CN100393898C - Method of recovering silver for silver-containing waste liquid - Google Patents
Method of recovering silver for silver-containing waste liquid Download PDFInfo
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- CN100393898C CN100393898C CNB031583423A CN03158342A CN100393898C CN 100393898 C CN100393898 C CN 100393898C CN B031583423 A CNB031583423 A CN B031583423A CN 03158342 A CN03158342 A CN 03158342A CN 100393898 C CN100393898 C CN 100393898C
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- containing compound
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Abstract
The present invention discloses a method for recovering silver from a silver-containing waste liquid. The method comprises the steps that a soluble metal salt is added into the silver-containing waste liquid to produce silver-containing compound precipitate; after dried to be in the form of granules, the silver-containing compound precipitate is put into a low-temperature plasma machine with hydrogen gas as the work gas to carry out reduction treatment so that silver-containing compounds are converted into a simple substance-silver. The method has the characteristics of low processing temperature, simple manufacturing process, low production cost, short processing time, high productive efficiency, no environment pollution, etc. The method can also be used for recovering other noble metals, such as Au, Ni, Co, Pt, Mo, etc.
Description
Technical field
The present invention relates to a kind of recovery method of noble metal, particularly a kind of method of utilizing the Low Temperature Plasma Treating technology from silver-containing liquid waste, to reclaim silver.
Background technology
As everyone knows, silver is a kind of noble metal, and very high using value is arranged.In industrial production or some other chemical reaction processes, can produce a large amount of silver-containing liquid wastes, the silver that is dissolved in the waste liquid goes out of use, and has not only caused waste, also can produce environmental pollution.Therefore, from silver-containing liquid waste, reclaim silver, turn waste into wealth, turn bane into boon, beyond doubt a positive and significant thing.
At present, from silver-containing liquid waste, reclaim silver-colored method and generally can be divided into electrolytic process and chemical method two big classes.Electrolytic process is electrolytic solution with the silver-containing liquid waste, and stainless steel is a negative electrode, and graphite is anode, adopts direct current to carry out electrolysis, and the silver that generates from negative electrode is stripped down directly becomes product, or with its melting ingot casting again.The subject matter that electrolytic process exists is still to leave a considerable amount of silver can not reclaim fully in final solution, its rate of recovery is less than the chemical method height, and easily cause generating the silver sulfide precipitation, though can adopt ways such as rotating cathode and low current density to reduce the generation of silver sulfide, but many inconveniences are arranged so again, and efficient is very low.
According to the difference of reduction mode, can be divided into two kinds of direct-reduction process and indirect reduction methods in the chemical method.Direct-reduction process is exactly directly to add strong reductant in silver-containing liquid waste, with Ag
+Directly be reduced into argent, then the washing, drying, the melting ingot casting gets final product.Indirect reduction method is called sodium sulfide method again, and leaching process is: add sodium sulfide solution earlier in silver-containing liquid waste, with Ag
+Post precipitation filters with decantation and suction method fully, washes.Silver sulfide after cleaning can make argent with methods such as aluminium powder high temperature reduction method, iron high temperature reduction method, wet method iron reduction method, sodium carbonate fusion reduction method and high-temperature roasting methods.
Be not difficult to find out above-mentioned from silver-containing liquid waste, the recovery in the silver-colored method, adopt the electrolytic process energy consumption big, and silver raising recovery rate be lower; And in chemical process, needing higher temperature, energy consumption is bigger, and is more serious to the damage ratio of environment.
Summary of the invention
The objective of the invention is to overcome the deficiency that prior art exists, provide a kind of practical, the processing efficiency height, cost is low, and does not produce the method for the recovery silver of environmental pollution.
For achieving the above object, the method that from silver-containing liquid waste, reclaims silver of the present invention, the technical scheme that adopts is: add soluble metallic salt in silver-containing liquid waste, generation Ag-containing compound precipitation, after described drying precipitate is processed into particulate state, it is carried out plasma deoxidization in low termprature handle, the working gas of adding is a hydrogen, and argentiferous chemical combination is converted into simple substance silver.
