CN107376883B - Regeneration method of activated carbon with saturated adsorption - Google Patents
Regeneration method of activated carbon with saturated adsorption Download PDFInfo
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- CN107376883B CN107376883B CN201710827085.4A CN201710827085A CN107376883B CN 107376883 B CN107376883 B CN 107376883B CN 201710827085 A CN201710827085 A CN 201710827085A CN 107376883 B CN107376883 B CN 107376883B
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3416—Regenerating or reactivating of sorbents or filter aids comprising free carbon, e.g. activated carbon
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
- B01J20/3475—Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase
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Abstract
A regeneration method of activated carbon with saturated adsorption comprises the following steps: putting an alkaline solvent or an alkaline regeneration solvent and activated carbon with saturated adsorption into a container with a heating device and a stirring device for mixing to obtain an alkaline mixture; carrying out solid-liquid separation on the obtained alkaline mixture to obtain activated carbon to be treated, and recycling an alkaline regenerated solvent generated in the solid-liquid separation process; putting the obtained activated carbon to be treated and an acidic solvent or an acidic regenerated solvent into a container with a heater and a stirrer for mixing to obtain an acidic mixture; carrying out solid-liquid separation on the obtained acidic mixture to obtain activated carbon to be washed, and recycling an acidic regenerated solvent generated in the solid-liquid separation process; and washing the obtained activated carbon to be washed by water to obtain regenerated activated carbon, reusing the regenerated activated carbon for treating the wastewater containing the benzoic acid, and adding acid into the acidic water generated in the washing process for recycling. The regeneration cost of the active carbon is reduced; the method is environment-friendly, and the quality of the regenerated activated carbon is guaranteed; the storage cost is reduced.
Description
Technical Field
The invention belongs to the technical field of adsorbent regeneration, and particularly relates to a regeneration method of activated carbon with saturated adsorption.
Background
The above-mentioned adsorption-saturated activated carbon mainly refers to, but is not absolutely limited to, adsorption-saturated activated carbon produced in the treatment of wastewater containing benzoic acid. The benzoic acid-containing wastewater refers to wastewater generated in the process of preparing organic peroxide or other chemical products from benzoyl chloride.
Because the activated carbon has the characteristics of large specific surface area, rich porosity, no toxicity, no odor, strong adsorption capacity and the like, the activated carbon is widely applied to the fields of pharmaceutical and chemical industry, food, municipal sewage treatment, industrial wastewater treatment, water purification and the like as an adsorbent, and becomes an indispensable important material in the fields.
Since activated carbon is expensive and is becoming a resource shortage, if activated carbon saturated in adsorption is discarded, there is no question of wasting the resource and causing secondary pollution to the environment. In view of this, from the economical, resource-saving and environmental-friendly points of view, the regeneration of the activated carbon saturated by adsorption for reuse is a beneficial measure to embody the spirit of economical, energy-saving and environmental-friendly recycling economy.
At present, the methods for regenerating adsorption saturated activated carbon mainly comprise the following steps: firstly, a thermal regeneration method; second, chemical agent regeneration (customarily called chemical regeneration); thirdly, a biological regeneration method; fourthly, electrochemical regeneration method. Technical information on the regeneration of activated carbon is not known in published chinese patent documents, such as CN103212391A (a microwave activated carbon regeneration method and a waste treatment apparatus thereof), CN106944025A (a powdered activated carbon regeneration method), and CN106732487A (TiO 106732487A)2A method for regenerating photocatalytic activated carbon), CN104741080B (a method for regenerating organic adsorption saturated activated carbon), CN1544142A (a method for removing organic matters by microwave-enhanced solvent elution regeneration of activated carbon), CN103212391A (a method for regenerating microwave activated carbon and a waste gas treatment device thereof), CN104190389B (a method for thermally regenerating activated carbon and a device thereof), CN103230785B (a method for producing regenerated activated carbon), CN104815633A (a method for biologically regenerating granular activated carbon which is saturated by nonylphenol adsorption) and CN105582904A (a method for regenerating activated carbon), and the like.
