CN103877934A - Method for preparing porous carbon material from bean dregs and application of porous carbon material serving as adsorbent in wastewater treatment - Google Patents
Method for preparing porous carbon material from bean dregs and application of porous carbon material serving as adsorbent in wastewater treatment Download PDFInfo
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- CN103877934A CN103877934A CN201410117797.3A CN201410117797A CN103877934A CN 103877934 A CN103877934 A CN 103877934A CN 201410117797 A CN201410117797 A CN 201410117797A CN 103877934 A CN103877934 A CN 103877934A
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Abstract
The invention discloses a method for preparing a porous carbon material from bean dregs. The method comprises the following steps: washing wet bean dregs by using distilled water, soaking in an alcoholic solution for 3-48 hours, filtering, and drying so as to obtain dried bean dregs; impregnating the dried bean dregs in an activating agent solution for 5-30 hours, and carbonizing at the temperature of 300-800 DEG C for 0.5-5 hours after filtering; cooling to the room temperature, washing by using a hydrochloric acid solution, and washing to be neutral by using the distilled water, and drying to obtain the amorphous carbon material which has the huge specific surface area and is porous. The experiments prove that the porous carbon material has the characteristics of high adsorptive power, high adsorption capacity and high decolorization ratio on organic cationic dyes in wastewater, and can be used for adsorbing and removing methylene blue and other organic dyes in the wastewater.
Description
Technical field
The invention belongs to technical field of macromolecules, relate to a kind of preparation method of natural polymer base porous carbon material, relate in particular to a kind of method of utilizing bean dregs to prepare porous carbon material; The present invention's this porous carbon material application in wastewater treatment as adsorbent simultaneously.
Background technology
Porous carbon material refers to the carbon based material with different pore structures, and its aperture can change at the nano level superfine micropore suitable with absorption molecular dimension to the wider scope of the micron order pore that is suitable for microbial growth and activity.Porous carbon material has flourishing pore structure and high specific area, and good acid-proof alkaline is widely used in fields such as water purification, separation, catalyst carrier, double layer capacitor, sensor and gas storage.
The preparation method of porous carbon material is varied, and wherein activation method is to prepare the conventional method of porous carbon material, comprises (a) chemical activation, physically activated or physical chemistry activation coupling; (b) catalytic activation of carbon precursor can charing and the high molecular polymer mixing charing of pyrolysis; (c) charing of polymer aerogel; (d) carbonization-activation of living beings.What utilize that these traditional carbonization-activation methods make is unordered porous carbon material mostly.In addition, it is various that traditional activation method is prepared the raw material type of porous carbon material, as long as can obtain charcoal and all can be used as the raw material of synthesizing porous charcoal.Therefore, mainly contain four classes such as biological material, synthesized polymer material, polymeric scrap material, tar and coal material.
Bean dregs are the insoluble sludges that produce in the bean product production processes such as soya-bean milk, soya-bean milk and bean curd producing.Bean dregs are as the refuse producing in bean product manufacture craft, and output is very large.Bean dregs are a kind of nontoxic, bio-compatible, edible natural polymer, bean dregs are as the accessory substance in bean product production, output is very large, but due to the inconvenience in its perishability and storage transportation, most bean dregs are all gone out of use, do not realize its value, economic benefit is low, and to environment.The main component of bean dregs has cellulose, protein, lipid, minerals and vitamins etc.Therefore, can it be raw material, by being prepared into Carbon Materials after chemical activation, charing, can not only realize the recycling of resource, reduce the pollution to environment, the more important thing is and can improve its economic use value.
Summary of the invention
The object of the invention is, for some problems that exist in prior art, provides a kind of method of utilizing bean dregs to prepare porous carbon material.
Another object of the present invention is to provide the above-mentioned porous carbon material application in wastewater treatment as adsorbent that utilizes bean dregs to prepare for raw material.
