CN110607539A - Processing technology of gold jewelry - Google Patents
Processing technology of gold jewelry Download PDFInfo
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- CN110607539A CN110607539A CN201910936426.0A CN201910936426A CN110607539A CN 110607539 A CN110607539 A CN 110607539A CN 201910936426 A CN201910936426 A CN 201910936426A CN 110607539 A CN110607539 A CN 110607539A
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- A—HUMAN NECESSITIES
- A44—HABERDASHERY; JEWELLERY
- A44C—PERSONAL ADORNMENTS, e.g. JEWELLERY; COINS
- A44C27/00—Making jewellery or other personal adornments
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G7/00—Compounds of gold
- C01G7/006—Compounds containing, besides gold, two or more other elements, with the exception of oxygen or hydrogen
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D1/00—Electroforming
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D1/00—Electroforming
- C25D1/20—Separation of the formed objects from the electrodes with no destruction of said electrodes
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/48—Electroplating: Baths therefor from solutions of gold
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- Manufacturing & Machinery (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
The invention discloses a processing technology of gold jewelry, and relates to the technical field of jewelry processing. The processing technology of the gold jewelry comprises the following steps: s1, tabletting; s2, melting; s3, nitrate removal; s4, exhausting; s5, washing chlorine; s6, preparing gold sodium sulfite; s7, adjusting the pH value; s8, adjusting stability; s9, preparing a blank and casting a die; s10, electroplating: during electroplating, a ruthenium iridium titanium network is selected as an anode, and the electroplating solution comprises the following components in mass concentration: 20-50g/L of the electroforming solution prepared in the step S8, 25-45g/L of a cylinder opening agent, 40-100g/L of a complexing agent, 20-70g/L of a hardening agent and 30-50g/L of a brightening agent; and S11, demolding. The processing technology of the gold jewelry adopts a cyanide-free production technology, has good product toughness, is not easy to break, has light weight and high hardness, and has advanced technology, so that the manufactured gold jewelry has the advantages of high hardness, good wear resistance, high glossiness and lasting glossiness.
Description
Technical Field
The invention relates to the technical field of jewelry processing, in particular to a processing technology of gold jewelry.
Background
With the continuous improvement of living standard of people, people wear ornaments more and more, and its purpose is not merely the value-retaining, but rather more tend to decorate, this makes the ornament market follow the requirement that noble metal such as single use diamond, gold satisfies user's value-retaining, changes to using the cheaper alloy of many varieties, manifold type, can better satisfy the demand direction that the user updated to seek different.
When people wear the gold jewelry, the gold can absorb toxins of human skin or interact with sweat on the skin to blacken and yellow, meanwhile, the gold can also react with mercury in cosmetics and sulfur in the air to blacken, when the gold and platinum rub against each other, platinum can be rubbed on the surface of the gold to whiten, and the gold loses metallic luster to influence the decorative value of the gold; when people wear the silver jewelry, besides silver can be oxidized by external environment, the surface smoothness of the silver jewelry is not enough, and the oxidation of the surface of the silver jewelry is accelerated, so that the silver jewelry loses metallic luster, and the decorative value of the jewelry is further influenced. In addition, the higher the purity of gold and silver, the higher their softness and lower their abrasion resistance, and when people wear these jewelry, the quality of gold and silver will slowly decrease during long-term scratching, thus causing economic loss to the owner.
The electroplating is a relatively complex process, which not only has the function of protecting the metal surface of the jewelry, but also can make the surface of the metal jewelry more beautiful. Although the process of gold potassium cyanide is low in cost and high in efficiency, and the problem of the hypertoxicity of cyanide is irreversible harm to the environment, the process of replacing the gold potassium cyanide with the sodium gold sulfite is gradually popular, but the gold electroplating by the sodium gold sulfite is unstable.
Therefore, the problem to be solved is to develop a gold jewelry which is processed by cyanide-free electroplating and has good wear resistance, high glossiness and good stability.
Disclosure of Invention
Aiming at the defects in the prior art, the first purpose of the invention is to provide a processing technology of gold jewelry, which has the advantages of high hardness, good wear resistance and high glossiness of the made gold jewelry.
In order to achieve the first object, the invention provides the following technical scheme: a processing technology of gold jewelry is characterized by comprising the following steps:
s1, tabletting: pressing 2kg of gold blocks into square gold sheets with the length and width of 0.15 +/-0.05 mm;
s2, melting: putting the square gold flakes into the king water, and gradually dropwise adding concentrated nitric acid until the mass ratio of the concentrated hydrochloric acid to the concentrated nitric acid is 1: 5;
s3, nitrate removal: continuously adding concentrated hydrochloric acid into the mixed solution of the concentrated hydrochloric acid and the concentrated nitric acid, heating to 78-82 ℃, and adding the concentrated hydrochloric acid until the mixed solution does not produce yellow flue gas any more;
s4, exhaust: pouring the mixed solution into a reaction kettle, cooling, slowly adding concentrated ammonia water for 1-2h, and exhausting while adding;
s5, chlorine washing: carrying out vacuum filtration on the mixed solution obtained in the step S4, and washing filter residues for 8 times by using warm water at 60 ℃;
s6, preparing gold sodium sulfite: adding filter residue into a reaction kettle, adding anhydrous sodium sulfite, heating in water bath to 60-70 ℃, stirring for 6-7h, adding dilute sulfuric acid with the mass concentration of 2% twice while stirring, wherein the adding amount of each time is 100ml, the adding interval time of the two times is 15-18min, heating to 90-95 ℃, and stirring for 3-4h;
s7, adjusting pH: taking liquid in the reaction kettle, and adjusting the pH value to 10 by using dilute sulfuric acid or potassium hydroxide;
s8, stability regulation: naturally cooling the liquid in the reaction kettle to 55-60 ℃, adding a stabilizer, uniformly stirring, cooling to 25-30 ℃, and filtering to obtain an electroforming liquid, wherein the mass ratio of the stabilizer to the liquid in the reaction kettle is 0.1-0.3: 1;
s9, blank making and mold casting: melting the tin-bismuth alloy, pouring into a mold, carrying out surface activation treatment on the mold, putting the mold into a copper acid cylinder, and electroplating on the mold to form a copper layer;
s10, electroplating: carrying out surface activation treatment on the mold with the copper layer, putting the mold into electroplating solution with the gold content of 10-16g/L, and electroplating to form a gold layer on the copper layer to obtain a semi-finished product;
during electroplating, a ruthenium iridium titanium network is selected as an anode, and the electroplating solution comprises the following components in mass concentration: 20-50g/L of the electroforming solution prepared in the step S8, 25-45g/L of a cylinder opening agent, 40-100g/L of a complexing agent, 20-70g/L of a hardening agent and 30-50g/L of a brightening agent;
s11, demolding: punching at least two convection holes on the semi-finished product, penetrating the convection holes through the gold layer and the copper layer, placing the semi-finished product in an oven at the temperature of 130-180 ℃, heating while performing centrifugal treatment, placing the semi-finished product in a nitric acid solution, boiling for 20-30min, and washing for 3-5 times with clear water.
