CN111438354A - Clean production method of high-purity gold powder - Google Patents
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Abstract
The invention relates to the technical field of high-purity gold preparation, and provides a clean production method of high-purity gold powder. The method provided by the invention has the advantages of high gold dissolving speed and simple flow, and the purity of the obtained high-purity gold powder can reach 5N level, thereby meeting the quality requirements of GB 25933-2010. Furthermore, the raffinate and the strip liquor can be used for recovering iodine through electrolysis, and the extracting agent can be recycled after regeneration, so that the method provided by the invention has the advantages of no wastewater discharge, energy conservation and emission reduction to the maximum extent, and further saves a large amount of environment-friendly facility investment and three-waste treatment cost.
Description
Technical Field
The invention relates to the technical field of high-purity gold preparation, in particular to a clean production method of high-purity gold powder.
Background
High-purity gold is used as an important raw material in the electronic industry, and the usage amount of the high-purity gold is increased year by year. China firstly puts forward the quality standard GB/T25933-2010 of high-purity gold products in 2010. The analytical method standard GB/T25934- (1, 2, 3) -2011 is proposed in 2011.
Currently, high-purity gold abroad is mainly prepared by a DBC extraction method and an electrolytic method. The patent with the publication number of CN101122032A provides a method for preparing high-purity gold by an electrolysis method, the method has a long flow, much gold is accumulated in the flow, the electrolysis time is long, electrolysis is required for 48-60 hours, the accumulation of impurities in the electrolyte is fast, impurities need to be frequently purified, and HCl wastewater is discharged. The patent publication No. CN104789794A proposes a method for preparing high-purity gold by secondary chlorination and secondary reduction, wherein the whole process takes more than 30 hours, and SO2, HCl and Cl are discharged in the preparation process2When the waste gas is used, waste hydrochloric acid with the concentration of 12% -18% can be discharged, the investment of environmental protection facilities is large, the treatment cost is high, and the clean production in the real sense can not be realized. The patent with the publication number of CN101985691A proposes a scheme for preparing high-purity gold by DBC extraction, the purity of the high-purity gold prepared by the method can only reach 99.995 percent, the quality requirements of GB25933-2010 cannot be met, and the method also has the problem of discharging waste water and waste gas.
Disclosure of Invention
In view of the above, the invention provides a clean production method of high-purity gold powder. The production method provided by the invention has the advantages of simple flow, high gold dissolving speed and no waste water and gas emission, and the purity of the obtained high-purity gold powder can reach 5N level.
In order to achieve the above object, the present invention provides the following technical solutions:
a clean production method of high-purity gold powder comprises the following steps:
(1) mixing low-purity gold powder, ion exchange water, potassium iodide, iodine and potassium iodate, and dissolving the low-purity gold powder to obtain a gold-containing solution; the purity level of the low-purity gold powder is 3N;
(2) adjusting the pH value of the gold-containing solution to 9.5-11 by using potassium hydroxide, and then filtering to obtain filtrate;
(3) extracting the filtrate to obtain an organic phase;
(4) and (3) performing back extraction on the organic phase by using a potassium hydroxide solution, and sequentially washing and drying the obtained solid product to obtain high-purity gold powder with the purity level of 5N.
Preferably, the particle size of the low-purity gold powder is 60-200 meshes.
Preferably, the dosage ratio of the low-purity gold powder to the ion exchange water to the potassium iodide to the iodine to the potassium iodate is 10kg to 95L to 35 to 40kg to 23 to 26kg to 3 to 5 kg.
Preferably, the dissolving temperature in the step (1) is 40-50 ℃, and the time is 30-50 min.
Preferably, the extractant for extraction is a mixed solution of N235 and sulfonated kerosene; the volume fraction of N235 in the extracting agent is 30-35%, and the volume fraction of sulfonated kerosene is 65-70%; the ratio of O/A of the extraction is 1: 1; the extraction stages are 3 stages.
Preferably, the mass concentration of the potassium hydroxide solution in the step (4) is 20-25%; the phase ratio O/A of the back extraction is 2: 1; the stage number of the back extraction is 2 stages.
Preferably, after the extraction and the back extraction are completed, the method further comprises the step of electrolyzing raffinate generated by the extraction and back extraction solution to regenerate and recycle iodine; the electrolytic regeneration comprises the following steps: and mixing the raffinate, the strip liquor and the potassium iodide, and electrolyzing.