The above-mentioned methods of regenerating activated carbon are not suitable for the regeneration of adsorption-saturated activated carbon. In particular, the thermal regeneration method mentioned in the above document has a problem of large energy consumption, and the organic matter is easily carbonized to block the pores of the carbon; the regeneration of activated carbon by microwave method cannot effectively separate solids from solids; microbial regeneration is difficult to decompose compounds with benzene rings.
Typically, CN106944024A recommends "a method for regenerating activated carbon saturated by adsorption", which comprises drying activated carbon with moisture content of 30-60% and saturated by adsorption at 130 ℃ of 100-. Although the method can regenerate the activated carbon with saturated adsorption, the method has the defects of large energy consumption, long regeneration time and high regeneration cost.
Disclosure of Invention
The invention aims to provide an activated carbon regeneration method with saturated adsorption, which does not need drying and activation, thereby saving energy consumption in the regeneration process, being beneficial to recycling a solvent generated in the regeneration process, avoiding environmental damage, reflecting good cyclic economy spirit, being beneficial to washing out a complex in the activated carbon, thereby ensuring the quality of the regenerated activated carbon and being convenient for putting the regenerated activated carbon into the wastewater treatment containing benzoic acid.
The task of the invention is achieved by a regeneration method of activated carbon saturated by adsorption, which comprises the following steps:
A) preparing an alkaline mixture, putting an alkaline solvent and activated carbon with saturated adsorption or putting an alkaline regeneration solvent and activated carbon with saturated adsorption into a container with a heating device and a stirring device for mixing, controlling the mass ratio of the alkaline solvent and the alkaline regeneration solvent to the activated carbon with saturated adsorption, controlling the heating temperature of the heating device and the stirring speed and the stirring time of the stirring device to obtain the alkaline mixture, wherein the activated carbon with saturated adsorption is the activated carbon with saturated adsorption generated in the treatment process of wastewater containing benzoic acid;
B) solid-liquid separation of the alkaline mixture, namely performing solid-liquid separation on the alkaline mixture obtained in the step A) to obtain activated carbon to be treated, and recycling an alkaline regeneration solvent generated in the solid-liquid separation process in the step A);
C) preparing an acidic mixture, namely putting the activated carbon to be treated obtained in the step B) and an acidic solvent or an acidic regenerated solvent into a container provided with a heater and a stirrer for mixing, controlling the mass ratio of the activated carbon to be treated and the acidic solvent or the acidic regenerated solvent, controlling the heating temperature of the heater and the stirring speed and the stirring time of the stirrer, and obtaining the acidic mixture;
D) c), performing solid-liquid separation on the acidic mixture obtained in the step C), so as to obtain activated carbon to be washed, and reusing an acidic regeneration solvent generated in the solid-liquid separation process in the step C);
E) washing, namely washing the activated carbon to be washed obtained in the step D) by using water and controlling the volume ratio of the activated carbon to be washed to the water to obtain regenerated activated carbon which is reused for treating the wastewater containing the benzoic acid, wherein: and (4) recycling the acidic wastewater generated in the water washing process to the step C) after adding acid.
In a specific embodiment of the invention, the step A) of controlling the mass ratio of the alkaline solvent or the alkaline regeneration solvent to the activated carbon saturated for adsorption is to control the mass ratio of the alkaline solvent or the alkaline regeneration solvent to the activated carbon saturated for adsorption to be 1: 10-15.
In another specific embodiment of the present invention, the heating temperature of the heating device is controlled to 40 ℃ in step a), the stirring speed and the stirring time of the stirring device are controlled to 30-120rpm, and the stirring time is controlled to 10-60 min.
In yet another specific embodiment of the present invention, the alkaline solvent described in step a) is a sodium hydroxide solution having a concentration of 1-5% by mass.
