CN107119311A - The quick clean online plating solution negative pressure evaporation reuse method of electronickelling production line and equipment - Google Patents
The quick clean online plating solution negative pressure evaporation reuse method of electronickelling production line and equipment Download PDFInfo
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- CN107119311A CN107119311A CN201710515409.0A CN201710515409A CN107119311A CN 107119311 A CN107119311 A CN 107119311A CN 201710515409 A CN201710515409 A CN 201710515409A CN 107119311 A CN107119311 A CN 107119311A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/16—Regeneration of process solutions
- C25D21/18—Regeneration of process solutions of electrolytes
Abstract
The quick clean online plating solution negative pressure evaporation reuse method of electronickelling production line and equipment, during electroplate liquid nickel ion 0.20~30mg/L of mass concentration, collect in advance and import accumulator tank (4), introduce to reclaim according to flow and equipment disposal ability and place bucket (6), in 0.08MPa, concentration board (7) is cycled through under the conditions of 55 70 DEG C to carry out introducing concentration placement bucket (9) after negative pressure drying, when being higher than 30mg/L by on-line monitoring nickel ion mass concentration containing nickel plating solution, dried treatment fluid is inputted into coating bath (10) reuse again, nickel ion is free of in the evaporation moisture being collected into drying process.Reduce and even avoid arranging outside waste water, overcome heavy metal nickel with the long-standing abuse that can not be administered that pollutes arranged outside waste water to environment at all, reduce wastewater treatment expense, lead back coating bath with the recovered liquid after concentration and carry out circulation supplement, save the consumption of nickel stoste, economic security environmental protection.
Description
Technical field
The present invention relates to the electrolysis of C25D coating in IPC classification or electrophoresis manufacturing technique method;Electroforming auxiliary equipment device
Structure improved technology, the especially quick clean online plating solution negative pressure evaporation reuse method of electronickelling production line and equipment.
Background technology
At present, as electroplating industry develops, plating plating material used is mainly the noble metals such as copper, chromium, nickel, per electricity together
There is one-level rinsing, two grades of rinsings, three-levels to rinse as plating process is latter etc., washing process can take part noble metal out of.The sector
Usual practice be that washings are directly discharged to sewage plant processing, the conventional treatment method of use is will a huge sum of money by physico-chemical process
Category precipitation, the consequence of generation is both to waste noble metal, and secondary heavy metal pollution may be caused again.
The waste component produced in electroplating process is extremely complex, and wherein heavy metal wastewater thereby is electroplating industry potential hazard pole
Big waste water classification.Nickel is a kind of heavy metal that can be carcinogenic, in addition it or a kind of metals resources costly, and price is copper
2~4 times.Electronickelling is widely used in plating production because it has excellent wearability, corrosion stability, solderability, and it adds
Work amount is only second to zinc-plated, and second is occupied in whole electroplating industry.A large amount of nickel-containing waste waters are produced in Ni-Speed.If nickeliferous
The untreated any discharge of waste water, can not only endanger environmental and human health impacts, can also cause the waste of Precious Metals Resources.
The type of nickel-plating liquid mainly has sulfate type, chloride type, sulfamic acid salt form, citric acid salt form, borofluoride
Type etc..It is that the referred to as application of meaning watt Watts nickel-plating liquids industrially is the most universal wherein with sulfate type subchloride.It is several
The physical property of nickel coating obtained in different nickel plating solutions, as listed by table 2-3-45.Sulfamic acid salt form, fluoboric acid salt form
Suitable for the thick nickel of plating or electroforming.Citric acid salt form is applied to the direct nickel plating on zine pressure casting.The cost of this several plating solution compares
It is high.Electroplate liquid environment directly affects operation quality, such as the white dot that electronickelling occurs is exactly one of wherein typical phenomenon,
This is caused by a kind of high-carbon thing, high-carbon thing be by heat treatment carburizing process and pre-electroplating treatment when acid cleaning process in produce
's.Existing corresponding solution includes:(1) pretreatment cleaning process is improved, the method cleaned using ultrasonic wave is made attached after carburizing
The particle for putting forth effort difference is split away off in cleaning;(2) plating solution is filtered in time;(3) acid cleaning process is improved:Mainly reduce
The concentration of pickle, the time for adding suitable corrosion inhibiter and suitable control pickling, it is to avoid excessive erosion.Implement these measures, electricity
Plating hickie problem has obtained the solution of essence.
