CN110422872A - A kind of Kocide SD of alkaline etching liquid and preparation method thereof - Google Patents
A kind of Kocide SD of alkaline etching liquid and preparation method thereof Download PDFInfo
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- CN110422872A CN110422872A CN201910751198.XA CN201910751198A CN110422872A CN 110422872 A CN110422872 A CN 110422872A CN 201910751198 A CN201910751198 A CN 201910751198A CN 110422872 A CN110422872 A CN 110422872A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
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Abstract
The present invention provides a kind of Kocide SD and preparation method thereof of alkaline etching liquid, cupric ammine complex will be contained, the alkaline etching liquid of ammonium chloride and ammonium hydroxide is added in reaction kettle, then selection contains copper chloride, stannous chloride, the acidic etching liquid of hydrogen peroxide and hydrochloric acid is slowly added in its reaction kettle, it is stirred, at normal temperatures and pressures by the pH value adjustment of mixed liquor in reaction kettle to 4.0-8.0, reaction time is 3-4 hours, generate Kocide SD precipitating, the mixed liquor of Kocide SD will be had, Kocide SD precipitating after filtering washing is put into enamel reactor, strong sulfuric acid response is added and generates copper sulphate concentrated solution, crystallization obtains crystal copper sulphate after cooling.The present invention adjusts pH value by the way that alkaline etching liquid and soda acid etching solution are carried out mixing, is conducive to alkaline etching liquid and soda acid etching solution merging utilization, prepares Kocide SD or new etching solution, be comprehensively utilized resource while reducing environmental pollution.
Description
Technical field
The present invention relates to Kocide SD extractive technique field more particularly to the Kocide SDs and its system of a kind of alkaline etching liquid
Preparation Method.
Background technique
In printed circuit board process, alkaline copper ammoniacal etchant liquid is usually used, is existed largely in waste liquid after etching
Copper ion is just used as discard solution discharge port after copper ion reaches a certain concentration in etching solution, not only causes the serious wave of resource
Take, and increase the cost and difficulty of subsequent sewage treatment, pollutes environment.Wherein alkaline etching waste liquid for producing main component is cuprammonium
Complex compound and ammonium chloride etc., the main component of acidic etching waste liquid are copper chloride and hydrochloric acid etc..It can be recycled in annual etching waste liquor
Amount of copper be up to 200,000 tons, have great significance to the copper recycling and reusing in etching waste liquor.
Therefore, it is necessary to solve the above problems to invent Kocide SD of a kind of alkaline etching liquid and preparation method thereof
Summary of the invention
The purpose of the present invention is to provide Kocide SDs of a kind of alkaline etching liquid and preparation method thereof, to solve above-mentioned skill
Art problem.
The present invention using following technical scheme in order to solve the above technical problems, realized:
A kind of Kocide SD of alkaline etching liquid, the Kocide SD are amorphous nano powder Kocide SD, the hydrogen
Cupric oxide powder partial size is 30-80nm, average grain diameter 46nm.
