CN102502777A - Method for preparing silver nitrate with various types of silver-ion-containing waste water as raw materials - Google Patents
Method for preparing silver nitrate with various types of silver-ion-containing waste water as raw materials Download PDFInfo
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- CN102502777A CN102502777A CN2011103355153A CN201110335515A CN102502777A CN 102502777 A CN102502777 A CN 102502777A CN 2011103355153 A CN2011103355153 A CN 2011103355153A CN 201110335515 A CN201110335515 A CN 201110335515A CN 102502777 A CN102502777 A CN 102502777A
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Abstract
The invention discloses a method for preparing silver nitrate with various types of silver-ion-containing waste water as raw materials, which is characterized in that an organic solvent is added to the silver-ion-containing waste water to extract organic matter by dissolving, ascorbic acid is then used for complexing of silver ions, and then silver nitrate is prepared through redox and nitration of concentrated nitric acid. According to the method, the ascorbic acid and metal ions can form complex compound to extract silver, then concentrated nitric acid is added, and the silver nitrate can be prepared through redox and nitratlon reaction. The method is simple in process, easy to operate, high in recovery rate and low in cost, does not require high temperature and high pressure in the whole process, has low requirement for equipment, and greatly lowers production cost of products. In addition, the recovered silver nitrate can be directly utilized.
Description
Technical field
The invention belongs to the chemical and medicine industry field, specifically, relate to a kind of method that is the feedstock production Silver Nitrate with various argentiferous ion waste waters.
Background technology
In organic synthesis, Silver Nitrate can improve chemical reaction rate as catalysts.But reaction itself is intricate, and a reaction usually is accompanied by several side reactions, the quite difficulty so the recovery of catalyzer becomes, and the price of precious metal silver was climbed to a higher point successively in recent years, and the recovery of precious metal silver is imperative.Along with the fast development of sensitive materials industry and electronic industry, the consumption surge of Silver Nitrate seeks to increase the raw material of Silver Nitrate output and the focus that the technology new channel has become research.The recovery of silver in the prior art mainly still adds hydrochloric acid and generates deposition, and high temperature sintering reclaims silver then, but this law is higher to equipment requirements.
Summary of the invention
For solving above technical problem, the object of the present invention is to provide that a kind of technology is simple, the recovery is high with the various argentiferous ion waste waters method that is the feedstock production Silver Nitrate.
The present invention seeks to realize like this:
A kind of method that is the feedstock production Silver Nitrate with various argentiferous ion waste waters; Its key is: add organic solvent separated and dissolved in the argentiferous ion waste water and go out organism; Utilize the xitix complexing to go out silver ions again, then with concentrated nitric acid oxidation reduction, nitrated and then make Silver Nitrate.
Specifically carry out as follows:
(1) the argentiferous ion waste water is used organic solvent extraction, separatory discards organic layer and gets water layer; In practical application, can be according to circumstances with the argentiferous ion waste water with the appropriate amount of organic extracted twice or more than twice.
(2) stir down, in the treated water layer, add xitix, 40～80 ℃ were reacted 30～120 minutes, and reaction is reduced to room temperature after finishing, and crosses to filter filter cake xitix silver complex;
(3) filter cake xitix silver complex is changed over to reaction kettle, stir down and drip concentrated nitric acid solution, drip and finish, control reaction temperature is 25～60 ℃ of stirring reactions 30～60 minutes, redox, nitrated nitric acid synthesis silver;
(4) with the reaction solution concentrating under reduced pressure, cooling was cooled to crystallization below 10～15 ℃ more than 60 minutes, and suction filtration, centrifugal, washing, 80～90 ℃ of dryings get product more than 120 minutes.
Before carrying out this art breading, need detect concentration, the content of silver ions in the waste water earlier.
The amount of above-mentioned adding xitix be that silver ions detects quality in the water 150～300%.
The above-mentioned concentration of nitric acid that adds to the xitix silver complex is 60～65%, and consumption detects 110～150% of quality with silver ions.
Organic organic solvent is trichloromethane, methylene dichloride, ETHYLE ACETATE or sherwood oil in the above-mentioned separated and dissolved silver ions waste water.
Beneficial effect: this law of the present invention is utilized xitix to form complex compound with metals ion and is extracted silver, adds concentrated nitric acid oxidation reduction then, nitration reaction is produced Silver Nitrate; Technology is simple, and is easy to operate, and the recovery is high, and is with low cost, and the Silver Nitrate that reclaims can directly utilize, and whole process does not need high temperature, high pressure, and is lower to equipment requirements yet, greatly reduces production cost of products.
