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CN112593261A - Gold foil manufacturing method - Google Patents

Gold foil manufacturing method Download PDF

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Publication number
CN112593261A
CN112593261A CN202011440815.3A CN202011440815A CN112593261A CN 112593261 A CN112593261 A CN 112593261A CN 202011440815 A CN202011440815 A CN 202011440815A CN 112593261 A CN112593261 A CN 112593261A
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CN
China
Prior art keywords
gold
copper foil
foil substrate
substrate
foil
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CN202011440815.3A
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Chinese (zh)
Inventor
李凯成
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Shenzhen Runfujin Technology Development Co ltd
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Shenzhen Runfujin Technology Development Co ltd
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Priority to CN202011440815.3A priority Critical patent/CN112593261A/en
Publication of CN112593261A publication Critical patent/CN112593261A/en
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D1/00Electroforming
    • C25D1/04Wires; Strips; Foils
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00Processes for servicing or operating cells for electrolytic coating
    • C25D21/12Process control or regulation
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/48Electroplating: Baths therefor from solutions of gold
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00Electroplating characterised by the article coated
    • C25D7/06Wires; Strips; Foils
    • C25D7/0614Strips or foils

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Automation & Control Theory (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention discloses a gold foil manufacturing scheme, which comprises the following steps: dissolving a gold raw material in aqua regia, and washing and filtering to obtain gold water; adding gold water into the electrolyte, and attaching gold ions to a copper foil substrate of the cathode in an electrolysis mode to form a gold foil layer; and taking out the copper foil substrate attached with the gold foil layer, and stripping the copper foil substrate by nitric acid or sulfuric acid to obtain the gold foil. The invention can obtain a gold foil layer with uniform thickness by making gold ions adhere to the copper foil substrate in an electrolytic way, and then control the thickness of the gold foil layer adhered to the copper foil substrate.