Based on a kind of above-mentioned Kocide SD preparation method of alkaline etching liquid, comprising the following steps:
S1: it will be added in reaction kettle containing the alkaline etching liquid of cupric ammine complex, ammonium chloride and ammonium hydroxide, then selection contains
There is the acidic etching liquid of copper chloride, stannous chloride, hydrogen peroxide and hydrochloric acid to be slowly added in its reaction kettle, be stirred, in room temperature
By the pH value adjustment of mixed liquor in reaction kettle to 4.0-8.0 under normal pressure, the reaction time is 3-4 hours, generates Kocide SD precipitating,
Its chemical equation is as follows:
S2: will have the mixed liquor of Kocide SD, be passed through filter-press dehydration in filter press, and wash the chloride ion etc. of its absorption
Kocide SD precipitating after filtering washing is put into enamel reactor by impurity, and it is dense molten that strong sulfuric acid response generation copper sulphate is added
Liquid, it is cooling after crystallization obtain crystal copper sulphate, stay in spare, and by the filter effluent collection after filter press filters pressing, carry out in next step
Remove the copper in waste liquid；
S3: the water that filters out collected in step S2 is added in reaction kettle, and it is 1%-5% hydrazine hydrate that concentration, which is then added, and
And pH value adjustment agent is added, it is 6.0 by the pH value adjustment for filtering out water, reaction temperature is heated to 40 degree, the reaction time is 45 points
Copper is prepared in clock, and chemical equation is as follows:
2Cu2++N2H4·H2O+4OH-→2Cu↓+N2+5H2O；
S4: weighing copper sulfate crystal in step S2, is added in distilled water, is configured to the copper-bath of 0.25mol/L, In
It is slowly stirred lower addition ammonium hydroxide in copper-bath, then mixed liquor is put into processor for ultrasonic wave, hydroxide is added by several times
Barium, ultrasonic treatment 4 hours in the case where power per liter density is 1.2W/cm2, four ammino copper of the hydroxide complexing that blue is prepared was molten
Liquid, chemical equation are as follows:
S5: being added distilled water in ultrasonic treatment chamber, and water temperature is controlled at 45 degree, and applying sound intensity degree is the super of 0.60 W/cm2
Acoustic vibration, then the four ammino copper complex solution of hydroxide in step S4 is disposably in the distilled water of falling people, reaction time 2-3 point
Clock generates blue Kocide SD precipitating, with ammonia scrubbing sediment 2-3 times that pH value is 9.0 after extraction filtering, then with anhydrous
It ethanol washing sediment 2 times, is dried under 55 degree to constant weight after filtering, obtains blue amorphous nano powder Kocide SD,
Chemical equation is as follows:
Cu(NH3)6(OH)2→Cu2++6NH3↑+ 2OH-
Cu2++2OH-→Cu(OH)2↓。
Preferably, the copper content of the step S1 neutral and alkali etching solution is 120-180g/L, acid erosion in the step S1
The copper content for carving liquid is 120-160g/L.
Preferably, the copper content after water and hydration hydrazine reaction are filtered out in the step S3 should be less than 0.2g/L.
Preferably, the concentration of copper sulfate crystal and distilled water ratio is 65g/L in the step S4, and ammonium hydroxide is dense in step S4
Degree is 8mol/L.
Preferably, the quality of barium hydroxide is added in the step S4 every time no more than 10g.
Preferably, it is filtered with the sediment that dehydrated alcohol washs using sand core funnel in the step S5.The present invention
Beneficial effect be:
(1) present invention adjusts pH value by the way that alkaline etching liquid and soda acid etching solution are carried out mixing, is conducive to lose alkalinity
It carves liquid and soda acid etching solution merges utilization, Kocide SD or new etching solution are prepared, while reducing environmental pollution
It is comprehensively utilized resource.
(2) present invention prepares Kocide SD by using hydrazine hydrate reduction, has kinetics rate fast, operating cost
Low, high-efficient feature, and poisonous and harmful by-product will not be generated in reaction process, pollution is small, has high economic benefit
And environmental benefit.
(3) present invention prepares amorphous nano powder Kocide SD by using ultrasonic technique and chemical precipitation technology,
Effectively to the abundant extraction of copper ion in alkaline etching liquid, and reduce pollution during the extraction process, increases economic efficiency.
Detailed description of the invention
Fig. 1 is the amorphous nano powder Kocide SD structure TEM schematic diagram of invention；
Fig. 2 is the concentration of hydrazine hydrate of invention to copper ion removal rate structural schematic diagram；
Fig. 3 is the alkaline etching liquid of invention and the pH value structure influence diagram of acidic etching liquid fusion.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Specific embodiment is closed, the present invention is further explained, and however, the following embodiments are merely preferred embodiments of the present invention, and not all.
Based on the implementation example in the implementation mode, those skilled in the art's obtained other realities without making creative work
Example is applied, protection scope of the present invention is belonged to.Experimental method in following embodiments is unless otherwise specified conventional method,
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Embodiment one:
The present invention provides a kind of Kocide SD of alkaline etching liquid as shown in Figs. 1-3, the Kocide SD is amorphous
State nano-powder Kocide SD, the Kocide SD diameter of particle are 30-80nm, average grain diameter 46nm.
