CN109589952B - Preparation method and application of episulfide-modified activated carbon - Google Patents
Preparation method and application of episulfide-modified activated carbon Download PDFInfo
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- CN109589952B CN109589952B CN201811352989.7A CN201811352989A CN109589952B CN 109589952 B CN109589952 B CN 109589952B CN 201811352989 A CN201811352989 A CN 201811352989A CN 109589952 B CN109589952 B CN 109589952B
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- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3214—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the method for obtaining this coating or impregnating
- B01J20/3225—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the method for obtaining this coating or impregnating involving a post-treatment of the coated or impregnated product
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Abstract
The invention discloses a preparation method and application of episulfide alcohol modified activated carbon, belonging to the technical field of precious metal recovery and preparation; the method adopts cyclic mercaptan as an active carbon modifier, modifies the active carbon by an impregnation method, and is used for adsorbing Au (S) in solution2O3)2 3－(ii) a The method solves the problem that the prior active carbon carries copper cyanide complex ions (Cu (CN))4 2‑) Adsorption recovery of Au (S)2O3)2 3－The existing defects of cyanide pollution and Prussian blue loaded such as complex modification process and difficult continuous adsorption; the modified activated carbon can effectively adsorb gold in thiosulfate gold leaching, and has the advantages of multistage adsorption capacity and the like.
Description
Technical Field
The invention relates to a preparation method and application of episulfide-modified activated carbon, and belongs to the technical field of precious metal recovery.
Background
The thiosulfate gold extraction technology hasThe method has the advantages of no toxicity, environmental protection, suitability for treating gold ores which are difficult to treat by cyanidation methods such as copper, arsenic, antimony, carbon and the like, no corrosion to equipment and the like, and is considered to be the nontoxic gold extraction technology with the most industrialization prospect. With the increasing complexity of gold ore and the improvement of environmental protection requirements, the thiosulfate gold extraction method becomes the first choice technology for gold extraction; but because of the activated carbon to Au (S)2O3)2 3－The adsorption capacity of the method is extremely low, and a CIP method commonly used in cyaniding gold extraction cannot be adopted, so that the economic benefit of the method cannot be compared with that of the traditional cyaniding method, and the popularization of the technology is limited.
In order to improve the ratio of active carbon to Au (S)2O3)2 3－The adsorption capacity of the method is that copper cyanide complex ions are loaded on activated carbon (see the document US 8,500,847B 2) and then Au (S) is exchanged with gold by using the related ions2O3)2 3－The adsorption is carried out, and certain effect is achieved. However, the copper cyanide complex ion itself has a high toxicity in CN-Can exist under the condition of higher concentration, and inevitably lets virulent CN in the adsorption process-The purpose of no cyanogen can not be achieved when the method enters the process flow. Some people (see document CN 104549147 a for details) load prussian blue-like compounds on activated carbon, the reagent is nontoxic and has good adsorption effect, but the preparation process of modified activated carbon is complex and time-consuming, involves multiphase chemical reaction, is difficult to control reaction uniformity and process flow, is difficult to amplify the process, and needs further improvement. In addition, there is no concern about continuous adsorption which is necessary in actual production.
Disclosure of Invention
The invention aims to provide a method for recovering Au (S) in solution2O3)2 3－The preparation method of the modified activated carbon adopts the solution of the episulfide as the modifier of the activated carbon, and prepares the episulfide modified activated carbon by an impregnation method; the method specifically comprises the following steps:
(1) washing with deionized water to remove ash content of the activated carbon, filtering, and drying;
(2) and (3) putting the activated carbon into an epithitic alcohol solution with the concentration of 0.1-20 g/L, soaking for 0.5-48 h at normal temperature, filtering, and drying to obtain the modified activated carbon.
Preferably, the thiol having a ring structure according to the present invention is a thiol having a molecular structure containing at least one mercapto group.
Furthermore, the cyclic mercaptan of the invention is one or a mixture of more of 2-mercaptobenzoxazole and derivatives thereof, 2-mercaptobenzimidazole and derivatives thereof, 2-mercaptothiazoline and derivatives thereof, dimercaptothiadiazole and derivatives thereof, trithiocyanuric acid and cyclopentanethiol.
