CN113713762A - Activated carbon regeneration method based on thermally activated peroxymonosulfate - Google Patents

Activated carbon regeneration method based on thermally activated peroxymonosulfate Download PDF

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Publication number
CN113713762A
CN113713762A CN202110916795.0A CN202110916795A CN113713762A CN 113713762 A CN113713762 A CN 113713762A CN 202110916795 A CN202110916795 A CN 202110916795A CN 113713762 A CN113713762 A CN 113713762A
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activated carbon
peroxymonosulfate
activated
regeneration
drying
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陶辉
林涛
顾颖
戚怡婷
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Hohai University HHU
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Hohai University HHU
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • B01J20/34Regenerating or reactivating
    • B01J20/3416Regenerating or reactivating of sorbents or filter aids comprising free carbon, e.g. activated carbon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • B01J20/34Regenerating or reactivating
    • B01J20/345Regenerating or reactivating using a particular desorbing compound or mixture
    • B01J20/3475Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • B01J20/34Regenerating or reactivating
    • B01J20/3483Regenerating or reactivating by thermal treatment not covered by groups B01J20/3441 - B01J20/3475, e.g. by heating or cooling
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/30Active carbon
    • C01B32/354After-treatment
    • C01B32/36Reactivation or regeneration
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/30Active carbon
    • C01B32/354After-treatment
    • C01B32/36Reactivation or regeneration
    • C01B32/366Reactivation or regeneration by physical processes, e.g. by irradiation, by using electric current passing through carbonaceous feedstock or by using recyclable inert heating bodies

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Toxicology (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Water Treatment By Sorption (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention discloses an activated carbon regeneration method based on thermally activated peroxymonosulfate, which comprises the following steps: drying activated carbon to be activated, eluting with hot water, reacting the activated carbon with an activating agent in boiling water under the condition of stirring, and finally filtering, cleaning and drying the activated carbon to obtain the regenerated activated carbon. The method for regenerating the activated carbon overcomes the defects of high regeneration energy consumption, low regeneration efficiency and large loss amount of the activated carbon in the conventional activated carbon thermal regeneration method, and the method for regenerating the activated carbon sequentially removes various organic matters on the activated carbon in a gradual progressive mode, does not cause the loss of the activated carbon, does not influence the strength of the activated carbon, and simultaneously ensures that the regenerated activated carbon has high adsorption performance.

