CN107974561A - The chemically method of nickel plating Ageing solution recycling nickel resources - Google Patents
The chemically method of nickel plating Ageing solution recycling nickel resources Download PDFInfo
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- CN107974561A CN107974561A CN201610938475.4A CN201610938475A CN107974561A CN 107974561 A CN107974561 A CN 107974561A CN 201610938475 A CN201610938475 A CN 201610938475A CN 107974561 A CN107974561 A CN 107974561A
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- 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
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- 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
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
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- 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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Abstract
The present invention relates to a kind of method of chemically nickel plating Ageing solution recycling nickel resources, including step:A, the pH value of chemical nickeling ageing liquid is adjusted to 10.5 ~ 11.5；B, by the temperature control of above-mentioned chemical nickeling ageing liquid at 30 ~ 45 DEG C, into membrane contactor deamination;C, after deamination, using remaining sodium hypophosphite, solid solution or amorphous nickel-phosphorus alloy are directly reduced to.The present invention has following technique effect：The pollution problem of chemical nickeling ageing liquid can be effectively solved, while has recycled precious metal nickel again；And institute is using equipment is simple, the rate of recovery is high, cost is low, environmentally friendly and be easily achieved etc..
Description
Technical field
Technical field , Te Do the present invention relates to trade waste recycling are to be related to chemically nickel plating Ageing solution recycling nickel
The method of resource.
Background technology
Chemical nickel plating is a kind of without additional power source, directly under the action of strong reductant hypophosphites, makes N+2With
The plating piece surface of catalytic forms the process for treating surface of Ni-P alloy layers.Its coating have uniformity, corrosion resistance, hardness and
The superiority of solderability etc., oneself is widely used in electronics, petrochemical industry, automobile component, machine-building and aerospace etc.
Field.After plating solution uses one number time, accessory substance phosphite largely accumulates, and the white phosphorous acid nickel that indissoluble is produced with nickel ion sinks
Form sediment, decline quality of coating, or even plating solution is muddy, the own aging of plating solution at this time, need to scrap.It is the general nickeliferous 3~5g/L of Ageing solution, secondary
30~60g/L of sodium phosphate, 130~180g/L of sodium phosphite, 7000~10,000mg/L of ammonia nitrogen, complexing agent (organic acid) ＞ 30g/
L and other trace metal impurities etc..This kind of discarded plating solution contains a class of pollutant of plurality of heavy metal nickel, directly discharges meeting
Human health and life security are threatened, also causes the waste of nickel resources, therefore chemically nickel plating Ageing solution recycling nickel resources
It is paid more and more attention.
The method of conventional chemically nickel plating Ageing solution recycling nickel resources can generally be divided into chemical method and Physical, main bag
Include chemical precipitation method, catalytic reduction method, electrolysis, Li Jiao Change resin methods, solvent extraction, absorption method and UF membrane branch art
Deng.
Chemical precipitation method is typically that various precipitating reagents are added into chemical nickeling ageing liquid, such as sodium hydroxide, lime, vulcanization
The precipitable Ni such as sodium and vulcanization amidocarbonic acid dimethyl ester (DTC)+2Material, then with precipitation form remove nickel.Chemical precipitation work
Skill is simple ripe and investment is small, but has the following disadvantages:Secondary pollution is easily caused, the quantity of slag is big, and reagent consumption amount is greatly and introduction is new
Material make system more complicated etc..Catalytic reduction method is that sodium borohydride strong reductant reduction Ni is added in the Ageing solution of heating+2
Nickel resources are recycled for nickel-phosphor-boron alloy particle, or adds palladium bichloride, nickel powder, iron powder etc. and triggers plating solution generation as derivant
Nickel phosphorus particle, these catalyst or activator are difficult to promote the use of since cost is higher.Electrolysis handles chemical nickeling ageing
Liquid is mostly to use insoluble anode (such as PbO2) handled, organic complex occurs oxidation in anode and cracks, and nickel is in cathode
Upper precipitation.Electrolysis electrode used therein material expensive, and energy consumption is big, electrolytic efficiency is not also high.The nickel of Li Jiao Change resin methods recycling
Quality is high, and consumption medicament is less and degree for the treatment of is deep, but shortcoming is Ageing solution complex compound height, strong with reference to power, need to use and be complexed
Resin, input cost are high.Solvent extraction processing chemical nickeling ageing liquid needs more extraction series, in extraction and regenerative process
Organic solvent consumption is larger, and processing cost is higher.Adsorption material section used in absorption method includes activated carbon, humic acid and sepiolite etc. often
For low complexing and low Ni+2Concentration, saturated extent of adsorption is small, is not suitable for Ageing solution processing.Membrane separation technique include anti-Seepage thoroughly, film
Extraction and electricity Seepage analysis etc., at present Come say that this kind of technology has that the of high cost and rate of recovery of the big processing of equipment investment is low etc., it is difficult to
Promote the use of.
