CN109464997B - Preparation method of medium-large pore diameter activated carbon - Google Patents
Preparation method of medium-large pore diameter activated carbon Download PDFInfo
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- CN109464997B CN109464997B CN201811212977.4A CN201811212977A CN109464997B CN 109464997 B CN109464997 B CN 109464997B CN 201811212977 A CN201811212977 A CN 201811212977A CN 109464997 B CN109464997 B CN 109464997B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28078—Pore diameter
- B01J20/28085—Pore diameter being more than 50 nm, i.e. macropores
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01J20/02—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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/354—After-treatment
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Abstract
The invention relates to a preparation method of medium and large aperture active carbon, which relates to the technical field of active carbon processing and manufacturing; putting the activated carbon to be modified and distilled water into a stainless steel pot together for boiling; the cleaned active carbon is sent into a drying box to be dried to constant weight; naturally cooling the activated carbon dried to constant weight to room temperature, and then flatly paving the activated carbon on a processing frame; then erecting the treatment frame with the active carbon in the container, soaking for 3-10 hours, and then moving the treatment frame out of the container with the oxidant; cleaning, and drying in a drying oven to constant weight; turning the activated carbon and the treatment frame for 180 degrees, erecting the whole in a container filled with a reducing agent, and soaking for 3-10 hours; the processing frame and the active carbon are put into a container filled with deionized water for cleaning and then naturally cooled to a constant temperature. The method can improve the content of acid groups and the content of alkaline groups of the same batch of activated carbon, so that the method can be applied to different adsorption conditions, the application range of the method is greatly increased, and the practicability is higher.
Description
Technical Field
The invention relates to the technical field of processing and manufacturing of activated carbon, in particular to a preparation method of medium and large aperture activated carbon.
Background
The active carbon is a black porous solid carbon, and is produced by crushing and molding coal or carbonizing and activating uniform coal particles. The main component is carbon and contains a small amount of elements such as oxygen, hydrogen, sulfur, nitrogen, chlorine and the like. The specific surface area of the common activated carbon is 500-1700 m2Between/g. Has strong adsorption performance and is an industrial adsorbent with wide application.
The modification of the activated carbon means that the surface functional groups are increased by changing the properties of the activated carbon through alkali treatment or acid treatment and the like so that the modified activated carbon has certain catalytic properties, and the modified activated carbon is mainly used for changing the pore structure and the surface acid-base property of the modified activated carbon in the field of special purposes or high-value products through physical and chemical treatment, or introducing or removing certain functional groups on the surface of the modified activated carbon so that the activated carbon has special adsorption performance and catalytic properties.
The active carbon is modified, so that the adsorption capacity of the active carbon can be greatly improved. At present, for the modification of the activated carbon in the same batch, only one way of modification can be adopted, for example, if the content of the acid group is to be increased, an oxidant is required to be added for surface oxidation treatment, and the activated carbon after surface oxidation treatment has the possibility of losing the content of the acid group if the content of the basic group is to be increased, so that the application range is limited undoubtedly, and improvement is needed urgently.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention provides the preparation method of the medium-large aperture activated carbon, which has the advantages of simple structure, reasonable design and convenient use, and can improve the acid group content and the alkaline group content of the activated carbon in the same batch, so that the preparation method can be applied to different adsorption conditions, the application range of the activated carbon is greatly increased, and the practicability is stronger.
In order to achieve the purpose, the invention adopts the technical scheme that: the operation steps are as follows:
firstly, putting activated carbon to be modified and distilled water into a stainless steel pot together for boiling, and repeatedly cleaning for a plurality of times by using the distilled water;
secondly, the cleaned active carbon is sent into a drying oven to be dried to constant weight;
naturally cooling the dried activated carbon to constant weight to room temperature, and then flatly paving the activated carbon on a processing frame to enable each activated carbon to be embedded in an opening of the processing frame;
adding an oxidant into the container, placing the container on an operation platform and horizontally placing the container, erecting the treatment frame with the active carbon placed in the container, enabling the liquid level of the oxidant to be in contact with the lower surface of the treatment frame, soaking the active carbon positioned at the lower part of the treatment frame in the oxidant, and moving the treatment frame out of the container with the oxidant after soaking for 3-10 hours;
fifthly, putting the processing frame removed in the fourth step and the active carbon into a container filled with deionized water for cleaning, sending the cleaned processing frame and the active carbon into a drying oven for drying until the weight is constant, and naturally cooling to room temperature;
sixthly, turning the cooled active carbon and the treatment frame together for 180 degrees, erecting the whole in a container filled with a reducing agent, enabling the liquid level of the reducing agent to be in contact with the bottom surface of the treatment frame, soaking the untreated active carbon positioned at the lower part of the treatment frame in the reducing agent, and removing the treatment frame out of the container filled with the reducing agent after soaking for 3-10 hours;
seventhly, putting the processing frame removed in the sixth step and the active carbon into a container filled with deionized water for cleaning, sending the cleaned processing frame and the active carbon into a drying oven for drying until the weight is constant, and naturally cooling to a constant temperature;
and eighthly, taking the cooled activated carbon out of the opening of the processing frame.
