CN115318247A - Eggplant porous carbon and preparation method and application thereof - Google Patents
Eggplant porous carbon and preparation method and application thereof Download PDFInfo
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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
-
- 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
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- Chemical & Material Sciences (AREA)
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to the technical field of adsorption materials, in particular to eggplant porous carbon and a preparation method and application thereof, and the eggplant porous carbon comprises the following steps: step one, carrying out acid liquor soaking and activating treatment on peeled and cut eggplants after alkali liquor treatment; step two, freeze-drying the eggplants subjected to the activation treatment in the step one to obtain an eggplant cavernous body; and step three, pre-oxidizing the eggplant cavernous body, heating to 450-550 ℃, preserving heat, carbonizing, washing and drying to obtain the eggplant porous carbon. The invention can quickly and efficiently adsorb and treat different types of printing and dyeing wastewater by realizing lower addition amount, can obviously change the chromaticity of the wastewater, achieves ideal water quality purification effect, and has good practical application prospect.
Description
Technical Field
The invention relates to the technical field of adsorption materials, and particularly relates to eggplant porous carbon and a preparation method and application thereof.
Background
Printing and dyeing wastewater is one of the main factors causing environmental pollution, and is difficult to biodegrade, reduces the penetration of light into water, inhibits photosynthesis of plants, causes eutrophication of water, and may pose a high risk of cancer to human health. Therefore, the purification of the printing and dyeing wastewater is very important for treating water pollution. The treatment methods of the printing and dyeing wastewater such as a photocatalysis method, an electrochemical oxidation method, a photodegradation method, a membrane technology, a photothermal conversion method and the like can remove or degrade organic pollutants and dyes in the wastewater, but the defects of secondary pollution, byproduct formation, long removal time, unsatisfactory efficiency and the like always bring a lot of limitations to practical application.
Adsorption technology has been successfully applied to water purification due to its simple method, high efficiency, and no by-products. Porous materials are commonly used as wastewater absorbents, such as activated carbon, bacterial cellulose, chitosan, carbon nanotubes, and composite porous materials, among others. However, due to the fact that the adsorption dye is single in type and the water quality is complex, the adsorption efficiency is low, the adsorption rate is slow, and some adsorbent materials are complex to synthesize in the preparation process, high in cost and the like, the performance price of practical application is low, and the large-scale production and application are not facilitated.
The existing Chinese patent CN 112774629A discloses a method for preparing corn-based biomass porous carbon and removing methylene blue in printing and dyeing wastewater by using the same, wherein the optimal adsorption conditions of the corn-based biomass porous carbon on methylene blue solution are as follows: the initial concentration is 5mg/L, the adding amount of the adsorbent is 5mg, the adsorption time is 30min, the final saturated adsorption amount is 158.7mg/g, the time for adsorbing the low-concentration dye is long, and the adsorption efficiency is low. Chinese patent CN 113929096A discloses a method for preparing a biomass carbon material by taking coconut shells as a main carbon source and performing premixed modification treatment through sodium hydroxide (potassium hydroxide), and the method is applied to the adsorption of methylene blue; its adsorption test for methylene blue: the initial concentration was 25ppm. The dosage of the adsorbent is 10mg, the adsorption time is 30min, the removal rate reaches 96.74%, and the dosage of the adsorbent is lower than the efficiency of treating wastewater and the time is longer. The prior patents only explore the application of methylene blue which is an alkaline cationic dye, the type of the absorption dye is single, and the practical wastewater treatment application is limited by considering the complexity of the components of the practical printing and dyeing wastewater.
Disclosure of Invention
In view of the above, the invention aims to provide eggplant porous carbon and a preparation method and application thereof, so as to solve the problems that the type of an adsorption dye is single, and the adsorption rate and the adsorption efficiency cannot meet the purification requirement of actual printing and dyeing wastewater in the prior art.
Based on the purpose, the invention provides a preparation method of eggplant porous carbon, which comprises the following steps:
step one, carrying out acid liquor soaking and activating treatment on peeled and cut eggplants after alkali liquor treatment;
step two, freeze-drying the eggplants subjected to the activation treatment in the step one to obtain an eggplant cavernous body;
and step three, pre-oxidizing the eggplant cavernous body, heating to 450-550 ℃, preserving heat, carbonizing, washing and drying to obtain the eggplant porous carbon.
