CN112342572A - Method for recycling low-concentration platinum in organic waste liquid - Google Patents
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Abstract
The invention provides a method for recovering and treating low-concentration platinum in organic waste liquid, which comprises the following steps: A. filling ion exchange resin, inert conductive materials and sacrificial anode metal balls into an electrochemical three-dimensional electrode bed layer to construct a three-dimensional electrode system; B. and (3) carrying out electrodeposition recovery on the platinum in the organic waste liquid by using the three-dimensional electrode system. The method solves the problem of difficult recovery of low-concentration platinum, has the advantages of simple process and low energy consumption, and is suitable for wide industrial application.
Description
Technical Field
The invention relates to a treatment method, in particular to a recovery treatment method of low-concentration platinum in organic waste liquid.
Background
Platinum Group Metal (PGM) -containing waste materials are valuable secondary energy sources, and enhancement of recovery of PGM from the waste materials is of great significance to social and economic development and realization of recycling economy. The traditional method for recovering platinum from organic waste liquid comprises the steps of burning an organic phase, dissolving residues by aqua regia, and then extracting and recovering platinum-containing substances in the residues by using an extracting agent, but because the further separation process of the platinum-containing substances and the extracting agent is complex, long in period and intermittent in operation, the separation is incomplete, the platinum loss in the separation process is large, platinum in the organic waste liquid with the platinum content of less than 200ppm is generally not recovered in the prior art, so that the great waste of rare resources is caused, and particularly under the condition of large platinum-containing organic waste liquid amount.
CN1493706A provides a solution for recovering platinum element from inorganic aqueous solution, in which platinum group metals in the solution are first formed into a chlorine complex, then adsorbed by polyamine-based anion exchange resin, and finally washed and desorbed by the exchange resin. The main treatment body of the technology is inorganic aqueous solution, is not suitable for organic waste liquid, and does not provide a solution for recovering platinum element in anhydrous (approximately anhydrous) organic waste liquid; meanwhile, the method of firstly adsorbing and then washing and desorbing by using the ion exchange resin can generate a large amount of salt-containing wastewater, and is not economical.
Disclosure of Invention
The invention provides a method for recovering and treating low-concentration platinum in organic waste liquid, which is characterized in that a three-dimensional electrode electrodeposition method is used for recovering platinum elements in anhydrous (approximately anhydrous) organic waste liquid, and cation exchange resin is arranged in a three-dimensional electrode to adsorb and intercept platinum ions, so that the technical problems of high difficulty and high energy consumption in recovering the low-concentration platinum in the organic waste liquid can be solved.
In order to solve the technical problems, the invention is realized by the following technical scheme:
a method for recovering and treating low-concentration platinum in organic waste liquid comprises the following steps:
A. uniformly mixing ion exchange resin, an inert conductive material and a sacrificial anode metal ball, and filling the mixture into an electrochemical three-dimensional electrode bed layer to construct a three-dimensional electrode system; wherein the ion exchange resin functions as a non-conductive material and the inert conductive material, the sacrificial anode metal balls function as a conductive material.
B. And (3) carrying out electrodeposition recovery on low-concentration platinum in the organic waste liquid by using the three-dimensional electrode system.
The inventors have surprisingly found that platinum ions in organic waste liquid can be rapidly deposited on the cathode in the presence of a small amount of water and in an electrolytic environment, and based on this method, low-cost enrichment of platinum group metals in organic waste liquid can be achieved. However, the process consumes a long time and consumes relatively high energy, so the method adopts the sacrificial anode to accelerate the recovery rate of the platinum and reduce the recovery energy consumption. In addition, the invention unexpectedly discovers that the ion exchange resin can continuously adsorb and desorb platinum ions in an electrolytic system, thereby being beneficial to buffering system fluctuation caused by large concentration change of the platinum ions in materials and ensuring the recovery effect of platinum.
In the invention, the organic waste liquid is industrial organic waste liquid containing 5-200ppm of platinum;
preferably, the organic waste liquid is selected from sebacate distillation still residue, anisic aldehyde distillation still residue, trimethylbenzoquinone distillation still residue and p-benzoquinone electrochemical reaction liquid containing organic platinum compounds in the production process.
