CN112295549A - Adsorbent for selectively separating gold and preparation method and application thereof - Google Patents
Adsorbent for selectively separating gold and preparation method and application thereof Download PDFInfo
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/268—Polymers created by use of a template, e.g. molecularly imprinted polymers
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28078—Pore diameter
- B01J20/28083—Pore diameter being in the range 2-50 nm, i.e. mesopores
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- 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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
An adsorbent for selectively separating gold, a preparation method and an application thereof, wherein the adsorbent is prepared by the following method: adopting a mesoporous material as a solid phase matrix, grafting polyethyleneimine onto the matrix material through a silane coupling agent, and soaking the prepared grafted material in HAuCl4Adsorbing template ions in the solution, adding ethylene glycol diglycidyl ether for crosslinking, and removing the template ions of AuCl by adopting thiourea4 ‑To obtain AuCl capable of being selectively adsorbed4 ‑The adsorbent of (1). The method is easy to operate. The obtained adsorbentThe gold-adsorbing material has the characteristics of large specific surface area, strong adsorption selectivity, stable performance and the like, can be used for selectively separating gold from a gold-containing hydrochloric acid solution, and effectively solves the problems of small adsorption capacity, weak selectivity, low direct recovery rate and the like of the adsorption material for separating gold from the current hydrochloric acid solution.
Description
Technical Field
The invention relates to a material for recovering valuable metal gold from secondary resources, in particular to an adsorbing material capable of selectively separating gold and a preparation method and application thereof.
Background
The gold has good electrical conductivity, thermal conductivity, ductility and biocompatibility, and stable chemical properties, and is widely applied to the fields of jewelry, electronics, aerospace and the like.
With the rapid development of science and technology, gold is increasingly demanded as a vitamin in modern industries.
Gold leaching by cyanidation is a commonly used gold extraction method, but is gradually replaced by non-cyanidation leaching because of strong toxicity of cyanide. Some gold-containing concentrates and anode mud are extracted by chlorination process.
Adsorption is one of the most efficient methods for recovering gold from chlorinated acidic solutions. Gold extraction by using an adsorption method, and the key is to select a proper adsorption material.
The currently reported adsorption materials for gold extraction mainly comprise a biomass adsorbent, activated carbon and ion exchange resin. These adsorbents have problems of low selectivity, low adsorption capacity, and the like in gold extraction.
As is known, mesoporous materials have the characteristics of large specific surface area, uniform pore diameter, strong stability, surface groups capable of being functionalized and the like, but the single mesoporous material does not have adsorption selectivity and cannot be used for extracting gold.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of the existing adsorbing material and providing an adsorbing agent for selectively separating gold, which has strong gold selectivity, large adsorption capacity and stable performance and is particularly suitable for extracting gold, and a preparation method thereof.
The invention adopts the technical scheme that the adsorbent for selectively separating gold is prepared by the following method:
(1) activation of the mesoporous material: placing the mesoporous material in a flask, adding an acidic solution, heating, refluxing for activation, filtering, washing and drying for later use;
(2) grafting polyethyleneimine on a mesoporous material: adding the activated mesoporous material and a silane coupling agent into a solvent for coupling reaction, adding a reaction product into a polyethyleneimine water solution for grafting reaction, washing with distilled water, and drying to obtain a polyethyleneimine grafted mesoporous material;
(3) imprinting of the grafting material: adding the prepared polyethyleneimine grafted mesoporous material into a solution containing a template agent for adsorption reaction, adding a crosslinking agent for crosslinking reaction, washing the reaction product by thiourea and distilled water in sequence, and drying to obtain the polyethyleneimine grafted mesoporous material.
Further, in the step (1), the mesoporous material is MCM-41 mesoporous molecular sieve or SBA-15 mesoporous molecular sieve.
Further, in the step (1), the acidic solution is an inorganic acid solution or an organic acid solution.
Further, the inorganic acid solution is preferably a hydrochloric acid solution.
Further, the concentration of the hydrochloric acid solution is 2.5-3.5mol/L (preferably 3 mol/L); the liquid-solid ratio of the hydrochloric acid solution to the mesoporous material is 5-10, the temperature of the reflux activation reaction is 105-.
