CN108823416B - Method for extracting gold and silver from clay graphite crucible slag - Google Patents
Method for extracting gold and silver from clay graphite crucible slag Download PDFInfo
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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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- 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
- C22B1/02—Roasting 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
- C22B11/044—Recovery of noble metals from waste materials from pyrometallurgical residues, e.g. from ashes, dross, flue dust, mud, skim, slag, sludge
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Abstract
The invention discloses a method for extracting gold and silver from clay graphite crucible slag, which comprises the following steps: reacting clay graphite crucible slag powder with a sulfuric acid/silicofluoric acid mixed solution, cooling, washing with water, and filtering to obtain filter residue and filtrate; drying the filter residue, calcining at high temperature, and then cooling and grinding to obtain enriched residue; placing the enriched slag in a nitric acid solution, reacting at normal temperature, diluting and filtering to obtain leaching slag I and leaching solution I, and reducing the leaching solution I to extract silver; and placing the leaching residue I in aqua regia, diluting and filtering after complete reaction to obtain leaching residue II and leaching solution II, and reducing and extracting gold from the leaching solution II. The clay graphite crucible slag of the application is firstly reacted with the sulfuric acid/fluosilicic acid mixed liquid before calcination, so that the agglomeration of the clay graphite crucible slag in the calcination process can be avoided, the separation of gold and silver from other impurities is realized, and the leaching recovery rate of gold and silver is improved.
Description
Technical Field
The invention belongs to the technical field of non-ferrous metal recovery, and particularly relates to a method for extracting gold and silver from clay graphite crucible slag.
Background
When metal is smelted by a pyrogenic process, clay graphite crucibles are often used for casting the smelted metal, and a small amount of crude metal permeates into the crucibles during pouring. The crucible can be used for many times, and a large amount of metal can be enriched on the inner wall of the crucible. Particularly, when gold is smelted, the clay graphite crucible is rich in more gold and silver, and the gold and the silver are high-value precious metals and have extremely high economic recovery value.
The Yexiqing discloses a method for extracting indium and germanium in crucible slag by a full-wet method (patent application No. CN201010169155.X method for extracting indium and germanium in crucible slag by a full-wet method), leaching indium by dilute sulfuric acid, and then adopting MnO2The concentrated sulfuric acid is used as an oxidant to leach germanium, so that most of germanium and indium can be respectively recovered, and a high recovery rate can be kept. The research on extracting metal gold and silver from the clay graphite crucible slag is less, because the clay graphite crucible slag contains clay components, if the gold and silver in the clay graphite crucible slag are extracted by directly adopting nitric acid and aqua regia or are extracted by calcining and then adding nitric acid and aqua regia, the gold and silver in the clay graphite crucible slag cannot be effectively extracted, the recovery rate is almost zero, and therefore, the technology for recovering gold and silver from the clay graphite crucible slag in the prior art has certain technologyThe difficulty of the operation.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for extracting gold and silver from clay graphite crucible slag.
The invention provides a method for extracting gold and silver from clay graphite crucible slag, which comprises the following steps:
1) reacting clay graphite crucible slag powder with a sulfuric acid/silicofluoric acid mixed solution at 50-70 ℃, and filtering the mixed solution after the reaction is finished to obtain filter residue;
2) drying the filter residue, calcining at the temperature of 900-1000 ℃, and then treating to obtain powdery enrichment slag;
3) placing the enrichment slag in a nitric acid solution, stirring at normal temperature for leaching reaction, diluting and filtering a mixed solution after complete reaction to obtain leaching slag I and leaching solution I, and reducing and extracting silver from the leaching solution I;
4) and (3) placing the leaching residue I in aqua regia, stirring at 50-80 ℃ for leaching reaction, diluting the mixed solution after complete reaction, filtering to obtain a leaching solution II, and reducing the leaching solution II to extract gold.
Preferably, the particle size of the clay graphite crucible slag powder in the step 1) is 150-325 meshes.
Preferably, the concentration of the sulfuric acid in the sulfuric acid/silicofluoric acid mixed solution in the step 1) is 80-150g/L, and the concentration of the silicofluoric acid is 100-340 g/L.
Preferably, the mass volume ratio of the clay graphite crucible slag powder to the sulfuric acid/silicofluoric acid mixed solution in the step 1) is 1:1-3 g/ml.
Preferably, the reaction time in step 1) is 6 to 12 hours.
