CN111534700A - Method for recovering residual precious metals in platinum purification wastewater - Google Patents
Method for recovering residual precious metals in platinum purification wastewater Download PDFInfo
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- CN111534700A CN111534700A CN202010588835.9A CN202010588835A CN111534700A CN 111534700 A CN111534700 A CN 111534700A CN 202010588835 A CN202010588835 A CN 202010588835A CN 111534700 A CN111534700 A CN 111534700A
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- wastewater
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- hydrazine hydrate
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The application relates to the field of recovery of platinum purification wastewater, in particular to a recovery method of residual precious metals in platinum purification wastewater, and solves the problem of high wastewater treatment cost caused by high content of precious metals in platinum purification wastewater. The process comprises the following steps: adding wastewater into a reaction container, starting stirring, adding sodium hydroxide into the wastewater to adjust the pH value of the wastewater to 9-10, adding hydrazine hydrate with the mass fraction of 50% into the wastewater to reduce the precious metals in the wastewater, continuously stirring and reducing for 1.5-3 hours, standing the wastewater for more than 5 hours after stirring, reducing and precipitating the precious metal residues in the wastewater, filtering residual liquid in the reaction container to obtain recycled precious metals, wherein the content of Pt in the residual liquid is less than 1mg/L, and the content of other precious metals is less than 0.2 mg/L. The method can greatly reduce the content of noble metals in the wastewater and reduce the treatment cost of the wastewater.
Description
Technical Field
The application relates to the field of recovery of platinum purification wastewater, in particular to a recovery method of residual precious metals in platinum purification wastewater.
Background
Platinum (Pt) is a naturally occurring white precious metal, which is chemically stable and superior, and can be used as a jewelry ornament or an artwork, as a catalyst in advanced chemical vessels, platinum crucibles, electrodes or chemical reactions, and further, in the field of special materials, platinum can be used as an important raw material for producing high temperature thermocouples. The purification of platinum is an important process in the processing of platinum, and the purity of the platinum has direct influence on the quality and the service life of a processed product.
In the processing flow of platinum purification, the dissolution of platinum is an important link in the platinum purification process, and the platinum has very stable chemical property, strong corrosion resistance and high work efficiencyThe process usually uses aqua regia to dissolve platinum, and the aqua regia is a very corrosive liquid which emits yellow fog and is concentrated hydrochloric acid (HCl) and concentrated nitric acid (HNO)3) Platinum dissolved in aqua regia in a 3:1 volume ratio mixture forms chloroplatinic acid (H2 PtCl 6). Then purifying by ammonium chloride repeated precipitation method, adding a certain amount of ammonium chloride into the solution of aqua regia dissolved platinum, so that platinum ions (Pt 4 +) are precipitated in the form of ammonium chloroplatinate compound, other impurity elements (Cu 2+, Fe2+, Ni2+, Pd4+, Ir4+, Au3+ and the like) still remain in the solution, separating platinum from impurities by washing and filtering the ammonium chloride solution, and adding a reducing agent into the platinum compound for reduction to obtain a pure spongy platinum product.
Various waste water can be generated in the platinum purification process, such as waste water after platinum precipitation, waste water for washing ammonium chloroplatinate and the like, and the waste water can often contain a small amount of platinum and other precious metals, so that the loss of the precious metals can be caused, and the waste water is difficult to treat in the later period due to excessive content of metal ions in the waste water, so that the treatment cost of the waste water is increased.
Disclosure of Invention
Aiming at the defects in the related technology, the application provides a method for recovering the residual precious metals in the platinum purification wastewater, which has the advantages that: most of noble metals in the wastewater can be recycled, the recovery rate is high, the content of the noble metals in the wastewater is greatly reduced, and the treatment cost of the wastewater is reduced.
