CN107986319A - Method without cyanogen gold salt is prepared using the molten method of iodine - Google Patents
Method without cyanogen gold salt is prepared using the molten method of iodine Download PDFInfo
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Abstract
The method without cyanogen gold salt is prepared using the molten method of iodine the invention discloses a kind of, which includes the following high pure gold for weighing 10g, be added in the iodine of 20g/l and the mixed solution of the potassium iodide of 40 80g/l and carry out dissolved solution；Obtained gold hydroxide precipitation is reacted after suitable sodium hydroxide solution, sodium carbonate liquor or sodium bicarbonate solution are added in above-mentioned solution；Precipitation is obtained into the gold hydroxide solid of purity higher after multiple washing and filtering；Prepare the sodium sulfite solution of 200g/l；Gold hydroxide sediment is added to prepared sodium sulfite solution again and carries out isothermal reaction, solution becomes colorless as terminal again from brown muddiness yellowing, finally obtains finished product gold sodium sulfide solution, and the control of gold ion content is in 50g/l or so；And this method can realize no toxic gas discharge, and process is simple and easy to control, and finished product is stable and purity is high.
Description
Technical field
The present invention relates to Material Field, more particularly to a kind of the method without cyanogen gold salt is prepared using the molten method of iodine.
Background technology
Gold is due to very high chemical stability, ductility, relatively low contact resistance, high temperature resistant and decoration anti-discoloration
The features such as energy, receive and are widely applied, especially have in Surface Processing Industry and be largely related to.All the time, it is surface-treated
The source of middle gold ion is mainly based on the compound potassium auricyanide containing cyanogen, due to the characteristic with severe toxicity, to human body and environment
Strong influence is caused, with environmental pollution getting worse, continuous enhancing of the people to environmental consciousness, environmentally friendly is free of cyaniding
The craft of gilding of thing is increasingly valued by people.Previous preparation of the someone to no cyanogen gold salt is studied, and common are
Gold chloride, gold sodium sulfide etc., poor relative to gold chloride stability, everybody generally tends to study gold sodium sulfide or sulfurous
The gold reagents such as sour gold potassium.In conventional patent（106637314 A of CN 105568269 A and CN）, the preparation of sulfurous acid gold salt,
Gold chloride is typically made by aqua regia dissolution gold, then is reacted by gold chloride and sulfurous acid gold salt reagent is made, due to production
During chlorauric acid solution stability by temperature, acidity, concentration, external condition and the easy absorption factor shadow such as on the wall
Ring, cause product qualified rate low, cost is very high.And toxic gas can be all produced in the technique of previous patent or paper:Nitrogen
Oxygen compound or chlorine, very big negative effect is all generated to equipment, production cost, environmental pollution etc., or perhaps secondary
Pollution, therefore can not meet the needs of market.Above-mentioned deficiency is solved in order to integrate, the present invention have developed a kind of new preparation side
Method, in preparation process is produced, employs iodine and liquor kalii iodide carries out the dissolving and preparation of gold, while with the addition of assisted oxidation
Agent carries out acceleration dissolving, improves production efficiency, avoids the wang aqueous solution of severe corrosive.And production technology is optimized, allow work
Skill operation is more stable, environment influences smaller, and properties of product are more preferably.
The content of the invention
For shortcoming present in above-mentioned technology, the present invention provides a kind of using molten side of the method preparation without cyanogen gold salt of iodine
Method, this method can realize no toxic gas discharge, and process is simple and easy to control, and finished product is stable and purity is high.
To achieve the above object, the present invention provides a kind of using molten method of the method preparation without cyanogen gold salt of iodine, including following step
Suddenly：
Step 1, the high pure gold of 10g is weighed, is added in the iodine of 20g/l and the mixed solution of the potassium iodide of 40-80g/l and carries out
Dissolved solution；The reaction equation produced in the step is I2+I-+H2O=I3 -.H2O,Au+I-+I3 -=AuI4 -；
Step 2, system is reacted after suitable sodium hydroxide solution, sodium carbonate liquor or sodium bicarbonate solution are added in above-mentioned solution
Obtain gold hydroxide precipitation；The reaction equation produced in the step is：2AuI4 -+12OH-=2Au(OH)3+I-+IO3-+3H2O；
Step 3, precipitation is obtained into the gold hydroxide solid of purity higher after multiple washing and filtering；
Step 4, the sodium sulfite solution of 200g/l is prepared；
Step 5, then gold hydroxide sediment is added to prepared sodium sulfite solution and carries out isothermal reaction, solution is from brown
Color muddiness yellowing becomes colorless as terminal again, finally obtains finished product gold sodium sulfide solution, and gold ion content controls
In 50g/l or so；The reaction equation of the isothermal reaction is Au (OH)3+4SO3 2-=Au(SO3)2 3-+2SO4 2-+H2O。
Wherein, the concentration of potassium iodide is 40-80g/l in the step 1, and temperature control is between 20-30 degree, and is started
Machinery is stirred.
