CN115970666A - Activated carbon regeneration process - Google Patents

Activated carbon regeneration process Download PDF

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Publication number
CN115970666A
CN115970666A CN202211606400.8A CN202211606400A CN115970666A CN 115970666 A CN115970666 A CN 115970666A CN 202211606400 A CN202211606400 A CN 202211606400A CN 115970666 A CN115970666 A CN 115970666A
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China
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activated carbon
acid
regeneration process
acid washing
temperature
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CN202211606400.8A
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Inventor
张呼生
杨晓东
宋坤
刘希军
李巍
李曙光
文志民
崔文俐
李强
赵鑫
孙星
栾文斌
肖发爱
秦世建
张旭阳
马登望
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Xihe County Zhongbao Mining Co ltd
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Xihe County Zhongbao Mining Co ltd
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Priority to CN202211606400.8A priority Critical patent/CN115970666A/en
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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Abstract

The invention discloses an activated carbon regeneration process, which comprises the following steps: step 1, acid washing, namely preparing acid washing solution by using hydrochloric acid and nitric acid, putting active carbon to be generated into the acid washing solution, and stirring the active carbon; and 2, accelerating acid washing, wherein when stirring and acid washing are carried out, the acid washing efficiency is accelerated through ultrasonic waves, so that the acid washing solution completely enters the activated carbon. The method has the advantage of good regeneration effect, and solves the problems that the existing activated carbon regeneration process is inconvenient to cause pickling solution to completely enter the pore diameter of the activated carbon in the process of regenerating the activated carbon, the pickling effect is reduced, the subsequent dissociation of the activated carbon is influenced, and the nitrified substances generated by the nitric acid reaction are inconvenient to remove and easily cause environmental pollution when the nitric acid is used for pickling.