In order to achieve the technical purpose, the application provides the following technical scheme:
a method for recovering residual precious metals in platinum purification wastewater comprises the following steps: s1, adding the wastewater into a reaction container, starting stirring, and adding sodium hydroxide into the wastewater to adjust the pH value of the wastewater to 9-10; s2, adding hydrazine hydrate with the mass fraction of 50% into the wastewater to reduce the noble metals in the wastewater, and continuously stirring and reducing for 1.5-3 hours, wherein the volume ratio of the hydrazine hydrate to the wastewater is (8-12) to 1000; s3, standing the wastewater for more than 5 hours after stirring, and reducing and precipitating the precious metal residues in the wastewater; s4, filtering the residual liquid in the reaction container, and performing vacuum suction filtration on the precipitate to obtain the recovered precious metal; wherein, the content of Pt in the residual liquid is less than 1mg/L, and the content of other noble metals is less than 0.2 mg/L.
By adopting the technical scheme, the hydrazine hydrate has very strong reducibility under an alkaline condition, the precious metals in the wastewater can be well precipitated, the volume ratio of the hydrazine hydrate to the wastewater is controlled to be (8-12): 1000, the sufficient amount of the hydrazine hydrate can be ensured, the recovery rate of the precious metals is improved, the waste caused by excessive hydrazine hydrate can be avoided, and the cost is saved; the content of Pt in the wastewater recovered by reduction is less than 1mg/L, the content of other noble metals is less than 0.2mg/L, the recovery rate of the noble metals is very high, the loss of the noble metals can be greatly reduced, the treatment cost of the wastewater can be reduced, and the method is beneficial to environmental protection.
Preferably, sodium hydroxide is added to the wastewater to adjust the pH of the wastewater to 9.
Through tests, the pH value of the wastewater is controlled to be 9 before precipitation, so that the reaction system can be ensured to be in an alkaline condition, hydrazine hydrate has good reducibility, the recovery rate of precious metals is improved, the wastewater after precipitation is ensured to be in alkalescence, the reaction is ensured to be thorough, the wastewater is treated, the treatment cost of the wastewater is saved, and in addition, the use amount of sodium hydroxide can be reduced as far as possible by controlling the pH value to be 9, so that the cost is saved.
Preferably, the volume ratio of hydrazine hydrate to wastewater is 10: 1000.
Tests show that the volume ratio of hydrazine hydrate to wastewater is controlled to be 10:1000, so that incomplete recovery caused by insufficient hydrazine hydrate is avoided, excessive hydrazine hydrate waste is avoided, and the cost is saved.
Preferably, the hydrazine hydrate is added at a flow rate of 0.5-0.7L/min.
Tests prove that the control of the adding flow of hydrazine hydrate to be 0.5-0.7L/min can ensure that the reaction is in a relatively stable state, avoid the over-violent reaction caused by the over-quick adding of hydrazine hydrate and prevent reaction liquid from overflowing upwards from a reaction container.
Preferably, the hydrazine hydrate is completely added and then stirred for 2 hours to reduce the noble metal.
Tests show that after the hydrazine hydrate is completely added, the precious metal in the wastewater can be fully precipitated by stirring for 2 hours, so that certain process time can be saved while high recovery rate of the precious metal is ensured, the time for wastewater recovery treatment is shortened, and the time cost is saved.
Preferably, the temperature of the waste water is controlled to be 85-90 ℃ after the hydrazine hydrate is completely added.
Tests show that the precious metal ions in the wastewater can form precipitates more quickly by controlling the temperature of hydrazine hydrate during reduction to be 85-90 ℃, so that the reduction reaction is accelerated, and the time for wastewater recovery treatment is shortened.
Preferably, the temperature of the wastewater is controlled to be 20-25 ℃ in the standing process.
Tests show that the wastewater is kept at 20-25 ℃ to reduce the solubility of noble metals in the wastewater, the noble metals dissolved in the wastewater are reduced as much as possible, the recovery rate of the noble metals is improved, the wastewater is kept at 20-25 ℃ relatively close to normal temperature, the cooling consumption cost is low, and the cost is saved.
