CN111534692A - Process method for extracting noble metal from homogeneous phase waste liquid - Google Patents
Process method for extracting noble metal from homogeneous phase waste liquid Download PDFInfo
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- CN111534692A CN111534692A CN201910834004.2A CN201910834004A CN111534692A CN 111534692 A CN111534692 A CN 111534692A CN 201910834004 A CN201910834004 A CN 201910834004A CN 111534692 A CN111534692 A CN 111534692A
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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
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of scrap
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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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- 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
- C22B7/007—Wet processes by acid leaching
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Abstract
The invention discloses a process method for extracting noble metal from homogeneous phase waste liquid, which comprises the steps of heating the homogeneous phase waste liquid to 80-300 ℃, adding an adsorbent into the heated homogeneous phase waste liquid, continuously stirring and adsorbing, then filtering and separating to obtain an adsorption solid phase containing noble metal and a lean phase waste liquid, and respectively cooling the adsorption solid phase and the lean phase waste liquid to room temperature; carrying out appropriate distillation separation on the obtained lean phase waste liquid to obtain triphenylphosphine and a light organic phase; carrying out high-temperature firing treatment on the obtained adsorption solid phase containing the noble metal to remove organic matters, thus obtaining solid slag containing the noble metal; dissolving the obtained solid residue containing the noble metal by acid liquor, and purifying to obtain pure noble metal. The process method for extracting the noble metal from the homogeneous phase waste liquid has the characteristics of low cost, high recovery rate, simple and convenient operation, environmental friendliness and the like.
Description
Technical Field
The invention relates to the technical field of precious metal recovery, in particular to a process method for extracting precious metals from homogeneous-phase waste liquid.
Background
The noble metals mainly refer to gold, silver and platinum group metals, the platinum group metals comprise ruthenium, rhodium, palladium, osmium, iridium and platinum, most of the metals have beautiful colors and high resistance to chemicals, and chemical reactions are not easily caused under common conditions, so the noble metals have high values and are widely applied to various fields. In recent years, the consumption of noble metals is increased year by year, but the abundance of the noble metals in the earth crust is low, the distribution is scattered, and the separation and the purification are difficult. In order to solve the contradiction between the shortage of resources and the increase in demand, one of the most important solutions is to recover and reuse precious metals from industrial waste liquid containing precious metals.
The noble metals mainly contained in the homogeneous industrial waste liquid comprise gold, silver, platinum, palladium and rhodium, the process method for extracting the noble metals from the homogeneous waste liquid is based on the prior art, the main recovery process is that the noble metals are directly burnt or directly evaporated at the temperature of 600-700 ℃, the obtained burnt ash or distillation residues are burnt, the obtained burning enrichment materials containing the noble metals are subjected to subsequent acid dissolution and separation and purification, and finally the pure metals are obtained. However, the equipment adopting the process has large investment at one time, and the following problems exist in the actual industrial production: the process has the advantages of severe operating environment, ineffective treatment and recycling of a large amount of triphenylphosphine left in distillation residues, low recovery rate of noble metals, certain explosion risk in the operating process, high operation and maintenance cost and the like.
Disclosure of Invention
In order to solve the problems in the background art, the invention aims to provide a process method for extracting precious metals from homogeneous-phase waste liquid, which has the characteristics of low cost, high recovery rate, simple and convenient operation, environmental friendliness and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a process method for extracting noble metal from homogeneous phase waste liquid, which comprises the following steps:
s1, heating the homogeneous phase waste liquid to 80-300 ℃, adding an adsorbent into the heated homogeneous phase waste liquid, continuously stirring and adsorbing, then filtering and separating to obtain an adsorption solid phase containing noble metals and a lean phase waste liquid, and respectively cooling the adsorption solid phase and the lean phase waste liquid to room temperature;
s2, distilling and crystallizing the lean phase waste liquid obtained in the step S1 to respectively obtain triphenylphosphine and a light organic phase;
s3, performing high-temperature burning treatment on the adsorption solid phase containing the noble metal obtained in the step S1 to remove organic matters, and obtaining solid slag containing the noble metal;
s4, dissolving the solid slag containing the precious metals obtained in the step S3 with acid liquor, and purifying to obtain pure precious metals.