The technology of being correspondingly improved discloses less.Chinese patent application 200510053288.X discloses a kind of for electroplating production
The device of line online recycling nickel metal, to one-level nickel plating washings, using secondary filter plus the method for evaporation and concentration, direct reuse
To coating bath;Using the moon of two sun one Jia one to two, three-level washings, mixed ion-exchange is separated, can from the regeneration of one-level male post
Obtain NiSO4 solution.Mixed column water outlet is up to pure water level, direct reuse to production line.
Chinese sewage treatment project net August in 2015 discloses more recent achievement in research on 19th, and the document is according to difference
Principle, the method that chemically method, physical-chemical process and biological treatment three major types review processing Treating Electroplate Wastewater Containing Nickel.Wherein:
Mainly there are traditional chemical precipitation method, novel process ferrite process using chemical Treatment Treating Electroplate Wastewater Containing Nickel, with
And efficient heavy chelate precipitation.Wherein chemical precipitation method includes hydroxide precipitation method, sulphide precipitation again.
In the experimental study of chemical precipitation method processing electroplating wastewater, with CaO, CaCl2、BaCl2Three kinds of contact break mixture processing platings
Nickel waste water, contrast is found:BaCl2Contact break close effect preferably, the clearance highest of nickel ion, CaCl2Effect it is worst.By CaO
With BaCl2Combination processing nickel-plating waste water, the clearance of nickel ion is up to more than 99%, and when the clearance of nickel ion is identical,
BaCl2Usage amount than its it is independent processing nickel-plating waste water when it is few a lot.Scientist first using Fenton reagent aoxidize, after adopt
Aoxidized with NaClO, be 3~5, Ni to pH2+Mass concentration carries out contact break pretreatment for 100~150mg/L nickel-containing waste water, finally
Handled through chemical precipitation, nickel ion mass concentration in final outflow water supernatant is less than 0.1mg/L.
In chemical precipitation method, relatively new type technique is ferrite process.FeSO4Various heavy metal ion formation iron can be made
Oxysome crystal and Precipitation, ferrite formula are FeOFe2O3.Ni in waste water2+Fe can be occupied2+Lattice formation co-precipitation
And remove.Experimental studies results show that ferrite process handles the process conditions of nickel-containing waste water] in pH=9.0, n (Fe2+)∶n(Ni2 +)=2: 1, temperature is under conditions of 70 DEG C, and the conversion ratio of nickel is up to more than 99.0%, the Ni in waste water2+It can be dropped from 100mg/L
To 0.47mg/L.Study the process conditions that ferrite process at room temperature handles low concentration nickel-containing waste water.Result of the test shows, with
Na2CO3It is 8.5~9.0, n (Fe in pH for pH adjusting agent3+)∶n(Fe2+)=1.5: 1, n (Fe2+)∶n(Ni2+)=12: 1, are stirred
The time is mixed under conditions of 15min, treatment effect is optimal.
All there is ferrous ion in 2 kinds of techniques of Fenton methods and ferrite process, work is combined using Fenton- ferrite process
The complexing electroplating wastewater of skill Treatment of Copper, nickel.As a result show, in initial pH on wastewater=3, H2O2Initial mass concentration is 3.33g/
L, m (Fe2+)∶m(H2O2Under the conditions of)=0.1, the optimal Fenton oxidation of 25 DEG C of temperature, 60min first is handled to waste water Fenton,
Wastewater sedimentation pH=11 is adjusted afterwards, and the mass ratio for controlling aeration flow to be metal ion in 25mL/min, iron and waste water is 10,
Reaction temperature is 50 DEG C, and aeration time of contact is 60min, and the clearance of nickel ion reaches 99.94% in waste water on this condition,
The mass concentration of water outlet nickel ion is 0.33mg/L.