In a further particular embodiment of the invention, the alkaline regeneration solvent described in step a) and step B) is a sodium hydroxide solution recovered and having a specific concentration of 1-5% by mass of sodium hydroxide.
In still another specific embodiment of the present invention, the step C) of controlling the mass ratio of the activated carbon to be treated to the acidic solvent or to the acidic regenerated solvent is to control the mass ratio of the activated carbon to be treated to the acidic solvent or to the acidic regenerated solvent to be 1: 10-15.
In a more specific embodiment of the present invention, the heating temperature of the heater in step C) is controlled to 40 ℃, the stirring speed and the stirring time of the stirrer are controlled to 30-120rpm, and the stirring time is controlled to 10-60 min.
In still another specific embodiment of the present invention, the acidic solvent in step C) is any one of a sulfuric acid solution having a 3-5% concentration by mass of sulfuric acid and a hydrochloric acid solution having a 3-5% concentration by mass of hydrochloric acid, or a mixture thereof.
In a still more particular embodiment of the invention, the acidic regeneration solvent described in step C) and step D) is a sulfuric acid solution and/or a hydrochloric acid solution recovered and having a specific concentration of sulfuric acid and/or hydrochloric acid of 3-5% by mass.
In yet another specific embodiment of the present invention, the step E) of controlling the volume ratio of the activated carbon to be washed to water is to control the volume ratio of the activated carbon to be washed to water to be 1: 2-5; the acid wastewater generated in the washing process is added with acid and then is reused in the step C), which means that: adding sulfuric acid and/or hydrochloric acid into the acidic wastewater generated in the water washing process, and enabling the mass percent specific concentration of the sulfuric acid and/or hydrochloric acid in the acidic wastewater to reach 3-5%.
The technical scheme provided by the invention has the technical effects that: compared with the prior art, the method does not need drying and activation, so that the energy consumption in the regeneration process can be saved, and the regeneration cost of the activated carbon is reduced; the alkaline regenerated solvent generated in the solid-liquid separation process of the alkaline mixture and the acidic regenerated solvent generated in the solid-liquid separation process of the acidic mixture are recycled, so that the environment pollution can be avoided, the circular economy spirit can be reflected, and the quality of the regenerated activated carbon can be ensured because the complex in the activated carbon can be washed away by water; the washed regenerated active carbon is directly used for treating the wastewater containing the benzoic acid, so that a corresponding storage container is not required to be arranged, and the storage cost is reduced.
Detailed Description
Example 1:
the regeneration method of the activated carbon with saturated adsorption comprises the following steps:
A) preparing an alkaline mixture, namely putting an alkaline solvent, namely a sodium hydroxide solution with the mass percent ratio concentration of 1 percent and activated carbon with saturated adsorption generated in the treatment process of wastewater containing benzoic acid into a container such as a stainless steel reaction kettle provided with a heating device and a stirring device according to the mass ratio of 1: 10, and stirring for 10min at the heating temperature of the heating device of 40 ℃ and the stirring speed of the stirring device of 75rpm to obtain the alkaline mixture;
B) solid-liquid separation of the alkaline mixture, namely performing solid-liquid separation on the alkaline mixture obtained in the step A) to obtain activated carbon to be treated, and recycling an alkaline regeneration solvent generated in the solid-liquid separation process in the step A);
C) preparing an acidic mixture, namely putting the activated carbon to be treated obtained in the step B) and an acidic solvent, namely a sulfuric acid solution with the mass percent concentration of 5 percent into a container such as a stainless steel reaction kettle which is provided with a heater and a stirrer according to the mass ratio of 1: 15, and stirring for 10min at the heating temperature of 40 ℃ and the stirring speed of 30rpm to obtain the acidic mixture;
D) c), performing solid-liquid separation on the acidic mixture obtained in the step C), so as to obtain activated carbon to be washed, and reusing an acidic regeneration solvent generated in the solid-liquid separation process in the step C);
E) washing, namely washing the activated carbon to be washed obtained in the step D) by using water, controlling the volume ratio of the activated carbon to be washed to the water to be 1: 2, obtaining regenerated activated carbon and recycling the regenerated activated carbon for treating the wastewater containing the benzoic acid, and recycling acidic water generated in the washing process to the step C) after adding acid, specifically: adding sulfuric acid into the acidic wastewater generated in the water washing process to enable the mass percent concentration of the sulfuric acid to reach 4%, or adding hydrochloric acid into the acidic wastewater generated in the water washing process to enable the mass percent concentration of the hydrochloric acid to reach 4%, or adding a mixture of sulfuric acid and hydrochloric acid into the acidic wastewater generated in the water washing process to enable the mass percent concentration of the mixture to reach 4%.