Embodiment
Embodiment 1
Example 1: 200Kg silver-containing waste water (containing silver concentration through analysis is 1%) is added in the 500L reaction kettle; Add trichloromethane 100Kg, stirred 10 minutes, leave standstill 30 minutes separatory and discard the trichloromethane layer; Add trichloromethane 100Kg once more; Stirred 10 minutes, and left standstill 30 minutes separatory and discard the trichloromethane layer, get water layer.Stir down, in the treated water layer, add the 2.5Kg xitix, steam is warmed up to 50 ℃ of reactions 60 minutes.Be cooled to 25 ℃, blowing, mistake filter filter cake xitix silver complex 6.2Kg.6.2Kg changes the reaction kettle to 30L over to filter cake xitix silver complex, stirs down and drips 65% concentrated nitric acid 6.0Kg, drips and finishes, and is warmed up to 60 ℃, stirring reaction 45 minutes.Reaction solution is evaporated to certain volume, and cooling is cooled to 10 ℃ of crystallizations 60 minutes, suction filtration, centrifugal, small amount of ethanol washing leaching cake, 120 minutes 1.8Kg that get product of 90 ℃ of dryings.
Example 2: silver-containing waste water 300Kg (containing silver concentration through analysis is 1.5%) is transferred in the 500L reaction kettle; Add methylene dichloride 150Kg, stirred 10 minutes, leave standstill 30 minutes separatory and discard dichloromethane layer; Add methylene dichloride 150Kg once more; Stirred 10 minutes, and left standstill 30 minutes separatory and discard dichloromethane layer, get water layer.Stir down, in the treated water layer, add the 6.5Kg xitix, be warmed up to 60 ℃ of reactions 45 minutes.Be cooled to 25 ℃, blowing, mistake filter filter cake xitix silver complex 12Kg.6.2Kg changes the reaction kettle to 50L over to filter cake xitix silver complex, stirs down and drips 65% concentrated nitric acid 15Kg, drips and finishes, and is warmed up to 60 ℃, stirring reaction 45 minutes.Reaction solution is evaporated to certain volume, and cooling is cooled to 10 ℃ of crystallizations 60 minutes, suction filtration, centrifugal, small amount of ethanol washing leaching cake, 120 minutes 4.2Kg that get product of 90 ℃ of dryings.
Example 3: 1000Kg silver-containing waste water (containing silver concentration through analysis is 1%) is added in the 2500L reaction kettle; Add ETHYLE ACETATE 600Kg, stirred 10 minutes, leave standstill 30 minutes separatory and discard ethyl acetate layer; Add ETHYLE ACETATE 400Kg once more; Stirred 10 minutes, and left standstill 30 minutes separatory and discard ethyl acetate layer, get water layer.Stir down, in the treated water layer, add the 7.5Kg xitix, steam is warmed up to 50 ℃ of reactions 60 minutes.Be cooled to 25 ℃, blowing, mistake filter filter cake xitix silver complex 31Kg.31Kg changes the reaction kettle to 150L over to filter cake xitix silver complex, stirs down and drips 65% concentrated nitric acid 30.0Kg, drips and finishes, and is warmed up to 60 ℃, stirring reaction 45 minutes.Reaction solution is evaporated to certain volume, and cooling is cooled to 10 ℃ of crystallizations 60 minutes, suction filtration, centrifugal, small amount of ethanol washing leaching cake, 120 minutes 9.0Kg that get product of 90 ℃ of dryings.
Example 4: 2000Kg silver-containing waste water (containing silver concentration through analysis is 1%) is added in the 5000L reaction kettle; Add sherwood oil 1200Kg, stirred 10 minutes, leave standstill 30 minutes separatory and discard petroleum ether layer; Add sherwood oil 800Kg once more; Stirred 10 minutes, and left standstill 30 minutes separatory and discard petroleum ether layer, get water layer.Stir down, in the treated water layer, add the 15Kg xitix, steam is warmed up to 50 ℃ of reactions 60 minutes.Be cooled to 25 ℃, blowing, mistake filter filter cake xitix silver complex 62Kg.62Kg changes the reaction kettle to 300L over to filter cake xitix silver complex, stirs down and drips 65% concentrated nitric acid 60.0Kg, drips and finishes, and is warmed up to 60 ℃, stirring reaction 45 minutes.Reaction solution is evaporated to certain volume, and cooling is cooled to 10 ℃ of crystallizations 60 minutes, suction filtration, centrifugal, small amount of ethanol washing leaching cake, 120 minutes 18.0Kg that get product of 90 ℃ of dryings.