Wherein, auxiliary agent oxide 2-10g is added in the step 1 in whipping process, and the auxiliary agent is hydrogen peroxide, height
One or more in potassium manganate, sodium peroxydisulfate, and stir to until auxiliary agent oxide is completely dissolved；When dissolution time 2-4 is small.
Wherein, the purity of the high pure gold is 99.99%, and the volume of the mixed solution of the iodine and potassium iodide is
1000ml
Wherein, the actual conditions in the step 2 is：The concentration of sodium hydroxide solution, sodium carbonate liquor or sodium bicarbonate solution
For 100g/l, and content is 10-100ml, and PH is controlled between 8-10；The temperature control of reaction in 30-40 degree, and while add while
Stirring, reaction time 1-3h, untill solution becomes water white transparency by dark-brown and has tan precipitate generation.
Wherein, the step 3 concretely comprises the following steps：Filtering separation of solid and liquid is carried out to obtained gold hydroxide precipitation, is used in combination
3-5 pure water is washed and repeats separation of solid and liquid, precipitates the gold hydroxide after untill being free of iodide ion in washings
The gold hydroxide of high-purity is obtained after being dried between 60-80 degree.
Wherein, if be detected as containing iodide ion:Washings are acidified with 10% dilute sulfuric acid 10-20ml, then use 5-10ml
30% hydrogen peroxide oxidation, the presence of iodide ion is finally judged with starch paper；The reaction equation of the process is：H2O2+2H++2I-→
2H2O+I2。
Wherein, the step 5 concretely comprises the following steps：It is added to the 200g/l's of 100ml in the gold hydroxide of high-purity
In sodium sulfite solution and continuously stir dissolving, 50-60 DEG C of constant temperature, and dissolution time for 3-4 it is small when, the solution after complex reaction
It is changed into from muddiness untill yellow becomes colourless transparent liquid again；Then the concentration of addition 2-10ml is in transparent liquid
The sodium hydroxide solution of 100g/l simultaneously adjusts pH value between 10-12, analyzing and adjust gold concentration for 50g/l or so, and finally
Obtain finished product gold sodium sulfide solution.
The beneficial effects of the invention are as follows：Compared with prior art, it is provided by the invention to be prepared using the molten method of iodine without cyanogen gold salt
Method, this preparation method employs dissolving and preparation that iodine and liquor kalii iodide carry out gold, at the same time in preparation process is produced
It with the addition of cooxidant and carry out acceleration dissolving, improve production efficiency, avoid the wang aqueous solution of severe corrosive, and optimize
Production technology, allows technological operation is more stable, environment influences smaller, and properties of product are more preferably；And this method can realize no toxic gas
Discharge, and process is simple and easy to control, finished product is stable and purity is high.
Embodiment
In order to more clearly state the present invention, the present invention is further described below.
The present invention's prepares the method without cyanogen gold salt using the molten method of iodine, comprises the following steps：
Step 1, the high pure gold of 10g is weighed, the purity of high pure gold is 99.99%, the mixed solution of the iodine and potassium iodide
Volume is 1000ml, is added in the iodine of 20g/l and the mixed solution of the potassium iodide of 40-80g/l and carries out dissolved solution；The step
The reaction equation produced in rapid is I2+I-+H2O=I3 -.H2O,Au+I-+I3 -=AuI4 -；
Step 2, system is reacted after suitable sodium hydroxide solution, sodium carbonate liquor or sodium bicarbonate solution are added in above-mentioned solution
Obtain gold hydroxide precipitation；The reaction equation produced in the step is：2AuI4 -+12OH-=2Au(OH)3+I-+IO3-+3H2O；
Step 3, precipitation is obtained into the gold hydroxide solid of purity higher after multiple washing and filtering；
Step 4, the sodium sulfite solution of 200g/l is prepared；
Step 5, then gold hydroxide sediment is added to prepared sodium sulfite solution and carries out isothermal reaction, solution is from brown
Color muddiness yellowing becomes colorless as terminal again, finally obtains finished product gold sodium sulfide solution, and gold ion content controls
In 50g/l or so；The reaction equation of the isothermal reaction is Au (OH)3+4SO3 2-=Au(SO3)2 3-+2SO4 2-+H2O。
It is provided by the invention that the method without cyanogen gold salt, this preparation are prepared using the molten method of iodine compared to the situation of the prior art
Method employs iodine and liquor kalii iodide carries out the dissolving and preparation of gold, while with the addition of auxiliary oxygen in preparation process is produced
Agent carries out acceleration dissolving, improves production efficiency, avoids the wang aqueous solution of severe corrosive, and optimizes production technology, allows
Technological operation is more stable, environment influences smaller, and properties of product are more preferably；And this method can realize no toxic gas discharge, and process
Simple and easy to control, finished product is stable and purity is high.