Description

Activated carbon regeneration method based on thermally activated peroxymonosulfate
Technical Field
The invention relates to an activated carbon regeneration method based on thermally activated peroxymonosulfate.
Background
The active carbon is a good adsorbent, and the granular active carbon shows good adsorption effect on organic matters in water by utilizing the abundant pore structure and the huge specific surface area, and can also effectively remove substances causing odor and chromaticity in the water body, thereby improving the water quality and taste. After the activated carbon is used for a period of time, pores are gradually blocked, and the adsorption reaches saturation, so that the adsorption effect is lost, the activated carbon becomes solid waste, and professional treatment is needed. In order to improve the resource recycling rate, reduce the operation cost and improve the environmental protection requirement, the regeneration of the activated carbon has important significance.
The regeneration of the activated carbon is carried out on the premise of not damaging the property and the structure of the activated carbon, and pollutants adsorbed by the activated carbon are removed by a series of means such as a biological method, a physical method, a chemical method and the like, so that the adsorption capacity of the activated carbon is recovered. The traditional activated carbon regeneration method comprises a heating regeneration method, a chemical agent regeneration method, a biological regeneration method and an electrochemical regeneration method, and the existing activated carbon regeneration method has the problems of secondary pollution, high regeneration energy consumption cost and the like.
Disclosure of Invention
The purpose of the invention is as follows: the invention provides an activated carbon regeneration method based on thermally activated peroxymonosulfate, aiming at the problems of the existing activated carbon regeneration method.
The technical scheme is as follows: the invention relates to an activated carbon regeneration method based on thermally activated peroxymonosulfate, which comprises the following steps: drying activated carbon to be activated, eluting with hot water, reacting the activated carbon with an activating agent in boiling water under the condition of stirring, and finally filtering, cleaning and drying the activated carbon to obtain the regenerated activated carbon.
Wherein the activating agent is peroxymonosulfate, and the addition amount of the activating agent is as follows: permonosulfate with the total mass of 200-400 g is added to each cubic meter of activated carbon.
Wherein, the heating temperature is heating to boiling water.
The activated carbon regeneration method based on thermally activated peroxymonosulfate specifically comprises the following steps:
(1) soaking the activated carbon to be activated in clear water, cleaning until the effluent is clear, filtering the washed activated carbon, and naturally drying;
(2) drying the dried active carbon at the drying temperature of 80 +/-10 ℃ to remove volatile organic matters adsorbed on the active carbon and enable the active carbon to be in loose granules; the particle size of the activated carbon is 2-3 mm, and the activated carbon is easy to agglomerate;
(3) dispersing the dried activated carbon in clear water, heating until the water is boiled, stirring for 20-25 min, washing the activated carbon with boiling hot water after stirring, and performing solid-liquid separation; dispersing the activated carbon subjected to solid-liquid separation in boiling hot water, stirring for 20-25 min, washing the surface of the activated carbon with the boiling hot water, and performing solid-liquid separation again;
the step (3) can remove fine carbon powder falling from the activated carbon on one hand and can also remove organic matters adsorbed in the activated carbon by dissolving the organic matters in hot water on the other hand;
(4) dispersing the filtered activated carbon in clear water, stirring and heating until the water is boiled, and adding peroxymonosulfate into the activated carbon dispersion liquid, wherein the adding amount of the peroxymonosulfate is 200-400 g/m3Activated carbon; adding 200-400 g of peroxymonosulfate into each cubic meter of activated carbon;
too little peroxymonosulfate is added, so that the active free radicals generated after thermal activation are insufficient, and the regeneration of the active carbon cannot be fully realized; the excessive addition amount can oxidize the activated carbon by excessive free radicals and destroy the carbon structure; the total amount of the additive is 200-400 g/m3The peroxymonosulfate of the activated carbon is in a safe dosage range which can not damage the structure of the activated carbon; sulfate radicals and hydroxyl radicals with strong oxidizing property are generated by thermally activated peroxymonosulfate, microorganisms attached to the activated carbon are inactivated by the active radicals and are subjected to redox reaction with organic matters adsorbed on the activated carbon, so that the organic matters adsorbed on the activated carbon are mineralized, and the organic matters are mineralized into inorganic C, N, so that the regeneration of the activated carbon is realized;
