CN115140735A - Preparation method and application of passion fruit peel-based activated carbon - Google Patents
Preparation method and application of passion fruit peel-based activated carbon Download PDFInfo
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- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
Abstract
The invention provides a method for preparing activated carbon by using passion fruit peel as a material and application thereof, wherein the method comprises the following steps: s1, preparing raw materials: drying, crushing and sieving the passion fruit peel to obtain passion fruit peel particles; s2, high-temperature carbonization: placing the raw materials in a muffle furnace for carbonization primary treatment; s3, soaking by using an activating agent: mixing carbonized passion flower particles with an activating aqueous solution, wherein the activating aqueous solution is prepared by neutralizing and reacting phosphoric acid and a potassium hydroxide solution, and soaking after uniformly stirring to obtain a mixed product; s4, high-temperature activation: and (3) putting the mixed product into a muffle furnace for activation, cooling to obtain a crude product, washing with water, drying and sieving to obtain a target activated carbon product. The passion fruit peel active carbon prepared by the method has the advantages of no toxicity, single pore structure, proper specific surface area, high yield and the like, has the function of adsorbing cholesterol, is safe to human bodies and environment, and has simple preparation process conditions, low cost and considerable application prospect.
Description
Technical Field
The invention relates to the field of material preparation (the field of activated carbon), in particular to activated carbon prepared by taking passion fruit peel as a raw material and application thereof.
Background
The improvement of national dietary conditions and the change of travel modes cause the average serum total cholesterol level of people to be remarkably increased. Cholesterol is mainly taken in by food, and the diet of normal people contains about 300-500 mg of cholesterol, most of which is from meat, livestock viscera and egg yolk. Long-term intake of foods rich in cholesterol and saturated fatty acids can cause increased levels of cholesterol in the human liver, decreased synthesis of plasma Low Density Lipoprotein (LDL) receptors, decreased activity of LDL receptors, and decreased ability of LDL to transport cholesterol, resulting in decreased metabolism of cholesterol in the blood into liver cells, and ultimately, increased levels of cholesterol in the blood. A large number of domestic and foreign documents and clinical tests show that the cholesterol content and atherosclerotic diseases are closely related, and the rise of the low-density lipoprotein cholesterol (LDL-c) level is easy to generate the pathogenic risk of coronary heart disease and the risk of ischemic stroke.
Prevention of hypercholesterolemia can be through dietary intervention, exercise intervention, health education intervention, pharmaceutical intervention, and the like. Among them, dietary intervention is one of the most important measures to prevent hypercholesterolemia. By controlling the intake of fat and cholesterol in foods, polyphagia with foods that lower serum cholesterol such as citrus, garlic, red yeast rice, etc. will help to prevent and treat hypercholesterolemia. Studies such as bougainvillea spectabilis suggest that simple dietary control has significant statistical significance for the reduction of serum Total Cholesterol (TC) levels in patients. In addition, some medicines, such as statins and cholestyramine, can be used for treatment, but the medicines have serious side effects and are easy to cause myalgia, osteoporosis, depression and the like. Strengthening exercise, by burning fat in vivo, and accelerating blood circulation will help prevent cholesterol deposition on the vessel wall. In addition to reducing the intake of meat, animal viscera and egg yolk in dietary intervention, the multi-food has the function of reducing the intake of serum cholesterol, and can also reduce the intake of cholesterol by adsorbing the cholesterol in the foods through activated carbon. The activated carbon has the characteristics of good effect, high efficiency and the like in absorbing cholesterol in food, not only retains the original taste of the ingested food, but also can reduce the content of cholesterol and prevent hypercholesterolemia. Until now, no related art has utilized activated carbon to adsorb cholesterol in foods, so the present invention is novel and innovative.