The application for a patent for invention of Publication No. CN101817607 discloses directly extracts in a kind of acidic chemical nickel plating waste solution
The method of nickel, by adding catalytic reducer and nickel METAL EXTRACTION carrier in waste liquid tank, recycles 97% nickel, and raffinate nickel is dense
Degree is down to 100mg/L.This method has the following disadvantages:1) substantial amounts of catalytic reducer is consumed；2) reaction temperature is up to 80~85
DEG C, increase energy consumption；3) rate of recovery only has 97%, and raffinate nickel concentration is up to 0.1g/L.
The application for a patent for invention of Publication No. CN102071410 discloses in a kind of chemically nickel-plating waste liquid and recycles nickel resources
Method, heat initiation reaction by adding catalytic reducer or nickel phosphorus particle derivant in waste liquid tank, chemical nickel plating is given up
The reducing agent initiation reaction of liquid remnants, precipitating nickel phosphorus particle.PH value in reaction is improved to 12,60~100 DEG C of reaction temperature, nickel recycles
Rate reaches as high as 99.9%.This method has the disadvantages that:1) reaction temperature height and Ageing solution ammonia containing 7000~10,000mg/L
Ammonia, under the reaction condition of high ph-values and high temperature, ammonia forms bubble, influences environment, and high energy consumption；3) raffinate nickel concentration is 3
~5mg/L, it is not yet up to standard.
The application for a patent for invention of Publication No. CN101892389 discloses in a kind of chemical nickel plating waste solution and prepares nano metal
The method of nickel, 2~3.3 grams of reducing agent thiourea dioxide is added in every liter of waste liquid, then adds 30~70 grams of sodium hydroxide Will
Waste liquid is adjusted to alkalescence, while is heated to 70~100 DEG C, isothermal reaction 5~20 minutes, and metal nickel powder, the rate of recovery 97% is made
More than.This method has the disadvantages that:1) additional a large amount of thiourea dioxide reducing agents；2) reaction temperature is high and Ageing solution contains 7000
~10,000mg/L ammonia ammonia, under the reaction condition of high ph-values and high temperature, ammonia forms bubble, influences environment, and high energy consumption；3)
Nickel recovery is low, and raffinate nickel concentration is up to 0.1g/L.
Publication No. CN102212842 discloses a kind of recovery method of nickel in chemical nickel-plating ageing liquid, and step is：1) take
1100~1300 parts by weight chemical nickeling ageing liquids add electrolytic cell, and it is 8~10 to adjust pH value with sodium hydroxide Will waste liquids；2) Will
0.01~0.03 parts by weight polyethanol, 0.01~0.02 parts by weight 2-mercaptobenzimidazole, 0.03~0.06 parts by weight thiocarbamide,
0.005~0.03 parts by weight hide glue, 0.3~0.5 parts by weight sodium hypophosphite, are dissolved in 40~70 parts by weight water, add electrolysis
Groove, adds 1/3 part of 5mol/L hydrochloric acid solution；3) at normal temperatures, using stainless steel as cathode, iridium dioxide titanium alloy reticulated Like plates are plated
For anode, kinetic current is 0.6~1A, and when the reaction time is 8~10 small, metallic nickel, nickel recovery 99.5% are recycled in cathode.
