CN111057861B - Method for recovering precious metal from wire drawing lubricating fluid - Google Patents
Method for recovering precious metal from wire drawing lubricating fluid Download PDFInfo
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- CN111057861B CN111057861B CN201911193804.7A CN201911193804A CN111057861B CN 111057861 B CN111057861 B CN 111057861B CN 201911193804 A CN201911193804 A CN 201911193804A CN 111057861 B CN111057861 B CN 111057861B
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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
- C22B11/046—Recovery of noble metals from waste materials from manufactured products, e.g. from printed circuit boards, from photographic films, paper or baths
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention provides a method for recovering precious metals from a wiredrawing lubricating fluid, which comprises the following steps of a lubricating fluid decomposition step (S1): mixing the lubricating liquid with alkali liquor and heating to decompose the lubricating liquid to obtain a decomposition liquid containing precious metals; noble metal extraction step (S2): and carrying out suction filtration and washing on the decomposition liquid, and removing water-soluble impurities in the decomposition liquid to obtain the noble metal powder. According to the technical scheme of the invention, the purpose of recovering the precious metal particles from the lubricating liquid can be realized, the recovery rate is more than 90%, resources can be effectively utilized, and the waste of the resources is avoided. According to the technical scheme of the invention, the purity of the noble metal can be further improved through steps of purification of the noble metal and the like, so that the high-quality noble metal with the purity as high as 99.95% can be obtained.
Description
Technical Field
The invention relates to the technical field of precious metal recovery, in particular to the technical field of precious metal recovery from wire drawing lubricating fluid.
Background
In the field of production and living, noble metals are often used as active ingredients to be widely applied to the production of various catalysts due to certain special structural forms of the noble metals. Because the reserves of precious metal mineral resources are limited and the yield is not high, more than 85 percent of precious metals need to be recycled as secondary resources globally.
In the preparation of nitric acid catalyst by ammoxidation, a noble metal mesh which takes platinum as a main material is required to be used, and a noble metal wire material used for preparing the noble metal mesh is required to be prepared by processes such as smelting, rolling, wire drawing and the like; in the wire drawing process, lubricating liquid is needed to ensure the yield of wire machining, and noble metal powder peeled off in the wire drawing process is mixed into the lubricating liquid. At present, precious metals in the lubricating liquid are not recycled, so that resource waste is caused.
Disclosure of Invention
In order to solve at least the drawbacks of the prior art described in the above background section, the present invention provides a method for recovering precious metals from a drawing lubricant, comprising the steps of, a lubricant decomposition step S1: mixing the lubricating liquid with alkali liquor and heating to decompose the lubricating liquid to obtain a decomposition liquid containing precious metals; precious metal extraction step S2: and carrying out suction filtration and washing on the decomposition liquid, and removing water-soluble impurities in the decomposition liquid to obtain the noble metal powder.
According to an embodiment of the present invention, the noble metal extracting step S2 includes: carrying out suction filtration and washing on the decomposition liquid to obtain first filter residue and colorless and transparent first filtrate; adding a precipitator into the first filtrate, and performing suction filtration and washing to obtain second filter residue and second filtrate, wherein the pH value of the second filtrate is neutral; and mixing the first filter residue and the second filter residue to obtain the precious metal powder.
According to another embodiment of the present invention, the method further comprises a noble metal purification step S3: crushing the noble metal powder to obtain a noble metal crude product; dissolving the noble metal crude product to obtain a first noble metal solution; and reducing and removing impurities from the first noble metal solution to obtain noble metal reducing powder.
According to still another embodiment of the present invention, the pulverization treatment comprises mixing the noble metal powder with a base metal powder, and sequentially performing sintering, acid washing and water washing to obtain the crude noble metal.
According to one embodiment of the present invention, the noble metal powder and the base metal powder are mixed in a mass ratio of 1: 3-8 mixing; the sintering temperature is 550-850 ℃, and the sintering time is 2-6 hours.
According to another embodiment of the present invention, the method further comprises a precious metal refining step S4: dissolving the noble metal reducing powder to obtain a second noble metal solution; and removing impurities in the second noble metal solution by resin exchange to obtain a third noble metal solution, and reducing and drying to obtain a noble metal finished product.
According to another embodiment of the invention, the dissolution is performed by using aqua regia as a solvent and performing acid-expelling and salt-transferring after the dissolution.