The commonly used preparation method of the activated carbon comprises two processes of carbonization and activation, and the activation method comprises chemical activation, physical activation and a combination method of the chemical activation and the physical activation. In physical activation, activation gas such as air or carbon dioxide is usually used for activation, the surface of the carbon substrate is corroded under high temperature conditions, and the morphology and the pore structure are changed accordingly. The temperature required in the physical activation process is high, so that the carbon-based surface is easily seriously burnt, and the carbon yield is reduced. Physical activation is mainly used for preparing microporous activated carbon, and has the defect of high energy consumption at high temperature, which is contrary to carbon neutralization and carbon peak reaching. Chemical activation involves the use of alkali metals, acids and salts, such as phosphoric acid, potassium hydroxide, sodium hydroxide, zinc chloride, and the like. The swelling, dehydration and aromatic condensation of the activated carbon and carbon occur in the chemical activation process, and a large amount of uniform mesoporous structures and higher specific surface areas are formed. The chemical activation has the advantages of low energy consumption and high efficiency. The preparation cost is low by taking the passion flower skin-based activated carbon as the porous carbon-containing adsorption material, the sustainable green development is facilitated, the economic value of passion flower can be improved, the 'turning waste into wealth' can be realized, more contribution is made to the life health, and the method is a significant research direction.
Disclosure of Invention
In view of the above, a method for preparing activated carbon by using passion fruit peel as a raw material is provided, and the defects of the prior art are overcome.
The technical scheme of the invention is realized as follows:
a method for preparing activated carbon by using passion fruit peel as a material comprises the following steps:
s1, preparing raw materials: oven drying, pulverizing, sieving, and sieving to obtain 50-200 mesh powder;
s2, high-temperature carbonization: placing the passion fruit peel powder obtained in the step S1 into a muffle furnace for primary carbonization treatment, wherein the carbonization temperature is 800 ℃, the carbonization time is 4h, and the heating rate is 5 ℃/min, so as to obtain carbonized passion fruit peel particles;
s3, soaking by using an activating agent: mixing the carbonized passion fruit peel powder particles obtained in the step S2 with an aqueous solution of an activator, wherein the aqueous solution of the activator is prepared from phosphoric acid and potassium hydroxide, and the concentration of the phosphoric acid in the aqueous solution of the activator is 30% and the concentration of the potassium hydroxide in the aqueous solution of the activator is 0.1mol/L; the mass volume ratio kg/L of the passion fruit peel powder particles to the activator aqueous solution is 1:4, uniformly stirring, and then, keeping the total soaking time to be 1h to obtain a mixed product;
s4, high-temperature activation: putting the activated mixed product obtained in the step S3 into a muffle furnace for activation, wherein the activation temperature is increased to 800 ℃ at the heating rate of 5 ℃/min, the activation time is 4 hours, and finally, the muffle furnace is cooled to 50 ℃ and then the product is taken out to obtain a crude product;
s5, finished product: and (4) carrying out acid washing, water washing and drying on the crude product obtained in the step (S4), and sieving to obtain an activated carbon product with 50-200 meshes.
S6, finished product application test: comparing the finished activated carbon obtained in S5 with commercial activated carbon, taking cholesterol adsorption as an example, DPPH free radical clearance rate, methylene blue adsorption values under different concentrations, cholesterol adsorption values under different concentrations, specific surface area, infrared spectrogram and diffraction pattern of passion fruit peel-based and commercial activated carbon are measured.
Further, in step S1, the passion fruit peel is dried until the water content is 5 percent.
Further, in step S1, the mesh number of the sieve is 50 meshes.
Further, in step S2, the temperature is raised to 800 ℃ at a temperature rise rate of 5 ℃/min to carry out carbonization.
Further, in step S3, the soaking temperature is 25 ± 2 ℃.
Further, in step S4, the temperature is raised to 400 ℃ at a temperature rise rate of 5 ℃/min for activation.
Further, in step S5, the activated carbon product with 50-200 meshes is obtained by sieving.
Compared with the prior art, the invention has the beneficial effects that:
(1) The method adopts passion fruit peel to prepare the active carbon, carries out primary carbonization at a specific carbonization temperature condition (800 ℃), then uses a certain amount of phosphoric acid and potassium hydroxide compound activator aqueous solution to soak the active carbon, carries out activation at a specific activation temperature condition, and finally washes and dries the active carbon to prepare the passion fruit-based active carbon. The preparation method has the characteristics of low energy consumption and simple operation, so the preparation method is suitable for wide application, can better adsorb cholesterol in food, and prevents hypercholesterolemia.