By adopting the technical scheme, as aqua regia is adopted to melt gold lumps, and concentrated nitric acid is slowly added into concentrated hydrochloric acid, the melting process can be slowed down, so that the gold lumps are slowly dissolved, excessive hydrochloric acid is added and heated, nitric oxide gas generated by the thermal reaction of nitrate ions escapes, so that the nitrate ions are removed, then concentrated ammonia water is added into liquid without the nitrate ions to react to prepare the gold fulminate, the gold fulminate is washed by warm water to remove chloride ions therein, the influence of the chloride ions on the brightness of the gold jewelry is reduced, the corrosion of the chloride ions on an electroplating cylinder is reduced, anhydrous sodium sulfite is added to react with the gold fulminate to prepare the gold sodium sulfite, and a stabilizer is added, so that the stability of the gold sodium sulfite in the electroplating solution can be improved, the electroplating process can be stably carried out, and the hardness and the brightness of the gold jewelry can be improved.
Pouring a mould with a tin-bismuth alloy, carrying out surface activation treatment on the mould, removing impurities on the surface of the mould, electroplating copper on the mould, wherein a copper layer can be filled on the surface of the mould to ensure that the surface of the mould is smooth, carrying out surface activation treatment on the mould plated with the copper layer to remove oil stains on the surface of the copper layer and enhance the adhesion between the gold layer and the copper layer, putting a semi-finished product plated with the gold layer into an oven for heating, melting the mould made of the tin-bismuth alloy by heating, throwing the molten tin-bismuth alloy out of a convection hole during centrifugation, putting the semi-finished product into nitric acid, and melting the copper layer in the gold layer by the nitric acid to remove the copper layer, thereby preparing the gold jewelry.
During electroplating, the cylinder opening agent can quickly emit light, has higher filling degree and brightness, prevents a plating layer from generating pinholes, pockmarks and white fog, improves the hardness and the anti-corrosion capability of the plating layer, improves the hardness of the electroplated gold jewelry by using the hardening agent, enhances the brightness of the gold jewelry by using the brightening agent, ensures that the brightness of the gold jewelry has better durability, ensures that a product has good toughness, is not easy to break, and has light weight, high hardness and advanced process.
Further, the stabilizer is sodium hypophosphite, chromium nitrate and anhydrous sodium sulfite in a mass ratio of (0.4-0.8) to (0.3-0.7) to (0.1-0.3).
By adopting the technical scheme, the sodium hypophosphite is not easy to precipitate, the stability is high, the dispersity and the covering capacity of the chromium nitrate are high, the brightness is good, and the chromium nitrate can be fully dispersed in the gold sodium sulfite under the coordination of the anhydrous sodium sulfite, so that the stability of the gold sodium sulfite is improved, and the hardness and the brightness of a gold-plated layer are enhanced.
Further, the complexing agent is prepared by mixing potassium citrate, chloride, phosphate and hydrogen phosphate according to the mass ratio of 1 (0.2-0.5) to (0.3-0.6) to (0.1-0.5).
By adopting the technical scheme, the potassium citrate is an auxiliary complexing agent of gold, gold citrate complex ions are generated in the electroplating solution, the stability of the electroplating solution is facilitated, the chloride can improve the conductivity and the cathode current density of the electroplating solution and improve the deposition speed of gold, and the phosphate and the hydrogen phosphate are conductive salt and a pH buffering agent, so that the pH value of the electroplating solution can be kept, and the sulfite is prevented from being decomposed due to the change of the pH value.
Further, the chloride is one or more of sodium chloride, hydrogen chloride, potassium chloride and ammonium chloride; the phosphate is one or the combination of potassium phosphate and sodium phosphate; the hydrogen phosphate is one or more of potassium dihydrogen phosphate, sodium hydrogen phosphate and potassium hydrogen phosphate.
Further, the hardening agent is antimony salt, selenium salt and potassium tartrate with the mass ratio of 0.25-1:0.8-1.2: 1.1-1.3; the antimonic salt is one or a composition of more of sodium antimonate tartrate, potassium antimonate, sodium antimonate and potassium antimonate, and the selenium salt is one or a composition of more of sodium selenosulfate, potassium selenosulfate, sodium selenite and potassium selenite.
By adopting the technical scheme, the stibium salt, the selenium salt and the potassium tartrate can enhance the hardness of the gold jewelry and can enhance the oxidation resistance and the discoloration resistance of the gold jewelry.
Further, the brightener is prepared by the following method: using 1.5-1.8 weight portions of distilled hydrosolvent saccharin sodium with 70-80 ℃, deionizing 0.5-0.8 weight portion, heating to 50-60 ℃, adding 0.1-0.3 weight portion of glucose while stirring, adding saccharin sodium dissolved in distilled water in advance, stirring strongly, adding 0.4-0.9 weight portion of cobalt sulfate and 0.2-0.5 weight portion of nickel sulfate, supplementing 0.5-1 weight portion of distilled water, adding 0.08-0.12 weight portion of 1, 3-propanediamine hydrazinodithioformamide, and stirring uniformly to obtain the brightener.