A kind of Kocide SD preparation method of alkaline etching liquid of the present invention, comprising the following steps:
S1: it will be added in reaction kettle containing the alkaline etching liquid of cupric ammine complex, ammonium chloride and ammonium hydroxide, then selection contains
There is the acidic etching liquid of copper chloride, stannous chloride, hydrogen peroxide and hydrochloric acid to be slowly added in its reaction kettle, be stirred, in room temperature
By the pH value adjustment of mixed liquor in reaction kettle to 4.0 under normal pressure, the reaction time is 3-4 hours, generates Kocide SD precipitating, changes
It is as follows to learn reaction equation:
S2: will have the mixed liquor of Kocide SD, be passed through filter-press dehydration in filter press, and wash the chloride ion etc. of its absorption
Kocide SD precipitating after filtering washing is put into enamel reactor by impurity, and it is dense molten that strong sulfuric acid response generation copper sulphate is added
Liquid, it is cooling after crystallization obtain crystal copper sulphate, stay in spare, and by the filter effluent collection after filter press filters pressing, carry out in next step
Remove the copper in waste liquid；
S3: the water that filters out collected in step S2 is added in reaction kettle, it is 1% hydrazine hydrate that concentration, which is then added, and is added
Enter pH value adjustment agent, be 6.0 by the pH value adjustment for filtering out water, reaction temperature is heated to 40 degree, the reaction time is 45 minutes, system
Standby to obtain copper, chemical equation is as follows:
2Cu2++N2H4·H2O+4OH-→2Cu↓+N2+5H2O；
S4: weighing copper sulfate crystal in step S2, is added in distilled water, is configured to the copper-bath of 0.25mol/L, In
It is slowly stirred lower addition ammonium hydroxide in copper-bath, then mixed liquor is put into processor for ultrasonic wave, hydroxide is added by several times
Barium, and the quality that barium hydroxide is added every time is not more than 10g, ultrasonic treatment 4 hours in the case where power per liter density is 1.2W/cm2,
The four ammino copper complex solution of hydroxide of blue is prepared, chemical equation is as follows:
S5: being added distilled water in ultrasonic treatment chamber, and water temperature is controlled at 45 degree, and applying sound intensity degree is the super of 0.60 W/cm2
Acoustic vibration, then the four ammino copper complex solution of hydroxide in step S4 is disposably in the distilled water of falling people, reaction time 2-3 point
Clock generates blue Kocide SD precipitating, with ammonia scrubbing sediment 2-3 times that pH value is 9.0 after extraction filtering, then with anhydrous
It ethanol washing sediment 2 times, is dried under 55 degree to constant weight after filtering, obtains blue amorphous nano powder Kocide SD,
Chemical equation is as follows:
Cu(NH3)6(OH)2→Cu2++6NH3↑+ 2OH-
Cu2++2OH-→Cu(OH)2↓。
Embodiment two:
A kind of Kocide SD of alkaline etching liquid of the present invention, the Kocide SD are amorphous nano powder Kocide SD,
The Kocide SD diameter of particle is 30-80nm, average grain diameter 46nm.