Preferably, the calcination time in step 2) is 1.5 to 3 hours.
Preferably, the concentration of the nitric acid solution in the step 3) is 63-130 g/L.
Preferably, the mass volume ratio of the enrichment slag to the nitric acid solution in the step 3) is 1:1-5 g/ml.
Preferably, the mass volume ratio of the leaching residue I to the aqua regia in the step 4) is 1:1-5 g/ml.
Preferably, the leaching reaction time in the step 4) is 4-6 h.
The invention provides a method for extracting gold and silver from clay graphite crucible slag, which comprises the following most preferable steps:
1) stirring and reacting clay graphite crucible slag powder with the particle size of 325 meshes and a sulfuric acid/silicofluoric acid mixed solution at 70 ℃ for 6 hours, cooling the reacted mixed solution to room temperature, washing the cooled mixed solution to be neutral, and filtering the mixed solution to obtain filter residue and filtrate; wherein the concentration of sulfuric acid in the sulfuric acid/silicofluoric acid mixed solution is 150g/L, and the concentration of silicofluoric acid is 340 g/L; the mass volume ratio of the clay graphite crucible slag powder to the sulfuric acid/silicofluoric acid mixed solution is 1:1 g/ml;
2) drying the filter residue at 105 ℃ for 12h, calcining the filter residue at 1000 ℃ for 1.5h, cooling the calcined filter residue, and grinding to obtain powdery enrichment residue;
3) placing the enrichment slag in a nitric acid solution with the concentration of 130g/L, stirring at normal temperature to carry out leaching reaction for 6 hours, diluting the mixed solution after the reaction is completed by 5 times, filtering to obtain leaching slag I and leaching solution I, and reducing the leaching solution I to extract silver; wherein the mass volume ratio of the enrichment slag to the nitric acid solution is 1:1 g/ml;
4) placing the leaching residue I in aqua regia, stirring at 80 ℃ for leaching reaction for 6 hours, diluting the mixed solution after complete reaction, filtering to obtain a leaching solution II and a leaching residue II, and reducing the leaching solution II to extract gold; wherein the mass volume ratio of the leaching residue I to the aqua regia is 1:1 g/ml.
The gold and silver extraction rate obtained by adopting the optimal steps is highest.
Diluting the mixed solution after the reaction in the step 3) by 3-5 times, and then filtering to obtain leaching residue I and leaching solution I.
According to the invention, the leaching solution II and the leaching residue II can be obtained by filtering in the step 4), and the leaching residue II can be continuously returned to the step 3) to replace the enrichment residue, so that gold and silver can be further extracted.
The clay graphite crucible slag powder is obtained by grinding and sieving clay graphite crucible slag.
The clay graphite crucible slag is obtained by crushing a clay graphite crucible for pyrometallurgical gold smelting scrapped by gold and silver industry Limited company in Chenzhou city, wherein the mass percent of metal elements in the clay graphite crucible slag is as follows: gold (Au): 0.013%, silver (Ag) 5.284%, copper (Cu): 0.710 percent.
The clay graphite crucible is a crucible which is prepared by firing graphite, silicon carbide, silica, clay, asphalt and tar serving as raw materials. Usually, the content of graphite is 35-55%, the content of aggregate (such as silicon carbide) is 25-45%, and the content of clay is: 15-25% and a small amount of asphalt and tar.
In the method for extracting gold and silver from clay graphite crucible slag, the drying conditions of the filter residue in the step 3) are as follows: the drying temperature is 105 ℃, and the drying time is 12 h.
The silicofluoric acid is the electrolyte for lead electrolysis of Chenzhou city gold noble silver industry, Inc.
The sulfuric acid/silicofluoric acid mixed solution is obtained by mixing concentrated sulfuric acid, silicofluoric acid and deionized water.