In a preferred embodiment, the three-dimensional electrode has an electrolytic potential of 3 to 5V, for example, 3V, 4V, 5V, etc., and an electrolytic current density of 200 to 800A/m, depending on the type of reaction in the three-dimensional electrode electrolytic cell and cost reduction considerations2E.g. 200A/m2、300A/m2、400A/m2、500A/m2、600A/m2、7000A/m2、800A/m2Etc., preferably 300 to 500A/m2；
Preferably, the three-dimensional electrode has an electrolysis reaction temperature of 20-80 deg.C, such as 20 deg.C, 30 deg.C, 50 deg.C, 60 deg.C, 80 deg.C, etc., and a reaction time of 5-20min, such as 5min, 10min, 15min, 20 min.
The invention does not limit the type and shape of the electrodes in the electrolytic bath, and all the types and shapes of the electrodes capable of realizing the electrolysis function are covered in the method of the invention.
In a preferred embodiment of the present invention, the ion exchange resin is a cation exchange resin, preferably at least one of cation exchange resins of type 732, type D001, type D113, type D072, type D151 or type D152.
In a preferred embodiment of the present invention, the material of the sacrificial anode metal ball is one or more of iron, zinc, magnesium, aluminum, carbon steel, magnesium alloy, and aluminum alloy.
In a preferred embodiment of the present invention, the inert conductive material is one or more of titanium balls, ferrite, titanium-plated glass or plastic balls, graphite, and activated carbon.
In a preferred embodiment of the present invention, the weight ratio of the ion exchange resin and the inert conductive material in the three-dimensional electrode is 1:1 to 5, such as 1:1, 1: 2. 1:3, 1:4, 1:5, etc., preferably 1: 2-4; the weight ratio of the sacrificial anode metal balls to the inert conductive material is 1:1-8, such as 1:1, 1: 2. 1: 3. 1:4, 1:6, 1:8, etc., preferably 1: 3-6.
In a preferred embodiment of the present invention, the organic waste liquid is mixed with an electrolyte solution before entering the three-dimensional electrode; the electrolyte is one or more of potassium methoxide, sodium methoxide, triethylamine, potassium hydroxide, sodium hydroxide, potassium sulfate and sodium sulfate, and potassium hydroxide and sodium hydroxide are more preferable;
preferably, the dosage of the electrolyte is 0.5-3% of the mass of the organic waste liquid.
In a preferred embodiment of the invention, the electrolyte solution can be pure water or a mixture of water and other alcohol solvents capable of promoting mutual solubility of the system according to different mutual solubility degrees of the solvent system and water in the organic waste liquid; preferably, the alcoholic solvent is one or more of methanol, ethanol, propanol, butanol, pentanol.
For example, the main component of the distillation still residue in the sebacate production process is a sebacate compound slightly soluble in water, so that the electrolyte solution needs to contain not only water but also an alcohol solvent (such as methanol) capable of promoting mutual solubility of water and the sebacate compound; for another example, the main component of the distillation still residual liquid in the succinic acid production process is succinic acid, and the succinic acid can be mutually soluble with water, so that the electrolyte solution only needs water as a solvent.
In a preferred embodiment, the amount of water added to the electrolyte solution is 2 to 3 times the mass of the electrolyte.
In another preferred embodiment, the amount of the alcohol solvent added to the electrolyte solution is 0.5 to 3 times the amount of water added.
The invention adopts an electrochemical three-dimensional electrode method to deposit and recover the low-concentration platinum in the organic waste liquid, thereby solving the problem of difficult recovery of the low-concentration platinum in an organic phase waste liquid system. The ion exchange resin in the three-dimensional electrode can intercept and buffer platinum in the waste liquid, so that the recovery effect is prevented from being influenced by large change of the content of platinum ions in the material; compared with the prior art, the method has the advantages of solving the problem of difficult recovery of low-concentration platinum, having simple process and low energy consumption, and being suitable for wide industrial application.