This method has the following disadvantages:1) additional multiple additives, the numerous Suo of operation, increases cost；2) iridium dioxide titanium alloy reticulated is used
Like plates are anode, and equipment is expensive, increase investment cost；3) nickel recovery is not high, raffinate nickel concentration 20mg/L, below standard.
It is clear that the recovery method of several nickel in chemical nickel-plating ageing liquid of Jie Shao respectively has feature, but these sides Shang Yi
Method has some disadvantages and using limitation, and as processing cost is high, cumbersome flow is complicated, nickel recovery is low, discharge is dense
Spend the problems such as high.
The content of the invention
Present invention solves the technical problem that it is to avoid shortcoming of the prior art from providing-kind of chemical nickeling ageing
The method that liquid recycles nickel resources, this method utilizes the reducing agent of Ageing solution remnants, and in the environment of higher ph, deamination, nickel is straight
Connect the nickel recovery method of reduction precipitating nickel phosphorus particle.
The technical solution adopted in the present invention is：
Using a kind of method of chemical nickeling ageing liquid recycling nickel resources, including step:
A, the pH value of chemical nickeling ageing liquid is adjusted to 10.5~11.5；
B, by the temperature control of above-mentioned chemical nickeling ageing liquid at 30~45 DEG C, into membrane contactor deamination；
C, after deamination, using remaining sodium hypophosphite, solid solution or amorphous nickel-phosphorus alloy, reaction equation are directly reduced to
It is as follows：
Ni2++H2PO2-+H2O→HPO3 2-+3[H+]+Ni
H2PO2-+[H+]→P+H2O+OH-
Nickle atom and phosphorus atoms are co-deposited, and form nickel phosphorus-alloy-layer
Ni+P → NI-P alloys
D, separation of solid and liquid is finally carried out, recycles nickel phosphorus particle.
Further,
Deamination is circulated, until the content of ammonia nitrogen is down to below 10mg/L.
The membrane contactor uses continuously elongated polypropylene hollow fiber hydrophobic film, and flux is 0.3~0.5m3/ h, gas
Liquid contact area is 10m2, water inlet maximum pressure is 6.0Pa.
The pH value of chemical nickeling ageing liquid is adjusted to 10.8 with NaOH.
The pH value of chemical nickeling ageing liquid is adjusted to 11.3 with NaOH.
Compared with prior art, the technical effects of the invention are that：Technique is simple, recovery cost is low, not additional reducing agent
And additive, nickel recovery are more than 99.99%, and it is recyclable be made 35% ammonium sulfate liquid (excellent nitrogenous fertilizer) accessory substance, it is nontoxic
Side effect, environmental protection, aqueous concentration is low, equipment investment is few, easy to operate and the advantages that be easily achieved.
Embodiment
For a better understanding of the technical solution of the present invention, the preferred embodiment of the present invention disclosed below is merely to illustrate
It is of the invention with explaining, but it is not used in the restriction present invention.
The method of-kind of chemical nickeling ageing liquid recycling nickel resources, the pH value of chemical nickeling ageing liquid is adjusted arrive first
10.5~11.5；Then temperature control is at 30~45 DEG C, into membrane contactor deamination；After deamination, using remaining sodium hypophosphite,
Solid solution or amorphous nickel-phosphorus alloy are directly reduced to, carries out separation of solid and liquid, recycles nickel phosphorus particle.Finally to molten after deamination
Liquid carries out separation of solid and liquid, recycles nickel phosphorus particle.Using remaining sodium hypophosphite, solid solution or amorphous nickel phosphorus are directly reduced to
The reaction equation of alloy is as follows：
Ni2++H2PO2-+H2O→HPO3 2-+3[H+]+Ni
H2PO2-+[H+]→P+H2O+OH-
Nickle atom and phosphorus atoms are co-deposited, and form nickel phosphorus-alloy-layer
Ni+P → NI-P alloys.