A kind of Kocide SD preparation method of alkaline etching liquid of the present invention, comprising the following steps:
S1: it will be added in reaction kettle containing the alkaline etching liquid of cupric ammine complex, ammonium chloride and ammonium hydroxide, then selection contains
There is the acidic etching liquid of copper chloride, stannous chloride, hydrogen peroxide and hydrochloric acid to be slowly added in its reaction kettle, be stirred, in room temperature
By the pH value adjustment of mixed liquor in reaction kettle to 5.0 under normal pressure, the reaction time is 3-4 hours, generates Kocide SD precipitating, changes
It is as follows to learn reaction equation:
S2: will have the mixed liquor of Kocide SD, be passed through filter-press dehydration in filter press, and wash the chloride ion etc. of its absorption
Kocide SD precipitating after filtering washing is put into enamel reactor by impurity, and it is dense molten that strong sulfuric acid response generation copper sulphate is added
Liquid, it is cooling after crystallization obtain crystal copper sulphate, stay in spare, and by the filter effluent collection after filter press filters pressing, carry out in next step
Remove the copper in waste liquid；
S3: the water that filters out collected in step S2 is added in reaction kettle, it is 2% hydrazine hydrate that concentration, which is then added, and is added
Enter pH value adjustment agent, be 6.0 by the pH value adjustment for filtering out water, reaction temperature is heated to 40 degree, the reaction time is 45 minutes, system
Standby to obtain copper, chemical equation is as follows:
2Cu2++N2H4·H2O+4OH-→2Cu↓+N2+5H2O；
S4: weighing copper sulfate crystal in step S2, is added in distilled water, is configured to the copper-bath of 0.25mol/L, In
It is slowly stirred lower addition ammonium hydroxide in copper-bath, then mixed liquor is put into processor for ultrasonic wave, hydroxide is added by several times
Barium, and the quality that barium hydroxide is added every time is not more than 10g, ultrasonic treatment 4 hours in the case where power per liter density is 1.2W/cm2,
The four ammino copper complex solution of hydroxide of blue is prepared, chemical equation is as follows:
S5: being added distilled water in ultrasonic treatment chamber, and water temperature is controlled at 45 degree, and applying sound intensity degree is the super of 0.60 W/cm2
Acoustic vibration, then the four ammino copper complex solution of hydroxide in step S4 is disposably in the distilled water of falling people, reaction time 2-3 point
Clock generates blue Kocide SD precipitating, with ammonia scrubbing sediment 2-3 times that pH value is 9.0 after extraction filtering, then with anhydrous
It ethanol washing sediment 2 times, is dried under 55 degree to constant weight after filtering, obtains blue amorphous nano powder Kocide SD,
Chemical equation is as follows:
Cu(NH3)6(OH)2→Cu2++6NH3↑+ 2OH-
Cu2++2OH-→Cu(OH)2↓。
Embodiment three:
A kind of Kocide SD of alkaline etching liquid of the present invention, the Kocide SD are amorphous nano powder Kocide SD,
The Kocide SD diameter of particle is 30-80nm, average grain diameter 46nm.
A kind of Kocide SD preparation method of alkaline etching liquid of the present invention, comprising the following steps:
S1: it will be added in reaction kettle containing the alkaline etching liquid of cupric ammine complex, ammonium chloride and ammonium hydroxide, then selection contains
There is the acidic etching liquid of copper chloride, stannous chloride, hydrogen peroxide and hydrochloric acid to be slowly added in its reaction kettle, be stirred, in room temperature
By the pH value adjustment of mixed liquor in reaction kettle to 6.0 under normal pressure, the reaction time is 3-4 hours, generates Kocide SD precipitating, changes
It is as follows to learn reaction equation:
S2: will have the mixed liquor of Kocide SD, be passed through filter-press dehydration in filter press, and wash the chloride ion etc. of its absorption
Kocide SD precipitating after filtering washing is put into enamel reactor by impurity, and it is dense molten that strong sulfuric acid response generation copper sulphate is added
Liquid, it is cooling after crystallization obtain crystal copper sulphate, stay in spare, and by the filter effluent collection after filter press filters pressing, carry out in next step
Remove the copper in waste liquid；
S3: the water that filters out collected in step S2 is added in reaction kettle, it is 3% hydrazine hydrate that concentration, which is then added, and is added
Enter pH value adjustment agent, be 6.0 by the pH value adjustment for filtering out water, reaction temperature is heated to 40 degree, the reaction time is 45 minutes, system