Further, in the step (1), the washing is carried out to be neutral, the drying temperature is 100-150 ℃, the drying time is 1-2 h, and the drying mode is vacuum drying.
Further, in the step (2), the silane coupling agent is one of 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane and 3-chloropropyltrimethoxysilane.
Further, in the step (2), the solvent is one of xylene and absolute ethyl alcohol.
Further, in the step (2), the solid-to-liquid ratio of the activated mesoporous material to the silane coupling agent to the solvent is S: V: V =1: 2-10: 10-20; the coupling reaction time is 4-10 h (preferably 5-8 h); the mass concentration of the polyethyleneimine water solution is 25-35% (preferably 28-32%, more preferably 30%) and the grafting reaction time is 4-10 h, and the reaction temperature is 80-90 ℃.
Further, in the step (3), the template is HAuCl4，HAuCl4The concentration of the solution is 0.6-1.5g/L (preferably 0.8-1.2g/L, more preferably 1.0 g/L), HAuCl4The pH value of the solution is 0-3.
Further, in the step (3), the temperature of the adsorption reaction is constant at 25 ℃, the adsorption is assisted by ultrasonic treatment, and the time of the adsorption reaction is 1-3 h.
Further, in the step (3), the crosslinking agent added after adsorption is ethylene glycol diglycidyl ether, and crosslinking is assisted by ultrasonic treatment, wherein the crosslinking reaction time is 1-3 h.
Further, the crosslinking reaction product in the step (3) is leached by thiourea or thiosulfate.
The adsorbent prepared by the invention has strong selective adsorption on gold, large adsorption capacity and stable performance. The method is applied to the recovery of gold from secondary gold-containing resources, and the direct recovery rate is high.
The invention relates to a method for separating gold from a gold-containing chlorinated acidic solution by using the adsorbent for selectively separating gold, which comprises the following steps:
step 1: placing a gold-containing chlorinated acidic solution into a container, adding the material prepared by the invention, oscillating, and selectively adsorbing gold;
step 2: and after adsorption saturation, filtering, washing with pure water, adding thiourea into the imprinted mesoporous material loaded with gold for desorption and elution to obtain gold enrichment solution.
Further, in the step 1, in the gold-containing chlorinated acidic solution, the gold content is 1-10 g/L, the platinum content is 1-5 g/L, the palladium content is 1-5 g/L, the copper content is 1-10 g/L, and the pH value of the solution is 0-3.
Further, in the steps 1 and 2, the temperature of adsorption and desorption is 20-40 ℃.
The gold-loaded imprinted mesoporous material can be recycled for more than 10 times after being desorbed by thiourea, washed by distilled water and dried again, and the performance is still stable.
Practice shows that the adsorbent prepared by the invention has strong selective adsorption on gold, large adsorption capacity and stable performance.
Researches show that the adsorbent prepared by taking the mesoporous material as the solid phase matrix and adopting the ion imprinting technology has the advantages of specific identification and adsorption of target ions. The mesoporous material is modified by adopting an ion imprinting technology, so that the mesoporous material has the advantages of both the mesoporous material and the chlorinated acidic solution, gold with low concentration can be selectively separated and recovered from the chlorinated acidic solution, the adsorption capacity is large, and the performance is stable; the adsorption rate can reach 94% or more.
The invention has the following beneficial effects: 1. the adsorbent prepared by the invention combines the advantages of large specific surface area, uniform aperture, strong stability, large adsorption capacity and the like of the mesoporous material and the advantage of strong selectivity of the ion imprinting technology; 2. the adsorbent prepared by the invention can realize selective recovery of low-concentration gold from a chlorinated acidic solution, and has strong anti-interference capability, which is not possessed by the existing adsorption material; 3. the adsorbent prepared by the invention can still maintain good stability performance after being repeatedly used for more than 10 times, has no obvious reduction on the performance of selectively adsorbing gold in a gold-containing low-concentration chlorinated acidic solution, and greatly improves the application value of the adsorbent; 4. according to the preferable scheme of the invention, ultrasonic treatment is adopted to assist adsorption and crosslinking in the imprinting process of the mesoporous material, so that the adsorption and crosslinking time can be greatly reduced, and imprinting cavities are more uniformly distributed on the surface of the material.
