CN102354571B - Nano-copper conductive slurry preparation method by utilizing printed circuit board alkaline etching waste liquid - Google Patents
Nano-copper conductive slurry preparation method by utilizing printed circuit board alkaline etching waste liquid Download PDFInfo
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- CN102354571B CN102354571B CN2011101310478A CN201110131047A CN102354571B CN 102354571 B CN102354571 B CN 102354571B CN 2011101310478 A CN2011101310478 A CN 2011101310478A CN 201110131047 A CN201110131047 A CN 201110131047A CN 102354571 B CN102354571 B CN 102354571B
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Abstract
The invention relates to a method for utilizing alkaline etching waste liquid in a printed circuit board to prepare nano-copper which is made into nano-copper conductive slurry. The method comprises the following steps: filtering alkaline etching waste liquid, adding a nonionic surfactant of 0.43%-4.24% of alkaline etching waste liquid by weight and an aqueous antifoaming agent of 0.08%-1.61% of the alkaline etching waste liquid by weight, preparing a reaction solution A; preparing a reducing agent solution B which comprises a reducing agent of 1.70%-8.49% of the alkaline etching waste liquidby weight, a highly basic substance of 6.80%-10.20 % of the alkaline etching waste liquid by weight, and organic phase turpentine which is used for a phase-transfer agent and has a volume ratio of 1:1-1:2 to the alkaline etching waste liquid; carrying out heating and stirring, and adding the reaction solution A in to the reducing agent solution B drop by drop. The method has the characteristics of easy operation and small energy consumption, prepared nano-copper powder has good antioxidation performance, by utilizing the etching waste liquid, conductive slurry of a high added value is prepared, a high economic benefit is created, emission reduction and no pollution of waste water are realized, and resource recycling is achieved.
Description
Technical field
the present invention relates to a kind of method of from alkaline etching waste liquid for producing printed circuit board, extracting utility, particularly produce nanometer copper and are made into the electrocondution slurry method of nanometer copper from printed circuit board neutral and alkali etching waste liquor.
Background technology
in PC board fabricating processes, alkali etching is a requisite operation.The copper ion concentration that constantly carries out in the etching solution along with etching can constantly rise, if when copper ion concentration reaches finite concentration, do not handle, will influence etched effect.Yet the factory of the overwhelming majority discharges later on through simple process, has also caused the serious environmental pollution thereby both wasted a large amount of precious resources.
The main component of
alkaline etching liquid is cupric ammine complex, ammonium chloride and ammoniacal liquor, and the mass concentration of copper can reach 120～180 g/L.Processing for copper in the alkaline etching liquid at present roughly can divide the three major types method: 1 ﹑ chemical method.Add NaOH, Na in the alcaliotropism etching waste liquor 2 CO 3 Deng alkaline matter, generate Cu (OH) 2 Deposition obtains Cu (OH) through filtering 2 Solid obtains CuO later on or adds H through heat then 2 SO 4 Solution obtains CuSO at last 4 2 ﹑ extract electro-deposition.Add the contact break agent in elder generation's alcaliotropism etching waste liquor and make copper from the complex compound of copper, dissociate out to become copper ion, inwards adds some extractants of copper again, has obtained the solution of copper ion through stripping, and utilizes the method for electro-deposition to obtain elemental copper then; The direct electro-deposition of 3 ﹑.Representational is German Elochen alkaline etching liquid recovery system.This method requires the CuCl in the etching solution 2 Become CuSO 4 After production process produces etching waste liquor.Owing to do not had Cl in the waste liquid - , can be out of use extraction and directly electro-deposition obtain Cu simple substance.The part yet these methods come with some shortcomings: 1. bigger and resulting CuO or CuSO of the consumption of chemical precipitation method alkali 4 Added value is not high, and economic benefit is low.2. extract electrodeposition process technology more complicated, consuming electric power is bigger, and the later waste liquid of electro-deposition does not reach emission standards yet.3. directly the electrodeposition process energy consuming ratio is bigger, and the rate of recovery is not high, complex procedures.