At present, people have few researches on metal recovery in crucible slag for pyrometallurgical metal smelting, and patent application No. CN201010169155.X discloses a method for extracting indium and germanium in crucible slag for pyrometallurgical metal smelting by a full wet method, wherein indium is leached by dilute sulfuric acid, and then MnO is adopted2The concentrated sulfuric acid is used as an oxidant to leach germanium, so that most of germanium and indium can be respectively recovered, and a high recovery rate can be kept. At present, the gold and silver are recovered from metal smelting slag by directly leaching with nitric acid and aqua regia, so on the basis of the prior art, a person skilled in the art can think of extracting the gold and silver in the clay graphite crucible slag by adopting a wet method, but the inventor of the application finds that the gold and silver in the clay graphite crucible slag are directly leached with nitric acid and aqua regia through research, so that the extraction rate of the gold and silver is greatly reduced, the impurities are more, the obtained metal purity is not high, and the practical value is reduced. In addition, if the clay graphite crucible slag is directly calcined, the clay graphite crucible slag can be sintered into blocks, and the later-stage gold and silver extraction effect is affected. The inventors of the present application thus conceived of removing the clay graphite crucible slagThe clay component is leached by hydrofluoric acid, but the conventional method for removing the clay at present has the disadvantages of great pollution and poor leaching effect. The method comprises the step of firstly reacting a sulfuric acid/silicofluoric acid mixed solution with clay graphite crucible slag powder at 50-70 ℃, wherein the concentration of sulfuric acid in the sulfuric acid/silicofluoric acid mixed solution is 80-150g/L, and the concentration of silicofluoric acid is 100-340g/L, so that clay components in the sulfuric acid/silicofluoric acid mixed solution can be effectively removed, and the problem that the blocks are formed in the later calcining process to influence the later extraction effect of gold and silver is avoided.
This application adopts fire method and wet process to combine together to extract gold and silver in the clay graphite crucible sediment, compares in only adopting the wet process, and this application gold and silver's extraction rate improves greatly. And the clay graphite crucible slag reacts with the sulfuric acid/fluosilicic acid mixed solution before being calcined, then is calcined at the temperature of 1000 ℃, and finally is separated by the acid and aqua regia leaching method, compared with the direct calcination without the sulfuric acid/fluosilicic acid mixed solution treatment, the clay graphite crucible slag reacts with the sulfuric acid/fluosilicic acid mixed solution before being calcined, so that the clay graphite crucible slag powder is prevented from being agglomerated in the calcining process, most of copper in the graphite crucible slag is removed, the separation of gold and silver from other impurities is realized, and the leaching recovery rate of gold and silver is improved.
The invention has the beneficial effects that:
1. this application adopts fire method and wet process to combine together to extract gold and silver in the clay graphite crucible sediment, compares in only adopting the wet process, and this application gold and silver's extraction rate improves greatly.
2. The method comprises the step of firstly reacting a sulfuric acid/silicofluoric acid mixed solution with clay graphite crucible slag powder at 50-70 ℃, wherein the concentration of sulfuric acid in the sulfuric acid/silicofluoric acid mixed solution is 80-150g/L, and the concentration of silicofluoric acid is 100-340g/L, so that clay components in the sulfuric acid/silicofluoric acid mixed solution can be effectively removed, and the problem that the blocks are formed in the later calcining process to influence the later extraction effect of gold and silver is avoided.
3. The clay graphite crucible slag is firstly reacted with the sulfuric acid/fluosilicic acid mixed solution before being calcined, then is calcined at the temperature of 900-1000 ℃, and finally is separated from gold and silver by using the acid and aqua regia leaching methods respectively, compared with the method of directly calcining without the sulfuric acid/fluosilicic acid mixed solution treatment, the clay graphite crucible slag is firstly reacted with the sulfuric acid/fluosilicic acid mixed solution before being calcined, the agglomeration of the clay graphite crucible slag in the calcining process can be avoided, the separation of the gold and silver from other impurities is realized, and the leaching recovery rate of the gold and the silver is improved.
4. By adopting the operation sequence of the invention, the gold and the silver can be separated from other impurities to the maximum extent, and the leaching recovery rate of the gold and the silver is improved.
5. The invention has the advantages of sufficient raw material source, low price and low production cost.
6. The gold and silver are not dispersed in the extraction process, the silver element is leached in the first step, and the gold element is leached in the second step, so that the gold and the silver can be recovered, and the higher recovery efficiency can be maintained.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to specific embodiments below.