Detailed Description
The following examples illustrate specific embodiments of the present invention.
The following examples are intended to further illustrate specific embodiments of the present invention and are not intended to limit the scope of the claims herein.
The raw material MCM-41 mesoporous material (i.e., MCM-41 mesoporous molecular sieve), the SBA-15 mesoporous material (i.e., SBA-15 mesoporous molecular sieve) and other reagents used in the examples were all purchased from conventional commercial sources.
Preparation of the adsorbent of the invention example 1
(1) Mixing the MCM-41 mesoporous material with hydrochloric acid according to the proportion of 1:10 (the concentration of the hydrochloric acid is 3mol/L, the activation temperature is 110 ℃, and the solid-liquid ratio is 1: 10), refluxing for 24h, washing and drying;
(2) reacting the mesoporous material with a mixed solution of 3-chloropropyltrimethoxysilane and absolute ethyl alcohol (the solid-to-liquid ratio of the three is S: V: V =1: 3: 10) at 80 ℃ for 4 hours to obtain a reaction solution; adding the obtained reaction solution into a polyethyleneimine water solution with the mass concentration of 30% according to the volume ratio of 1:1, reacting for 4 hours at the temperature of 90 ℃, washing with distilled water, and drying to obtain a polyethyleneimine grafted mesoporous material;
(3) the prepared polyethyleneimine grafted mesoporous material and a template agent HAuCl4The solution was mixed at a ratio of 1:500 (1: 500 is the solid-to-liquid ratio (g/ml), HAuCl4Concentration of 1 g/L), adopting ultrasonic treatment to assist adsorption for 1h, filtering, mixing with ethylene glycol diglycidyl ether in a volume ratio of 1:1, and carrying out crosslinking reaction for 1 h; and removing template ions from the reaction product by adopting 1g/L thiourea solution, washing with distilled water, and drying to obtain the adsorbent for selectively separating gold.
Application example 1 of the adsorbent for selectively separating gold according to the present invention
Step 1: weighing 50g of adsorbent, mixing with 500 ml of gold-containing chlorinated acid solution, and performing vibration adsorption for 1h in a conical flask at the constant temperature of 30 ℃; filtering and washing to obtain the gold-loaded adsorbent;
step 2: and (2) desorbing the gold-loaded adsorbent obtained in the step (1) by adopting 1g/L thiourea solution to obtain a high-concentration gold-containing desorption solution, wherein the gold concentration in the solution is 143.6 g/L, the gold adsorption rate can reach 97.3 percent, the gold adsorption rate can still reach more than 94 percent after 10 times of circulation, and better adsorption selectivity is kept.
The imprinted mesoporous material product of the embodiment can still maintain higher adsorption capacity and adsorption selectivity after 10 cycles.
The contents of the main elements in the gold-containing chlorinated acidic solution before and after adsorption using the adsorbent product of this example are shown in tables 1-1 and 1-2.