A kind of experiment heavy metal ion chelating agent HMCA of synthesis, HMCA is applied in nickel-plating waste water, pH be 6.5~
When 7.5, Ni2+Clearance up to more than 98.5%.The chelating agent is to Ni2+With good trapping ability, and and Ni2+Effect
The chelate products compact structure of formation is stable.When metal-chelator mass concentration is 3.79g/L, Ni2+Mass concentration it is minimum
For 0.45mg/L, the treatment effect to nickel-plating waste water is significantly improved.A kind of new having has been synthesized in the basic conditions to wad a quilt with cotton
Coagulate, chelate difunctional heavy metal chelant --- PAS, and the PAS chelatings for being used for heavy metal nickel ion are tested, experimental result
Show, add 0.6mL PAS to the clearance of 50mg/L nickel-containing waste water up to more than 98%, it is seen that PAS is to Ni2+It is a kind of
Good chelating agent.
Absorption method is a kind of effective ways of the unique texture heavy-metal ion removal using adsorbent.Zeolite, activated carbon,
Humic acid etc. is often by the adsorbent as processing Treating Electroplate Wastewater Containing Nickel.
Artificial zeolite function is similar to natural zeolite, but foreign organic matter is fewer in duct, and application is wider.With oblique hair
Zeolite is to Ni2+Adsorbed, maximal absorptive capacity is up to 13.03mg/g.Zeolite surface is modified with dimethylglyoxime (DMG),
With the Ni adsorbed through the modified artificial zeolite of cetyl trimethylammonium bromide (CTAB) in simulated wastewater2+.As a result show:Solution
Volume is 25mL, and initial mass concentration is 20mg/L, pH=7.0, and when temperature is 35 DEG C, adding quality in modified zeolite is
1.1g, under the conditions of adsorption time is 50min, adsorption rate is up to more than 98%, and by other interfering ions (Cu2+、Pb2+) influence
Less.Using studies on Spectrophotometric Determination, new modified zeolite (Na-Y types) is to Ni in electroplating wastewater2+The influence of removal effect.Knot
Fruit shows, under conditions of room temperature, pH=4, when it is 2h to add modified zeolite mass fraction to be 0.4%, adsorption time, waste water
Ni in solution2+Clearance up to more than 99%, Na-Y types zeolite after HCl and NaCl mixed solution leaching regenerations repeat make
With adsorbance has declined after regeneration, but declines unobvious.
Activated carbon can more efficiently remove the complex ni-ion in waste water, under the conditions of Static Adsorption, have studied powder
Absorption behavior of the shaped activated carbon to low quality concentration citric acid complex nickel ion in the aqueous solution.Result of the test shows:Solution is initial
PH=11.0, when activated carbon adds mass concentration for 10.0g/L, the clearance of nickel ion reaches 72.3%.
Heavy metal Ni is handled by using humic acid resin2+Experiment show:It is 5.0~7.0, Ni in wastewater pH2+Quality
Concentration is 50mg/L, and humic acid resin is by ion exchange and Absorptive complex wave to Ni2+Clearance up to more than 98%, and processing
Waste water is close neutral afterwards, Ni in waste water2+Content be substantially less than discharging standards.
At present, the adsorbent industrially generally used is expensive, constrains the extensive use of adsorption technology, adsorbs simultaneously
The regeneration and secondary pollution of agent be also adsorption technology processing waste water during should emphatically consider the problem of.
With continuing to develop for new macroporous type ion exchange resin and ion exchange continuous process, ion-exchange is made
Once causing the interest of academia for the means of nickel plating rinse water " zero-emission ".