Optionally, in the first step, the alkaline solution is treated with sodium hydroxide with a concentration of 0.5-2/L for 3.5-4.5h. Preferably, the lye is treated with 1g/L NaOH for 4h. By adopting the concentration and the treatment time, the wax and the impurities on the surface of the material can be removed on the basis of small loss of the treated eggplant pieces, the internal structure can be maximally eroded, pectin, water-soluble substances and the like are removed, the smooth surface is more wrinkled, and the formation of holes is increased.
Preferably, the acid liquor soaking activation treatment method comprises the step of soaking eggplant pieces in 10-30vol% phosphoric acid solution for activation for 12 hours. By adopting the activating treatment mode, the eggplant has a better hole-shaped structure, the specific surface area of the eggplant is increased, and more active sites are provided for dye molecule adsorption.
Optionally, the freeze-drying time is 35-40h. Preferably, the freeze-drying time is 36 ℃. At the temperature of minus 35 ℃, the machine is in a vacuum-pumping state, water contained in the eggplant forms ice microcrystals in the freezing process under the vacuum environment, and pores with certain sizes are formed due to sublimation of the ice microcrystals in the vacuum freeze drying process, so that a spongy porous structure is formed. Preferably, the freeze-drying time is 36h. The aim is to maximize the retention of its porous morphology. If the time is too short, the crystal water contained in the eggplant is not completely sublimated and is exposed in the air, so that the ice crystals are melted into water, and the spongy porous structure collapses. The time is too long, and the resource waste is caused.
Preferably, the temperature of the pre-oxidation in the third step is 200 ℃ and the time is 90min. The material is thermally stabilized against pyrolysis against subsequent high temperature carbonization.
Optionally, the heating rate of heating to 450-550 ℃ in the third step is 4-6 ℃/min. Preferably, the temperature is raised to 500 ℃ at a rate of 5 ℃/min. Better forms a developed pore structure.
Eggplant porous carbon prepared by the preparation method of the eggplant porous carbon.
The eggplant porous carbon is applied to adsorption treatment of printing and dyeing wastewater. The printing and dyeing wastewater can be efficiently and rapidly adsorbed.
The eggplant porous carbon is used for adsorbing and treating dyes in printing and dyeing wastewater, and the types of the eggplant porous carbon comprise basic cationic dyes, acid anions and reactive dyes.
The dye comprises rhodamine B (RhB) dye liquor, methylene Blue (MB) dye liquor, methyl Orange (MO) dye liquor and actual printing and dyeing wastewater with complex components (three reactive dye mixed dye liquor such as reactive cyan B, reactive yellow 3RS, reactive brilliant red 3BSN and the like).
The invention has the beneficial effects that: the eggplant made of natural biomass material is used as a substrate, the concept of environment-friendly and green development of the eggplant is reflected, the eggplant has a loose macroporous structure, and the waxy substances and other impurities on the surface of the eggplant are removed by soaking the eggplant in sodium hydroxide alkali solution, so that the smooth surface of the eggplant becomes wrinkled, and the formation of holes is increased; the basic body is kept after freeze drying, and the specific surface area is increased and more active sites are provided for dye molecule adsorption through activation treatment; finally, a developed pore structure is further formed through a carbonization process; the characterization shows that most of the pore diameter distribution of the eggplant-based porous carbon is mesoporous, and the performance of adsorbing large dye molecules can be met. The invention can quickly and efficiently adsorb various dyes (alkaline cations, acid anions, reactive dyes and the like) on the printing and dyeing wastewater at a lower dosage, and experiments show that the invention has excellent adsorption effect, provides a green and environment-friendly efficient adsorbent for the application of actual wastewater treatment, and lays a solid foundation for the actual application and popularization.
Drawings
In order to more clearly illustrate the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the description in the prior art will be briefly described below, it is obvious that the drawings in the following description are only the present invention, and other drawings can be obtained by those skilled in the art without inventive efforts.
