CN111218563A - Method for efficiently recovering palladium from black gold powder - Google Patents
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- CN111218563A CN111218563A CN202010096128.8A CN202010096128A CN111218563A CN 111218563 A CN111218563 A CN 111218563A CN 202010096128 A CN202010096128 A CN 202010096128A CN 111218563 A CN111218563 A CN 111218563A
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Abstract
The invention provides a method for efficiently recovering palladium from black gold powder, which comprises the following process steps: leaching platinum and palladium in the black gold powder by nitric acid according to a liquid-solid ratio of 4: 1; after the solid-liquid separation of the nitrate leaching solution, adding a palladium collecting agent into the nitrate leaching solution at normal temperature, and collecting and precipitating palladium in a liquid phase in a complex form, namely crude palladium salt; calcining the crude palladium salt at a high temperature of 580-620 ℃, dissolving the crude palladium salt by using a chlorination method, and precipitating and recovering palladium in the form of ammonium chloropalladate; the ammonium chloropalladate is subjected to chlorination and precipitation for multiple times to produce a high-quality crude ammonium chloropalladate intermediate product; complexing ammonium chloropalladate by using ammonia water, filtering, adding hydrochloric acid into filtrate for precipitation, and producing an intermediate product of the dichloro-tetra-ammino-palladium solution; heating the purified solution of dichlorotetraammine palladium to 50 +/-5 ℃, filtering, washing for 2-3 times by using dilute hydrochloric acid, and drying the palladium in vacuum at 110 ℃ to obtain the sponge palladium product. The method has the advantages of short time, high efficiency, low energy consumption, high direct yield of palladium and simple operation.
Description
Technical Field
The invention belongs to the technical field of metallurgy, and particularly relates to a method for efficiently recovering palladium from black gold powder.
Background
In the prior art, the following process is generally adopted for recovering palladium from black gold powder: the method comprises the steps of leaching the black gold powder by nitric acid, firstly, precipitating and recovering silver element in a nitrate leaching solution in a silver chloride form by using industrial salt, adding sulfide into the solution after silver precipitation to enrich platinum and palladium, wherein the content of palladium in produced crude platinum and palladium slag is about 0.5-2%, the content of palladium is low, the refining and purification efficiency of palladium is influenced, and the direct yield of palladium is low due to the fact that the content of platinum and palladium in silver chloride is high. Meanwhile, the method for enriching platinum and palladium by utilizing sulfide has the problems of long production period, high energy consumption, poor environment, high labor intensity of workers and the like.
Disclosure of Invention
The invention provides a method for efficiently recovering palladium from black gold powder in order to solve the problems.
The technical scheme of the invention is realized as follows: a method for efficiently recovering palladium from black gold powder comprises the following process steps:
a. leaching platinum and palladium in the black gold powder by nitric acid according to a liquid-solid ratio of 4:1, wherein the platinum and the palladium enter a liquid phase in the form of chloroplatinic acid and chloropalladic acid respectively;
b. after solid-liquid separation of the nitrate leaching solution, adding a palladium collecting agent of a neutral medium into the nitrate leaching solution at normal temperature, wherein the adding amount of the collecting agent is 3-5 times of the amount of palladium metal in the nitrate leaching solution, and collecting and precipitating palladium in a liquid phase in a complex form, namely crude palladium salt;
c. calcining the crude palladium salt at a high temperature of 580-620 ℃, dissolving by a chlorination method, adding ammonium chloride for precipitation, wherein the addition amount of the ammonium chloride is 2-3 times of the amount of palladium metal, and precipitating and recovering palladium in the form of ammonium chloropalladate;
d. chloridizing and precipitating ammonium chloropalladate for 4-5 times to remove most of base metals in the crude palladium salt and produce a high-quality crude ammonium chloropalladate intermediate product;
e. complexing ammonium chloropalladate by using ammonia water, firstly adding 1 time of pure water into the ammonium chloropalladate for slurrying, then adding analytically pure ammonia water under stirring, wherein the addition amount is 2-3 times of the amount of palladium metal, filtering, adding hydrochloric acid into filtrate for precipitation, wherein the addition amount of the hydrochloric acid is 3-5 times of that of palladium salt, detecting the pH value of palladium-precipitated solution to be 1, namely reaching the reaction end point, and performing 3-5 times of circulating operation to produce an intermediate product of the dichlorotetraamminepalladium solution;
f. heating the purified dichlorotetraammine palladium solution to 50 +/-5 ℃, adding hydrazine hydrate under the stirring state, reducing the added amount to be 2-5 times of the amount of palladium metal, reducing the solution to be colorless, standing, filtering, washing for 2-3 times by using dilute hydrochloric acid, washing to be neutral by using distilled water, and drying the palladium at 110 ℃ in vacuum to obtain a sponge palladium product, wherein the main grade of the sponge palladium reaches more than 99.95%;
preferably, the palladium collector comprises the following components in parts by weight: 30-50% of oxime group, 20-30% of ethyl and 30-40% of hydroxyl.