According to one embodiment of the invention, the first noble metal solution is subjected to reduction impurity removal by using a reducing agent, wherein the reducing agent is selected from one or more of hydrazine hydrate, sodium borohydride, formic acid and ethylene glycol.
According to another embodiment of the present invention, the resin exchange is to exchange noble metal ions in the second noble metal solution with a strong acid cation exchange resin and to elute with a hydrochloric acid solution.
According to yet another embodiment of the invention, the lye is a 40-60% NaOH solution.
Through the above description of the scheme and the embodiments of the present invention, those skilled in the art can understand that the method for recovering precious metal from wiredrawing lubricating fluid of the present invention can realize the recovery of precious metal particles in the lubricating fluid through the decomposition step of the lubricating fluid and the extraction step of the precious metal, and the method is simple, and can effectively utilize resources and avoid the waste of resources. Furthermore, the method can effectively remove impurities through the steps of purifying the noble metal, finely purifying the noble metal and the like, can obviously improve the recovery rate of the noble metal, can obtain a high-quality and high-purity noble metal finished product, is favorable for further processing and utilization, and has wide application prospect.
Drawings
The above and other objects, features and advantages of exemplary embodiments of the present invention will become readily apparent from the following detailed description read in conjunction with the accompanying drawings. In the accompanying drawings, several embodiments of the present invention are illustrated by way of example and not by way of limitation, and like reference numerals designate like or corresponding parts throughout the several views, in which:
FIG. 1 is a flow diagram generally illustrating a method of recovering precious metals from a wiredrawing lubricating fluid in accordance with the present invention;
FIG. 2 is a flow chart illustrating a method including a purification step of a noble metal according to the present invention;
fig. 3 is a flow chart illustrating a method including a fine purification step of a noble metal according to the present invention.
Detailed Description
Aiming at the defects of the prior art, the invention provides a solution for recovering precious metals from wire drawing lubricating fluid. The lubricating liquid is decomposed, so that the grease components in the lubricating liquid are decomposed into water-soluble molecules, and subsequent suction filtration and cleaning are facilitated, so that the precious metals are extracted. Further, the noble metal can be gradually refined through the purification step and the fine purification step of the noble metal, specifically comprising the operations of fragmentation, dissolution, reduction, impurity removal and the like, so that the recovery rate and the purity of the noble metal are improved, and a high-quality noble metal product is obtained.
Embodiments will now be described with reference to the accompanying drawings. It will be appreciated that for simplicity and clarity of illustration, where considered appropriate, reference numerals may be repeated among the figures to indicate corresponding or analogous elements. In addition, this application sets forth numerous specific details in order to provide a thorough understanding of the embodiments described herein. However, it will be understood by those of ordinary skill in the art that the embodiments described herein may be practiced without these specific details. In other instances, well-known methods, procedures, and components have not been described in detail so as not to obscure the embodiments described herein. Moreover, this description is not to be taken as limiting the scope of the embodiments described herein.
FIG. 1 is a flow diagram generally illustrating a method of recovering precious metals from wiredrawing lubricating fluid in accordance with the present invention. As shown in fig. 1, the present invention provides a method for recovering precious metals from a wiredrawing lubricating fluid, comprising the steps of, a lubricating fluid decomposition step S1: mixing the lubricating liquid with alkali liquor and heating to decompose the lubricating liquid to obtain a decomposition liquid containing precious metals; precious metal extraction step S2: and carrying out suction filtration and washing on the decomposition liquid, and removing water-soluble impurities in the decomposition liquid to obtain the noble metal powder.
Because the main components of the lubricating liquid are sodium stearate and propylene glycol, the precious metal powder is suspended in the lubricating liquid and decomposed by adding alkali liquor, the sodium stearate in the lubricating liquid is decomposed, the molecules are reduced, and meanwhile, the precious metal powder is dissolved in water, so that the precious metal powder is settled, and the subsequent suction filtration and washing are facilitated. Wherein the washing adopts a water washing mode to remove the decomposed water-soluble impurities, so as to obtain the noble metal powder. The whole operation process has strong operability, small loss of noble metals and high recovery rate. In one embodiment, heating is applied during the decomposition of the lubricating fluid to facilitate the progress of the decomposition. In another embodiment, the lye may be a 40-60% NaOH solution. In yet another embodiment, the volume ratio of the lubricating liquid to the lye can be 1:1 to 2: 1.
