CN106191867B - A kind of route board acidic etching waste liquor resource reusing method - Google Patents
A kind of route board acidic etching waste liquor resource reusing method Download PDFInfo
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- CN106191867B CN106191867B CN201610721596.3A CN201610721596A CN106191867B CN 106191867 B CN106191867 B CN 106191867B CN 201610721596 A CN201610721596 A CN 201610721596A CN 106191867 B CN106191867 B CN 106191867B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/46—Regeneration of etching compositions
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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
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
- C22B15/0091—Treating solutions by chemical methods by cementation
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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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- 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 etching waste liquor recovery technology fields in wiring board manufacture, more particularly to a kind of route board acidic etching waste liquor resource reusing method: using the acidic etching waste liquid of containing copper chloride as raw material, remove copper ion by copper-removing method (copper-removing method can be the precipitation method, electrolysis method, resin adsorption method), mother liquor after removing copper, the aqueous solution that chloracid sodium and sodium chloride are prepared by electrolysis method, is back to etch system.It is characterized in that the copper and sodium chloride resource fully recovering of etching waste liquor, zero-emission is environmental-friendly, good in economic efficiency；Etch system no longer additionally adds the sub- liquid of etching or oxidant completely, realizes the online repeats itself of etch system, substantially reduces the cost of etching.While the Crystallization Procedure that feed purification and product in traditional handicraft are saved in sodium chlorate technique is prepared in electrolysis waste solution, energy efficiency is high, and cost is lower.
Description
Technical field
The present invention relates to etching waste liquor recovery technology fields in wiring board manufacture, lose more particularly to a kind of wiring board acidity
Carve waste liquid resource reusing method.
Background technique
World technology is fast-developing, promotes the rise of circuit board etching industry, and acidic etchant is major class etching body
System, is discharged a large amount of cupric mother liquors after etching, this is valuable resource, insider given height note that proposing perhaps
The methods of more effective recycling copper, such as CN103290415A, CN200610032589.9, CN 105016373.A,
CN201620528081.7 etc., but its main focus is all placed in the recycling of copper, and others in etching waste liquor it is useful at
Part, it is had not been reported if the online reuse of the resources such as sodium chloride.It is well known that sodium chloride be industrially by seawater, salt lake saline,
Subsurface brine, rock salt extract, and are important industrial products.The present invention then utilizes sodium chloride-containing mother liquor after various method copper removals,
It is converted into sodium chlorate by electrolysis method, is back to etching work procedure, no longer needs to add sub- liquid or oxidant, saves cost, realize
Producing line recycles online.Sodium chlorate industrially produces more than hundred years existing, current 3,000,000 tons of annual output in the whole world or more, China's annual output
Amount is still establishing 100,000 tons/year at 200,000 tons or so, since sodium chlorate increases day by day in the demand that industry was bleached and sterilized to paper industry, supply and demand
It is relatively tight.The acidic etching liquid chloracid sodium of wiring board industry need to be by market purchasing.Global production of sodium chlorate method is in the majority to be used with chlorine
Change sodium is raw material electrolytic method, and the present invention saves feed purification (such as removing calcium and magnesium sulfate radical) process and chlorine in traditional sodium chlorate industry
Sour sodium Crystallization Procedure.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, and provide a kind of route board acidic etching waste liquor resource time
With method, the various sodium chloride-containing mother liquors of output during copper are recycled for route board acidic etching waste liquor, which compares
It is pure, it need to only remove trace copper, so that it may produce qualified sodium chlorate solution with electrolysis method, then be back to erosion after removing chromium with precipitation method etc.
Etching system.
To achieve the above object, the present invention adopts the following technical scheme that.
A kind of route board acidic etching waste liquor resource reusing method recycles whole copper resources by the sodium carbonate precipitation method,
Copper rate of deposition reaches 99.9%, and cupric sediment is used to prepare copper fine work, and the mother liquor sodium chloride-containing after cement copper removes trace copper,
Then the aqueous solution of chloracid sodium and sodium chloride is prepared with electrolysis method, it is not necessary to solid product be made, be back to etching system again
System, makes the copper and sodium chloride resource fully recovering of etching waste liquor.Mother liquor income approach further includes oxalic acid heavy the copper precipitation method, carbonic acid alkali
Heavy the copper precipitation method, hydroxide neutralization precipitation method equally further include extraction copper extraction process, resin adsorption copper extraction process, electrolysis copper extraction process
Deng.
Preferably, the cupric sediment is used to prepare product, produces particularly for preparation chlorination copper products, copper sulphate
Product, basic carbonate copper products or oxidation copper products, but it is not limited to the above product.