In the present embodiment, the concentration of potassium iodide is 40-80g/l in the step 1, and temperature control 20-30 degree it
Between, and start machinery and be stirred.Auxiliary agent oxide 2-10g is added in whipping process, and the auxiliary agent is hydrogen peroxide, Gao Meng
One or more in sour potassium, sodium peroxydisulfate, and stir to until auxiliary agent oxide is completely dissolved；When dissolution time 2-4 is small.
In the present embodiment, the actual conditions in the step 2 is：Sodium hydroxide solution, sodium carbonate liquor or bicarbonate
The concentration of sodium solution is 100g/l, and content is 10-100ml, and PH is controlled between 8-10；The temperature control of reaction is in 30-40
Degree, and stir while adding, reaction time 1-3h, until solution becomes water white transparency by dark-brown and has tan precipitate generation
Untill.
In the present embodiment, the step 3 concretely comprises the following steps：Filtering solid-liquid point is carried out to obtained gold hydroxide precipitation
From, and washed with 3-5 pure water and repeat separation of solid and liquid, by the hydroxide after untill being free of iodide ion in washings
Gold is deposited in dry between 60-80 degree after obtain the gold hydroxide of high-purity.Whether it is detected as containing iodide ion:Washings are used
10% dilute sulfuric acid 10-20ml acidifyings, then 30% hydrogen peroxide oxidation with 5-10ml, finally judge depositing for iodide ion with starch paper
；The reaction equation of the process is：H2O2+2H++2I-→2H2O+I2。
In the present embodiment, the step 5 concretely comprises the following steps：It is added to 100ml's in the gold hydroxide of high-purity
In the sodium sulfite solution of 200g/l and continuously stir dissolving, 50-60 DEG C of constant temperature, and dissolution time for 3-4 it is small when, it is anti-through being complexed
Should after solution be changed into from muddiness untill yellow becomes colourless transparent liquid again；Then the dense of 2-10ml is added in transparent liquid
It is 50g/l or so to spend the sodium hydroxide solution for 100g/l and adjust pH value between 10-12, analyzing and adjusting gold concentration, and
Finally obtain finished product gold sodium sulfide solution.
Preparation method of the present invention specifically includes specific examples below：
Embodiment one：1）Take the high pure gold of 10g（99.99%）It is put into container, the mixing for adding 1000ml iodine and potassium iodide is molten
In liquid, content of iodine 20g/l, iodate potassium concn is 40g/l, and temperature control starts mechanical agitation at 20 degree, is slowly added dropwise double
Oxygen water 2ml, 2 it is small when after be completely dissolved；2）The sodium hydroxide solution 10ml of 100g/l is slowly added into said vesse, pays attention to PH
Control is between 8-10, and temperature control is in 30-40 degree, preferably 30 degree, and stirring while adding, reaction time 1h, solution is by dark brown
Discoloration is into water white transparency and has brown precipitate generation；3）Above-mentioned precipitation is subjected to filtering separation of solid and liquid, and is washed with 100ml pure water
Wash, repeated washing simultaneously filters, and detects washings after 3 times, and the washings of third time are acidified and 30% pair through 10% dilute sulfuric acid 10ml
After oxygen water 5ml oxidations, starch paper detection is free of iodide ion, the gold hydroxide 12.42g of gained high-purity；4）Will be above-mentioned high-purity
The gold hydroxide of degree, which is added in the sodium sulfite solution of the 200g/l of 100ml, continuously stirs dissolving, 50 DEG C of constant temperature, and reaction 3 is small
When, solution is changed into yellow from muddiness and becomes colourless transparent liquid again to being completely dissolved after complex reaction；5）2ml is added in solution
Concentration be 100g/l sodium hydroxide solution adjust pH value to 10.3, it is 50.1g/l to analyze and adjust gold concentration, obtains finished product
Gold sodium sulfide solution 198ml, golden utilization rate is up to 99.2%.After the completion of preparation, the total amount of gained gold sodium sulfide gold it is dense
The grams of degree=gold, the utilization rate % of quality=gold before golden grams ÷ gold dissolvings.