In summary, the present application includes at least one of the following beneficial technical effects:
hydrazine hydrate has very strong reducibility under alkaline conditions, the pH value of a reaction system is controlled to be 9-10, precious metals in wastewater can be well precipitated, the volume ratio of the hydrazine hydrate to the wastewater is controlled to be (8-12) to 1000, the sufficient amount of the hydrazine hydrate can be ensured, the recovery rate of the precious metals is improved, the waste caused by excessive hydrazine hydrate can be avoided, the cost is saved, the content of Pt in the wastewater recovered by reduction is less than 1mg/L, the content of other precious metals is less than 0.2mg/L, the recovery rate of the precious metals is very high, the loss of the precious metals can be greatly reduced, the treatment cost of the wastewater can be reduced, and the environmental protection is facilitated;
the control of the flow rate of the added hydrazine hydrate is 0.5-0.7L/min, so that the reaction can be ensured to be in a relatively stable state, the phenomenon that the reaction is too violent due to the over-quick addition of the hydrazine hydrate is avoided, and the reaction liquid is prevented from overflowing upwards from a reaction container;
the wastewater is controlled to be kept at 20-25 ℃ to reduce the solubility of the noble metal in the wastewater, the noble metal dissolved in the wastewater is reduced as much as possible, the recovery rate of the noble metal is improved, and meanwhile, the wastewater is controlled to be closer to normal temperature at 20-25 ℃, the cooling consumption cost is low, and the cost is saved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the tables in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, other embodiments obtained by persons of ordinary skill in the art with the understanding of the inventive concept of the present invention are within the scope of the present invention.
The invention discloses a method for recovering residual noble metals in platinum purification wastewater, and aims to recover the residual noble metals in the platinum purification wastewater.
In the field of precious metal recovery, the lower the precious metal content in the wastewater is, the greater the recovery difficulty is, the more difficult it is to achieve high recovery rate, and after the recovery rate of the precious metal in the wastewater reaches more than 97%, it is very difficult to increase the recovery rate by 1%.
The experimental method comprises the following steps: setting an experiment group A, taking 1500L of mixed wastewater of the wastewater after platinum separation and purification and the washing ammonium chloroplatinate wastewater to carry out a wastewater precious metal recovery experiment, detecting the mixed wastewater, and measuring that the content of Pt in the mixed wastewater is 100mg/L and the content of Pd in the mixed wastewater is 500 mg/L.
The experimental steps are as follows:
s1, adding the mixed wastewater into a reaction kettle, starting stirring, adding sodium hydroxide into the mixed wastewater to adjust the pH value of the wastewater to 9, and adding 75kg of flaky sodium hydroxide in total.
S2 adding 50% hydrazine hydrate by mass into the mixed wastewater to reduce the noble metals in the wastewater, wherein the adding flow rate of the hydrazine hydrate is 0.5L/min, 15L hydrazine hydrate is added in total, and the mixture is continuously stirred and reduced for 2 hours at 90 ℃.
S3, cooling the wastewater to 20 ℃ after stirring and reduction, and standing for 5h to reduce and precipitate the precious metal residues in the wastewater.
And after S4 standing, filtering residual liquid in the reaction kettle, and performing vacuum suction filtration on the precipitate to obtain the recovered noble metal.
And (4) detecting a result: the content of the noble metal ions in the residual liquid is detected, and the specific detection result is shown in table 1.
Table 1: content of noble Metal ions in the raffinate of Experimental group A
| Pt | Pd | Au | Ir | Rh | Other noble metals | |
| Content (mg/L) | 0.71 | 0.12 | 0.05 | 0.08 | 0.06 | ＜0.2 |
| Percent recovery% | 99.29 | 99.976 | - | - | - | - |
According to the data in the table 1, the content of Pt in the raffinate of the experimental group a is only 0.71mg/L, the recovery rate is 99.29%, the content of Pd is only 0.12mg/L, the recovery rate is 99.976%, the content of other noble metals is controlled below 0.2mg/L, the noble metals in the wastewater treated by the method are completely recovered, the recovery rate is high, the wastewater does not need to be treated again by other methods, and the method has the advantages of simple process, convenient operation, less investment funds and lower cost. In addition, the content of the precious metals in the wastewater treated in the experiment is very low, but the recovery rate is still good, the recovery effect on the precious metals in the wastewater is very good, the residual liquid in the experimental group A is alkalescent, a lot of cost for later-stage wastewater purification treatment can be saved, the industrial feasibility and the practicability are very high, and the method is suitable for large-scale treatment of platinum purification wastewater.