Example 2:
only changing the alkaline solvent, namely the sodium hydroxide solution in the step A), into an alkaline regeneration solvent, namely a recovered sodium hydroxide solution with the mass percent concentration of 3 percent; the acid solvent in step C) is changed to an acid regenerated solvent, i.e. a sulfuric acid solution or a hydrochloric acid solution (or a mixture of both a sulfuric acid solution and a hydrochloric acid solution) which is recovered and has a concentration of 4% by mass of sulfuric acid or hydrochloric acid, and the rest is the same as that described in example 1.
Claims (8)
1. A regeneration method of activated carbon with saturated adsorption is characterized by comprising the following steps:
A) preparing an alkaline mixture, putting an alkaline solvent and activated carbon with saturated adsorption or putting an alkaline regeneration solvent and activated carbon with saturated adsorption into a container with a heating device and a stirring device for mixing, controlling the mass ratio of the alkaline solvent and the alkaline regeneration solvent to the activated carbon with saturated adsorption, controlling the heating temperature of the heating device and the stirring speed and the stirring time of the stirring device to obtain the alkaline mixture, wherein the activated carbon with saturated adsorption is the activated carbon with saturated adsorption generated in the treatment process of wastewater containing benzoic acid;
B) solid-liquid separation of the alkaline mixture, namely performing solid-liquid separation on the alkaline mixture obtained in the step A) to obtain activated carbon to be treated, and recycling an alkaline regeneration solvent generated in the solid-liquid separation process in the step A);
C) preparing an acidic mixture, namely putting the activated carbon to be treated obtained in the step B) and an acidic solvent or an acidic regenerated solvent into a container provided with a heater and a stirrer for mixing, controlling the mass ratio of the activated carbon to be treated and the acidic solvent or the acidic regenerated solvent, controlling the heating temperature of the heater and the stirring speed and the stirring time of the stirrer, and obtaining the acidic mixture;
D) c), performing solid-liquid separation on the acidic mixture obtained in the step C), so as to obtain activated carbon to be washed, and reusing an acidic regeneration solvent generated in the solid-liquid separation process in the step C);
E) washing, namely washing the activated carbon to be washed obtained in the step D) by using water and controlling the volume ratio of the activated carbon to be washed to the water to obtain regenerated activated carbon which is reused for treating the wastewater containing the benzoic acid, wherein: acid wastewater generated in the washing process is added with acid and then is recycled in the step C);
the heating temperature of the heating control device in the step A) is controlled to be 40 ℃, the stirring speed and the stirring time of the stirring control device are controlled to be 30-120rpm, and the stirring time is controlled to be 10-60 min;
the heating temperature of the heater in the step C) is controlled to be 40 ℃, the stirring speed and the stirring time of the stirrer are controlled to be 30-120rpm, and the stirring time is controlled to be 10-60 min.
2. The method for regenerating activated carbon saturated by adsorption according to claim 1, wherein the controlling of the mass ratio of the alkaline solvent or alkaline regeneration solvent to the activated carbon saturated by adsorption in step a) is to control the mass ratio of the alkaline solvent or alkaline regeneration solvent to the activated carbon saturated by adsorption to be 1: 10-15.
3. The method for regenerating activated carbon saturated by adsorption according to claim 1, characterized in that said alkaline solvent in step a) is a sodium hydroxide solution having a concentration of 1-5% by mass.
