CN106077700A - A kind of method utilizing circuit board waste liquid to prepare Nanometer Copper catalysis slurry - Google Patents
A kind of method utilizing circuit board waste liquid to prepare Nanometer Copper catalysis slurry Download PDFInfo
- Publication number
- CN106077700A CN106077700A CN201610547550.4A CN201610547550A CN106077700A CN 106077700 A CN106077700 A CN 106077700A CN 201610547550 A CN201610547550 A CN 201610547550A CN 106077700 A CN106077700 A CN 106077700A
- Authority
- CN
- China
- Prior art keywords
- circuit board
- waste liquid
- nanometer copper
- catalysis slurry
- board waste
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/38—Treatment of water, waste water, or sewage by centrifugal separation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
Abstract
The present invention relates to circuit board field of waste liquid treatment, particularly to a kind of method utilizing circuit board waste liquid to prepare Nanometer Copper catalysis slurry.Waste liquid is first centrifuged remove impurity by the inventive method, is subsequently adding reducing agent reduction and obtains Nanometer Copper, and Nanometer Copper and various additive are finally mixed to get Nanometer Copper catalysis slurry.The present invention has simple to operate, consumes energy little, low cost, and the Nanometer Copper prepared catalysis slurry catalytic performance is excellent.The method alleviates the pressure that circuit board company waste water processes, and has createed higher economic benefit, has also reached the purpose of resources circulation recycling simultaneously.
Description
Technical field
The present invention relates to circuit board field of waste liquid treatment, utilize circuit board waste liquid to prepare Nanometer Copper catalysis particularly to one
The method of slurry.
Background technology
In the circuit boards manufacturing high multilamellar, acid etching is a requisite operation.So-called acid etching
It is exactly to utilize the liquid medicine with acid and oxidisability that the elemental copper being not required to is etched into from circuit board liquid medicine according to engineering design
, but be as etching the copper ion concentration being constantly etched in liquid and the most constantly increase, work as copper ion concentration
If do not processed when reaching finite concentration, it will the effect of impact etching.The most a lot of circuit board companies are especially
Small-sized company sells out or discharges after being all by simply processing for acidic etching waste liquid.
The main component of acidic etching waste liquid is copper chloride, hydrochloric acid, water, and the mass concentration of copper is up to 120～150 g/L.
At present substantially can be divided into following methods for the process of copper in alkaline etching liquid: 1 metal replacement method.Utilize metal activity
Difference, oxytropism etching waste liquor adds iron powder or aluminium powder copper ion is reduced into spongiform elemental copper；2 extraction electricity
Solution.First oxytropism etching waste liquor adds some extractants of copper, then obtains the copper ion solution of high concentration through back extraction,
Then the method utilizing electrolysis obtains elemental copper；3 electrolytic reductions.This method is based on electrochemical principle, acidity is lost
Carve copper ion in liquid to obtain electronics at negative electrode and be reduced into elemental copper；4, roasting method is utilized to reclaim copper oxide method.By acid etching
Waste liquid sprays from nozzle through high pressure, is dispersed in the roaster of 550 DEG C with droplet state, resolves into copper oxide.But these
In place of method comes with some shortcomings: 1. the displacement method response rate is low, and copper purity is low, and accompanies the side reaction of liberation of hydrogen in replacement process
Thus cause the instability of technique.2. extraction electrolysis technics comparing is complicated, and consuming electric power is bigger, and electro-deposition is later
Waste liquid does not reaches the standard of discharge yet.3. roasting method, the response rate is the highest, complex procedures, and cost is the biggest.
Catalysis slurry rose in recent years, it has been researched and developed by domestic company and scientific research institution, the most main still
Be used in circuit board manufacturing area, by by catalysis slurry with spray printing by the way of print on board substrate, low in then passing through
After the solidification of temperature, metal is exposed to surface, places into plated with copper in plating solution and forms circuit.Existing catalysis slurry catalyst mostly is
The noble metals such as palladium, platinum, gold, silver, but in recent years, these noble metal spurts in prices so that various noble metal electric slurries manufacture
Cost drastically increases.Elemental copper also has catalytic performance, when the size of copper reaches nanoscale due to the catalysis of dimensional effect copper
Performance is more preferable.
