CN101260559A - Technique for purifying nickel-plating liquid by extracting sprinkling method - Google Patents

Technique for purifying nickel-plating liquid by extracting sprinkling method Download PDF

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Publication number
CN101260559A
CN101260559A CNA2007100270782A CN200710027078A CN101260559A CN 101260559 A CN101260559 A CN 101260559A CN A2007100270782 A CNA2007100270782 A CN A2007100270782A CN 200710027078 A CN200710027078 A CN 200710027078A CN 101260559 A CN101260559 A CN 101260559A
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plating
resin
exchange column
extracting
liquid
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CNA2007100270782A
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郭焕林
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Abstract

The invention relates to a technology for purifying nickel plating solution with the extraction-elution method. The invention is characterized in that: organophosphorous extractant P507 or CL-P507 extraction-elution resin is adopted in the technology and is loaded by ion exchange columns; carbon supported P507 or the CL-P507 extraction-elution resin are filled in the ion exchange columns; an acid proof pump is used to extract plating solution, so that the plating solution passes through the exchange columns in sequence; under the condition that pH is less than four, Cu, Fe, Zn, Al, Cr, Ca and other metal foreign ions in the plating solution in the exchange columns are absorbed by the resin; and the plating solution performed with the absorption of foreign ions flows out from the exchange columns and directly enters a plating bath for recycling. In the invention, the ion exchange columns, a valve, the acid proof pump and the plating bath form a plating solution recycling system. The technology neither needs to stop production, nor wastes metallic nickel, can be operated easily, greatly reduce manufacture cost, and remove various foreign ions which do not accord with the plating requirement once until the plating solution accords with the plating requirement.