FIG. 1 is a schematic diagram of a preparation process of the present invention;
FIG. 2 is an SEM photograph of EMs before and after activation and EPCMs after carbonization in example 1 of the present invention; wherein, (a) is SEM form before activation treatment, (b) is SEM form after activation treatment, and (c) is SEM form of EPCMs after carbonization;
FIG. 3 is a BET-500 adsorption analysis curve and a pore size distribution curve of example 1 of the present invention; wherein (a) is an adsorption/desorption isotherm; (b) is a BET-BJH pore size analysis curve;
FIG. 4 is an adsorption/desorption analysis curve of BET-450 and BET-500 according to the present invention;
FIG. 5 is a graph of the effect of EPCMs on RhB dye adsorption performance at different contact times for inventive example 1; wherein, (a) is an optical image in the adsorption process, and (b) is the removal rate of the RhB dye; (c) Is a recorded ultraviolet-visible absorption spectrogram in the adsorption process;
FIG. 6 is an optical image and an ultraviolet-visible spectrum before and after the adsorption of EPCMs on rhodamine B prepared in example 1 of the present invention;
FIG. 7 is an optical image and UV-Vis spectrum before and after the EPCMs prepared in example 1 of the present invention adsorb methylene blue dye solution;
FIG. 8 is an optical image and UV-Vis spectrum before and after the EPCMs prepared in example 1 of the present invention adsorb methyl orange dye solution;
FIG. 9 is an optical image and UV-Vis spectrum before and after the adsorption of the actual dyeing wastewater by EPCMs prepared in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to specific embodiments below.
It is to be noted that technical terms or scientific terms used herein should have the ordinary meaning as understood by those having ordinary skill in the art to which the present invention belongs, unless otherwise defined. The word "comprising" or "comprises", and the like, means that the element or item listed before the word covers the element or item listed after the word and its equivalents, but does not exclude other elements or items.
For convenience, eggplant-based Porous activated Carbon Materials (eggplants) are hereinafter referred to as EPCMs.
Example 1
In this example, the preparation process of EPCMs is shown in FIG. 1.
And 2, cleaning the activated eggplant pieces by using deionized water, pre-freezing the eggplant pieces in a freeze dryer, and freeze-drying the eggplant pieces for 36 hours.
And 3, placing the eggplant cavernous body obtained in the step 2 in a muffle furnace, pre-oxidizing for 90min at 200 ℃, increasing to 500 ℃ at the speed of 5 ℃/min, and keeping carbonization for 70min. Subsequently, the carbonized EPCMs are removed, washed with deionized water, dried and the final EPCMs are collected.
FIG. 2 shows SEM morphologies for EMs before (FIG. 2 a) and after (FIG. 2 b) activation treatment, and for EPCMs after charring (FIG. 2 c). FIG. 2a shows that the original EMs were relatively smooth, with a lamellar structure with irregular wrinkles on the surface. Subsequently, after alkali and acid activation treatment, the sheet structure collapses, holes are formed, and the surface roughness is enhanced (fig. 2 b); these changes are more pronounced after the carbonization process. The sheet-like structure completely collapsed and more micro-scale pores appeared (fig. 2 c). The increase of the specific surface area provides more dye adsorption sites for the obtained bio-based material with enhanced roughness and porous structure to effectively adsorb the dye in the wastewater.
BET characterization further discusses the pore type and pore size distribution of EPCMs. The adsorption analysis curve and the pore size distribution curve are shown in fig. 3. N is a radical of 2 The adsorption results show that EPCMs exhibit a typical type IV isotherm (FIG. 3 a). In the low pressure range there is a small tendency to rise rapidly (fig. 3 a), indicating the presence of micropores in the material. In the high pressure range, the latter part of the curve rises again, and an "H2" type adsorption hysteresis loop appears in the middle part, indicating the existence of mesopores and complex pore structures (fig. 3 a). When the relative pressure approaches 1, there is a slight upward trend in the isotherm, indicating that some large pores are also present (fig. 3 a). FIG. 3b shows the BJH pore size distribution of EPCMs. The pore diameter is in the range of 1.7496-100 nm, and the pore diameter is a hierarchical structure of micropores, including micropores, mesopores and macropores (figure 3 b). The average pore diameter of EPCMs was reduced from 13.4840 to 4.9828nm (Tab 1) and the pore volume from 0.0058cm, compared to the original EMs 3 The/g is remarkably increased to 0.6379cm 3 The change of the average pore diameter and the pore volume of the/g (Tab 1) leads to the remarkable improvement of the specific surface area, and reaches 516.0060m 2 The highly developed porosity and surface area provide a large number of active sites for the adsorption of the dye on the surface of the material per gram (Tab 1). At the same time, the rich mesoporous structure (fig. 3 b) plays a key role in the diffusion process, making it more effective in improving the dye removal performance.
