CN110980732A - Preparation method of kiwi pruning branch-based activated carbon - Google Patents

Preparation method of kiwi pruning branch-based activated carbon Download PDF

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CN110980732A
CN110980732A CN202010000523.1A CN202010000523A CN110980732A CN 110980732 A CN110980732 A CN 110980732A CN 202010000523 A CN202010000523 A CN 202010000523A CN 110980732 A CN110980732 A CN 110980732A
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activated carbon
kiwi
temperature
zinc chloride
speed
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张文林
唐建民
兰建彬
廖钦洪
李哲馨
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Chongqing University of Arts and Sciences
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    • 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
    • C01B32/312Preparation
    • C01B32/342Preparation characterised by non-gaseous activating agents
    • C01B32/348Metallic compounds
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    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/30Active carbon
    • C01B32/312Preparation
    • C01B32/318Preparation characterised by the starting materials
    • 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
    • C01B32/312Preparation
    • C01B32/342Preparation characterised by non-gaseous activating agents
    • 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

Abstract

A preparation method of kiwi pruning branch-based activated carbon is characterized by comprising the following steps: cutting, drying and crushing kiwi fruit pruned branches, then violently stirring the kiwi fruit pruned branches and a mixed solution consisting of zinc chloride, phosphoric acid and water, then performing high-temperature carbonization and activation, then performing modification treatment, and finally performing centrifugal washing and drying; the concentration of the zinc chloride is 50% -90%, the concentration of the phosphoric acid is 70% -85%, and the mixing ratio of the zinc chloride, the phosphoric acid and water is 1-5: 1-10: 30-50. The active carbon prepared based on the kiwi fruit pruning branches has the advantages of large specific surface area, high porosity, uniform pore size distribution and good stability; the method obtains a large number of types of surface functional groups in the pore-forming process, and the acidic functional groups are obviously increased through modification treatment, so that the method has excellent adsorption performance on cationic dyes.

Description

Preparation method of kiwi pruning branch-based activated carbon
Technical Field
The invention relates to the technical field of activated carbon preparation, in particular to a preparation method of kiwi pruning branch-based activated carbon.
Background
Nowadays, resources in China are increasingly tense, and the realization of resource utilization of agricultural wastes is undoubtedly of great practical significance. Chinese gooseberry planting area and yield are the first in the world, and the Chinese gooseberry planting area and yield are the largest production base of the Chinese gooseberries in the world. Meanwhile, the number of waste branches generated by pruning or variety updating is increased every year, and the pruned branches are directly burned or piled by farmers to form agricultural solid wastes, so that huge resource waste and environmental pollution are caused. Therefore, how to reasonably use the kiwi fruit pruning branches, realizing the resource utilization of agricultural wastes, and improving the environment deserves discussion.
The activated carbon has an amorphous structure based on graphite microcrystals, has large specific surface area and porosity, and has strong adsorption force, antimicrobial decomposition capability and oxidation resistance, so that the activated carbon has strong application potential in the fields of activated carbon pollutant adsorption and environmental remediation. With the improvement of the concern of people on environmental protection, the demand of various industries on activated carbon is continuously increased. At present, the raw materials for preparing the activated carbon mainly comprise coal, wood and fruit shells, but the supply price of the activated carbon is high due to the limitation of the raw material sources. Therefore, more and more attention is paid to the development of cheap and easily available activated carbon raw materials and the reduction of the production cost of activated carbon. However, the source and composition of the raw materials of the activated carbon are very different, and the types and the number of the surface functional groups are limited, so that the application of the biochar in the aspect of polluted environment restoration is greatly limited. The active carbon raw material containing more mineral substances and the higher pyrolysis temperature usually destroy the pore diameter structure and the surface functional group structure of the biochar, so that the pore diameter of the active carbon is collapsed, the specific surface area is reduced, and the types and the number of the active functional groups on the surface of the active carbon are limited, thereby being not beneficial to the adsorption of dyes such as methylene blue, crystal violet and the like.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a preparation method of kiwi pruning branch-based activated carbon rich in acidic functional groups.