Table 1-1 gold-containing chlorinated acidic solutions before and after the 1 st adsorption using the adsorbent product of example 1
Content of major elements (unit: g/L)
| Element(s) | Au | Cu | Pt | Pd |
| Before adsorption | 5.107 | 7.576 | 1.592 | 0.938 |
| After adsorption | 0.137 | 7.508 | 1.583 | 0.937 |
Tables 1-2 gold-containing chlorinated acidic solutions before and after the 10 th adsorption using the adsorbent product of example 1
Content of major elements (unit: g/L)
| Element(s) | Au | Cu | Pt | Pd |
| Before adsorption | 5.173 | 7.428 | 1.507 | 0.914 |
| After adsorption | 0.279 | 7.411 | 1.493 | 0.911 |
Preparation of adsorbent of the invention example 2
(1) Mixing the MCM-41 mesoporous material with hydrochloric acid according to the proportion of 1:10 (the concentration of the hydrochloric acid is 3mol/L, the activation temperature is 110 ℃, and the solid-liquid ratio is 1: 10), refluxing for 24 hours, washing and drying;
(2) reacting the MCM-41 mesoporous material activated in the step (1) with a mixed solution of 3-aminopropyltrimethoxysilane and xylene (the volume ratio is 1:3: 10) at 80 ℃ for 4 hours to obtain a reaction solution; adding the obtained reaction solution into 30% PEI aqueous solution according to the volume ratio of 1:1, reacting for 6 hours at the temperature of 90 ℃, washing and drying to obtain the polyethyleneimine grafted mesoporous material;
(3) mixing the polyethyleneimine grafted mesoporous material with a HAuCl4 solution in a ratio of 1:500 (1: 500 is the solid-to-liquid ratio (g/ml), HAuCl4Concentration of 1 g/L), adopting ultrasonic treatment to assist adsorption for 1h, filtering, mixing with ethylene glycol diglycidyl ether according to a volume ratio of 1:1, mixing and carrying out crosslinking reaction for 1 h; and washing the reaction product by adopting 1g/L thiourea solution to remove template ions, washing by using distilled water, and drying to obtain the adsorbent for selectively adsorbing gold.
Application example 2 of the adsorbent for selectively separating gold according to the present invention
Step 1: weighing 50g of imprinted mesoporous material, mixing with 500 ml of gold-containing chlorinated acid solution, performing vibration adsorption in a conical flask for 1h at the temperature of 30 ℃, filtering, and washing with distilled water to obtain gold-loaded imprinted mesoporous material;
step 2: desorbing the gold-loaded imprinted mesoporous material in the step 1 by adopting 1g/L thiourea solution to obtain a high-concentration gold-containing desorption solution, wherein the gold concentration in the solution is 108.4g/L, the highest gold adsorption rate can reach 98.5%, the gold adsorption rate is still more than 94% after 10 times of circulation, and better adsorption selectivity is maintained.
The adsorbent product of the embodiment can still maintain higher adsorption capacity and adsorption selectivity after 10 cycles.
The contents of the main elements in the gold-containing chlorinated acidic solution before and after adsorption using the adsorbent of this example are shown in tables 2-1 and 2-2.
Table 2-1 use of the adsorbent product of example 2 before and after the 1 st adsorption, in a gold-containing chlorinated acidic solution
Content of major elements (unit: g/L)
| Element(s) | Au | Cu | Pt | Pd |
| Before adsorption | 3.532 | 4.433 | 2.048 | 1.461 |
| After adsorption | 0.053 | 4.417 | 2.029 | 1.453 |
Table 2-2 use of the adsorbent product of example 2 before and after the 10 th adsorption in a gold-containing chlorinated acidic solution
Content of major elements (unit: g/L)
| Element(s) | Au | Cu | Pt | Pd |
| Before adsorption | 3.597 | 4.336 | 2.053 | 1.348 |
| After adsorption | 0.212 | 4.314 | 2.018 | 1.317 |
Preparation of adsorbent of the invention example 3
(1) Mixing the SBA-15 mesoporous material with hydrochloric acid in a ratio of 1:10 (the concentration of the hydrochloric acid is 3mol/L, the activation temperature is 110 ℃, and the solid-to-liquid ratio is 1: 10), refluxing for 24 hours, washing and drying;
(2) reacting the MCM-41 mesoporous material activated in the step (1) with a mixed solution of 3-aminopropyltriethoxysilane and absolute ethyl alcohol (volume ratio is 1:3: 10) at 80 ℃ for 4 hours to obtain a reaction solution; adding the obtained reaction solution into 30% PEI aqueous solution according to the volume ratio of 1:1, reacting for 6 hours at the temperature of 90 ℃, washing and drying to obtain the polyethyleneimine grafted mesoporous material;
(3) grafting polyethyleneimine onto mesoporous material and HAuCl4The solution is prepared by mixing the following components in percentage by weight: 500 (1: 500 is the solid-to-liquid ratio (g/ml), HAuCl4Concentration of 1 g/L), adopting ultrasonic treatment to assist adsorption for 1h, filtering, mixing with ethylene glycol diglycidyl ether according to a volume ratio of 1:1, mixing and carrying out crosslinking reaction for 1 h; and washing the reaction product by adopting 1g/L thiourea solution to remove template ions, washing by using distilled water, and drying to obtain the adsorbent for selectively adsorbing gold.
