CN113289576A - Lotus seedpod hydrothermal carbon and preparation method and application thereof - Google Patents
Lotus seedpod hydrothermal 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
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- 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
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4843—Algae, aquatic plants or sea vegetals, e.g. seeweeds, eelgrass
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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
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
Abstract
The invention discloses lotus seed pot hydrothermal carbon and a preparation method and application thereof. The preparation method of the lotus water-heating charcoal comprises the following steps: mixing lotus seed pot powder with water, carrying out hydrothermal reaction for 8-12 h at 160-200 ℃, cooling to room temperature, washing with water, filtering, and drying to obtain lotus seed pot hydrothermal carbon. The lotus seed pot is used as a raw material, and the lotus seed pot hydrothermal carbon is prepared through a simple hydrothermal process, so that the resource utilization rate of the lotus seed pot is improved; the obtained lotus water-heating carbon has good adsorption effect on quinoline in water, and can be applied to treatment of quinoline in wastewater.
Description
Technical Field
The invention relates to the technical field of wastewater treatment, and particularly relates to lotus seed pot hydrothermal carbon and a preparation method and application thereof.
Background
Quinoline is a heterocyclic compound with aromaticity, is toxic, and can cause symptoms such as headache, dizziness, nausea and the like after being inhaled; it has irritation to eyes and skin; oral administration can stimulate oral cavity and stomach, and has strong teratogenicity and carcinogenicity. Quinoline is a relatively difficult component in coal chemical wastewater, and can cause immeasurable damage to human beings, animals and plants when being discharged randomly, so that the quinoline removal method is very important for removing quinoline in industrial wastewater.
At present, three technologies of biological method, adsorption method and advanced oxidation are mainly used for adsorbing quinoline in wastewater. The adsorption method belongs to a physical process, can not decompose quinoline, is suitable for wastewater with low quinoline wastewater content, is simple to operate and takes less time, and the adsorbent can be recycled after treatment.
The hydrothermal carbon is a black solid product which is prepared by taking biomass or components thereof as a raw material, taking water as a solvent and a reaction medium and carrying out hydrothermal reaction at 150-375 ℃ and autogenous pressure, takes carbon as a main body and is rich in oxygen-containing functional groups, and generally has large specific surface area and high porosity, so that the black solid product has good adsorbability, and can be widely applied to adsorption of heavy metal ions and atmospheric pollutants.
The lotus seed pot is dried receptacle of lotus seed of Nymphaeaceae. Harvesting the mature fruit in autumn, removing the fruit, drying in the sun, and making the fruit into an inverted cone shape or a funnel shape, wherein the fruit is torn mostly, the diameter of the fruit is 5-8 cm, and the height of the fruit is 4.5-6 cm. The lotus seed pot has grayish brown to purple brown surface, fine longitudinal lines and wrinkles, most circular holes on the top surface, peduncle residues on the base part, loose texture, broken sponge-like shape, brown color, slight smell and slightly astringent taste, only a few lotus seed pots are used as traditional Chinese medicines at present, and most lotus seed pots are thrown away. At present, no report exists for preparing the lotus seedpod into hydrothermal carbon for adsorbing quinoline in wastewater.
Disclosure of Invention
In view of the above, a need exists for a lotus seedpod hydrothermal carbon, and a preparation method and an application thereof, so as to solve the technical problems of high treatment difficulty of quinoline-containing wastewater and low utilization rate of lotus seedpod resources in the prior art.
The first aspect of the invention provides a preparation method of lotus water-heating charcoal, which comprises the following steps:
mixing lotus seed pot powder with water, carrying out hydrothermal reaction for 8-12 h at 160-200 ℃, cooling to room temperature, washing with water, filtering, and drying to obtain lotus seed pot hydrothermal carbon.
The second aspect of the invention provides lotus seedpod hydrothermal carbon which is obtained by the preparation method of lotus seedpod hydrothermal carbon provided by the first aspect of the invention.
The third aspect of the invention provides application of lotus seedpod hydrothermal carbon in adsorption of quinoline in wastewater, and the lotus seedpod hydrothermal carbon is obtained by the preparation method of lotus seedpod hydrothermal carbon provided by the first aspect of the invention.