In the precious metal extraction step S2, the decomposed solution is subjected to suction filtration to obtain a filtrate and a precious metal-containing filter residue, and the filter residue is washed, wherein one or more times of washing can be performed during washing to remove water-soluble impurities doped therein, so as to obtain precious metal powder. In one embodiment, the filter residue may be dried after washing to obtain a dried noble metal powder.
According to an embodiment of the present invention, in the precious metal extraction step S2, the decomposed solution may be first filtered and washed to obtain a first filter residue and a colorless and transparent first filtrate; the washing can be repeated for a plurality of times until the first filtrate is colorless and transparent, so as to reduce water-soluble impurities in the first filter residue as much as possible, thereby improving the purity of the noble metal in the first filter residue. In order to further increase the recovery of precious metal, further extraction of precious metal particles possibly present in the first filtrate may be performed. In one embodiment, the step of extracting precious metal particles that may be present in the first filtrate comprises: and adding a precipitator into the first filtrate, and performing suction filtration and washing on the first filtrate added with the precipitator to obtain second filter residue and second filtrate, wherein the second filtrate is washed until the pH value of the second filtrate is neutral. And mixing the first filter residue and the second filter residue to obtain the precious metal powder. It will be appreciated by those skilled in the art that the precipitation conditions may be adjusted according to the choice of the precipitating agent, for example, the pH of the first filtrate may be adjusted according to the appropriate pH of the precipitating agent, etc. For example, in another embodiment, the pH of the first filtrate can be adjusted to 1 or less prior to adding the precipitant. The precipitant may be polyaluminum chloride (PAC) used under strongly acidic conditions.
The method for recovering precious metals from wiredrawing lubricating fluid of the invention is described above with reference to fig. 1, and it can be known from the above description that according to the technical scheme of the invention, the purpose of recovering precious metals from wiredrawing lubricating fluid can be achieved, and the recovery rate of more than 90% can be achieved, thus fully utilizing wiredrawing lubricating fluid resources and avoiding the waste of precious metal resources. In order to further improve the purity of the noble metal, the present invention provides various embodiments to further optimize and perfect the method for recovering noble metal of the present invention, and further embodiments of the present invention are described in detail below with reference to fig. 2 and 3.
Fig. 2 is a flow chart illustrating a method including a purification step of a noble metal according to the present invention. As shown in fig. 2, according to one embodiment of the present invention, the method of recovering precious metals from a wiredrawing lubricating fluid may include a decomposition step S1 of the lubricating fluid, an extraction step S2 of precious metals, and a purification step S3 of precious metals. Here, the decomposition step S1 of the lubricating liquid and the extraction step S2 of the precious metal are the same as or similar to the embodiment of the step shown in fig. 1, and are not described herein again, and a specific embodiment of the purification step S3 of the precious metal will be described below.
The purpose of the noble metal purification step S3 is to purify the noble metal powder obtained in the noble metal extraction step S2 to further improve the purity and quality thereof. The noble metal purifying step S3 may include pulverizing the noble metal powder to obtain a crude noble metal product; dissolving the noble metal crude product to obtain a first noble metal solution; and reducing and removing impurities from the first noble metal solution to obtain noble metal reducing powder. Wherein the noble metal powder is subjected to a pulverization treatment, which can refine the noble metal powder and improve the activity of the metal powder.
In one embodiment, the pulverization process may include mixing noble metal powder with base metal powder, and sequentially performing sintering, acid washing, and water washing to obtain a crude noble metal product. The base metal may include one or more of zinc, tin, tungsten, iron, copper, nickel, and the like. In another embodiment, the noble metal powder and the base metal powder can be mixed according to the mass ratio of 1: 3-8, the sintering temperature of the mixture of the noble metal powder and the base metal powder can be 550-850 ℃, and the constant temperature holding time is 2-6 hours. After cooling to room temperature, acid washing may be performed using a hydrochloric acid solution to dissolve impurity metals in the mixture, and then a water washing step may be performed using pure water to wash to neutrality.
The crude noble metal may be dissolved using an acid as a solvent, for example, in one embodiment, aqua regia may be used as a solvent for dissolving the crude noble metal to achieve sufficient dissolution. After the dissolution with the acid, the acid-expelling and salt-transferring may be carried out to obtain the first noble metal solution. When the first noble metal solution is subjected to reduction and impurity removal, one or more of hydrazine hydrate, sodium borohydride, formic acid, ethylene glycol and the like can be used as a reducing agent. The preferred scheme is that hydrazine hydrate is used as a reducing agent to reduce the first noble metal solution, and the hydrazine hydrate has moderate reducing property and selectivity on noble metal ions, so that the noble metal can be selectively reduced, and impurity removal is facilitated. In one embodiment, the first noble metal solution may be reduced under alkaline conditions.