Adsorption experiment is carried out to low-concentration sulfuric acid nickel solution using ion-exchange, as a result shown:At room temperature, 001 × 8 type
Highly acid gel-network precipitation method 4.0g, nickel ion mass concentration 1.0g/L, reaction time 60min, pH 5~6, nickel
The ion rate of recovery can reach more than 95%.Dynamics research shows that the rate of adsorption is mainly by Liquid film diffusion control.Pass through amino phosphorus
Sour chelating resin is drawn with other chelating resins to the nickel ion absorption property comparative test in faintly acid electroplating wastewater:Amino phosphorus
Sour chelating resin is by H+Type turns Na+To Ni after type2+Adsorbance improve 29.5%.Ni in water after processing2+Mass concentration is less than
0.020mg/L.Electroplating wastewater processing, Ni are carried out using ion exchange technique2+Clearance can be more than 99%.
Ion exchange technique is combined with membrane technology, composition novel process has been obtained very for handling Treating Electroplate Wastewater Containing Nickel
Good treatment effect.Using ion exchange-ultrafiltration-counter-infiltration group technology processing nickel-plating rinsing waste water, the system is by connecting
After the operation of continuous four wheat harvesting periods, monitoring result is shown, Ni in nickel-plating rinsing waste water2+Mass concentration is down to 1.0mg/L by 424mg/L
Hereinafter, Ni2+The rate of recovery is more than 99%, and waste water entirety reclamation rate is more than 60%, and system water outlet can be back to use in nickel-plating rinsing groove.Should
Method has the advantages that stable effluent quality and recyclable nickel resources, water resource.
Using ultrafiltration-counter-infiltration group technology concentrating and separating nickel-plating rinsing waste water, effluent quality is close to pure water.Using
Two-stage RO membranous systems are handled nickeliferous 250~350mg/L poaching wastewater, to the rejection of nickel up to more than 99.9%.
Using nanofiltration UF membrane electronickelling washings, to the clearance of nickel ion up to 99.5%, water outlet can be arranged directly
Put or be back to workshop.Using membrane electrolysis to Ni2+Mass concentration is 2000mg/L, and pH=5.32 nickeliferous simulated wastewater is carried out
Processing.And to single pole room of anode membrane two, single pole room of cavity block two and the different film electrolytic combination treatment effects of three kinds of three pole room of double films
Compare, as a result show:Single cavity block electrolysis is during electrolysis, and the H+ that anode reaction is produced is by anolyte
OH-Neutralize, while cavity block also prevents H+Pass through, so as to improve the rate of recovery of nickel.And current efficiency may be up to more than 90%, with
General electrolytic method is compared to improving 30%, and electrolyzing rate is above single anode membrane and dual membranes and three chambers electrolysis.Handle nickeliferous using electroosmose process
Electroplating wastewater requires nickel ion mass concentration >=1.5g/L in rinse water, to improve dialysis rate.Concentrate after electrodialysis process
Cocnentration factor than reverse osmosis concentration than high, can realize that chemical nickel-plating liquid regenerates using this advantage.Proof has been tested by the country, adopts
With the nickel sulfate of electroosmose process recyclable 90%, the nickel sulfate mass concentration of recovery reaches 80~100g/L, can directly return coating bath
Use.
To sum up it is known that application of membrane separation technology has unique advantage in the processing of Treating Electroplate Wastewater Containing Nickel, can not only have
Effect removes the Ni in waste water2+, make it with low concentration qualified discharge or waste water recycling, and filter membrane be retained down it is nickeliferous heavy
Slag can be recycled, environment friendliness.Compared with other technologies, membrane technology equipment is simple, wide using scope, handling rate
Height, without adding chemical reagent, therefore does not result in secondary pollution.But membrane module is expensive, and can produce film in use
Where pollution, the problem of this is limitation membrane technology extensive use.
Treating Electroplate Wastewater Containing Nickel is handled using ion floatation method, there is higher clearance to nickel ion.Pass through ion floatation method
The research for handling electroplating wastewater finds that ion flotation has very high clearance, wherein nickel to metal ions such as cadmium, zinc, copper, nickel
Residual qualities concentration it is minimum up to 0.33mg/L, nickel grade is 13.2% in froth pulp, with high resource reclaim valency
Value.Binary metal ion copper and mickel is handled using floatation, copper, the clearance of nickel can respectively reach 92.46%,
93.14%.Single treatment and mixed processing experiment, nickel ion in single experiment are carried out using floatation to nickel ion and copper ion
The rate of recovery up to more than 99.5%.