Description

Gold foil manufacturing method
Technical Field
The invention relates to the technical field of gold foil processing, in particular to a gold foil manufacturing method.
Background
The gold foil is a thin sheet made of gold, the existing gold foil production mostly adopts a physical processing method, generally a mechanical forging method and a manual forging method, the mechanical method is to roll the gold foil by using a rolling mill, and the defect is that the minimum thickness of the rolled gold foil can only reach 0.02mm, and the requirement of thin gold foil in the industry and the food industry can not be met; the gold foil produced by hand has a non-uniform thickness and a low productivity. The thickness of the gold foil produced by the traditional manufacturing method is not uniformly controlled, and the minimum limit value of the thickness of the product is larger.
Disclosure of Invention
In view of this, the invention discloses a method for manufacturing gold foil, which can manufacture gold foil with uniform thickness and small thickness by a chemical method.
The invention discloses a gold foil manufacturing method, which comprises the following steps:
s1, placing the gold raw material in aqua regia for dissolving, and washing and filtering to obtain gold water;
s2, adding the gold water into the electrolyte, and attaching gold ions to the copper foil substrate of the cathode in an electrolysis mode to form a gold foil layer;
s3, taking out the copper foil substrate with the gold foil layer, and stripping the copper foil substrate by nitric acid or sulfuric acid to obtain the gold foil.
Further, the step S1 specifically includes:
s11, pressing the gold raw material into a gold sheet with a certain thickness by using a piece pressing device;
s12, cutting the pressed gold sheet;
and S13, placing the cut gold sheet into aqua regia for dissolving, and then washing and filtering to obtain the gold liquid.
Further, the step S13 specifically includes:
s131, transferring the gold thin sheet into a reaction kettle, adding aqua regia into the reaction kettle, and carrying out water bath reaction for 1-3H at the water bath reaction temperature of 60-100 ℃;
s132, after the gold thin sheet is completely reacted, adding ultrapure water with a corresponding volume, and naturally cooling for 1-3H;
s133, after cooling, adding strong ammonia water into the reaction kettle to adjust the pH value of the solution to 8-10, and generating yellow precipitate;
s134, taking out the neutralized solution, washing and filtering for 1-3 times under the vacuum filtration condition, and washing ionic substances remained in the precipitate to obtain yellow precipitate;
and S135, transferring the yellow precipitate into a complexing solution with the constant temperature of 65-75 ℃, stirring to dissolve the yellow precipitate, and cooling to obtain the required gold water.
Further, in step S2, the maximum width of the copper foil base material is 50 CM.
Further, in step S2, the thickness of gold ions attached to the copper foil is controlled by controlling the current level and the electrolysis time; the current density in the electrolyte is 0.05-0.2ASD, the electrolysis time is 30-60min, and a gold foil layer with the thickness of 1-3 mu m can be obtained.
Further, the step S3 specifically includes:
s31, taking out the copper foil substrate attached with the gold foil layer, and slitting the copper foil substrate by slitting equipment;
and S32, placing the copper foil substrate with the gold foil layer after cutting in nitric acid or sulfuric acid to strip the copper foil substrate to obtain the gold foil.
Furthermore, a shielding film is attached to one side surface of the gold foil substrate, and the gold foil layer is attached to the other side surface of the copper foil substrate.
Further, the purity of the gold raw material is 99.99%.
Compared with the prior art, the technical scheme disclosed by the invention has the beneficial effects that:
the gold ions are attached to the copper foil substrate in an electrolytic mode, a gold foil layer with uniform thickness is formed on the copper foil substrate, and the gold foil layer with uniform thickness is obtained after the copper foil substrate is stripped; the thickness of the gold foil layer is controlled by controlling the current and the electrolysis time, so that the gold foil with smaller thickness can be obtained compared with a physical method, and the processing efficiency can be improved.
Drawings
FIG. 1 is a general flow chart of gold foil fabrication;
fig. 2 is a detailed flowchart of step S1;
fig. 3 is a detailed flowchart of step S13;
FIG. 4 is a table of data for examples 1 to 4;
FIG. 5 is a table of data for examples 5 to 10.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention discloses a gold foil manufacturing method, which can obtain a gold foil with uniform thickness and thinner thickness by a chemical manufacturing mode.
As shown in fig. 1, the method specifically comprises the following steps:
s1, placing the gold raw material in aqua regia for dissolving, and washing and filtering to obtain gold water;
s2, adding the gold water into the electrolyte, and attaching gold ions to the copper foil substrate of the cathode in an electrolysis mode to form a gold foil layer;
s3, taking out the copper foil substrate with the gold foil layer, and stripping the copper foil substrate by nitric acid or sulfuric acid to obtain the gold foil.
Wherein, the purity of the gold raw material adopted in the step S1 is 99.99%. The aqua regia is a mixed solution of hydrochloric acid and nitric acid in a certain proportion, and can dissolve the gold raw material. For example, aqua regia dissolves gold raw materials,
when the weight of the gold raw material is 1kg, the amounts of nitric acid and hydrochloric acid are 0.8-1.0L and 2.0-2.5L, preferably, the amounts of nitric acid and hydrochloric acid are 0.9L and 2.5L;