In order to further improve the purity and quality of the noble metal, the present invention provides another embodiment, further comprising a step S4 of refining and purifying the noble metal, which will be described in detail in conjunction with fig. 3. Fig. 3 is a flow chart illustrating a method including a fine purification step of a noble metal according to the present invention. As shown in fig. 3, the method may include a decomposition step S1 of the lubricating liquid, an extraction step S2 of the precious metal, a purification step S3 of the precious metal, and a fine purification step S4 of the precious metal. The decomposition step S1 of the lubricating fluid, the extraction step S2 of the precious metal, and the purification step S3 of the precious metal are the same as or similar to the embodiments of the steps shown in fig. 1 or fig. 2, and are not described herein again, and a specific embodiment of the fine purification step S4 of the precious metal will be described below.
The precious metal purification step S4 may include: dissolving the noble metal reducing powder to obtain a second noble metal solution; and removing impurities in the second noble metal solution by resin exchange to obtain a third noble metal solution, and reducing and drying to obtain a noble metal finished product. The dissolving method for dissolving the precious metal reducing powder and the dissolving method for dissolving the crude precious metal product described in fig. 2 can be the same or similar, and are not described in detail here.
According to an embodiment of the present invention, the resin exchange may be performed by exchanging noble metal ions in the second noble metal solution with a strong acid cation exchange resin and eluting with a hydrochloric acid solution. The strong acid cation exchange resin is an acidic gel type cation exchange resin with uniform size (monodispersion) based on styrene-divinylbenzene copolymer, and can be Na type. For example, a strong acid cation exchange resin can be converted to the Na form by treating it with a NaCl solution. And (3) contacting the strong acid cation exchange resin with the second noble metal solution for exchange, removing impurities, and eluting noble metal ions adsorbed by the strong acid cation exchange resin with a hydrochloric acid solution to obtain a third noble metal solution. In one embodiment, the pH of the hydrochloric acid solution as the elution solution may be 1.2 to 1.8.
And reducing and drying the third noble metal solution to obtain a noble metal finished product. The reduction may be performed using a reducing agent, which may be selected from one or more of hydrazine hydrate, sodium borohydride, formic acid, ethylene glycol, and the like. According to the technical scheme of the invention, the precious metal in the wire drawing lubricating liquid is recovered, the recovery rate of the precious metal can reach more than 90%, and the purity of the recovered precious metal finished product can reach 99.95%.
The following description will be given with reference to specific examples.
Example 1: taking 20L of wiredrawing lubricating fluid, mixing and heating by using 10L of 40% NaOH solution according to the ratio of 2:1 to decompose the grease solvent, and then carrying out suction filtration, cleaning and drying to obtain 241g of precious metal powder.
Example 2: taking 20L of wiredrawing lubricating fluid, mixing and heating by using 10L of 45% NaOH solution according to the ratio of 2:1 to decompose the grease solvent, and then carrying out suction filtration, cleaning and drying to obtain 243g of precious metal powder.
The noble metal powder is sampled and analyzed to obtain various metals with the mass percentages as follows: 56.52% of Fe, 10.22% of Ni, 13.85% of Pt, 6.93% of Pd, 2.32% of Rh, 5.02% of Cr and 5.14% of Cu, and the theoretical amounts of the three noble metals of Pt, Rh and Pd are 56.13 g.
Noble metal powder and zinc powder are mixed according to the mass ratio of 1: 4, keeping the temperature at 750 ℃ for 3 hours, taking out, cooling to room temperature, dissolving impurity metals by using an 18% HCl solution, cleaning to neutrality by using pure water to obtain a precious metal crude product, and mixing the components in percentage by using HCl: HNO3Dissolving the crude noble metal in aqua regia solution of 3:1, and using 80% of the first noble metal solution after acid expelling and salt conversionReducing the hydrazine hydrate solution to remove impurities to obtain the noble metal reducing powder.