Preferably, the liquid-solid ratio mL/g of the episulfide solution to the activated carbon is 1-50.
The activated carbon prepared by the method is used for recovering Au (S) in solution2O3)2 3－。
The invention has the beneficial effects that:
(1) the invention improves the content of Au (S) in the activated carbon by loading the cyclic mercaptan on the surface of the activated carbon2O3)2 3－The adsorption capacity of the method can effectively adsorb gold in thiosulfate gold leaching solution, and no Cyanide (CN) is used in the whole modification process-) Or toxic substances such as heavy metals; overcomes the defects that the prior active carbon carries copper cyanide complex ions (Cu (CN)4 2-) Adsorption recovery of Au (S)2O3)2 3－The existing modification process for cyanogen pollution and Prussian blue loading is complex and difficult to continuously adsorb.
(2) The modified activated carbon has the advantages of simple preparation process, low modification cost and high gold recovery rate; the prepared active carbon has multiple adsorption capacity; and the solvent and the cyclic mercaptan can be fully recovered and recycled for multiple times, toxic waste is not discharged, and the method is environment-friendly.
(3) The modified activated carbon has a wide pH range suitable for adsorption solution, and has a good adsorption effect in the range of pH more than or equal to 6; the prepared active carbon can be continuously adsorbed, and the industrial production requirements are met.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the scope of the present invention is not limited to the examples.
Example 1
A preparation method of episulfide-modified activated carbon specifically comprises the following steps:
(1) 2g of granular activated carbon is taken, washed by deionized water, powdered dust is removed, filtered and dried for 12 hours at the temperature of 100 ℃.
(2) And (2) placing the activated carbon dried in the step (1) into a 2-mercaptobenzoxazole solution with the concentration of 1g/L according to the liquid-solid ratio (mL: g) of 50, soaking for 24 hours at normal temperature, filtering, drying, and storing for later use.
Three 100mL portions of 10ppm Au (S) were prepared2O3)2 3-Adjusting the pH value of the solution (adsorption solution for short) to 8 before adsorption; adding 1g of the activated carbon obtained in the step (2) into the first part of adsorption solution, adsorbing for 24 hours, filtering, adding into the second part of adsorption solution, adsorbing for 24 hours; filtering, adding into the third part of adsorption solution, and adsorbing for 24 hr (three times of continuous adsorption). The three adsorption rates are respectively as follows: 100 percent, 100 percent and 85 percent, and the gold loading capacity on the activated carbon after three times of adsorption is 2.85 kg/t.
Example 2
A preparation method of episulfide-modified activated carbon specifically comprises the following steps:
(1) 3g of powdered activated carbon is taken, washed by deionized water, filtered and dried for 12 hours at 100 ℃.
(2) Drying the product obtained in the step (1) according to the liquid-solid ratio (mL: g) of 30
Placing the activated carbon in a 2-mercaptobenzimidazole acetone solution with the concentration of 10g/L, and stirring at normal temperature (the stirring speed is 100 rpm) for 2 hours; filtering, oven drying, and storing.
100mL of Au (S) was prepared at a concentration of 100ppm2O3)2 3-Adjusting the pH value of the solution (adsorption solution for short) to 9 before adsorption; adding 0.5g of the activated carbon obtained in the step (2) into a simulated thiosulfate gold leaching solution, adsorbing for 48 hours, and then absorbingThe adsorption rate was 43.1%. The loading was 8.62 kg/t.
Example 3
A preparation method of episulfide-modified activated carbon specifically comprises the following steps:
(1) 3g of powdered activated carbon is taken, washed by deionized water, filtered and dried for 12 hours at 100 ℃.
(2) And (2) according to the liquid-solid ratio (mL: g) of 40, putting the dried activated carbon in the step (1) into an ethanol solution of benzyl mercaptan with the concentration of 8g/L, stirring at normal temperature (the stirring speed is 100 rpm) for 0.5h, filtering, drying, and storing for later use.