Preferably, the anode of the electrolysis is an iridium-plated titanium plate, the cathode of the electrolysis is a titanium plate, the temperature of the electrolysis is 10-40 ℃, the time is 18-24 h, the voltage is 3.0-3.6V, and the current density is 230-360A/m2。
Preferably, after the back extraction, the method further comprises the step of regenerating the waste extracting agent obtained by the back extraction; the regeneration is as follows: the spent extractant is washed counter-currently with a potassium iodide-potassium hydroxide mixture.
Preferably, the concentration of potassium iodide in the potassium iodide-potassium hydroxide mixed solution is 1-2 mol/L, and the concentration of potassium hydroxide is 0.5-1.0 mol/L.
The invention provides a clean production method of high-purity gold powder, which is characterized by dissolving low-purity gold powder by using iodine, potassium iodide, potassium iodate and ion exchange water, then adjusting the pH value of an obtained gold-containing solution to 9.5-11 by using potassium hydroxide, then filtering, and extracting and back-extracting filtrate to obtain the high-purity gold powder. The invention utilizes iodine, potassium iodide and potassium iodate to assist gold powder to dissolve, can make gold enter solution in the form of potassium iodoaurate, then remove metallic impurity such as silver and copper in the gold-containing solution through regulating pH value and filtering, extract the iodogold acid radical into organic phase through extracting, make gold precipitate out in the form of simple substance through back extraction finally, thus get the high-purity gold powder. The method provided by the invention has the advantages of high gold dissolving speed and simple flow, and the purity of the obtained high-purity gold powder can reach 5N level, thereby meeting the quality requirements of GB 25933-2010. Furthermore, the raffinate and the strip liquor can be used for recovering iodine through electrolysis, and the extracting agent can be recycled after regeneration, so that the method provided by the invention has the advantages of no wastewater discharge, energy conservation and emission reduction to the maximum extent, and further saves a large amount of environment-friendly facility investment and three-waste treatment cost.
Drawings
FIG. 1 is a schematic flow chart of the clean production method of high purity gold powder according to the present invention;
FIG. 2 is a schematic diagram of the high purity gold powder prepared in example 1.
Detailed Description
The invention provides a clean production method of high-purity gold powder, which comprises the following steps:
(1) mixing low-purity gold powder, ion exchange water, potassium iodide, iodine and potassium iodate, and dissolving the low-purity gold powder to obtain a gold-containing solution; the purity level of the low-purity gold powder is 3N;
(2) adjusting the pH value of the gold-containing solution to 9.5-11 by using potassium hydroxide, and then filtering to obtain filtrate;
(3) extracting the filtrate to obtain an organic phase;
(4) and (3) performing back extraction on the organic phase by using a potassium hydroxide solution, and sequentially washing and drying the obtained solid product to obtain high-purity gold powder with the purity level of 5N.
The method mixes low-purity gold powder, ion exchange water, potassium iodide, iodine and potassium iodate, and dissolves the low-purity gold powder to obtain the gold-containing solution. In the invention, the purity grade of the low-purity gold powder is 3N, and the particle size of the low-purity gold powder is preferably 60-200 meshes, and more preferably 100-180 meshes; the low-purity gold powder is preferably obtained by pulverizing gold with the purity level of 3N, wherein the gold content in the gold with the purity level of 3N is more than 99.9%, and the low-purity gold powder also contains a small amount of elements such as silver, copper, palladium, platinum and the like; the invention has no special requirements on the powder preparation, and the gold powder with the grain diameter meeting the requirements can be obtained by using a method well known by the technical personnel in the field.
In the invention, the dosage ratio of the low-purity gold powder to the ion exchange water to the potassium iodide to the potassium iodate is preferably 10kg to 95L: 35-40 kg to 23-26 kg to 3-5 kg, more preferably 10kg to 95L: 36-38 kg to 24-25 kg to 3.5-4.5 kg..
In the invention, the dissolving temperature is preferably 40-50 ℃, more preferably 42-45 ℃, and the dissolving time is preferably 30-50 min, more preferably 35-45 min; in the present invention, the dissolution is preferably carried out in a plastic reaction vessel; in the dissolving process, the gold powder reacts with iodine and potassium iodide to generate gold potassium iodate, and the reaction formula is shown as a formula I; in the dissolving process, potassium iodate is added to play a role in assisting oxidation and promote the dissolution of the low-purity gold powder.
2Au+3I2+2KI＝2KAuI4Formula I.