(1) preparation of porous carbon material
Utilizing bean dregs to prepare the method for porous carbon material, is by after wet bean dregs distilled water washing, soaks 3～48 h in ethanolic solution or methanol solution, filters, dry, obtains dry bean dregs; Again dry bean dregs are flooded to 5～30 h in activator solution, filter; Then charing 0.5～5 h at 300～800 ℃; Be cooled to room temperature, first with hydrochloric acid solution washing, then be washed till neutrality with distilled water, dry, obtain porous charcoal sorbing material.
Described wet bean dregs are the insoluble sludge producing in production process of bean products; Described activator adopts the K of quality 10～80%
2cO
3or H
3pO
4solution.
(2) structure and properties of porous carbon material
Structure, character by FT-IR, nitrogen adsorption desorption isotherm and SEM to bean dregs base porous carbon material characterize and analyze.
1, FT-IR analyzes
Fig. 1 is the infrared spectrogram of bean dregs base porous carbon material of the present invention, and wherein curve 1 is dry bean dregs, and curve 2 is porous carbon material.As seen from the figure, main absworption peak 3422 cm of dry bean dregs
-1it is the stretching vibration absworption peak of alcohol, phenol-OH; 2925 and 2855 cm
-1be-stretching vibration peak of CH; 1061 and 794 cm
-1respectively C-O-C and the C-H vibration absorption peak of fiber prime ring; 1744 and 1647 cm
-1the characteristic absorption peak of carbonyl, 1417 cm
-1it is the stretching vibration peak of C-O in carboxyl.Bean dregs three major polymers: cellulose, the compositions such as lignin, mainly contain oxygen-containing functional group in cellulose, be present in as hydroxyl, in ether and carbon back.In porous carbon material, 3433 cm
-1be-the stretching vibration absworption peak of OH; 1594 cm
-1belong to the stretching vibration of C-O; 1253 cm
-1belong to C-O-C vibration absorption peak.Correlation curve 1,2 can find out, the most of organo-functional group in bean dregs has all lost after charing.The oxygen-containing functional groups such as hydroxyl, carboxyl, lactone group all may be contained in porous carbon material surface.
2, pore structure analysis (nitrogen adsorption desorption isotherm)
Fig. 2 is the nitrogen adsorption desorption figure of the porous carbon material prepared of the present invention.As seen from Figure 2, nitrogen Adsorption and desorption isotherms is I type adsorption isotherm, belongs to the mono layer adsorption of typical microporous solids.Specific area can be by BET(Brunauer – Emmett – Teller) formula calculates, and the porous carbon material specific area obtaining can reach 1455.406 m
2/ g, can find out by the pore-size distribution in figure, micropore size is distributed between 1.17 ~ 1.85 nm, and contains the mesoporous of some between 2.21 ~ 2.64 nm, and its average pore size is 1.41 nm.The porous carbon material that shows preparation has very high specific area and abundant microcellular structure, makes it have good absorption property to dye molecules such as methylene blues.
3, sem analysis
Fig. 3 is the ESEM of the porous carbon material of the present invention's preparation.As can be seen from Figure 3, the porous carbon material after activated dose of activation charing is porous honeycomb.When bean dregs flood in activator, with reacting of activator generation series of complex, make the microstructure of the charcoal formation porous in bean dregs, through the strong calcination of high temperature, obtain having huge specific area, be cavernous amorphous carbon material, and the existence of huge specific area porous is more conducive to the absorption to methylene blue.
(3) absorption property of porous carbon material adsorbent
Adsorption test to containing methylene blue simulated wastewater: getting containing methylene blue concentration is simulated wastewater 50 mL of 300 mg/L, pH=6 ~ 7.In simulated wastewater, add the present invention to prepare porous carbon material adsorbent, the initial amount that adds of adsorbent is 0.05 g/L, mixed liquor 30 min of constant temperature oscillation waste water and bean dregs base porous carbon material adsorbent, leave standstill, suction filtration, measures the concentration of remaining methylene blue, calculates percent of decolourization.
