloy by selecting appropriate extractant2+The high-efficiency extraction is carried out, and meanwhile, the D2EHPA solution and the methyl isobutyl ketone in the invention can greatly improve the Ni content by the synergistic effect2+The extraction rate of (2).
The above are merely characteristic embodiments of the present invention, and do not limit the scope of the present invention in any way. All technical solutions formed by equivalent exchanges or equivalent substitutions fall within the protection scope of the present invention.

Claims (10)

1. A method for synergistically extracting nickel from nickel plating wastewater is characterized by comprising the following steps:
s1, preparing a D2EHPA solution, adding alkali liquor into the D2EHPA solution, stirring to ensure that the saponification rate of the D2EHPA is 30-70%, layering reaction liquid after stirring, and taking upper-layer reaction liquid;
s2, adding a diluent into the upper layer reaction liquid in the step S1, and stirring, wherein the reaction temperature is controlled to be 15-35 ℃;
s3, continuously adding methyl isobutyl ketone into the upper layer reaction liquid in the step S1, stirring, and controlling the reaction temperature at 15-35 ℃ to obtain an extracting agent;
s4, adding an extracting agent into the nickel plating wastewater, uniformly stirring and mixing, layering the reacted solution after stirring, and taking the upper layer solution;
s5, adding an acid solution into the upper solution in the step S4 for back extraction, and obtaining a nickel-containing reclaimed material.
2. The method of claim 1, wherein in step S1, the concentration of the D2EHPA solution is 0.5-15 mol/L.
3. The method of claim 1, wherein in step S1, the concentration of the D2EHPA solution is 0.8mol/L, and the saponification rate of D2EHPA is 55%.
4. The method of claim 1, wherein in step S2, the diluent is sulfonated kerosene, and the volume ratio of the D2EHPA solution to the diluent is 1: 2-4.
5. The method of claim 1, wherein the volume of methylisobutylketone added in step S3 is 15-50% of the volume of the D2EHPA solution.
6. The method of claim 1, wherein the reaction temperature in steps S2 and S3 is controlled at 25 ℃.
7. The method of claim 1, wherein in step S4, the volume ratio of the nickel plating wastewater to the extracting agent is 1: 0.6-1.02, and the stirring is carried out for 15-40 min.
8. The method of claim 1, wherein in step S4, the volume ratio of the nickel plating wastewater to the extracting agent is 1:1, and the stirring is performed for 30 min.
9. The method of claim 1, wherein the volume ratio of the acid solution to the upper solution is 1: 0.8-1.5 in step S5.
10. The method of claim 1, wherein in step S5, the acid solution is one or more of sulfuric acid, hydrochloric acid and nitric acid.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113354024A (en) * 2021-06-08 2021-09-07 江西省核工业地质局机械研究所 Method for preparing nickel nitrate by using electroplating wastewater

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CN103224259A (en) * 2013-05-15 2013-07-31 大冶有色金属有限责任公司 Method for refining crude nickel sulphate and recycling valuable metals
CN106315731A (en) * 2016-09-13 2017-01-11 苏州湛清环保科技有限公司 Method for producing nickel oxide from nickel-plating wastewater
CN106521164A (en) * 2016-11-07 2017-03-22 清华大学 Composite extraction agent and method for recycling nickel from chemical nickel-plating waste liquid through composite extraction agent
CN107815542A (en) * 2017-10-17 2018-03-20 中南大学 A kind of synergic reagent and method for being used for nickel selective extraction in acid solution

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Publication number Priority date Publication date Assignee Title
JP2011052250A (en) * 2009-08-31 2011-03-17 Kansai Univ Method for recovering nickel from electroless nickel plating waste liquid, and nickel ion extraction agent used therefor
CN103224259A (en) * 2013-05-15 2013-07-31 大冶有色金属有限责任公司 Method for refining crude nickel sulphate and recycling valuable metals
CN106315731A (en) * 2016-09-13 2017-01-11 苏州湛清环保科技有限公司 Method for producing nickel oxide from nickel-plating wastewater
CN106521164A (en) * 2016-11-07 2017-03-22 清华大学 Composite extraction agent and method for recycling nickel from chemical nickel-plating waste liquid through composite extraction agent
CN107815542A (en) * 2017-10-17 2018-03-20 中南大学 A kind of synergic reagent and method for being used for nickel selective extraction in acid solution

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Publication number Priority date Publication date Assignee Title
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