After the gold-containing solution is obtained, the pH value of the gold-containing solution is adjusted to 9.5-11 by using potassium hydroxide, and then the gold-containing solution is filtered to obtain filtrate. In the present invention, the purity of the potassium hydroxide is preferably superior grade purity; the method preferably adjusts the pH value of the gold-containing solution to 10-10.5 and then filters the gold-containing solution; in the invention, the pH value of the gold-containing solution obtained in the step (1) is about 7-7.5, and a small amount of metal ions such as silver, copper and the like existing in the gold-containing solution are precipitated by adjusting the pH value of the gold-containing solution to 10-10.5 and are removed by filtering. In the present invention, the filtration is preferably carried out in a precision filter; the filter residue obtained by filtering is preferably retained for recovering silver and copper. The method for recovering silver and copper in the invention has no special requirements, and the method which is well known to the person skilled in the art can be used.
After the filtrate is obtained, the invention extracts the filtrate to obtain an organic phase. In the present invention, the extraction solvent is preferably a mixture of N235 (trioctyl decyl tertiary amine) and sulfonated kerosene; the volume fraction of N235 in the extracting agent is preferably 30-35%, more preferably 32-33%, and the volume fraction of sulfonated kerosene is preferably 65-70%, more preferably 66-68%; the phase ratio O/A of the extraction is preferably 1: 1; the extraction stage number is preferably 3, and the extraction rate of gold after 3-stage extraction can reach more than 99.92%; the extraction is preferably carried out in a centrifugal extractor. The invention uses the mixed liquid of N235 and sulfonated kerosene as an extracting agent to extract the gold iodate into an organic phase, and a small amount of platinum and palladium in the filtrate is not extracted basically. In the present invention, the raffinate from the extraction is subjected to electrolysis together with the strip liquor in the subsequent steps to recover iodine, as will be described in detail later.
After the organic phase is obtained, the method uses potassium hydroxide solution to perform back extraction on the organic phase, and the obtained solid product is washed and dried in sequence to obtain the high-purity gold powder with the purity level of 5N. In the invention, the mass concentration of the potassium hydroxide solution is preferably 20-25%, and more preferably 22-24%; the preferable ratio of O/A of the back extraction is 2: 1; the number of stages of the stripping is preferably 2.
In the present invention, the washing is preferably: firstly, the solid product is soaked and washed by nitric acid, and then is washed to be neutral by ion exchange water; the nitric acid is preferably superior pure nitric acid with the mass concentration of 5-10%; the time of the immersion is preferably 30min, and the immersion is preferably carried out under boiling conditions. The invention removes trace metal impurities such as silver, copper and the like in the solid product through nitric acid immersion cleaning.
According to the invention, the gold iodate in an organic phase is precipitated in the form of a gold simple substance by potassium hydroxide back extraction, and is separated by filtration, wherein the reaction generated in the back extraction process is shown as a formula II.
2N235*AuI4+6KOH＝2N235+2Au+5KI+KIO3+3H2O is shown as formula II.
In the present invention, the water phase remaining after stripping is a strip liquor, and the strip liquor produced in the stripping process and the strip liquor are preferably combined for electrolytic regeneration to recover iodine.
In the invention, the electrolytic regeneration preferably comprises the following steps of mixing raffinate, strip liquor and potassium iodide, then carrying out electrolysis, preferably mixing the raffinate and the strip liquor, then concentrating, then mixing the concentrated solution and the potassium iodide, and carrying out electrolysis, wherein the concentration is preferably carried out by using a vacuum concentration device, the concentration is not particularly limited, and the concentration is carried out according to a method well known by a person skilled in the art, the addition amount of the potassium iodide is not particularly limited, in a specific embodiment of the invention, the concentration of the potassium iodide in the mixed solution for electrolysis is preferably controlled to be not less than 580 g/L, the electrolysis is preferably carried out in a diaphragm electrolytic cell made of a sealed polyvinyl chloride plate, a diaphragm of the diaphragm cell is preferably an ion exchange membrane, an electrolytic anode is an iridium-plated titanium plate, a cathode is a titanium plate, the temperature of the electrolysis is preferably 10-40 ℃, more preferably 15-30 ℃, the time of the electrolysis is preferably 18-24 h, more preferably 20-22 h, the voltage of the electrolysis is preferably 3.0-3.6V, more preferably 3.2V, and the density of the electrolysis is preferably 3.2-3.4V, and the current of the electrolysis is preferably 360A/230-3602More preferably 250 to 320A/m2(ii) a The electrolytic time is excellentThe anode region and the cathode region are both cooled by adopting low-temperature circulating cooling pumps to prevent iodine volatilization loss, and in the invention, the electrolysis is preferably stopped when the iodine concentration in the electrolytic bath reaches 230-260 g/L and the KI concentration reaches 220-250 g/L.
