CN115041137B - Preparation and application of recyclable humic acid biomass carbon material - Google Patents

Preparation and application of recyclable humic acid biomass carbon material Download PDF

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CN115041137B
CN115041137B CN202210736171.5A CN202210736171A CN115041137B CN 115041137 B CN115041137 B CN 115041137B CN 202210736171 A CN202210736171 A CN 202210736171A CN 115041137 B CN115041137 B CN 115041137B
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humic acid
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CN115041137A (en
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陈欢
张斯童
乔煦
王刚
陈四季
唐珊珊
陈�光
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Jilin Agricultural University
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract

A preparation method of a recyclable humic acid biomass carbon material comprises the steps of preparing and regenerating the carbon material, wherein the carbon material is prepared by soaking humic acid in a sodium carbonate aqueous solution under ultraviolet light, adding hydrogen peroxide into the treated humic acid, mixing, carrying out first high-temperature treatment to obtain humic acid carbon, treating the humic acid carbon by using potassium hydroxide and sodium hydroxide as composite activators, carrying out second high-temperature treatment, carrying out acid pickling and drying, and the mass ratio of black humic acid in the humic acid is more than 85%. The humic acid biomass carbon material prepared by the invention has excellent physicochemical properties, and the specific surface area reaches 2376m 2 G, pore volume up to 2.27cm 3 The adsorption capacity of the humic acid biomass carbon material to malachite green and tetracycline hydrochloride reaches 1059.4mg/g and 872.3mg/g, and after the humic acid biomass carbon material is recycled for 5 times, the removal rate of the humic acid biomass carbon material to malachite green and tetracycline hydrochloride still reaches 69.7% and 58.6%, and the humic acid biomass carbon material has excellent cycle stability.

Description

Preparation and application of recyclable humic acid biomass carbon material
Technical Field
The invention relates to the technical field of organic wastewater treatment, and particularly relates to a preparation and application of a recyclable humic acid biomass carbon material.
Background
In recent years, water pollution has become an increasingly serious problem due to rapid development of society, and dyes and antibiotics are one of the main sources of wastewater pollution. The adsorption and degradation of organic dyes and antibiotics in wastewater has become a research hotspot. Common methods for treating water pollution comprise chemical flocculation, membrane filtration, reverse osmosis, ion exchange, adsorption, electrochemical processes and the like, wherein the adsorption method has the advantages of simple operation, low cost and high efficiency, and becomes a popular wastewater treatment method.
Malachite green has been widely used for preventing and treating diseases of various aquatic animals, such as saprolegniasis, branchiomycosis, ichthyophthirius multiformis and the like, and is also used as a dye for silk, leather and paper, but the malachite green has potential carcinogenic, teratogenic and mutagenic effects, and is forbidden by the state in the field of pollution-free aquaculture.
The tetracyclic antibiotic is a broad-spectrum antibiotic, can inhibit the synthesis of bacterial proteins, and is widely applied to the pharmaceutical industry, the animal husbandry and the aquaculture industry, but the tetracyclic antibiotic is difficult to completely degrade, the degraded intermediate product of the tetracyclic antibiotic has great toxicity, and the enrichment of drug-resistant flora and the generation of resistance genes are caused by general residues. When the tetracycline hydrochloride is adsorbed and treated by the biomass carbon, the technical problems of low adsorption capacity, agglomeration, difficult separation and the like often occur, so that the application of the method in the tetracycline hydrochloride adsorption is hindered.
Humic acid has strong ion exchange capacity, adsorption capacity and impurity removal capacity, so that the humic acid is widely applied to the field of wastewater treatment and can be used as a cationic dye decolorant to treat cationic printing and dyeing wastewater. In the prior art, the malachite green and tetracycline hydrochloride are directly adsorbed and degraded by using humic acid, but the degradation efficiency is not high, and the stability is poor. The prior literature reports that the specific surface area of the biomass carbon prepared by adopting fulvic acid through high-temperature carbonization and adopting sodium hydroxide as an activating agent through high-temperature activation reaches 2922m 2 The adsorption amounts reached 2250mg/g and 941mg/g for brilliant green and sulfadiazine sodium salt, respectively. However, the adsorption performance of the biomass carbon prepared by the method for treating malachite green and tetracycline hydrochloride is poor, and based on the poor adsorption performance, further improvement is needed to prepare the humic acid biomass carbon material with excellent adsorption performance on the malachite green and the tetracycline hydrochloride.
Disclosure of Invention
The invention aims to provide a preparation method of a humic acid biomass carbon material capable of being recycled.