By adopting the technical scheme, the cobalt nickel layer can be formed by cobalt sulfate and nickel sulfate under the action of current density, the coating is bright, fine, high in hardness and good in abrasion resistance under an alkaline condition, and the tension of the cobalt nickel layer can be reduced under the action of 1, 3-propane diamine hydrazinodithioformamide, so that the coating has ductility, grain refinement and improved glossiness.
Further, the surface activation processing in step S9 and step S10 includes the steps of: (1) carrying out ultrasonic cleaning on the die, wherein the frequency is 30-40KHz, and the cleaning time is 20-30 min; (2) putting the die into deoiling liquid for electrolytic deoiling, keeping the voltage at 6V, the temperature at 25-30 ℃, and the time at 30-120 s; (3) placing the mold into dilute sulfuric acid, heating to boil, maintaining for 10-20min, and washing with deionized water for 1-2 min.
By adopting the technical scheme, the mould is cleaned by ultrasonic waves to remove oil stains on the surface, so that the copper layer is tightly attached to the mould, the copper layer can be filled in the surface of the mould to ensure that the surface of the mould is smooth and flat, then dilute sulfuric acid is used for removing surface oxides, and deionized water is used for cleaning, so that the mould with a smooth and clean surface is prepared; ultrasonic cleaning, electrolytic degreasing and dilute sulfuric acid cleaning are carried out on the die plated with the copper layer, oil stains and oxides on the surface of the copper layer can be removed, and the influence of impurities on the brightness of the gold layer is reduced.
Further, the deoiling liquid is prepared by mixing the following components in parts by weight: 10-20 parts of electrolytic powder, 4-6 parts of sodium carbonate, 20-25 parts of trisodium phosphate, 1-2 parts of sodium benzoate and 3-4 parts of penetrating agent.
By adopting the technical scheme, the degreasing liquid is prepared by mixing the electrolytic powder and sodium carbonate and other substances, and can quickly remove oil stains on the surfaces of the die and the copper-plated die.
Further, the pH value of the electroplating solution is 6.5-7.5, the electroplating time is 8-20h, and the current density is 0.6-1A/dm2The temperature of the electroplating solution is 40-60 ℃.
By adopting the technical scheme, the pH value of the electroplating solution is adjusted to 6.5-7.5, the temperature of the electroplating solution is controlled to be 40-60 ℃, the stability of the electroplating process can be improved, and the electroplating can be stably carried out.
Further, after the washing in the step S5, 1-2mg of filter residue is taken and put into silver nitrate solution, whether the precipitate is generated or not is observed, and if the precipitate is generated, the washing is continued with warm water of 60 ℃ until the precipitate is not generated any more.
By adopting the technical scheme, the chlorine ions in the filter residue can be washed by warm water, and the silver nitrate solution is used for detecting whether the filter residue contains the chlorine ions, if white precipitate occurs, the chlorine ions are proved not to be removed, the filter residue is continuously washed by the warm water, and if no white precipitate occurs, the next step of operation is continued, so that the operation is simple and convenient, and the observation is convenient.
In conclusion, the invention has the following beneficial effects:
firstly, because the gold block is dissolved, and the gold sodium nitrite is prepared through the operations of nitrate removal, air exhaust, chlorine washing and the like, and the cylinder opening agent, the complexing agent, the hardening agent and the brightening agent are added to prepare the electroplating solution, the influence of impurities on the hardness and the brightness of the gold jewelry is reduced because the gold sodium nitrite is free of chloride ions, nitrate ions and cyanides, so that the brightness, the hardness and the wear resistance of the gold jewelry are enhanced.
Secondly, sodium hypophosphite, chromium nitrate and anhydrous sodium sulfite are preferably mixed to prepare the electroplating solution with good stability, and the chromium nitrate has strong dispersibility and covering capability, can assist the sodium hypophosphite to be uniformly dispersed in the sodium gold sulfite, so that the stability of the electroplating solution is further enhanced; antimony salt, selenium salt and potassium tartrate are used as hardening agents, so that the hardness and the wear resistance of the gold plating layer can be improved.
Thirdly, in the invention, cobalt sulfate, nickel sulfate and other substances are preferentially used to prepare the brightener, and as the cobalt-nickel plating layer has good brightness, fine density, high hardness and good abrasion resistance, the tension of the cobalt-nickel layer can be reduced under the action of the 1, 3-propane diamine hydrazinodithioformamide, so that the plating layer has ductility, refined grains and improved glossiness.
Detailed Description
The present invention will be described in further detail with reference to examples.
Preparation examples 1 to 3 of brightener
Preparation examples 1-3 the sodium saccharin was selected from sodium saccharin sold by Guangxi Mich export Inc. under the model GXJM-1 and the glucose was selected from glucose sold by Suzhou Deno chemical Inc. under the model RG-0040.
Preparation example 1: 1.5kg of distilled water solvent saccharin sodium at 70 ℃ is used, 0.5kg of deionized water is heated to 50 ℃, 0.1kg of glucose is added while stirring, saccharin sodium dissolved in distilled water in advance is added, strong stirring is carried out, 0.4kg of cobalt sulfate and 0.2kg of nickel sulfate are added, 0.5kg of distilled water is supplemented, 0.08kg of 1, 3-propane diamine hydrazinodithioformamide is added, and the mixture is uniformly stirred, so that the brightener is prepared.
Preparation example 2: 1.6kg of distilled water solvent saccharin sodium at 75 ℃ is used, 0.7kg of deionized water is heated to 55 ℃, 0.2kg of glucose is added while stirring, saccharin sodium dissolved in distilled water in advance is added, strong stirring is carried out, 0.7kg of cobalt sulfate and 0.3kg of nickel sulfate are added, 0.8kg of distilled water is supplemented, 0.1kg of 1, 3-propane diamine hydrazinodithioformamide is added, and the mixture is uniformly stirred, so that the brightener is prepared.