Description

A kind of technique for purifying nickel-plating liquid by extracting sprinkling method
Technical field
The present invention relates to the purifying nickel-plating liquid production technique, particularly a kind of technique for purifying nickel-plating liquid by extracting sprinkling method is the innovation to traditional purifying nickel-plating electroplate liquid technology, belongs to the electroplating industry technical field.
Background technology
At present, during Electroplate Factory both domestic and external nickel plating, be main plating bath all generally with single nickel salt type or amino acid nickel type, chloride type, less uses such as Citrate trianion, fluoroborate.But the sort of plating bath no matter, technological specification all requires acidity control between pH value 3.5~5.5, the nickeliferous 50-60g/L of solution, metallic cations such as copper, iron, zinc, aluminium, chromium, calcium all require in several PPm scopes, negatively charged ion such as nitrate radical and chlorine root, certain requirement is arranged, could ordinary production when plating bath is electroplated.But in the production process (electro-coppering and copper alloy part, ironware, zinc alloy piece, the calcium ions and magnesium ions in the wash water), all must bring a large amount of each metal ion species identical into and enter electroplate liquid with workpiece.Along with the increase of the amount of bringing into, when total impurities ion or single metal ion behind finite concentration, must influence electroplating quality, can't plate out qualified product when serious.Current electroplating technology all must refilter by the stopping production oxidation precipitation, then carries out electrolysis treatment.So all Electroplate Factories all must carry out purifying treatment to plating bath every more than three days, just can keep and continue to produce.
Existing Electroplate Factory handles the purification and impurity removal matter of nickel plating, adopts the method for oxidation, complex-precipitation basically, removes impurity.In treatment progress, to add soda acid and adjust acidity, add hydrogen peroxide, chemical agents such as complexing agent, but increased again and deleterious other impurity of plating bath.Behind the contamination precipitation, with filter plating bath is filtered again.Because precipitation can't effectively be removed the various impurity in the plating bath, so plating is crossed also and must be proceeded electrolytic cleaning with electrolytic method.But, in electrolysis removal of impurities process, must there be a large amount of nickel ions to fold with impurity because the plating bath major ingredient is a nickel, form useless nickel, owing to the control difference of each tame Electroplate Factory, generally to waste 5~10% of power down nickel consumption, really the heavy burden of Electroplate Factory's production.
Summary of the invention
In order to solve a difficult problem that perplexs electroplating industry always, the invention provides a kind of technique for purifying nickel-plating liquid by extracting sprinkling method, it utilizes a kind of brand new concept, promptly both without stop work and production, do not waste metallic nickel again, and simple to operate, cost is again low, and a performance is negatively charged ion such as metallic cations such as the copper in the plating bath, iron, zinc, aluminium, chromium, calcium and nitrate radical chlorine roots, all except that to meeting the plating requirement.
The technical solution used in the present invention:
A kind of technique for purifying nickel-plating liquid by extracting sprinkling method is characterized in that adopting organophosphorus extraction agent P507 in technology.
A kind of technique for purifying nickel-plating liquid by extracting sprinkling method comprises following technological process:
1, liquid P507 (2-ethyl hexamethyl phosphoric acid, single (ethyl hexyl) ester) is made as charcoal and carries P507 resin or synthetic CL-P507 extration resin;
2, load with ion exchange column, charcoal is housed in ion exchange column carries P507 or CL-P507 resin;
3, with acid proof pump with the electroplate liquid extracting, make plating bath successively by above-mentioned exchange column, metallic impurity ions such as the copper in the exchange column plating bath, iron, zinc, aluminium, chromium, calcium are by resin absorption, and the plating bath that was adsorbed foreign ion flows out from exchange column and directly enters plating tank and recycle;
4, when the resin absorption impurity in the exchange column reaches capacity, resin is carried out desorb with hydrochloric acid;
5, if nitrate radical or chlorine ion concentration exceed and electroplate when requiring in the plating bath, can behind above-mentioned exchange column, add again and the basic anion resin is housed, remove and hinder galvanized ionic impurity as 717 resins or CL-TPB resin column.
Described bath temperature is 15~60 ℃, and plating bath acidity pH value is 3.5~4; Best pH value is 3.8.
Be connected in series between the exchange column, exchange column and valve, acid proof pump, plating tank partly connect the formation electroplate liquid and recycle system.The quantity of exchange column, the total loading capacity of resin and liquid flow rate, look the plating bath treatment capacity what and adjust.
Described organophosphorus extraction agent still has CYamex272 and P229, and both are isomers.
Below technological principle of the present invention is described further.
This technology is to utilize organophosphorus extraction agent P507 or CYamex272 solvent under the condition of acid PH<4, and not with the nickel complexing, but the characteristic of metal ions such as complex copper, iron, zinc, aluminium, chromium, calcium is preferably removed the various metallic impurity positively charged ions in the plating bath.But, be a kind of extraction agent of non-ferrous metal because above-mentioned two kinds of medicines are solution all.So this technology must be flooded wherein a kind of in above-mentioned two kinds with the said products synthetic resin (CL-P507 extration resin) or with gac, loads with ion exchange column and uses.
The present invention utilizes basic anion resin or CL-TBP resin, nitrate ion and chlorion there be the characteristic of preferentially adsorbed in sulfate ion, remove nitrate radical in the plating bath and unnecessary chlorion, also available gac dipping TBP dress post uses (TBP is tributyl phosphate) in the process.
P507, TBP, CYamex272 equal solvent, the ready-made extration resin of both available its synthetic, also available other macroporous resin or gac flood the exchange column (or tower) of packing into, with sulfuric acid plating bath acidity are transferred to PH3.5~4 then, and temperature is in 15~60 ℃ of degree scopes.Utilize the characteristic of above-mentioned extraction agent, promptly in PH<4 o'clock not with the nickel complexing, but in PH3~4 o'clock, metallic impurity ions such as complex copper, iron, zinc, aluminium, chromium, calcium are adsorbed by resin effectively, flow out solution and can directly arrive plating tank.Electroplate impurities removing efficiency and reach more than 90%, multiple metallic impurity ion can be lower than 1 PPm.When the saturated back of resin absorption impurity or flow out plating bath and do not meet and electroplate when requiring, stop to purify, with hydrochloric acid resin is carried out desorb.After regeneration, can continue the life-time service that circulates.If nitrate radical or chlorion exceed and electroplate when requiring in the plating bath, can be on above-mentioned exchange column basis add again and the basic anion resin is housed as 717 or the exchange column of CL-TBP resin, just can hinder electroplated metal positively charged ions and nitrate anion impurity remove simultaneously all once.The quantity of whole exchange column, the total loading capacity of resin, plating bath flow, the root a tree name need be handled plating bath amount, impurity and turnout can do flexible adjustment.
Beneficial effect of the present invention
Technology of the present invention is not wasted the metallic nickel processing ease again both without stop work and production, reduce production costs greatly, and disposable various metallic cations and the negatively charged ion of electroplating requirement of will not meeting of energy removes to meeting the plating requirement.
Description of drawings
Fig. 1 uses synoptic diagram for electroplate liquid of the present invention sorption cycle in exchange column.
Embodiment
As shown in Figure 1, ion exchange column comprises 4,5 and 6 three exchange columns of ion exchange column, all injects charcoal and carry P507 resin or CL-P507 extration resin in three exchange columns.Exchange column 4,5,6 is connected, and recycles system with acid proof pump 2, valve 3 and plating tank 1 formation electroplate liquid.Electroplate liquid is under the extracting of durable sour pump 2 in the plating tank 1, and plating bath enters exchange column 4,5,6 successively by valve 3 controls.Electroplate liquid enters plating tank again and recycles removed undesirable ionic impurity by the organophosphorus extration resin in exchange column after.This plating bath treatment process is neither stopped work and is not stopped production, and does not waste metallic nickel again, and processing ease reduces production costs significantly.