100mL of Au (S) was prepared at a concentration of 100ppm2O3)2 3-Adjusting the pH value of the solution (adsorption solution for short) to 12 before adsorption; and (3) adding 0.5g of the activated carbon obtained in the step (2) into a simulated thiosulfate gold leaching solution, wherein the adsorption rate is 46% after 48-hour adsorption. The loading was 9.2 kg/t.
Example 4
A preparation method of episulfide-modified activated carbon specifically comprises the following steps:
(1) 2g of granular coconut shell activated carbon is cleaned by deionized water, filtered and dried for 12 hours at 100 ℃.
(2) And (2) according to the liquid-solid ratio (mL: g) of 20, soaking the dried activated carbon in the step (1) in a 0.5g/L N, N-dimethylformamide solution containing 2, 5-dimercaptothiadiazole at normal temperature for 6 hours, filtering, drying and storing for later use.
Taking an ore leach solution containing about 2.67 g/t gold as an example, Au (S) is contained in the leach solution2O3)2 3-Has a concentration of 12mg/L, Cu2+The concentration is 5mmol/L, NH3/NH4 +The concentration is 3 mol/L, and the pH value is 11; preparing three 100mL portions of the leaching solution, adding 1g of the activated carbon obtained in the step (2) into the first portion of the leaching solution, adsorbing for 24 hours, filtering, adding into the second portion of the adsorption solution, adsorbing for 24 hours; filtering, adding into the third part of adsorption solution, and adsorbing for 24 hr (four times of continuous adsorption). The adsorption rates of the four times of continuous adsorption are respectively 80 percent and 60 percent,30 percent and 20 percent, and the loading amount of gold on the activated carbon is 2.28 kg/t.
Example 5
A preparation method of episulfide-modified activated carbon specifically comprises the following steps:
(1) washing 2g of granular coconut shell activated carbon with deionized water, removing powder dust, filtering, and drying at 100 ℃ for 12 h.
(2) And (2) according to the liquid-solid ratio (mL: g) of 1, soaking the dried activated carbon in the step (1) in a trithiocyanuric acid-containing ethanol solution with the concentration of 3g/L for 48h at normal temperature, filtering, drying, and storing for later use.
Taking an ore leachate containing 1.39 g/t gold as an example, the leachate contains dithiosulfuric acid alloy (I) (Au (S)2O3)2 3－) Has a concentration of 9 mg/L and contains Cu2+The concentration is 10 mmol/L, and the NH is contained3/NH4+The concentration is 1 mol/L, and the pH value is 8.0; preparing three 100mL portions of the leachate, adding 1g of the activated carbon in the step (2) into the first portion of the leachate, adsorbing for 24 hours, filtering and replacing the adsorption solution, and continuously adsorbing for four times in such a way that the adsorption rates are 63%, 39%, 17% and 7% respectively, and the loading amount of gold on the activated carbon is 1.134 kg/t.
Example 6
A preparation method of episulfide-modified activated carbon specifically comprises the following steps:
(1) 2g of granular activated carbon is taken, washed by deionized water, powdered dust is removed, filtered and dried for 12 hours at the temperature of 100 ℃.
(2) And (2) according to the liquid-solid ratio (mL: g) of 10, putting the dried activated carbon in the step (1) into a 2-mercaptothiazoline ethanol solution with the concentration of 0.1g/L, soaking for 12 hours at normal temperature, filtering, drying, and storing for later use.
Three 100mL portions of 10ppm Au (S) were prepared2O3)2 3-Adjusting the pH value of the solution (adsorption solution for short) to 9 before adsorption; adding 1g of the activated carbon obtained in the step (2) into the first part of adsorption solution, adsorbing for 24 hours, filtering, adding into the second part of adsorption solution, adsorbing for 24 hours; filtering, and adding into the third part of adsorption solutionThe adsorption is carried out for 24h (three times of continuous adsorption). The three adsorption rates are respectively as follows: 62 percent, 41 percent and 19 percent, and the gold loading on the activated carbon after three times of adsorption is 1.220 kg/t.