(5) and filtering the activated carbon, washing the activated carbon for 2-3 times by using clear water after filtering, and drying the activated carbon after washing.
Wherein, in the step (1), the active carbon is naturally dried until the water content of the active carbon is not higher than 45%. Too high moisture content of the activated carbon can lead to too long drying time in the second step, and if the moisture content of the activated carbon is too low, the subsequent dispersion of the activated carbon in clear water is difficult to absorb water and floats on the water surface, so that the activation reaction time is long.
Wherein, in the step (2), the drying time is 1h, and the drying is carried out until the water content of the activated carbon is less than 8%.
In the step (4), the mixing mass ratio of the activated carbon to the clear water is 1: 1.
in the step (4), the peroxymonosulfate is added into the activated carbon dispersion liquid for 1-2 hours in 3 times on average. The active free radicals can be generated by thermally activating the peroxymonosulfate, if too much peroxymonosulfate is added at one time, the active free radicals can be quenched, and the peroxymonosulfate is added little by little, for example, the active free radicals can be continuously generated in the solution by adding the peroxymonosulfate for three times, so that the mutual elimination of the free radicals is reduced, the conversion rate of the peroxymonosulfate is improved, and the regeneration rate of the active carbon is improved.
Wherein, in the step (5), the drying temperature is 80 +/-10 ℃.
Has the advantages that: the method for regenerating the activated carbon provided by the invention overcomes the defects of high regeneration energy consumption, low regeneration efficiency and large loss amount of the activated carbon existing in the conventional activated carbon thermal regeneration method, and sequentially removes various organic matters on the activated carbon by adopting a gradual progressive mode (the gradual progressive mode means that firstly soaking and cleaning are carried out to remove the easily-eluted organic matters adsorbed on the surface of the activated carbon, then the dissolved organic matters are dissolved by hot water to remove the complex and difficultly-degraded organic matters, and finally the thermally-activated peroxymonosulfate is used to remove the complex and difficultly-degraded organic matters), so that the loss of the activated carbon is avoided, the strength of the activated carbon is not influenced, and the regenerated activated carbon also has high adsorption performance.
Detailed Description
Example 1
The invention relates to an activated carbon regeneration method based on thermally activated peroxymonosulfate, which specifically comprises the following steps:
(1) cleaning: soaking and cleaning waste activated carbon for water treatment of a certain plant with clear water, stirring and cleaning until effluent is clear, filtering the washed activated carbon, and naturally drying the filtered activated carbon, wherein the water content of the activated carbon is 42.6%;
(2) and (3) drying: drying the dried activated carbon in a forced air drying oven at the temperature of 75 ℃ to obtain the dried activated carbon with the water content of 6.2%;
(3) low-temperature thermal activation: placing the dried activated carbon in a stirring tank, adding clear water into the stirring tank, stirring for 20min at the water temperature of 100 ℃, washing the surface of the activated carbon by using clear water at the temperature of 100 ℃ after stirring, and performing solid-liquid separation; dispersing the activated carbon after solid-liquid separation into clear water at 100 ℃, stirring for 20min, washing the surface of the activated carbon with clear water at 100 ℃, and filtering after washing;
(4) activation of peroxymonosulfate: placing the filtered activated carbon in a stirring tank, adding clear water into the stirring tank to obtain an activated carbon dispersion liquid, stirring and heating to 100 ℃, wherein the activation temperature of 100 ℃ not only improves the activation degree of peroxymonosulfate and generates a large amount of active free radicals, but also increases the reaction rate of the active free radicals and organic matters, and improves the mineralization rate; adding peroxymonosulfate into the activated carbon dispersion liquid for three times on average, wherein 200g of peroxymonosulfate is added into each cubic meter of activated carbon in total, and the regeneration time is 1 h;
(5) and (3) drying: filtering the activated carbon, washing the filtered activated carbon with clear water for 2 times, drying the washed activated carbon in a blast drier at 70 ℃, recovering the adsorption performance of the dried activated carbon to be more than 85% of that of new carbon, and finally packaging and storing the dried activated carbon.