when the weight of the gold raw material is 2kg, the amounts of nitric acid and hydrochloric acid are preferably 1.6L and 5.2L;
when the weight of the gold raw material is 3kg, the amounts of nitric acid and hydrochloric acid are preferably 2.5L and 7.5L.
As shown in fig. 2, the step S1 specifically includes:
s11, pressing the gold raw material into a gold sheet with a certain thickness by using a piece pressing device;
s12, cutting the pressed gold sheet;
and S13, placing the cut gold sheet into aqua regia for dissolving, and then washing and filtering to obtain the gold liquid.
And pressing the gold raw material into a sheet with a certain thickness, so that the gold raw material is conveniently dissolved by using aqua regia. Furthermore, the gold raw material is generally pressed into a thin sheet with the thickness of 0.02MM-0.1MM, and the dissolution speed of the gold raw material in aqua regia can be improved compared with the whole gold raw material.
The pressed gold sheet is cut, and the size of the gold sheet can be controlled to control the dissolving speed of the gold sheet in the aqua regia.
As shown in fig. 3, in the above operation steps, the step S13 specifically includes:
s131, transferring the gold thin sheet into a reaction kettle, adding aqua regia into the reaction kettle, and carrying out water bath reaction for 1-3H at the water bath reaction temperature of 60-100 ℃;
s132, after the gold thin sheet is completely reacted, adding ultrapure water with a corresponding volume, and naturally cooling for 1-3H;
s133, after cooling, adding strong ammonia water into the reaction kettle to adjust the pH value of the solution to 8-10, and generating yellow precipitate;
s134, taking out the neutralized solution, washing and filtering for 1-3 times under the vacuum filtration condition, and washing ionic substances remained in the precipitate to obtain yellow precipitate;
and S135, transferring the yellow precipitate into a complexing solution with the constant temperature of 65-75 ℃, stirring to dissolve the yellow precipitate, and cooling to obtain the required gold water.
Wherein, after the gold thin slice is completely dissolved in the aqua regia, the ultrapure water is added into the mixed solution after the gold thin slice is dissolved for neutralizing the acidity of the mixed solution, and the strong reaction after adding the concentrated ammonia water in the next step is prevented.
Adding strong ammonia water into the mixed solution dissolved with the gold flakes to make the pH value reach 8-10, and then greatly separating out gold ions in the mixed solution to form yellow precipitates. And the strong ammonia water is required to be slowly added when being added, so that a violent reaction is prevented.
And then, obtaining yellow precipitate, namely gold mud, in a vacuum filtration mode. Further, the gold mud is cleaned and filtered for 3 times or 5 times under the vacuum filtering condition, and ionic substances remained in the sediment are cleaned to obtain mud-shaped yellow sediment, so that the gold mud impurities after cleaning are less.
And adding the obtained yellow precipitate into the complexing solution, dissolving the yellow precipitate in the complexing solution to form gold water, placing the formed gold water into an electrolyte, and attaching gold ions to a cathode in an electrolytic manner.
In the first embodiment of the present invention,
(1) pressing 1.000Kg of gold raw material into slices, and cutting the pressed slices into gold slices of 3 x 3cm-3 x 5 cm;
(2) transferring the gold slices into a reaction kettle, and performing reaction according to the ratio of gold: nitric acid: adding nitric acid and hydrochloric acid according to the proportion of 1Kg to 0.8L to 2.4L of hydrochloric acid, and reacting in a water bath at the water bath reaction temperature of 80 ℃ for 1H;
(3) after the reaction of the gold thin sheet is completed, adding 3.2L of ultrapure water, and naturally cooling for 1H;
(4) after cooling, slowly adding strong ammonia water into the reaction kettle to adjust the pH value of the solution to 10, wherein a large amount of yellow precipitates appear;
(5) and (3) discharging the neutralized solution, washing and filtering for 2 times under the vacuum filtration condition, and washing ionic substances remained in the precipitate as clean as possible to obtain 0.995kg of mud-shaped yellow precipitate.
In the second embodiment of the present invention,
(1) pressing 2.000Kg of gold raw material into slices, and cutting the pressed slices into gold slices of 3 x 3cm-3 x 5 cm;
(2) transferring the gold slices into a reaction kettle, and performing reaction according to the ratio of gold: nitric acid: adding nitric acid and hydrochloric acid according to the proportion of 2Kg to 1.6L to 5.2L of hydrochloric acid, and reacting in a water bath at the water bath reaction temperature of 75 ℃ for 2H;
(3) after the reaction of the gold thin sheet is completed, adding 7.0L of ultrapure water, and naturally cooling for 1.5H;
(4) after cooling, slowly adding strong ammonia water into the reaction kettle to adjust the pH value of the solution to 9.5, wherein a large amount of yellow precipitates appear;
(5) and (3) discharging the neutralized solution, washing and filtering for 3 times under the vacuum filtration condition, and washing ionic substances remained in the precipitate as clean as possible to obtain 1.984kg of mud-shaped yellow precipitate.
In the third embodiment of the present invention,
(1) pressing 3.000Kg of gold raw material into slices, and cutting the pressed slices into 3 x 3cm-3 x 5cm gold slices;
(2) transferring the gold slices into a reaction kettle, and performing reaction according to the ratio of gold: nitric acid: adding nitric acid and hydrochloric acid according to the proportion of 3Kg to 2.5L to 7.5L of hydrochloric acid, and reacting in a water bath at the water bath reaction temperature of 75 ℃ for 2H;