The purpose of the invention is realized by the following technical scheme:
a preparation method of kiwi pruning branch-based activated carbon is characterized by comprising the following steps: cutting, drying and crushing kiwi pruned branches to obtain kiwi pruned branch powder, then adding the kiwi pruned branch powder into a mixed solution consisting of zinc chloride, phosphoric acid and water, violently stirring, carrying out high-temperature carbonization and activation after centrifugal separation, then carrying out modification treatment, and finally carrying out centrifugal washing and drying; the mass concentration of the zinc chloride is 50% -90%, the mass concentration of the phosphoric acid is 70% -85%, the mixing volume ratio of the zinc chloride to the phosphoric acid to the water is 1-5: 1-10: 30-50, the mass volume ratio of the kiwi fruit pruning branch powder to the mixed liquid is 1g: 20-100 mL.
Further, the pretreatment specifically comprises pruning kiwi fruits, cutting the pruned kiwi fruits into 2-3cm small sections, drying the small sections in a forced air drying oven at 80 ℃ for 2-4 h, then crushing the small sections at 25000 r/min, and sieving the crushed small sections with a 40-80-mesh sieve to obtain kiwi fruit pruned branch powder.
Further, the violent stirring is 1000-1500 revolutions per minute, and the stirring time is 1-2 hours.
Further, the high-temperature carbonization and activation are specifically that the kiwi pruned branch powder after centrifugal separation is heated to 300-400 ℃ at a speed of 5-8 ℃/min under the inert gas atmosphere, and is carbonized for 0.5-1h at constant temperature; then heating to 650 ℃ at the speed of 10-20 ℃/min, and carbonizing for 1-1.5h at constant temperature; then slowly cooling to 400-450 ℃ at the speed of 3-4 ℃/min, keeping the temperature for 30-50min, and then continuously cooling to room temperature at the same speed to obtain the activated carbon coarse body.
Preferably, the high-temperature carbonization and activation specifically comprises the steps of heating the centrifugally separated kiwi fruit pruning branch powder to 350-400 ℃ at a speed of 6 ℃/min in a nitrogen atmosphere, and carbonizing for 45min at a constant temperature; then raising the temperature to 550-600 ℃ at the speed of 15 ℃/min, and keeping the temperature for 1-1.5 h; then slowly cooling to 450 ℃ at the speed of 4 ℃/min, keeping the temperature for 40min, and then continuously cooling to room temperature at the same speed to obtain the activated carbon coarse body.
The inventor finds that phosphoric acid has a weak expansion effect on cellulose in the pruning branches of the kiwi fruits and is difficult to permeate into the kiwi fruits to form pores due to the existence of lignin; the zinc chloride has very strong inflation effect to the cellulose in the kiwi fruit pruning branch, uses the kiwi fruit pruning branch and mixes the back with the mixed aqueous solution of zinc chloride, phosphoric acid for inside the zinc chloride fully got into the raw materials, the preliminary pore-forming of dissolved cellulose, the zinc chloride is to the inflation effect of cellulose and the participation of water simultaneously, provides the condition for the quick infiltration entering cellulose of phosphoric acid.