Preparation example 3: 1.8kg of distilled water solvent saccharin sodium at 80 ℃ is used, 0.8kg of deionized water is heated to 60 ℃, 0.3kg of glucose is added while stirring, saccharin sodium dissolved in distilled water in advance is added, strong stirring is carried out, 0.9kg of cobalt sulfate and 0.5kg of nickel sulfate are added, 1kg of distilled water is supplemented, 0.12kg of 1, 3-propane diamine hydrazinodithioformamide is added, and the stirring is uniform, so that the brightener is prepared.
Examples
In examples 1-3, the firing agent is selected from the firing agent sold by Huaqian surface treatment technology Limited in Shenzhen, model number WK-2081, the electrolytic powder is selected from the electrolytic powder sold by Guangzhou Shanghai trade Limited, model number CW-186, and the penetrating agent is selected from the AT-2 penetrating agent sold by Xinjiang science Limited in Shenzhen.
Example 1: a processing technology of gold jewelry comprises the following steps:
s1, tabletting: pressing 2kg of gold blocks into square gold sheets with the length and width of 0.15 mm;
s2, melting: putting the square gold flakes into the king water, and gradually dropwise adding concentrated nitric acid until the mass ratio of the concentrated hydrochloric acid to the concentrated nitric acid is 1: 5;
s3, nitrate removal: continuously adding concentrated hydrochloric acid into the mixed solution of the concentrated hydrochloric acid and the concentrated nitric acid, heating to 78 ℃, and adding the concentrated hydrochloric acid until the mixed solution does not generate yellow smoke;
s4, exhaust: pouring the mixed solution into a reaction kettle, cooling, slowly adding 25mol/L concentrated ammonia water for 1h while exhausting, wherein the amount of the concentrated ammonia water is added until no gas is discharged;
s5, chlorine washing: carrying out vacuum filtration on the mixed solution in the step S4, washing the filter residue for 8 times by using warm water at 60 ℃, taking 1mg of the filter residue after washing, putting the filter residue into a silver nitrate solution, observing whether a precipitate is generated, and if the precipitate is generated, continuously washing the filter residue by using the warm water at 60 ℃ until the precipitate is not generated any more;
s6, preparing gold sodium sulfite: adding filter residue into a reaction kettle, adding anhydrous sodium sulfite, heating in a water bath to 60 ℃, stirring for 6 hours, adding dilute sulfuric acid with the mass concentration of 2% twice while stirring, wherein the adding amount is 100ml each time, the adding interval time of the two times is 15min, heating to 90 ℃, and stirring for 4 hours;
s7, adjusting pH: taking liquid in the reaction kettle, and adjusting the pH value to 10 by using dilute sulfuric acid or potassium hydroxide, wherein the concentration of the dilute sulfuric acid is 37 percent, and the concentration of the potassium hydroxide is 1 percent;
s8, stability regulation: naturally cooling the liquid in the reaction kettle to 55 ℃, adding a stabilizer, uniformly stirring, cooling to 25 ℃, filtering to obtain an electroforming liquid, wherein the mass ratio of the stabilizer to the liquid in the reaction kettle is 0.1:1, and the stabilizer is prepared by mixing sodium hypophosphite, chromium nitrate and anhydrous sodium sulfite in a mass ratio of 0.4:0.3: 0.1;
s9, blank making and mold casting: melting the tin-bismuth alloy, pouring into a mold, carrying out surface activation treatment on the mold, putting the mold into a copper acid cylinder, and electroplating on the mold to form a copper layer, wherein the thickness of the copper layer is 30 microns;
the surface activation treatment comprises the following steps: (1) carrying out ultrasonic cleaning on the die, wherein the frequency is 30KHz, and the cleaning time is 30 min; (2) putting the die into deoiling liquid for electrolytic deoiling, keeping the voltage at 6V, the temperature at 25 ℃ and the time at 30 s; (3) placing the mould into dilute sulphuric acid, heating to boil, keeping for 10min, washing with deionized water for 1min, and mixing deoiling liquid with 10kg of electrolytic powder, 4kg of sodium carbonate, 20kg of trisodium phosphate, 1kg of sodium benzoate and 3kg of penetrant;
s10, electroplating: carrying out surface activation treatment on the mold with the copper layer, putting the mold into electroplating solution with the gold content of 10g/L, and electroplating to form a gold layer on the copper layer to obtain a semi-finished product, wherein the thickness of the gold layer is 50 microns;
the pH value of the electroplating solution is 6.5, the electroplating time is 8h, and the current density is 0.6A/dm2The temperature of the electroplating solution is 40 ℃;
during electroplating, a ruthenium iridium titanium network is selected as an anode, and the electroplating solution is prepared by mixing the following components in mass concentration: 20g/L of the electroforming solution prepared in the step S8, 25g/L of a cylinder opener, 40g/L of a complexing agent, 20g/L of a hardening agent and 30g/L of a brightening agent, wherein the brightening agent is prepared by preparation example 1, the complexing agent is prepared by mixing potassium citrate, chloride, phosphate and hydrogen phosphate according to the mass ratio of 1:0.2:0.3:0.1, the chloride is sodium chloride, the phosphate is potassium phosphate, the hydrogen phosphate is monopotassium phosphate, the hardening agent is prepared by mixing antimonate, selenium salt and potassium nitrate according to the mass ratio of 0.25:0.8:1.1, the antimonate is sodium antimonate, and the selenium salt is sodium selenosulfate;
the surface activation treatment comprises the following steps: (1) carrying out ultrasonic cleaning on the die, wherein the frequency is 30KHz, and the cleaning time is 30 min; (2) putting the die into deoiling liquid for electrolytic deoiling, keeping the voltage at 6V, the temperature at 25 ℃ and the time at 30 s; (3) placing the mould into dilute sulphuric acid, heating to boil, keeping for 10min, washing with deionized water for 1min, and mixing deoiling liquid with 10kg of electrolytic powder, 4kg of sodium carbonate, 20kg of trisodium phosphate, 1kg of sodium benzoate and 3kg of penetrant;
s11, demolding: punching at least two convection holes on the semi-finished product, penetrating the gold layer and the copper layer into the convection holes, placing the semi-finished product in an oven at the temperature of 130 ℃, heating while performing centrifugal treatment, placing the semi-finished product in a nitric acid solution, boiling for 20min, and washing with clear water for 3 times.