The invention has the beneficial effects that: according to the invention, the high-efficiency palladium collecting agent is adopted, so that the palladium can be efficiently recovered from the black gold powder nitrate leaching solution, and the palladium content in the solution after palladium precipitation can be reduced to below 10 mg/L; the content of the crude palladium residue produced by using the palladium collecting agent is high and reaches over 75 percent, thereby being beneficial to the subsequent purification and refining of palladium; the invention carries out enrichment operation at normal temperature, has short time, high efficiency, greatly reduced energy consumption and high economic benefit; the process has the advantages of high direct yield of palladium up to more than 92.5%, simple operation, high economic benefit and the like.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
For a better understanding and appreciation of the invention, it will be further described in connection with the accompanying drawings:
example 1: take batch 86 of Black powder of this company as an example:
350Kg of black gold powder in the 86 th batch is taken, the palladium content is 1250g/t, the palladium metal content is 437.5g, and the process steps are as follows:
a. leaching platinum and palladium in the black gold powder by nitric acid according to a liquid-solid ratio of 4:1, reacting for 3 hours, allowing the platinum and the palladium to enter a liquid phase in the form of chloroplatinic acid and chloropalladic acid respectively, wherein the platinum and palladium contents in a nitric acid leaching solution are shown in table 1;
TABLE 1 platinum and Palladium element content (/ mg/L) in Black gold powder Mirabilite immersion liquid
| Name (R) | Pt | Pd | Remarks for note |
| Nitre immersion liquid | 85.0 | 450.0 |
b. After the solid-liquid separation of the nitrate leaching solution, adding 1530g of palladium collecting agent into the nitrate leaching solution at normal temperature, wherein the palladium collecting agent comprises 688g of oxime group, 368g of ethyl group and 474g of hydroxyl group, the palladium collecting agent is white solid powder in appearance, is odorless and insoluble in water, and hydrogen in the collecting agent reduces palladium to produce a palladium complex compound, and the main reaction mechanism is as follows: [ HCn-HC=N-O](abbreviation R)-）+Pd2+=PdR2+2H+The adding amount is 1530g, the reaction time is 1 hour, palladium in the liquid phase is collected and precipitated in a complex form (commonly called crude palladium salt), and the analysis results of the liquid after palladium precipitation and the obtained crude palladium salt are shown in tables 2 and 3;
TABLE 2 platinum palladium element content (/ mg/L) after palladium collector addition
| Name (R) | Pt | Pd | Remarks for note |
| After palladium precipitation, the solution | 75.0 | 4.6 |
Table 3 analysis of Palladium content in crude Palladium salt yielded (/%)
| Name (R) | Pt | Pd | Remarks for note |
| Crude palladium salt | 0.5 | 78.80 |
c. Calcining the crude palladium salt at a high temperature of 600 ℃, dissolving by using a chlorination method, adding 875g of ammonium chloride for precipitation, and precipitating and recovering palladium in the form of ammonium chloropalladate; (534 g total of the calcined crude palladium salt, 420.8g of palladium metal and 96.18% direct yield of palladium)
d. Most of base metals in the crude palladium salt can be removed by chlorination and precipitation of the ammonium chloropalladate for 4 times, and a high-quality crude ammonium chloropalladate intermediate product is produced;
e. complexing ammonium chloropalladate by using ammonia water, firstly adding 1 time of pure water into the ammonium chloropalladate for slurrying, then adding 875g of analytically pure ammonia water under stirring, filtering, adding 1602g of hydrochloric acid into filtrate for precipitation, detecting the pH value of palladium-precipitated liquid to be 1, namely reaching the reaction end point, and performing 4 times of circulating operation to obtain an intermediate product of the dichloro-tetra-ammino-palladium solution;
f. heating the purified solution of dichlorotetraammine palladium to 50 ℃, adding 1750g of hydrazine hydrate under the stirring state, reducing the solution until the solution is colorless, standing, filtering, washing for 3 times by using dilute hydrochloric acid, washing to be neutral by using distilled water, and drying the palladium under the vacuum condition at the temperature of 110 ℃ to obtain the sponge palladium product, wherein the main grade of the sponge palladium reaches more than 99.95 percent.