Description

Activated carbon regeneration process
Technical Field
The invention relates to the field of activated carbon, in particular to an activated carbon regeneration process.
Background
Gold beneficiation is mature on the method, cyanidation is used for gold leaching to dissolve gold, and activated carbon is used for absorption. In other studies, most cyanide-free agents are used for improvement, but the large-scale application is impossible due to problems such as economic cost and equipment cost. There is still room for improvement in the cyanide leaching process of gold beneficiation. The key point of the problem is that in the activated carbon adsorption process, most of the commonly used activated carbon is prepared by processing coconut shells, sugarcane and other materials, the surface of the activated carbon is loose and porous, and a plurality of adsorption points exist, so that not only a gold complex can be adsorbed on the sites in the precious liquid adsorption process, but also organic matters such as gangue minerals, engine oil and lubricating oil in the production process are adsorbed. The adsorbed activated carbon can not completely release gold in the cleavage process, and the gold can be retained in the activated carbon, so that the recovery rate of the gold is reduced.
In the secondary activation process of the activated carbon, due to the undifferentiated adsorption performance of the activated carbon, a lot of Ca < 2+ > and Fe < 3+ > plasma can be adsorbed on the activated carbon, the ions are mainly generated in gangue minerals and beneficiation equipment, pH adjustment is performed by using NaOH, lime and the like in beneficiation, so that the pulp seed ions are complex, the Ca < 2+ > ions can react with CO2 to generate calcium carbonate, and the impurities can be adsorbed on the activated carbon and occupy adsorption points in the activated carbon. The general treatment method is to remove the substances by using acid washing, but the solution cannot be rapidly diffused in the activated carbon due to the internal structure problem of the activated carbon, and cavities are even formed at some adsorption sites due to the hydrophobic property problem of the activated carbon, so that the adsorption efficiency of the activated carbon is influenced.
The existing activated carbon regeneration process is inconvenient for enabling the pickling solution to completely enter the aperture of the activated carbon in the process of regenerating the activated carbon, reduces the pickling effect, influences the subsequent dissociation of the activated carbon, is inconvenient for removing the nitrate generated by the nitric acid reaction when the nitric acid is used for pickling, and is easy to cause environmental pollution.
Disclosure of Invention
The invention aims to provide an activated carbon regeneration process, which has the advantage of good regeneration effect and solves the problems that the existing activated carbon regeneration process is inconvenient to enable pickling solution to completely enter the pore diameter of activated carbon in the process of regenerating the activated carbon, the pickling effect is reduced, the subsequent dissociation of the activated carbon is influenced, and the nitrate generated by the nitric acid reaction is inconvenient to remove when nitric acid is used for pickling, so that the environmental pollution is easily caused.
In order to achieve the purpose, the invention provides the following technical scheme: an activated carbon regeneration process, comprising the steps of:
step 1, acid washing, namely preparing acid washing solution by using hydrochloric acid and nitric acid, putting active carbon to be generated into the acid washing solution, and stirring the active carbon;
step 2, accelerating acid washing, wherein when stirring and acid washing are carried out, the acid washing efficiency is accelerated through ultrasonic waves, so that an acid washing solution completely enters the activated carbon;
step 3, removing hydrocyanic acid, namely removing hydrocyanic acid by using a chlorine dioxide solution, oxidizing cyanide into cyanate through the oxidation action of the chlorine dioxide solution, and finally further oxidizing the cyanate into carbon dioxide and hydrogen;
step 4, removing the nitrified substances, and after the pickling is finished, carrying out denitration treatment on the nitrified substances in the waste activated carbon by using microwaves and a denitration catalyst;
step 5, dissociation, namely soaking the activated carbon in a sodium chloride solution and a sodium hydroxide solution, and washing the activated carbon by using ionized water after soaking is finished, wherein the gold in the activated carbon is washed away by the ionized water;
step 6, cleaning, namely performing secondary washing on the dissociated active carbon to wash away impurities on the surface of the active carbon;
step 7, drying, namely drying and dehydrating the cleaned activated carbon so that the activated carbon can be subjected to subsequent regeneration;
step 8, high-temperature carbonization, namely carbonizing the volatile substances adsorbed on the activated carbon and the high-boiling-point organic substances remained in the pores of the activated carbon by using high temperature, thermally decomposing the high-boiling-point organic substance adsorbates, directly desorbing the part converted into the small molecular substances, and performing polycondensation reaction on the rest part to form a fixed carbon form and remain in the pores;
and 9, high-temperature activation, namely cleaning micropores of the activated carbon by adding water vapor and gases such as CO2 generated by oxidation reaction in the roasting stage, and vaporizing organic carbon residues blocked in the micropores of the activated carbon so as to recover the adsorption performance of the activated carbon.
As a preferable preference of the activated carbon regeneration process of the present invention, the stirring time in the step 1 is 30 to 60min.
Preferably, in the activated carbon regeneration process of the present invention, the ultrasonic frequency in step 2 is 20 to 30HZ.
Preferably, the denitration temperature in the step 4 is 100-300 ℃, and the denitration time is 20-40min.
Preferably, in the step 5, the concentration of the sodium chloride solution is 4% -5%, the concentration of the sodium hydroxide solution is 2%, and the soaking time is 1-2h.
Preferably, in the activated carbon regeneration process, the ionized water washing time in the step 5 is 6-8 hours, and the washing temperature is 80-120 ℃.
Preferably, in the activated carbon regeneration process of the present invention, the drying temperature in step 7 is 100 to 150 ℃.
Preferably, in the activated carbon regeneration process of the present invention, the high-temperature carbonization temperature in step 8 is 350 to 800 ℃.
As one preferable activated carbon regeneration process of the present invention, the high temperature activation temperature in the step 9 is 800 to 1000 ℃.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, the active carbon is subjected to acid washing, so that impurities adsorbed in pores of the active carbon can be removed, the influence on subsequent dissociation and gold removal of the active carbon is avoided, the acid washing effect can be increased by using a solution prepared from hydrochloric acid and nitric acid in the acid washing process, and the acid solution and the active carbon can be uniformly contacted by stirring in the acid washing process.