Embodiment two：1）Take the high pure gold of 10g（99.99%）It is put into container, adds the mixed of 1000ml iodine and potassium iodide
Close in solution, content of iodine 20g/l, iodate potassium concn is 40g/l, and temperature control starts mechanical agitation at 20 degree, slowly drop
Increase potassium manganate 4g, 2 it is small when after be completely dissolved；2）The sodium hydroxide solution 10ml of 100g/l is slowly added into said vesse,
PH controls are paid attention between 8-10, and temperature control is in 30-40 degree, preferably 30 degree, stirring while adding, reaction time 1h, solution
Water white transparency is become by dark-brown and has brown precipitate generation；3) above-mentioned precipitation is subjected to filtering separation of solid and liquid, and it is pure with 100ml
Water washing, repeated washing simultaneously filter, and detect washings after 3 times, the washings of third time be acidified through 10% dilute sulfuric acid 10ml and
After 30% hydrogen peroxide 5ml oxidations, starch paper detection is free of iodide ion, the gold hydroxide 12.39g of gained high-purity；4）Will be above-mentioned
The gold hydroxide of high-purity, which is added in the sodium sulfite solution of the 200g/l of 100ml, continuously stirs dissolving, 50 DEG C of constant temperature, reaction
3 it is small when, solution is changed into yellow from muddiness and becomes colourless transparent liquid again to being completely dissolved after complex reaction；5）Added in solution
The sodium hydroxide solution that the concentration of 2ml is 100g/l adjusts pH value to 10.8, and it is 50.0g/l to analyze and adjust gold concentration, is obtained
Finished product gold sodium sulfide solution 198ml, golden utilization rate reach：99%.
Embodiment three, takes the high pure gold of 10g（99.99%）It is put into container, adds the mixing of 1000ml iodine and potassium iodide
In solution, content of iodine 20g/l, iodate potassium concn is 40g/l, and temperature control starts mechanical agitation at 20 degree, is slowly added dropwise
Sodium peroxydisulfate 3g, 2 it is small when after be completely dissolved；（2）, toward the sodium hydroxide solution 10ml that 100g/l is slowly added in said vesse,
PH controls are paid attention between 8-10, and temperature control is in 30-40 degree, preferably 30 degree, stirring while adding, reaction time 1h, solution
Water white transparency is become by dark-brown and has brown precipitate generation；3) above-mentioned precipitation is subjected to filtering separation of solid and liquid, and it is pure with 100ml
Water washing, repeated washing simultaneously filter, and detect washings after 3 times, the washings of third time be acidified through 10% dilute sulfuric acid 10ml and
After 30% hydrogen peroxide 5ml oxidations, starch paper detection is free of iodide ion, the gold hydroxide 12.40g of gained high-purity；4）Will be above-mentioned
The gold hydroxide of high-purity, which is added in the sodium sulfite solution of the 200g/l of 100ml, continuously stirs dissolving, 50 DEG C of constant temperature, reaction
3 it is small when, solution is changed into yellow from muddiness and becomes colourless transparent liquid again to being completely dissolved after complex reaction；5）Added in solution
The sodium hydroxide solution that the concentration of 2ml is 100g/l adjusts pH value to 10.5, and it is 49.9g/l to analyze and adjust gold concentration, is obtained
Finished product gold sodium sulfide solution 198ml, golden utilization rate reach：98.8%.
Disclosed above is only several specific embodiments of the present invention, but the present invention is not limited to this, any ability
What the technical staff in domain can think change should all fall into protection scope of the present invention.