The invention also aims to provide application of the humic acid biomass carbon material.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a humic acid biomass carbon material capable of being recycled is characterized by comprising the following steps: the method comprises the steps of preparing a carbon material and performing regeneration treatment, wherein the carbon material is prepared by adding humic acid into a sodium carbonate aqueous solution, performing ultrasonic treatment, adding hydrogen peroxide into the treated humic acid, mixing, performing first high-temperature treatment to obtain humic acid carbon, treating the humic acid carbon by using potassium hydroxide and sodium hydroxide as composite activators, performing second high-temperature treatment, and performing acid pickling and drying, wherein the mass ratio of the humic acid to the black humic acid is more than 85%.
Further, the concentration of the sodium carbonate aqueous solution is 0.6-1mmol/L, and the power of ultrasonic treatment is 60-100W.
The molecular weight of the humic acid is larger, the activity is lower, the humic acid is directly carbonized at high temperature and then activated, the physical and chemical properties of the prepared biochar are poorer, and the overall adsorption performance is not ideal.
According to the method, sodium carbonate is combined with ultrasound for pretreatment, a small amount of black humic acid is removed by activating the sodium carbonate with ultrasound, the effect of loosening the stable structure of the black humic acid is achieved, hydrogen peroxide is added, the molecular chain of the black humic acid is further broken on the basis of loosening the structure of the black humic acid through the oxidizing property of the hydrogen peroxide, the sodium carbonate serves as an activating agent to activate and form pores for the humic acid after oxidation treatment of the hydrogen peroxide in the first high-temperature treatment process, active groups on the surface of the carbon material are increased, then potassium hydroxide and sodium hydroxide are adopted to further adjust the activation degree of the humic acid carbon on the basis of the first activation and adjust the change trend of the surface functional groups, and therefore the biomass carbon material which has high-efficiency adsorption performance for malachite green and tetracycline hydrochloride and excellent adsorption stability is prepared.
Preferably, the concentration of the sodium carbonate aqueous solution is 0.8mmol/L, and the power of ultrasonic treatment is 80W.
Further, the mass fraction of the hydrogen peroxide is 20%, and the dosage relationship of the humic acid, the sodium carbonate aqueous solution and the hydrogen peroxide is 10g:15-20mL:4-5mL.
Further, the first high-temperature treatment is to put the pretreated humic acid under the protection of nitrogen, raise the temperature to 550-600 ℃ at a rate of 2-3 ℃/min, and preserve the temperature for 40-50min to obtain humic acid carbon.
Further, mixing and grinding humic acid carbon and the composite activator according to a mass ratio of 1:2-3 in the second high-temperature treatment, then placing the mixture in a tube furnace, heating to 600-650 ℃ at a speed of 6-8 ℃/min, and preserving heat for 60min; after the heat preservation is finished, washing the mixture by hydrochloric acid and then washing the mixture by deionized water until the mixture is neutral.
Further, the mass ratio of potassium hydroxide to sodium hydroxide in the composite activator is 1:1.
In the preparation process, sodium hydroxide is tried to be used as an activating agent for activation, physical properties such as specific surface area, pore volume and the like of the biomass carbon material can be improved, but the prepared biomass carbon has poor adsorbability on malachite green and tetracycline hydrochloride, and the biomass carbon material prepared by the compound activation of sodium hydroxide and potassium hydroxide has remarkable improvement on the adsorbability on malachite green and tetracycline hydrochloride.
The preparation method of the humic acid biomass carbon material is characterized by comprising the following steps of:
step 1: pretreatment of
Adding a sodium carbonate aqueous solution with the concentration of 0.6-1mmol/L into the powder, carrying out ultrasonic treatment for 40-60min under the power of 60-100W, adding hydrogen peroxide with the mass fraction of 20% into the solid component after filtering, stirring and mixing, wherein the content of the humic acid is 85%, and the content ratio of the humic acid, the sodium carbonate aqueous solution and the hydrogen peroxide is 10g:15-20mL:4-5mL;
step 2: first high temperature
Placing the pretreated humic acid in a tubular furnace, heating to 550-600 ℃ at a speed of 2-3 ℃/min under the protection of nitrogen, and preserving heat for 40-50min to obtain humic acid carbon;
and 3, step 3: second high temperature
Mixing and grinding humic acid carbon and a composite activator according to a mass ratio of 1:2-3, then placing the mixture in a tube furnace, heating to 600-650 ℃ at a speed of 6-8 ℃/min, and preserving heat for 60min; after the heat preservation is finished, washing the mixture by hydrochloric acid, and then washing the mixture by deionized water to be neutral, wherein the composite activating agent is composed of KOH and NaOH according to the mass ratio of 1:1.