(3) after the reaction of the gold thin sheet is completed, 10.0L of ultrapure water is added, and natural cooling is carried out for 1.0H;
(4) after cooling, slowly adding strong ammonia water into the reaction kettle to adjust the pH value of the solution to 10.0, and then, a large amount of yellow precipitates appear;
(5) discharging the neutralized solution, washing and filtering for 3 times under vacuum filtration condition, and washing ionic substances remained in the precipitate as clean as possible to obtain 2.967kg of mud-like yellow precipitate;
in the fourth embodiment of the present invention,
(1) pressing 4.000Kg of gold raw material into slices, and cutting the pressed slices into gold slices of 3 x 3cm-3 x 5 cm;
(2) transferring the gold slices into a reaction kettle, and performing reaction according to the ratio of gold: nitric acid: adding nitric acid and hydrochloric acid according to the proportion of 3Kg to 3.5L to 10.5L of hydrochloric acid, and reacting in a water bath at the water bath reaction temperature of 70 ℃ for 2H;
(3) after the gold plate is completely reacted, adding 15.0L of ultrapure water, and naturally cooling for 1.0H;
(4) after cooling, slowly adding strong ammonia water into the reaction kettle to adjust the pH value of the solution to 9.8, wherein a large amount of yellow precipitates appear;
(5) discharging the neutralized solution, washing and filtering for 3 times under the vacuum filtration condition, and washing ionic substances remained in the precipitate as clean as possible to obtain 3.952kg of mud-like yellow precipitate;
in step S2, the cathode in the electrolyte is made of copper foil, and when electricity is applied, gold ions in the electrolyte can be dissociated to the cathode and attached to the outer surface of the copper foil substrate to form a gold foil layer. The gold foil layer is formed on the outer surface of the copper foil substrate in an electrolysis mode, so that the thickness of the gold foil layer is uniform, the thickness of the gold foil can be controlled according to the attachment amount of gold ions outside the copper foil substrate, and compared with a physical processing mode, the gold foil with smaller thickness can be obtained.
In this embodiment, a shielding film is attached to one side surface of the copper foil substrate, so that gold ions can only be attached to the side surface of the copper foil substrate to which the shielding film is not attached, and a gold foil layer is formed on the side surface, thereby facilitating the later peeling of the copper foil substrate. The shielding film can be a PET film.
Furthermore, under the condition of a certain electrolyte, the thickness of gold ions attached to the copper foil substrate can be controlled by controlling the current and the electrolysis time. The speed of gold ions moving to the cathode is controlled by changing the current density in the electrolyte, and the thickness of the gold ions attached to the copper foil substrate is controlled by adjusting the electrolysis time.
Generally, the current density in the electrolyte is 0.05-0.2ASD, the electrolysis time is 30-60min, and a gold foil layer with the thickness of 1-3 μm can be obtained.
In a fifth example, the current density was 0.05ADS, the electrolysis time was 30min, and the thickness of the gold foil layer attached to the copper foil substrate was 1 μm.
In the sixth embodiment, the current density was 0.08ADS, the electrolysis time was 40min, and the thickness of the gold foil layer attached to the copper foil substrate was 1.4 μm.
In the seventh example, the current density was 0.05ADS, the electrolysis time was 40min, and the thickness of the gold foil layer attached to the copper foil substrate was 1.15 μm.
In the eighth embodiment, the current density was 0.1ADS, the electrolysis time was 45min, and the thickness of the gold foil layer attached to the copper foil substrate was 2 μm.
In the ninth embodiment, the current density was 0.2ADS, the electrolysis time was 50min, and the thickness of the gold foil layer attached to the copper foil substrate was 2.65 μm.
In the tenth embodiment, the current density was 0.2ADS, the electrolysis time was 60min, and the thickness of the gold foil layer attached to the copper foil substrate was 3 μm.
Further, the step S3 specifically includes:
s31, taking out the copper foil substrate attached with the gold foil layer, and slitting the copper foil substrate by slitting equipment;
and S32, placing the copper foil substrate with the gold foil layer after cutting in nitric acid or sulfuric acid to strip the copper foil substrate to obtain the gold foil.
Wherein, earlier cut the copper foil substrate that has the gold foil layer to adhering to through cutting equipment before peeling off the copper foil substrate, obtain required corresponding size, cut thinner gold foil for alone, operate more easily. And after cutting, putting the copper foil substrate with the gold foil layer into nitric acid or sulfuric acid, and dissolving the copper foil substrate to obtain the processed gold foil.
Before the gold foil is cut, the shielding film attached to the copper foil substrate needs to be taken down, then the copper foil substrate is cut and put into nitric acid or sulfuric acid to be dissolved to form the gold foil.
After the gold foil is obtained, the gold foil is sandwiched between two copy sheets, the gold foil is taken out from the copy sheets, and the copy sheets and the gold foil are collectively put into respective storage containers.
The present invention may be embodied in many different forms and modifications without departing from the spirit and scope of the present invention, and the above-described embodiments are intended to illustrate the present invention but not to limit the scope of the present invention.

