CN115212843A - Preparation method and application of doped modified activated carbon loaded with metal oxide - Google Patents
Preparation method and application of doped modified activated carbon loaded with metal oxide Download PDFInfo
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- CN115212843A CN115212843A CN202210855267.3A CN202210855267A CN115212843A CN 115212843 A CN115212843 A CN 115212843A CN 202210855267 A CN202210855267 A CN 202210855267A CN 115212843 A CN115212843 A CN 115212843A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/102—Carbon
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention discloses a preparation method of doped modified activated carbon loaded with metal oxide, which comprises the following steps: a, step a: processing raw materials; step b: preparing a solution A; step c: preparing a solution B; step d: preparing solution C and solution D; step e: preparing doped modified active carbon; step f: and (3) preparing the doped modified activated carbon loaded with metal oxide. The invention provides a preparation method of doped modified activated carbon loaded with metal oxide, and the design of the method is adopted, so that the arranged doped modified activated carbon loaded with metal oxide has a good adsorption effect on heavy metal ions in wastewater, and in addition, the doped modified activated carbon loaded with metal oxide can also be used for purifying indoor air, and has wide application.
Description
Technical Field
The invention belongs to the technical field of activated carbon preparation, and particularly relates to a preparation method and application of doped modified activated carbon loaded with metal oxide.
Background
With the rapid development of the economic society, the urbanization progress is accelerated, the heavy metal industry develops rapidly, and with the rapid development of the industries, a large amount of heavy metals enter water and atmosphere, so that the health of people is seriously affected. The adsorption by using activated carbon is a common method in wastewater treatment. The common activated carbon has poor adsorption on heavy metal ions such as copper, chromium and the like in wastewater treatment.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a preparation method of doped modified activated carbon loaded with metal oxide.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
a preparation method of doped modified activated carbon loaded with metal oxide comprises the following steps:
step a: treatment of raw materials
Weighing a certain amount of animal hair, placing the animal hair in a clean water tank for repeated cleaning, wherein the cleaning frequency is 3 times, placing the cleaned animal hair in a first reactor after cleaning, and adding ammonia water into a first reaction container, wherein the mass ratio of the animal hair to the ammonia water is 1:10, heating the first reactor to 120 ℃, carrying out heat preservation reaction for 2 hours to obtain a pyrolysis product, and carrying out nitric acid modification on the pyrolysis product to obtain a second sample;
step b: preparation of solution A
Measuring a certain amount of tetrabutyl titanate in a reactor, stirring at the stirring speed of 300r/min, and dropwise adding a certain amount of absolute ethyl alcohol into the reactor in the stirring process, wherein the volume ratio of the tetrabutyl titanate to the absolute ethyl alcohol is 1: and 10, after the dropwise addition is finished, continuously stirring for 30min to obtain a first mixed solution, and adding a certain amount of acetylacetone into the first mixed solution to prepare a solution A, wherein the volume ratio of the acetylacetone to the tetrabutyl titanate is 1:5;
step c: preparation of solution B
Measuring a certain amount of concentrated nitric acid, adding the concentrated nitric acid into a container containing absolute ethyl alcohol, and adding deionized water into the container, wherein the volume ratio of the concentrated nitric acid to the absolute ethyl alcohol to the deionized water is 1:5: and 5, after uniformly stirring, obtaining a second mixed solution, adding ammonium chloride into the second mixed solution, stirring and dissolving, and moving into a first funnel to obtain a solution B, wherein the molar ratio of the ammonium chloride to the tetrabutyl titanate is 1:20;
step d: preparation of solutions C and D
Measuring a certain amount of 0.1mol/L boric acid solution, placing the boric acid solution in a second funnel to obtain solution C, and measuring a certain amount of 0.1mol/L lanthanum nitrate solution, placing the lanthanum nitrate solution in a third funnel to obtain solution D;
step e: preparation of doped modified activated carbon
Stirring the solution A at a stirring speed of 300r/min, dropwise adding the solution B, the solution C and the solution D into the solution A in the stirring process, continuously stirring for 2 hours after dropwise adding is completed to obtain a composite solution, adding a second sample into the composite solution for immersion treatment to obtain a composite product, ultrasonically immersing the composite product, setting the ultrasonic power to be 800W and the ultrasonic time to be 2 hours, standing and placing for 12 hours after the ultrasonic immersion is completed to obtain a product to be dried, drying the product to be dried in an oven, setting the drying temperature to be 80 ℃ and the drying time to be 24 hours to obtain a dried product, placing the dried product in a muffle furnace, heating to 250 ℃ for heat treatment, setting the heating rate to be 3 ℃/min and the heat treatment time to be 4 hours, and obtaining doped modified activated carbon after the heat treatment is completed;
step f: preparation of doped modified active carbon loaded with metal oxide
Weighing a certain amount of doped modified activated carbon in a crucible, weighing a certain amount of 0.5mol/L Cu (NO 3) 2 solution and 0.5mol/L NiNO3 solution, pouring the solutions into the crucible to impregnate the doped modified activated carbon for 30min, after the impregnation is finished, placing the impregnated doped modified activated carbon in a constant-temperature water bath to adsorb for 24h, setting the water bath temperature to be 40 ℃, filtering after the adsorption, drying after the filtration, placing the dried doped modified activated carbon in a muffle furnace to calcine for 2h, setting the calcining temperature to be 400 ℃, and cooling to obtain the doped modified activated carbon loaded with metal oxide.