Example 1
1) Stirring and reacting 150-mesh clay graphite crucible slag powder and a sulfuric acid/silicofluoric acid mixed solution at 50 ℃ for 12 hours, cooling the reacted mixed solution to room temperature, washing the cooled mixed solution to be neutral, and filtering to obtain filter residue and filtrate; wherein the concentration of sulfuric acid in the sulfuric acid/silicofluoric acid mixed solution is 80g/L, and the concentration of silicofluoric acid is 100 g/L; the mass volume ratio of the clay graphite crucible slag powder to the sulfuric acid/silicofluoric acid mixed solution is 1:3 g/ml;
2) drying the filter residue at 105 ℃ for 12h, calcining the filter residue at 950 ℃ for 3h, cooling and grinding the calcined filter residue to obtain powdery enrichment residue;
3) placing the enrichment slag in a nitric acid solution with the concentration of 100g/L, stirring at normal temperature to carry out leaching reaction for 5 hours, diluting the mixed solution after the reaction is completed by 3 times, filtering to obtain leaching slag I and leaching solution I, and reducing the leaching solution I to extract silver; wherein the mass volume ratio of the enrichment slag to the nitric acid solution is 1:5 g/ml;
4) placing the leaching residue I in aqua regia, stirring at 50 ℃ for leaching reaction for 5 hours, diluting the mixed solution after complete reaction, filtering to obtain a leaching solution II and a leaching residue II, and reducing the leaching solution II to extract gold; wherein the mass volume ratio of the leaching residue I to the aqua regia is 1:5 g/ml.
Example 2
1) Stirring and reacting clay graphite crucible slag powder with the particle size of 200 meshes and a sulfuric acid/silicofluoric acid mixed solution at 60 ℃ for 8 hours, cooling the reacted mixed solution to room temperature, washing the cooled mixed solution to be neutral, and filtering to obtain filter residue and filtrate; wherein the concentration of sulfuric acid in the sulfuric acid/silicofluoric acid mixed solution is 100g/L, and the concentration of silicofluoric acid is 220 g/L; the mass volume ratio of the clay graphite crucible slag powder to the sulfuric acid/silicofluoric acid mixed solution is 1:2 g/ml;
2) drying the filter residue at 105 ℃ for 12h, calcining the filter residue at 900 ℃ for 2h, cooling the calcined filter residue, and grinding to obtain powdery enrichment residue;
3) placing the enrichment slag in a nitric acid solution with the concentration of 63g/L, stirring at normal temperature to carry out leaching reaction for 4 hours, diluting the mixed solution after the reaction is completed by 4 times, filtering to obtain leaching slag I and leaching solution I, and reducing the leaching solution I to extract silver; wherein the mass volume ratio of the enrichment slag to the nitric acid solution is 1:3 g/ml;
4) placing the leaching residue I in aqua regia, stirring at 60 ℃ for leaching reaction for 4h, diluting the mixed solution after complete reaction, filtering to obtain a leaching solution II and a leaching residue II, and reducing the leaching solution II to extract gold; wherein the mass volume ratio of the leaching residue I to the aqua regia is 1:2 g/ml.
Example 3
1) Stirring and reacting clay graphite crucible slag powder with the particle size of 325 meshes and a sulfuric acid/silicofluoric acid mixed solution at 70 ℃ for 6 hours, cooling the reacted mixed solution to room temperature, washing the cooled mixed solution to be neutral, and filtering the mixed solution to obtain filter residue and filtrate; wherein the concentration of sulfuric acid in the sulfuric acid/silicofluoric acid mixed solution is 150g/L, and the concentration of silicofluoric acid is 340 g/L; the mass volume ratio of the clay graphite crucible slag powder to the sulfuric acid/silicofluoric acid mixed solution is 1:1 g/ml;
2) drying the filter residue at 105 ℃ for 12h, calcining the filter residue at 1000 ℃ for 1.5h, cooling the calcined filter residue, and grinding to obtain powdery enrichment residue;
3) placing the enrichment slag in a nitric acid solution with the concentration of 130g/L, stirring at normal temperature to carry out leaching reaction for 6 hours, diluting the mixed solution after the reaction is completed by 5 times, filtering to obtain leaching slag I and leaching solution I, and reducing the leaching solution I to extract silver; wherein the mass volume ratio of the enrichment slag to the nitric acid solution is 1:1 g/ml;
4) placing the leaching residue I in aqua regia, stirring at 80 ℃ for leaching reaction for 6 hours, diluting the mixed solution after complete reaction, filtering to obtain a leaching solution II and a leaching residue II, and reducing the leaching solution II to extract gold; wherein the mass volume ratio of the leaching residue I to the aqua regia is 1:1 g/ml.