Example 7
A preparation method of episulfide-modified activated carbon specifically comprises the following steps:
(1) 2g of granular activated carbon is taken, washed by deionized water, powdered dust is removed, filtered and dried for 12 hours at the temperature of 100 ℃.
(2) And (2) according to the liquid-solid ratio (mL: g) of 20, placing the activated carbon dried in the step (1) in an ethanol solution of pentanethiol with the concentration of 5g/L, soaking for 72 hours at normal temperature, filtering, drying, and storing for later use.
Three 100mL portions of 10ppm Au (S) were prepared2O3)2 3-Adjusting the pH value of the solution (adsorption solution for short) to 9 before adsorption; adding 0.5g of the activated carbon obtained in the step (2) into the first part of adsorption solution, adsorbing for 24 hours, filtering, adding into the second part of adsorption solution, and adsorbing for 24 hours; filtering, adding into the third part of adsorption solution, and adsorbing for 24 hr (three times of continuous adsorption). The three adsorption rates are respectively as follows: 58 percent, 35 percent and 16 percent, and the gold loading on the activated carbon after three times of adsorption is 2.18 kg/t.
Claims (3)
1. A preparation method of episulfide-modified activated carbon is characterized by comprising the following steps:
(1) washing with deionized water to remove ash content of the activated carbon, filtering, and drying;
(2) putting the activated carbon into an epithio-alcohol solution with the concentration of 0.1-20 g/L, soaking for 0.5-48 h at normal temperature, filtering, and drying to obtain modified activated carbon;
the cyclic mercaptan is one or a mixture of more of 2-mercaptobenzoxazole and derivatives thereof, 2-mercaptobenzimidazole and derivatives thereof, 2-mercaptothiazoline and derivatives thereof, dimercaptothiadiazole and derivatives thereof, trithiocyanuric acid and cyclopentanethiol.
2. The method of claim 1, further comprising: the liquid-solid ratio mL/g of the solution of the epithiolic acid to the activated carbon is 1-50.
3. Use of the activated carbon prepared by the method of claim 1 or 2 for recovery of Au (S) in solution2O3)2 3－。
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| CN110280219A (en) * | 2019-06-27 | 2019-09-27 | 济南大学 | A kind of preparation method of the modified certain herbaceous plants with big flowers stem marrow adsorbent of trithiocyanuric acid |
| CN111004922A (en) * | 2019-12-12 | 2020-04-14 | 昆明理工大学 | Method for recovering gold in thiosulfate system |
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| CN111889068A (en) * | 2020-06-19 | 2020-11-06 | 昆明理工大学 | For adsorbing and recovering Au (S)2O3)2]3-Modification method of ion-complexed active carbon |
| CN111841492A (en) * | 2020-06-19 | 2020-10-30 | 昆明理工大学 | For adsorbing and recovering Au (S)2O3)2]3-Preparation method of ionic carbonaceous material |
| CN112375911B (en) * | 2020-11-02 | 2022-07-05 | 昆明理工大学 | Direct recovery of (Au (S) with active carbon2O3)23-) Method (2) |
| CN115612857B (en) * | 2022-10-25 | 2023-10-20 | 昆明理工大学 | Method for selectively recycling gold (III) in waste circuit board leaching solution |
| CN116920832A (en) * | 2023-07-21 | 2023-10-24 | 昆明理工大学 | Method for preparing acetylene hydrochlorination catalyst by using secondary gold resource |
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| CN101851335A (en) * | 2010-05-26 | 2010-10-06 | 鲁东大学 | Preparation method of dual-functional group modified silica gel adsorptive material and application thereof in metal ion adsorption |
| CN104549147A (en) * | 2014-12-23 | 2015-04-29 | 昆明理工大学 | Preparation method and application of activated carbon for recycling gold |
| CN104745814A (en) * | 2015-03-25 | 2015-07-01 | 苏州鼎驰金属材料有限公司 | Method for adsorbing and recovering metal ions in solution by modified silica gel of propanethiol containing substituent groups |
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