Summary of the invention
The technical problem to be solved is to provide and a kind of utilizes circuit board waste liquid to prepare Nanometer Copper catalysis slurry
Method.
A kind of method utilizing circuit board waste liquid to prepare Nanometer Copper catalysis slurry, comprises the steps of: a takes a certain amount of electricity
Road plate waste liquid is poured into and is utilized centrifuge to be centrifuged filtering to remove the float in waste liquid and precipitated impurities in centrifuge tube, centrifugal
After take filtrate and put in reactor, add Tetramethylammonium hydroxide by pH regulator to 8.5, add and account for circuit board waste liquid weight 0.1-
The surfactant of 5.0%, adds the transfer agent accounting for circuit board waste liquid weight 20-50%, adds and accounts for circuit board waste liquid weight
The reducing agent of 1.0-10%, then seals reactor；
Airtight good reactor is put in isothermal reactor by b, and regulation reaction temperature is to 80 DEG C, and the response time is 120 minutes, with
Time stir reactant liquor with the rotating speed of 80 revs/min, question response is poured reactant into centrifuge tube after terminating and is centrifuged separating, and takes and contains
The organic layer of nano copper particle；
C adds other components according to following parts by weight:
The organic layer 10 ~ 20 parts containing nano copper particle of gained in step b；Coupling agent 1 ~ 3 part；Defoamer 1 ~ 3 part；Diluent 40
~ 70 parts；Polyethylene glycol 6000 20 ~ 40 parts；
Described Nanometer Copper catalysis slurry is obtained after finally being stirred by above-mentioned substance.
Further, the surfactant in described step a is the mixture of polyethylene glycol laurate and sodium stearate,
Wherein polyethylene glycol laurate and sodium stearate compare 1:2 for both mass weight.Surfactant used is the Polyethylene Glycol moon
Cinnamic acid ester and the mixture of sodium stearate, material both this has hydrophile function and oleophylic function simultaneously, time in aqueous with
The nano copper particle restored combines, and is wrapped up by Nanometer Copper and prevents polymerization between granule and oxidized, will simultaneously
The copper nanoparticle wrapped up can be transferred in transfer agent, so reduces the Nanometer Copper time of staying in aqueous, prevents
Nanometer Copper is aoxidized by oxygen in aqueous solution.
Further, the transfer agent in described step a is dodecylic acid.It had both served as the consisting of phase-transferring agent of Nanometer Copper, so
Obtained by organic oil reservoir can be directly as the composition of catalysis slurry, thus the Nanometer Copper greatly reduced in solution is transferred to
The step gone in slurry, decreases the chance that Nanometer Copper is oxidized in transfer process, improves the purity of Nanometer Copper, the most also
Copper dispersion in catalysis slurry can be promoted as the lubricant of Nanometer Copper in catalysis slurry, prevents the reunion of nano-particle,
Strengthen the catalytic performance of slurry.
Further, the reducing agent in described step a is ascorbic acid.Ascorbic acid provides electronics to incite somebody to action in course of reaction
Copper ion in solution is reduced into copper simple substance, and owing to ascorbic acid reproducibility is gentleer, rate of reduction is slow, reduces nanometer
The probability that copper crystal is grown up in reduction process.
Catalysis slurry in use polyethylene glycol 6000, its catalyst pulp after hardening in provide one connect base material with
" bridge " that copper nanoparticle is basic, is on the one hand connectable to base material, on the other hand utilizes itself and polyethylene glycol laurate phase
The feature that capacitive is good connects copper nanoparticle；And have part polyethylene glycol 6000 to vapor away after hardening so that originally by poly-second
The Nanometer Copper that glycol 6000 covers is exposed to provide catalytic performance.
Further, the coupling agent in described step c is silane coupler.Silane coupler used is that the art is normal
Silane coupler all can realize the present invention, such as KH550, KH570 etc..
Further, the defoamer tributyl phosphate in described step c.
Further, the diluent in described step c is alcohols solvent.Alcohols solvent used is that the art is conventional
Alcohols solvent all can realize the present invention, present invention preferably uses isoamyl alcohol.