Further, the specific operation flow of the nitric acid modification is as follows: crushing the dried pyrolysis product, sieving the crushed pyrolysis product by a 80-mesh sieve to obtain a first raw material, mixing a certain amount of the first raw material with 70% nitric acid solution, wherein the addition amount of the 70% nitric acid solution is 2mL in every 1g of the first raw material, placing the mixture under the condition of 80 ℃ water bath for refluxing for 2h to obtain a first sample, cleaning the first sample by using deionized water, placing the washed first sample in a 120 ℃ drying oven for drying, setting the drying time to be 3h, placing the dried first sample in a muffle furnace for activation after drying, wherein the activation temperature is 400 ℃, the activation time is 2h, and cooling the activated first sample to room temperature to obtain a second sample.
Further, in the step e, in the doped modified activated carbon, the ratio of Ti: b: the ratio of La is 1:0.05:0.01.
furthermore, in step f, the addition amount of 0.5mol/L Cu (NO 3) 2 solution and 0.5mol/L NiNO3 solution is 5mL per 1g of the doped modified activated carbon.
The doped modified activated carbon loaded with the metal oxide is prepared by the method.
The application of the doped modified activated carbon loaded with the metal oxide in wastewater treatment is provided.
The invention has the beneficial effects that:
the invention provides a preparation method of doped modified activated carbon loaded with metal oxide, and the design of the method is adopted, so that the arranged doped modified activated carbon loaded with metal oxide has a good adsorption effect on heavy metal ions in wastewater, and in addition, the doped modified activated carbon loaded with metal oxide can also be used for purifying indoor air, and has wide application.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the invention without limiting the invention. In the drawings:
fig. 1 is a flow chart of a preparation method of a metal oxide-loaded doped modified activated carbon provided by the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of a metal oxide-loaded doping modified activated carbon as shown in figure 1, which comprises the following steps:
a, step a: treatment of raw materials
Weighing a certain amount of animal hair, placing the animal hair in a clean water tank for repeated cleaning, wherein the cleaning frequency is 3 times, placing the cleaned animal hair in a first reactor after cleaning, and adding ammonia water into a first reaction container, wherein the mass ratio of the animal hair to the ammonia water is 1:10, heating the first reactor to 120 ℃, carrying out heat preservation reaction for 2 hours to obtain a pyrolysis product, and carrying out nitric acid modification on the pyrolysis product to obtain a second sample;
the specific operation flow of the nitric acid modification comprises the following steps: crushing the dried pyrolysis product, sieving with a 80-mesh sieve to obtain a first raw material, mixing a certain amount of the first raw material with 70% nitric acid solution, wherein the addition amount of the 70% nitric acid solution is 2mL in every 1g of the first raw material, placing the mixture under a 80 ℃ water bath condition for refluxing for 2 hours after mixing to obtain a first sample, cleaning the first sample by using deionized water, placing the washed first sample in a 120 ℃ drying oven for drying, setting the drying time to be 3 hours, placing the dried first sample in a muffle furnace for activation after drying, wherein the activation temperature is 400 ℃, the activation time is 2 hours, and cooling the activated first sample to room temperature to obtain a second sample;
in the step, biochar prepared from animal hair is modified to obtain a modified second sample;
step b: preparation of solution A
Measuring a certain amount of tetrabutyl titanate in a reactor, stirring at the stirring speed of 300r/min, and dropwise adding a certain amount of absolute ethyl alcohol into the reactor in the stirring process, wherein the volume ratio of the tetrabutyl titanate to the absolute ethyl alcohol is 1: and 10, after the dropwise addition is finished, continuously stirring for 30min to obtain a first mixed solution, adding a certain amount of acetylacetone into the first mixed solution to prepare a solution A, wherein the volume ratio of the acetylacetone to the tetrabutyl titanate is 1:5;