According to the method, an experimental group B, an experimental group C and a control group D are set, the mixed wastewater in the experimental group B, the experimental group C and the control group D and the mixed wastewater in the experimental group A are mixed wastewater in the same batch, the pH value of the wastewater in the experimental group B is adjusted to 9.5 by changing the adding amount of sodium hydroxide, the pH value of the wastewater in the experimental group C is adjusted to 10, the pH value of the wastewater in the control group D is adjusted to 5, and a comparison experiment is carried out, wherein specific detection results are shown in Table 2.
Table 2: content of noble metal ions in residual liquid of experiment group B, experiment group C and control group D
Comparing the data in table 1 and table 2, the pH value of the mixed wastewater in the control group D is acidic, the recovery rates of Pt and Pd after recovery treatment are significantly reduced compared with the recovery rates in the experimental groups a to C, and the contents of other noble metals are also above 0.3mg/L, so that it can be seen that the recovery rate of noble metals is significantly higher when the wastewater is in an alkaline condition than when the wastewater is in an acidic condition. However, in the field of precious metal recovery from wastewater, it is difficult to continuously increase the recovery rate after the recovery rate of precious metal reaches above 97%, but the content of precious metal in wastewater treated in this experiment is originally low, although the recovery rate of precious metal in control group D is reduced compared with experimental groups a-C, the recovery rate of precious metal is still very high in the industry, and when the content of precious metal in wastewater is high, the wastewater treated by the method under acidic condition has good recovery rate. In addition, the reaction phenomenon in the control group D is not violent in the reaction in the experimental group A-the experimental group C, the reduction reaction time is longer, and the time cost is high, so that the control of the pH value of the wastewater under the alkaline condition is favorable for accelerating the reaction speed and reducing the time cost.
Comparing the data in the experimental group B and the experimental group C with the data in the experimental group A, adjusting the pH value of the mixed wastewater to be more than 9 has less influence on the recovery rate of the noble metal in the wastewater, but the cost of sodium hydroxide is additionally increased, and the alkalinity of the residual liquid in the experimental group B and the experimental group C is stronger than that in the experimental group A, the cost of post-treatment is higher than that in the experimental group A, so the pH value of the control wastewater is 9 and more excellent.
And setting an experiment group E and an experiment group F according to the experiment method in the experiment group A and the addition amount of the sodium hydroxide, wherein the volume ratio of the hydrazine hydrate to the wastewater in the experiment group E is 8:1000, the using amount of the hydrazine hydrate is 12L, the volume ratio of the hydrazine hydrate to the wastewater in the experiment group F is 12:1000, and the using amount of the hydrazine hydrate is 18L, and carrying out a comparison experiment, wherein specific detection results are shown in Table 3.
Table 3: content of noble Metal ions in the raffinate from experiment group E and experiment group F
The data in tables 1 and 3 show that the recovery rate of the noble metal in the experimental group E is slightly lower than that in the experimental group a, but the difference is not large, it can be seen that the amount of hydrazine hydrate has an influence on the recovery rate of the noble metal, the recovery rate of the noble metal in the experimental group F is substantially the same as that in the experimental group a, it can be seen that when the addition amount of hydrazine hydrate reaches a certain value, the improvement effect of increasing the amount of hydrazine hydrate on the recovery rate of the noble metal is small, and in combination with the cost of hydrazine hydrate and the time cost spent on adding hydrazine hydrate, the volume ratio of hydrazine hydrate to wastewater is controlled to be 10:1000, which is more preferable, not only can ensure the recovery rate of the noble metal, but also is beneficial to saving.
