CN103740935A - Method for recovering ruthenium from ruthenium electroplating main salt waste material - Google Patents
Method for recovering ruthenium from ruthenium electroplating main salt waste material Download PDFInfo
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- CN103740935A CN103740935A CN201310719019.7A CN201310719019A CN103740935A CN 103740935 A CN103740935 A CN 103740935A CN 201310719019 A CN201310719019 A CN 201310719019A CN 103740935 A CN103740935 A CN 103740935A
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Abstract
The invention discloses a method for recovering ruthenium from a ruthenium electroplating main salt waste material. The invention relates to the technical fields of precious metal ruthenium recovery and precious metal chemical industry, aims to provide a method for recovering ruthenium from the ruthenium electroplating main salt waste material, and particularly relates to a method for recovering precious metal ruthenium from a ruthenium-containing waste material produced in the production process of ruthenium electroplating main salt potassium (mu-nitrido-bis[terachloroaquoruthenate (IV)]) through a fire-wet combined process and preparing high-purity ruthenium powder through purifying the precious metal ruthenium. Potassium ions in the organic ruthenium waste material are removed through an ion exchange column; then the organic ruthenium waste material is distilled and concentrated viscous paste in a beaker; then, the viscous paste is calcined in a porcelain bowl, and a calcined product is taken out and ground into powder, thus obtaining precious metal ruthenium concentrate; and hydrogen is introduced for reducing the precious metal ruthenium concentrate into high-purity ruthenium powder. The method disclosed by the invention has the characteristics of concise technological process, high recovery rate of precious metal and high product purity; the ruthenium recovery rate is above 99.1% and the ruthenium powder purity is above 99.99%.
Description
Technical field
The invention belongs to precious metal chemical technology field, relate to a kind of from there being ruthenium to electroplate the method that reclaims ruthenium main waste salt, more precisely from produce ruthenium electroplate main salt ([μ-nitrogen-bis-(tetrachloro one hydration ruthenium)] sour potassium) process, produce containing in ruthenium waste material, fiery wet method combined recovery noble ruthenium is also reduced to the method for high-purity ruthenium powder.
Background technology
Platinum metals, as the raw material of making all kinds of chemical catalysts and all kinds of electronic chemical products, is subject to the attention of every profession and trade.Ruthenium is the very special element of character in platinum metals, has the features such as fusing point is high, hardness is large.Although the range of application of ruthenium powder does not have other noble metal powders so extensive, ruthenium powder has vital role at aspects such as unicircuit, organic synthesis.The topmost application of ruthenium powder is at present to produce ruthenium target, uses the material with memory of ruthenium target scheduler hard disk.Ruthenium target dimensions of market is large, and added value is high, thereby is subject to great attention.The performance of ruthenium is similar with rhodium, as high rigidity and corrosion resistance nature.But the cost ratio rhodium of ruthenium is cheaply a lot, and the internal stress of plating ruthenium is lower than rhodium plating.The development of electroplating ruthenium will be very attractive, and it even likely replaces rhodium plating.Electroplating ruthenium is widely used in the functional electronics product plating such as magnetic wire switch, rly., junctor and decorates in plating.[μ-nitrogen-bis-(tetrachloro one hydration ruthenium)] sour potassium is the main salt that a kind of ruthenium is electroplated use, and chemical structure is as follows:
Produce ruthenium and electroplate in main salt ([μ-nitrogen-bis-(tetrachloro one hydration ruthenium)] sour potassium) process and can generation contain ruthenium waste material, for the better noble ruthenium reclaiming in waste material, prepare high-purity ruthenium powder, invented following technique.
Summary of the invention
The object of this invention is to provide a kind of method of preparing high-purity ruthenium powder from organic ruthenium waste material, technical problem to be solved by this invention is that fiery wet method combined recovery noble ruthenium is prepared high-purity ruthenium powder.
Enriching method of the present invention is divided into five steps: (1) ion-exchange takes off potassium; (2) distillation and concentration; (3) high-temperature calcination; (4) grinding flour; (5) logical hydrogen reduction.