Compared with the prior art, the invention has the beneficial effects that:
the lotus seed pot is used as a raw material, and the lotus seed pot hydrothermal carbon is prepared through a simple hydrothermal process, so that the resource utilization rate of the lotus seed pot is improved; the obtained lotus water-heating carbon has good adsorption effect on quinoline in water, and can be applied to treatment of quinoline in wastewater.
Drawings
FIG. 1 is an SEM image of lotus seedpod powder;
FIG. 2 is an SEM micrograph of lotus seedpod hydrothermal carbon;
FIG. 3 is an SEM high power image of lotus water hot carbon;
FIG. 4 is an infrared spectrum of lotus seed pot powder and lotus seed pot hydrothermal charcoal.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The first aspect of the invention provides a preparation method of lotus water-heating charcoal, which comprises the following steps:
mixing lotus seed pot powder with water, carrying out hydrothermal reaction for 8-12 h at 160-200 ℃, cooling to room temperature, washing with water, filtering, and drying to obtain lotus seed pot hydrothermal carbon.
In the embodiment, the lotus seed pot powder is obtained by drying, crushing and sieving a lotus seed pot with a 80-mesh sieve.
In the present embodiment, the ratio of the lotus seed pot powder to the water is (1-5) g:20ml, preferably 3 g:20 ml.
In this embodiment, the temperature of the hydrothermal reaction is 180 ℃ and the time of the hydrothermal reaction is 10 hours. Under the condition, the obtained lotus aqueous heating carbon has the optimal adsorption effect on quinoline.
In this embodiment, the steps of washing and filtering are specifically: and washing and filtering the cooled water-heated charcoal, wherein the color of the filtrate in the filter flask is bright yellow when the filtration is started, and washing and filtering the filtrate by using distilled water until the color of the filtrate is only slightly yellowish until the filtrate is colorless.
In the embodiment, the drying temperature is 60-120 ℃, and the drying time is 4-12 h.
In this embodiment, the preparation method of the lotus water-heating carbon further comprises grinding the dried hydrothermal carbon, and sieving the ground hydrothermal carbon with a 80-mesh sieve to obtain the lotus water-heating carbon.
The second aspect of the invention provides lotus seedpod hydrothermal carbon which is obtained by the preparation method of lotus seedpod hydrothermal carbon provided by the first aspect of the invention.
The third aspect of the invention provides application of lotus seedpod hydrothermal carbon in adsorption of quinoline in wastewater, and the lotus seedpod hydrothermal carbon is obtained by the preparation method of lotus seedpod hydrothermal carbon provided by the first aspect of the invention.
In this embodiment, the pH of the wastewater is 3 to 5. Within the pH range, the adsorbent has a good adsorption effect. Preferably, the pH of the wastewater is 3. When the pH value of the wastewater is 3, the adsorption effect on quinoline in the wastewater is optimal.
Example 1
Drying and crushing the lotus seed pot, and sieving the lotus seed pot with a 80-mesh sieve to obtain lotus seed pot powder; weighing 15g of lotus seed pot powder, putting the lotus seed pot powder into a stainless steel high-pressure reaction kettle, adding 100ml of distilled water, stirring, uniformly mixing, putting the mixture into the reaction kettle, adjusting the temperature of the reaction kettle to 180 ℃, heating and reacting for 10 hours at the temperature, and then cooling to room temperature; washing and filtering the cooled water-heated carbon, wherein the color of the filtrate in the filter flask is bright yellow when the filtration is started, and the filtrate is washed and filtered by distilled water when the color of the filtrate is only slightly yellowish until the filtrate is colorless; and (3) drying the filtered hydrothermal carbon in an oven at 100 ℃ for 8h, grinding the dried hydrothermal carbon, and sieving by a 80-mesh sieve to obtain the lotus water-heating carbon.
Referring to fig. 1-3, fig. 1 is an SEM image of lotus seed pot powder, and fig. 2-3 are SEM images of lotus seed pot hydrothermal charcoal under different magnifications. As can be seen from figure 1, the lotus seed pot powder surface presents the characteristics of regularity and compactness, the lotus seed pot powder becomes loose from compactness after hydrothermal carbonization, the surface is rough, and a pore structure with different sizes and distributions is formed, and the pore structure is favorable for adsorption of hydrothermal carbon.