Further, the drying temperature of the drying oven in the second step is 60-100 ℃.
Further, the drying temperature of the drying oven in the fifth step is 80-120 ℃.
Further, the drying temperature of the drying oven in the seventh step is 80-120 ℃.
Further, in the fourth step, when the activated carbon is soaked in the oxidant, the container filled with the oxidant is heated, so that the temperature of the oxidant in the container is 30-50 ℃.
Further, in the sixth step, when the activated carbon is soaked in the reducing agent, the container filled with the reducing agent is heated, so that the temperature of the reducing agent in the container is 30-50 ℃.
Further, the oxidant is HNO3、HClO、H2SO4One or more of them.
Further, the reducing agent is NO3·H2O。
Furthermore, the processing frame is a toughened glass plate, a plurality of openings are formed in the processing frame, and the aperture of each opening is equal to the particle size of the activated carbon.
After the process is adopted, the invention has the beneficial effects that: the preparation method of the medium and large aperture active carbon can improve the acid group content and the alkaline group content of the same batch of active carbon, so that the active carbon can be applied to different adsorption conditions, the application range of the active carbon is greatly increased, the practicability is higher, and the preparation method has the advantages of simple structure, reasonable arrangement, low manufacturing cost and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic diagram of the processing framework of the present invention in step four.
Description of reference numerals:
container 1, processing frame 2, opening 2-1, active carbon 3.
Detailed Description
The invention will be further described with reference to the accompanying drawings.
Referring to fig. 1, the technical solution adopted in the present embodiment (example one) is: the operation steps are as follows:
firstly, putting the activated carbon 3 to be modified and distilled water into a stainless steel pot together for boiling, and then repeatedly cleaning for a plurality of times by using the distilled water;
secondly, the cleaned active carbon 3 is sent into a drying oven to be dried to constant weight, and the drying temperature is 90 ℃;
naturally cooling the dried activated carbon 3 with constant weight to room temperature, and then flatly paving the dried activated carbon on a processing frame 2 (circular), so that each activated carbon is embedded in an opening 2-1 of the processing frame;
fourthly, adding an oxidant (HNO) into the container 1 (a beaker with a large caliber)3) The container is placed on an operation platform and is placed horizontally, then the treatment frame 2 with the active carbon 3 placed is erected in the container 1, the liquid level of an oxidant is enabled to be in contact with the lower surface of the treatment frame 2, the active carbon 3 located at the lower portion of the treatment frame 2 is soaked in the oxidant at the moment, the container 1 with the oxidant is heated by an alcohol burner, the temperature of the oxidant in the container is enabled to be 50 ℃, and after the container is soaked for 5 hours, the treatment frame 2 is moved out of the container 1 with the oxidant;
fifthly, putting the processing frame 2 removed in the fourth step and the active carbon 3 into a container 1 (a large-caliber beaker) filled with deionized water for cleaning, then sending the cleaned processing frame and the active carbon into a drying box for drying to constant weight, wherein the drying temperature is 100 ℃, and then naturally cooling to room temperature;
sixthly, turning over the activated carbon 3 cooled in the step five together with the treatment frame 2 by 180 degrees, and erecting the whole body in a frame filled with a reducing agent (NO)3·H2O) in the container 1 (large-diameter beaker), the liquid level of the reducing agent is brought into contact with the bottom surface of the processing frame 2, the untreated activated carbon 3 located at the lower part of the processing frame 2 is immersed in the reducing agent, the container 1 containing the reducing agent is heated by an alcohol lamp so that the temperature of the reducing agent therein is 50 ℃, and after the immersion for 5 hours, the processing frame 2 is removed from the container containing the reducing agent;
seventhly, putting the processing frame 2 removed in the sixth step and the active carbon 3 into a container 1 (a large-caliber beaker) filled with deionized water for cleaning, then sending the cleaned processing frame and the active carbon into a drying box for drying to constant weight, wherein the drying temperature is 100 ℃, and then naturally cooling to a constant temperature;
eighthly, taking the cooled activated carbon out of the opening 2-1 of the processing frame 2.