And dissolving the noble metal reducing powder again by using aqua regia, repeatedly removing acid and converting salt, removing impurities from the obtained second noble metal solution through resin exchange, carrying out fine purification to obtain a third noble metal solution, reducing the third noble metal solution, and drying to obtain a noble metal finished product weighing 51.68 g. From the above data by the formula: the recovery rate of the noble metal (weight of the noble metal after final reduction/theoretical weight of the noble metal calculated from the analysis sampling result) was 100%, and the recovery rate of the noble metal in this example was calculated to be 92.07% and the purity was calculated to be 99.95%.
Example 3: 20L of wire drawing lubricating fluid is prepared by mixing and heating 60 percent NaOH solution 20L according to the proportion of 1:1 to decompose the grease solvent, and then carrying out suction filtration, cleaning and drying to obtain 252g of precious metal powder.
The noble metal powder is sampled and analyzed to obtain various metals with the mass percentages as follows: 57.55% of Fe, 11.22% of Ni, 14.35% of Pt, 7.23% of Pd, 3.32% of Rh, 4.16% of Cr and 2.17% of Cu, and the theoretical amounts of the three noble metals of platinum, rhodium and palladium are calculated to be 62.75 g.
Noble metal powder and zinc powder are mixed according to the mass ratio of 1: 6, uniformly mixing, keeping the temperature at 850 ℃ for 2 hours, taking out, cooling to room temperature, dissolving impurity metals by using an 18% HCl solution, cleaning to be neutral by using pure water to obtain a noble metal crude product, and adding HCl: HNO3Dissolving the crude noble metal in aqua regia solution with the ratio of 3:1, reducing the first noble metal solution after acid expelling and salt conversion by using 80% hydrazine hydrate solution to remove impurities, and obtaining the noble metal reducing powder.
And dissolving the noble metal reducing powder again by using aqua regia, repeatedly removing acid and converting salt, removing impurities from the obtained second noble metal solution through resin exchange, carrying out fine purification to obtain a third noble metal solution, reducing the third noble metal solution, and drying to obtain a noble metal finished product weighing 58.50 g. From the above data by the formula: the recovery rate of the noble metal (weight of the noble metal after final reduction/theoretical weight of the noble metal calculated from the analysis sampling result) was 100%, and the recovery rate of the noble metal in this example was calculated to be 93.22% and the purity was 99.95%.
Example 4: 20L of precious metal wire drawing lubricating fluid is prepared by mixing and heating 55 percent of NaOH solution 20L according to the proportion of 1:1 to decompose grease solvents in the precious metal wire drawing lubricating fluid, and then carrying out suction filtration and cleaning to obtain 246g of precious metal powder.
The noble metal powder is sampled and analyzed to obtain various metals with the mass percentages as follows: 56.45% of Fe, 11.27% of Ni, 13.85% of Pt, 7.56% of Pd, 3.86% of Rh, 4.38% of Cr and 2.63% of Cu, and the theoretical amounts of the three noble metals of platinum, rhodium and palladium are calculated to be 62.16 g.
Noble metal powder and tin powder are mixed according to the mass ratio of 1:3, keeping the temperature at 650 ℃ for 5 hours, taking out, cooling to room temperature, dissolving impurity metals by using an 18% HCl solution, cleaning to neutrality by using pure water to obtain a precious metal crude product, and mixing the components in percentage by using HCl: HNO3Dissolving the crude noble metal in aqua regia solution with the ratio of 3:1, reducing the first noble metal solution after acid expelling and salt conversion by using 80% hydrazine hydrate solution to remove impurities, and obtaining the noble metal reducing powder.
And dissolving the noble metal reducing powder again by using aqua regia, repeatedly removing acid and converting salt, removing impurities from the obtained second noble metal solution through resin exchange, carrying out fine purification to obtain a third noble metal solution, reducing the third noble metal solution, and drying to obtain a noble metal finished product weighing 57.95 g. From the above data by the formula: the recovery rate of the noble metal (weight of the noble metal after final reduction/theoretical weight of the noble metal calculated from the analysis sampling result) was 100%, and the recovery rate of the noble metal in this example was 93.23% and the purity was 99.95% as calculated.
Example 5: 20L of precious metal wire drawing lubricating fluid is mixed and heated by using 20L of 50% NaOH solution according to the proportion of 1:1 to decompose the grease solvent, and then 267g of precious metal powder is obtained through suction filtration and cleaning.
The noble metal powder is sampled and analyzed to obtain various metals with the mass percentages as follows: 53.25 percent of Fe, 13.22 percent of Ni, 15.37 percent of Pt, 8.23 percent of Pd, 2.35 percent of Rh, 4.56 percent of Cr and 3.02 percent of Cu, and the theoretical amount of the three noble metals of platinum, rhodium and palladium is 69.29g according to calculation.