There is advantages that
1. this invention takes under the method preparing Nanometer Copper and phase transfer in empty sealing system, prepare Nanometer Copper catalysis slurry
Material, the Nanometer Copper good separating effect prepared, shape are uniformly, good dispersion, purity are high, size is little, the catalysis slurry of gained
Catalytic performance is good；2. process conditions relatively easily operate, without big power consumption；3. final products are that the Nanometer Copper that added value is the highest is urged
Slurrying material, has createed higher economic benefit, it is achieved that the purpose turned waste into wealth.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be described in detail, and embodiment is only the preferred embodiment of the present invention,
It it not limitation of the invention.
Embodiment
Take the acidic etching waste liquid of Huizhou PCB maker production line, therefrom take 80 milliliters (about 100 grams) and put into centrifuge tube
Middle centrifuge is utilized to be centrifuged filtering to remove the float in waste liquid and precipitated impurities, centrifugation rate 7000 revs/min, from
30 minutes heart time, taking in the reactor that filtrate pours good leak tightness into after being centrifuged, adding Tetramethylammonium hydroxide regulation pH is
8.5, add 1 gram of polyethylene glycol laurate and 2 grams of sodium stearates, add 25 grams of dodecylic acids, add 5 grams of ascorbic acid, close
Seal reactor and put in thermostatic heater, control 120 minutes response time, reaction temperature 80 DEG C, stir speed (S.S.) 80 revs/min
Clock.Take out cooling after having reacted, after ageing, pour the oil reservoir containing Nanometer Copper of centrifuging and taking in centrifuge tube into, centrifugation rate 7000 turns/
Minute, centrifugation time 30 minutes.Then add polyethylene glycol 6000 to the organic layer containing nano copper particle, sequentially add dispersion
Agent Silane coupling agent KH550, isoamyl alcohol, defoamer tributyl phosphate, put into and ultrasonic stirrer is stirred 30 minutes, stirring
Speed 1000 revs/min, has obtained Nanometer Copper catalysis slurry after stirring.
The Nanometer Copper catalysis slurry of gained is by the component of following mass fraction: the organic layer containing nano copper particle 15 parts；
KH550 2 parts；Tributyl phosphate 2 parts；Isoamyl alcohol 50 parts；Polyethylene glycol 6000 30 parts.
Comparative example
Take the acidic etching waste liquid of Huizhou PCB maker production line, therefrom take 80 milliliters (about 100 grams) and put into profit in centrifuge tube
Being centrifuged filtering to remove the float in waste liquid and precipitated impurities with centrifuge, centrifugation rate 7000 revs/min, time centrifugal
Between 30 minutes, centrifugal after take in the reactor that filtrate pours good leak tightness into, adding Tetramethylammonium hydroxide regulation pH is 8.5, adds
Entering 25 grams of dodecylic acids, add 5 grams of ascorbic acid, good seal reactor is put in thermostatic heater, controls the response time 120 points
Clock, reaction temperature 80 DEG C, stir speed (S.S.) 80 revs/min.Take out cooling after having reacted, after ageing, pour centrifuging and taking in centrifuge tube into
Oil reservoir containing Nanometer Copper, centrifugation rate 7000 revs/min, centrifugation time 30 minutes.Then to the organic layer containing nano copper particle
Add polyethylene glycol 6000, sequentially add dispersant Silane coupling agent KH550, isoamyl alcohol, defoamer tributyl phosphate, put into
Ultrasonic stirrer is stirred 30 minutes, stir speed (S.S.) 1000 revs/min, after stirring, has obtained Nanometer Copper catalysis slurry
Material.
The Nanometer Copper catalysis slurry of gained is by the component of following mass fraction: the organic layer containing nano copper particle 15 parts；
KH550 2 parts；Tributyl phosphate 2 parts；Isoamyl alcohol 50 parts；Polyethylene glycol 6000 30 parts.
Then the Nanometer Copper of above-described embodiment and comparative example gained is catalyzed slurry and utilizes Malvern laser particle size analyzer
Carry out grain size analysis.By test, in embodiment, the mean diameter of Nanometer Copper is 120 nm, and is evenly distributed；And it is right
In ratio, the mean diameter of Nanometer Copper is 326 nm.Therefore, we understand is had by the specific surface activator composition of interpolation
It is beneficial to control the particle diameter of Nanometer Copper so that the Nanometer Copper catalysis slurry of gained has more excellent performance.