Comparative example 1
1) Drying clay graphite crucible slag powder with the particle size of 200 meshes at 105 ℃ for 12 hours, calcining at 900 ℃ for 2 hours, cooling and grinding calcined filter residues to obtain powdery enrichment slag;
2) placing the enrichment slag in a nitric acid solution with the concentration of 63g/L, stirring at normal temperature to carry out leaching reaction for 4 hours, diluting the mixed solution after the reaction is completed by 4 times, filtering to obtain leaching slag I and leaching solution I, and reducing the leaching solution I to extract silver; wherein the mass volume ratio of the enrichment slag to the nitric acid solution is 1:3 g/ml;
3) placing the leaching residue I in aqua regia, stirring at 60 ℃ for leaching reaction for 4h, diluting the mixed solution after complete reaction, filtering to obtain a leaching solution II and a leaching residue II, and reducing the leaching solution II to extract gold; wherein the mass volume ratio of the leaching residue I to the aqua regia is 1:2 g/ml.
Comparative example 2
1) Putting clay graphite crucible slag powder with the particle size of 200 meshes into a nitric acid solution with the concentration of 63g/L, stirring at normal temperature to carry out leaching reaction for 4 hours, diluting a mixed solution after complete reaction, filtering to obtain leaching slag I and leaching solution I, and reducing the leaching solution I to extract silver; wherein the mass volume ratio of the clay graphite crucible slag powder to the nitric acid solution is 1:3 g/ml;
2) placing the leaching residue I in aqua regia, stirring at 60 ℃ for leaching reaction for 4h, diluting the mixed solution after complete reaction, filtering to obtain a leaching solution II and a leaching residue II, and reducing the leaching solution II to extract gold; wherein the mass volume ratio of the leaching residue I to the aqua regia is 1:2 g/ml.
The results of measuring the mass change before and after calcination and the state after calcination of the filter residue obtained by the leaching reaction of the clay graphite crucible slag powder of example 2 with a sulfuric acid/silicofluoric acid mixed solution and the clay graphite crucible slag powder of comparative example 1 are shown in table 1.
TABLE 1 Clay graphite crucible residue powder and residue before and after calcination Mass changes and calcined State
As can be seen from the data in table 1, the filter residue obtained by leaching the clay graphite crucible slag powder of example 2 with a persulfuric acid/silicofluoric acid mixed solution and the clay graphite crucible slag powder of comparative example 1 are reduced in quality after calcination, which indicates that combustible components are removed during calcination, and the purpose of removing impurities by calcination is achieved. In addition, the mass reduction amount of the filter residue obtained after the clay graphite crucible slag powder of the example 2 is subjected to the leaching reaction by the sulfuric acid/silicofluoric acid mixed solution at the high temperature of 900 ℃ is obviously larger than that of the clay graphite crucible slag powder of the comparative example 1 after being calcined, and the clay graphite crucible slag powder of the comparative example 1 is easy to sinter into blocks; the combustion rate of easily oxidized combustion components in the clay graphite crucible slag powder is improved through the treatment of the sulfuric acid/silicofluoric acid mixed solution, the calcination impurity removal efficiency is improved, and the high-temperature calcination cannot cause agglomeration, so that the extraction rate of gold and silver in the later period is improved.
The contents of gold (Au), silver (Ag) and copper (Cu) in the 5 kinds of materials, i.e., the clay graphite crucible residue powder, i.e., the leaching residue I, i.e., the leaching residue II and ii, of example 1 were measured, and from these, the extraction rates of Au and Ag in the clay graphite crucible residue powder of example 2 were calculated, and the results are shown in Table 2.
TABLE 2 contents of Au, Ag and Cu in the respective substances and extraction rates of Au and Ag
| Substance(s) | Content of Au | Content of Ag | Content of Cu |
| Clay graphite crucible slag powder (50g) | 0.013％ | 5.284％ | 0.71％ |
| Leachate I (75mL) | 0.06mg/L | 33.113g/L | 0.07mg/L |
| Leaching residue I (22.355g) | 0.0288％ | 0.71％ | 0％ |
| Leachate II (50mL) | 0.119g/L | 4.01mg/L | 0mg/L |
| Leaching residue II (22.349g) | 0.002％ | 0.704％ | 0％ |
| Extraction ratio (%) | 91.54％ | 94.00％ | — |
As can be seen from the data in table 2, after the clay graphite crucible slag powder in the present invention is treated with the persulfuric acid/silicofluoric acid mixed solution, a large amount of copper elements therein are removed, so that the separation of the copper elements from gold and silver is well achieved, and the final extraction efficiency of gold and silver is improved.