Detailed Description
The present invention is further illustrated by the following specific examples, which are intended to be illustrative of the invention and are not to be construed as limiting the scope of the invention.
Description of the symbols:
ppm represents 10-6No dimension; ppb represents 10-9And is dimensionless.
The raw material information is as follows:
and (3) residual liquid of a dimethyl sebacate rectifying still: the main components are dimethyl sebacate and heavy components, the platinum content is 20ppm, and the product source is a production process of dimethyl sebacate of Wanhua chemical group Limited company;
and (3) residual liquid of the anisic aldehyde rectifying still: the main components are anisic aldehyde and heavy components, the platinum content is 37ppm, and the product source is the production process of anisic aldehyde of Wanhua chemical group Limited company;
residual liquid of the succinic acid rectifying still: the main components are maleic acid, succinic acid and heavy components, the platinum content is 16ppm, and the product source is a succinic acid production process of Wanhua chemical group Limited company;
type 732 cation exchange resin: the total exchange capacity mmol/g of the gallery ancient resource chemical building materials Limited company is more than or equal to 4.50, (the grain diameter is 1.0 mm);
type D113 cation exchange resin: the total exchange capacity mmol/g of the gallery ancient resource chemical building materials Limited company is more than or equal to 10.8 and the particle size is 1.0 mm;
type D001 cation exchange resin: shanghai Kaiping resin Co., Ltd., total exchange capacity mmol/g is not less than 4.6, (particle diameter 1.0 mm);
type D072 cation exchange resin: shanghai Kaiping resin Co., Ltd., total exchange capacity mmol/g is not less than 4.8, (particle diameter 1.0 mm);
type D151 cation exchange resin: shanghai Kaiping resin Co., Ltd., total exchange capacity mmol/g is not less than 4.8, (particle diameter 1.0 mm);
carbon steel ball: 37075, city county Kangda Steel ball, Inc., Q235 x 1.0 mm;
titanium ball: bao Ji ezueli Metal materials, Inc., TA1 x 1.5 mm;
zinc ball: shijiazha, Zinc industries, Inc., 4N x 1.0 mm;
magnesium ball: shanghai Aladdin Biotechnology GmbH, M109146 x 1.0 mm;
aluminum ball: 37075, kang Da Steel ball, Inc., city, ZL101A × 1.0 mm;
spherical ferrite: 1.5mm of Vitta magnetoelectric technology, Inc., Dongguan, Y10T;
spherical active carbon: zhengzhou xing sen activated carbon Co., Ltd., XS-006 × 1.5 mm;
graphite particles: guiyang county Hua Yi graphite Limited, graphite particles 2 mm;
plating titanium glass balls: Peak Plastic hardware Limited, TA1 x 2 mm;
glass ball: glass beads for grinding 1.0mm, available from Hebei ancient New Material science and technology Co., Ltd;
other raw materials or reagents are commercially available unless otherwise specified.
Platinum deposited in the following examples was characterized by elements using an energy spectrometer (EDS SU 3500); the platinum content in the organic waste liquid before and after electrodeposition is characterized by adopting an inductively coupled plasma-mass spectrometry (Agilent 7500 CS).
In the following examples, the three-dimensional electrode bed layer is uniformly provided with a DSA electrode [ Ti/(Ru-Ir-Sn) O2]The anode is adopted, the 316L stainless steel electrode is adopted as the cathode, the size of the polar plate is unified, the length is 10cm, and the width is 4.8 cm.
In the following examples, the platinum recovery (η) was calculated according to the following formula:
η＝(C0*M0-Ce*me)/(C0*M0)
eta is the recovery rate of platinum; ceThe concentration of platinum in the electrolyzed organic waste liquid is ppm; m iseThe mass of the organic waste liquid after electrolysis is g; c0The concentration of platinum in the organic waste liquid is ppm before the electrolyte solution is added; m0Mass of organic waste liquid before adding electrolyte solution, g.