Referring to FIG. 4, FIG. 4 is a chart showing the infrared spectra of lotus seedpod and lotus seedpod hydrothermal charcoal. The adsorption capacity of the hydrothermal carbon is related to surface functional groups, and the richer the surface functional groups are, the more beneficial the organic pollutant removal is. As can be seen from FIG. 4, the thickness is 3000-3600 cm-1Has a wide and strong absorption peak mainly due to stretching vibration of-OH, which shows that the lotus aqueous hot carbon contains a large amount of oxygen-containing functional groups such as hydroxyl, carbonyl, carboxyl and the like, and is 3000-3600 cm-1the-OH peak in the range is enhanced, which is beneficial to the adsorption of organic matters. In the figure at 1618cm-1、1522cm-1、1442cm-1The left characteristic peak and the right characteristic peak are characteristic absorption peaks of a benzene ring structure, and are reflected in infrared spectrograms of the lotus seedpod powder and the hydrothermal carbon, which shows that the benzene ring structure in the lotus seedpod powder is relatively stable. At 1063cm-1The peak of stretching vibration of carbonyl group in aromatic ring is 780cm-1And 669cm-1The absorption peaks with obvious carbon chain intervals prove the existence of the oxygen-containing functional groups of the cellulose.
Test group
Scanning the whole wave band of 20mg/L quinoline solution, measuring a series of quinoline solutions with known concentration c at the maximum absorption wavelength of 306nmThe absorbance A of (a) is plotted by taking the concentration c as an abscissa and the absorbance A of the solution as an ordinate, and a graph of the relationship of A to c is drawn. The standard curve of the quinoline aqueous solution is obtained by fitting, wherein y is 0.01527x +0.02364, R20.9995. As can be seen from FIG. 1, the concentration and absorbance of the quinoline solution conform to Lambert-beer's law, so that the remaining quinoline concentration of the solution can be calculated from the absorbance of the filtrate.
The calculation formula of the adsorption rate and the unit adsorption amount is as follows:
E＝(Ct–C0)/C*100；
Q＝(Ct–C0)*V/m；
wherein E represents an adsorption rate (%); q is the unit adsorption amount (mg. g)-1)；C0Is the initial concentration (mg. L) of solute in the solution-1)；CtThe residual concentration of solute in the solution at time t; v is the volume of solution adsorbed (L); m is the mass (g) of the adsorbent.
(1) Influence of the amount of adsorbent added on the adsorption effect
Ten sets of 50mL quinoline solutions having a concentration of 50mg/L were prepared, pH was controlled to 3, and 0.05g, 0.1g, 0.15g, 0.2g, 0.25g, 0.3g, 0.35g, 0.4g, 0.45g, 0.5g of lotus seedpod hydrothermal charcoal were added in an amount of 1g/L, 2g/L, 3g/L, 5g/L, 6g/L, 7g/L, 8g/L, 9g/L, 10g/L, respectively, and the mixture was placed in a constant temperature water bath kettle at a temperature of 30 ℃ and a rotational speed of 100rad/min to carry out a constant temperature reaction for 90min, after filtration, an adsorbed quinoline aqueous solution was obtained, and the absorbance of the reacted solution was measured with an ultraviolet spectrophotometer, and the results are shown in Table 1.
TABLE 1 influence of hydrothermal carbon dosage on adsorption Effect
As can be seen from FIG. 2, the adsorption rate of quinoline gradually increased as the amount of hydrothermal carbon added to the lotus seedpot increased. As the amount of adsorbent added increased from 1g/L to 3g/L, the removal rate of quinoline adsorption increased from 44.42% to 75.88% before reaching equilibrium. Because the number of the adsorption sites of quinoline is in direct proportion to the number of the adsorbents used in the measurement, the number of the active sites can be increased by increasing the adding amount of the lotus seedpod hydrothermal carbon adsorbent, so that the number of the prepared hydrothermal carbon adsorption quinoline is increased approximately linearly. When the addition amount is more than or equal to 3g/L, the increase of the adsorption rate is not obvious, which indicates that the quinoline and the adsorption site are close to the adsorption balance at the moment. The results show that 3g/L of the prepared lotus seedpod hydrothermal carbon is sufficient for optimal removal of quinoline from water. Therefore, when the subsequent experiments are not specially explained, the adding amount of the hydrothermal carbon of the lotus seedpod in the adsorption experiments is 3 g/L.