Test result: adsorbent consumption is 0.05 g/L, after room temperature (25 ℃) vibration absorption 30 min, adsorption effect the best, percent of decolourization is 97.7%, adsorption capacity reaches 295.8 mg/g, reaches national grade one discharge standard.
In sum, the present invention utilizes porous carbon material prepared by bean dregs to have good absorption property to the methylene blue in waste water, therefore, can be used for processing the organic cation dye waste water containing methylene blue.
Accompanying drawing explanation
Fig. 1 is the infrared spectrogram of the porous carbon material prepared of the present invention.
Fig. 2 is the nitrogen adsorption desorption figure of the porous carbon material prepared of the present invention.
Fig. 3 is the scanning electron microscope (SEM) photograph of the porous carbon material prepared of the present invention.
The specific embodiment
The method and the absorption property that utilize bean dregs to prepare porous carbon material to the present invention below by specific embodiment are described further.
embodiment 1
1, the preparation of bean dregs base porous carbon material
The bean dregs that first will wet wash with water after 9 times, then use alcohol solution dipping 6 h, after filtration, dry, pulverize and sieve, and obtain dry bean dregs.Take the dry bean dregs of 5 g, flood 5 h with 60% solution of potassium carbonate of 10 mL mass concentrations, put into crucible after removing by filter solution, at 300 ℃, charing 1 h, is cooled to room temperature; First with 20 mL hydrochloric acid solutions washings, then be washed till neutrality with distilled water, dry, obtain porous carbon material.Specific area can be 1256.3 m
2/ g, aperture is 1.17 nm.
2, the mensuration of absorption property
Adsorption test to containing methylene blue simulated wastewater: waste water Methylene Blue concentration is 300 mg/L, pH=6 ~ 7; Adsorbent consumption is 0.05 g/L, and after room temperature (25 ℃) vibration absorption 30 min, percent of decolourization is 95.6%, and adsorption capacity reaches 280.4 mg/g, reaches national grade one discharge standard.
embodiment 2
1, the preparation of porous carbon material
The bean dregs that first will wet wash with water after 6 times, then use alcohol solution dipping 12 h.After filtration, dry, pulverize and sieve, obtain dry bean dregs.Take the dry bean dregs of 10 g, flood 10 h with the solution of potassium carbonate of 15 mL mass concentrations 20%, put into crucible after removing by filter solution; At 700 ℃, charing 2 h, are cooled to room temperature; First with 40 mL hydrochloric acid solutions washings, then be washed till neutrality with distilled water, dry, obtain bean dregs base porous carbon material.Specific area can be 1176.5 m
2/ g, aperture is 1.32 nm.
2, the mensuration of absorption property
Adsorption test to containing methylene blue simulated wastewater: waste water Methylene Blue concentration is 300 mg/L, pH=6 ~ 7; Adsorbent consumption is 0.05 g/L, and after room temperature (25 ℃) vibration absorption 5 min, percent of decolourization is 97.6%, and adsorption capacity reaches 294.4 mg/g, reaches national grade one discharge standard.
embodiment 3
1, the preparation of porous carbon material
The bean dregs that first will wet wash with water after 8 times, then soak 24 h with methanol solution; After filtration, dry, pulverize and sieve, obtain dry bean dregs.Take the dry bean dregs of 15 g, flood 12 h with the solution of potassium carbonate of 30 mL mass concentrations 25%, put into crucible after removing by filter solution, at 700 ℃, after charing 1 h, be cooled to room temperature; First with 50 mL hydrochloric acid solutions washings, then be washed till neutrality with distilled water, dry, obtain bean dregs base porous carbon material.Specific area can be 1387.5 m
2/ g, aperture is 1.74 nm.
