CN105568269A - Preparation method of cyanide-free gold plating reagent sodium gold sulfite - Google Patents
Preparation method of cyanide-free gold plating reagent sodium gold sulfite Download PDFInfo
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- CN105568269A CN105568269A CN201510942820.7A CN201510942820A CN105568269A CN 105568269 A CN105568269 A CN 105568269A CN 201510942820 A CN201510942820 A CN 201510942820A CN 105568269 A CN105568269 A CN 105568269A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/42—Coating with noble metals
- C23C18/44—Coating with noble metals using reducing agents
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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
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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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Abstract
The invention relates to a preparation method of a gold salt for gold plating, particularly a preparation method of a cyanide-free gold plating reagent sodium gold sulfite, belonging to the technical field of chemistry. The preparation method comprises the following steps: gold rolling, gold bullion cleaning, gold dissolution, nitre removal, solonization, solonization, cleaning, complexing reaction, and crystallization by concentration. The method has the advantages of simple technique and high safety, can not generate dangerous intermediates in the process, can effectively lower chlorine ions, and can be used for producing the odorless green environment-friendly product.
Description
Technical field
The present invention relates to the preparation method of the golden salt of a kind of gold-plated use, be a kind of preparation method of cyanogen-less gold reagent gold sodium sulfide specifically, belong to technical field of chemistry.
Background technology
At present, technique mainly chloric acid gold direct-reduction process and the Lei Jin reduction method of gold sodium sulfide, chloric acid gold direct-reduction process, technique difficulty controls, and finished product is low, also has finished product to contain a large amount of chlorion, affects product and uses.Although thunder gold reduction method can remove chlorion, thunder gold is powerful explosive, and explosive, bad operation, and product constantly decomposes ammonia, and taste is unpleasant.
Summary of the invention
In order to solve the problem, the invention discloses a kind of preparation method of cyanogen-less gold reagent gold sodium sulfide, present invention process is simple, safety, process can not produce dangerous intermediate, not only effectively can reduce chlorion but also can produce the product of tasteless environmental protection.
A preparation method for cyanogen-less gold reagent gold sodium sulfide, preparation process is:
(1) gold rolls: the purity gold bar that is 99.99% is placed on tabletting machine and carries out spreading, be pressed into the block that thickness is 2mm, and cut block, cut into common rectangular parallelepiped gold bullion, obtain gold bullion a;
(2) clean gold bullion: the gold bullion a in process (1) cleans, first adopt ethanol to carry out repeatedly oil removing, after oil removing, then adopt deionized water repeatedly to rinse it, obtain gold bullion b;
(3) gold dissolves: the gold bullion b in process (2) is placed in reactor; add analytical pure hydrochloric acid, after adding hydrochloric acid, start slowly to heat; after being heated to 45-50 DEG C; slowly add analytical pure nitric acid 0.5L again, add in the process of nitric acid and there will be tobacco in prolong, after tobacco disappears; again repeat the process adding nitric acid; repeated multiple times, until gold bullion all dissolves, obtain solution c;
(4) nitre process is caught up with: in the solution c in process (3), slowly add hydrochloric acid, limit heating edge must add hydrochloric acid, Heating temperature is between 45-50 DEG C, until produce without reddish-brown gas, stop adding hydrochloric acid, continue heating, gold concentration is detected through ICP, treat that gold concentration in solution is between 300-400g/L, stop heating, after cooling, obtain solution d;