[ example 1 ]
10g of 732 type cation exchange resin, 10g of carbon steel balls and 10g of titanium balls are uniformly mixed and then filled into a three-dimensional electrode bed layer.
Stirring 200g of dimethyl sebacate rectifying still residual liquid, 2g of water, 1g of potassium hydroxide and 4g of methanol uniformly (the platinum content after mixing is 19.3ppm), pumping the mixed material into a three-dimensional electrode electrolytic cell at a feeding rate of 80L/h, reacting for 20min at the temperature of 60 ℃, and controlling the current density of the electrolytic cell to be 200A/m2And the electrolytic voltage is 4.2V. After the reaction was completed, the platinum ion content in the waste liquid was detected to be 0.3ppm, and the calculated platinum recovery rate was 98.45%.
Recovery and post-treatment of metal platinum: taking out the filling material in the three-dimensional electrode bed layer, and sieving by using a 14-mesh sieve (sieve pore size is 1.40mm) according to different particle sizes of the material to separate the inert conductive material deposited with the platinum layer; mixing inert conductive material and aqua regia (mass ratio is 1:2), and dissolving for 3 hours at 80 ℃; then adding ammonium chloride with the mass 2 times of that of the platinum in the filling material, stirring and filtering to obtain ammonium chloroplatinate precipitate; mixing ammonium chloroplatinate with hydrazine hydrate with twice molar weight, continuously stirring at 80 ℃, reducing to generate metal platinum, and filtering to obtain spongy solid, namely the metal platinum.
[ example 2 ]
4.3g D113 type cation exchange resin, 8.6g magnesium balls and 17.2g spherical ferrite are mixed uniformly and filled into a three-dimensional electrode bed layer.
Stirring 200g of dimethyl sebacate rectifying still residual liquid, 6g of water, 2g of sodium hydroxide and 8g of ethanol uniformly (the platinum content after mixing is 18.5ppm), pumping the mixed material into a three-dimensional electrode electrolytic cell at a feeding rate of 80L/h, reacting for 10min at 20 ℃,the current density of the electrolytic cell is 400A/m2And the electrolytic voltage is 5.0V.
High-quality pure platinum was obtained by the aftertreatment method in example 1. The content of platinum ions in the detection waste liquid is 0.1ppm, and the calculated platinum recovery rate is 99.5%.
[ example 3 ]
5.5g D001 type cation exchange resin, 2.73g of aluminum balls and 16.4g of spherical activated carbon are uniformly mixed and filled into a three-dimensional electrode bed layer.
Stirring 200g dimethyl sebacate rectifying still residual liquid, 12g water, 6g potassium methoxide and 20g amyl alcohol uniformly (the platinum content after mixing is 16.8ppm), pumping the mixed material into a three-dimensional electrode electrolytic cell at a feeding rate of 80L/h, reacting for 5min at 80 ℃, and ensuring the current density of the electrolytic cell to be 800A/m2And the electrolytic voltage is 4.8V.
High-quality pure platinum was obtained by the aftertreatment method in example 1. The content of platinum ions in the detection waste liquid is 153ppb, and the calculated platinum recovery rate is 99.1%.
[ example 4 ]
5.3g D072 type cation exchange resin, 3.53g of zinc balls and 10.6g of graphite particles are uniformly mixed and filled into a three-dimensional electrode bed layer.
Uniformly stirring 200g of dimethyl sebacate rectifying still residual liquid, 15g of water, 5g of sodium methoxide and 12g of propanol (the platinum content after mixing is 17.2ppm), pumping the mixed material into a three-dimensional electrode electrolytic cell at a feeding rate of 80L/h, reacting for 10min at 40 ℃, wherein the current density of the electrolytic cell is 600A/m2The electrolytic voltage was 3.0V.
High-quality pure platinum was obtained by the aftertreatment method in example 1. The content of platinum ions in the detection waste liquid is 110ppb, and the calculated platinum recovery rate is 99.36%.
[ example 5 ]
4.5g D151 type cation exchange resin, 2.8g carbon steel balls and 22g titanium-plated glass balls are uniformly mixed and filled into a three-dimensional electrode bed layer.