Embodiment described above only have expressed embodiments of the present invention, and it describes more concrete and detailed, but can not
Therefore the restriction to the scope of the claims of the present invention it is interpreted as, as long as using the skill that the form of equivalent or equivalent transformation is obtained
Art scheme, all should fall within the scope and spirit of the invention.
Claims (7)
1. one kind utilizes the method that circuit board waste liquid prepares Nanometer Copper catalysis slurry, it is characterised in that comprise the steps of: a takes one
Quantitative circuit board waste liquid is poured into and is utilized centrifuge to be centrifuged filtering to remove the float in waste liquid and precipitation in centrifuge tube
Impurity, takes filtrate after being centrifuged and puts in reactor, adds Tetramethylammonium hydroxide and pH regulator to 8.5, addition are accounted for circuit board and given up
The surfactant of liquid weight 0.1-5.0%, adds the transfer agent accounting for circuit board waste liquid weight 20-50%, and addition accounts for circuit board and gives up
The reducing agent of the 1.0-10% of liquid weight, then seals reactor；
Airtight good reactor is put in isothermal reactor by b, and regulation reaction temperature is to 80 DEG C, and the response time is 120 minutes, with
Time stir reactant liquor with the rotating speed of 80 revs/min, question response is poured reactant into centrifuge tube after terminating and is centrifuged separating, and takes and contains
The organic layer of nano copper particle；
C adds other components according to following parts by weight:
The organic layer 10 ~ 20 parts containing nano copper particle of gained in step b；Coupling agent 1 ~ 3 part；Defoamer 1 ~ 3 part；Diluent 40
~ 70 parts；Polyethylene glycol 6000 20 ~ 40 parts；
Described Nanometer Copper catalysis slurry is obtained after finally being stirred by above-mentioned substance.
A kind of method utilizing circuit board waste liquid to prepare Nanometer Copper catalysis slurry the most according to claim 1, its feature exists
In, the surfactant in described step a is the mixture of polyethylene glycol laurate and sodium stearate, wherein the Polyethylene Glycol moon
Cinnamic acid ester and sodium stearate compare 1:2 for both mass weight.
A kind of method utilizing circuit board waste liquid to prepare Nanometer Copper catalysis slurry the most according to claim 1, its feature exists
In, the transfer agent in described step a is dodecylic acid.
A kind of method utilizing circuit board waste liquid to prepare Nanometer Copper catalysis slurry the most according to claim 1, its feature exists
In, the reducing agent in described step a is ascorbic acid.
A kind of method utilizing circuit board waste liquid to prepare Nanometer Copper catalysis slurry the most according to claim 1, its feature exists
In, the coupling agent in described step c is silane coupler.
A kind of method utilizing circuit board waste liquid to prepare Nanometer Copper catalysis slurry the most according to claim 1, its feature exists
In, the defoamer tributyl phosphate in described step c.
A kind of method utilizing circuit board waste liquid to prepare Nanometer Copper catalysis slurry the most according to claim 1, its feature exists
In, the diluent in described step c is alcohols solvent.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610547550.4A CN106077700A (en) | 2016-07-13 | 2016-07-13 | A kind of method utilizing circuit board waste liquid to prepare Nanometer Copper catalysis slurry |
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| CN201610547550.4A CN106077700A (en) | 2016-07-13 | 2016-07-13 | A kind of method utilizing circuit board waste liquid to prepare Nanometer Copper catalysis slurry |
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| CN106077700A true CN106077700A (en) | 2016-11-09 |
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| CN201610547550.4A Pending CN106077700A (en) | 2016-07-13 | 2016-07-13 | A kind of method utilizing circuit board waste liquid to prepare Nanometer Copper catalysis slurry |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108436104A (en) * | 2018-06-05 | 2018-08-24 | 黔南民族师范学院 | - kind of the technique for preparing copper nano-wire with acidic etching waste liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108436104A (en) * | 2018-06-05 | 2018-08-24 | 黔南民族师范学院 | - kind of the technique for preparing copper nano-wire with acidic etching waste liquid |
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Application publication date: 20161109 |
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