Example 1 the yield of the regenerated activated carbon after activation (i.e. the mass of the activated carbon after regeneration is 100% of the mass of the activated carbon before regeneration) is 90%, and the activated carbon after activation in example 1 is ground by a ball mill, and the strength of the activated carbon by the activation method of the present invention is consistent with that before activation, and the strength is not affected.
Example 2
(1) Cleaning: soaking and cleaning waste activated carbon for water treatment of a certain plant with clear water, stirring and cleaning until effluent is clear, filtering the washed activated carbon, and naturally drying the filtered activated carbon until the water content of the activated carbon is 43.7%;
(2) and (3) drying: drying the dried activated carbon in a forced air drying oven at the temperature of 90 ℃ to obtain the dried activated carbon with the water content of 5.4%;
(3) low-temperature thermal activation: placing the dried activated carbon in a stirring tank, adding clear water into the stirring tank, stirring for 25min at the water temperature of 100 ℃, washing the surface of the activated carbon by using clear water at the temperature of 100 ℃ after stirring, and performing solid-liquid separation; dispersing the activated carbon after solid-liquid separation into clear water at 100 ℃, stirring for 25min, washing the surface of the activated carbon with clear water at 100 ℃, and filtering after washing;
(4) activation of peroxymonosulfate: placing the filtered activated carbon in a stirring tank, adding clear water into the stirring tank to obtain an activated carbon dispersion liquid, stirring and heating to 100 ℃; adding peroxymonosulfate into the activated carbon dispersion liquid for three times on average, wherein 400g of peroxymonosulfate is added into each cubic meter of activated carbon in total, and the regeneration time is 1.5 h;
(5) and (3) drying: filtering the activated carbon, washing the filtered activated carbon with clear water for 2 times, drying the washed activated carbon in a blast drier at 90 ℃, recovering the adsorption performance of the dried activated carbon to be more than 87% of that of new carbon, and finally packaging and storing the dried activated carbon.
Example 2 the regeneration yield of activated carbon after activation (i.e. the mass of activated carbon after regeneration is 100% of the mass of activated carbon before regeneration) was 93%, and the activated carbon after activation in example 2 was ground by a ball mill, and it was found that the strength of activated carbon by the activation method of the present invention was consistent with that before activation, and the strength was not affected.
Comparative example 1
(1) Cleaning: soaking and cleaning waste activated carbon for water treatment of a certain plant with clear water, stirring and cleaning until effluent is clear, filtering the washed activated carbon, and naturally drying the filtered activated carbon, wherein the water content of the activated carbon is 55%;
(2) and (3) drying: drying the dried activated carbon in a forced air drying oven at the temperature of 75 ℃ to obtain the dried activated carbon with the water content of 7.2%;
(3) low-temperature thermal activation: placing the dried activated carbon in a stirring tank, adding clear water into the stirring tank, stirring for 25min at the water temperature of 100 ℃, washing the surface of the activated carbon by using clear water at the temperature of 100 ℃ after stirring, and performing solid-liquid separation; dispersing the activated carbon after solid-liquid separation into clear water at 100 ℃, stirring for 25min, washing the surface of the activated carbon with clear water at 100 ℃, and filtering after washing;
(4) activation of peroxymonosulfate: placing the filtered activated carbon in a stirring tank, adding clear water into the stirring tank to obtain an activated carbon dispersion liquid, stirring and heating to 50 ℃; adding peroxymonosulfate into the activated carbon dispersion liquid for three times on average, wherein 150g of peroxymonosulfate is added into each cubic meter of activated carbon in total, and the regeneration time is 0.5 h;
(5) and (3) drying: filtering the activated carbon, washing the filtered activated carbon with clear water for 2 times, drying the washed activated carbon in a blast drier at 90 ℃, and recovering the adsorption performance of the dried activated carbon to be about 42% of that of new carbon.
In comparative example 1, the adding amount of the peroxymonosulfate is small, so that enough active free radicals can not be generated to attach to the activated carbon to sufficiently remove organic matters; the activation temperature is low, the regeneration rate of the activated carbon is inhibited, meanwhile, the activation time is short, the peroxymonosulfate does not have enough reaction time to be fully activated by heat, so that the conversion rate of the peroxymonosulfate is low, the generation rate of active free radicals is low, and the regeneration rate of the waste activated carbon is reduced.