(1) the de-potassium of ion-exchange: using natural clinoptilolite is put into ion exchange column as sorbent material, make ruthenium electroplate main bisulfate waste liquor and carry out ion-exchange removal potassium ion by exchange column,
(2) distillation and concentration: will put into beaker containing liquid after the exchange of ruthenium organic waste materials and keep 70 ~ 85 ℃ of slow distillation and concentrations of temperature to pasty state;
(3) high-temperature calcination: pasty state waste material is made to pelletizing and put into porcelain alms bowl and be built in chamber type electric resistance furnace, the calcining that heats up, further volatilizees organic matter and Cl ion, 800 ℃ of calcining temperatures, time 0.5 ~ 2h;
(4) grinding flour: after calcining, material is used ball mill grinding powder process, and after grinding flour, raw meal particle size need reach 100 ~ 200 orders;
(5) logical hydrogen reduction: powdered solid fuel is put into quartz boat, put into the logical hydrogen reduction of tube furnace, 700 ~ 850 ℃ of reduction temperatures, recovery time 1h.
The material that the present invention uses for produce ruthenium electroplate in main salt ([μ-nitrogen-bis-(tetrachloro one hydration ruthenium)] sour potassium) process, produce containing ruthenium waste material.
What ion-exchange of the present invention was used is that using natural clinoptilolite is as sorbent material.
What distillation and concentration of the present invention was used is the slowly method of distillation of low temperature.
The present invention uses ball mill to carry out material grinding flour.
The reductive agent that the present invention uses is hydrogen.
The present invention is prepared into high-purity ruthenium powder by hydrogen reduction, the technical indicator of acquisition:
(1) ruthenium content of ruthenium powder is not less than 99.99%;
(2) rate of recovery of precious metal is greater than 99.1%.
Advantage of the present invention is mainly: technique is simple, low cost, the rate of recovery are high.Adopt the inventive method, prepare gained ruthenium grade powder and be greater than 99.99%, the noble ruthenium rate of recovery is greater than 99.1%.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Accompanying drawing 1 is process flow diagram of the present invention.
Embodiment
Embodiment 1, referring to accompanying drawing 1, the production ruthenium that experiment takes 1L electroplate in main salt ([μ-nitrogen-bis-(tetrachloro one hydration ruthenium)] sour potassium) process, produce containing ruthenium waste material, by using natural clinoptilolite ion-exchange, except after potassium, 70 ℃ of distillation and concentrations are to pasty state.Ball processed is put into 800 ℃ of calcinings of chamber type electric resistance furnace, and time 0.5h is ground to waste material after calcining after 150 orders, puts into 750 ℃ of logical hydrogen reductions of tube furnace.After 1h, cooling is taken out, and obtains high-purity ruthenium powder, and grade is greater than 99.99%, the rate of recovery 99.1%.
Embodiment 2, referring to accompanying drawing 1, the production ruthenium that experiment takes 1L electroplate in main salt ([μ-nitrogen-bis-(tetrachloro one hydration ruthenium)] sour potassium) process, produce containing ruthenium waste material, by using natural clinoptilolite ion-exchange, except after potassium, 75 ℃ of distillation and concentrations are to pasty state.Ball processed is put into 800 ℃ of calcinings of chamber type electric resistance furnace, and time 1h is ground to waste material after calcining after 150 orders, puts into 750 ℃ of logical hydrogen reductions of tube furnace.After 1h, cooling is taken out, and obtains high-purity ruthenium powder, and grade is greater than 99.99%, the rate of recovery 99.1%.
Embodiment 3, referring to accompanying drawing 1, the production ruthenium that experiment takes 1L electroplate in main salt ([μ-nitrogen-bis-(tetrachloro one hydration ruthenium)] sour potassium) process, produce containing ruthenium waste material, by using natural clinoptilolite ion-exchange, except after potassium, 80 ℃ of distillation and concentrations are to pasty state.Ball processed is put into 800 ℃ of calcinings of chamber type electric resistance furnace, and time 1.5h is ground to waste material after calcining after 150 orders, puts into 800 ℃ of logical hydrogen reductions of tube furnace.After 1h, cooling is taken out, and obtains high-purity ruthenium powder, and grade is greater than 99.99%, the rate of recovery 99.1%.