Application example 3 of the adsorbent for selectively separating gold according to the present invention.
Step 1: weighing 50g of imprinted mesoporous material, mixing with 500 ml of gold-containing chlorinated acid solution, performing vibration adsorption in a conical flask for 1h at the temperature of 30 ℃, filtering, and washing with distilled water to obtain gold-loaded imprinted mesoporous material;
step 2: desorbing the gold-loaded imprinted mesoporous material in the step 1 by adopting 1g/L thiourea solution to obtain a high-concentration gold-containing desorption solution, wherein the gold concentration in the solution is 121.8g/L, the highest gold adsorption rate can reach 94.8%, the gold adsorption rate is still more than 94% after 10 times of circulation, and better adsorption selectivity is maintained.
The adsorbent product of the embodiment can still maintain higher adsorption capacity and adsorption selectivity after 10 cycles.
The contents of the main elements in the gold-containing chlorinated acidic solution before and after adsorption using the adsorbent of this example are shown in tables 3-1 and 3-2.
Table 3-1 using the imprinted mesoporous material product of example 3 before and after the 1 st adsorption, in a gold-containing chlorinated acidic solution
Content of major elements (unit: g/L)
| Element(s) | Au | Cu | Pt | Pd |
| Before adsorption | 2.048 | 3.143 | 2.088 | 1.514 |
| After adsorption | 0.106 | 3.138 | 2.073 | 1.511 |
Table 3-2 gold-containing chlorinated acidic solution before and after the 10 th adsorption using the product of the imprinted mesoporous material of example 3
Content of major elements (unit: g/L)
| Element(s) | Au | Cu | Pt | Pd |
| Before adsorption | 2.103 | 3.126 | 2.033 | 1.513 |
| After adsorption | 0.122 | 3.119 | 2.031 | 1.513 |
Claims (15)
1. An adsorbent for selectively separating gold is characterized by being prepared by the following method:
(1) activation of the mesoporous material: placing the mesoporous material in a flask, adding the mesoporous material into an acidic solution, refluxing, filtering, washing and drying to obtain an activated mesoporous material for later use;
(2) grafting polyethyleneimine on a mesoporous material: adding the activated mesoporous material and a silane coupling agent into a solvent for coupling reaction, adding a reaction product into a polyethyleneimine water solution for grafting reaction, washing with distilled water, and drying to obtain a polyethyleneimine grafted mesoporous material;
(3) imprinting of the grafting material: adding the prepared polyethyleneimine grafted mesoporous material into a solution containing a template agent for adsorption reaction, adding a crosslinking agent for crosslinking reaction, washing the reaction product by thiourea and distilled water in sequence, and drying to obtain the polyethyleneimine grafted mesoporous material.
2. The adsorbent for selectively separating gold according to claim 1, characterized in that: the mesoporous material is MCM-41 mesoporous molecular sieve or SBA-15 mesoporous molecular sieve.
3. The adsorbent for selectively separating gold according to claim 1 or 2, characterized in that: in the step (1), the acid solution is an inorganic acid solution or an organic acid solution, preferably a hydrochloric acid solution; the concentration of the hydrochloric acid solution is 2.5-3.5mol/L, the liquid-solid ratio of the hydrochloric acid solution to the mesoporous material is 5-10, the activation reaction temperature is 105-.
4. The adsorbent for selectively separating gold according to any one of claims 1 to 3, further comprising: in the step (1), the washing is carried out to be neutral, the drying temperature is 100-150 ℃, the drying time is 1-2 h, and the drying mode is vacuum drying.
5. The adsorbent for selectively separating gold according to any one of claims 1 to 4, wherein: in the preparation method, in the step (2), the silane coupling agent is one of 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane and 3-chloropropyltrimethoxysilane.