Palladium, platinum, gold, silver have good electric conductivity and antioxygenic property in
existing electrocondution slurry, on certain degree, have the status that can not be substituted.Right over nearly 20 years, nearly 10 times of various noble metal spurts in prices make various noble metal electric slurry manufacturing costs sharply increase, and make the electronic product profit continue to drop.90 mid-nineties 90s were guide with Taiwan, Japanese enterprises, had begun the once thoroughly innovation of electric slurry industry, replaced some noble metals, the i.e. lowpriced metallization of pulp preparation with some base metals.
Summary of the invention
the present invention is that the deficiency according to prior art proposes a kind of cleaning, low energy consumption prepare nanometer copper electrocondution slurry from alkaline etching waste liquid for producing printed circuit board method.
the objective of the invention is to realize through following step.
A kind of PCB of utilization alkaline etching waste liquid for producing is produced the method for nanometer copper electrocondution slurry, and alkaline etching waste liquid for producing is filtered to remove suspended matter and precipitated impurities; After filtering filtrating is transferred in the container, added nonionic surface active agent that accounts for alkaline etching waste liquid for producing weight 0.43%-4.24% and the water-based antifoaming agent that accounts for alkaline etching waste liquid for producing weight 0.08%-1.61%, as reaction solution A;
Preparation reductant solution B; The reducing agent that accounts for alkaline etching waste liquid for producing weight 1.70%-8.49%, the strong alkaline substance that accounts for alkaline etching waste liquid for producing weight 6.80%-10.20% and organic facies turpentine oil have been comprised in the B solution; Contain consisting of phase-transferring agent in the organic facies turpentine oil; The volume ratio of consisting of phase-transferring agent and alkaline etching waste liquid for producing is 1:1-1:2, and solution B is heated to 30 ℃～100 ℃, stirs with 100 rev/mins～1000 rev/mins speed simultaneously; Again solution A is dropped in the solution B;
The back cooling is accomplished in reaction, and ageing is then transferred to and carried out water in the separatory funnel and separate with organic facies, the removal water, and collection contains the organic facies of copper powder;
The organic oil reservoir that contains copper nanoparticle that
obtain adds the dispersant of one of sizing agent earlier; Put into ultrasonic agitation device ultrasonic agitation 30 minutes-60 minutes; Ultrasonic agitation finishes the back and adds organic polymer and remaining sizing agent; Constantly high-speed stirred obtains the nano copper slurry material at last.Concrete technological parameter: organic polymer is 10%-40%, and copper powder is 50%-80%, and various auxiliary agents are 2.1%-11%, and surplus is an isopropyl alcohol, and mixing speed is more than 200 rev/mins.
said method also can be done following further perfect.
said nonionic Surfactant is tween or polyvinyl pyrrolidone or gelatin or the combination in them.
said water-based antifoaming agent is German Bi Ke BYK-023 or German Bi Ke BYK-051.
said reducing agent is hydrazine hydrate or vitamin C or sodium borohydride or inferior sodium phosphate or glucose.
said turpentine oil is gum turpentine or steam-distilled turpentine or sulfate turpentine.
said organic high molecular compound is epoxy resin or polyurethanes or aqueous phenolic aldehyde resin.
said sizing agent comprises coupling agent, curing agent, dispersant, and three's weight ratio scope is between 1:5:5-1:10:10.Said coupling agent is gamma-aminopropyl-triethoxy-silane or γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane coupling agent or titanate esters.Said curing agent is alcamines curing agent or polyamine curing agent or their combination, and said alcamines curing agent is diethanol amine or triethanolamine, and said polyamine curing agent is triethylamine or trien.Said dispersant is oleic acid or polyethylene glycol or Tissuemat E or their combination.