In the process of heating to 300-400 ℃, zinc chloride enters the inside of the kiwi pruning branches and acts on lignin, so that volatile substances in the lignin are gasified and dehydrogenated, the zinc chloride hydrolyzes cellulose to form pores, the lignocellulose is catalyzed to dehydrate to promote aromatization, the zinc chloride is deposited on a zinc chloride framework, graphite-like microcrystals are formed in the initial step, and the yield of activated carbon is improved; and then, the temperature is further rapidly increased to 650 ℃ at 500-. The zinc chloride has swelling effect on cellulose, and can decompose lignin and participate in water, so that the phosphoric acid can be rapidly diffused into the carbon body. And then slowly cooling to 400-450 ℃, hydrolyzing the residual lignocellulose by phosphoric acid to obtain polysaccharide and monosaccharide with lower relative molecular weight, further uniformly diffusing in the carbon body to form a framework, so that the pore diameter formed by carbon deposition is uniformly distributed to form a larger topological structure staggered graphite microcrystal, and cross-linking the phosphoric acid with high glycan (a general name of cellulose and hemicellulose) and degradation products thereof in the raw material during cooling at a specific speed to form a phosphate ester bond, so that the shrinkage of cell walls after hydrolysis and dehydration of the raw material is prevented, and the prepared activated carbon is ensured to have a developed pore diameter structure. In the whole high-temperature treatment process, the phosphoric acid has the slow oxidation pore-forming effect on the kiwi fruit pruned branches serving as raw materials. The zinc chloride and the phosphoric acid are used for cooperatively forming pores in a specific high-temperature carbonization and activation process, a developed graphite-like microcrystal structure is formed, and the prepared activated carbon is uniform in pore size distribution, various in pore size and developed.
Further, the modification treatment is to oxidize the activated carbon coarse body after high-temperature carbonization and activation for 20-40 min at 55-65 ℃ by using hydrochloric acid with the concentration of 0.2-0.5 mol/L, repeatedly carry out centrifugal washing on the activated carbon coarse body by using distilled water after the oxidation is finished until the activated carbon coarse body is neutral, then carry out heat treatment for 1h, wherein the heat treatment temperature is 160-300 ℃, and then naturally cool the activated carbon coarse body to the room temperature.
It is known in the art that acidic functional groups have cation exchange properties and basic functional groups have anion exchange properties. The inventor finds that the kiwi pruning branch-based activated carbon is modified by hydrochloric acid and then is subjected to heat treatment at a lower temperature, so that the damage to the pore structure of the activated carbon is small, the influence of low-concentration hydrochloric acid on the pore structure of the coarse activated carbon prepared by the method is mainly small, the pore diameter of the activated carbon is relatively reduced through the heat treatment, the influence of the hydrochloric acid on the pore structure is compensated, the change of the whole pore structure of the activated carbon is small, and the cation exchange capacity of the activated carbon is remarkably improved.
Further, the mass volume ratio of the activated carbon coarse body to the hydrochloric acid is 1: 10-20.
Specifically, the preparation method of the kiwi pruning branch-based activated carbon comprises the following steps:
(1) pruning kiwi fruits, cutting into 2-3cm small sections, drying for 2-4 h in a forced air drying oven at 80 ℃, then crushing at 25000 r/min, and sieving with a 40-80 mesh sieve to obtain kiwi fruit pruning branch powder;
(2) adding the kiwi fruit pruned branch powder prepared in the step (1) into a mixed solution composed of zinc chloride, phosphoric acid and water, stirring at the speed of 1000-1500 rpm for 1-2 h, wherein the mass concentration of the zinc chloride is 50-90%, the mass concentration of the phosphoric acid is 70-85%, the mixing ratio of the zinc chloride, the phosphoric acid and the water is 1-5: 1-10: 30-50, and the mass-volume ratio of the kiwi fruit pruned branch powder to the mixed solution is 1g: 20-100 mL;
(3) centrifugally separating the kiwi pruned branch powder from the mixed solution, heating to 300-400 ℃ at the speed of 5-8 ℃/min under the inert gas atmosphere, and carbonizing at constant temperature for 0.5-1 h; then heating to 500-650 ℃ at the speed of 10-20 ℃/min, and keeping the temperature for 1-1.5 h; then slowly cooling to 400-450 ℃ at the speed of 3-4 ℃/min, keeping the temperature for 30-50min, and then continuously cooling to room temperature at the same speed to obtain the activated carbon coarse body;
(4) oxidizing the activated carbon crude body prepared in the step (3) with hydrochloric acid at 55-65 ℃ for 20-40 min, repeatedly performing centrifugal washing on the activated carbon crude body with distilled water after oxidation is completed until the activated carbon crude body is neutral, then performing heat treatment for 1h, wherein the heat treatment temperature is 160-300 ℃, and then naturally cooling to room temperature, the concentration of the hydrochloric acid is 0.2-0.5 mol/L, and the mass volume ratio of the activated carbon crude body to the hydrochloric acid is 1g: 10-20 mL.