Ion floatation method has the two-fold advantage of extraction and ion-exchange, has in processing electroplating wastewater and adapts to model
The features such as enclosing wide, clearance high, and precious metals in waste water can be reclaimed.But, current ion floatation method is useless for heavy metal
The processing application of water is confined to the separation to one pack system, and the research handled two components and Multicomponent Wastewater is less.
At present, the key issue of biosorption process processing nickel-containing waste water is the strain adsorbance that can be used for absorption nickel ion
It is universal relatively low.Mutagenesis is carried out to absorption nickel bacterium B8 using RF low-temperature plasma, and tests suction of the mutant to nickel ion
Attached ability.Test result indicates that, obtained mutant Ni12 (Pseudomonas cedrina) reaches to the adsorbance of nickel ion
136.7mg/g (dry mycelium), 11.7% is improved than original strain B8.Using porous ceramics as carrier, it is aerated using microorganism
Biofilm method fixed mutation body Ni12, is handled the solution containing nickel ion, its adsorption rate is up to 86%.Mutant Ni12 is to nickel
Ion has stronger adsorptivity, can stablize heredity, have good application prospect to the processing of nickel-containing waste water.Screen a kind of thermophilic nickel bacterium
And have studied special efficacy absorption of the thermophilic nickel bacterium to nickel ion under optimal conditions.Pass through adsorption rate versus time curve:Nickel
Mass of ion concentration is 25mg/L, and absorption 2h adsorption reactions are to tend to balance, and adsorption rate reaches as high as 97.7%, to exceeded 50 times
Nickel-containing waste water, single treatment is close to the discharge standard of nickel;The bacterium is to the Ni in nickel-containing waste water2+There is wholesomeness absorption.
Scientist makees carrier with rice husk to being fixed of sulfate reducing bacteria, can effectively remove the nickel ion in waste water,
Clearance is up to 99%.There is experimental study to show, red bacillus is to Ni2+Clearance up to 90%.Whiterot fungi
(P.chrysosporium) to Ni2+Maximal absorptive capacity up to 56mg/g.Gene recombination bacterium E.coli JM10 are to Ni2+Enrichment
Ability is added more than 6 times than original strain.
At present, both at home and abroad on biological adsorption research more be in laboratory stage, laboratory has been achieved with fixation cell
The continuous operation of cell space system.Technique for gene engineering has also been applied in terms of microorganism adsorption.However, current to biological adsorption agent
The understanding of kinetics and thermodynamics and biosorption mechanism between heavy metal is also insufficient, more inexpensively, adsorbs
The bigger biological adsorption agent of capacity also awaits exploitation.Therefore, biotechnology will industrially be widely used an also spacing
From.
New《Electroplating industry pollutant discharging standards》The promulgation of (GB21900-2008), compared to former《Sewage
Comprehensive discharge standard》(GB 8978-1996), improves the emission request of nickel-containing waste water.
To reach requirements at the higher level discharge standard, conventional processing method is after flocculation treatment plus ion exchange, film at
The techniques such as reason, electrodialysis do further advanced treating, which adds processing unit number, substantially increase processing cost.Cause
This, can improve the efficiency of heavy metal containing wastewater treatment and can simplify handling process, and reduction electroplating enterprise cost for wastewater treatment will be
Handle an important directions of Treating Electroplate Wastewater Containing Nickel research.
Handle Treating Electroplate Wastewater Containing Nickel conventional adsorption technology, ion exchange technique, membrane separation technique, ion flotation technology etc.
The new and effective water technology for being all based on resource reclaim and growing up, physical chemistry new technology, the rise of new technology with
The progressive electroplating enterprise clean manufacturing that makes it possible.