Furthermore, the processing frame is a round toughened glass plate, a plurality of openings are formed in the processing frame, and the aperture of each opening is equal to the particle size of the activated carbon.
After the process is adopted, the specific embodiment has the beneficial effects that: the preparation method of the medium-and large-aperture activated carbon can improve the content of acid groups and the content of alkaline groups of the same batch of activated carbon, so that the activated carbon can be applied to different adsorption conditions, the application range of the activated carbon is greatly increased, and the preparation method has stronger practicability.
Example two:
the technical scheme adopted by the embodiment is as follows: the operation steps are as follows:
firstly, putting the activated carbon 3 to be modified and distilled water into a stainless steel pot together for boiling, and then repeatedly cleaning for a plurality of times by using the distilled water;
secondly, the cleaned active carbon 3 is sent into a drying oven to be dried to constant weight, and the drying temperature is 100 ℃;
naturally cooling the dried activated carbon 3 with constant weight to room temperature, and then flatly paving the dried activated carbon 3 on a processing frame 2 (circular), so that each activated carbon 3 is embedded in an opening 2-1 of the processing frame 2;
fourthly, adding oxidants (HClO, H) into the container 1 (beaker with large caliber)2SO4The container is placed on the operation platform and is placed horizontally, the treatment frame 2 with the active carbon 3 placed is erected in the container 1, the liquid level of the oxidant is in contact with the lower surface of the treatment frame 2, the active carbon 3 positioned at the lower part of the treatment frame 2 is soaked in the oxidant, the container 1 with the oxidant is heated by an alcohol lamp, the temperature of the oxidant in the container is 45 ℃, and after the container is soaked for 10 hours, the treatment frame 2 is moved out of the container 1 with the oxidant;
fifthly, putting the processing frame 2 removed in the fourth step and the active carbon 3 into a container 1 (a large-caliber beaker) filled with deionized water for cleaning, then sending the cleaned processing frame and the active carbon into a drying oven for drying to constant weight, wherein the drying temperature is 80 ℃, and then naturally cooling to room temperature;
sixthly, turning over the activated carbon 2 cooled in the step five together with the processing frame 2Rotated 180 degrees and the whole is arranged and provided with a reducing agent (NO)3·H2O) in the container 1 (large-caliber beaker) so that the liquid level of the reducing agent is in contact with the bottom surface of the processing frame 2, the untreated activated carbon 3 located at the lower portion of the processing frame 2 is immersed in the reducing agent, and after 10 hours of immersion, the processing frame 2 is removed from the container 1 containing the reducing agent;
seventhly, putting the processing frame 2 removed in the sixth step and the active carbon 3 into a container 1 (a large-caliber beaker) filled with deionized water for cleaning, then sending the cleaned processing frame and the active carbon into a drying box for drying to constant weight, wherein the drying temperature is 80 ℃, and then naturally cooling to constant temperature;
eighthly, taking the cooled activated carbon 3 out of the opening 2-1 of the processing frame 2.