Standby to obtain copper, chemical equation is as follows:
2Cu2++N2H4·H2O+4OH-→2Cu↓+N2+5H2O；
S4: weighing copper sulfate crystal in step S2, is added in distilled water, is configured to the copper-bath of 0.25mol/L, In
It is slowly stirred lower addition ammonium hydroxide in copper-bath, then mixed liquor is put into processor for ultrasonic wave, hydroxide is added by several times
Barium, and the quality that barium hydroxide is added every time is not more than 10g, ultrasonic treatment 4 hours in the case where power per liter density is 1.2W/cm2,
The four ammino copper complex solution of hydroxide of blue is prepared, chemical equation is as follows:
S5: being added distilled water in ultrasonic treatment chamber, and water temperature is controlled at 45 degree, and applying sound intensity degree is the super of 0.60 W/cm2
Acoustic vibration, then the four ammino copper complex solution of hydroxide in step S4 is disposably in the distilled water of falling people, reaction time 2-3 point
Clock generates blue Kocide SD precipitating, with ammonia scrubbing sediment 2-3 times that pH value is 9.0 after extraction filtering, then with anhydrous
It ethanol washing sediment 2 times, is dried under 55 degree to constant weight after filtering, obtains blue amorphous nano powder Kocide SD,
Chemical equation is as follows:
Cu(NH3)6(OH)2→Cu2++6NH3↑+ 2OH-
Cu2++2OH-→Cu(OH)2↓。
Example IV:
A kind of Kocide SD of alkaline etching liquid of the present invention, the Kocide SD are amorphous nano powder Kocide SD,
The Kocide SD diameter of particle is 30-80nm, average grain diameter 46nm.
A kind of Kocide SD preparation method of alkaline etching liquid of the present invention, comprising the following steps:
S1: it will be added in reaction kettle containing the alkaline etching liquid of cupric ammine complex, ammonium chloride and ammonium hydroxide, then selection contains
There is the acidic etching liquid of copper chloride, stannous chloride, hydrogen peroxide and hydrochloric acid to be slowly added in its reaction kettle, be stirred, in room temperature
By the pH value adjustment of mixed liquor in reaction kettle to 7.0 under normal pressure, the reaction time is 3-4 hours, generates Kocide SD precipitating, changes
It is as follows to learn reaction equation:
S2: will have the mixed liquor of Kocide SD, be passed through filter-press dehydration in filter press, and wash the chloride ion etc. of its absorption
Kocide SD precipitating after filtering washing is put into enamel reactor by impurity, and it is dense molten that strong sulfuric acid response generation copper sulphate is added
Liquid, it is cooling after crystallization obtain crystal copper sulphate, stay in spare, and by the filter effluent collection after filter press filters pressing, carry out in next step
Remove the copper in waste liquid；
S3: the water that filters out collected in step S2 is added in reaction kettle, it is 4% hydrazine hydrate that concentration, which is then added, and is added
Enter pH value adjustment agent, be 6.0 by the pH value adjustment for filtering out water, reaction temperature is heated to 40 degree, the reaction time is 45 minutes, system
Standby to obtain copper, chemical equation is as follows:
2Cu2++N2H4·H2O+4OH-→2Cu↓+N2+5H2O；
S4: weighing copper sulfate crystal in step S2, is added in distilled water, is configured to the copper-bath of 0.25mol/L, In
It is slowly stirred lower addition ammonium hydroxide in copper-bath, then mixed liquor is put into processor for ultrasonic wave, hydroxide is added by several times
Barium, and the quality that barium hydroxide is added every time is not more than 10g, ultrasonic treatment 4 hours in the case where power per liter density is 1.2W/cm2,
The four ammino copper complex solution of hydroxide of blue is prepared, chemical equation is as follows:
S5: being added distilled water in ultrasonic treatment chamber, and water temperature is controlled at 45 degree, and applying sound intensity degree is the super of 0.60 W/cm2
Acoustic vibration, then the four ammino copper complex solution of hydroxide in step S4 is disposably in the distilled water of falling people, reaction time 2-3 point
Clock generates blue Kocide SD precipitating, with ammonia scrubbing sediment 2-3 times that pH value is 9.0 after extraction filtering, then with anhydrous
It ethanol washing sediment 2 times, is dried under 55 degree to constant weight after filtering, obtains blue amorphous nano powder Kocide SD,
Chemical equation is as follows:
Cu(NH3)6(OH)2→Cu2++6NH3↑+ 2OH-
Cu2++2OH-→Cu(OH)2↓。
Embodiment five:
A kind of Kocide SD of alkaline etching liquid of the present invention, the Kocide SD are amorphous nano powder Kocide SD,
The Kocide SD diameter of particle is 30-80nm, average grain diameter 46nm.