The extraction rates of gold and silver in the clay graphite crucible slag powders of examples 1 to 3 and comparative examples 1 to 2 were measured, and the results are shown in table 3.
TABLE 3 extraction rates of gold and silver from clay graphite crucible slag powder
| Examples | Extraction ratio of gold (%) | Extraction ratio of silver (%) |
| Example 1 | 90.04％ | 92.87％ |
| Example 2 | 91.54％ | 94.00％ |
| Example 3 | 92.26％ | 94.87％ |
| Comparative example 1 | 7.66％ | 4.34％ |
| Comparative example 2 | 6.49％ | 2.38％ |
As can be seen from the data in table 3, the extraction rate of gold and silver from the clay graphite crucible slag powder using the method of the present invention was greatly improved as compared to the comparative example, and most preferably example 3, in which the extraction rate of gold was 92.26% and the extraction rate of silver was 94.87% in the clay graphite crucible slag powder. The method adopts the combination of the fire method and the wet method to extract the gold and the silver in the clay graphite crucible slag, and compared with the method only adopting the wet method, the method greatly improves the extraction rate of the gold and the silver. And the clay graphite crucible slag reacts with the sulfuric acid/fluosilicic acid mixed solution before being calcined, then is calcined at the temperature of 1000 ℃, and finally is separated by the acid and aqua regia leaching method, compared with the direct calcination without the sulfuric acid/fluosilicic acid mixed solution treatment, the clay graphite crucible slag reacts with the sulfuric acid/fluosilicic acid mixed solution before being calcined, so that the clay graphite crucible slag powder is prevented from being agglomerated in the calcining process, most of copper in the graphite crucible slag is removed, the separation of gold and silver from other impurities is realized, and the leaching recovery rate of gold and silver is improved.
Claims (9)
1. A method for extracting gold and silver from clay graphite crucible slag is characterized by comprising the following steps:
1) reacting clay graphite crucible slag powder with a sulfuric acid/silicofluoric acid mixed solution at 50-70 ℃, and filtering the mixed solution after the reaction is finished to obtain filter residue; the concentration of sulfuric acid in the sulfuric acid/silicofluoric acid mixed solution is 80-150g/L, and the concentration of silicofluoric acid is 100-340 g/L;
2) drying the filter residue, calcining at the temperature of 900-1000 ℃, and then treating to obtain powdery enrichment slag;
3) placing the enrichment slag in a nitric acid solution, stirring at normal temperature for leaching reaction, diluting and filtering a mixed solution after complete reaction to obtain leaching slag I and leaching solution I, and reducing and extracting silver from the leaching solution I;
4) and (3) placing the leaching residue I in aqua regia, stirring at 50-80 ℃ for leaching reaction, diluting the mixed solution after complete reaction, filtering to obtain a leaching solution II, and reducing the leaching solution II to extract gold.
2. The method for extracting gold and silver from clay-graphite crucible slag as claimed in claim 1, wherein the particle size of the clay-graphite crucible slag powder in step 1) is 150-325 mesh.
3. The method for extracting gold and silver from clay graphite crucible slag according to claim 1 or 2, wherein the mass-to-volume ratio of the clay graphite crucible slag powder to the sulfuric acid/silicofluoric acid mixed solution in the step 1) is 1:1-3 g/ml.
4. The method for extracting gold and silver from clay graphite crucible slag as claimed in claim 1 or 2, wherein the reaction time in step 1) is 6-12 h.
5. The method for extracting gold and silver from clay graphite crucible slag as claimed in claim 1 or 2, wherein the calcination time in step 2) is 1.5-3 h.
6. The method for extracting gold and silver from clay graphite crucible slag according to claim 1 or 2, wherein the concentration of the nitric acid solution in the step 3) is 63-130 g/L.
7. The method for extracting gold and silver from clay graphite crucible slag as claimed in claim 1 or 2, wherein the mass volume ratio of the enriched slag to the nitric acid solution in the step 3) is 1:1-5 g/ml.
8. The method for extracting gold and silver from clay graphite crucible slag as claimed in claim 1 or 2, wherein the mass volume ratio of the leaching slag I to aqua regia in the step 4) is 1:1-5 g/ml.
9. The method for extracting gold and silver from clay graphite crucible slag as claimed in claim 1 or 2, wherein the leaching reaction time in the step 4) is 4-6 h.
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