Example 2: a processing technology of gold jewelry comprises the following steps:
s1, tabletting: pressing 2kg of gold blocks into square gold sheets with the length and width of 0.2 mm;
s2, melting: putting the square gold flakes into the king water, and gradually dropwise adding concentrated nitric acid until the mass ratio of the concentrated hydrochloric acid to the concentrated nitric acid is 1: 5;
s3, nitrate removal: continuously adding concentrated hydrochloric acid into the mixed solution of the concentrated hydrochloric acid and the concentrated nitric acid, heating to 80 ℃, and adding the concentrated hydrochloric acid until the mixed solution does not generate yellow smoke;
s4, exhaust: pouring the mixed solution into a reaction kettle, cooling, slowly adding concentrated ammonia water with the concentration of 26mol/L for 1.5h, exhausting while adding, wherein the adding amount of the concentrated ammonia water is until no gas is discharged;
s5, chlorine washing: carrying out vacuum filtration on the mixed solution in the step S4, washing the filter residue for 8 times by using warm water at 60 ℃, taking 1.5mg of the filter residue after washing, putting the filter residue into a silver nitrate solution, observing whether a precipitate is generated or not, and if the precipitate is generated, continuing washing by using the warm water at 60 ℃ until the precipitate is not generated any more;
s6, preparing gold sodium sulfite: adding filter residue into a reaction kettle, adding anhydrous sodium sulfite, heating in a water bath to 65 ℃, stirring for 6.5 hours, adding dilute sulfuric acid with the mass concentration of 2% twice while stirring, wherein the adding amount of each time is 100ml, the adding interval time of the two times is 17min, heating to 93 ℃, and stirring for 3.5 hours;
s7, adjusting pH: taking liquid in the reaction kettle, and adjusting the pH value to 10 by using dilute sulfuric acid or potassium hydroxide, wherein the concentration of the dilute sulfuric acid is 37.5 percent, and the concentration of the potassium hydroxide is 5 percent;
s8, stability regulation: naturally cooling the liquid in the reaction kettle to 58 ℃, adding a stabilizer, uniformly stirring, cooling to 28 ℃, and filtering to obtain an electroforming liquid, wherein the mass ratio of the stabilizer to the liquid in the reaction kettle is 0.2:1, and the stabilizer is prepared by mixing sodium hypophosphite, chromium nitrate and anhydrous sodium sulfite in a mass ratio of 0.6:0.5: 0.2;
s9, blank making and mold casting: melting the tin-bismuth alloy, pouring into a mold, carrying out surface activation treatment on the mold, putting the mold into a copper acid cylinder, and electroplating on the mold to form a copper layer, wherein the thickness of the copper layer is 45 microns;
the surface activation treatment comprises the following steps: (1) carrying out ultrasonic cleaning on the die, wherein the frequency is 35KHz, and the cleaning time is 25 min; (2) putting the die into deoiling liquid for electrolytic deoiling, keeping the voltage at 6V, the temperature at 28 ℃ and the time at 75 s; (3) placing the mould into dilute sulphuric acid, heating to boil, keeping for 15min, cleaning with deionized water for 1.5min, and mixing deoiling liquid with 15kg of electrolytic powder, 5kg of sodium carbonate, 23kg of trisodium phosphate, 1.5kg of sodium benzoate and 3.5kg of penetrant;
s10, electroplating: carrying out surface activation treatment on the mold with the copper layer, putting the mold into electroplating solution with the gold content of 13g/L, and electroplating to form a gold layer on the copper layer to obtain a semi-finished product, wherein the thickness of the gold layer is 100 mu m;
the pH value of the electroplating solution is 7, the electroplating time is 14h, and the current density is 0.8A/dm2The temperature of the electroplating solution is 50 ℃;
during electroplating, a ruthenium iridium titanium network is selected as an anode, and the electroplating solution is prepared by mixing the following components in mass concentration: 35g/L of the electroforming solution prepared in the step S8, 35g/L of a cylinder opening agent, 70g/L of a complexing agent, 45g/L of a hardening agent and 40g/L of a brightening agent, wherein the brightening agent is prepared by a preparation example 2, the complexing agent is prepared by mixing potassium citrate, chloride, phosphate and hydrogen phosphate according to the mass ratio of 1:0.4:0.5:0.3, the chloride is hydrogen chloride, the phosphate is sodium phosphate, the hydrogen phosphate is sodium dihydrogen phosphate, the hardening agent is prepared by mixing antimony salt, selenium salt and potassium nitrate according to the mass ratio of 0.5:1:1.2, the antimony salt is antimony potassium tartrate, and the selenium salt is potassium selenosulfate;
the surface activation treatment comprises the following steps: (1) carrying out ultrasonic cleaning on the die, wherein the frequency is 35KHz, and the cleaning time is 25 min; (2) putting the die into deoiling liquid for electrolytic deoiling, keeping the voltage at 6V, the temperature at 28 ℃ and the time at 75 s; (3) placing the mould into dilute sulphuric acid, heating to boil, keeping for 15min, cleaning with deionized water for 1.5min, and mixing deoiling liquid with 15kg of electrolytic powder, 5kg of sodium carbonate, 23kg of trisodium phosphate, 1.5kg of sodium benzoate and 3.5kg of penetrant;
s11, demolding: punching at least two convection holes on the semi-finished product, penetrating the gold layer and the copper layer into the convection holes, placing the semi-finished product in an oven at the temperature of 150 ℃, heating while performing centrifugal treatment, placing the semi-finished product in a nitric acid solution, boiling for 25min, and washing with clear water for 4 times.