Stirring 200g of dimethyl sebacate rectifying still residual liquid, 6g of water, 3g of potassium sulfate and 16g of butanol uniformly (the platinum content after mixing is 17.8ppm), pumping the mixed material into a three-dimensional electrode electrolytic cell at a feeding rate of 80L/h, and feeding the mixed material into a three-dimensional electrode electrolytic cell at a feeding rate of 5gReacting at 0 deg.C for 15min, with current density of 300A/m2And the electrolytic voltage is 4.1V.
High-quality pure platinum was obtained by the aftertreatment method in example 1. The content of platinum ions in the detection waste liquid is 186ppb, and the calculated platinum recovery rate is 98.95%.
[ example 6 ]
4.3g D113 type ion exchange resin, 8.6g magnesium balls and 17.2g spherical ferrite are mixed uniformly and filled into a three-dimensional electrode bed layer.
Stirring 200g of anisic aldehyde rectifying still residual liquid, 6g of water, 2g of sodium hydroxide and 8g of ethanol uniformly (the platinum content is 34.3ppm after mixing), pumping the mixed material into a three-dimensional electrode electrolytic cell at a feeding rate of 80L/h, reacting for 10min at 20 ℃, wherein the current density of the electrolytic cell is 400A/m2And the electrolytic voltage is 4.2V. The inert conductive material of the deposited platinum layer was separated by centrifugation, and pure platinum of good quality was obtained by the post-treatment method in example 1. The content of platinum ions in the detection waste liquid is 125ppb, and the calculated platinum recovery rate is 99.63%.
[ example 7 ]
4.3g D113 type ion exchange resin, 8.6g magnesium balls and 17.2g spherical ferrite are mixed uniformly and filled into a three-dimensional electrode bed layer.
Stirring 200g of succinic acid rectifying still residual liquid, 6g of water and 2g of sodium hydroxide uniformly (the platinum content is 15.4ppm after mixing), pumping the mixed material into a three-dimensional electrode electrolytic cell at a feeding rate of 80L/h, reacting for 10min at 20 ℃, wherein the current density of the electrolytic cell is 500A/m2And the electrolytic voltage is 4.5V. The inert conductive material of the deposited platinum layer was separated by centrifugation, and pure platinum of good quality was obtained by the post-treatment method in example 1. The content of platinum ions in the detection waste liquid is 151ppb, and the calculated platinum recovery rate is 99.02%.
Comparative example 1
4.5g D151 type cation exchange resin and 22g titanium-plated glass balls are uniformly mixed and filled into a three-dimensional electrode bed layer.
200g of dimethyl sebacate rectifying still residual liquid, 6g of water, 3g of potassium sulfate and 16g of butanol are uniformly stirred (the platinum content after mixing is 17.8ppm), and the mixed material is pumped into a three-dimensional electrode at a feeding rate of 80L/h for electrolysisReacting in a cell at 50 ℃ for 15min, wherein the current density of the electrolytic cell is 300A/m2And the electrolytic voltage is 6.8V.
High-quality pure platinum was obtained by the aftertreatment method in example 1. The platinum ion content in the detection waste liquid is 13.685ppm, and the calculated platinum recovery rate is 23.05%.
Comparative example 2
Electrodeposition was carried out using the same three-dimensional electrode and feed rate as in comparative example 1, the reaction time was extended to 360min at 50 ℃, and other electrolysis conditions were the same as in comparative example 1. The platinum ion content in the detection waste liquid is 4.7ppm, and the calculated platinum recovery rate is 73.53%.
Comparative example 3
Non-conductive material glass spheres were used instead of the non-conductive material D151 type cation exchange resin in example 5, and other three-dimensional electrode construction materials were the same as in example 5.