Related improved technology also includes being concentrated by evaporation recovery process, and consumption of raw and auxiliary materials is larger, and operating cost is higher, it is difficult to pay
It is all to be widely implemented, especially, it is impossible to which the basic outer discharge capacity of sludge that solves is huge and the problem of can not be fully cleaned up processing, it is difficult to long
Phase stable practical application.
The content of the invention
It is an object of the invention to provide the quick clean online plating solution negative pressure evaporation reuse method of electronickelling production line and equipment,
With relatively low device fabrication and operating cost, decontamination cycle Water circulation while realizing recovery noble metal nickel completes clean manufacturing
Process.
The purpose of the present invention will be realized by following technical measures:Reclaim placement bucket and connect dense by pipeline and circulating pump
Contracting board and concentration are placed and install heater on bucket, concentration board, meanwhile, concentration board connection vacuum and negative pressure pump, moreover, vacuum
Negative pressure pump is connected with exhaust treatment system.Contain nickel plating solution for what is produced in electroplating assembly line production process, by online prison
Survey, during nickel ion 0.20~30mg/L of mass concentration, collect import accumulator tank in advance, then, energy is handled according to flow and equipment
Power, which introduces to reclaim, places bucket, then, and concentration board is cycled through under the conditions of -0.08MPa, 55-70 DEG C and is carried out after negative pressure drying
Introduce concentration and place bucket, when being higher than 30mg/L by on-line monitoring nickel ion mass concentration containing nickel plating solution, then after drying
Treatment fluid input coating bath, realize online rapid concentration reuse, at the same time, in the evaporation moisture being collected into drying process not
Containing nickel ion.
Especially, vacuum and negative pressure pump, circulating pump, recovery are placed bucket, concentration board and concentration placement bucket and installed concentratedly in machine
In vivo, body upper connects out pipeline access exhaust treatment system, wherein, exhaust treatment system is accessed dense by vacuum and negative pressure pump
In contracting board.
Especially, accumulator tank is connected by pipeline by circulating pump, meanwhile, bucket is placed by concentration and passes through pipeline coating bath.
Advantages of the present invention and effect:The plating solution containing heavy metal nickel produced in electroplating assembly line production process can be realized
Line rapid concentration, not only improves the normal reuse of support, is also effectively reclaimed so as to follow-up, accordingly obtains clean while being concisely and efficiently
Recovery washings, using water wisely reduces and even avoids arranging outside waste water, overcome heavy metal nickel to be caused to environment with being arranged outside waste water
The long-standing abuse that can not be administered at all is polluted, wastewater treatment expense is reduced.Meanwhile, lead back coating bath with the recovered liquid after concentration and circulated
Supplement, saves the consumption of nickel stoste, reduces production cost, economic security environmental protection.
Brief description of the drawings
Fig. 1 is the online nickel recovery process step schematic diagram in the embodiment of the present invention 1.
Fig. 2 is the structural representation of the embodiment of the present invention 1.
Reference includes:
Bucket 6, concentration board are placed in body 1, exhaust treatment system 2, vacuum and negative pressure pump 3, accumulator tank 4, circulating pump 5, recovery
7th, bucket 9, coating bath 10 are placed in heater 8, concentration.
Embodiment
Nickel is both heavy metal and noble metal, changes the understanding of traditional handicraft, and the same for the treatment of fluid water content is reduced to dry
Shi Tigao wherein goes forward side by side method of the step as working solution reuse containing nickel concentration, substitutes tradition early stage and starts to solve to remove waste water
In nickel ion way, with pursue more make full use of precious metal nickel, to greatest extent reduction be even up to zero-emission, realize
Circulate the purpose of clean manufacturing.
When nickel ion mass concentration is 30~200mg/L in general nickeliferous electroplating processes liquid, after being handled using ferrite process
The precipitation particle of formation is big and is easily isolated, and particle will not be redissolved, non-secondary pollution, and effluent quality is good, can reach discharge mark
It is accurate.The clearance of nickel reaches more than 98%, and nickel ion mass concentration reaches below 0.20mg/L in the waste water after processing, reaches state
Family's discharge standard.In addition, the material phase analysis of precipitating sludge shows under these conditions, obtained under optimum process condition
NiFe2O4、Fe3O4Recycled Deng ferrite sediment both non-secondary pollution but also as magnetic material.