TABLE 1 comparison of BET specific surface area, average pore diameter and pore volume of EPCMs prepared in example 1 with virgin EMs
Example 2
This example is different from example 1 in that it was treated with 0.5g/L NaOH aqueous alkali for 4 hours. And influence is brought to subsequent work.
Example 3
This example is different from example 1 in that it was treated with 2g/L NaOH aqueous alkali for 4 hours.
Through the concentration comparison research of the embodiment 2 and the embodiment 3, the low-concentration alkali solution has incomplete effect of removing wax and water-soluble substances on the surface, and still can leave some impurities; the material structure can excessively be eroded by too high concentration, so that the three-dimensional network structure between the small holes collapses to form large holes, the material is broken as a whole, the subsequent process is affected, the alkaline liquor remained by too high concentration is difficult to clean and completely remove, and the subsequent acid activation treatment effect can be reduced.
Experiments prove that under the comparison of the three concentrations, the material treated by the 1g/L aqueous alkali achieves the effect of removing impurities and keeps the whole material, and electron microscope results show that the smooth surface of the material treated by the 1g/L aqueous alkali becomes wrinkled and the surface roughness is enhanced. Then the high specific surface area and the porous structure are obtained through the activating and carbonizing processes.
Example 4
This example is different from example 1 in that the temperature in step 3 was increased to 450 ℃ at a rate of 5 ℃/min, and the carbonization was maintained for 70min.
Example 5
This example is different from example 1 in that the temperature in step 3 was increased to 550 ℃ at a rate of 5 ℃/min, and the carbonization was maintained for 70min.
FIG. 4 shows adsorption analysis curves of BET-450 and BET-500. The carbonization temperature comparison studies of example 4 and example 5 show that the BET-450 ℃ specific surface area is 317.9689m 2 (ii)/g; the specific surface area of BET-550 ℃ is 488.5923m 2 Specific surface area per g, BET-500 ℃Is 516.0060m 2 (iv) g. According to BET characterization and dye adsorption experiments, the material carbonized at 500 ℃ has the largest specific surface area and the best adsorption effect. According to BET representation and dye adsorption experiments, the material carbonized at 500 ℃ has the largest specific surface area and the best adsorption effect.
Adsorption test of EPCMs prepared in example 1 on rhodamine B (RhB)
10mL of 10mg/L rhodamine B solution is prepared in advance, 3mg of EPCMs adsorbent is weighed in a 15mL glass bottle, and is placed in the glass bottle to be vibrated and adsorbed on a magnetic stirrer with the temperature of 303K and the rotating speed of 200rpm for different time (0, 5,10,15,20, 25min). The adsorption effect is shown in fig. 5 and 6, and fig. 5a is an optical image of EPCMs adsorbing rhodamine B solution at different times. It can be seen that the dye solution gradually turned colorless with increasing adsorption time. As shown in fig. 5b, the dye removal rate was 80.2% after 10min of adsorption. The adsorption efficiency is obviously improved and reaches 99.9 percent after 20min. Subsequently, at 25min of adsorption, the dye removal efficiency reached 100%, indicating that the adsorption efficiency of the EPCMs was fast and high. The ultraviolet-visible absorption spectrum (figure 5 c) further confirms that the characteristic peak of the solution concentration is sharply reduced after the solution is adsorbed for 15 minutes, and the solution concentration reaches a level close to the horizontal line after the solution is adsorbed for 20 minutes and 25 minutes, thereby showing the good effect of removing the rhodamine B dye solution.
Adsorption test of Methylene Blue (MB) by EPCMs prepared in example 1
A10 mL,10mg/L methylene blue solution was prepared in advance, and 3mg of EPCMs adsorbent was weighed in a 15mL glass bottle and placed in the glass bottle, and adsorbed for 20min by shaking on a magnetic stirrer at a temperature of 303K and a rotation speed of 200 rpm. FIG. 7 is an optical image and UV-VIS absorption spectrum of EPCMs after adsorbing methylene blue solution. Therefore, after 20min of oscillation adsorption treatment, the dye solution is changed from high chroma to colorless, and the adsorption spectrum is reduced to be close to zero, which shows that the EPCMs have high adsorption efficiency and excellent removal effect on methylene blue dye liquor.