Mixing noble metalPowder and zinc powder are mixed according to the proportion of 1: 5, keeping the temperature at 850 ℃ for 2 hours, taking out, cooling to room temperature, dissolving impurity metals by using an 18% HCl solution, cleaning to neutrality by using pure water to obtain a precious metal crude product, and mixing the components in percentage by using HCl: HNO3Dissolving the crude noble metal product in aqua regia solution with the ratio of 3:1, reducing the first noble metal solution after acid expelling and salt conversion by using 80% hydrazine hydrate solution to remove impurities, and obtaining noble metal reducing powder.
And dissolving the noble metal reducing powder again by using aqua regia, repeatedly removing acid and converting salt, removing impurities from the obtained second noble metal solution through resin exchange, carrying out fine purification to obtain a third noble metal solution, reducing the third noble metal solution, and drying to obtain a noble metal finished product weighing 65.49 g. From the above data by the formula: the recovery rate of the noble metal (weight of the noble metal after final reduction/theoretical weight of the noble metal calculated from the analysis sampling result) was 100%, and the recovery rate of the noble metal in this example was 94.52% and the purity was 99.95% as calculated.
Example 6: 20L of wire drawing lubricating fluid is mixed and heated by using 10L of 60 percent NaOH solution according to the proportion of 2:1 to decompose the grease solvent, and then 265g of precious metal powder is obtained through suction filtration and cleaning.
The noble metal powder is sampled and analyzed to obtain various metals with the mass percentages as follows: 55.75 percent of Fe, 11.82 percent of Ni, 15.38 percent of Pt, 6.28 percent of Pd, 3.65 percent of Rh, 4.56 percent of Cr and 2.56 percent of Cu, and the theoretical amount of the three noble metals of platinum, rhodium and palladium is 67.07 g.
Noble metal powder and tin powder are mixed according to the mass ratio of 1: 8, keeping the temperature at 550 ℃ for 6 hours, taking out, cooling to room temperature, dissolving impurity metals by using an 18% HCl solution, cleaning to neutrality by using pure water to obtain a precious metal crude product, and mixing the components in percentage by using HCl: HNO3Dissolving the crude noble metal in aqua regia solution with the ratio of 3:1, reducing the first noble metal solution after acid expelling and salt conversion by using 80% hydrazine hydrate solution to remove impurities, and obtaining the noble metal reducing powder.
And dissolving the noble metal reducing powder again by using aqua regia, repeatedly removing acid and converting salt, removing impurities from the obtained second noble metal solution through resin exchange, carrying out fine purification to obtain a third noble metal solution, reducing the third noble metal solution, and drying to obtain a noble metal finished product weighing 61.22 g. From the above data by the formula: the recovery rate of the noble metal (weight of the noble metal after final reduction/theoretical weight of the noble metal calculated from the analysis sampling result) was 100%, and the recovery rate of the noble metal in this example was 91.28% and the purity was 99.95% as calculated.
Through the above description, those skilled in the art can understand that in the above-mentioned scheme and different embodiments of the present invention, the steps of decomposing the lubricating fluid and extracting the precious metal are performed first, so that the precious metal particles in the lubricating fluid can be recovered, the operability is strong, the resources can be effectively utilized, and the resource waste caused by the fact that the precious metal in the wire drawing lubricating fluid in the prior art cannot be recovered is avoided. Furthermore, the invention can effectively remove impurities such as water-soluble and base metals through the purification step of the noble metal or the fine purification step of the noble metal, such as the selection of processes such as fragmentation treatment, twice dissolution, selective reduction and the like, and can obtain high-quality noble metal with the recovery rate of more than 90 percent and the purity of 99.95 percent.
While various embodiments of the present invention have been shown and described herein, it will be obvious to those skilled in the art that such embodiments are provided by way of example only. Numerous modifications, changes, and substitutions will occur to those skilled in the art without departing from the spirit and scope of the present invention. It should be understood that various alternatives to the embodiments of the invention described herein may be employed in practicing the invention. It is intended that the following claims define the scope of the invention and that the module compositions, equivalents, or alternatives falling within the scope of these claims be covered thereby.