Preferably, the adsorbent in step S1 is one or a mixture of several of resin, silica gel, activated carbon and diatomite.
Preferably, the addition amount of the adsorbent in the step S1 is 10-30% of the volume of the homogeneous waste liquid.
Preferably, the distillation treatment temperature in the step S2 is 80-300 ℃.
Preferably, the high-temperature ignition temperature in the step S3 is 600-900 ℃.
Preferably, the acid solution for dissolving the solid residue containing the precious metal in step S4 is aqua regia, a hydrochloric acid/sodium chlorate mixed solution, or a hydrochloric acid/hydrogen peroxide mixed solution.
Compared with the prior art, the invention has the following beneficial effects:
the invention takes homogeneous waste liquid containing noble metal as raw material, and adopts the processes of adsorption, distillation, incineration, acid dissolution and the like to treat, the noble metal in the homogeneous waste liquid is adsorbed to a solid phase, the lean waste liquid is distilled, crystallized and separated to obtain triphenylphosphine by-product and light organic phase which can be used as fuel, and the adsorbed solid phase containing noble metal is incinerated, dissolved and purified to obtain pure metal. The process has the advantages that: the treatment cost is lower, the process operation is simple and easy to control, the normal pressure operation is realized, the explosion risk is avoided, and the operation and maintenance cost is lower.
According to the process method for extracting the noble metal from the homogeneous-phase waste liquid, the one-time acid extraction rate of the noble metal is higher than 75%, and the total recovery rate of the noble metal can reach more than 95%; the process equipment used in the extraction process can be completely made into a home, and the one-time investment cost is greatly reduced; the whole process flow is simple and convenient to operate, control and use, the treatment amount of the homogeneous-phase waste liquid can be increased or decreased according to the actual production condition, flexible control on production management is achieved, and the maintenance cost in the treatment process is low.
Detailed Description
Example 1
S1, measuring 5kg of homogeneous phase waste liquid, placing the homogeneous phase waste liquid in a heating container, heating to 80 ℃, adding resin accounting for 10% of the volume of the homogeneous phase waste liquid into the heated homogeneous phase waste liquid for adsorption, continuously stirring in the resin adding process, standing and settling for 2 hours after the resin is completely added, and filtering and separating to obtain an adsorption solid phase containing precious metals and a lean phase waste liquid;
s2, transferring the lean-phase waste liquid obtained in the step S1 into a distillation kettle, heating and distilling to 95 ℃ to obtain triphenylphosphine and a light organic phase;
s3, placing the adsorption solid phase containing the precious metals in the step S1 in an incinerator to be fully incinerated at 600 ℃ to obtain solid slag containing the precious metals;
s4, dissolving the solid slag containing the precious metals obtained in the step S3 in aqua regia, filtering to obtain filtrate, namely precious metal solution, and separating and purifying the obtained precious metal solution to obtain pure precious metals.
In this example, the one-time acid extraction rate of the noble metal was 75.0%, and the total recovery rate of the noble metal was 91%.
Example 2
S1, measuring 10kg of homogeneous phase waste liquid, placing the homogeneous phase waste liquid in a heating container, heating to 95 ℃, adding silica gel accounting for 20% of the volume of the homogeneous phase waste liquid into the heated homogeneous phase waste liquid for adsorption, continuously stirring in the resin adding process, standing and settling for 2 hours after the resin is completely added, and filtering and separating to obtain an adsorption solid phase containing precious metals and a lean phase waste liquid;
s2, transferring the lean-phase waste liquid obtained in the step S1 into a distillation kettle, heating and distilling the lean-phase waste liquid to 80 ℃ to obtain triphenylphosphine and a light organic phase;
s3, placing the adsorption solid phase containing the precious metals in the step S1 in an incinerator to be fully incinerated at 700 ℃ to obtain solid slag containing the precious metals;
s4, dissolving the solid residue containing the precious metals obtained in the step S3 in hydrochloric acid/sodium chlorate, filtering to obtain filtrate, namely precious metal solution, and separating and purifying the obtained precious metal solution to obtain pure precious metals.
In this example, the one-time acid extraction rate of the noble metal was 81.0%, and the total recovery rate of the noble metal was 93%.