Adsorption testing of Methyl Orange (MO) by EPCMs prepared in example 1
A10 mL and 10mg/L methyl orange solution was prepared in advance, and 3mg of EPCMs adsorbent was weighed in a 15mL glass vial and placed in the glass vial, and adsorbed by shaking on a magnetic stirrer at a temperature of 303K and a rotation speed of 200rpm for 20min. FIG. 8 is an optical image and UV-VIS absorption spectrum of EPCMs after adsorbing methyl orange solution. Therefore, after 20min of oscillation adsorption treatment, the dye solution is changed from high chroma to colorless, and the adsorption spectrum is reduced to be close to zero, which shows that the EPCMs have high adsorption efficiency and excellent removal effect on the methyl orange dye solution.
Adsorption test of EPCMs prepared in example 1 on actual printing wastewater
Measuring 10mL of actual printing and dyeing wastewater (three reactive dye mixed solutions of reactive cyan B, reactive yellow 3RS, reactive brilliant red 3BSN and the like) with unknown concentration, putting 10mg of EPCMs adsorbent in a 15mL glass bottle, placing in the glass bottle, and carrying out oscillatory adsorption for 120min on a magnetic stirrer with the temperature of 303K and the rotating speed of 200 rpm. FIG. 9 is an optical image and UV-VIS absorption spectrum of EPCMs after adsorption of actual printing wastewater. Therefore, after 120min oscillation adsorption treatment, the dye solution is changed from high chroma to colorless, and the adsorption spectrum is reduced to be close to zero, which shows that EPCMs have good removal effect on actual wastewater.
Those of ordinary skill in the art will understand that: the discussion of any embodiment above is meant to be exemplary only, and is not intended to intimate that the scope of the disclosure, including the claims, is limited to those examples; within the idea of the invention, also technical features in the above embodiments or in different embodiments may be combined, steps may be implemented in any order, and there are many other variations of the different aspects of the invention as described above, which are not provided in detail for the sake of brevity.
The present invention is intended to embrace all such alternatives, modifications and variances which fall within the broad scope of the appended claims. Therefore, any omissions, modifications, substitutions, improvements and the like that may be made without departing from the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (9)
1. The preparation method of the eggplant porous carbon is characterized by comprising the following steps:
step one, carrying out acid liquor soaking and activating treatment on peeled and cut eggplants after alkali liquor treatment;
step two, freeze-drying the eggplants subjected to the activation treatment in the step one to obtain an eggplant cavernous body;
and step three, pre-oxidizing the eggplant cavernous body, heating to 450-550 ℃, preserving heat, carbonizing, washing and drying to obtain the eggplant porous carbon.
2. The preparation method of eggplant porous carbon according to claim 1, wherein the alkaline solution in the first step is treated with sodium hydroxide with a concentration of 0.5-2g/L for 3.5-4.5h.
3. The preparation method of eggplant porous carbon according to claim 1, wherein the acid soaking activation treatment is carried out by soaking eggplant pieces in 10-30vol% phosphoric acid solution for 12h.
4. The preparation method of eggplant porous carbon according to claim 1, wherein the freeze-drying time is 35-40h.
5. The preparation method of eggplant porous carbon according to claim 1, wherein the temperature of the pre-oxidation in the third step is 200 ℃ and the time is 90min.
6. The preparation method of eggplant porous carbon according to claim 1, wherein the temperature rise rate of the temperature rise to 450-550 ℃ in the third step is 4-6 ℃/min.
7. Eggplant porous carbon is characterized by being prepared by the preparation method of the eggplant porous carbon as claimed in any one of claims 1 to 6.
8. Use of eggplant porous carbon as claimed in claim 7 for adsorption treatment of printing and dyeing wastewater.
9. The application as claimed in claim 8, wherein the type of eggplant porous carbon used for adsorption treatment of dye in printing and dyeing wastewater comprises basic cationic dye, acid anion and dye reactive dye.
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| CN114560548A (en) * | 2022-02-08 | 2022-05-31 | 湖南大学 | Method for removing dye in water by activating persulfate through loofah sponge charcoal catalyst |
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Application publication date: 20221111 |