2. In the acid washing process, the acid washing is accelerated by using ultrasonic waves, so that the acid washing solution can uniformly enter pores of the activated carbon, the acid washing solution can completely remove organic matters, and the subsequent dissociation effect of the activated carbon is improved.
3. According to the method, hydrocyanic acid is removed in the pickling process, so that the safe and reliable operation of the whole reaction is ensured, in the pickling process, due to the existence of cyanide ions in the waste activated carbon, hydrocyanic acid is separated out under the condition of weak acid, a chlorine dioxide solution is used for eliminating hydrocyanic acid, cyanide is oxidized into cyanate through the oxidation effect of the chlorine dioxide solution, and finally, the cyanate is further oxidized into carbon dioxide and hydrogen.
4. According to the invention, the activated carbon and the denitration catalyst are heated by microwaves, so that the denitration catalyst removes the nitrified substances in the activated carbon, the pollution to the environment caused by the emission of the nitrified substances is avoided, the activated carbon is soaked in a sodium chloride solution and a sodium hydroxide solution for dissociation, and after the dissociation is finished, the activated carbon is washed by ionized water, so that the gold in the activated carbon can be washed away.
5. According to the invention, the activated carbon is washed for the second time, so that impurities on the surface of the activated carbon can be removed, the subsequent regeneration of the activated carbon is facilitated, and the activated carbon is dried after the secondary washing is completed, so that the subsequent transportation and high-temperature carbonization of the activated carbon are facilitated.
6. According to the invention, the organic matters on the active carbon can be carbonized through high-temperature carbonization of the active carbon, the organic matters are decomposed at high temperature and are separated from the surface of the active carbon, and after the high-temperature carbonization, the active carbon is activated at high temperature, and the organic matter residues in the pores of the active carbon are vaporized through the high-temperature activation, so that the active carbon has adsorption performance in regeneration.
Detailed Description
Example (b):
an activated carbon regeneration process, comprising the following steps:
step 1, pickling, blending hydrochloric acid and nitric acid to prepare a pickling solution, putting the active carbon to be produced into the pickling solution, stirring the active carbon, wherein the stirring time is 45min, and by pickling the active carbon, impurities adsorbed inside pores of the active carbon can be removed, so that influence on subsequent dissociation of the active carbon is avoided and gold is removed.
And 2, accelerating acid washing, wherein when stirring and acid washing are carried out, the acid washing efficiency is accelerated through ultrasonic waves, so that the acid washing solution completely enters the activated carbon, the frequency of the ultrasonic waves is 25HZ, and the acid washing solution can uniformly enter pores of the activated carbon by using the ultrasonic waves to accelerate the acid washing in the acid washing process, so that the organic matters are completely removed by the acid washing solution, and the subsequent dissociation effect of the activated carbon is increased.
And 3, removing hydrocyanic acid, using a chlorine dioxide solution to remove hydrocyanic acid, oxidizing cyanide into cyanate through the oxidation action of the chlorine dioxide solution, and finally further oxidizing into carbon dioxide and hydrogen.
And 4, removing the nitrates, using microwaves and a denitration catalyst to denitrate the nitrates in the waste activated carbon after the pickling is finished, wherein the denitration temperature is 200 ℃, the denitration time is 30min, and heating the activated carbon and the denitration catalyst by using the microwaves to remove the nitrates from the activated carbon by the denitration catalyst, so that the nitrates are prevented from being discharged to pollute the environment.
And 5, dissociating, namely soaking the activated carbon in a sodium chloride solution and a sodium hydroxide solution, washing the activated carbon by using ionized water after soaking is finished, washing the activated carbon by using the ionized water, wherein the gold in the activated carbon is washed away by the ionized water, the concentration of the sodium chloride solution is 5%, the concentration of the sodium hydroxide solution is 2%, the soaking time is 1.5h, the washing time of the ionized water is 7h, the washing temperature is 100 ℃, dissociating by soaking the activated carbon in the sodium chloride solution and the sodium hydroxide solution, and washing the activated carbon by using the ionized water after dissociation is finished, so that the gold in the activated carbon can be washed away.
And 6, washing, namely washing the dissociated active carbon for the second time to wash away impurities on the surface of the active carbon, and washing the active carbon for the second time to remove the impurities on the surface of the active carbon so as to facilitate the subsequent regeneration of the active carbon.
And 7, drying, namely drying and dehydrating the cleaned activated carbon to enable the activated carbon to be subjected to subsequent regeneration, wherein the drying temperature is 125 ℃, and drying the activated carbon after finishing the regeneration again to facilitate subsequent transportation and high-temperature carbonization of the activated carbon.
And 8, high-temperature carbonization, namely carbonizing the volatile substances adsorbed on the activated carbon and the high-boiling-point organic matters remained in the pores of the activated carbon by using high temperature, wherein the high-boiling-point organic matter adsorbates are thermally decomposed, part of the high-boiling-point organic matter adsorbates converted into small molecular substances are directly desorbed, the rest part of the high-boiling-point organic matter adsorbates are in a fixed carbon form through polycondensation and remain in the pores, the high-temperature carbonization temperature is 350-800 ℃, the organic matters on the activated carbon can be carbonized through high-temperature carbonization of the activated carbon, and the organic matters are decomposed at high temperature and are separated from the surface of the activated carbon.
And 9, high-temperature activation, namely cleaning micropores of the activated carbon by adding water vapor and gases such as CO2 generated by oxidation reaction in the roasting stage, vaporizing the organic carbon residues blocked in the micropores of the activated carbon so as to recover the adsorption performance, wherein the high-temperature activation temperature is 800-1000 ℃, and after high-temperature carbonization, performing high-temperature activation on the activated carbon, and vaporizing the organic residues in the pores of the activated carbon by the high-temperature activation so as to ensure that the activated carbon has the adsorption performance in regeneration.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (9)