Example 3
S1, weighing 15kg of homogeneous phase waste liquid, placing the homogeneous phase waste liquid in a heating container, heating to 120 ℃, adding a mixture of resin and activated carbon accounting for 25% of the volume of the homogeneous phase waste liquid into the heated homogeneous phase waste liquid for adsorption, continuously stirring in the resin adding process, standing and settling for 2 hours after the resin is completely added, and filtering and separating to obtain an adsorption solid phase containing precious metals and a lean phase waste liquid;
s2, transferring the lean-phase waste liquid obtained in the step S1 into a distillation kettle, heating and distilling the lean-phase waste liquid to 170 ℃ to obtain triphenylphosphine and a light organic phase;
s3, placing the adsorption solid phase containing the precious metals in the step S1 in an incinerator to be fully incinerated at 750 ℃ to obtain solid slag containing the precious metals;
s4, dissolving the solid slag containing the precious metals obtained in the step S3 in aqua regia, filtering to obtain filtrate, namely precious metal solution, and separating and purifying the obtained precious metal solution to obtain pure precious metals.
In this example, the one-time acid extraction rate of the noble metal was 78.0%, and the total recovery rate of the noble metal was 93%.
Example 4
S1, weighing 20kg of homogeneous phase waste liquid, placing the homogeneous phase waste liquid in a heating container, heating to 150 ℃, adding a mixture of resin and diatomite accounting for 20% of the volume of the homogeneous phase waste liquid into the heated homogeneous phase waste liquid for adsorption, continuously stirring in the resin adding process, standing and settling for 2 hours after the resin is completely added, and filtering and separating to obtain an adsorption solid phase containing precious metals and a lean phase waste liquid;
s2, transferring the lean-phase waste liquid obtained in the step S1 into a distillation kettle, heating and distilling the lean-phase waste liquid to 240 ℃ to obtain triphenylphosphine and a light organic phase;
s3, placing the adsorption solid phase containing the precious metals in the step S1 in an incinerator to be fully incinerated at 800 ℃ to obtain solid slag containing the precious metals;
s4, dissolving the solid slag containing the precious metals obtained in the step S3 in aqua regia, filtering to obtain filtrate, namely precious metal solution, and separating and purifying the obtained precious metal solution to obtain pure precious metals.
In this example, the one-time acid extraction rate of the noble metal was 75.0%, and the total recovery rate of the noble metal was 96%.
Example 5
S1, weighing 30kg of homogeneous phase waste liquid, placing the homogeneous phase waste liquid in a heating container, heating to 300 ℃, adding resin accounting for 30% of the volume of the homogeneous phase waste liquid into the heated homogeneous phase waste liquid for adsorption, continuously stirring in the resin adding process, standing and settling for 2 hours after the resin is completely added, and filtering and separating to obtain an adsorption solid phase containing precious metals and a lean phase waste liquid;
s2, transferring the lean-phase waste liquid obtained in the step S1 into a distillation kettle, heating and distilling the lean-phase waste liquid to 300 ℃ to obtain triphenylphosphine and a light organic phase;
s3, placing the adsorption solid phase containing the precious metals in the step S1 in an incinerator to be fully incinerated at 900 ℃ to obtain solid slag containing the precious metals;
s4, dissolving the solid residue containing the precious metals obtained in the step S3 in a hydrochloric acid-hydrogen peroxide solution, filtering to obtain a filtrate, namely a precious metal solution, and separating and purifying the obtained precious metal solution to obtain pure precious metals.
In this example, the one-time acid extraction rate of the noble metal was 76.0%, and the total recovery rate of the noble metal was 96%.
The invention relates to a process for extracting noble metal from homogeneous waste liquid, which comprises using the homogeneous waste liquid containing noble metal as raw material, treating by adsorption, distillation, crystallization, incineration, acid dissolution and other processes, adsorbing the noble metal in the homogeneous waste liquid to solid phase, distilling, crystallizing and separating the poor phase waste liquid to obtain triphenylphosphine byproduct and light organic phase which can be used as fuel, and incinerating, dissolving and purifying the adsorbed solid phase containing noble metal to obtain pure metal. The one-time acid extraction rate of the noble metal by adopting the process is higher than 75%, the total recovery rate of the noble metal can reach more than 95%, the treatment cost is lower, the process operation is simple and easy to control, the normal-pressure operation is realized, the explosion risk is avoided, and the operation and maintenance cost is lower.