4. The regeneration process of activated carbon saturated by adsorption according to claim 1, characterized in that said alkaline regeneration solvent in step a) and step B) is a sodium hydroxide solution recovered and having a sodium hydroxide concentration of 1-5% by mass.
5. The regeneration method of activated carbon with saturated adsorption according to claim 1, wherein the controlling of the mass ratio of the activated carbon to be treated to the acidic solvent or to the acidic regeneration solvent in step C) is to control the mass ratio of the activated carbon to be treated to the acidic solvent or to the acidic regeneration solvent to be 1: 10-15.
6. The method for regenerating adsorption-saturated activated carbon according to claim 1, wherein the acidic solvent in step C) is any one of a sulfuric acid solution having a 3-5% concentration by mass of sulfuric acid and a hydrochloric acid solution having a 3-5% concentration by mass of hydrochloric acid, or a mixture thereof.
7. The regeneration process of activated carbon saturated by adsorption according to claim 1, characterized in that said acidic regeneration solvent in step C) and step D) is a sulfuric acid solution and/or a hydrochloric acid solution recovered and having a mass% specific concentration of sulfuric acid and/or hydrochloric acid of 3-5%.
8. The regeneration method of activated carbon saturated by adsorption according to claim 1, characterized in that the volume ratio of activated carbon to be washed to water in step E) is controlled to be 1: 2-5; the acid wastewater generated in the washing process is added with acid and then is reused in the step C), which means that: adding sulfuric acid and/or hydrochloric acid into the acidic wastewater generated in the water washing process, and enabling the mass percent specific concentration of the sulfuric acid and/or hydrochloric acid in the acidic wastewater to reach 3-5%.
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| CN110605108A (en) * | 2019-09-26 | 2019-12-24 | 西安建筑科技大学 | Method for regenerating desulfurization and denitrification waste active carbon |
| CN111013542A (en) * | 2020-01-06 | 2020-04-17 | 刘德庆 | Regeneration method of powdered activated carbon |
| CN115121235B (en) * | 2021-03-29 | 2023-11-17 | 湖南大学 | Regeneration and utilization method of edible tree fungus charcoal for adsorbing heavy metals |
| FR3124742A1 (en) * | 2021-07-02 | 2023-01-06 | Suez Groupe | ON-SITE ADSORBENT MEDIA REGENERATION PROCESS |
| CN114247437A (en) * | 2021-12-21 | 2022-03-29 | 甘肃银光化学工业集团有限公司 | Chemical regeneration method of granular active carbon for adsorbing nitramine compound |
| CN115672298A (en) * | 2022-10-24 | 2023-02-03 | 中国石油化工股份有限公司 | Green energy-saving regeneration method of adsorbent for removing impurities from ester oil |
| CN117160184A (en) * | 2023-08-17 | 2023-12-05 | 清远市富盈电子有限公司 | Processing device and processing method for VOCs (volatile organic compounds) during PCB production |
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| CN101590399A (en) * | 2008-05-28 | 2009-12-02 | 北京紫光英力化工技术有限公司 | A kind of renovation process of powdered activated carbon |
| CN106582538A (en) * | 2016-12-16 | 2017-04-26 | 昆明理工大学 | Preparation and regeneration method of EDTA-Na2 modified active carbon |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101590399A (en) * | 2008-05-28 | 2009-12-02 | 北京紫光英力化工技术有限公司 | A kind of renovation process of powdered activated carbon |
| CN106582538A (en) * | 2016-12-16 | 2017-04-26 | 昆明理工大学 | Preparation and regeneration method of EDTA-Na2 modified active carbon |
Non-Patent Citations (1)
| Title |
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| Regeneration of carbonaceous adsorbents. Part II: Chemical,Microbiological and Vacuum Regeneration;Francisco Salvador等;《Microporous and Mesoporous Materials》;20140818;第202卷;277-296 * |
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