Stirring 200g of dimethyl sebacate rectifying still residual liquid, 6g of water, 3g of potassium hydroxide and 16g of butanol uniformly (the platinum content after mixing is 17.8ppm), pumping the mixed material into a three-dimensional electrode electrolytic cell at a feeding rate of 80L/h, reacting for 15min at 50 ℃, wherein the current density of the electrolytic cell is 300A/m2。
High-quality pure platinum was obtained by the aftertreatment method in example 1. The content of platinum ions in the detection waste liquid is 6.53ppm, and the recovery rate of platinum is 63.27%.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and additions can be made without departing from the method of the present invention, and these modifications and additions should also be regarded as the protection scope of the present invention.
Claims (10)
1. A method for recovering and treating low-concentration platinum in organic waste liquid is characterized by comprising the following steps:
A. filling ion exchange resin, inert conductive materials and sacrificial anode metal balls into an electrochemical three-dimensional electrode bed layer to construct a three-dimensional electrode system;
B. and (3) carrying out electrodeposition recovery on low-concentration platinum in the organic waste liquid by using the three-dimensional electrode system.
2. The method according to claim 1, wherein the organic waste liquid is an industrial organic waste liquid containing 5-200ppm of platinum;
preferably, the organic waste liquid is selected from sebacate rectification still residue, succinic acid rectification still residue, anisic aldehyde rectification still residue, trimethylbenzoquinone rectification still residue and p-benzoquinone electrochemical reaction liquid containing an organic platinum compound in a production process.
3. The method for recovering and treating low-concentration platinum in organic waste liquid according to claim 1 or 2, wherein the three-dimensional electrode has an electrolytic potential of 3-5V and an electrolytic current density of 200-800A/m2Preferably 300-500A/m2；
Preferably, the electrolytic reaction temperature of the three-dimensional electrode is 20-80 ℃, and the reaction time is 5-20 min.
4. The method according to claim 3, wherein the ion exchange resin is a cation exchange resin, preferably at least one of 732, D001, D113, D072, D151, or D152 type cation exchange resins.
5. The method for recycling low-concentration platinum in organic waste liquid according to claim 4, wherein the sacrificial anode metal ball is made of one or more of iron, zinc, magnesium, aluminum, carbon steel, magnesium alloy and aluminum alloy.
6. The method for recycling low-concentration platinum in organic waste liquid according to claim 5, wherein the inert conductive material is one or more of titanium balls, ferrite, titanium-plated glass balls or plastic balls, graphite and activated carbon.
7. The method for recovering and treating low-concentration platinum in organic waste liquid according to any one of claims 1 to 6, wherein in the three-dimensional electrode, the weight ratio of the ion exchange resin to the inert conductive material is 1:1-5, preferably 1: 2-4; the weight ratio of the sacrificial anode metal balls to the inert conductive material is 1:1-8, preferably 1: 3-6.
8. The method for recovering and treating low-concentration platinum in organic waste liquid according to any one of claims 1 to 7, wherein the organic waste liquid is mixed with an electrolyte solution before entering the three-dimensional electrode; the electrolyte is one or more of potassium methoxide, sodium methoxide, triethylamine, potassium hydroxide, sodium hydroxide, potassium sulfate and sodium sulfate, and preferably one or two of potassium hydroxide and sodium hydroxide.
9. The method according to claim 8, wherein the amount of the electrolyte is 0.5-3% of the organic waste liquid.
10. The method according to claim 8, wherein the solvent in the electrolyte solution is pure water or a mixture of water and an alcohol solvent; preferably, the alcoholic solvent is one or more of methanol, ethanol, propanol, butanol, pentanol.
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| CN106350672A (en) * | 2016-08-31 | 2017-01-25 | 贵研资源（易门）有限公司 | Method for separating iridium from base metal and other platinum family metals |
| WO2018234637A1 (en) * | 2017-06-22 | 2018-12-27 | Aalto University Foundation Sr | A method of recovering pt or ag or pt and ag from sulfate based metal solutions |
| CN207828382U (en) * | 2018-02-11 | 2018-09-07 | 紫金铜业有限公司 | Platinum palladium removing means in a kind of silver electrolyte |
| CN110635185A (en) * | 2018-06-22 | 2019-12-31 | 中天储能科技有限公司 | Discharge method of waste lithium battery |
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