innovation of the present invention and advantage have: 1. the thinking of phase transfer is taked in this experiment; When being reduced, the copper ion in the alkaline etching waste liquid for producing directly transfers in the organic facies oil reservoir when agent reduction generates copper simple substance; And the solvent that the organic substance turpentine oil in the organic facies can be used as in the slurry uses, thus water with obtain directly slurryization of organic facies after organic facies is separated.2. process conditions are not harsh, operation easily, no big power consumption.3. the copper nanoparticle antioxygenic property of producing out is good, and size dimension is in 100 nanometers.4. utilize etching waste liquor to prepare the very high electrocondution slurry of added value, createed higher economic benefit, realized the purpose that turns waste into wealth.5. meet the requirement of " Green Chemistry " in the whole process of preparation, reality waste water discharge-reducing, pollution-free, reached resources circulation and utilized again.
Embodiment
Instance 1
The alkaline etching waste liquid for producing of No. 1 production line of Foshan City PCB manufactory is got in
.Therefrom get 50 milliliters of (about 58.88 grams) alkaline etching waste liquid for producing and carry out three-stage filtration, collect and filter later filtrating, add 0.50 gram tween simultaneously, 0.500 gram polyvinyl pyrrolidone and 0.50 gram water-based antifoaming agent Germany Bi Ke BYK-023 are as A solution.Preparation contains 4.00 gram hydrazine hydrates, the NaOH of 6 grams, and 50 milliliters terebinthine reduction solvent B.B solution is poured in the there-necked flask, regulated the water bath with thermostatic control temperature at 80 ℃, open and stir, mixing speed is about 200 rev/mins.In there-necked flask, drip A solution, take out cooling, ageing after having reacted.Then reacted solution is transferred in the separatory funnel; Remove wherein water; Collect organic oil reservoir, add dispersant to organic facies earlier and carried out ultrasonic agitation 30 minutes, ultrasonic agitation finishes the back and adds organic polymer and remaining sizing agent; Constantly high-speed stirred obtains the nano copper slurry material at last.Nano copper slurry material component is following: the amount with the nano copper slurry material is a reference, and its quality is 100; Organic polymer (polyurethanes) 10, curing agent (triethanolamine and trien) 1, coupling agent (gamma-aminopropyl-triethoxy-silane) 0.1, dispersant (polyethylene glycol) 1, copper nanoparticle 80, surplus is an isopropyl alcohol.
Instance 2
The alkaline etching waste liquid for producing of No. 2 production lines of Foshan City PCB manufactory is got in
; Therefrom get 50ml (about 58.88 grams) alkali etching waste water and carry out three-stage filtration; Collect and filter later filtrating, the polyvinyl pyrrolidone and 0.50 that adds 1.0 grams simultaneously restrains antifoaming agent Germany Bi Ke BYK-023 as A solution.Preparation contains 4.00 gram sodium borohydrides, the potassium hydroxide of 6 grams, and the reduction solvent B of the steam-distilled turpentine of 50ml.B solution is poured in the there-necked flask, regulated the water bath with thermostatic control temperature at 85 ℃, open and stir, mixing speed is about 200 rev/mins.In there-necked flask, drip A solution, take out cooling, ageing after having reacted.Then reacted solution is transferred in the separatory funnel; Remove wherein water; Collect organic oil reservoir, add dispersant to organic facies earlier and carried out ultrasonic agitation 30 minutes, ultrasonic agitation finishes the back and adds organic polymer and remaining sizing agent; Constantly high-speed stirred obtains the nano copper slurry material at last.Nano copper slurry material component is following: the amount with the nano copper slurry material is a reference, and its quality is 100; Organic polymer (polyurethanes) 35, curing agent (trien and triethanolamine) 5, coupling agent (γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane) 1, dispersant (polyethylene glycol) 5, copper nanoparticle 50, surplus is an isopropyl alcohol.