And the regeneration treatment is to perform centrifugal separation from the wastewater after the humic acid biomass carbon adsorbs pollutants, dry the wastewater and place the wastewater in a tubular furnace, heat the wastewater to 550-600 ℃ at a speed of 2-3 ℃/min, and keep the temperature for 40-50min.
The humic acid biomass carbon material is applied to adsorbing organic dyes and antibiotics.
Specifically, the humic acid biomass carbon material is used for adsorbing malachite green and tetracycline hydrochloride.
The invention has the following technical effects:
the humic acid biomass carbon material prepared by the invention has excellent physicochemical properties, and the specific surface area reaches 2376m 2 G, pore volume up to 2.27cm 3 The surface of the material has rich active groups, the adsorption capacity of the material to malachite green and tetracycline hydrochloride reaches 1059.4mg/g and 872.3mg/g, and after the material is recycled for 5 times, the removal rate of the humic acid biomass carbon material to malachite green and tetracycline hydrochloride still reaches 69.7 percent and 58.6 percent, so that the material has excellent cycle stability.
Drawings
FIG. 1: scanning electron microscope images of humic acid raw materials, carbonized humic acid carbon and humic acid biomass carbon material finished products.
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 variations to the present invention based on the above disclosure.
According to the document "Preparation of biological carbon material based on fThe carbon specific surface area of fulvic acid biomass prepared by the protocol described in ulvic acid and its application in dye and anti-biological assays, xu Qiao et al is 2250m 2 G, pore volume 1.8cm 3 The maximum adsorption amount of the carbon material to sulfadiazine sodium salt is 941mg/g at the pH value of 3 and 2250mg/g at the pH value of 9, but when the fulvic acid biomass carbon is used for adsorbing malachite green and tetracycline hydrochloride, the adsorption performance is not high and is only 388.4mg/g and 363.5mg/g, and after 5 cycles of cyclic use, the removal rate of the malachite green and the tetracycline hydrochloride is only 31.4 percent and 27.9 percent of the first time.
Example 1
A preparation method of a humic acid biomass carbon material comprises the following steps:
step 1: pretreatment of
Adding a sodium carbonate aqueous solution with the concentration of 0.8mmol/L into the powder, carrying out ultrasonic treatment for 60min under the power of 80W, adding hydrogen peroxide with the mass fraction of 20% into solid components after filtration, stirring and mixing, wherein the content of the humic acid in the humic acid is 85%, and the content ratio of the humic acid to the sodium carbonate aqueous solution to the hydrogen peroxide is 10g:20mL of: 5mL;
and 2, step: first high temperature
Placing the pretreated humic acid in a tubular furnace, heating to 600 ℃ at the speed of 2 ℃/min under the protection of nitrogen, and preserving heat for 40min to obtain humic acid carbon;
and step 3: second high temperature
Mixing and grinding humic acid carbon and a composite activator according to a mass ratio of 1:2, then placing the mixture in a tubular furnace, heating to 650 ℃ at a speed of 8 ℃/min, and preserving heat for 60min; after the heat preservation is finished, washing the mixture by hydrochloric acid with the mass fraction of 10%, and then washing the mixture by deionized water to be neutral, wherein the composite activating agent consists of KOH and NaOH according to the mass ratio of 1:1.
Example 2
A preparation method of a humic acid biomass carbon material comprises the following steps:
step 1: pretreatment of
Adding a sodium carbonate aqueous solution with the concentration of 1mmol/L into the powder, performing ultrasonic treatment for 40min under the power of 60W, adding hydrogen peroxide with the mass fraction of 20% into solid components after filtering, stirring and mixing, wherein the content of the humic acid in the humic acid is 85%, and the dosage ratio of the humic acid to the sodium carbonate aqueous solution to the hydrogen peroxide is 10g:15mL of: 4mL;
and 2, step: first high temperature
Placing the pretreated humic acid in a tubular furnace, heating to 550 ℃ at a speed of 3 ℃/min under the protection of nitrogen, and preserving heat for 50min to obtain humic acid carbon;
and step 3: second high temperature
Mixing and grinding humic acid carbon and a composite activator according to a mass ratio of 1:3, then placing the mixture in a tubular furnace, heating to 600 ℃ according to a speed of 6 ℃/min, and preserving heat for 60min; after the heat preservation is finished, washing the mixture by hydrochloric acid with the mass fraction of 10%, and then washing the mixture by deionized water to be neutral, wherein the composite activating agent is composed of KOH and NaOH according to the mass ratio of 1:1.