In the invention, potassium iodide and potassium hydroxide respectively react at the anode and the cathode in the electrolysis process, and a mixed solution of iodine and potassium iodide is obtained in the anode tank, and the mixed solution is preferably returned to the previous step for dissolving the low-purity gold powder; the mixed solution of potassium iodide and potassium hydroxide is obtained in the cathode tank, and the mixed solution is preferably returned to the back extraction step to be used as a back extractant, and when the mixed solution is used as the back extractant, the mixed solution can be used only once, and the back extractant is electrolyzed and regenerated after the back extraction once.
In the invention, the residual organic phase after back extraction is the waste extractant, the waste extractant is preferably regenerated, in the invention, the regeneration is preferably carried out by using a potassium iodide-potassium hydroxide mixed solution to carry out countercurrent washing on the waste extractant, the concentration of potassium iodide in the potassium iodide-potassium hydroxide mixed solution is preferably 1-2 mol/L, the concentration of potassium hydroxide is preferably 0.5-1 mol/L, the stage number of the countercurrent washing is preferably 3, in the invention, impurity metal complex anions (mainly platinum group metal complex anions) adsorbed in the waste extractant are removed by virtue of countercurrent washing, in the invention, the regenerated extractant is preferably returned to the extraction step for recycling, the washing liquid generated by the countercurrent washing is preferably recycled, in the invention, the washing liquid which cannot be used continuously is preferably recycled for 20 times, then the washing liquid, the back extraction liquid and the extraction liquid are mixed, and the electrolytic regeneration is carried out after the joint concentration.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention.
In the embodiment, a schematic diagram of a preparation process of high-purity gold powder is shown in fig. 1, wherein 3N gold is prepared into gold powder, the pH value of a solution is adjusted to 9.5-11 after the gold powder is dissolved, then silver residue is obtained by filtering, filtrate is extracted, an organic phase obtained by extraction is subjected to back extraction, and the obtained gold powder is subjected to digestion and washing to obtain 5N gold powder; the extractant generated by back extraction is regenerated and then returns to the extraction step for reuse; and electrolyzing the strip liquor generated by strip extraction and the raffinate generated by extraction, obtaining a mixed liquor of iodine and potassium iodide at the anode, returning to the step of dissolving the gold powder for recycling, obtaining a mixed liquor of potassium iodide and potassium hydroxide at the cathode, and returning to the strip step for recycling.
Example 1
(1) Milling: the gold powder of 60 meshes is prepared by powder making equipment by using 3N gold as a raw material.
(2) And (3) gold dissolving, namely putting 10kg of 60-mesh gold powder into a plastic reaction kettle, adding 95L of ion exchange water, 35kg of potassium iodide, 23kg of iodine and 3kg of potassium iodate, stirring at 40 ℃ to dissolve for 30min, and completely dissolving gold to obtain a gold-containing solution, wherein the purities of the potassium iodide and the potassium iodate are analytically pure.
(3) Adjusting the pH value of the gold-containing solution to 9.5 by using high-grade pure potassium hydroxide, filtering by using a precision filter, retaining filter residues and recovering silver and copper, and sending filtrate to a centrifugal extractor for extraction.
(4) And (3) extraction: gold was extracted with 30% N235+ 70% sulfonated kerosene, comparing O/a to 1:1, stage 3, gold extraction rate more than or equal to 99.92%, almost no extraction of platinum and palladium, separation of organic phase and back extraction, combination of raffinate and back extraction liquid, supplement of proper amount of potassium iodide, electrolysis and regeneration of iodine.
(5) Back extraction: the organic phase was back-extracted with 25% potassium hydroxide solution, comparing O/a to 2:1, the back extraction stage number is 2, so that gold powder is obtained, the obtained gold powder is soaked and washed by 5 percent high-grade pure nitric acid for 30 minutes, then washed by ion exchange water to be neutral, and vacuum-dried, so that high-purity gold powder is obtained.
The first-stage stripping solution generated in the stripping process is directly combined with the raffinate for electrolysis and regeneration, and the second-stage stripping solution is returned for once electrolysis and regeneration.