(5) alkalinization: the solution d in process (4) is stirred, stirring velocity is 30r/min, slowly adding analytical pure sodium hydroxide, add in the process of sodium hydroxide and test pH value, as pH=7, stop adding sodium hydroxide, treat that solution is cooled to continue to add sodium hydroxide between 30 DEG C-35 DEG C, when pH=9, stop adding sodium hydroxide, now occur in solution that auric hydroxide precipitates, continue to stir, now the pH of solution can reduce, when pH=7, continue to add sodium hydroxide, until during pH=10, stop adding sodium hydroxide, now there will be a large amount of auric hydroxide precipitation in solution, continue to stir, stop stirring when solution temperature drops to room temperature, now solution is muddy state, be separated as in whizzer, obtain solid e,
(6) cleaning process: add the distilled water that temperature is 45-55 DEG C in the solid e of process (5), wherein the ratio of distilled water and gold is 10L:1kg, carry out solid-liquid separation again, repeated washing process repeatedly, until the chlorine ion concentration in parting liquid is lower than 80ppm, stop cleaning process, obtain solid f;
(7) complex reaction: it is in the deionized water of 50-60 DEG C that S-WAT is dissolved in temperature, solid f under agitation in slow adition process (6), now solution turned cloudy, stop adding solid f, become after glassy yellow until solution from muddiness, continue the process repeating to add solid f, till solid f adds, continue constant temperature between 50-60 DEG C, within every 60 minutes, detect pH, pH and will control between 9-10, if during pH < 9, drip 5% sulphuric acid soln to pH between 9-10, constant temperature 10h, obtain clear solution g;
(8) condensing crystal: add stablizer in the solution g of process (7), wherein stablizer is (weight ratio): 1:5 with the ratio of gold, after adding stablizer, be placed in rotatory evaporator heating under reduced pressure, temperature controls at 50-60 DEG C, until after there is crystal, cold filtration, obtain gold sodium sulfide solid, then dry in 50-60 DEG C of vacuum drier, obtain final gold sodium sulfide.
A preparation method for cyanogen-less gold reagent gold sodium sulfide, is characterized in that: in process (3) dissolution process, add analytical pure hydrochloric acid, and wherein the ratio of gold and hydrochloric acid is 1 kilogram of gold: 4L hydrochloric acid.
A preparation method for cyanogen-less gold reagent gold sodium sulfide, is characterized in that: the meltage of process (7) S-WAT is 2.5:1 with the ratio of gold.
A preparation method for cyanogen-less gold reagent gold sodium sulfide, is characterized in that: in process (8), stablizer is the one in dipotassium hydrogen phosphate, quadrol or sodium sulphite anhydrous 99.3.
Embodiment
A preparation method for cyanogen-less gold reagent gold sodium sulfide, preparation process is:
(1) gold rolls: the purity gold bar that is 99.99% is placed on tabletting machine and carries out spreading, be pressed into the block that thickness is 2mm, and cut block, cut into common rectangular parallelepiped gold bullion, obtain gold bullion a;
(2) clean gold bullion: the gold bullion a in process (1) cleans, first adopt ethanol to carry out repeatedly oil removing, after oil removing, then adopt deionized water repeatedly to rinse it, obtain gold bullion b;
(3) gold dissolves: the gold bullion b in process (2) is placed in reactor; add analytical pure hydrochloric acid, after adding hydrochloric acid, start slowly to heat; after being heated to 45-50 DEG C; slowly add analytical pure nitric acid 0.5L again, add in the process of nitric acid and there will be tobacco in prolong, after tobacco disappears; again repeat the process adding nitric acid; repeated multiple times, until gold bullion all dissolves, obtain solution c;
(4) nitre process is caught up with: in the solution c in process (3), slowly add hydrochloric acid, limit heating edge must add hydrochloric acid, Heating temperature is between 45-50 DEG C, until produce without reddish-brown gas, stop adding hydrochloric acid, continue heating, gold concentration is detected through ICP, treat that gold concentration in solution is between 300-400g/L, stop heating, after cooling, obtain solution d;