Mechanism of Electroless Nickel is:In an acidic solution, the electronics that sodium hypophosphite is produced with water reaction is reduced into nickel ion
Metallic nickel, in the process electronics also at the same time reduced small part phosphorus.Reaction process is as follows:
NaH2PO2+H2O→H2PO3 2-+2H++2e
Ni2++2e→Ni
H2PO2 -+2H++e→2H2O+P
2H++2e→H2
Carried out when reaction is lasting, nickel sulfate is reduced into metallic nickel, generates sulfate radical, and the pH value of plating solution reduces.Reacted
Journey is as follows:
NiSO4+NaH2PO2+H2O→Ni+NaH2PO3+H2SO4
Addition ammonium hydroxide is needed to maintain pH value to be more than 4 in operation.When aging is scrapped, ammonia nitrogen concentration is up to 10,000mg/L, this
And Ageing solution processing, nickel are difficult to the reason for up to standard.
Membrane contactor is with the membrane module of microporous hydrophobic doughnut film production.Gaseous state embrane method is to utilize microporous hydrophobic membrane
Nitrogen-containing wastewater and absorbing liquid are separated, the side of film is nitrogen-containing wastewater, and opposite side is acid absorbing liquid, adjusts waste water
PH value makes waste water ammonium ion be changed into free ammonia NH3, it diffuses to hydrophobic microporous film surface in waste water side by concentration boundary layer,
Then in film both sides NH3Under the promotion of concentration difference, NH3Gasification is through fenestra at waste water and microporous membrane interface, in microporous barrier and suction
Receive the generation ammonium salt solution that reacts on liquid interface with the H+ in acid absorbing liquid.Reaction equation is such as:
2NH3+H2SO4→(NH4)SO4
By temperature control at 30~45 DEG C, into membrane contactor.When Ageing solution temperature is improved to 60 DEG C from 10 DEG C, mass transfer
Coefficient is by 1.05 × 10-6M/s increases to 1.86 × 10-6M/s, ammonia-nitrogen removal rate are changed into 99.84% from 93%.Although improve temperature
It can accelerate the removing of ammonia, but consider to need to consume largely energy original to Ageing solution heating, so 30~45 DEG C of choosing pool.
The pH value of Ageing solution is adjusted to 10.5~11.5；With the NH in the increase Ageing solution of pH value4 +More easily it is converted into
NH3, that is, have more NH3Fenestra is passed through from Ageing solution, reacts and is removed with acid absorbing liquid on absorbing liquid interface.When
Ammonia nitrogen mass tranfer coefficient and removal efficiency tend towards stability substantially after pH value is more than 11.5, vary less.Therefore preferable ph for 10.5~
11.5；But not limited to this.
According to chemical nickel plating reaction equation and the utilization rate definition of sodium hypophosphite, the utilization of sodium hypophosphite can be calculated
Rate is as follows:
Because sodium hypophosphite utilization rate is not high, when chemical nickel plating is scrapped, remaining sodium hypophosphite, still there is enough reduction
Amount, therefore not additional reducing agent sodium hypophosphite.
Nickeliferous Ageing solution nickel ion content is in 4~6g/L, so when scrapping, nickel ion content is generally in 4g/L or so.Always
After changing the deamination film that liquid passes through membrane contactor, while temperature is controlled at 30~45 DEG C, pH value is more than 10.5, circulates deamination, works as ammonia
When nitrogen is down to below 10mg/L, nickel ion content is less than 0.3mg/L, and nickel recovery is more than 99.99%.
It is two specific embodiments below：
The deamination film specification of membrane contactor employed in experiment:Continuously elongated PP doughnuts hydrophobic film, shape ruler
It is very little0.3~0.5m of flux3/h；Gas liquid interfacial area is 10m2；Water inlet maximum pressure is 6.0pa.
Embodiment 1
Ageing solution source:The chemical nickeling ageing liquid of Kunshan Electronics Co., Ltd., through analysis:Nickel content 4318mg/L；
Ammonia-nitrogen content 8250mg/L；TP6070mg/L；COD22100mg/L；PH value is 1.34 (event of tank liquor containing nitre pH is low).
Take 20 to go up and state chemical nickeling ageing liquid, with NaOH adjustings pH to 10.8, electrical heating makes temperature maintain 40 DEG C,
Enter deamination film after filtering, continuous to circulate deamination one hour, ammonia-nitrogen content is down to 31mg/L；Reacting liquid filtering obtains black
Nickel phosphorus particle, particle 153.42g, nickel content 56.29%, filtrate nickel 0.3mg/L are obtained after dry；The rate of recovery>99.99%.