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
Claims (7)
1. A method for recovering precious metals remained in platinum purification wastewater is characterized by comprising the following steps: s1, adding the wastewater into a reaction container, starting stirring, and adding sodium hydroxide into the wastewater to adjust the pH value of the wastewater to 9-10; s2, adding hydrazine hydrate with the mass fraction of 50% into the wastewater to reduce the noble metals in the wastewater, and continuously stirring and reducing for 1.5-3 hours, wherein the volume ratio of the hydrazine hydrate to the wastewater is (8-12) to 1000; s3, standing the wastewater for more than 5 hours after stirring, and reducing and precipitating the precious metal residues in the wastewater; s4, filtering the residual liquid in the reaction container, and performing vacuum suction filtration on the precipitate to obtain the recovered precious metal; wherein, the content of Pt in the residual liquid is less than 1mg/L, and the content of other noble metals is less than 0.2 mg/L.
2. The method for recovering the residual precious metals in the platinum purification wastewater as claimed in claim 1, wherein the method comprises the following steps: sodium hydroxide is added into the wastewater to adjust the pH of the wastewater to 9.
3. The method for recovering the residual precious metals in the platinum purification wastewater as claimed in claim 1, wherein the method comprises the following steps: the volume ratio of hydrazine hydrate to waste water is 10: 1000.
4. The method for recovering the residual precious metals in the platinum purification wastewater as claimed in claim 1, wherein the method comprises the following steps: the flow rate of adding hydrazine hydrate is 0.5-0.7L/min.
5. The method for recovering the residual precious metals in the platinum purification wastewater as claimed in claim 1, wherein the method comprises the following steps: after the hydrazine hydrate is completely added, stirring for 2 hours to reduce the noble metal.
6. The method for recovering the residual precious metals in the platinum purification wastewater as claimed in claim 1, wherein the method comprises the following steps: after the hydrazine hydrate is completely added, the temperature of the waste water is controlled to be 85-90 ℃.
7. The method for recovering the residual precious metals in the platinum purification wastewater as claimed in claim 1, wherein the method comprises the following steps: controlling the temperature to be 20-25 ℃ in the standing process of the wastewater.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1370845A (en) * | 2001-10-09 | 2002-09-25 | 金川集团有限公司 | Refined platinum producing process |
| CN101074458A (en) * | 2006-05-19 | 2007-11-21 | 中国石油化工股份有限公司 | Method for recovering noble-metal from waste catalyst |
| CN101376923A (en) * | 2007-08-27 | 2009-03-04 | 中国石油化工股份有限公司 | Method for recycling noble metal from spent catalyst |
| CN102242265A (en) * | 2011-06-13 | 2011-11-16 | 白银万山稀贵金属科技有限责任公司 | Technology for extracting precious metal platinum from industrial solid waste materials |
| CN102797018A (en) * | 2012-08-30 | 2012-11-28 | 贵研资源（易门）有限公司 | Method for separating and purifying platinum by adopting holding potential |
| CN107150128A (en) * | 2017-05-12 | 2017-09-12 | 江西铜业集团公司 | A kind of preparation method of high-purity platinum powder |
| CN108655415A (en) * | 2018-06-20 | 2018-10-16 | 南京东锐铂业有限公司 | A kind of new process preparing high-purity platinum |
-
2020
- 2020-06-24 CN CN202010588835.9A patent/CN111534700A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1370845A (en) * | 2001-10-09 | 2002-09-25 | 金川集团有限公司 | Refined platinum producing process |
| CN101074458A (en) * | 2006-05-19 | 2007-11-21 | 中国石油化工股份有限公司 | Method for recovering noble-metal from waste catalyst |
| CN101376923A (en) * | 2007-08-27 | 2009-03-04 | 中国石油化工股份有限公司 | Method for recycling noble metal from spent catalyst |
| CN102242265A (en) * | 2011-06-13 | 2011-11-16 | 白银万山稀贵金属科技有限责任公司 | Technology for extracting precious metal platinum from industrial solid waste materials |
| CN102797018A (en) * | 2012-08-30 | 2012-11-28 | 贵研资源（易门）有限公司 | Method for separating and purifying platinum by adopting holding potential |
| CN107150128A (en) * | 2017-05-12 | 2017-09-12 | 江西铜业集团公司 | A kind of preparation method of high-purity platinum powder |
| CN108655415A (en) * | 2018-06-20 | 2018-10-16 | 南京东锐铂业有限公司 | A kind of new process preparing high-purity platinum |
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