Claims (8)
1. A method for recovering precious metals from a wiredrawing lubricating fluid comprises the following steps,
decomposition step (S1) of lubricating liquid: mixing the lubricating liquid with alkali liquor and heating to decompose the lubricating liquid to obtain a decomposition liquid containing precious metals, wherein the main components of the lubricating liquid are sodium stearate and propylene glycol;
noble metal extraction step (S2): carrying out suction filtration and washing on the decomposition liquid, and removing water-soluble impurities in the decomposition liquid to obtain noble metal powder; and
noble metal purification step (S3):
crushing the noble metal powder to obtain a noble metal crude product;
dissolving the noble metal crude product to obtain a first noble metal solution;
reducing and removing impurities from the first noble metal solution to obtain noble metal reducing powder,
wherein the pulverization treatment comprises mixing the precious metal powder and base metal powder, and sequentially carrying out sintering, acid washing and water washing to obtain the precious metal crude product.
2. The method of claim 1, wherein the noble metal extracting step (S2) comprises:
carrying out suction filtration and washing on the decomposition liquid to obtain first filter residue and colorless and transparent first filtrate;
adding a precipitator into the first filtrate, and performing suction filtration and washing to obtain second filter residue and second filtrate, wherein the pH value of the second filtrate is neutral;
and mixing the first filter residue and the second filter residue to obtain the precious metal powder.
3. The method according to claim 1, wherein the noble metal powder and the base metal powder are mixed in a mass ratio of 1: 3-8 mixing;
the sintering temperature is 550-850 ℃, and the sintering time is 2-6 hours.
4. The method of claim 2, further comprising a precious metal refining step (S4):
dissolving the noble metal reducing powder to obtain a second noble metal solution;
and removing impurities in the second noble metal solution by resin exchange to obtain a third noble metal solution, and reducing and drying to obtain a noble metal finished product.
5. The method according to claim 2 or 4, wherein the dissolution is carried out using aqua regia as a solvent, and acid-expelling and salt-converting are carried out after the dissolution.
6. The method according to claim 2, wherein the first noble metal solution is subjected to reduction impurity removal by using a reducing agent, and the reducing agent is selected from one or more of hydrazine hydrate, sodium borohydride, formic acid and ethylene glycol.
7. The method of claim 4, wherein said resin exchange is an exchange of noble metal ions in said second noble metal solution with a strong acid cation exchange resin and elution with a hydrochloric acid solution.
8. The method of claim 1, wherein the lye is a 40-60% NaOH solution.
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| JP4366804B2 (en) * | 2000-01-13 | 2009-11-18 | 住友金属鉱山株式会社 | Method for recovering precious metal from precious metal fine particle dispersion |
| CN1230386C (en) * | 2001-06-15 | 2005-12-07 | 住友金属矿山株式会社 | Process for recovering noble metal from noble metal microparticle dispersive liquid |
| US8715388B2 (en) * | 2011-04-29 | 2014-05-06 | Momentive Performance Materials | Process of precious metal recovery and color removal from an organosilicon product-containing liquid reaction medium |
| CN102560140B (en) * | 2012-02-24 | 2013-12-11 | 西安凯立化工有限公司 | Method for recycling palladium from organic waste liquid |
| CN104232286B (en) * | 2013-06-13 | 2016-05-11 | 中国石油化工股份有限公司 | A kind of separation method of aluminium wire waste oil |
| CN103773967B (en) * | 2014-02-12 | 2015-08-19 | 湘潭大学 | The method of recover silver, copper and zinc from steel works sintering dust |
| US9580770B2 (en) * | 2014-10-22 | 2017-02-28 | Chevron U.S.A. Inc. | Process for preparing a spent catalyst for precious metals recovery |
| CN107469456A (en) * | 2016-06-07 | 2017-12-15 | 沈阳芯源微电子设备有限公司 | A kind of metal recovery system for tearing golden degumming process |
| CN106756036A (en) * | 2016-12-07 | 2017-05-31 | 广东先导稀材股份有限公司 | The method that noble metal is reclaimed from waste plastics |
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2019
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Address after: 030600 North Street of Machinery Industrial Park, Huitong Industrial Park, Jinzhong Development Zone, Shanxi demonstration zone, Jinzhong City, Shanxi Province Patentee after: CNOOC (Shanxi) precious metal Co.,Ltd. Address before: 030000 6th floor, block a, Chuangye building, Kaifa lane, high tech Development Zone, Taiyuan, Shanxi Patentee before: CNOOC TAIYUAN PRECIOUS METALS Co.,Ltd. |