Claims (8)

1. A method for manufacturing gold foil is characterized by comprising the following steps:
s1, placing the gold raw material in aqua regia for dissolving, and washing and filtering to obtain gold water;
s2, adding the gold water into the electrolyte, and attaching gold ions to the copper foil substrate of the cathode in an electrolysis mode to form a gold foil layer;
s3, taking out the copper foil substrate with the gold foil layer, and stripping the copper foil substrate by nitric acid or sulfuric acid to obtain the gold foil.
2. The method for manufacturing gold foil according to claim 1, wherein the step S1 specifically includes:
s11, pressing the gold raw material into a gold sheet with a certain thickness by using a piece pressing device;
s12, cutting the pressed gold sheet;
and S13, placing the cut gold sheet into aqua regia for dissolving, and then washing and filtering to obtain the gold liquid.
3. The method for manufacturing gold foil according to claim 2, wherein the step S13 specifically includes:
s131, transferring the gold thin sheet into a reaction kettle, adding aqua regia into the reaction kettle, and carrying out water bath reaction for 1-3H at the water bath reaction temperature of 60-100 ℃;
s132, after the gold thin sheet is completely reacted, adding ultrapure water with a corresponding volume, and naturally cooling for 1-3H;
s133, after cooling, adding strong ammonia water into the reaction kettle to adjust the pH value of the solution to 8-10, and generating yellow precipitate;
s134, taking out the neutralized solution, washing and filtering for 1-3 times under the vacuum filtration condition, and washing ionic substances remained in the precipitate to obtain yellow precipitate;
and S135, transferring the yellow precipitate into a complexing solution with the constant temperature of 65-75 ℃, stirring to dissolve the yellow precipitate, and cooling to obtain the required gold water.
4. The method of claim 1, wherein the maximum width of the copper foil substrate in step S2 is 50 CM.
5. The method of claim 1, wherein in step S2, the thickness of gold ions attached to the copper foil is controlled by controlling the current and the electrolysis time; the current density in the electrolyte is 0.05-0.2ASD, the electrolysis time is 30-60min, and a gold foil layer with the thickness of 1-3 mu m can be obtained.
6. The method for manufacturing gold foil according to claim 1, wherein the step S3 specifically includes:
s31, taking out the copper foil substrate attached with the gold foil layer, and slitting the copper foil substrate by slitting equipment;
and S32, placing the copper foil substrate with the gold foil layer after cutting in nitric acid or sulfuric acid to strip the copper foil substrate to obtain the gold foil.
7. The method of claim 6, wherein a shielding film is attached to one side of the gold foil substrate and the gold foil layer is attached to the other side of the copper foil substrate.
8. A method of manufacturing gold foil according to any one of claims 1 to 7 wherein the gold source has a purity of 99.99%.
CN202011440815.3A 2020-12-08 2020-12-08 Gold foil manufacturing method Pending CN112593261A (en)

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Application Number Priority Date Filing Date Title
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1214430A (en) * 1981-12-04 1986-11-25 Arnold F. Griffin Gold recovery in fractionating column containing particulate absorbent using organic liquid
JPH09155441A (en) * 1995-11-29 1997-06-17 Mitsubishi Materials Corp Manufacture of gold foil
CN1240240A (en) * 1998-06-23 2000-01-05 陈希龙 Technology for making gold foil
CN104928488A (en) * 2015-06-17 2015-09-23 郴州市金贵银业股份有限公司 Gold-bearing aqua regia gold extraction method
CN108728873A (en) * 2018-06-20 2018-11-02 深圳市金宝盈文化股份有限公司 A kind of production method of casting gold process product

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1214430A (en) * 1981-12-04 1986-11-25 Arnold F. Griffin Gold recovery in fractionating column containing particulate absorbent using organic liquid
JPH09155441A (en) * 1995-11-29 1997-06-17 Mitsubishi Materials Corp Manufacture of gold foil
CN1240240A (en) * 1998-06-23 2000-01-05 陈希龙 Technology for making gold foil
CN104928488A (en) * 2015-06-17 2015-09-23 郴州市金贵银业股份有限公司 Gold-bearing aqua regia gold extraction method
CN108728873A (en) * 2018-06-20 2018-11-02 深圳市金宝盈文化股份有限公司 A kind of production method of casting gold process product

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
巴尔特尔等: "《金属表面化学及电化学加工工艺学》", 31 August 1965, 国防工业出版社, *
曾华梁等: "《电镀工艺手册》", 30 August 1997, 机械工业出版社 *
韩长日等: "《精细化工品实用生产技术手册 电子与信息化学品制造技术》", 31 October 2001, 科学技术文献出版社 *

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Application publication date: 20210402