(6) Regeneration
Mixing raffinate and stripping solution, concentrating, adding a proper amount of potassium iodide, feeding the obtained mixed solution (the concentration of potassium iodide in the mixed solution is not lower than 580 g/L) into a diaphragm electrolytic cell made of a sealed polyvinyl chloride plate for electrolysis, wherein a diaphragm of the electrolytic cell adopts a cation exchange membrane, an iridium-plated titanium plate is adopted as an anode, a titanium plate is adopted as a cathode, the area of the anode is 50 x 65cm, the area of the cathode is 50 x 65cm, the temperature of the cell is 20-35 ℃, the voltage is 3.0V, and the current density is 230-360A/m2Cooling the cathode region of the anode region by adopting a low-temperature circulating cooling pump, electrolyzing for 18-24 hours until the iodine concentration reaches 230-260 g/L, stopping electrolysis, obtaining a mixed solution of iodine and potassium iodide in an anode tank, returning to the gold dissolving step for recycling, obtaining a mixed solution of potassium iodide and potassium hydroxide in a cathode tank, and returning to the back extraction step for recycling;
(7) and (3) regenerating the extractant, namely performing countercurrent washing on the waste extractant by using a potassium iodide-potassium hydroxide mixed solution (the concentration of potassium iodide in the mixed solution is 1-2 mol/L, and the concentration of potassium hydroxide in the mixed solution is 0.5-1 mol/L), wherein the washing stage number is 3, the regenerated extractant can be returned to the extraction step for reuse, and the washing solution is recycled for 20 times and then is merged into secondary back-extraction solution for concentration for electrolytic regeneration.
The material diagram of the obtained high-purity gold powder is shown in fig. 2, the element content of the obtained high-purity gold powder is detected according to GB/T25933-2010, and the detection results are shown in table 1.
TABLE 1 test results of high purity gold element content
According to the results in the table 1, the purity of the high-purity gold powder prepared by the invention reaches 5N level, and meets the requirements of GB/T25933-2010.
Example 2
Other conditions were the same as in example 1 except that the ratio of the amounts of the low-purity gold powder, ion-exchanged water, potassium iodide, iodine and potassium iodate in step 2 was changed to 10 kg: 95L: 40 kg: 25 kg: 5kg, the dissolution temperature was changed to 50 ℃ and the dissolution time was changed to 35 min.
The purity of the obtained high-purity gold powder is detected, and the result shows that the purity of the high-purity gold powder can reach 5N level and meet the requirement of GB/T25933-2010.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The clean production method of the high-purity gold powder is characterized by comprising the following steps:
(1) mixing low-purity gold powder, ion exchange water, potassium iodide, iodine and potassium iodate, and dissolving the low-purity gold powder to obtain a gold-containing solution; the purity level of the low-purity gold powder is 3N;
(2) adjusting the pH value of the gold-containing solution to 9.5-11 by using potassium hydroxide, and then filtering to obtain filtrate;
(3) extracting the filtrate to obtain an organic phase;
(4) and (3) performing back extraction on the organic phase by using a potassium hydroxide solution, and sequentially washing and drying the obtained solid product to obtain high-purity gold powder with the purity level of 5N.
2. The production method according to claim 1, wherein the low-purity gold powder has a particle size of 60 to 200 mesh.
3. The production method according to claim 1, wherein the low-purity gold powder, the ion-exchange water, the potassium iodide, the iodine and the potassium iodate are used in a ratio of 10kg to 95L: 35 to 40kg to 23kg to 26kg to 3kg to 5 kg.
4. The production method according to claim 1, wherein the dissolving in the step (1) is carried out at a temperature of 40 to 50 ℃ for 30 to 50 min.
5. The production method according to claim 1, wherein the extractant for extraction is a mixed solution of N235 and sulfonated kerosene; the volume fraction of N235 in the extracting agent is 30-35%, and the volume fraction of sulfonated kerosene is 65-70%; the ratio of O/A of the extraction is 1: 1; the extraction stages are 3 stages.
6. The production method according to claim 1, wherein the mass concentration of the potassium hydroxide solution in the step (4) is 20-25%; the phase ratio O/A of the back extraction is 2: 1; the stage number of the back extraction is 2 stages.
7. The production method of claim 1, wherein after the extraction and the stripping are completed, the method further comprises the steps of performing electrolytic regeneration on raffinate produced by the extraction and strip liquor produced by the stripping to recover iodine; the electrolytic regeneration comprises the following steps: and mixing the raffinate, the strip liquor and the potassium iodide, and electrolyzing.
8. The production method according to claim 7, wherein the anode of the electrolysis is an iridium-plated titanium plate, the cathode is a titanium plate, the temperature of the electrolysis is 10-40 ℃, the time is 18-24 h, the voltage is 3.0-3.6V, and the current density is 230-360A/m2。
9. The production method according to claim 1, characterized in that after the back extraction, the method further comprises regenerating the waste extractant obtained by the back extraction; the regeneration is as follows: the spent extractant is washed counter-currently with a potassium iodide-potassium hydroxide mixture.
10. The method of claim 9, wherein the potassium iodide-potassium hydroxide mixture has a potassium iodide concentration of 1 to 2 mol/L and a potassium hydroxide concentration of 0.5 to 1.0 mol/L.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114453589A (en) * | 2022-02-18 | 2022-05-10 | 贵研铂业股份有限公司 | Preparation method of high-purity gold |
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