Treating Electroplate Wastewater Containing Nickel mostlys come from coating bath waste liquid and plating piece washings in nickel plating production process, waste plating solution amount it is few but
Wherein nickel ion concentration content is very high, and plating piece washings are the main sources of electroplating wastewater, accounts for plant effluent discharge capacity
More than 80%.Plating piece washings water is big, but wherein nickel ion concentration is much smaller compared with waste plating solution.According to《Plating pollution
Thing discharge standard》(GB 21900-2008) table 2, it is allowed to which being discharged into the electroplating wastewater of water body total nickel mass concentration is up to
0.5mg/L。
The principle of the invention is, changes and break through the theory that tradition administers waste water, will contain nickel plating bath as generation and safeguard complete
Working solution is treated, and using low-temperature evaporation principle under negative pressure, the moisture in recovered liquid is quickly proposed, its nickel concentration is effectively carried
Height, then it is back to use coating bath progress treatment fluid circulation supplement.
Negative pressure evaporation belongs to atypia vacuum drying, also known as parsing-desiccation, is that material is placed in negative pressure of vacuum condition by one kind
Under, making the boiling point of water reduces, and the boiling point of water at one atm is 100 DEG C, and the boiling point of water can be made under the conditions of negative pressure of vacuum
80 DEG C are dropped to, 60 DEG C, 40 DEG C start evaporation, and prior art supports that vacuum drying can be at a temperature of 20 DEG C, 5 DEG C, -5 DEG C, -10 DEG C
By moisture evaporation, it is especially suitable for solving the stoving process of heat sensitive material, this is for being avoided in electroplate liquid other materials in high temperature
Extraction and cleaning water is polluted in evaporation significant.Considered based on production cost, at reduced pressure conditions, with relatively low heating temperature
The Technological Economy that degree completes this evaporation process is relatively reasonable.It is demonstrated experimentally that influenceing vacuum drying factor mainly to have:Concentrate
Relative density, the dry temperature of vacuum ten, vacuum drying vacuum, vacuum drying time etc..Vacuum drying temperature is not higher than 70 DEG C,
It is preferably controlled within 60 DEG C or so;Negative-pressure vacuum degree is controlled in 0.08MPa or so, and the too low rate of drying of vacuum can be very slow,
The too high electroplate liquid of vacuum easily splashes cruelly;The negative pressure drying time is controlled with moisture, simultaneously as nickel salt is non-volatile, institute
To be free of nickel ion in the evaporation water being collected into.It is more dry for the concentration electroplate liquid after 60 DEG C under the conditions of this processing in 5 hours
Dry hot mass metering relative density preferably controls the thick paste for 1.30~1.35.Because the operating temperature of nickel-plating liquid is 55-60 DEG C,
Generally there is large quantity of moisture evaporation in electroplating process, therefore dilute nickel-plating liquid of the concentration discharge after negative pressure drying can smoothly add plating
Reuse in nickel groove, is also beneficial to maintain normal production.
Nickel ion concentration conventional determining method is to use EDTA complexometries in plating solution, and murexide is indicator.
Reagent:
(1) concentrated ammonia liquor (density:0.91g/ml);
(2) murexide indicator (murexide: sodium chloride=1: 100);
(3) EDTA solution 0.05mol, is routinely demarcated;
Analysis method:
The chemical nickel-plating liquid after 10ml coolings is taken out in 250ml conical flask with pipette, and adds 100ml distillations
Shake up, titrated with calibrated 0.05mol EDTA solution after water, 15ml concentrated ammonia liquors, addition about 0.2g murexide indicator,
When solution colour by light brown fades to purple as terminal.
The calculating of nickel content:
Ni2+=5.87M × V (g/L)
M in formula --- the molar concentration of standard EDTA solution;
V --- the milliliter number of usage standard EDTA solution.