step c: preparation of solution B
Measuring a certain amount of concentrated nitric acid, adding the concentrated nitric acid into a container containing absolute ethyl alcohol, and adding deionized water into the container, wherein the volume ratio of the concentrated nitric acid to the absolute ethyl alcohol to the deionized water is 1:5: and 5, after uniform stirring, obtaining a second mixed solution, adding ammonium chloride into the second mixed solution, stirring and dissolving, moving into a first funnel, and obtaining a solution B, wherein the molar ratio of the ammonium chloride to the tetrabutyl titanate is 1:20;
step d: preparation of solutions C and D
Measuring a certain amount of 0.1mol/L boric acid solution, placing the boric acid solution in a second funnel to obtain solution C, and measuring a certain amount of 0.1mol/L lanthanum nitrate solution, placing the lanthanum nitrate solution in a third funnel to obtain solution D;
step e: preparation of doped modified active carbon
Stirring the solution A at a stirring speed of 300r/min, dropwise adding the solution B, the solution C and the solution D into the solution A in the stirring process, continuously stirring for 2h after dropwise adding is completed to obtain a composite solution, adding a second sample into the composite solution for impregnation treatment to obtain a composite product, ultrasonically impregnating the composite product, setting the ultrasonic power to be 800W and the ultrasonic time to be 2h, standing and placing for 12h after the ultrasonic impregnation is completed to obtain a product to be dried, drying the product to be dried in an oven, setting the drying temperature to be 80 ℃ and the drying time to be 24h to obtain a dried product, placing the dried product in a muffle furnace, heating to 250 ℃ for heat treatment, setting the heating rate to be 3 ℃/min and the heat treatment time to be 4h, and obtaining doped modified activated carbon after the heat treatment is completed;
wherein, in the doped modified active carbon, ti: b: the ratio of La is 1:0.05:0.01;
in the step, modified titanium dioxide is obtained through the liquid B, the liquid C and the liquid D, in the process of preparing the titanium dioxide, when gel is formed, a second sample is added, and then titanium-loaded active carbon, namely doped modified active carbon, can be obtained, and the doped modified active carbon loaded with metal oxides has a certain effect in the aspect of indoor air purification based on the photocatalytic oxidation mechanism of the titanium dioxide;
step f: preparation of doped modified active carbon loaded with metal oxide
Weighing a certain amount of doped modified activated carbon in a crucible, and weighing a certain amount of 0.5mol/L Cu (NO) 3 ) 2 Solution and 0.5mol/L NiNO 3 Pouring the solution into a crucible to impregnate the doped modified activated carbon for 30min, after the impregnation is finished, placing the impregnated doped modified activated carbon in a constant-temperature water bath condition to adsorb for 24h, setting the water bath temperature to be 40 ℃, filtering after the adsorption, drying after the filtration, placing the dried doped modified activated carbon in a muffle furnace to calcine for 2h, setting the calcining temperature to be 400 ℃, and cooling to obtain the doped modified activated carbon loaded with metal oxide;
wherein, every 1g of the modified activated carbon is doped with 0.5mol/L of Cu (NO) 3 ) 2 Solution and 0.5mol/L NiNO 3 The amount of the solution added was 5mL.
Example 2
An application of doped modified active carbon loaded with metal oxide in wastewater treatment.
The invention provides a preparation method of doped modified activated carbon loaded with metal oxide, and the design of the method is adopted, so that the arranged doped modified activated carbon loaded with metal oxide has a good adsorption effect on heavy metal ions in wastewater, and in addition, the doped modified activated carbon loaded with metal oxide can also be used for purifying indoor air, and has wide application.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are given by way of illustration of the principles of the present invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, and such changes and modifications are within the scope of the invention as claimed.