(5) alkalinization: the solution d in process (4) is stirred, stirring velocity is 30r/min, slowly adding analytical pure sodium hydroxide, add in the process of sodium hydroxide and test pH value, as pH=7, stop adding sodium hydroxide, treat that solution is cooled to continue to add sodium hydroxide between 30 DEG C-35 DEG C, when pH=9, stop adding sodium hydroxide, now occur in solution that auric hydroxide precipitates, continue to stir, now the pH of solution can reduce, when pH=7, continue to add sodium hydroxide, until during pH=10, stop adding sodium hydroxide, now there will be a large amount of auric hydroxide precipitation in solution, continue to stir, stop stirring when solution temperature drops to room temperature, now solution is muddy state, be separated as in whizzer, obtain solid e,
(6) cleaning process: add the distilled water that temperature is 45-55 DEG C in the solid e of process (5), wherein the ratio of distilled water and gold is 10L:1kg, carry out solid-liquid separation again, repeated washing process repeatedly, until the chlorine ion concentration in parting liquid is lower than 80ppm, stop cleaning process, obtain solid f;
(7) complex reaction: it is in the deionized water of 50-60 DEG C that S-WAT is dissolved in temperature, solid f under agitation in slow adition process (6), now solution turned cloudy, stop adding solid f, become after glassy yellow until solution from muddiness, continue the process repeating to add solid f, till solid f adds, continue constant temperature between 50-60 DEG C, within every 60 minutes, detect pH, pH and will control between 9-10, if during pH < 9, drip 5% sulphuric acid soln to pH between 9-10, constant temperature 10h, obtain clear solution g;
(8) condensing crystal: add stablizer in the solution g of process (7), wherein stablizer is (weight ratio): 1:5 with the ratio of gold, after adding stablizer, be placed in rotatory evaporator heating under reduced pressure, temperature controls at 50-60 DEG C, until after there is crystal, cold filtration, obtain gold sodium sulfide solid, then dry in 50-60 DEG C of vacuum drier, obtain final gold sodium sulfide.
Wherein, in process (3), Heating temperature is 40-50 DEG C, and preferred Heating temperature is 48 DEG C.
Wherein, in process (4), Heating temperature is between 45-50 DEG C, and preferred Heating temperature is 45 DEG C, and gold concentration is between 300-400g/L, and preferred gold concentration is 320g/L.
Wherein, in process (5), be cooled to, between 30 DEG C-35 DEG C, preferably be cooled to 33 DEG C.
Wherein, in process (6), temperature is the distilled water of 45-55 DEG C, is preferably the distilled water that temperature is 55 DEG C.
Wherein, in process (7), it is in the deionized water of 50-60 DEG C that S-WAT is dissolved in temperature, and preferred dissolution temperature is 50 DEG C, and constant temperature is between 50-60 DEG C, and preferred constant temperature is at 50 DEG C.
Wherein, in process (8), temperature controls at 50-60 DEG C, and preferable temperature controls at 60 DEG C, then dries in 50-60 DEG C of vacuum drier, and preferable temperature is 55 DEG C.
Further, a kind of preparation method of cyanogen-less gold reagent gold sodium sulfide, in process (3) dissolution process, adds analytical pure hydrochloric acid, and wherein the ratio of gold and hydrochloric acid is 1 kilogram of gold: 4L hydrochloric acid.
Further, a kind of preparation method of cyanogen-less gold reagent gold sodium sulfide, the meltage of process (7) S-WAT is 2.5:1 with the ratio of gold.
Further, a kind of preparation method of cyanogen-less gold reagent gold sodium sulfide, is characterized in that: in process (8), stablizer is the one in dipotassium hydrogen phosphate, quadrol or sodium sulphite anhydrous 99.3, and preferred stabilizer is quadrol.
Present invention process is simple, safety, and process can not produce dangerous intermediate, not only effectively can reduce chlorion but also can produce the product of tasteless environmental protection.
The present embodiment might not be most preferred embodiment of the present invention, and the ratio between other summary of the invention materials all belongs to protection scope of the present invention within the scope of this.