Example 3
A preparation method of a humic acid biomass carbon material comprises the following steps:
step 1: pretreatment of
Adding a sodium carbonate aqueous solution with the concentration of 0.6mmol/L into the powder, carrying out ultrasonic treatment for 50min under the power of 100W, adding hydrogen peroxide with the mass fraction of 20% into solid components after filtering, stirring and mixing, wherein the content of the humic acid in the humic acid is 85%, and the dosage ratio of the humic acid to the sodium carbonate aqueous solution to the hydrogen peroxide is 10g:16mL of: 4mL;
step 2: first high temperature
Placing the pretreated humic acid in a tubular furnace, heating to 580 ℃ at the speed of 2 ℃/min under the protection of nitrogen, and preserving heat for 45min to obtain humic acid carbon;
and step 3: second high temperature
Mixing and grinding humic acid carbon and a composite activating agent according to a mass ratio of 1; after the heat preservation is finished, washing the mixture by hydrochloric acid with the mass fraction of 10%, and then washing the mixture by deionized water to be neutral, wherein the composite activating agent is composed of KOH and NaOH according to the mass ratio of 1:1.
The adsorption performance and the cycle stability of the humic acid biomass carbon prepared by the embodiments of the invention on malachite green and tetracycline hydrochloride are shown in table 1.
Table 1:
Figure GDA0003963859010000061
the humic acid biomass carbon prepared by the invention has excellent adsorption performance on malachite green and tetracycline hydrochloride, the removal rate of the humic acid biomass carbon in the first adsorption respectively reaches 90.7 percent and 88.2 percent, after 5 times of cyclic adsorption, the humic acid biomass carbon still can be kept at more than 58.4 percent and 50.5 percent, and the humic acid biomass carbon has excellent cyclic stability.
Comparative example 1
The difference from the embodiment 1 is that the humic acid in the embodiment 1 is soaked in sodium carbonate, then hydrogen peroxide is added, the first high-temperature treatment is carried out, an activating agent is NaOH, and the rest steps are the same as the embodiment 1.
Comparative example 2
Different from the embodiment 1, after the first high temperature treatment, the activating agent is NaOH, and then the second high temperature treatment is carried out under the same parameters, and the rest steps are the same as the embodiment 1.
Comparative example 3
Unlike example 1, humic acid in example 1 was treated in sodium carbonate solution by external light and then directly treated at high temperature, and the rest of the procedure was the same as example 1.
Comparative example 4
Humic acid with 90 percent of fulvic acid is used as a raw material and is prepared according to the method.
The adsorption performance of the biomass carbon prepared in each proportion on malachite green and tetracycline hydrochloride is shown in table 2.
Table 2:
Figure GDA0003963859010000071
in the comparative example 1, the black humic acid with larger molecular weight is used as the raw material, the structure of the black humic acid is basically not changed before carbonization by only soaking the humic acid in sodium carbonate, the pore-forming is only carried out during carbonization, and hydrogen peroxide is added, so that the oxidation effect of the black humic acid with a stable structure is weaker, the activity of the black humic acid is lower, the specific surface area and the pore volume of the prepared biomass are not high, and the adsorption capacity of the biomass to peacock Dan Sulv and tetracycline hydrochloride is limited. And after the sodium carbonate is soaked and ultrasonic treatment is combined, a very small amount of humic acid in the humic acid is degraded, the stable integral structure of the humic acid is loosened, in the high-temperature carbonization process, the sodium carbonate is used as a first activating agent to synchronously activate and form pores, and composite alkali is adopted to perform secondary pore formation subsequently, so that the specific surface area, pore volume and the like of the prepared biomass carbon are obviously improved, and the surface functional groups are changed, so that the adsorption performance of the biomass carbon to malachite green and operational tetracycline is improved to a certain extent. On the basis of the invention, humic acid mainly containing black humic acid is replaced by humic acid mainly containing yellow humic acid with smaller molecular weight, the humic acid is soaked by sodium carbonate under ultraviolet light, the degradation degree of the yellow humic acid is uncontrollable, so that the original structure of the yellow humic acid is destroyed, when hydrogen peroxide is subsequently added, the strong oxidizing property of the hydrogen peroxide destroys the internal structure of the yellow humic acid again, so that the carbon specific surface area and the pore volume of the finally prepared biomass are in a descending trend, the adsorption performance is extremely poor, and the adsorption performance is seriously attenuated in the cyclic adsorption process.