In the technique scheme, described plasma deoxidization in low termprature is handled, and the treatment time is 3～5 minutes, and power is 60～100W, and the working vacuum degree is 40～50Pa; Described working gas is the mixed gas of hydrogen and rare gas element.
Further technical scheme, dried particulate state Ag-containing compound can also be made Powdered after, carry out plasma deoxidization in low termprature again and handle.
Because the technique scheme utilization, the present invention compared with prior art has following advantage:
The present invention is owing to adopted the low-temperature plasma method at H
2Under the atmosphere Ag-containing compound is handled, under the vacuum plasma state, high energy H ion has very strong reducing activity, Ag-containing compound can be precipitated (as Ag
2S, AgCl etc.) reduction reaction takes place with H, thereby generate simple substance silver, therefore, compared with prior art, have processing temperature low (room temperature), technology is simple, production cost is low, the treatment time is relatively short, production efficiency is high, and outstanding advantage such as non-environmental-pollution.
Embodiment
Below in conjunction with embodiment the present invention is further described:
Embodiment one: a kind of method that reclaims silver from silver-containing liquid waste, wherein, silver-containing liquid waste is the waste liquid after stop bath uses.At ambient temperature sodium sulphite is configured to concentration and is 20% sodium sulfide solution, with above-mentioned Na
2S solution joins in the waste fixer solution, stirs while adding, and generates Ag-containing compound Ag
2The S precipitation; Left standstill 24 hours after precipitation is complete, drip 1～2 20% Na again on the upper strata in the stillness of night
2S solution, check Ag
+Restore All whether; Treat Ag
+After the reduction, filter Ag fully with the decompress filter method
2S is with the rare HNO of 0.1mol/l
3Wash 2～3 times, to remove impurity, use deionized water wash again 2～3 times, in order to the residual HNO of flush away
3, and with the Ag of gained
2S is deposited under 100 ℃ of conditions and is dried into particulate state.
Dried particulate state silver sulfide is ground to form finely powdered, be placed in the plasma processor, plasma processor adopts radio-frequency power supply, jigger coupling form, feeds high-purity hydrogen in vacuum chamber, at H
2Under the reducing atmosphere, open radio-frequency power supply, handled 3 minutes under power 80W, working vacuum degree 40Pa condition, the silver sulfide particle is converted into simple substance silver.
Embodiment two: a kind of method that reclaims silver from silver-containing liquid waste, wherein, silver-containing liquid waste is the argentiferous electroplating effluent after using.At ambient temperature NaCl is configured to concentration and is 30% sodium chloride solution, above-mentioned NaCl solution is joined in the spent plating bath, stir while adding, generate Ag-containing compound AgCl precipitation; Left standstill 24 hours after precipitation is complete, drip 1～2 30% NaCl solution again on the upper strata in the stillness of night, check Ag
+Restore All whether; Treat Ag
+After the reduction, filter AgCl fully, with the rare HNO of 0.1mol/l with the decompress filter method
3Wash 2～3 times, to remove impurity, use deionized water wash again 2～3 times, in order to the residual HNO of flush away
3, and the AgCl of gained is deposited under 100 ℃ of conditions is dried into particulate state.
Dried particulate state silver chloride is placed plasma processor, plasma processor adopts radio-frequency power supply, condenser coupling form, in vacuum chamber, feed the mixed gas of high-purity hydrogen and argon gas, open radio-frequency power supply, handled 4 minutes under power 90W, working vacuum degree 40Pa condition, silver chloride particle is converted into simple substance silver.
Adopt the foregoing description 1 or 2 described low-temperature plasmas to reclaim the method for silver from silver-containing liquid waste, same principle can be used for reclaiming these noble metals from the waste liquid that contains metals such as Au, Ni, Co, Pt, Mo.
Claims (3)
1. one kind is reclaimed silver-colored method from silver-containing liquid waste, in silver-containing liquid waste, add soluble metallic salt, generation Ag-containing compound precipitation, it is characterized in that: after described drying precipitate is processed into particulate state, it is carried out plasma deoxidization in low termprature handles, the working gas that adds is a hydrogen, and Ag-containing compound is converted into simple substance silver.