Example 3: a processing technology of gold jewelry comprises the following steps:
s1, tabletting: pressing 2kg of gold blocks into square gold sheets with the length and width of 0.1 mm;
s2, melting: putting the square gold flakes into the king water, and gradually dropwise adding concentrated nitric acid until the mass ratio of the concentrated hydrochloric acid to the concentrated nitric acid is 1: 5;
s3, nitrate removal: continuously adding concentrated hydrochloric acid into the mixed solution of the concentrated hydrochloric acid and the concentrated nitric acid, heating to 82 ℃, and adding the concentrated hydrochloric acid until the mixed solution does not generate yellow smoke;
s4, exhaust: pouring the mixed solution into a reaction kettle, cooling, slowly adding 28mol/L concentrated ammonia water for 2 hours while exhausting, wherein the adding amount of the concentrated ammonia water is up to no gas discharge;
s5, chlorine washing: carrying out vacuum filtration on the mixed solution in the step S4, washing the filter residue for 8 times by using warm water at 60 ℃, taking 2mg of the filter residue after washing, putting the filter residue into a silver nitrate solution, observing whether a precipitate is generated, and if the precipitate is generated, continuously washing the filter residue by using the warm water at 60 ℃ until no precipitate is generated;
s6, preparing gold sodium sulfite: adding filter residue into a reaction kettle, adding anhydrous sodium sulfite, heating in a water bath to 70 ℃, stirring for 6 hours, adding dilute sulfuric acid with the mass concentration of 2% twice while stirring, wherein the adding amount is 100ml each time, the adding interval time of the two times is 18min, heating to 95 ℃, and stirring for 3 hours;
s7, adjusting pH: taking liquid in the reaction kettle, and adjusting the pH value to 10 by using dilute sulfuric acid or potassium hydroxide, wherein the concentration of the dilute sulfuric acid is 38 percent, and the concentration of the potassium hydroxide is 10 percent;
s8, stability regulation: naturally cooling the liquid in the reaction kettle to 60 ℃, adding a stabilizer, uniformly stirring, cooling to 30 ℃, filtering to obtain an electroforming liquid, wherein the mass ratio of the stabilizer to the liquid in the reaction kettle is 0.3:1, and the stabilizer is prepared by mixing sodium hypophosphite, chromium nitrate and anhydrous sodium sulfite in a mass ratio of 0.8:0.7: 0.3;
s9, blank making and mold casting: melting the tin-bismuth alloy, pouring into a mold, carrying out surface activation treatment on the mold, putting the mold into a copper acid cylinder, and electroplating on the mold to form a copper layer with the thickness of 60 mu m;
the surface activation treatment comprises the following steps: (1) carrying out ultrasonic cleaning on the die, wherein the frequency is 40KHz, and the cleaning time is 20 min; (2) putting the die into deoiling liquid for electrolytic deoiling, keeping the voltage at 6V, the temperature at 30 ℃ and the time at 120 s; (3) placing the mould into dilute sulphuric acid, heating to boil, keeping for 20min, cleaning with deionized water for 2min, and mixing deoiling liquid with 20kg of electrolytic powder, 6kg of sodium carbonate, 25kg of trisodium phosphate, 2kg of sodium benzoate and 4kg of penetrant;
s10, electroplating: carrying out surface activation treatment on the mold with the copper layer, putting the mold into electroplating solution with the gold content of 16g/L, and electroplating to form a gold layer on the copper layer to obtain a semi-finished product, wherein the thickness of the gold layer is 150 mu m;
the pH value of the electroplating solution is 7.5, the electroplating time is 20h, and the current density is 1A/dm2The temperature of the electroplating solution is 60 ℃;
during electroplating, a ruthenium iridium titanium network is selected as an anode, and the electroplating solution is prepared by mixing the following components in mass concentration: 50g/L of the electroforming solution prepared in the step S8, 45g/L of a cylinder opening agent, 100g/L of a complexing agent, 70g/L of a hardening agent and 50g/L of a brightening agent, wherein the brightening agent is prepared by preparation example 3, the complexing agent is prepared by mixing potassium citrate, chloride, phosphate and hydrogen phosphate according to the mass ratio of 1:0.5:0.6:0.5, the chloride is potassium chloride and ammonium chloride according to the mass ratio of 1:1, the phosphate is sodium phosphate and potassium phosphate according to the mass ratio of 1:1, the hydrogen phosphate is sodium monohydrogen phosphate and potassium monohydrogen phosphate according to the mass ratio of 1:1, the hardening agent is prepared by mixing antimonate, selenium salt and potassium nitrate according to the mass ratio of 1:1.2:1.3, the antimonate is sodium antimonate and potassium antimonate according to the mass ratio of 1:1, and the selenium salt is sodium selenite and potassium selenite according to the mass ratio of 1: 1;
the surface activation treatment comprises the following steps: (1) carrying out ultrasonic cleaning on the die, wherein the frequency is 40KHz, and the cleaning time is 20 min; (2) putting the die into deoiling liquid for electrolytic deoiling, keeping the voltage at 6V, the temperature at 30 ℃ and the time at 120 s; (3) placing the mould into dilute sulphuric acid, heating to boil, keeping for 20min, cleaning with deionized water for 2min, and mixing deoiling liquid with 20kg of electrolytic powder, 6kg of sodium carbonate, 25kg of trisodium phosphate, 2kg of sodium benzoate and 4kg of penetrant;
s11, demolding: punching at least two convection holes on the semi-finished product, penetrating the gold layer and the copper layer into the convection holes, placing the semi-finished product in an oven at 180 ℃, heating while performing centrifugal treatment, placing the semi-finished product in a nitric acid solution, boiling for 30min, and washing with clear water for 5 times.
Comparative example
Comparative example 1: the difference between the processing technology of gold jewelry and the embodiment 1 is that no stabilizer is added in the step S8.
Comparative example 2: the difference between the processing technology of gold jewelry and the embodiment 1 is that no hardening agent is added into the electroplating solution.
Comparative example 3: the processing technology of the gold jewelry is different from the processing technology of the embodiment 1 in that no brightener is added into the electroplating solution.