(2) Influence of pH on the adsorption Effect
Preparing 12 groups of 50mL quinoline solution with the concentration of 50mg/L, controlling the adding amount of hydrothermal carbon to be 3g/L, namely 0.15g, respectively controlling the pH of the solution to be 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11 and 12, putting the solution into a constant-temperature water bath kettle, setting the temperature to be 30 ℃, rotating the speed to be 100rad/min, reacting for 90min at a constant temperature, filtering to obtain adsorbed quinoline aqueous solution, and measuring the absorbance of the reacted solution by using an ultraviolet spectrophotometer. The results are shown in Table 2.
TABLE 2 influence of pH on the adsorption Effect
As can be seen from table 2, the adsorption rate of quinoline increases and then gradually decreases as the pH of the solution increases. The removal rate of quinoline adsorption increased from 25.76% to 76.90% when the pH increased from 1 to 3, reaching a maximum at pH 3; when the acidity is gradually weakened, the adsorption rate and the unit adsorption amount are also gradually reduced, and when the solution is close to neutrality, the adsorption rate and the unit adsorption amount are maintained at a stable platform; when the alkalinity of the solution is gradually increased, the adsorption rate and the unit adsorption amount are reduced. It can be known that the lotus aqueous hot charcoal has strong pH dependence on the adsorption of quinoline. When the pH value is 3-5, the prepared lotus seedpod hydrothermal carbon has a large adsorption potential to quinoline, and the preferred value is 3.
(3) Influence of adsorption time on adsorption Effect
Nine sets of 50mL quinoline solutions with a concentration of 50mg/L were prepared, the amount of hydrothermal charcoal added was 3g/L, that is, 0.15g, and the pH of the solution was controlled to 3. Placing into a constant temperature water bath kettle, setting the temperature at 30 deg.C and the rotation speed at 100 rad/min. Controlling the reaction time of each group to be 5, 10, 20, 40, 80, 90, 120, 150 and 180min respectively, and filtering to obtain the adsorbed quinoline aqueous solution. The absorbance of the reacted solution was measured by an ultraviolet spectrophotometer, and the results are shown in Table 3.
TABLE 3 influence of adsorption time on the adsorption Effect
As can be seen from Table 3, the removal rate and the adsorption amount of quinoline sharply increase with time in the first 30min, and the removal rate of quinoline is 80.18% when the contact time reaches 120 min; after 120min, both remained substantially constant. The reason is that in the initial adsorption stage, the surface of the hydrothermal carbon has more adsorption active centers, quinoline in a solution can be quickly adsorbed, and in the initial 30min, the adsorption rate and the adsorption quantity are increased rapidly due to more active adsorption sites on the surface; when the adsorption time reaches 120min, the active adsorption sites on the surface of the hydrothermal carbon tend to be saturated, and the adsorption and desorption behaviors and the speed of quinoline reach dynamic balance, so that the adsorption rate and the adsorption quantity are kept at a relatively stable level. Therefore, the optimal adsorption time of the lotus aqueous hot carbon on quinoline is 120 min.
(4) Effect of initial concentration of quinoline solution on adsorption Effect
13 sets of 50mL quinoline solutions were prepared, the concentrations of which were 20, 30, 40, 50, 60, 70, 80, 90, 100, 120, 140, 160, and 180mg/L, the amount of hydrothermal charcoal added was 3g/L, that is, 0.15g, and the pH of the solution was controlled to 3. Placing into a constant temperature water bath kettle, setting the temperature at 30 deg.C and the rotation speed at 100 rad/min. Controlling the reaction time for 120min, and filtering after the reaction is finished to obtain the adsorbed quinoline aqueous solution. The absorbance of the reacted solution was measured by an ultraviolet spectrophotometer, and the results are shown in Table 4.