A kind of Kocide SD preparation method of alkaline etching liquid of the present invention, comprising the following steps:
S1: it will be added in reaction kettle containing the alkaline etching liquid of cupric ammine complex, ammonium chloride and ammonium hydroxide, then selection contains
There is the acidic etching liquid of copper chloride, stannous chloride, hydrogen peroxide and hydrochloric acid to be slowly added in its reaction kettle, be stirred, in room temperature
By the pH value adjustment of mixed liquor in reaction kettle to 8.0 under normal pressure, the reaction time is 3-4 hours, generates Kocide SD precipitating, changes
It is as follows to learn reaction equation:
S2: will have the mixed liquor of Kocide SD, be passed through filter-press dehydration in filter press, and wash the chloride ion etc. of its absorption
Kocide SD precipitating after filtering washing is put into enamel reactor by impurity, and it is dense molten that strong sulfuric acid response generation copper sulphate is added
Liquid, it is cooling after crystallization obtain crystal copper sulphate, stay in spare, and by the filter effluent collection after filter press filters pressing, carry out in next step
Remove the copper in waste liquid；
S3: the water that filters out collected in step S2 is added in reaction kettle, it is 5% hydrazine hydrate that concentration, which is then added, and is added
Enter pH value adjustment agent, be 6.0 by the pH value adjustment for filtering out water, reaction temperature is heated to 40 degree, the reaction time is 45 minutes, system
Standby to obtain copper, chemical equation is as follows:
2Cu2++N2H4·H2O+4OH-→2Cu↓+N2+5H2O；
S4: weighing copper sulfate crystal in step S2, is added in distilled water, is configured to the copper-bath of 0.25mol/L, In
It is slowly stirred lower addition ammonium hydroxide in copper-bath, then mixed liquor is put into processor for ultrasonic wave, hydroxide is added by several times
Barium, and the quality that barium hydroxide is added every time is not more than 10g, ultrasonic treatment 4 hours in the case where power per liter density is 1.2W/cm2,
The four ammino copper complex solution of hydroxide of blue is prepared, chemical equation is as follows:
CuSO4+Ba(OH)2+6NH4OH=Cu (NH3)6OH2+BaSO4↓+ 6H2O；
S5: being added distilled water in ultrasonic treatment chamber, and water temperature is controlled at 45 degree, and applying sound intensity degree is the super of 0.60 W/cm2
Acoustic vibration, then the four ammino copper complex solution of hydroxide in step S4 is disposably in the distilled water of falling people, reaction time 2-3 point
Clock generates blue Kocide SD precipitating, with ammonia scrubbing sediment 2-3 times that pH value is 9.0 after extraction filtering, then with anhydrous
It ethanol washing sediment 2 times, is dried under 55 degree to constant weight after filtering, obtains blue amorphous nano powder Kocide SD,
Chemical equation is as follows:
Cu(NH3)6(OH)2→Cu2++6NH3↑+ 2OH-
Cu2++2OH-→Cu(OH)2↓。
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
For personnel it should be appreciated that the present invention is not limited to the above embodiments, described in the above embodiment and specification is only the present invention
Preference, be not intended to limit the invention, without departing from the spirit and scope of the present invention, the present invention also has various
Changes and improvements, these changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by institute
Attached claims and its equivalent thereof.
Claims (7)
1. a kind of Kocide SD of alkaline etching liquid, it is characterised in that: the Kocide SD is amorphous nano powder hydroxide
Copper, the Kocide SD diameter of particle are 30-80nm, average grain diameter 46nm.