Through the synergistic cooperation of the steps, the active carbon with developed pore size and specific surface area and uniform pore size distribution is prepared, and the surface of the active carbon has rich acidic functional groups and excellent adsorption performance on cationic dyes.
The invention has the following beneficial effects:
the active carbon prepared based on kiwi pruned branches has large specific surface area, and the BET specific surface area of the active carbon reaches 1591m2The porosity is high, the pore size distribution is uniform, and the stability is good; according to the invention, a large number of types of surface functional groups are obtained in the pore-forming process, and the acidic functional groups are obviously increased through modification treatment, so that the cationic dye has excellent adsorption performance, such as adsorption capacity of 1010.6mg/g for methylene blue, adsorption capacity of 936.3mg/g for crystal violet, and adsorption capacity of 410.3mg/g for methyl orange; the recycling performance is good, and when the cationic dye is recycled for 20 times, the removal rate of the cationic dye can reach 86.6% of that of the cationic dye used for the first time.
Drawings
FIG. 1: SEM image of activated carbon prepared in example 1 of the present invention.
Detailed Description
The present invention is described in detail below by way of examples, it should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and those skilled in the art can make some insubstantial modifications and adaptations of the present invention based on the above-mentioned disclosure.
Example 1
A preparation method of kiwi pruning branch-based activated carbon comprises the following steps:
(1) pruning kiwi fruits, cutting into 2cm small sections, drying in a forced air drying oven at 80 ℃ for 3h, then crushing at 25000 r/min, and sieving with a 60-mesh sieve to obtain kiwi fruit pruning branch powder;
(2) adding the kiwi fruit pruned branch powder prepared in the step (1) into a mixed solution composed of zinc chloride, phosphoric acid and water, stirring at the speed of 1200 r/min for 1.5h, wherein the mass concentration of the zinc chloride is 80%, the mass concentration of the phosphoric acid is 80%, the mixing ratio of the zinc chloride, the phosphoric acid and the water is 3:7:40, and the mass-volume ratio of the kiwi fruit pruned branch powder to the mixed solution is 1g: 100 mL;
(3) centrifugally separating the kiwi pruned branch powder from the mixed solution, heating to 350 ℃ at the speed of 6 ℃/min under the atmosphere of nitrogen gas, and carbonizing for 45min at constant temperature; then the temperature is raised to 600 ℃ at the speed of 15 ℃/min, and the temperature is kept for 1 h; then slowly cooling to 450 ℃ at the speed of 4 ℃/min, keeping the temperature for 40min, and then continuously cooling to room temperature at the same speed to obtain the activated carbon coarse body;
(4) adding hydrochloric acid into the activated carbon coarse body prepared in the step (3), oxidizing at 60 ℃ for 40min, repeatedly carrying out centrifugal washing on the activated carbon coarse body by using distilled water after the oxidation is finished until the activated carbon coarse body is neutral, then carrying out heat treatment for 1h, wherein the heat treatment temperature is 300 ℃, and then naturally cooling to room temperature, the concentration of the hydrochloric acid is 0.4mol/L, and the mass-to-volume ratio of the activated carbon coarse body to the hydrochloric acid is 1: 15;
the content of each acidic group before and after treatment of the activated carbon prepared by the invention is obtained by a Boehm titration test, and is shown in Table 1.