(2) The invention adopts specific activation temperature (400 ℃) and activation time (2 h) to further control the micropore and macropore structures of the active carbon.
(3) According to the invention, the carbonized passion flower peel particles are soaked in a certain amount of activating agent aqueous solution (consisting of phosphoric acid and potassium hydroxide) at normal temperature, so that the pore structure and the specific surface area of the carbonized carbon particles can be well enhanced, the ash content can be greatly reduced, the energy consumption is reduced, and the formation of multiple pores is facilitated. Phosphoric acid mainly plays a role in developing a small pore structure.
(4) The active carbon of the invention not only enables the passion fruit peel to be effectively utilized, thereby improving the economic value of the passion fruit; the active carbon has proper pore size and can effectively adsorb cholesterol in food.
(5) The preparation method of the active carbon is simple, the raw materials are easy to obtain, the cost is low, the preparation method is suitable for mass production, and the preparation cost for preparing the active carbon adsorbent can be effectively reduced.
Drawings
FIG. 1 scanning electron micrographs of passion fruit peel-based activated carbon (a) (500X), (b) (30,000X) and commercial activated carbon (c) (500X), (d) (70,000X);
FIG. 2 is a graph comparing the cholesterol adsorption rates of passion fruit peel-based activated carbon and commercial activated carbon;
FIG. 3 is a graph comparing the methylene blue adsorption values of passion fruit peel-based activated carbon and commercial activated carbon;
FIG. 4X-ray diffraction (XRD) patterns of a passion fruit peel-based activated carbon (a) and a commercial activated carbon (b);
FIG. 5 is a graph of infrared spectra (FTIR) of passion fruit peel-based activated carbon and commercial activated carbon;
FIG. 6 adsorption and desorption isotherms of Passiflora edulis pericarp-based activated carbon (a) and commercial activated carbon (b).
Detailed Description
In order that the technical contents of the invention may be better understood, specific examples are provided below to further illustrate the invention.
The experimental methods used in the examples of the present invention are all conventional methods unless otherwise specified.
The materials, reagents and the like used in the examples of the present invention are commercially available unless otherwise specified.
The technical features described below are explained based on typical embodiments and specific examples of the present invention, but the present invention is not limited to these embodiments and specific examples. It should be noted that:
in the present specification, the numerical range represented by "numerical value a to numerical value B" means a range including the end points of numerical values a and B.
In the present specification, "plurality" of "plural", and the like means a numerical value of 2 or more unless otherwise specified.
In the present specification, "%" denotes mass% unless otherwise specified.
In the present specification, the meaning of "may" includes both the meaning of performing a certain process and the meaning of not performing a certain process.
1.1 Experimental Equipment and Chemicals
Reagents such as phosphoric acid, methylene blue, hydrochloric acid and the like are all chemically pure; the passion fruit peel is directly sampled locally. An electrothermal blowing dry box, a tube furnace, a crucible, an electronic precision balance, a nitrogen bottle, a glass instrument and the like.
1.2 preparation of activated carbon
S1, preparing raw materials: washing selected passion fruit whole fruits with water to remove surface dirt, drying passion fruit peel until the water content is 5 percent, and the drying temperature is 80 +/-5 ℃, crushing the dried product, and sieving the crushed product with a 50-mesh sieve to obtain passion fruit peel particles;
s2, high-temperature carbonization: placing the passion fruit peel particles obtained in the step S1 into a muffle furnace for primary carbonization treatment, heating the muffle furnace from room temperature to 800 ℃ at a heating rate of 5 ℃/min from 20-30 ℃, preserving heat for carbonization for 4h, and finally cooling to room temperature to obtain carbonized passion fruit peel particles;
s3, soaking by using an activating agent: mixing the carbonized passion fruit peel powder particles obtained in the step S2 with an aqueous solution of an activator, wherein the aqueous solution of the activator is prepared from phosphoric acid and potassium hydroxide, and the concentration of the phosphoric acid in the aqueous solution of the activator is 30% and the concentration of the potassium hydroxide in the aqueous solution of the activator is 0.1mol/L; the mass volume ratio kg/L of the passion fruit peel powder particles to the activator aqueous solution is 1:4, uniformly stirring, and soaking at 25 +/-2 ℃ for 24 hours to obtain a mixed product;
s4, high-temperature activation: putting the activated mixed product obtained in the step S3 into a muffle furnace for activation, and heating the activation temperature to 800 ℃ at the heating rate of 5 ℃/min from the room temperature of 20-30 ℃ for heat preservation and activation for 4h; finally, cooling the muffle furnace to 50 ℃, and taking out a product to obtain a crude product;
s5, finished product: carrying out acid washing, water washing and drying on the crude product obtained in the step S4, and sieving to obtain a target activated carbon product; the method comprises the following specific operations: and repeatedly washing the prepared crude product with distilled water to remove other inorganic matters, drying at 65 +/-2 ℃ to constant weight, and sieving with a 50-mesh sieve to obtain the passionflower pericarp-based activated carbon product.