6. The adsorbent for selectively separating gold according to any one of claims 1 to 5, wherein: in the step (2), the solvent is one of xylene and absolute ethyl alcohol.
7. The adsorbent for selectively separating gold according to any one of claims 1 to 6, wherein: in the step (2), the solid-to-liquid ratio S: V: V =1: 2-10: 10-20 of the activated mesoporous material to the silane coupling agent and the solvent, and the coupling reaction time is 4-10 h; the mass concentration of the polyethyleneimine water solution is 25-35%, the grafting reaction time is 4-10 h, and the reaction temperature is 80-90 ℃.
8. The adsorbent for selectively separating gold according to any one of claims 1 to 7, wherein: in the step (3), the template is HAuCl4HAuCl as template agent4The concentration of the solution is 0.6-1.5g/L, HAuCl4The pH value of the solution is 0-3.
9. The adsorbent for selectively separating gold according to any one of claims 1 to 8, wherein: in the step (3), the temperature of the adsorption reaction is 20-30 ℃, the adsorption is assisted by ultrasonic treatment, and the time of the adsorption reaction is 1-3 h.
10. The adsorbent for selectively separating gold according to any one of claims 1 to 9, wherein: in the step (3), the crosslinking agent added after adsorption is ethylene glycol diglycidyl ether, and crosslinking is assisted by ultrasonic treatment, wherein the crosslinking reaction time is 1-3 h.
11. The adsorbent for selectively separating gold according to any one of claims 1 to 10, wherein: and (3) leaching the crosslinking reaction product in the step (3) by using thiourea or thiosulfate.
12. Use of an adsorbent according to claims 1-11 for selective separation of gold for adsorptive separation recovery of gold from gold-containing hydrochloric acid solutions.
13. The use of the adsorbent for selectively separating gold according to claim 12 for adsorptive separation and recovery of gold from gold-containing hydrochloric acid solution, characterized by comprising the following specific operation steps:
step 1: placing a gold-containing chlorinated acidic solution into a container, adding the preparation material, oscillating, and selectively adsorbing gold;
step 2: and after adsorption saturation, filtering, washing with pure water, adding thiourea into the imprinted mesoporous material loaded with gold for desorption and elution to obtain gold enrichment solution.
14. Use of the adsorbent for selective separation of gold according to claim 13 for adsorptive separation recovery of gold from gold-containing hydrochloric acid solution, characterized in that: in the step 1, in the gold-containing chlorinated acidic solution, the gold content is 1-10 g/L, the platinum content is 1-5 g/L, the palladium content is 1-5 g/L, the copper content is 1-10 g/L, and the pH value of the solution is 0-3.
15. Use of the adsorbent for selective separation of gold according to claim 13 or 14 for adsorptive separation recovery of gold from gold-containing hydrochloric acid solution, characterized in that: in the steps 1 and 2, the temperature of adsorption and desorption is 20-50 ℃.