Preferably, recycling the waste liquid that generates after copper can be all electrolysed by electrolysis method as the molten of sodium chloride-containing and sodium chlorate
Liquid, wherein sodium chloride in aqueous solution, sodium chlorate concentration chlorination back can be electrolysed by electrolytic process state modulator completely
Sodium and sodium chlorate aqueous solution can be back to etch system after except chromium completely, be not required to any additional processing.
Preferably, filtrate removes trace copper after the copper removal, and the precipitation method can be used or qualification is made in chelating resin exchange process
Liquid before being electrolysed, wherein copper content can be down to 5PPM or less.
Preferably, after the aqueous solution that chloracid sodium and sodium chloride are prepared with electrolysis method, using the precipitation method except chromium or
Resin method removes chromium, chromium can be down to 5ppm or less.
Preferably, it includes frerrous chloride, sodium sulfite, nitrous acid that the electrolytic liquid, which removes the chromium precipitating reagent that removes that chromium uses,
Sodium, lead chloride, barium chloride.The chromate of recycling can be used as pigment, no waste sludge discharge.
Preferably, the aqueous solution that chloracid sodium and sodium chloride are prepared with electrolysis method specifically: remove trace copper stepmother
The sodium dichromate of 0-10g/L is added in liquid, in 40-100 degree Celsius, makees anode with titanium plating ruthenium electrode, in 500 A/ of current strength
It is electrolysed under 4000 A/m2 of m2-, and controls PH in reactor and obtain it in 6.3-6.8 and be electrolysed post mother liquor density of sodium chlorate in 0-
600g/L。
The invention has the following beneficial effects: a kind of route board acidic etching waste liquor resource reusing method of the present invention, for line
The sodium chloride-containing mother liquor of output during road board acidic etching waste liquor recycling copper, the mother liquor is purer, can be without purification just
Qualified sodium chlorate solution can be produced with electrolysis method be back to etch system.
Detailed description of the invention
Attached drawing 1 is simple process process of the invention.
Attached drawing 2 is detailed process flow of the invention.
Specific embodiment
The present invention is further illustrated with embodiment with reference to the accompanying drawing.
A kind of route board acidic etching waste liquor resource reusing method of the present invention, simple process process such as Fig. 1, acid etching
Waste liquid carries out copper removal, and then copper recycling and generation mother liquor, are electrolysed mother liquor, form reuse etching solution, reuse etching solution is again
It is secondary to be used as acid etching waste liquid.Detailed process flow such as Fig. 2, acid etching waste liquid carry out copper removal, form sodium carbonate and sink copper, and sodium carbonate sinks copper
Crude product copper carbonate and filtrate are formed, then filtrate refines, and filtrate electrolysis, electrolytic liquid removes chromium, then forms etching reuse liquid, leads to
Peracidity etching line again acts as acid etching waste liquid.
Required sodium carbonate liquor is placed in reactor, under room temperature and stirring condition, acid etching is added by head tank
Waste liquid, control reaction end of a period acidity, stirs 45 minutes, is then separated by filtration sediment (crude product copper carbonate), copper rate of deposition reaches
99.9%, crude product copper carbonate can be used for preparing copper essence product；Mother liquor sodium chloride-containing after cement copper, refines mother liquor, then
The aqueous solution of chloracid sodium and sodium chloride is prepared with electrolysis method, except after chromium, it is not necessary to solid product be made, be back to etching again
System makes the copper and sodium chloride resource fully recovering of etching waste liquor.
Wherein, the mother liquor subtractive process are as follows:
Mother liquor refines embodiment one, passes through mother liquid obtained, copper after acid etching waste liquid copper-coating: 24ppm;Sodium chloride:
300g/L；PH:7.5.Its liquid hydrochloric acid is adjusted into PH to 2.0 or so, is stirred evenly, then adjust PH to 6.5 with sodium hydroxide
Left and right, stirring are filtered after standing, filtrate after must refining: sodium chloride solution 298g/L;Copper 1.3PPM, PH:6.5.Electrolysis is made
Preceding liquid.
Mother liquor refines embodiment two: passing through mother liquid obtained, copper after acid etching liquid waste processing copper-coating: 30ppm;Chlorination
Sodium: 280g/L； PH:7.5.It is handed over into resin by complex ion, obtains refinement mother liquor: sodium chloride: 270 g/L；PH:7.1；
Copper: 0.3ppm, then 6.5 or so are adjusted to sodium hydroxide, liquid before being electrolysed is made.
Wherein, the electrolysis sodium chlorate process are as follows:
Electrolysis sodium chlorate embodiment one: taking purification post mother liquor 5L, the sodium dichromate of 3g/L be added, and is warming up to 85 degree of left sides
The right side is made anode with titanium plating ruthenium electrode, is electrolysed at current strength 500 A/m2-3000 A/m2, and control PH in reactor and exist
6.3-6.8 obtains its electrolytic liquid chloracid sodium 250g/L.