Table 1:
example 1 Carboxy (mmol/L) Lactone group (mmol/L) Phenolic hydroxy group (mmol/L)
Activated carbon before modification 4.379 0.0836 7.817
Modified activated carbon 4.820 2.045 7.486
As can be seen from table 1, both carboxyl groups and lactone groups in the acidic groups on the activated carbon surface increased after the modification treatment, the phenolic hydroxyl groups decreased slightly, and the total acidic functional groups increased.
The activated carbon prepared in example 1 was repeatedly used 20 times for methylene blue, crystal violet and methyl orange, and the removal rates thereof were 86.6%, 82.3% and 83.6% of the initial use in this order.
Example 2
A preparation method of kiwi pruning branch-based activated carbon comprises the following steps:
(1) pruning kiwi fruits, cutting into 3cm small sections, drying for 4h in a forced air drying oven at 80 ℃, then crushing at 25000 r/min, and sieving with a 80-mesh sieve to obtain kiwi fruit pruning branch powder;
(2) adding the kiwi fruit pruned branch powder prepared in the step (1) into a mixed solution composed of zinc chloride, phosphoric acid and water, stirring at the speed of 1000 r/min for 2h, wherein the mass concentration of the zinc chloride is 90%, the mass concentration of the phosphoric acid is 70%, the mixing ratio of the zinc chloride, the phosphoric acid and the water is stirred to be 5:1:30, and the mass-volume ratio of the kiwi fruit pruned branch powder to the mixed solution is 1g: 20 mL;
(3) centrifugally separating the kiwi pruned branch powder from the mixed solution, heating to 300 ℃ at a speed of 5 ℃/min in the nitrogen atmosphere, and carbonizing for 1h at constant temperature; then the temperature is raised to 650 ℃ at the speed of 20 ℃/min, and the constant temperature is kept for 1.5 h; then slowly cooling to 400 ℃ at the speed of 3 ℃/min, keeping the temperature for 50min, and then continuously cooling to room temperature at the same speed to obtain the activated carbon coarse body;
(4) adding the activated carbon crude body prepared in the step (3) into hydrochloric acid, oxidizing for 20min at 65 ℃, repeatedly carrying out centrifugal washing on the activated carbon crude body by using distilled water after the oxidation is finished until the activated carbon crude body is neutral, then carrying out heat treatment for 1h, wherein the heat treatment temperature is 160 ℃, and then naturally cooling to room temperature, the concentration of the hydrochloric acid is 0.2mol/L, and the mass-to-volume ratio of the activated carbon crude body to the hydrochloric acid is 1: 10;
the activated carbon prepared in this example was used repeatedly 20 times for methylene blue, crystal violet and methyl orange, and the removal rates thereof were 84.7%, 80.4% and 80.9% of the initial use in this order.
Example 3
A preparation method of kiwi pruning branch-based activated carbon comprises the following steps:
(1) pruning kiwi fruits, cutting into 2cm small sections, drying in a forced air drying oven at 80 ℃ for 4h, then crushing at 25000 r/min, and sieving with a 40-mesh sieve to obtain kiwi fruit pruning branch powder;
(2) adding the kiwi fruit pruned branches prepared in the step (1) into a mixed solution composed of zinc chloride, phosphoric acid and water, stirring at the speed of 1500 revolutions per minute for 1 hour, wherein the mass concentration of the zinc chloride is 50 percent, the mass concentration of the phosphoric acid is 85 percent, the mixing ratio of the zinc chloride, the phosphoric acid and the water is 1:10:50, and the mass-volume ratio of the kiwi fruit pruned branch powder to the mixed solution is 1g: 60 mL;
(3) centrifugally separating the kiwi pruned branch powder from the mixed solution, heating to 400 ℃ at the speed of 8 ℃/min under the atmosphere of nitrogen gas, and carbonizing for 0.5-1h at constant temperature; then heating to 500 ℃ at the speed of 10 ℃/min, and keeping the temperature for 70 min; then slowly cooling to 420 ℃ at the speed of 3 ℃/min, keeping the temperature for 30min, and then continuously cooling to room temperature at the same speed to obtain the activated carbon coarse body;
(4) adding the activated carbon crude body prepared in the step (3) into hydrochloric acid, oxidizing for 30min at 55 ℃, repeatedly carrying out centrifugal washing on the activated carbon crude body by using distilled water after the oxidation is finished until the activated carbon crude body is neutral, then carrying out heat treatment for 1h, wherein the heat treatment temperature is 200 ℃, and then naturally cooling to room temperature, the concentration of the hydrochloric acid is 0.3mol/L, and the mass-to-volume ratio of the activated carbon crude body to the hydrochloric acid is 1: 20;
after the activated carbon prepared in this example was repeatedly used for 20 times for the methylene blue, crystal violet and methyl orange, the removal rates thereof were 81.4%, 80.2% and 79.8% of the initial use in this order.