S6, finished product application test: comparing the finished activated carbon obtained in S5 with commercial activated carbon, taking cholesterol adsorption as an example, DPPH free radical clearance rate, methylene blue adsorption values under different concentrations, cholesterol adsorption values under different concentrations, specific surface area, infrared spectrogram and diffraction pattern of passion fruit peel-based and commercial activated carbon are measured.
1.3 results
(1) In order to understand the morphology of activated carbon, the morphology of the pyrolyzed activated carbon at different magnifications, microscopic surface morphology of the carbon samples was observed using a scanning electron microscope (Thermo Scientific Verios G4 UC, usa).
As shown in fig. 1, it can be observed that passion fruit peel-based activated carbon has a developed irregular surface and is rich in loose texture. Meanwhile, there are many abundant pore structures on the surface of the activated carbon, and many slit structures are formed. These slits help the cholesterol to migrate to the interior of the activated carbon, thereby enhancing the adsorption capacity. This is caused by the fact that during carbonization the activated carbon forms a preliminary network structure, which accelerates the further erosion of the pores and deeper pore structure during activation. The result shows that the passion flower pericarp-based activated carbon prepared by the method effectively increases the surface area of the activated carbon. Therefore, pyrolysis at 800 ℃ causes more pores to widen into macropores, and promotes the conversion of organic molecules into a developed porous structure.
(2) Calculating the yield, wherein the mass yield of the activated carbon is calculated according to the following formula:
wherein m is the actual weight of the product active carbon MS The actual weight of the passion fruit peel before the initial trial. The results show that the passion fruit peel-based activated carbon product of example 1, produced a yield of 35.77%.
(3) The methylene blue adsorption filter is an index for representing the adsorption capacity of the activated carbon, and the lower the concentration of the methylene blue is, the stronger the adsorption capacity of the prepared activated carbon is. The adsorption of passion fruit peel-based and commercial activated carbon on methylene blue solutions of different concentrations was tested with reference to the national standard GB/T12496.10-1999 for obtaining microscopic surface information of activated carbon. The results show (figure 2) that the passion flower pericarp based activated carbon product is effective in adsorbing low concentrations of methylene blue (0.1 mg/mL), but is not suitable for adsorbing high concentrations of methylene blue.
(4) The cholesterol solution adsorption is an index for representing the cholesterol adsorption effect of the activated carbon, and the lower the cholesterol concentration is, the better the effect of the prepared activated carbon is. The adsorption of passion fruit peel-based and commercial activated carbon to cholesterol solutions of different concentrations was tested for obtaining microscopic surface information of activated carbon. The results show (FIG. 3) that the passion flower pericarp based activated carbon product of example 1 is effective in adsorbing low concentrations of cholesterol (0.3 mg/mL), while the average concentration of cholesterol in liquid foods (e.g., milk) is 0.1 + -0.05 mg/mL.