Instance 3
The alkaline etching waste liquid for producing of No. 2 production lines of Foshan City PCB manufactory is got in
; Therefrom get 100ml (about 117.77 grams) alkali etching waste water and carry out three-stage filtration; Collect and filter later filtrating, add 2.00 gram tweens and 1.00 gram water-based antifoaming agent Germany Bi Ke BYK-051 simultaneously as A solution.Preparation contains 8.00 gram hydrazine hydrates, the potassium hydroxide of 12 grams, and the reduction solvent B of the gum turpentine of 80ml.B solution is poured in the there-necked flask, regulated the water bath with thermostatic control temperature at 70 ℃, open and stir, mixing speed is about 200 rev/mins.In there-necked flask, drip A solution, take out cooling, ageing after having reacted.Then reacted solution is transferred in the separatory funnel; Remove wherein water; Collect organic oil reservoir, add dispersant to organic facies earlier and carried out ultrasonic agitation 45 minutes, ultrasonic agitation finishes the back and adds organic polymer and remaining sizing agent; Constantly high-speed stirred obtains the nano copper slurry material at last.
are reference with the amount of nano copper slurry material, and its quality is 100; Organic polymer (polyurethanes) 25, curing agent (triethanolamine) 2.5, coupling agent (gamma-aminopropyl-triethoxy-silane) 0.5, dispersant (oleic acid) 2.5, copper nanoparticle 65, surplus is an isopropyl alcohol.
Instance 4
The alkaline etching waste liquid for producing of No. 2 production lines of Foshan City PCB manufactory is got in
; Therefrom get 100ml (about 117.77 grams) alkali etching waste water and carry out three-stage filtration; Collection will be filtered later filtrating, add 2.00 gram polyvinyl pyrrolidones and 1.00 gram antifoaming agent Germany Bi Ke BYK-051 simultaneously as A solution.Preparation contains 10.00 gram sodium hypophosphites, the potassium hydroxide of 12 grams, and the reduction solvent B of the gum turpentine of 80ml.B solution is poured in the there-necked flask, regulated the water bath with thermostatic control temperature at 75 ℃, open and stir, mixing speed is about 200 rev/mins.In there-necked flask, drip A solution, take out cooling, ageing after having reacted.Then reacted solution is transferred in the separatory funnel; Remove wherein water; Collect organic oil reservoir, add dispersant to organic facies earlier and carried out ultrasonic agitation 45 minutes, ultrasonic agitation finishes the back and adds organic polymer and remaining sizing agent; Constantly high-speed stirred obtains the nano copper slurry material at last.
are reference with the amount of nano copper slurry material, and its quality is 100; Organic polymer (polyurethanes) 35, curing agent (trien and triethanolamine) 3, coupling agent (butyl titanate) 0.4, dispersant (oleic acid) 2, copper nanoparticle 56, surplus is an isopropyl alcohol.
Instance 5
The alkaline etching waste liquid for producing of No. 3 production lines of Foshan City PCB manufactory is got in
; Therefrom get 200ml (about 235.54 grams) alkali etching waste water and carry out three-stage filtration; Collection will be filtered later filtrating, add 4.00 gram tweens and 2.00 gram antifoaming agent Germany Bi Ke BYK-023 simultaneously as A solution.Preparation contains 15.00 gram vitamin Cs, the potassium hydroxide of 20 grams, and the reduction solvent B of the gum turpentine of 100ml.B solution is poured in the there-necked flask, regulated the water bath with thermostatic control temperature at 90 ℃, open and stir, mixing speed is about 200 rev/mins.In there-necked flask, drip A solution, take out cooling, ageing after having reacted.Then reacted solution is transferred in the separatory funnel, removed wherein water, collect organic oil reservoir; Add dispersant to organic facies earlier and carried out ultrasonic agitation 60 minutes; Ultrasonic agitation finishes the back and adds organic polymer and remaining sizing agent, and constantly high-speed stirred obtains copper slurry at last.
are reference with the amount of nano copper slurry material, and its quality is 100; Organic polymer (epoxy resin E-44) 28, curing agent (triethylamine) 2, coupling agent (gamma-aminopropyl-triethoxy-silane) 0.7, dispersant (Tissuemat E) 3, copper nanoparticle 63, surplus is an isopropyl alcohol.