Claims (6)
1. A preparation method of doped modified activated carbon loaded with metal oxide is characterized by comprising the following steps: the method comprises the following steps:
step a: treatment of raw materials
Weighing a certain amount of animal hair, placing the animal hair in a clean water tank for repeated cleaning, wherein the cleaning frequency is 3 times, placing the cleaned animal hair in a first reactor after cleaning, and adding ammonia water into a first reaction container, wherein the mass ratio of the animal hair to the ammonia water is 1:10, heating the first reactor to 120 ℃, carrying out heat preservation reaction for 2 hours to obtain a pyrolysis product, and carrying out nitric acid modification on the pyrolysis product to obtain a second sample;
step b: preparation of solution A
Measuring a certain amount of tetrabutyl titanate, stirring in a reactor at a stirring speed of 300r/min, and dropwise adding a certain amount of absolute ethyl alcohol into the reactor in the stirring process, wherein the volume ratio of the tetrabutyl titanate to the absolute ethyl alcohol is 1: and 10, after the dropwise addition is finished, continuously stirring for 30min to obtain a first mixed solution, and adding a certain amount of acetylacetone into the first mixed solution to prepare a solution A, wherein the volume ratio of the acetylacetone to the tetrabutyl titanate is 1:5;
step c: preparation of solution B
Measuring a certain amount of concentrated nitric acid, adding the concentrated nitric acid into a container containing absolute ethyl alcohol, and adding deionized water into the container, wherein the volume ratio of the concentrated nitric acid to the absolute ethyl alcohol to the deionized water is 1:5: and 5, after uniformly stirring, obtaining a second mixed solution, adding ammonium chloride into the second mixed solution, stirring and dissolving, and then moving into a first funnel to obtain a solution B, wherein the molar ratio of the ammonium chloride to the tetrabutyl titanate is 1:20;
step d: preparation of solutions C and D
Measuring a certain amount of 0.1mol/L boric acid solution, placing the boric acid solution in a second funnel to obtain a solution C, measuring a certain amount of 0.1mol/L lanthanum nitrate solution, placing the lanthanum nitrate solution in a third funnel to obtain a solution D;
step e: preparation of doped modified active carbon
Stirring the solution A at a stirring speed of 300r/min, dropwise adding the solution B, the solution C and the solution D into the solution A in the stirring process, continuously stirring for 2 hours after dropwise adding is completed to obtain a composite solution, adding a second sample into the composite solution for immersion treatment to obtain a composite product, ultrasonically immersing the composite product, setting the ultrasonic power to be 800W and the ultrasonic time to be 2 hours, standing and placing for 12 hours after the ultrasonic immersion is completed to obtain a product to be dried, drying the product to be dried in an oven, setting the drying temperature to be 80 ℃ and the drying time to be 24 hours to obtain a dried product, placing the dried product in a muffle furnace, heating to 250 ℃ for heat treatment, setting the heating rate to be 3 ℃/min and the heat treatment time to be 4 hours, and obtaining doped modified activated carbon after the heat treatment is completed;
step f: preparation of doped modified active carbon loaded with metal oxide
Weighing a certain amount of doped modified activated carbon in a crucible, and weighing a certain amount of 0.5mol/L Cu (NO) 3 ) 2 Solution and 0.5mol/L NiNO 3 Pouring the solution into a crucible to impregnate the doped modified activated carbon for 30min, after the impregnation is finished, placing the impregnated doped modified activated carbon in a constant-temperature water bath for adsorption for 24h, setting the water bath temperature to be 40 ℃, filtering after the adsorption, and filteringAnd drying, namely placing the dried doped modified activated carbon in a muffle furnace to calcine for 2 hours at the calcining temperature of 400 ℃, and cooling to obtain the doped modified activated carbon loaded with the metal oxide.
2. The preparation method of the metal oxide-loaded doping modified activated carbon according to claim 1, characterized in that: the specific operation flow of the nitric acid modification is as follows: crushing the dried pyrolysis product, sieving the crushed pyrolysis product with a 80-mesh sieve to obtain a first raw material, mixing a certain amount of the first raw material with 70% nitric acid solution, wherein the addition amount of the 70% nitric acid solution is 2mL in every 1g of the first raw material, placing the mixture under a water bath condition of 80 ℃ for refluxing for 2h after mixing to obtain a first sample, cleaning the first sample by using deionized water, placing the washed first sample in a 120 ℃ drying oven for drying, setting the drying time to be 3h, placing the dried first sample in a muffle furnace for activation after drying, setting the activation temperature to be 400 ℃ and the activation time to be 2h, and cooling the activated first sample to the room temperature to obtain a second sample.
3. The preparation method of the metal oxide-loaded doping modified activated carbon according to claim 1, characterized in that: in the step e, doping modified activated carbon, wherein Ti: b: the ratio of La is 1:0.05:0.01.
4. the preparation method of the metal oxide-loaded doping modified activated carbon according to claim 1, characterized in that: in step f, 0.5mol/L of Cu (NO) is added into every 1g of the doped modified activated carbon 3 ) 2 Solution and 0.5mol/L NiNO 3 The addition amount of the solution was 5mL.
5. A metal oxide-supporting doped modified activated carbon prepared by the method according to any one of claims 1 to 4.
6. The use of the metal oxide-loaded doped modified activated carbon of claim 5 in wastewater treatment.
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CN113333011A (en) * | 2021-06-01 | 2021-09-03 | 中国科学院过程工程研究所 | Composite catalyst and preparation method and application thereof |
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JPH09192485A (en) * | 1996-01-22 | 1997-07-29 | Kuraray Chem Corp | Activated carbon molded body carrying metal oxide |
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