The production period of the crude palladium salt after purification and refining is 6 days, the production cost is 11500 yuan/Kg, 405.50g of palladium product with the content of more than 99.95 percent is obtained, and the total direct yield of palladium reaches 92.68 percent, which is shown in Table 4.
TABLE 4 recovery of Palladium from Black gold powder Nitro leach solution (%)
| Element(s) | Pd | |
| Direct yield of Palladium (%) | 92.68 |
Comparative example 1: 350Kg of 86 th batch of black gold powder is taken, the palladium content is 1250g/t, the palladium metal content is 437.5g, the production cost of palladium enrichment by adopting the traditional vulcanization method is 26800 yuan/Kg, the production period is 15 days, and the direct yield of palladium is 45%.
Example 2: 375Kg of black gold powder of 87 th batch with palladium content of 680g/t and palladium metal content of 255.0g is taken, and the process steps are as follows:
a. leaching platinum and palladium in the black gold powder by nitric acid according to a liquid-solid ratio of 4:1, reacting for 3 hours, allowing the platinum and the palladium to enter a liquid phase in the form of chloroplatinic acid and chloropalladic acid respectively, wherein the platinum and palladium contents in a nitric acid leaching solution are shown in table 5;
TABLE 5 platinum and Palladium element content (/ mg/L) in Black gold powder Mirabilitum immersion liquid
| Name (R) | Pt | Pd | Remarks for note |
| Nitre immersion liquid | 42.0 | 225.0 |
b. After solid-liquid separation of the nitre leaching solution, 1025g of palladium collecting agent is added into the nitre leaching solution at normal temperature, wherein the palladium collecting agent comprises 462g of oxime group, 245g of ethyl group and 318g of hydroxyl group, and the appearance of the palladium collecting agent is white solid powderThe method is odorless and water-insoluble, palladium is reduced by hydrogen in the collecting agent to produce a palladium complex, and the main reaction mechanism is as follows: [ HCn-HC=N-O](abbreviation R)-） + Pd2+= PdR2+ 2H+The adding amount is 1025g, the reaction time is 1 hour, palladium in the liquid phase is collected and precipitated in a complex form (commonly called crude palladium salt), and the analysis results of the liquid after palladium precipitation and the obtained crude palladium salt are shown in tables 6 and 7;
TABLE 6 elemental platinum and Palladium content (/ mg/L) after Palladium collector addition
| Name (R) | Pt | Pd | Remarks for note |
| After palladium precipitation, the solution | 38.0 | 8.6 |
Table 7 analysis of Palladium content in crude Palladium salt yielded (/%)
| Name (R) | Pt | Pd | Remarks for note |
| Crude palladium salt | 0.45 | 76.5 |
c. Calcining the crude palladium salt at the high temperature of 620 ℃, dissolving by using a chlorination method, adding 765g of ammonium chloride for precipitation, recovering 318g of palladium by using ammonium chloropalladate as precipitate, wherein the total amount of the calcined crude palladium salt is 243.27g, and the direct yield of palladium is 95.40%;
d. most of base metals in the crude palladium salt can be removed by chlorination and precipitation of the ammonium chloropalladate for 5 times, and a high-quality crude ammonium chloropalladate intermediate product is produced;
e. complexing ammonium chloropalladate by using ammonia water (palladium enters a liquid phase in a form of dichloro tetraammine palladium), firstly adding 1 time of pure water into the ammonium chloropalladate for slurrying, then adding analytical pure ammonia water under stirring, wherein the adding amount is 765g, filtering, adding hydrochloric acid into filtrate for precipitation, wherein the adding amount of hydrochloric acid is 1590g, detecting the pH value of a solution after palladium precipitation to be 1, namely reaching the reaction end point, and carrying out 5 times of circulating operation to produce an intermediate product of dichloro tetraammine palladium solution;
f. heating the purified solution of dichlorotetraammine palladium to 55 ℃, adding 1275g of hydrazine hydrate under the stirring state, reducing the solution until the solution is colorless, standing, filtering, washing for 3 times by using dilute hydrochloric acid, washing to be neutral by using distilled water, and drying the palladium under the vacuum condition at the temperature of 110 ℃ to obtain the sponge palladium product, wherein the main grade of the sponge palladium reaches more than 99.95 percent.
The production period of the crude palladium salt after purification and refining is 6 days, the production cost is 12100 yuan/Kg, 236.00g of palladium product with the content of more than 99.95 percent is obtained, and the total direct yield of palladium reaches 92.55 percent, which is shown in Table 8.