2, the mensuration of absorption property
Adsorption test to containing methylene blue simulated wastewater: waste water Methylene Blue concentration is 300 mg/L, pH=6 ~ 7; Adsorbent consumption is 0.05 g/L, and after room temperature (25 ℃) vibration absorption 30 min, percent of decolourization is 96.4%, and adsorption capacity reaches 283.2 mg/g, reaches national grade one discharge standard.
embodiment 4
1, the preparation of porous carbon material
The bean dregs that first will wet wash with water after 7 times, then use alcohol solution dipping 32 h; After filtration, dry, pulverize and sieve, obtain dry bean dregs.Take the dry bean dregs of 20 g, flood 30 h with the phosphoric acid solution of 30 mL mass percents 20%, put into crucible after removing by filter solution, at 700 ℃, after charing 3 h, be cooled to room temperature; First with 100 mL hydrochloric acid solutions washings, then be washed till neutrality with distilled water, dry, obtain bean dregs base porous carbon material.Specific area can be 1067.9 m
2/ g, aperture is 1.67 nm.
2, the mensuration of absorption property
Adsorption test to containing methylene blue simulated wastewater: waste water Methylene Blue concentration is 300 mg/L, pH=6 ~ 7; Adsorbent consumption is 0.05 g/L, and after room temperature (25 ℃) vibration absorption 30 min, percent of decolourization is 96.8%, and adsorption capacity reaches 285.3 mg/g, reaches national grade one discharge standard.
embodiment 5
1, the preparation of porous carbon material
The bean dregs that first will wet wash with water after 5 times, then soak 24 h with methanol solution; After filtration, dry, pulverize and sieve, obtain dry bean dregs.Take the dry bean dregs of 10 g, flood 6 h with the phosphoric acid solution of 15 mL mass percents 60%, put into crucible after removing by filter solution, at 700 ℃, charing 1 h, is cooled to room temperature; First with 50 mL hydrochloric acid solutions washings, then be washed till neutrality with distilled water, dry, obtain bean dregs base porous carbon material.Specific area can be 1354.7 m
2/ g, aperture is 1.32 nm.
2, the mensuration of absorption property
Adsorption test to containing methylene blue simulated wastewater: waste water Methylene Blue concentration is 300 mg/L, pH=6 ~ 7; Adsorbent consumption is 0.05 g/L, and after room temperature (25 ℃) vibration absorption 30 min, percent of decolourization is 97.7%, and adsorption capacity reaches 295.8mg/g, reaches national grade one discharge standard.
embodiment 6
1, the preparation of porous carbon material
The bean dregs that first will wet wash with water after 8 times, then soak 24 h with methanol solution; After filtration, dry, pulverize and sieve, obtain dry bean dregs.Take the dry bean dregs of 10 g, flood 6 h with the phosphoric acid solution of 40 mL mass percents 30%, put into crucible after removing by filter solution; At 500 ℃, after charing 1 h, be cooled to room temperature; First with 50 mL hydrochloric acid solutions washings, then be washed till neutrality with distilled water, dry, obtain bean dregs base porous carbon material.Specific area can be 1257.9 m
2/ g, aperture is 1.72 nm.
2, the mensuration of absorption property
Adsorption test to containing methylene blue simulated wastewater: waste water Methylene Blue concentration is 300 mg/L, pH=6 ~ 7; Adsorbent consumption is 0.05 g/L, and after room temperature (25 ℃) vibration absorption 30 min, percent of decolourization is 90.3%, and adsorption capacity reaches 268.6mg/g, reaches national grade one discharge standard.
Claims (5)
1. utilizing bean dregs to prepare the method for porous carbon material, is by after wet bean dregs distilled water washing, at alcohol solution for soaking 3～48 h, filters, dry, obtains dry bean dregs; Again dry bean dregs are flooded to 5～30 h in activator solution, after filtration at 300～800 ℃ charing 0.5～5 h; Be cooled to room temperature, first with hydrochloric acid solution washing, then be washed till neutrality with distilled water, dry, obtain porous charcoal sorbing material.
2. utilize as claimed in claim 1 bean dregs to prepare the method for porous carbon material, it is characterized in that: described wet bean dregs are the insoluble sludge producing in production process of bean products.