(5) As shown in fig. 4, strong and weak diffraction peaks appear at 2 θ =25 ° and 2 θ =45 °, respectively. The experimental data of XRD show that graphite microcrystals exist in the activated carbon sample. The diffraction peak of the passion fruit peel-based activated carbon is sharper than that of the industrial activated carbon, the graphitization degree of the passion fruit peel-based activated carbon is proved to be greater than that of the industrial activated carbon, and the existence of the carbon is also indicated by the appearance of a broad peak between 22 degrees and 24 degrees. The four small sharp peaks at 2 θ =21-28 ° in the XRD pattern are derived from the high crystallinity of potassium compounds in activated carbon, with the main elements being C, O, si and K.
(6) As shown in FIG. 5, 3500cm -1 The nearby broad peak is an O-H stretching vibration region and also comprises>3500 cm -1 Absorption peak, 3300-3000cm -1 The weaker absorption peak in between can be the C-H group stretching vibration region, and 2350cm -1 Nearby absorption peaks are C-N or C = N groups. Furthermore, 1550cm -1 The nearby absorption peak is the characteristic absorption peak of C = C, 1500cm -1 The absorption peak is also a C-O-C telescopic vibration area, 1150cm -1 And 1080 cm -1 The nearby absorption peaks represent the presence of C-O and C-C groups, respectively, in the molecular structure of the activated carbon sample. Fingerprint areas 810, 740 and 510cm -1 The small absorption peak of (A) is a characteristic absorption peak of an industrial type activated carbon sample, and indicates that the carbon sample has C-S, C-Cl and C-Br groups. This is achieved byThese alkyl halide groups are present only in industrial type activated carbon, and have not been found in activated carbon prepared from passion fruit peel. Thus, the activated carbon prepared from pericarp is of low toxicity, and the C-O-C and CH groups in the activated carbon structure also demonstrate the presence of methoxy groups in the activated carbon sample.
(7) The structural characteristics of the solid sample were obtained using a specific surface area analyzer (amamerremike ASAP 2460, usa). Detection of N at Low temperature (77.35K) 2 Adsorption/desorption curves and pore characteristics. The specific surface area of the activated carbon was calculated according to BET (Brunauer-Emmett-Teller) and Langmuir equation:
the BET equation:
(for N) 2 )
Single Point BET equation (C)>>1)：V m ＝C×(1-P/P o )(4)
Langmuir equation:
(8) the t-plot method measures the external surface area, internal micropore surface area, total adsorption volume and total micropore (< 2 nm) volume of the active oxygen sample.
t-plot thickness curve equation:
(9) BJH (Barrett-Joiner-Halenda) is a method of calculating pore size distribution in porous materials using adsorption or desorption isotherms. The BJH adsorption/desorption isotherms were calculated according to Kelvin and Halsey equations:
the Kelvin equation:
halsey equation:
the experimental results show that the specific surface area of the passion fruit peel-based activated carbon is less than 10 times that of the commercial activated carbon, but the cholesterol adsorption effect is not inferior to that of the commercial activated carbon. The micro-particle activated carbon with large specific surface area (< 200 meshes) can completely adsorb chemical substances in liquid and is not suitable for adsorbing cholesterol in liquid diet. Although the specific surface and volume of the passion fruit pericarp-based activated carbon are smaller than those of the commercial type, there is not much difference in pore size between the pericarp and commercial type, and the most probable pore size of the pericarp-based activated carbon (2.25 nm) is slightly larger (2.19 nm) than that of the commercial type.
The adsorption and desorption isotherms of the passion fruit peel-based activated carbon prepared by the invention are shown in fig. 6, the adsorption of nitrogen in a low-pressure area is possibly related to the single-layer adsorption of micropores, and the adsorption quantity of nitrogen can reach 58.61cm 3 (ii) in terms of/g. A clear hysteresis loop (0.4) is observed in the region of the relative pressure<P/P 0 <1.0 This is considered to be characteristic of the small pore material. Phosphoric acid is a weak acid, has a poorer pore corrosion effect than a strong acid, and is estimated to be activated by strong acid corrosion of commercial activated carbon, and alkyl halide exists in a carbon structure, so that the commercial activated carbon is not suitable for adsorbing cholesterol in liquid diet. Multipoint BET specific surface area 111m of passion fruit peel-based active carbon 2 The concentration is enough to fully adsorb cholesterol in the liquid diet and reserve most nutrient substances.