Comparative example 4: the process for manufacturing the hollow jewelry by taking the jewelry prepared in the embodiment 1 in the Chinese invention patent application with the application number of CN201910487882.1 as a reference comprises the following steps: A. manufacturing a wax piece; B. conductive oil is coated on the wax piece; C. hanging the wax piece; D. electro-copper; E. putting the copper piece into deoiling liquid for electrolytic deoiling; F. electroforming in an electric cylinder, selecting an electroforming gold solution, selecting a ruthenium iridium titanium net as an anode, wherein the electroforming gold solution has Ph7.3 and gold content of 10g/L, and the mass concentration of each component is as follows: 10g/L of main salt, 80g/L of complexing agent, 15g/L of light agent, 10g/L of hardening agent and 0.1ppm of additive; G. removing the core, namely punching at least two convection holes on each semi-finished product, wherein the convection holes penetrate through the thick gold layer and the copper layer; then, putting the semi-finished product into a depoling furnace for heating at 190 ℃ for 1H; in addition, the method also comprises the following steps: g1, boiling nitric acid: putting the semi-finished product in the step G into a beaker, adding nitric acid into the beaker, and heating the nitric acid in the beaker to boil for 20-30 minutes until the reaction is stopped; g2, boiled sulfuric acid: after the semi-finished product is taken out of the beaker, the semi-finished product is placed into the beaker, sulfuric acid is added until the position of 3cm of the semi-finished product is submerged, the semi-finished product is heated to boiling, impurity residues are removed through the strong oxidizing property and the strong corrosivity of the sulfuric acid, the semi-finished product is kept for 30 minutes until the semi-finished product is naturally cooled, and then the semi-finished product is placed into a cleaning container to be cleaned for 1 to 2 minutes by clean water; H. and (3) carrying out die holding, carrying out hole sealing operation on the convection holes of the semi-finished product by adopting a laser machine, cleaning coarse grains or burrs on the surface of the hollow semi-finished product to achieve a smooth or required surface effect, and carrying out cleaning, drying and quality inspection to obtain a finished product of the hollow ornament.
Performance test
The gold jewelry was prepared according to the methods in examples 1 to 3 and comparative examples 1 to 4, and various properties of the gold jewelry were measured according to the following test methods, and the test results were recorded in table 1:
1. hardness: according to GB/T4340.1-2009 part 1 of Vickers hardness experiment of metal materials: test method ", detection environment: 60% RH at 26 ℃;
2. wear resistance: the palm brush with the weight of 450g reciprocates to observe whether the surface of the jewelry is worn or not, the abrasion resistance is qualified if the palm brush does not wear after 1000 times of reciprocation, the number of times of reciprocation can be increased to 3000 times, and whether the jewelry is worn or not is observed;
3. sweat resistance: paving a layer of cotton at the bottom of a glass ware, introducing artificial sweat to ensure that the cotton is thoroughly wetted, soaking jewelry products prepared in each embodiment and each proportion by the artificial sweat, then placing the jewelry products into the glass ware, covering the glass ware with a cover, placing the glass ware into a constant temperature box, controlling the temperature to be 40 +/-2 ℃, checking once every 8 hours to check whether the jewelry products are corroded, degraded or blackened, and judging that the jewelry products are qualified if no corrosion trace exists in 48 hours, wherein the time can be prolonged to 96 hours;
4. salt spray resistance: preparing a test solution, pouring the prepared acid test solution into a salt spray machine, adjusting the air pressure to be 0.2-0.4MPa and the spraying pressure to be 0.07-0.17MPa, putting the jewelry product into a salt spray test box, turning on a power supply, adjusting the test temperature to be 30 ℃, adjusting the temperature of a saturator to be 35-40 ℃, turning on a spraying switch after the temperature is constant, setting the spraying time to be generally set to be 48 hours, checking once every 8 hours, checking whether the product is corroded, degraded or the surface coating falls off, judging that the product is qualified if the product is not corroded in 48 hours, and prolonging the observation time to 96 hours;
5. and (3) the care product resistance: spraying cologne, a hairstyle fixing solution spray or cosmetics on the surface of a product, placing the product in an environment with normal temperature and relative humidity of 50-60%, taking out the product after 24 hours, checking that no change is generated on the surface of the jewelry product, recording the surface as qualified, and prolonging the observation time to 48 hours.
Table 1 performance test results of gold jewelry prepared in each example and each comparative example
As can be seen from the data in table 1, the gold jewelry prepared according to the examples 1 to 3 has high vickers hardness which is more than 170Hv, and the brown brush is not worn after being repeatedly used for more than 3000 times, has good wear resistance, does not have blackening phenomenon on the surface after being soaked by sweat for 96 hours, has no corrosion phenomenon after being soaked in acid liquor for 96 hours, and is sprayed with perfume, hair style setting liquid or skin care product, and the surface of the gold jewelry has no change after 48 hours, which indicates that the gold jewelry is not easy to be oxidized after being contacted with skin care products and the like, and has good stability.
Comparative example 1 because no stabilizer is added during the preparation of the gold sodium sulfite, the wear resistance, sweat resistance and salt spray resistance of the prepared gold jewelry are all reduced, comparative example 2 and comparative example 3 respectively because no hardening agent and brightening agent are added in the electroplating solution, the gold jewelry prepared in comparative example 2 has poor wear resistance and hardness, wear occurs in a palm brush reciprocating brush for 2000 times, and the gold jewelry prepared in comparative example 3 has poor detection results of salt spray resistance, sweat resistance and the like although the wear resistance and hardness are not much different from those of examples 1-3.
Comparative example 4 is a gold jewelry prepared by the prior art, which has the hardness of only 110.5Hv, small hardness, poor oxidation resistance and easy occurrence of blackening.