2. a kind of Kocide SD preparation method of alkaline etching liquid according to claim 1, it is characterised in that: including following
Step:
S1: it will be added in reaction kettle containing the alkaline etching liquid of cupric ammine complex, ammonium chloride and ammonium hydroxide, then selection contains chlorine
The acidic etching liquid for changing copper, stannous chloride, hydrogen peroxide and hydrochloric acid is slowly added in its reaction kettle, is stirred, in normal temperature and pressure
For the lower pH value adjustment by mixed liquor in reaction kettle to 4.0-8.0, the reaction time is 3-4 hours, generates Kocide SD precipitating, changes
It is as follows to learn reaction equation:
S2: the mixed liquor of Kocide SD will be had, chloride ion for being passed through filter-press dehydration in filter press, and washing its absorption etc. is miscellaneous
Kocide SD precipitating after filtering washing is put into enamel reactor, strong sulfuric acid response is added and generates copper sulphate concentrated solution by matter,
Crystallization obtains crystal copper sulphate after cooling, stays in spare, and by the filter effluent collection after filter press filters pressing, carries out next step removing
Copper in waste liquid；
S3: the water that filters out collected in step S2 is added in reaction kettle, it is 1%-5% hydrazine hydrate that concentration, which is then added, and is added
Enter pH value adjustment agent, be 6.0 by the pH value adjustment for filtering out water, reaction temperature is heated to 40 degree, the reaction time is 45 minutes, system
Standby to obtain copper, chemical equation is as follows:
2Cu2++N2H4·H2O+4OH-→2Cu↓+N2+5H2O；
S4: weighing copper sulfate crystal in step S2, is added in distilled water, the copper-bath of 0.25mol/L is configured to, in sulfuric acid
It is slowly stirred lower addition ammonium hydroxide in copper solution, then mixed liquor is put into processor for ultrasonic wave, barium hydroxide, In are added by several times
Power per liter density is ultrasonic treatment 4 hours under 1.2W/cm2, and the four ammino copper complex solution of hydroxide of blue is prepared,
Chemical equation is as follows:
S5: being added distilled water in ultrasonic treatment chamber, and water temperature controls the ultrasound vibration for applying that sound intensity degree is 0.60W/cm2 at 45 degree
Dynamic, then the four ammino copper complex solution of hydroxide in step S4 disposably in the distilled water of falling people, give birth to by reaction time 2-3 minute
Au bleu Kocide SD precipitating, it is ammonia scrubbing sediment 2-3 times of 9.0 that pH value is used after extraction filtering, then is washed with dehydrated alcohol
It washs sediment 2 times, is dried under 55 degree to constant weight after filtering, obtain blue amorphous nano powder Kocide SD, chemistry is anti-
Answer equation as follows:
Cu(NH3)6(OH)2→Cu2++6NH3↑+2OH-
Cu2++2OH-→Cu(OH)2↓。
3. a kind of Kocide SD preparation method of alkaline etching liquid according to claim 2, it is characterised in that: the step
The copper content of S1 neutral and alkali etching solution is 120-180g/L, and the copper content of acidic etching liquid is 120-160g/ in the step S1
L。
4. a kind of Kocide SD preparation method of alkaline etching liquid according to claim 2, it is characterised in that: the step
Copper content after filtering out water and hydration hydrazine reaction in S3 should be less than 0.2g/L.
5. a kind of Kocide SD preparation method of alkaline etching liquid according to claim 2, it is characterised in that: the step
The concentration of copper sulfate crystal and distilled water ratio is 65g/L in S4, and the concentration of ammonium hydroxide is 8mol/L in step S4.
6. a kind of Kocide SD preparation method of alkaline etching liquid according to claim 2, it is characterised in that: the step
The quality of barium hydroxide is added in S4 every time no more than 10g.
7. a kind of Kocide SD preparation method of alkaline etching liquid according to claim 2, it is characterised in that: the step
It is filtered with the sediment that dehydrated alcohol washs using sand core funnel in S5.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111792667A (en) * | 2020-05-25 | 2020-10-20 | 先导薄膜材料有限公司 | Preparation method of hydroxide nano powder |
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