Instance 6
The alkaline etching waste liquid for producing of No. 3 production lines of Foshan City PCB manufactory is got in
; Therefrom get 200ml (about 235.54 grams) alkali etching waste water and carry out the three-stage filtration collection and will filter later filtrating, add 4.00 gram gelatin and 2.00 gram water-based antifoaming agents Germany Bi Ke BYK-023 simultaneously as A solution.Preparation contains 15.00 gram hydrazine hydrates, the potassium hydroxide of 20 grams, and the reduction solvent B of the gum turpentine of 150ml.B solution is poured in the there-necked flask, regulated the water bath with thermostatic control temperature at 90 ℃, open and stir, mixing speed is about 200 rev/mins.In there-necked flask, drip A solution, take out cooling, ageing after having reacted.Then reacted solution is transferred in the separatory funnel; Remove wherein water; Collect organic oil reservoir, add dispersant to organic facies earlier and carried out ultrasonic agitation 45 minutes, ultrasonic agitation finishes the back and adds organic polymer and remaining sizing agent; Constantly high-speed stirred obtains the nano copper slurry material at last.
Amount with the nano copper slurry material is a reference, and its quality is 100; Organic polymer (aqueous phenolic aldehyde resin) 36, curing agent (trien) 3, coupling agent (butyl titanate) 0.6, dispersant (polyethylene glycol) 3, copper nanoparticle 56, surplus is an isopropyl alcohol
Claims (11)
1. method of utilizing alkaline etching waste liquid for producing printed circuit board to prepare nanometer copper electrocondution slurry is characterized in that:
A gets a certain amount of alkaline etching waste liquid for producing and filters to remove suspended impurity and precipitated impurities; After filtering filtrating is transferred in the container, added nonionic surface active agent that accounts for alkaline etching waste liquid for producing weight 0.43%-4.24% and the water-based antifoaming agent that accounts for alkaline etching waste liquid for producing weight 0.08%-1.61% simultaneously and obtain solution A;
B preparation reductant solution B; The reducing agent that accounts for alkaline etching waste liquid for producing weight 1.70%-8.49%, the strong alkaline substance that accounts for alkaline etching waste liquid for producing weight 6.80%-10.20% and organic facies turpentine oil have been comprised in the B solution; Contain consisting of phase-transferring agent in the organic facies turpentine oil; The volume ratio of consisting of phase-transferring agent and alkaline etching waste liquid for producing is 1:1-1:2, and solution B is heated to 30 ℃～100 ℃, stirs with 100 rev/mins～1000 rev/mins speed simultaneously; Again solution A is dropped in the solution B;
Cooling after the c reaction is accomplished, ageing; Then transfer to and carry out water in the separatory funnel and separate, remove water, collect the organic facies that contains copper nanoparticle with organic facies;
D adds the dispersant of one of sizing agent earlier to the organic oil reservoir that contains copper nanoparticle that obtains; Put into ultrasonic agitation device ultrasonic agitation 30 minutes-60 minutes; Ultrasonic agitation finishes the back adding and accounts for nano copper slurry material weight 10%-40% organic high molecular compound; With surplus be sizing agent, constantly stir, obtain the nano copper slurry material at last.
2. according to the said method of utilizing alkaline etching waste liquid for producing printed circuit board to prepare nanometer copper electrocondution slurry of claim 1, it is characterized in that: said nonionic Surfactant is tween or polyvinyl pyrrolidone or gelatin or the combination in them.
3. according to the said method of utilizing alkaline etching waste liquid for producing printed circuit board to prepare nanometer copper electrocondution slurry of claim 1, it is characterized in that: said water-based antifoaming agent is German Bi Ke BYK-023 or German Bi Ke BYK-051.
4. according to the said method of utilizing alkaline etching waste liquid for producing printed circuit board to prepare nanometer copper electrocondution slurry of claim 1, it is characterized in that: said reducing agent is hydrazine hydrate or vitamin C or sodium borohydride or inferior sodium phosphate or glucose.