TABLE 8 recovery of Palladium from Black gold powder Nitro leach liquor (%)
| Element(s) | Pd | |
| Direct yield of Palladium (%) | 92.55 |
Comparative example 2:
375Kg of black gold powder of 87 th batch is taken, the palladium content is 680g/t, the palladium metal content is 255.0g, the production cost of palladium enrichment by adopting the traditional vulcanization method is 26000 yuan/Kg, the production period is 15 days, and the total direct yield of palladium is 40.5 percent.
The comparative results are shown in Table 9.
TABLE 9
| Production cost (Yuan/Kg) | Production period (sky) | Direct yield of Palladium (%) | |
| Example 1 | 11500 | 6 | 92.68 |
| Example 2 | 12100 | 6 | 92.55 |
| Comparative example 1 | 26800 | 15 | 45 |
| Comparative example 2 | 26000 | 15 | 40.5 |
According to the invention, palladium is efficiently recovered from the black gold powder nitrate leaching solution by adopting a palladium collecting agent, and the palladium content in the solution after palladium precipitation can be reduced to below 10 mg/L; the content of palladium in the crude palladium residue produced by using the palladium collecting agent is high, and reaches more than 75%, so that the subsequent purification and refining of palladium are facilitated; the invention carries out enrichment operation at normal temperature, has short time, high efficiency and greatly reduced energy consumption, and can generate larger economic benefit; the palladium enrichment process has the advantages of high direct yield of palladium up to more than 92.5%, simple operation, high economic benefit and the like.
Claims (2)
1. A method for efficiently recovering palladium from black gold powder is characterized by comprising the following process steps:
a. leaching platinum and palladium in the black gold powder by nitric acid according to a liquid-solid ratio of 4:1, wherein the platinum and the palladium enter a liquid phase in the form of chloroplatinic acid and chloropalladic acid respectively;
b. after solid-liquid separation of the nitrate leaching solution, adding a palladium collecting agent of a neutral medium into the nitrate leaching solution at normal temperature, wherein the adding amount of the collecting agent is 3-5 times of the amount of palladium metal in the nitrate leaching solution, and collecting and precipitating palladium in a liquid phase in a complex form, namely crude palladium salt;
c. calcining the crude palladium salt at a high temperature of 580-620 ℃, dissolving by a chlorination method, adding ammonium chloride for precipitation, wherein the addition amount of the ammonium chloride is 2-3 times of the amount of palladium metal, and precipitating and recovering palladium in the form of ammonium chloropalladate;
d. chloridizing and precipitating ammonium chloropalladate for 4-5 times to remove most of base metals in the crude palladium salt and produce a high-quality crude ammonium chloropalladate intermediate product;
e. complexing ammonium chloropalladate by using ammonia water, firstly adding 1 time of pure water into the ammonium chloropalladate for slurrying, then adding analytically pure ammonia water under stirring, wherein the addition amount is 2-3 times of the amount of palladium metal, filtering, adding hydrochloric acid into filtrate for precipitation, wherein the addition amount of the hydrochloric acid is 3-5 times of that of palladium salt, detecting the pH value of palladium-precipitated solution to be 1, namely reaching the reaction end point, and performing 3-5 times of circulating operation to produce an intermediate product of the dichlorotetraamminepalladium solution;
f. heating the purified dichlorotetraammine palladium solution to 50 +/-5 ℃, adding hydrazine hydrate under the stirring state, reducing the added amount to be 2-5 times of the amount of palladium metal, standing, filtering, washing for 2-3 times by using dilute hydrochloric acid, washing to be neutral by using distilled water, and drying the palladium at 110 ℃ in vacuum to obtain the sponge palladium product, wherein the main grade of the sponge palladium reaches more than 99.95%.
2. The method of claim 1, wherein the palladium collector comprises the following components in parts by weight: 30-50% of oxime group, 20-30% of ethyl and 30-40% of hydroxyl.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111850300A (en) * | 2020-06-19 | 2020-10-30 | 西部矿业股份有限公司 | Method for efficiently enriching platinum and palladium from low-concentration platinum-palladium nitric acid system solution |
| CN114807616A (en) * | 2022-04-27 | 2022-07-29 | 南京桦冠生物技术有限公司 | Method for recovering enriched palladium from palladium-containing organic waste liquid |
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| CN111850300A (en) * | 2020-06-19 | 2020-10-30 | 西部矿业股份有限公司 | Method for efficiently enriching platinum and palladium from low-concentration platinum-palladium nitric acid system solution |
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