Claims (6)

1. a technique for purifying nickel-plating liquid by extracting sprinkling method is characterized in that adopting organophosphorus extraction agent P507 in technology.
2. a kind of technique for purifying nickel-plating liquid by extracting sprinkling method according to claim 1 is characterized in that comprising following technological process:
1), liquid P507 is made into charcoal and carries P507 resin or CL-P507 extration resin;
2), load, charcoal is housed in ion exchange column carries P507 resin or CL-P507 extration resin with ion exchange column;
3), with acid proof pump electroplate liquid is carried and being taken out, make electroplate liquid successively by above-mentioned exchange column, copper in the exchange column plating bath, iron, zinc, aluminium, chromium, calcium metallic impurity ion be by resin absorption, and the electroplate liquid that was adsorbed foreign ion flows out from exchange column and directly enters plating tank and recycle;
4), when the resin absorption impurity in the exchange column reaches capacity, with hydrochloric acid resin is carried out desorb;
5), if nitrate radical or chlorine ion concentration exceed and electroplate when requiring in the plating bath, on above-mentioned exchange column basis, be added into again and the basic anion resin be housed as 717 resins or CL-TPB resin column, remove and hinder galvanized ionic impurity.
3. technique for purifying nickel-plating liquid by extracting sprinkling method according to claim 1 and 2, the temperature that it is characterized in that described plating bath is 15~60 ℃, plating bath acidity pH value is 3.5~4.
4. according to claim 2 or 3 described a kind of technique for purifying nickel-plating liquid by extracting sprinkling method, it is characterized in that the best pH value of described plating bath acidity is 3.8.
5. a kind of technique for purifying nickel-plating liquid by extracting sprinkling method according to claim 1 is characterized in that described organophosphorus extraction agent can replace with CYamex272 or P229.
6. a kind of technique for purifying nickel-plating liquid by extracting sprinkling method according to claim 2 is characterized in that each ion exchange column serial connection, and ion exchange column is connected in series the formation electroplate liquid and recycles system with valve, acid proof pump, plating tank.
CNA2007100270782A 2007-03-08 2007-03-08 Technique for purifying nickel-plating liquid by extracting sprinkling method Pending CN101260559A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101817607A (en) * 2010-03-24 2010-09-01 埃梯星(厦门)电子科技有限公司 Method for directly extracting nickel in acidic chemical nickel plating waste solution
CN108251886A (en) * 2016-12-28 2018-07-06 南京源泉环保科技股份有限公司 A kind of online reuse method of nickel plating with impurity removal function
CN109985420A (en) * 2019-03-11 2019-07-09 西安蓝晓科技新材料股份有限公司 A kind of preparation method for nickel sulfate solution cleansed resin
CN113800494A (en) * 2021-09-14 2021-12-17 广东中金岭南环保工程有限公司 Method for selectively recovering aluminum from acid leaching solution of waste lithium iron phosphate battery material

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101817607A (en) * 2010-03-24 2010-09-01 埃梯星(厦门)电子科技有限公司 Method for directly extracting nickel in acidic chemical nickel plating waste solution
CN101817607B (en) * 2010-03-24 2011-08-10 埃梯星(厦门)电子科技有限公司 Method for directly extracting nickel in acidic chemical nickel plating waste solution
CN108251886A (en) * 2016-12-28 2018-07-06 南京源泉环保科技股份有限公司 A kind of online reuse method of nickel plating with impurity removal function
CN109985420A (en) * 2019-03-11 2019-07-09 西安蓝晓科技新材料股份有限公司 A kind of preparation method for nickel sulfate solution cleansed resin
CN113800494A (en) * 2021-09-14 2021-12-17 广东中金岭南环保工程有限公司 Method for selectively recovering aluminum from acid leaching solution of waste lithium iron phosphate battery material
CN113800494B (en) * 2021-09-14 2023-11-17 广东中金岭南环保工程有限公司 Method for selectively recycling aluminum from acid leaching solution of waste lithium iron phosphate battery material

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Open date: 20080910