Claims (4)
1. a preparation method for cyanogen-less gold reagent gold sodium sulfide, preparation process is:
(1) gold rolls: the purity gold bar that is 99.99% is placed on tabletting machine and carries out spreading, be pressed into the block that thickness is 2mm, and cut block, cut into common rectangular parallelepiped gold bullion, obtain gold bullion a;
(2) clean gold bullion: the gold bullion a in process (1) cleans, first adopt ethanol to carry out repeatedly oil removing, after oil removing, then adopt deionized water repeatedly to rinse it, obtain gold bullion b;
(3) gold dissolves: the gold bullion b in process (2) is placed in reactor; add analytical pure hydrochloric acid, after adding hydrochloric acid, start slowly to heat; after being heated to 45-50 DEG C; slowly add analytical pure nitric acid 0.5L again, add in the process of nitric acid and there will be tobacco in prolong, after tobacco disappears; again repeat the process adding nitric acid; repeated multiple times, until gold bullion all dissolves, obtain solution c;
(4) nitre process is caught up with: in the solution c in process (3), slowly add hydrochloric acid, limit heating edge must add hydrochloric acid, Heating temperature is between 45-50 DEG C, until produce without reddish-brown gas, stop adding hydrochloric acid, continue heating, gold concentration is detected through ICP, treat that gold concentration in solution is between 300-400g/L, stop heating, after cooling, obtain solution d;
(5) alkalinization: the solution d in process (4) is stirred, stirring velocity is 30r/min, slowly adding analytical pure sodium hydroxide, add in the process of sodium hydroxide and test pH value, as pH=7, stop adding sodium hydroxide, treat that solution is cooled to continue to add sodium hydroxide between 30 DEG C-35 DEG C, when pH=9, stop adding sodium hydroxide, now occur in solution that auric hydroxide precipitates, continue to stir, now the pH of solution can reduce, when pH=7, continue to add sodium hydroxide, until during pH=10, stop adding sodium hydroxide, now there will be a large amount of auric hydroxide precipitation in solution, continue to stir, stop stirring when solution temperature drops to room temperature, now solution is muddy state, be separated as in whizzer, obtain solid e,
(6) cleaning process: add the distilled water that temperature is 45-55 DEG C in the solid e of process (5), wherein the ratio of distilled water and gold is 10L:1kg, carry out solid-liquid separation again, repeated washing process repeatedly, until the chlorine ion concentration in parting liquid is lower than 80ppm, stop cleaning process, obtain solid f;
(7) complex reaction: it is in the deionized water of 50-60 DEG C that S-WAT is dissolved in temperature, solid f under agitation in slow adition process (6), now solution turned cloudy, stop adding solid f, become after glassy yellow until solution from muddiness, continue the process repeating to add solid f, till solid f adds, continue constant temperature between 50-60 DEG C, within every 60 minutes, detect pH, pH and will control between 9-10, if during pH < 9, drip 5% sulphuric acid soln to pH between 9-10, constant temperature 10h, obtain clear solution g;
(8) condensing crystal: add stablizer in the solution g of process (7), wherein stablizer is (weight ratio): 1:5 with the ratio of gold, after adding stablizer, be placed in rotatory evaporator heating under reduced pressure, temperature controls at 50-60 DEG C, until after there is crystal, cold filtration, obtain gold sodium sulfide solid, then dry in 50-60 DEG C of vacuum drier, obtain final gold sodium sulfide.
2. the preparation method of a kind of cyanogen-less gold reagent gold sodium sulfide according to claim 1, is characterized in that: in process (3) dissolution process, add analytical pure hydrochloric acid, and wherein the ratio of gold and hydrochloric acid is 1 kilogram of gold: 4L hydrochloric acid.
3. the preparation method of a kind of cyanogen-less gold reagent gold sodium sulfide according to claim 1, is characterized in that: the meltage of process (7) S-WAT is 2.5:1 with the ratio of gold.