2. the method that from silver-containing liquid waste, reclaims silver according to claim 1, it is characterized in that: the plasma deoxidization in low termprature treatment time is 3～5 minutes, and power is 60～100 watts, and the working vacuum degree is 40～50Pa.
3. the method that reclaims silver from silver-containing liquid waste according to claim 1 is characterized in that: dried particulate state Ag-containing compound is made Powdered, carried out plasma deoxidization in low termprature again and handle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031583423A CN100393898C (en) | 2003-09-24 | 2003-09-24 | Method of recovering silver for silver-containing waste liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031583423A CN100393898C (en) | 2003-09-24 | 2003-09-24 | Method of recovering silver for silver-containing waste liquid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1526839A CN1526839A (en) | 2004-09-08 |
| CN100393898C true CN100393898C (en) | 2008-06-11 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB031583423A Expired - Fee Related CN100393898C (en) | 2003-09-24 | 2003-09-24 | Method of recovering silver for silver-containing waste liquid |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101705359B (en) * | 2009-11-10 | 2011-03-09 | 南京信息工程大学 | Method for recovering silver in silver-containing waste water by biological method |
| CN102747234A (en) * | 2011-04-22 | 2012-10-24 | 苏州市奥普斯等离子体科技有限公司 | Method for recovering silver from silver-containing waste liquid |
| CN111057864A (en) * | 2019-12-25 | 2020-04-24 | 苏州希图环保科技有限公司 | Process for recovering silver from waste liquid of photosensitive material |
| CN112730142B (en) * | 2020-12-02 | 2022-12-30 | 昆山鸿福泰环保科技有限公司 | Method for detecting silver content in silver-containing waste liquid based on gravimetric method |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4740244A (en) * | 1986-10-31 | 1988-04-26 | E. I. Du Pont De Nemours And Company | Process for recovery of silver from spent, waste, acidic processing fluids |
| US4755453A (en) * | 1986-06-11 | 1988-07-05 | The Governors Of The University Of Alberta | Method for recovering silver from waste solutions containing thiosulfate compounds |
| CN1060162A (en) * | 1990-09-29 | 1992-04-08 | 中国有色金属工业总公司昆明贵金属研究所 | Method for recovering silver from waste color photosensitive material |
| CN1118015A (en) * | 1993-11-18 | 1996-03-06 | 中国有色金属工业总公司昆明贵金属研究所 | Method for recovering silver from trace silver waste liquid |
| CN1122836A (en) * | 1995-07-14 | 1996-05-22 | 西藏藏药天然药物研究开发中心 | Method for recovering silver from waste liquor containing silver chloride |
| US5536387A (en) * | 1994-05-06 | 1996-07-16 | United Kingdom Atomic Energy Authority | Silver removal |
-
2003
- 2003-09-24 CN CNB031583423A patent/CN100393898C/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4755453A (en) * | 1986-06-11 | 1988-07-05 | The Governors Of The University Of Alberta | Method for recovering silver from waste solutions containing thiosulfate compounds |
| US4740244A (en) * | 1986-10-31 | 1988-04-26 | E. I. Du Pont De Nemours And Company | Process for recovery of silver from spent, waste, acidic processing fluids |
| CN1060162A (en) * | 1990-09-29 | 1992-04-08 | 中国有色金属工业总公司昆明贵金属研究所 | Method for recovering silver from waste color photosensitive material |
| CN1118015A (en) * | 1993-11-18 | 1996-03-06 | 中国有色金属工业总公司昆明贵金属研究所 | Method for recovering silver from trace silver waste liquid |
| US5536387A (en) * | 1994-05-06 | 1996-07-16 | United Kingdom Atomic Energy Authority | Silver removal |
| CN1122836A (en) * | 1995-07-14 | 1996-05-22 | 西藏藏药天然药物研究开发中心 | Method for recovering silver from waste liquor containing silver chloride |
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| CN1526839A (en) | 2004-09-08 |
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