1. The activated carbon regeneration process is characterized by comprising the following steps:
step 1, acid washing, namely preparing acid washing solution by using hydrochloric acid and nitric acid, putting active carbon to be generated into the acid washing solution, and stirring the active carbon;
step 2, accelerating acid washing, wherein when stirring and acid washing are carried out, the acid washing efficiency is accelerated through ultrasonic waves, so that acid washing solution completely enters the activated carbon;
step 3, removing hydrocyanic acid, namely removing hydrocyanic acid by using a chlorine dioxide solution, oxidizing cyanide into cyanate through the oxidation action of the chlorine dioxide solution, and finally further oxidizing the cyanate into carbon dioxide and hydrogen;
step 4, removing the nitrified substances, and after the pickling is finished, carrying out denitration treatment on the nitrified substances in the waste activated carbon by using microwaves and a denitration catalyst;
step 5, dissociation, namely soaking the activated carbon in a sodium chloride solution and a sodium hydroxide solution, and washing the activated carbon by using ionized water after soaking is finished, wherein the gold in the activated carbon is washed away by the ionized water;
step 6, cleaning, namely performing secondary washing on the dissociated active carbon to wash away impurities on the surface of the active carbon;
step 7, drying, namely drying and dehydrating the cleaned activated carbon so that the activated carbon can be subjected to subsequent regeneration;
step 8, high-temperature carbonization, namely carbonizing volatile substances adsorbed on the activated carbon and high-boiling-point organic matters remained in pores of the activated carbon by using high temperature, thermally decomposing the high-boiling-point organic matter adsorbates, directly desorbing a part converted into small molecular substances, and forming a fixed carbon form by condensation polymerization of the rest part and remaining in the pores;
and 9, high-temperature activation, namely cleaning micropores of the activated carbon by adding water vapor and gases such as CO2 generated by oxidation reaction in the roasting stage, and vaporizing organic carbon residues blocked in the micropores of the activated carbon so as to recover the adsorption performance of the activated carbon.
2. The activated carbon regeneration process of claim 1, wherein: the stirring time in the step 1 is 30-60min.
3. The activated carbon regeneration process of claim 1, wherein: the ultrasonic frequency in the step 2 is 20-30HZ.
4. The activated carbon regeneration process of claim 1, wherein: the denitration temperature in the step 4 is 100-300 ℃, and the denitration time is 20-40min.
5. The activated carbon regeneration process of claim 1, wherein: the concentration of the sodium chloride solution in the step 5 is 4% -5%, the concentration of the sodium hydroxide solution is 2%, and the soaking time is 1-2h.
6. The activated carbon regeneration process of claim 1, wherein: the ionized water washing time in the step 5 is 6-8h, and the washing temperature is 80-120 ℃.
7. The activated carbon regeneration process of claim 1, wherein: the drying temperature in the step 7 is 100-150 ℃.
8. The activated carbon regeneration process of claim 1, wherein: the high-temperature carbonization temperature in the step 8 is 350-800 ℃.
9. The activated carbon regeneration process of claim 1, wherein: the high-temperature activation temperature in the step 9 is 800-1000 ℃.
CN202211606400.8A 2022-12-12 2022-12-12 Activated carbon regeneration process Pending CN115970666A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116832771A (en) * 2023-05-12 2023-10-03 深圳共田生态环境有限公司 Preparation method of artificial wetland filler bagasse biochar and biochar
CN117160432A (en) * 2023-08-17 2023-12-05 清远市富盈电子有限公司 Desorption liquid, preparation method, active carbon desorption method and active carbon

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116832771A (en) * 2023-05-12 2023-10-03 深圳共田生态环境有限公司 Preparation method of artificial wetland filler bagasse biochar and biochar
CN117160432A (en) * 2023-08-17 2023-12-05 清远市富盈电子有限公司 Desorption liquid, preparation method, active carbon desorption method and active carbon
CN117160432B (en) * 2023-08-17 2024-03-19 清远市富盈电子有限公司 Desorption liquid, preparation method, active carbon desorption method and active carbon

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