Embodiment 4, referring to accompanying drawing 1, the production ruthenium that experiment takes 1L electroplate in main salt ([μ-nitrogen-bis-(tetrachloro one hydration ruthenium)] sour potassium) process, produce containing ruthenium waste material, by using natural clinoptilolite ion-exchange, except after potassium, 85 ℃ of distillation and concentrations are to pasty state.Ball processed is put into 850 ℃ of calcinings of chamber type electric resistance furnace, and time 2h is ground to waste material after calcining after 150 orders, puts into 850 ℃ of logical hydrogen reductions of tube furnace.After 1h, cooling is taken out, and obtains high-purity ruthenium powder, and grade is greater than 99.99%, the rate of recovery 99.1%.
Claims (6)
1. from there being ruthenium to electroplate a method that reclaims ruthenium main waste salt, it is characterized in that completing according to the following steps:
(1) the de-potassium of ion-exchange: using natural clinoptilolite is put into ion exchange column as sorbent material, make ruthenium electroplate main bisulfate waste liquor by exchange column, and wash sorbent material;
(2) distillation and concentration: liquid after exchange is put into beaker, and heating distillation and concentration is to pasty state;
(3) high-temperature calcination: pasty solid is put into porcelain alms bowl and be built in chamber type electric resistance furnace, calcining heats up;
(4) grinding flour: material after calcining is ground to powdery;
(5) logical hydrogen reduction: powdered solid fuel is put into quartz boat and insert tube furnace, heat up and pass into hydrogen reducing, obtain ruthenium powder product.
2. according to claim 1ly a kind ofly from ruthenium, electroplate the method that reclaims ruthenium main waste salt, it is characterized in that the described ion-exchange of step (1) used using natural clinoptilolite as sorbent material k adsorption ion.
3. according to claim 1ly a kind ofly from ruthenium, electroplate the method that reclaims ruthenium main waste salt, it is characterized in that the described distillation and concentration temperature of step (2) is controlled at 70～85 ℃ and slowly carries out.
4. according to claim 1ly a kind ofly from ruthenium, electroplate the method that reclaims ruthenium main waste salt, it is characterized in that the described calcining temperature of step (3) is 800 ℃, time 0.5～2h.
5. according to claim 1ly a kind ofly from ruthenium, electroplate the method that reclaims ruthenium main waste salt, it is characterized in that the described grinding flour of step (4) after raw meal particle size need reach-100～200 orders.
6. according to claim 1ly a kind ofly from ruthenium, electroplate the method that reclaims ruthenium main waste salt, it is characterized in that the described logical hydrogen reduction temperature of step (5) is 700～850 ℃, slowly heat up, reach and reduce 1h after temperature.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110616330A (en) * | 2019-09-30 | 2019-12-27 | 江苏奇纳新材料科技有限公司 | Method for recovering rare and noble metals in rhenium-containing high-temperature alloy waste |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101509077A (en) * | 2009-02-19 | 2009-08-19 | 昆明贵金属研究所 | Method for extracting platinum, palladium, rhodium from automotive catalyst of ore phase reconstruction |
| CN101583729A (en) * | 2006-11-21 | 2009-11-18 | 株式会社古屋金属 | Method for recovering ruthenium |
| CN103253686A (en) * | 2013-05-03 | 2013-08-21 | 广东顺德弘顺达环保产业技术投资有限公司 | Method for producing vegetalitas fulvic acid/potassium sulfate concentrated solution/vegetalitas organic bacterial manure by utilizing alcohol biologic wastewater |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101583729A (en) * | 2006-11-21 | 2009-11-18 | 株式会社古屋金属 | Method for recovering ruthenium |
| CN101509077A (en) * | 2009-02-19 | 2009-08-19 | 昆明贵金属研究所 | Method for extracting platinum, palladium, rhodium from automotive catalyst of ore phase reconstruction |
| CN103253686A (en) * | 2013-05-03 | 2013-08-21 | 广东顺德弘顺达环保产业技术投资有限公司 | Method for producing vegetalitas fulvic acid/potassium sulfate concentrated solution/vegetalitas organic bacterial manure by utilizing alcohol biologic wastewater |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110616330A (en) * | 2019-09-30 | 2019-12-27 | 江苏奇纳新材料科技有限公司 | Method for recovering rare and noble metals in rhenium-containing high-temperature alloy waste |
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Application publication date: 20140423 |