4. the preparation method of a kind of cyanogen-less gold reagent gold sodium sulfide according to claim 1, is characterized in that: in process (8), stablizer is the one in dipotassium hydrogen phosphate, quadrol or sodium sulphite anhydrous 99.3.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106637314A (en) * | 2016-12-15 | 2017-05-10 | 广东光华科技股份有限公司 | Preparation method of sodium gold sulfide solution for cyanide-free gold plating |
| CN107986319A (en) * | 2017-12-01 | 2018-05-04 | 深圳市前海绿智源科技有限公司 | Method without cyanogen gold salt is prepared using the molten method of iodine |
| CN110894618A (en) * | 2019-10-10 | 2020-03-20 | 深圳市金质金银珠宝检验研究中心有限公司 | Environment-friendly surface modified electroformed gold solution and preparation method thereof |
| CN112111764A (en) * | 2020-08-21 | 2020-12-22 | 深圳润福金技术开发有限公司 | Preparation method of efficient cyanide-free gold water |
| CN112301388A (en) * | 2019-07-25 | 2021-02-02 | 山东亿福金业珠宝首饰有限公司 | Cyanide-free electroplating process |
| CN113046800A (en) * | 2021-02-04 | 2021-06-29 | 深圳市金正龙科技有限公司 | Gold sodium sulfite electroplating solution and preparation method thereof |
| CN113529144A (en) * | 2020-08-07 | 2021-10-22 | 深圳市鼎泰盈盛科技有限公司 | Finished product of sulfite cyanide-free electroformed gold liquid capable of being burnt |
| CN114108040A (en) * | 2020-08-25 | 2022-03-01 | 周大福珠宝文化产业园(武汉)有限公司 | Cyanide-free gold plating solution and gold electroforming part manufactured by cyanide-free electroplating process |
| CN114164465A (en) * | 2021-11-15 | 2022-03-11 | 深圳市联合蓝海黄金材料科技股份有限公司 | Sodium gold sulfite gold water and synthesis method and application thereof |
| CN115198257A (en) * | 2022-07-12 | 2022-10-18 | 深圳市创智成功科技有限公司 | Cyanide-free gold immersion environment-friendly solution for wafer packaging and chemical plating method |
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Non-Patent Citations (1)
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| 黄世盛等: "一种无氰镀金试剂的生产工艺及应用", 《广东化工》 * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106637314A (en) * | 2016-12-15 | 2017-05-10 | 广东光华科技股份有限公司 | Preparation method of sodium gold sulfide solution for cyanide-free gold plating |
| CN106637314B (en) * | 2016-12-15 | 2018-08-31 | 广东光华科技股份有限公司 | A kind of preparation method of the gold sodium sulfide solution of cyanogen-less gold |
| CN107986319A (en) * | 2017-12-01 | 2018-05-04 | 深圳市前海绿智源科技有限公司 | Method without cyanogen gold salt is prepared using the molten method of iodine |
| CN112301388A (en) * | 2019-07-25 | 2021-02-02 | 山东亿福金业珠宝首饰有限公司 | Cyanide-free electroplating process |
| CN110894618A (en) * | 2019-10-10 | 2020-03-20 | 深圳市金质金银珠宝检验研究中心有限公司 | Environment-friendly surface modified electroformed gold solution and preparation method thereof |
| CN113529144A (en) * | 2020-08-07 | 2021-10-22 | 深圳市鼎泰盈盛科技有限公司 | Finished product of sulfite cyanide-free electroformed gold liquid capable of being burnt |
| CN112111764A (en) * | 2020-08-21 | 2020-12-22 | 深圳润福金技术开发有限公司 | Preparation method of efficient cyanide-free gold water |
| CN114108040A (en) * | 2020-08-25 | 2022-03-01 | 周大福珠宝文化产业园(武汉)有限公司 | Cyanide-free gold plating solution and gold electroforming part manufactured by cyanide-free electroplating process |
| CN113046800A (en) * | 2021-02-04 | 2021-06-29 | 深圳市金正龙科技有限公司 | Gold sodium sulfite electroplating solution and preparation method thereof |
| CN114164465A (en) * | 2021-11-15 | 2022-03-11 | 深圳市联合蓝海黄金材料科技股份有限公司 | Sodium gold sulfite gold water and synthesis method and application thereof |
| CN115198257A (en) * | 2022-07-12 | 2022-10-18 | 深圳市创智成功科技有限公司 | Cyanide-free gold immersion environment-friendly solution for wafer packaging and chemical plating method |
| CN115198257B (en) * | 2022-07-12 | 2024-02-02 | 深圳创智芯联科技股份有限公司 | Environment-friendly cyanide-free gold-depositing solution for wafer packaging and electroless plating method |
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