The above description is only for the purpose of illustrating the technical solutions of the present invention and not for the purpose of limiting the same, and other modifications or equivalent substitutions made by those skilled in the art to the technical solutions of the present invention should be covered within the scope of the claims of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (1)
1. A preparation method of medium and large pore diameter activated carbon is characterized by comprising the following steps: the operation steps are as follows:
putting activated carbon to be modified and distilled water into a stainless steel pot together for boiling, and repeatedly cleaning for several times by using the distilled water;
secondly, the cleaned active carbon is sent into a drying oven to be dried to constant weight, and the drying temperature of the drying oven is 60-100 ℃;
naturally cooling the dried activated carbon to constant weight to room temperature, and then flatly paving the activated carbon on a processing frame to enable each activated carbon to be embedded in an opening of the processing frame;
(IV) adding an oxidizing agent into the container, wherein the oxidizing agent is HNO3、HClO、H2SO4Is placed on the operation platform and is horizontally placed, then the treatment frame in which the active carbon is placed is erected in the container, so that the liquid level of the oxidant and the treatment frame are mixedThe lower surfaces are contacted, the activated carbon positioned at the lower part of the processing frame is soaked in an oxidant, when the activated carbon is soaked in the oxidant, the container filled with the oxidant is heated, the temperature of the oxidant in the container is 30-50 ℃, and after the container is soaked for 3-10 hours, the processing frame is moved out of the container filled with the oxidant;
fifthly, putting the processing frame removed in the step (IV) and the activated carbon into a container filled with deionized water for cleaning, sending the cleaned processing frame and the activated carbon into a drying oven for drying until the weight is constant, and naturally cooling to room temperature, wherein the drying temperature of the drying oven is 80-120 ℃;
turning the cooled active carbon in the step (five) and the treatment frame by 180 degrees, erecting the whole body in a container filled with a reducing agent, enabling the liquid level of the reducing agent to be in contact with the bottom surface of the treatment frame, soaking untreated active carbon positioned at the lower part of the treatment frame in the reducing agent, wherein the treatment frame is a toughened glass plate, a plurality of openings are formed in the toughened glass plate, the aperture of each opening is equal to the particle size of the active carbon, heating the container filled with the reducing agent when the active carbon is soaked in the reducing agent, enabling the temperature of the reducing agent in the container to be 30-50 ℃, and removing the treatment frame out of the container filled with the reducing agent after soaking for 3-10 hours;
seventhly, putting the processing frame removed in the step six and the activated carbon into a container filled with deionized water for cleaning, conveying the cleaned processing frame into a drying box for drying until the weight is constant, wherein the drying temperature of the drying box is 80-120 ℃, and naturally cooling to a constant temperature;
and (eighthly), taking the cooled activated carbon out of the opening of the processing frame.
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| CN201811212977.4A CN109464997B (en) | 2018-10-18 | 2018-10-18 | Preparation method of medium-large pore diameter activated carbon |
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| CN201811212977.4A CN109464997B (en) | 2018-10-18 | 2018-10-18 | Preparation method of medium-large pore diameter activated carbon |
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Citations (6)
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|---|---|---|---|---|
| CA2030369A1 (en) * | 1989-11-22 | 1991-05-23 | Calgon Carbon Corporation | Product/process/application for removal of mercury from liquid hydrocarbon |
| CN202620307U (en) * | 2011-11-14 | 2012-12-26 | 大理学院 | Acid-base modified activated carbon three-layer composite bolt type device |
| CN103506077A (en) * | 2013-09-30 | 2014-01-15 | 中国科学技术大学 | Preparation method of modified biochar |
| CN104339213A (en) * | 2013-08-08 | 2015-02-11 | 洛阳双兴电气科技有限公司 | Overturning fixture for machining |
| CN107189072A (en) * | 2016-06-02 | 2017-09-22 | 中国科学院化学研究所 | Janus rod-like nano materials and preparation method thereof |
| CN109364881A (en) * | 2018-12-13 | 2019-02-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of feeble-acid-ammonium salt modified activated carbon and products thereof and application |
-
2018
- 2018-10-18 CN CN201811212977.4A patent/CN109464997B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2030369A1 (en) * | 1989-11-22 | 1991-05-23 | Calgon Carbon Corporation | Product/process/application for removal of mercury from liquid hydrocarbon |
| CN202620307U (en) * | 2011-11-14 | 2012-12-26 | 大理学院 | Acid-base modified activated carbon three-layer composite bolt type device |
| CN104339213A (en) * | 2013-08-08 | 2015-02-11 | 洛阳双兴电气科技有限公司 | Overturning fixture for machining |
| CN103506077A (en) * | 2013-09-30 | 2014-01-15 | 中国科学技术大学 | Preparation method of modified biochar |
| CN107189072A (en) * | 2016-06-02 | 2017-09-22 | 中国科学院化学研究所 | Janus rod-like nano materials and preparation method thereof |
| CN109364881A (en) * | 2018-12-13 | 2019-02-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of feeble-acid-ammonium salt modified activated carbon and products thereof and application |
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| Title |
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| "还原和氧化改性活性炭对亚甲基蓝吸附性能的影响";骆红超等;《化工新型材料》;20130131;第41卷(第1期);第76-79页 * |
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