The present invention has been described in terms of specific examples, which are provided to aid understanding of the invention and are not intended to be limiting. For a person skilled in the art to which the invention pertains, several simple deductions, modifications or substitutions may be made according to the idea of the invention.
Claims (6)
1. A process method for extracting noble metal from homogeneous phase waste liquid is characterized by comprising the following steps:
s1, heating the homogeneous phase waste liquid to 80-300 ℃, adding an adsorbent into the heated homogeneous phase waste liquid, continuously stirring and adsorbing, then filtering and separating to obtain an adsorption solid phase containing noble metals and a lean phase waste liquid, and respectively cooling the adsorption solid phase and the lean phase waste liquid to room temperature;
s2, distilling and crystallizing the lean phase waste liquid obtained in the step S1 to obtain triphenylphosphine and a light organic phase;
s3, performing high-temperature burning treatment on the adsorption solid phase containing the noble metal obtained in the step S1 to remove organic matters, and obtaining solid slag containing the noble metal;
s4, dissolving the solid slag containing the precious metals obtained in the step S3 with acid liquor, and purifying to obtain pure precious metals.
2. The process of claim 1, wherein the adsorbent in step S1 is one or more selected from the group consisting of resin, silica gel, activated carbon, and diatomaceous earth.
3. The process of claim 2, wherein the adsorbent added in step S1 is 10-30% of the volume of the homogeneous waste liquid.
4. The process of claim 3, wherein the distillation and crystallization temperature in step S2 is 80-300 ℃.
5. The process of claim 4, wherein the high temperature ignition temperature in step S3 is 600-900 ℃.
6. The process method for extracting noble metals from homogeneous waste liquid according to claim 5, wherein the acid solution for dissolving the solid residue containing noble metals in step S4 is aqua regia, a mixed solution of hydrochloric acid/sodium chlorate or a mixed solution of hydrochloric acid/hydrogen peroxide.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111910082A (en) * | 2020-08-31 | 2020-11-10 | 武汉北湖云峰环保科技有限公司 | Method for recovering noble metal from strong acid waste liquid |
| CN113233569A (en) * | 2021-04-17 | 2021-08-10 | 北京化工大学 | Method for quickly removing manganese ions in wastewater and application of manganese-containing product in precious metal recovery |
| CN113528827A (en) * | 2021-06-30 | 2021-10-22 | 济南恒誉环保科技股份有限公司 | Method for separating precious metals from waste liquid phase organic matter by adopting thermal cracking |
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| CN107641719A (en) * | 2017-08-25 | 2018-01-30 | 金川集团股份有限公司 | A kind of method that noble metal is reclaimed from low concentration solution |
| CN107955038A (en) * | 2017-12-19 | 2018-04-24 | 天津渤化永利化工股份有限公司 | Catalyst mother liquor comprehensive reutilization method and device in a kind of propenecarbonyl |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102796877A (en) * | 2012-08-27 | 2012-11-28 | 贵研铂业股份有限公司 | Method for enriching rhodium from rhodium-containing organic dead catalyst |
| CN107641719A (en) * | 2017-08-25 | 2018-01-30 | 金川集团股份有限公司 | A kind of method that noble metal is reclaimed from low concentration solution |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111910082A (en) * | 2020-08-31 | 2020-11-10 | 武汉北湖云峰环保科技有限公司 | Method for recovering noble metal from strong acid waste liquid |
| CN111910082B (en) * | 2020-08-31 | 2022-08-02 | 武汉北湖云峰环保科技有限公司 | Method for recovering noble metal from strong acid waste liquid |
| CN113233569A (en) * | 2021-04-17 | 2021-08-10 | 北京化工大学 | Method for quickly removing manganese ions in wastewater and application of manganese-containing product in precious metal recovery |
| CN113528827A (en) * | 2021-06-30 | 2021-10-22 | 济南恒誉环保科技股份有限公司 | Method for separating precious metals from waste liquid phase organic matter by adopting thermal cracking |
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