5. according to the said method of utilizing alkaline etching waste liquid for producing printed circuit board to prepare nanometer copper electrocondution slurry of claim 1, it is characterized in that: said turpentine oil is gum turpentine or steam-distilled turpentine or sulfate turpentine.
6. according to the said method of utilizing alkaline etching waste liquid for producing printed circuit board to prepare nanometer copper electrocondution slurry of claim 1, it is characterized in that: said organic high molecular compound is epoxy resin or polyurethanes or aqueous phenolic aldehyde resin.
7. according to the said method of utilizing alkaline etching waste liquid for producing printed circuit board to prepare nanometer copper electrocondution slurry of claim 1; It is characterized in that: said sizing agent comprises coupling agent, curing agent, dispersant, and three's weight ratio scope is between 1:5:5-1:10:10.
8. according to the said method of utilizing alkaline etching waste liquid for producing printed circuit board to prepare nanometer copper electrocondution slurry of claim 7; It is characterized in that: said coupling agent is gamma-aminopropyl-triethoxy-silane or γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane coupling agent or titanate esters.
9. according to the said method of utilizing alkaline etching waste liquid for producing printed circuit board to prepare nanometer copper electrocondution slurry of claim 7, it is characterized in that: said curing agent is alcamines curing agent or polyamine curing agent or their combination.
10. according to the said method of utilizing alkaline etching waste liquid for producing printed circuit board to prepare nanometer copper electrocondution slurry of claim 7, it is characterized in that: said dispersant is oleic acid or polyethylene glycol or Tissuemat E or their combination.
11. according to the said method of utilizing alkaline etching waste liquid for producing printed circuit board to prepare nanometer copper electrocondution slurry of claim 9, it is characterized in that: said alcamines curing agent is diethanol amine or triethanolamine, said polyamine curing agent is triethylamine or trien.
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| CN103480860B (en) * | 2013-09-25 | 2016-01-06 | 广东致卓精密金属科技有限公司 | Alkaline etching waste liquid for producing printed circuit board is utilized to prepare the method for high-purity nano copper |
| CN103506632B (en) * | 2013-09-27 | 2015-09-09 | 暨南大学 | A kind of from containing the method reclaiming ultra tiny copper powder complex copper waste liquid |
| CN106077700A (en) * | 2016-07-13 | 2016-11-09 | 许勤峰 | A kind of method utilizing circuit board waste liquid to prepare Nanometer Copper catalysis slurry |
| CN106041122A (en) * | 2016-07-13 | 2016-10-26 | 许勤峰 | Method for preparing nanometre copper-catalyzed slurry by virtue of PCB acidic waste liquid |
| CN106618598A (en) * | 2016-11-15 | 2017-05-10 | 惠州市力道电子材料有限公司 | Tungsten alloy micro-needle electrode capable of limiting piercing depth, preparation method thereof, and blood glucose monitoring device |
| CN108436104B (en) * | 2018-06-05 | 2021-04-06 | 黔南民族师范学院 | Process for preparing copper nanowires by using acidic etching waste liquid |
| CN112010488B (en) * | 2020-09-09 | 2021-05-25 | 佛山经纬纳科环境科技有限公司 | Method for preparing nano particles from heavy metal wastewater |
| CN113707362A (en) * | 2021-07-23 | 2021-11-26 | 厦门大学 | High-conductivity copper paste, preparation method, flexible high-conductivity copper film and application thereof |
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Address after: 528300 Guangdong city of Foshan province Shunde Daliang District neighborhood Honggang Doo group Patentee after: GUANGDONG CHENGDE ELECTRONIC TECHNOLOGY CO., LTD. Patentee after: Guangdong University of Technology Address before: 528300 Guangdong city of Foshan province Shunde Daliang District neighborhood Honggang Doo group Patentee before: Foshan Chengde Circuit Co., Ltd. Patentee before: Guangdong University of Technology |