Claims (5)
1. method that is the feedstock production Silver Nitrate with various argentiferous ion waste waters; It is characterized in that: add organic solvent separated and dissolved in the argentiferous ion waste water and go out organism; Utilize the xitix complexing to go out silver ions again, then with concentrated nitric acid oxidation reduction, nitrated and then make Silver Nitrate.
2. according to the said method that is the feedstock production Silver Nitrate with various argentiferous ion waste waters of claim 1, it is characterized in that specifically being pressed into down step carries out:
(1) the argentiferous ion waste water is used organic solvent extraction, separatory discards organic layer and gets water layer;
(2) stir down, in the treated water layer, add xitix, 40～80 ℃ were reacted 30～120 minutes, and reaction is reduced to room temperature after finishing, and crosses to filter filter cake xitix silver complex;
(3) filter cake xitix silver complex is changed over to reaction kettle, stir down and drip concentrated nitric acid solution, drip and finish, control reaction temperature is 25～60 ℃ of stirring reactions 30～60 minutes, redox, nitrated nitric acid synthesis silver;
(4) with the reaction solution concentrating under reduced pressure, cooling was cooled to crystallization below 10～15 ℃ more than 60 minutes, and suction filtration, centrifugal, washing, 80～90 ℃ of dryings get product more than 120 minutes.
3. according to claim 1 or the 2 said methods that are the feedstock production Silver Nitrate with various argentiferous ion waste waters, it is characterized in that: the amount of said adding xitix be that silver ions detects quality in the water 150～300%.
4. according to claim 1 or the 2 said methods that are the feedstock production Silver Nitrate with various argentiferous ion waste waters, it is characterized in that: the said concentration of nitric acid that adds to the xitix silver complex is 60～65%, and consumption detects 110～150% of quality with silver ions.
5. according to claim 1 or the 2 said methods that are the feedstock production Silver Nitrate with various argentiferous ion waste waters, it is characterized in that: organic organic solvent is trichloromethane, methylene dichloride, ETHYLE ACETATE or sherwood oil in the said separated and dissolved silver ions waste water.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103738035A (en) * | 2013-10-21 | 2014-04-23 | 江阴华东装饰材料有限公司 | Antifouling antibacterial high-molecular furniture decorative film and preparation method thereof |
| CN105293561A (en) * | 2015-11-05 | 2016-02-03 | 南昌航空大学 | Method for preparing needle-shaped Ag2S microparticles through organic molten salt method |
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| US5749940A (en) * | 1996-05-27 | 1998-05-12 | Nippon Mining & Metals Co., Inc. | Method for producing high grade reduced silver |
| CN101838012A (en) * | 2010-05-07 | 2010-09-22 | 南京化工职业技术学院 | Method for recovering silver sulfate from CODCr measuring waste liquid |
| CN102180511A (en) * | 2010-12-19 | 2011-09-14 | 何侠 | Method for preparing silver nitrate and aluminum nitrate hexahydrate by waste silver catalyst in ethane oxidation |
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2011
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5749940A (en) * | 1996-05-27 | 1998-05-12 | Nippon Mining & Metals Co., Inc. | Method for producing high grade reduced silver |
| CN101838012A (en) * | 2010-05-07 | 2010-09-22 | 南京化工职业技术学院 | Method for recovering silver sulfate from CODCr measuring waste liquid |
| CN102180511A (en) * | 2010-12-19 | 2011-09-14 | 何侠 | Method for preparing silver nitrate and aluminum nitrate hexahydrate by waste silver catalyst in ethane oxidation |
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| 刘奇等: "抗坏血酸络合活性炭吸附光度法测定痕量银", 《河南师范大学学报(自然科学版)》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103738035A (en) * | 2013-10-21 | 2014-04-23 | 江阴华东装饰材料有限公司 | Antifouling antibacterial high-molecular furniture decorative film and preparation method thereof |
| CN103738035B (en) * | 2013-10-21 | 2015-07-15 | 江阴华东装饰材料有限公司 | Antifouling antibacterial high-molecular furniture decorative film and preparation method thereof |
| CN105293561A (en) * | 2015-11-05 | 2016-02-03 | 南昌航空大学 | Method for preparing needle-shaped Ag2S microparticles through organic molten salt method |
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Effective date of registration: 20170126 Address after: 401221 Changshou District, Chongqing city in the middle of the road No. 7 Patentee after: Chongqing Kangpu Formosan Union Chemical Corporation Address before: 401121 Yubei District City, the northern part of the New District of Chongqing avenue of stars on the ground floor, No. 60 Venus science and technology incubator center, building 17 Patentee before: Chongqing Hallochem Pharma Co.,Ltd. |