In the present invention, contain nickel plating solution for what is produced in electroplating assembly line production process, by on-line monitoring, nickel ion
During 0.20~30mg/L of mass concentration, collect import accumulator tank in advance, then, introduced and reclaimed according to flow and equipment disposal ability
Bucket is placed, then, introducing concentration after concentration board progress negative pressure drying is cycled through under the conditions of -0.08MPa, 55-70 DEG C and is put
Bucket is put, when being higher than 30mg/L by on-line monitoring nickel ion mass concentration containing nickel plating solution, then dried treatment fluid is defeated
Enter coating bath, realize online rapid concentration reuse, at the same time, nickel ion is free of in the evaporation moisture being collected into drying process.
On the other hand, terminate the final process liquid of rear volume or limited quality for plating production, can take and store for future use, or,
Recycled with foregoing art methods, though this process than it is relatively time-consuming in addition it is costly be also worth.
The invention will be further described with reference to the accompanying drawings and examples.
Embodiment 1:One kind of equipment of the present invention realizes structure, as shown in Figure 2, reclaim place bucket 6 by pipeline and
The connection of circulating pump 5 concentration board 7 and concentration are placed and install heater 8 on bucket 9, concentration board 7, meanwhile, concentration board 7 is connected very
Idling press pump 3, moreover, vacuum and negative pressure pump 3 is connected with exhaust treatment system 2.
In the present embodiment, vacuum and negative pressure pump 3, circulating pump 5, recovery place bucket 6, concentration board 7 and concentration and place bucket 9
Install concentratedly in body 1, the top of body 1 connects out pipeline access exhaust treatment system 2, wherein, exhaust treatment system 2 passes through
In the access concentration board 7 of vacuum and negative pressure pump 3.
In the present embodiment, accumulator tank 4 is connected by pipeline by circulating pump 5, meanwhile, bucket 9 is placed by concentration and passes through pipeline
Coating bath 10.
Claims (4)
1. the quick clean online plating solution negative pressure evaporation reuse method of a kind of electronickelling production line, it is characterised in that given birth to for plating
What is produced in producing line production process contains nickel plating solution, by monitoring on-line, during nickel ion 0.20~30mg/L of mass concentration, in advance
Collect and import accumulator tank (4), then, introduce to reclaim according to flow and equipment disposal ability and place bucket (6), then ,-
Cycled through under the conditions of 0.08MPa, 55-70 DEG C concentration board (7) carry out negative pressure drying after introduce concentration place bucket (9), containing
When nickel plating solution process on-line monitoring nickel ion mass concentration is higher than 30mg/L, then dried treatment fluid is inputted into coating bath
(10) online rapid concentration reuse, is realized, at the same time, nickel ion is free of in the evaporation moisture being collected into drying process.
2. the equipment of the quick clean online plating solution negative pressure evaporation reuse of a kind of electronickelling production line, it is characterised in that reclaim and place
Bucket (6) is placed by pipeline and circulating pump (5) connection concentration board (7) and concentration and installs heating on bucket (9), concentration board (7)
Device (8), meanwhile, concentration board (7) connection vacuum and negative pressure pump (3), moreover, vacuum and negative pressure pump (3) connects with exhaust treatment system (2)
Connect.
3. the equipment of the quick clean online plating solution negative pressure evaporation reuse of electronickelling production line as claimed in claim 2, its feature
It is, vacuum and negative pressure pump (3), circulating pump (5), recovery place bucket (6), concentration board (7) and concentration and place bucket (9) concentration peace
In body (1), body (1) top connects out pipeline access exhaust treatment system (2), wherein, exhaust treatment system (2) leads to
Cross in vacuum and negative pressure pump (3) access concentration board (7).
4. the equipment of the quick clean online plating solution negative pressure evaporation reuse of electronickelling production line as claimed in claim 2, its feature
It is, accumulator tank (4) is connected by pipeline by circulating pump 5, meanwhile, bucket (9) is placed by concentration and passes through pipeline coating bath (10).
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