Electrolysis sodium chlorate embodiment two: taking purification post mother liquor 5L, the sodium dichromate of 5g/L be added, and is warming up to 85 degree of left sides
The right side is made anode with titanium plating ruthenium electrode, is electrolysed at current strength 500 A/m2-3000 A/m2, and control PH in reactor and exist
6.3-6.8 obtains its electrolytic liquid chloracid sodium 190g/L.
Wherein, the electrolytic liquid removes chromium process are as follows:
Electrolytic liquid removes chromium embodiment one: taking electrolytic liquid 3L, sodium chlorate 220g/L;Sodium dichromate 3g/L.It is added
The barium chloride of 8g/L, then PH7-8 is adjusted, 30min is stirred, filtering obtains its filtrate: sodium chlorate 218g/L;Chromium: 3.2ppm.
Electrolytic liquid removes chromium embodiment two: taking electrolytic liquid 3L, sodium chlorate 240g/L;Sodium dichromate 3g/L.It is added
The lead chloride of 8.4g/L, then PH7-8 is adjusted, 30min is stirred, filtering obtains its filtrate: sodium chlorate 237g/L;Chromium: 2.9ppm.
Electrolytic liquid removes chromium embodiment three: taking electrolytic liquid 3L, sodium chlorate 240g/L;Sodium dichromate 3g/L.Except chromium
Resin adsorption obtains liquid after its exchange: sodium chlorate 115g/L;Chromium: 1.2ppm.
In conclusion a kind of route board acidic etching waste liquor resource reusing method of the present invention, is related to containing copper chloride
Acidic etching waste liquid be raw material, by the whole copper resource of sodium carbonate precipitation method recycling, copper rate of deposition reaches 99.9%, cupric
Sediment can be used for preparing the products such as copper chloride.Mother liquor sodium chloride-containing 200-320g/L after cement copper, is prepared with electrolysis method
The aqueous solution of chloracid sodium and sodium chloride, it is not necessary to solid product be made, be back to etch system.It is characterized in that etching waste liquor
Copper and sodium chloride resource fully recovering, zero-emission is environmental-friendly, good in economic efficiency.Tradition is saved in preparing sodium chlorate technique
The Crystallization Procedure of feed purification and product in technique, energy efficiency is high, and cost is lower.It does not need in whole system as existing
Etch system will also persistently add the sub- liquid of etching, and the copper and sodium chloride resource whole circulating repetition of etching waste liquor use, this is
Completely new process, zero-emission is environmental-friendly, good in economic efficiency.
The above description is only a preferred embodiment of the present invention, thus it is all according to the configuration described in the scope of the patent application of the present invention,
The equivalent change or modification that feature and principle are done, is included in the scope of the patent application of the present invention.
Claims (9)
1. a kind of route board acidic etching waste liquor resource reusing method, it is characterised in that: recycle copper ion by copper-removing method, remove
Mother liquor after copper, main component are sodium chloride solution, and the aqueous solution of chloracid sodium and sodium chloride, reuse are prepared by electrolysis method
In etch system, make the copper and sodium chloride resource fully recovering of etching waste liquor, realizes the online repeats itself of etch system；
Wherein, the mother liquor subtractive process are as follows:
Mother liquor refines embodiment one, passes through mother liquid obtained, copper after acid etching waste liquid copper-coating: 24ppm;Sodium chloride: 300g/
L；pH:7.5；It by its liquid salt acid for adjusting pH to 2.0 or so, stirs evenly, then adjusts pH to 6.5 or so with sodium hydroxide,
Stirring is filtered after standing, filtrate after must refining: sodium chloride solution 298g/L;Copper 1.3ppm, pH: 6.5；Before electrolysis is made
Liquid；
Wherein, the electrolysis sodium chlorate process are as follows:
Electrolysis sodium chlorate embodiment one: purification post mother liquor 5L is taken, the sodium dichromate of 3g/L is added, is warming up to 85 degrees Celsius of left sides
Anode is made with titanium plating ruthenium electrode, in 500 A/m of current strength in the right side2—3000 A/m2Lower electrolysis, and control pH in reactor and exist
6.3-6.8 obtains its electrolytic liquid chloracid sodium 250g/L；
Wherein, the electrolytic liquid removes chromium process are as follows:
Electrolytic liquid removes chromium embodiment one: taking electrolytic liquid 3L, sodium chlorate 220g/L;Sodium dichromate 3g/L；8g/L is added
Barium chloride, then adjust pH7-8, stir 30min, filtering obtains its filtrate: sodium chlorate 218g/L;Chromium: 3.2ppm.