According to IUPAC regulations, micropores are pores with the diameter of 0-2 nm, mesopores are pores with the diameter of 2-50 nm, and macropores are pores with the diameter of more than 50 nm.
The pore size structure and distribution were analyzed and the results are shown in table 2.
Table 2:
Figure BDA0002353103000000071
respectively adding the activated carbon prepared in each embodiment of the invention into a solution containing 100mL of 300mg/L methylene blue, crystal violet and methyl orange, wherein the adding amount is 0.01g, adjusting the pH value of the solution to 6-7, placing the solution in a constant temperature shaking table at 30 ℃ and 160r/min, adsorbing for 1h, measuring the adsorption value of the solution by using an ultraviolet spectrophotometer, and calculating the adsorption capacity of the activated carbon of each embodiment on each dye.
The adsorption capacities of the activated carbon prepared in each example of the present invention to methylene blue, crystal violet and methyl orange are shown in table 3.
Table 3:
adsorption of cationic dyes Methylene blue Crystal violet Methyl orange
Example 1 1010.6mg/g 936.3mg/g 374.8mg/g
Example 2 947.4mg/g 922.7mg/g 410.3mg/g
Example 3 964.9mg/g 925.1mg/g 382.5mg/g

Claims (7)

1. A preparation method of kiwi pruning branch-based activated carbon is characterized by comprising the following steps: cutting, drying and crushing kiwi pruned branches to obtain kiwi pruned branch powder, then adding the kiwi pruned branch powder into a mixed solution consisting of zinc chloride, phosphoric acid and water, violently stirring, carrying out high-temperature carbonization and activation after centrifugal separation, then carrying out modification treatment, and finally carrying out centrifugal washing and drying; the mass concentration of the zinc chloride is 50% -90%, the mass concentration of the phosphoric acid is 70% -85%, the mixing volume ratio of the zinc chloride to the phosphoric acid to the water is 1-5: 1-10: 30-50, the mass volume ratio of the kiwi fruit pruning branch powder to the mixed liquid is 1g: 20-100 mL.
2. The method of preparing a kiwi pruned branch-based activated carbon as claimed in claim 2, wherein: the pretreatment specifically comprises the steps of pruning kiwi fruits, cutting into 2-3cm small sections, drying for 2-4 h at 80 ℃ in a forced air drying oven, then crushing at 25000 r/min, and sieving with a 40-80 mesh sieve to obtain kiwi fruit pruning powder.
3. The method of preparing a kiwi pruned branch-based activated carbon as claimed in claim 2, wherein: the violent stirring is carried out for 1-2 h at the speed of 1000-1500 rpm.
4. The method of preparing a kiwi pruned branch-based activated carbon as claimed in claim 1 or 2, wherein: the high-temperature carbonization and activation are specifically that kiwi pruned branch powder is centrifugally separated from the mixed solution, heated to 300-400 ℃ at a speed of 5-8 ℃/min in an inert gas atmosphere, and carbonized at constant temperature for 0.5-1 h; then heating to 650 ℃ at the speed of 10-20 ℃/min, and keeping the temperature for 1-1.5 h; then slowly cooling to 400-450 ℃ at the speed of 3-4 ℃/min, keeping the temperature for 30-50min, and then continuously cooling to room temperature at the same speed to obtain the activated carbon coarse body.