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| CN114540636A (en) * | 2022-02-24 | 2022-05-27 | 北京工业大学 | Method for recovering metal elements from metal-containing fluid |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101423612A (en) * | 2008-12-04 | 2009-05-06 | 中北大学 | Method for preparing silica gel surface phenols molecularly imprinted polymer |
| US20100051561A1 (en) * | 2008-08-29 | 2010-03-04 | Kwangyeol Lee | Porous membrane and method of making the same |
| CN103285837A (en) * | 2013-06-27 | 2013-09-11 | 武汉科梦环境工程有限公司 | Preparation method of adsorption material with high selectivity on different heavy metal ions |
| CN103599757A (en) * | 2013-10-28 | 2014-02-26 | 江苏大学 | Preparation method of magnetic temperature-sensitive surface strontium ion blotting adsorbent |
| CN104258826A (en) * | 2014-09-15 | 2015-01-07 | 江苏大学 | Active/controllable mesoporous material ion-surface imprinted polymer as well as preparation method and application of ion-surface imprinted polymer |
| CN105396555A (en) * | 2015-11-04 | 2016-03-16 | 安阳工学院 | Preparation method of mesoporous print material capable of selectively adsorbing cadmium ions |
| CN105709690A (en) * | 2016-03-07 | 2016-06-29 | 河南师范大学 | Adsorbent capable of preferentially adsorbing gold and preparing method and application thereof |
| CN106929671A (en) * | 2017-05-03 | 2017-07-07 | 中南大学 | A kind of method and device for controlling current potential reinforcing leaching gold |
| CN107376876A (en) * | 2017-09-13 | 2017-11-24 | 武汉大学 | Gold ion trace magnetic adsorbent and preparation method and application |
| US9950307B1 (en) * | 2013-08-29 | 2018-04-24 | University Of South Florida | Metal chelating composites, methods of using composites, and methods of making composites |
| CN108950202A (en) * | 2018-07-26 | 2018-12-07 | 中南大学 | A method of recycling gold from Acidic Thiourea Leaching Liquor |
| CN110290853A (en) * | 2016-10-12 | 2019-09-27 | Pq公司 | For carrying out the stable immobilization amine sorbent of REE and heavy metal recovery from fluid supply |
-
2020
- 2020-09-11 CN CN202010951206.8A patent/CN112295549A/en active Pending
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100051561A1 (en) * | 2008-08-29 | 2010-03-04 | Kwangyeol Lee | Porous membrane and method of making the same |
| CN101423612A (en) * | 2008-12-04 | 2009-05-06 | 中北大学 | Method for preparing silica gel surface phenols molecularly imprinted polymer |
| CN103285837A (en) * | 2013-06-27 | 2013-09-11 | 武汉科梦环境工程有限公司 | Preparation method of adsorption material with high selectivity on different heavy metal ions |
| US9950307B1 (en) * | 2013-08-29 | 2018-04-24 | University Of South Florida | Metal chelating composites, methods of using composites, and methods of making composites |
| CN103599757A (en) * | 2013-10-28 | 2014-02-26 | 江苏大学 | Preparation method of magnetic temperature-sensitive surface strontium ion blotting adsorbent |
| CN104258826A (en) * | 2014-09-15 | 2015-01-07 | 江苏大学 | Active/controllable mesoporous material ion-surface imprinted polymer as well as preparation method and application of ion-surface imprinted polymer |
| CN105396555A (en) * | 2015-11-04 | 2016-03-16 | 安阳工学院 | Preparation method of mesoporous print material capable of selectively adsorbing cadmium ions |
| CN105709690A (en) * | 2016-03-07 | 2016-06-29 | 河南师范大学 | Adsorbent capable of preferentially adsorbing gold and preparing method and application thereof |
| CN110290853A (en) * | 2016-10-12 | 2019-09-27 | Pq公司 | For carrying out the stable immobilization amine sorbent of REE and heavy metal recovery from fluid supply |
| CN106929671A (en) * | 2017-05-03 | 2017-07-07 | 中南大学 | A kind of method and device for controlling current potential reinforcing leaching gold |
| CN107376876A (en) * | 2017-09-13 | 2017-11-24 | 武汉大学 | Gold ion trace magnetic adsorbent and preparation method and application |
| CN108950202A (en) * | 2018-07-26 | 2018-12-07 | 中南大学 | A method of recycling gold from Acidic Thiourea Leaching Liquor |
Non-Patent Citations (3)
| Title |
|---|
| FANG-FANG YANG ET AL.: ""Enhanced molecular recognition for imprinted monolithic column containing polyhedral oligomeric silsesquioxanes by dendritic effect of mesoporous molecular sieve scaffolds"", 《ANALYTICAL AND BIOANALYTICAL CHEMISTRY》 * |
| 安富强 等: ""PEI/SiO2复合材料对 Zn2+、Cd2+的螯合吸附性能研究"", 《化学通报》 * |
| 岳晓霞 等: ""硅胶表面 AuCl4-印迹聚乙烯亚胺的制备及识别特性研究"", 《贵金属》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114540636A (en) * | 2022-02-24 | 2022-05-27 | 北京工业大学 | Method for recovering metal elements from metal-containing fluid |
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