Claims (11)

1. A preparation method of a humic acid biomass carbon material capable of being recycled is characterized by comprising the following steps: the method comprises the steps of preparing a carbon material and performing regeneration treatment, wherein the carbon material is prepared by adding humic acid into a sodium carbonate aqueous solution, performing ultrasonic treatment, adding hydrogen peroxide into the treated humic acid, mixing, performing first high-temperature treatment to obtain humic acid carbon, treating the humic acid carbon by using potassium hydroxide and sodium hydroxide as composite activators, performing second high-temperature treatment, and performing acid pickling and drying, wherein the mass ratio of the humic acid to the black humic acid is more than 85%.
2. The method for preparing the humic acid biomass carbon material capable of being recycled according to claim 1, wherein: the concentration of the sodium carbonate aqueous solution is 0.6-1mmol/L, and the power of ultrasonic treatment is 60-100W.
3. The method for preparing the humic acid biomass carbon material capable of being recycled according to claim 2, wherein: the mass fraction of the hydrogen peroxide is 20%, and the dosage relationship of the humic acid, the sodium carbonate aqueous solution and the hydrogen peroxide is 10g:15-20mL:4-5mL.
4. A method for preparing a humic acid biomass carbon material capable of being recycled according to any one of claims 1 to 3, wherein: the first high-temperature treatment is to put the pretreated humic acid under the protection of nitrogen, raise the temperature to 550-600 ℃ at the speed of 2-3 ℃/min, and preserve the temperature for 40-50min to obtain humic acid carbon.
5. A method for preparing a humic acid biomass carbon material capable of being recycled according to any one of claims 1 to 3, wherein: in the second high-temperature treatment, the humic acid carbon and the composite activator are mixed and ground according to the mass ratio of 1:2-3, then the mixture is placed in a tubular furnace, the temperature is raised to 600-650 ℃ according to the speed of 6-8 ℃/min, and the temperature is kept for 60min; after the heat preservation is finished, washing the mixture by hydrochloric acid and then washing the mixture by deionized water until the mixture is neutral.
6. The method for preparing the humic acid biomass carbon material capable of being recycled according to claim 4, wherein: mixing and grinding humic acid carbon and a composite activator according to the mass ratio of 1:2-3, then placing the mixture into a tubular furnace, heating to 600-650 ℃ at the speed of 6-8 ℃/min, and keeping the temperature for 60min; after the heat preservation is finished, washing the mixture by hydrochloric acid and then washing the mixture by deionized water until the mixture is neutral.
7. The method for preparing the humic acid biomass carbon material capable of being recycled according to claim 6, wherein: the mass ratio of potassium hydroxide to sodium hydroxide in the composite activator is 1:1.
8. The method for preparing the humic acid biomass carbon material capable of being recycled according to claim 7, wherein the step of preparing the carbon material is as follows; and the regeneration treatment is to perform centrifugal separation from the wastewater after the humic acid biomass carbon material adsorbs pollutants, dry the wastewater and place the wastewater in a tubular furnace, heat the wastewater to 550-600 ℃ at a speed of 2-3 ℃/min, and preserve the temperature for 40-50min.
9. The preparation method of the humic acid biomass carbon material is characterized by comprising the following steps of:
step 1: pretreatment of
Adding a sodium carbonate aqueous solution with the concentration of 0.6-1mmol/L into humic acid powder, carrying out ultrasonic treatment for 40-60min under the power of 60-100W, adding hydrogen peroxide with the mass fraction of 20% into solid components after filtering, stirring and mixing, wherein the content of the humic acid is 85%, and the dosage ratio of the humic acid, the sodium carbonate aqueous solution and the hydrogen peroxide is 10g:15-20mL:4-5mL;
step 2: first high temperature
Placing the pretreated humic acid in a tubular furnace, heating to 550-600 ℃ at a speed of 2-3 ℃/min under the protection of nitrogen, and preserving heat for 40-50min to obtain humic acid carbon;
and 3, step 3: second high temperature
Mixing and grinding humic acid carbon and a composite activator according to a mass ratio of 1:2-3, then placing the mixture in a tube furnace, heating to 600-650 ℃ at a speed of 6-8 ℃/min, and preserving heat for 60min; after the heat preservation is finished, washing the mixture by hydrochloric acid, and then washing the mixture by deionized water to be neutral, wherein the composite activating agent is composed of KOH and NaOH according to the mass ratio of 1:1.
10. Use of humic acid biomass carbon material prepared by the process of claim 9 wherein: used for adsorbing organic dyes and antibiotics.
11. Use of humic acid biomass carbon material according to claim 10 wherein: the humic acid biomass carbon material is used for adsorbing malachite green and tetracycline hydrochloride.
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