Claims (9)

1. A regeneration method of activated carbon based on thermally activated peroxymonosulfate is characterized by comprising the following steps: drying activated carbon to be activated, eluting with hot water, reacting the activated carbon with an activating agent in boiling water under the condition of stirring, and finally filtering, cleaning and drying the activated carbon to obtain the regenerated activated carbon.
2. The process for the regeneration of activated carbon based on thermally activated peroxymonosulfate according to claim 1, characterized in that: the activating agent is peroxymonosulfate, and the adding amount of the activating agent is as follows: permonosulfate with the total mass of 200-400 g is added to each cubic meter of activated carbon.
3. The process for the regeneration of activated carbon based on thermally activated peroxymonosulfate according to claim 1, characterized in that: wherein, the heating temperature is heating to boiling water.
4. The activated carbon regeneration method based on thermally activated peroxymonosulfate as claimed in claim 1, comprising the following steps:
(1) soaking the activated carbon to be activated in clear water, cleaning until the effluent is clear, filtering the washed activated carbon, and naturally drying;
(2) drying the dried active carbon at the drying temperature of 80 +/-10 ℃;
(3) dispersing the dried activated carbon in clear water, heating until the water is boiled, stirring for 20-25 min, washing the activated carbon with boiling hot water after stirring, and performing solid-liquid separation; dispersing the activated carbon subjected to solid-liquid separation in boiling hot water, stirring for 20-25 min, washing the surface of the activated carbon with the boiling hot water, and performing solid-liquid separation again;
(4) dispersing the filtered activated carbon in clear water, stirring and heating until the water is boiled, and adding peroxymonosulfate into the activated carbon dispersion liquid, wherein the adding amount of the peroxymonosulfate is 200-400 g/m3Activated carbon;
(5) and filtering the activated carbon, washing the activated carbon for 2-3 times by using clear water after filtering, and drying the activated carbon after washing.
5. The process for the regeneration of activated carbon based on thermally activated peroxymonosulfate according to claim 4, characterized in that: and (2) naturally airing until the water content of the activated carbon is not higher than 45 percent in the step (1).
6. The process for the regeneration of activated carbon based on thermally activated peroxymonosulfate according to claim 4, characterized in that: in the step (2), drying is carried out until the water content of the activated carbon is less than 8%.
7. The process for the regeneration of activated carbon based on thermally activated peroxymonosulfate according to claim 4, characterized in that: in the step (4), the mixing mass ratio of the activated carbon to the clear water is 1: 1.
8. the process for the regeneration of activated carbon based on thermally activated peroxymonosulfate according to claim 4, characterized in that: in the step (4), the peroxymonosulfate is added into the activated carbon dispersion liquid for 1-2 hours in 3 times on average.
9. The process for the regeneration of activated carbon based on thermally activated peroxymonosulfate according to claim 4, characterized in that: in the step (5), the drying temperature is 80 +/-10 ℃.
CN202110916795.0A 2021-08-11 2021-08-11 Activated carbon regeneration method based on thermally activated peroxymonosulfate Pending CN113713762A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4299805A (en) * 1978-03-30 1981-11-10 Calgon Corporation Regeneration of carbon employed in the wet process production of phosphoric acid
CN103203227A (en) * 2013-04-12 2013-07-17 复旦大学 Method for absorbing saturated active carbon by in situ regeneration of peroxysulphate
US20170113202A1 (en) * 2015-10-22 2017-04-27 King Fahd University Of Petroleum And Minerals Modified activated carbon preparation and methods thereof
CN111318254A (en) * 2020-02-17 2020-06-23 吉林农业大学 Preparation method of high-efficiency regenerated activated carbon

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4299805A (en) * 1978-03-30 1981-11-10 Calgon Corporation Regeneration of carbon employed in the wet process production of phosphoric acid
CN103203227A (en) * 2013-04-12 2013-07-17 复旦大学 Method for absorbing saturated active carbon by in situ regeneration of peroxysulphate
US20170113202A1 (en) * 2015-10-22 2017-04-27 King Fahd University Of Petroleum And Minerals Modified activated carbon preparation and methods thereof
CN111318254A (en) * 2020-02-17 2020-06-23 吉林农业大学 Preparation method of high-efficiency regenerated activated carbon

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
李朝略等: "《化工小商品生产法》", 30 November 1985, 湖南科学技术出版社 *
谭德俊等: ""基于硫酸根自由基的高级氧化技术原位再生活性炭"", 《东华大学学报》 *
陈红英等: "载亚甲基蓝改性活性炭再生的试验研究", 《浙江工业大学学报》 *

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