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
Claims (10)
1. A processing technology of gold jewelry is characterized by comprising the following steps:
s1, tabletting: pressing 2kg of gold blocks into square gold sheets with the length and width of 0.15 +/-0.05 mm;
s2, melting: putting the square gold flakes into the king water, and gradually dropwise adding concentrated nitric acid until the mass ratio of the concentrated hydrochloric acid to the concentrated nitric acid is 1: 5;
s3, nitrate removal: continuously adding concentrated hydrochloric acid into the mixed solution of the concentrated hydrochloric acid and the concentrated nitric acid, heating to 78-82 ℃, and adding the concentrated hydrochloric acid until the mixed solution does not produce yellow flue gas any more;
s4, exhaust: pouring the mixed solution into a reaction kettle, cooling, slowly adding concentrated ammonia water for 1-2h, and exhausting while adding;
s5, chlorine washing: carrying out vacuum filtration on the mixed solution obtained in the step S4, and washing filter residues for 8 times by using warm water at 60 ℃;
s6, preparing gold sodium sulfite: adding filter residue into a reaction kettle, adding anhydrous sodium sulfite, heating in water bath to 60-70 ℃, stirring for 6-7h, adding dilute sulfuric acid with the mass concentration of 2% twice while stirring, wherein the adding amount of each time is 100ml, the adding interval time of the two times is 15-18min, heating to 90-95 ℃, and stirring for 3-4h;
s7, adjusting pH: taking liquid in the reaction kettle, and adjusting the pH value to 10 by using dilute sulfuric acid or potassium hydroxide;
s8, stability regulation: naturally cooling the liquid in the reaction kettle to 55-60 ℃, adding a stabilizer, uniformly stirring, cooling to 25-30 ℃, and filtering to obtain an electroforming liquid, wherein the mass ratio of the stabilizer to the liquid in the reaction kettle is 0.1-0.3: 1;
s9, blank making and mold casting: melting the tin-bismuth alloy, pouring into a mold, carrying out surface activation treatment on the mold, putting the mold into a copper acid cylinder, and electroplating on the mold to form a copper layer;
s10, electroplating: carrying out surface activation treatment on the mold with the copper layer, putting the mold into electroplating solution with the gold content of 10-16g/L, and electroplating to form a gold layer on the copper layer to obtain a semi-finished product;
during electroplating, a ruthenium iridium titanium network is selected as an anode, and the electroplating solution comprises the following components in mass concentration: 20-50g/L of the electroforming solution prepared in the step S8, 25-45g/L of a cylinder opening agent, 40-100g/L of a complexing agent, 20-70g/L of a hardening agent and 30-50g/L of a brightening agent;
s11, demolding: punching at least two convection holes on the semi-finished product, penetrating the convection holes through the gold layer and the copper layer, placing the semi-finished product in an oven at the temperature of 130-180 ℃, heating while performing centrifugal treatment, placing the semi-finished product in a nitric acid solution, boiling for 20-30min, and washing for 3-5 times with clear water.
2. The process of claim 1, wherein the stabilizer is sodium hypophosphite, chromium nitrate and anhydrous sodium sulfite in a mass ratio of (0.4-0.8) to (0.3-0.7) to (0.1-0.3).
3. The processing technology of gold jewelry as claimed in claim 1, wherein the complexing agent is prepared by mixing potassium citrate, chloride, phosphate and hydrogen phosphate according to a mass ratio of 1 (0.2-0.5) to (0.3-0.6) to (0.1-0.5).
4. The processing technology of gold jewelry according to claim 3, wherein the chloride is one or more of sodium chloride, hydrogen chloride, potassium chloride and ammonium chloride; the phosphate is one or the combination of potassium phosphate and sodium phosphate; the hydrogen phosphate is one or more of potassium dihydrogen phosphate, sodium hydrogen phosphate and potassium hydrogen phosphate.
5. The processing technology of the gold jewelry according to claim 1, wherein the hardening agent is antimony salt, selenium salt and potassium tartrate in a mass ratio of 0.25-1:0.8-1.2: 1.1-1.3;
the antimonic salt is one or a composition of more of sodium antimonate tartrate, potassium antimonate, sodium antimonate and potassium antimonate, and the selenium salt is one or a composition of more of sodium selenosulfate, potassium selenosulfate, sodium selenite and potassium selenite.
6. The processing technology of the gold jewelry according to claim 1, wherein the brightener is prepared by the following method: using 1.5-1.8 weight portions of distilled hydrosolvent saccharin sodium with 70-80 ℃, deionizing 0.5-0.8 weight portion, heating to 50-60 ℃, adding 0.1-0.3 weight portion of glucose while stirring, adding saccharin sodium dissolved in distilled water in advance, stirring strongly, adding 0.4-0.9 weight portion of cobalt sulfate and 0.2-0.5 weight portion of nickel sulfate, supplementing 0.5-1 weight portion of distilled water, adding 0.08-0.12 weight portion of 1, 3-propanediamine hydrazinodithioformamide, and stirring uniformly to obtain the brightener.
7. The processing technology of gold jewelry according to claim 1, wherein the surface activation treatment in steps S9 and S10 comprises the following steps: (1) carrying out ultrasonic cleaning on the die, wherein the frequency is 30-40KHz, and the cleaning time is 20-30 min; (2) putting the die into deoiling liquid for electrolytic deoiling, keeping the voltage at 6V, the temperature at 25-30 ℃, and the time at 30-120 s; (3) placing the mold into dilute sulfuric acid, heating to boil, maintaining for 10-20min, and washing with deionized water for 1-2 min.
8. The processing technology of gold jewelry according to claim 7, wherein the deoiling liquid is prepared by mixing the following components in parts by weight: 10-20 parts of electrolytic powder, 4-6 parts of sodium carbonate, 20-25 parts of trisodium phosphate, 1-2 parts of sodium benzoate and 3-4 parts of penetrating agent.
9. The processing technology of gold jewelry according to claim 1, wherein the pH value of the electroplating solution is 6.5-7.5, the electroplating time is 8-20h, and the current density is 0.6-1A/dm2The temperature of the electroplating solution is 40-60 ℃.
10. The processing technology of gold jewelry according to claim 1, wherein after the washing in step S5, 1-2mg of the filter residue is taken and put into silver nitrate solution, whether or not a precipitate is generated is observed, and if the precipitate is generated, the washing with warm water at 60 ℃ is continued until no precipitate is generated.
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Application publication date: 20191224 |