5. A process for the preparation of a kiwi pruned branch-based activated carbon as claimed in any one of claims 1 to 4, wherein: the modification treatment is to oxidize the activated carbon coarse body after high-temperature carbonization and activation for 20-40 min at 55-65 ℃ by using hydrochloric acid with the concentration of 0.2-0.5 mol/L, repeatedly carry out centrifugal washing on the activated carbon coarse body by using distilled water after the oxidation is finished until the activated carbon coarse body is neutral, then carry out heat treatment for 1h, wherein the heat treatment temperature is 160-300 ℃, and then naturally cool the activated carbon coarse body to the room temperature.
6. The method of making a kiwi pruned branch-based activated carbon of claim 5, wherein: the mass volume ratio of the activated carbon coarse body to the hydrochloric acid is 1g: 10-20 mL.
7. A preparation method of kiwi pruning branch-based activated carbon comprises the following steps:
(1) pruning kiwi fruits, cutting into 2-3cm small sections, drying for 2-4 h in a forced air drying oven at 80 ℃, then crushing at 25000 r/min, and sieving with a 40-80 mesh sieve to obtain kiwi fruit pruning branch powder;
(2) adding the kiwi fruit pruned branch powder prepared in the step (1) into a mixed solution composed of zinc chloride, phosphoric acid and water, stirring at the speed of 1000-1500 rpm for 1-2 h, wherein the mass concentration of the zinc chloride is 50-90%, the mass concentration of the phosphoric acid is 70-85%, the mixing ratio of the zinc chloride, the phosphoric acid and the water is 1-5: 1-10: 30-50, and the mass-volume ratio of the kiwi fruit pruned branch powder to the mixed solution is 1g: 20-100 mL;
(3) centrifugally separating the kiwi pruned branch powder from the mixed solution, heating to 300-400 ℃ at the speed of 5-8 ℃/min under the inert gas atmosphere, and carbonizing at constant temperature for 0.5-1 h; then heating to 500-650 ℃ at the speed of 10-20 ℃/min, and keeping the temperature for 1-1.5 h; then slowly cooling to 400-450 ℃ at the speed of 3-4 ℃/min, keeping the temperature for 30-50min, and then continuously cooling to room temperature at the same speed to obtain the activated carbon coarse body;
(4) oxidizing the activated carbon coarse body prepared in the step (4) with hydrochloric acid at 55-65 ℃ for 20-40 min, repeatedly performing centrifugal washing on the activated carbon coarse body with distilled water after oxidation is completed until the activated carbon coarse body is neutral, then performing heat treatment for 1h, wherein the heat treatment temperature is 160-300 ℃, and then naturally cooling to room temperature, the concentration of the hydrochloric acid is 0.2-0.5 mol/L, and the mass volume ratio of the activated carbon coarse body to the hydrochloric acid is 1: 10-20.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112973628A (en) * 2021-02-06 2021-06-18 重庆文理学院 Preparation method of activated carbon rich in basic functional groups
CN115487792A (en) * 2021-02-06 2022-12-20 重庆文理学院 Preparation method of magnetic activated carbon
CN115924915A (en) * 2022-11-18 2023-04-07 安徽农业大学 Preparation method of solidago canadensis activated carbon

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112973628A (en) * 2021-02-06 2021-06-18 重庆文理学院 Preparation method of activated carbon rich in basic functional groups
CN115487792A (en) * 2021-02-06 2022-12-20 重庆文理学院 Preparation method of magnetic activated carbon
CN115924915A (en) * 2022-11-18 2023-04-07 安徽农业大学 Preparation method of solidago canadensis activated carbon

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Application publication date: 20200410