Embodiment 2
Ageing solution source:The chemical nickeling ageing liquid of Wuxi Electronics Co., Ltd., through analysis:Nickel content 4520mg/L,
Ammonia-nitrogen content 9870mg/L, TP6890mg/L, COD24600mg/L, pH value are 2.3 (event of tank liquor containing nitre pH is low).
Take 20 to go up and state chemical nickeling ageing liquid, with NaOH adjusting pH value to 11.3, electrical heating makes temperature maintain 45 DEG C,
Enter deamination film after filtering, continuous to circulate deamination one hour, ammonia-nitrogen content is down to 8mg/L；Reacting liquid filtering obtains the nickel of black
Phosphorus particle, obtains particle 158.03g, nickel content 57.2% after dry, filtrate nickel content is less than 0.3mg/L, and the rate of recovery is more than
99.99%.
As can be seen from the above-described embodiment, method provided by the present invention can be recycled efficiently in chemical nickeling ageing liquid
The rate of recovery of nickel can reach more than 99.99%.It is of the invention to contrast with existing technology, not only with technique is simple, cost
It is cheap, reaction condition is gentle, the advantage such as nickel recovery height, and concentration of emission is low, it is easy to accomplish industrialized production.
Claims (5)
- A kind of 1. method of chemical nickeling ageing liquid recycling nickel resources, it is characterised in that：Including step:A, the pH value of chemical nickeling ageing liquid is adjusted to 10.5 ~ 11.5；B, by the temperature control of above-mentioned chemical nickeling ageing liquid at 30 ~ 45 DEG C, into membrane contactor deamination;C, after deamination, using remaining sodium hypophosphite, solid solution or amorphous nickel-phosphorus alloy are directly reduced to, reaction equation is such as Under：Ni2+ + H2PO2- + H2O → HPO3 2- +3[H+] + Ni H2PO2-+[H+] →P+H2O+OH-Nickle atom and phosphorus atoms are co-deposited, and form nickel phosphorus-alloy-layer,Ni+P → NI-P alloys；D, separation of solid and liquid is finally carried out, recycles nickel phosphorus particle.
- 2. the method for chemical nickeling ageing liquid recycling nickel resources as claimed in claim 1, it is characterised in that：Circulate deamination, Until the content of ammonia nitrogen is down to below 10mg/L.
- 3. the method for chemical nickeling ageing liquid recycling nickel resources as claimed in claim 1, it is characterised in that：The film contact Device uses continuously elongated polypropylene hollow fiber hydrophobic film, and flux is 0.3 ~ 0.5m3/ h, gas liquid interfacial area 10m2, water inlet Maximum pressure is 6.0Pa.
- 4. the method for chemical nickeling ageing liquid recycling nickel resources as claimed in claim 1, it is characterised in that：By chemical nickel plating The pH value of Ageing solution is adjusted to 10.8 with NaOH.
- 5. the method for chemical nickeling ageing liquid recycling nickel resources as claimed in claim 1, it is characterised in that：By chemical nickel plating The pH value of Ageing solution is adjusted to 11.3 with NaOH.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114032558A (en) * | 2021-12-14 | 2022-02-11 | 北京科技大学 | Method for preparing NiP micron particles from chemical nickel plating waste liquid through electrolysis |
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| CN104668576A (en) * | 2014-12-11 | 2015-06-03 | 张志莲 | Chemical nickel-plating waste liquid recycling method |
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| RU2166551C2 (en) * | 1998-11-11 | 2001-05-10 | Открытое акционерное общество "Ижевский радиозавод" | Method of nickel recovery from spent alkali solutions of electroless nickel |
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| CN102942280A (en) * | 2012-11-14 | 2013-02-27 | 北京赛科康仑环保科技有限公司 | Method for decomplexing heavy metal ammonia complex in high-concentration ammonia-nitrogen wastewater |
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| CN114032558A (en) * | 2021-12-14 | 2022-02-11 | 北京科技大学 | Method for preparing NiP micron particles from chemical nickel plating waste liquid through electrolysis |
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Application publication date: 20180501 |