3. utilize as claimed in claim 1 bean dregs to prepare the method for porous carbon material, it is characterized in that: described activator is the K of quality 10～80%
2cO
3or H
3pO
4solution.
4. utilize as claimed in claim 1 bean dregs to prepare the method for porous carbon material, it is characterized in that: described alcoholic solution is ethanolic solution or methanol solution.
5. porous carbon material application in wastewater treatment as adsorbent that as claimed in claim 1 prepared by method.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104760948A (en) * | 2015-04-22 | 2015-07-08 | 燕山大学 | Preparation method for high-performance porous carbon electrode material for super capacitor |
| CN105000620A (en) * | 2015-08-13 | 2015-10-28 | 北京工业大学 | Method for removing triclosan in wastewater by using protonated bean cakes |
| CN108745300A (en) * | 2018-05-23 | 2018-11-06 | 北京林业大学 | A kind of natural soapberry air purification medium and preparation method thereof |
| CN110697710A (en) * | 2019-11-21 | 2020-01-17 | 北京工商大学 | Bean dreg-based porous carbon material, preparation method and application thereof |
| CN111097382A (en) * | 2019-12-04 | 2020-05-05 | 天津城建大学 | Preparation method and application of bean dreg biochar adsorbent |
| CN111378525A (en) * | 2018-12-28 | 2020-07-07 | 丰益(上海)生物技术研发中心有限公司 | Frying oil treating agent and application thereof |
| CN111548973A (en) * | 2020-06-04 | 2020-08-18 | 江西康乾环保科技有限公司 | Culture method of strain and application of strain in water treatment |
| CN116375301A (en) * | 2023-06-05 | 2023-07-04 | 山东国宏生物科技有限公司 | Soybean oil wastewater treatment method |
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| CN102951698A (en) * | 2012-12-18 | 2013-03-06 | 福州大学 | Method for treating PX (para-xylene) wastewater by using active carbon as adsorbent |
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| CN1465521A (en) * | 2002-07-01 | 2004-01-07 | 金车股份有限公司 | Method for making active carbon utilizing coffee bean dregs |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104760948A (en) * | 2015-04-22 | 2015-07-08 | 燕山大学 | Preparation method for high-performance porous carbon electrode material for super capacitor |
| CN105000620A (en) * | 2015-08-13 | 2015-10-28 | 北京工业大学 | Method for removing triclosan in wastewater by using protonated bean cakes |
| CN108745300A (en) * | 2018-05-23 | 2018-11-06 | 北京林业大学 | A kind of natural soapberry air purification medium and preparation method thereof |
| CN108745300B (en) * | 2018-05-23 | 2021-08-03 | 北京林业大学 | Natural soapberry air purification medium and preparation method thereof |
| CN111378525A (en) * | 2018-12-28 | 2020-07-07 | 丰益(上海)生物技术研发中心有限公司 | Frying oil treating agent and application thereof |
| CN111378525B (en) * | 2018-12-28 | 2022-07-05 | 丰益(上海)生物技术研发中心有限公司 | Frying oil treating agent and application thereof |
| CN110697710A (en) * | 2019-11-21 | 2020-01-17 | 北京工商大学 | Bean dreg-based porous carbon material, preparation method and application thereof |
| CN110697710B (en) * | 2019-11-21 | 2022-02-08 | 北京工商大学 | Bean dreg-based porous carbon material, preparation method and application thereof |
| CN111097382A (en) * | 2019-12-04 | 2020-05-05 | 天津城建大学 | Preparation method and application of bean dreg biochar adsorbent |
| CN111548973A (en) * | 2020-06-04 | 2020-08-18 | 江西康乾环保科技有限公司 | Culture method of strain and application of strain in water treatment |
| CN116375301A (en) * | 2023-06-05 | 2023-07-04 | 山东国宏生物科技有限公司 | Soybean oil wastewater treatment method |
| CN116375301B (en) * | 2023-06-05 | 2023-08-18 | 山东国宏生物科技有限公司 | Soybean oil wastewater treatment method |
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