Claims (8)
1. a kind of prepare the method without cyanogen gold salt using the molten method of iodine, it is characterised in that comprises the following steps：
Step 1, the high pure gold of 10g is weighed, is added in the iodine of 20g/l and the mixed solution of the potassium iodide of 40-80g/l and carries out
Dissolved solution；The reaction equation produced in the step is I2+I-+H2O=I3 -.H2O,Au+I-+I3 -=AuI4 -；
Step 2, system is reacted after suitable sodium hydroxide solution, sodium carbonate liquor or sodium bicarbonate solution are added in above-mentioned solution
Obtain gold hydroxide precipitation；The reaction equation produced in the step is：2AuI4 -+12OH-=2Au(OH)3+I-+IO3-+3H2O；
Step 3, precipitation is obtained into the gold hydroxide solid of purity higher after multiple washing and filtering；
Step 4, the sodium sulfite solution of 200g/l is prepared；
Step 5, then gold hydroxide sediment is added to prepared sodium sulfite solution and carries out isothermal reaction, solution is from brown
Color muddiness yellowing becomes colorless as terminal again, finally obtains finished product gold sodium sulfide solution, and gold ion content controls
In 50g/l or so；The reaction equation of the isothermal reaction is Au (OH)3+4SO3 2-=Au(SO3)2 3-+2SO4 2-+H2O。
2. according to claim 1 prepare the method without cyanogen gold salt using the molten method of iodine, it is characterised in that in the step 1
The concentration of potassium iodide is 40-80g/l, and temperature control is between 20-30 degree, and starts machinery and be stirred.
3. according to claim 2 prepare the method without cyanogen gold salt using the molten method of iodine, it is characterised in that in the step 1
Auxiliary agent oxide 2-10g is added in whipping process, and the auxiliary agent is hydrogen peroxide, one kind in potassium permanganate, sodium peroxydisulfate
Or it is a variety of, and stir to until auxiliary agent oxide is completely dissolved；When dissolution time 2-4 is small.
4. according to claim 1 prepare the method without cyanogen gold salt using the molten method of iodine, it is characterised in that the high pure gold
Purity be 99.99%, the volume of the mixed solution of the iodine and potassium iodide is 1000ml.
5. according to claim 1 prepare the method without cyanogen gold salt using the molten method of iodine, it is characterised in that in the step 2
Actual conditions be：The concentration of sodium hydroxide solution, sodium carbonate liquor or sodium bicarbonate solution is 100g/l, and content is 10-
100ml, PH are controlled between 8-10；The temperature control of reaction is stirred while adding in 30-40 degree, reaction time 1-3h,
Untill solution becomes water white transparency by dark-brown and has tan precipitate generation.
6. according to claim 1 prepare the method without cyanogen gold salt using the molten method of iodine, it is characterised in that the step 3
Concretely comprise the following steps：Filtering separation of solid and liquid is carried out to obtained gold hydroxide precipitation, and is washed and repeated solid with 3-5 pure water
Liquid separates, and the gold hydroxide is deposited between 60-80 degree after untill being free of iodide ion in washings and obtains height after drying
The gold hydroxide of purity.
7. according to claim 6 prepare the method without cyanogen gold salt using the molten method of iodine, it is characterised in that whether containing iodine from
Son is detected as:Washings are acidified with 10% dilute sulfuric acid 10-20ml, then 30% hydrogen peroxide oxidation with 5-10ml, finally with shallow lake
Powder test paper judges the presence of iodide ion；The reaction equation of the process is：H2O2+2H++2I-→2H2O+I2。
8. according to claim 1 prepare the method without cyanogen gold salt using the molten method of iodine, it is characterised in that the step 5
Concretely comprise the following steps：It is added in the sodium sulfite solution of the 200g/l of 100ml and continuously stirs in the gold hydroxide of high-purity
When dissolving, 50-60 DEG C of constant temperature, and dissolution time are 3-4 small, solution is changed into yellow from muddiness and becomes colourless again after complex reaction
Untill transparency liquid；Then the concentration that 2-10ml is added in transparent liquid is the sodium hydroxide solution of 100g/l and adjusts PH
Value is 50g/l or so between 10-12, analyzing and adjusting gold concentration, and finally obtains finished product gold sodium sulfide solution.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108754554A (en) * | 2018-09-18 | 2018-11-06 | 泉州益丰贵金属科技有限公司 | A kind of gold plating liquid and a kind of gold plating method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105568269A (en) * | 2015-12-16 | 2016-05-11 | 励福(江门)环保科技股份有限公司 | Preparation method of cyanide-free gold plating reagent sodium gold sulfite |
| 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 |
-
2017
- 2017-12-01 CN CN201711252759.9A patent/CN107986319A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105568269A (en) * | 2015-12-16 | 2016-05-11 | 励福(江门)环保科技股份有限公司 | Preparation method of cyanide-free gold plating reagent sodium gold sulfite |
| 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 |
Non-Patent Citations (1)
| Title |
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| 张亦飞等: "《现代黄金冶炼技术》", 31 October 2014 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108754554A (en) * | 2018-09-18 | 2018-11-06 | 泉州益丰贵金属科技有限公司 | A kind of gold plating liquid and a kind of gold plating method |
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