The result shows that the passion fruit peel-based active carbon prepared by the method has larger particles (50-150 meshes), is suitable for selectively adsorbing cholesterol in liquid diet and human body, and can also be used as a food adsorbent; however, the commercial activated carbon lacks the characteristic of selective adsorption of cholesterol because the commercial activated carbon of fine particles has a large specific surface area and adsorption rate. Commercial activated carbon is mostly made of wood material and can adsorb almost all substances in water and air. The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
TABLE 1 surface area, pore volume and pore diameter of activated carbon samples
TABLE 2 pore volume and percent pore volume for different pore size ranges for activated carbon samples
Claims (10)
1. A preparation method of passion fruit peel-based activated carbon is characterized by comprising the following steps:
s1, preparing raw materials: oven drying Passiflora edulis pericarp (80 deg.C, 24 hr), pulverizing, sieving, and sieving to obtain Passiflora edulis pericarp powder with particle size of 50-200 meshes;
s2, high-temperature carbonization: placing the passion fruit peel powder obtained in the step S1 in a muffle furnace for primary carbonization treatment, wherein the carbonization temperature is 800 ℃, the carbonization time is 4h, and the temperature rise rate is 5 ℃/min, so as to obtain carbonized passion fruit peel powder;
s3, soaking by using an activating agent: mixing the passion fruit peel powder particles carbonized in the step S2 with an activator aqueous solution, wherein the activator aqueous solution is prepared by mixing phosphoric acid and potassium hydroxide, the concentration of the phosphoric acid in the activator aqueous solution is 30% and the concentration of the potassium hydroxide is 0.1mol/L, adding the phosphoric acid, soaking for 30min, and adding potassium hydroxide; the mass volume ratio kg/L of the passion fruit peel powder particles to the activator aqueous solution is 1:4, uniformly stirring and soaking for 30min at the room temperature of 25 +/-2 ℃ to obtain a mixed product;
s4, high-temperature activation: putting the activated mixed product obtained in the step S3 into a muffle furnace for activation, wherein the activation temperature is increased to 400 ℃ at the temperature increase rate of 5 ℃/min, the activation time is 2 hours, and finally, the muffle furnace is cooled to 50 ℃ and then the product is taken out to obtain a crude product;
s5, finished product: carrying out acid washing, water washing and drying on the crude product obtained in the step S4, and sieving to obtain an activated carbon product with 20-200 meshes;
s6, finished product application test: comparing the finished activated carbon obtained in the step S4 with commercial activated carbon, taking cholesterol adsorption as an example, determining DPPH free radical clearance rate, methylene blue adsorption values under different concentrations, cholesterol adsorption values, specific surface area, infrared spectrogram and diffraction pattern of passion fruit peel-based and commercial activated carbon.
2. The method for preparing activated carbon from passion fruit peel according to claim 1, wherein in step S1, the passion fruit peel is dried until the water content is-5%.
3. The method for preparing activated carbon from passion fruit peels as claimed in claim 1, wherein in the step S1, the mesh number of the sieve is 50 meshes.
4. The method for preparing activated carbon from passion fruit peels as claimed in claim 1, wherein in the step S2, the temperature is raised to 800 ℃ at a temperature raising rate of 5 ℃/min for carbonization.
5. The method for preparing activated carbon from passion fruit peels as claimed in claim 1, wherein in the step S3, the soaking temperature is 25 +/-2 ℃.
6. The method for preparing activated carbon from passion fruit peels as claimed in claim 1 or 4, wherein in the step S4, the temperature is raised to 400 ℃ at a temperature raising rate of 5 ℃/min for activation.
7. The method for preparing activated carbon from passion fruit peels as claimed in claim 1, wherein in the step S5, the activated carbon product with 50-200 meshes is obtained by sieving.
8. The method of claim 1, wherein 0.3-3.0mg/mL of cholesterol is adsorbed by passion fruit peel-based activated carbon in step S6.
9. An activated carbon based on passion fruit peel produced by the production method according to any one of claims 1 to 8.
10. Use of a passion fruit peel-based activated carbon as claimed in claim 9 in the fields of food adsorption and chemical industry.
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