TABLE 4 Effect of initial concentration on adsorption Effect
As can be seen from table 4, the unit adsorption amount of quinoline gradually increased and the adsorption rate gradually decreased with the increase in the initial concentration. When the initial concentration of quinoline is low, the unit adsorption amount of quinoline increases more as the initial concentration increases. When the initial concentration reaches 140mg/L, the unit adsorption amount reaches a peak value, and the hydrothermal carbon reaches saturated adsorption, the adsorption amount is 29.8951mg/g, the hydrothermal carbon tends to be balanced around 30mg/g, the adsorption rate is 64.06%, and the adsorption rate is continuously reduced along with the increase of the initial concentration. Therefore, the optimal initial concentration of the lotus aqueous hot carbon to quinoline is 140 mg/L.
As can be seen from the comprehensive tables 1-4, the surface of the lotus seedpod hydrothermal carbon prepared by the method contains abundant surface functional groups, and when the lotus seedpod hydrothermal carbon is used as an adsorbent for quinoline in water, the addition amount of the adsorbent, the pH value of a quinoline solution, the adsorption time and the initial quinoline concentration all have great influences on the adsorption rate and the adsorption amount. The result shows that under the conditions that the adding amount of the lotus seedpod hydrothermal carbon is 3g/L, the pH value is 3.0 and the reaction time is 120min, the optimal adsorption removal rate can reach 64.06% and the highest adsorption amount is 30mg/L for 50ml of quinoline solution with the initial concentration of 140mg/L, which indicates that the low-cost lotus seedpod hydrothermal carbon obtained from abundant natural resources can be used as an effective adsorbent for removing quinoline in wastewater, the preparation process is simple and the adsorption effect is good.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (10)
1. A preparation method of lotus water-heating charcoal is characterized by comprising the following steps:
mixing lotus seed pot powder with water, carrying out hydrothermal reaction for 8-12 h at 160-200 ℃, cooling to room temperature, washing with water, filtering, and drying to obtain lotus seed pot hydrothermal carbon.
2. The preparation method of lotus seedpod water-heating charcoal as claimed in claim 1, wherein the usage ratio of lotus seedpod powder to water is (1-5) g:20 ml.
3. The preparation method of lotus seedpod hydrothermal charcoal as claimed in claim 2, wherein the ratio of lotus seedpod powder to water is 3 g:20 ml.
4. The method for preparing lotus water-heated carbon as claimed in claim 1, wherein the temperature of the hydrothermal reaction is 180 ℃ and the time of the hydrothermal reaction is 10 h.
5. The method for preparing lotus water-heated carbon as claimed in claim 1, wherein the steps of water washing and filtering are specifically as follows: and washing and filtering the cooled water-heated charcoal, wherein the color of the filtrate in the filter flask is bright yellow when the filtration is started, and washing and filtering the filtrate by using distilled water until the color of the filtrate is only slightly yellowish until the filtrate is colorless.
6. The method for preparing lotus aqueous hydrothermal carbon as claimed in claim 1, further comprising grinding the dried hydrothermal carbon and sieving with a 80-mesh sieve to obtain lotus aqueous hydrothermal carbon.
7. A lotus seedpod hydrothermal charcoal obtained by the preparation method of the lotus seedpod hydrothermal charcoal as claimed in any one of claims 1-6.
8. The use of the lotus water-heated carbon of claim 7 in the adsorption of quinoline in wastewater.
9. The application of the lotus water-heated carbon in adsorbing quinoline in wastewater as claimed in claim 8, wherein the pH of the wastewater is 3-5.
10. The use of lotus water thermal carbon according to claim 9 for adsorbing quinoline in wastewater, wherein the pH of the wastewater is 3.
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| CN110773124A (en) * | 2019-11-06 | 2020-02-11 | 天津城建大学 | Preparation method and application of coffee grounds hydrothermal carbon adsorbent |
| CN110817864A (en) * | 2019-11-22 | 2020-02-21 | 上海工程技术大学 | Plant-based activated carbon and preparation method and application thereof |
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| CN110773124A (en) * | 2019-11-06 | 2020-02-11 | 天津城建大学 | Preparation method and application of coffee grounds hydrothermal carbon adsorbent |
| CN110817864A (en) * | 2019-11-22 | 2020-02-21 | 上海工程技术大学 | Plant-based activated carbon and preparation method and application thereof |
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