2. a kind of route board acidic etching waste liquor resource reusing method according to claim 1, it is characterised in that: etching system
System no longer additionally adds the sub- liquid of etching or oxidant completely, realizes the online repeats itself of etch system, substantially reduce etching at
This.
3. a kind of route board acidic etching waste liquor resource reusing method according to claim 1, it is characterised in that: after copper removal
Resulting mother liquor is not limited only to the resulting purer mother liquor of carbonate precipitation method, further includes sinking the copper precipitation method, carbonic acid alkali by oxalic acid
Heavy the copper precipitation method, hydroxide neutralization precipitation method equally further include extraction copper extraction process, resin adsorption copper extraction process, electrolysis copper extraction process
Resulting purer mother liquor.
4. a kind of route board acidic etching waste liquor resource reusing method according to claim 1, it is characterised in that: described heavy
Cupric sediment obtained by the method for shallow lake is used to prepare copper fine work product, particularly for preparation chlorination copper products, sulfuric acid copper products, alkali formula
Carbonic acid copper products or oxidation copper products.
5. a kind of route board acidic etching waste liquor resource reusing method according to claim 1, it is characterised in that: recycling copper
The waste liquid generated afterwards can all be the solution of sodium chloride-containing and sodium chlorate, wherein chlorination in aqueous solution by electrolysis method electrolysis
Sodium, sodium chlorate concentration can be electrolysed sodium chloride back by electrolytic process state modulator completely and sodium chlorate aqueous solution is complete
It can be back to etch system entirely, realize the online repeats itself of etch system.
6. a kind of route board acidic etching waste liquor resource reusing method according to claim 1, it is characterised in that: after removing copper
Mother liquor, can continue that qualified liquid before being electrolysed is made using sour adjusting PH with base precipitating filtration method or chelating resin exchange process, wherein copper contains
Amount is down to 2ppm or less.
7. a kind of route board acidic etching waste liquor resource reusing method according to claim 1, it is characterised in that: the use
It after electrolysis method prepares the aqueous solution of chloracid sodium and sodium chloride, carries out electrolytic liquid and removes chromium, remove chromium or resin using the precipitation method
Method is removed, and chromium can be down to 5ppm or less.
8. a kind of route board acidic etching waste liquor resource reusing method according to claim 7, it is characterised in that: the electricity
It includes frerrous chloride, sodium sulfite, sodium nitrite, lead chloride, barium chloride that liquid, which removes the precipitating reagent that chromium uses, after solution.
9. a kind of route board acidic etching waste liquor resource reusing method according to claim 1, it is characterised in that: the use
Electrolysis method prepares the aqueous solution of chloracid sodium and sodium chloride specifically: the dichromic acid of 0-10g/L is added in electrolyte after purification
Sodium, temperature is in 40-100 degree Celsius, in current strength 0-4000 A/m2Lower electrolysis obtains its electrolytic liquid density of sodium chlorate 0-
600g/L。
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| CN107354461A (en) * | 2017-09-13 | 2017-11-17 | 田成 | A kind of printed circuit board acidic etching waste liquor process for regenerating, recovering and reutilizing |
| CN108793546B (en) * | 2018-05-24 | 2021-11-19 | 山东中天国际工程有限公司 | Method for recovering sodium chloride from sodium chlorate wastewater |
| CN115466957A (en) * | 2021-08-19 | 2022-12-13 | 叶涛 | Electrolytic regeneration method and device for precipitating and taking copper from acidic copper chloride etching waste liquid |
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| CN100510188C (en) * | 2003-03-28 | 2009-07-08 | 巫协森 | Method of recovering copper metal from waste printed circuit board and copper containing waste liquid and device thereof |
| CN101748430B (en) * | 2009-09-23 | 2014-10-29 | 王红华 | Copper recovery system of printed board acid etching waste solution and etching solution regeneration method |
| CN102732888A (en) * | 2012-07-19 | 2012-10-17 | 湖南万容科技股份有限公司 | Method and system for regenerating and recycling acidic etching waste liquor |
| CN102912352A (en) * | 2012-11-08 | 2013-02-06 | 上海绿澄环保科技有限公司 | Method for recycling acidic copper-etching waste solution |
| CN103602988B (en) * | 2013-10-30 | 2016-06-01 | 中国科学院过程工程研究所 | The recycling treatment of a kind of PCB etching waste liquor and recycle method |
| CN104611703A (en) * | 2014-12-26 | 2015-05-13 | 锦州清源嘉华环保科技有限公司 | Device and method for regenerating PCB etching waste liquid and recycling heavy metal |
| CN105314668B (en) * | 2015-11-23 | 2018-01-16 | 东莞市广华化工有限公司 | A kind of method from circuit board acidic etching waste liquor recovery basic copper carbonate |
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