CN109046250B - Garden waste biomass charcoal modification method - Google Patents

Garden waste biomass charcoal modification method Download PDF

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CN109046250B
CN109046250B CN201811052582.2A CN201811052582A CN109046250B CN 109046250 B CN109046250 B CN 109046250B CN 201811052582 A CN201811052582 A CN 201811052582A CN 109046250 B CN109046250 B CN 109046250B
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biomass charcoal
garden
stirring
deionized water
charcoal
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CN109046250A (en
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申圆圆
林倩
麻李娜
郝恒星
李乐
刘田田
王雪梅
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Xian Unversity of Arts and Science
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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
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B01J20/28061—Surface area, e.g. B.E.T specific surface area being in the range 100-500 m2/g
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
    • B01J20/3234—Inorganic material layers
    • 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
    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • 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

Abstract

The invention discloses a garden waste biomass charcoal modification method, S1, crushing garden biomass charcoal to pass through a screen; s2, preprocessing garden biomass charcoal; s3, modification treatment of garden biomass charcoal: stirring and dipping the garden biomass charcoal II in a constant-temperature water bath by using a ferrous sulfate solution for 10-12 h, performing suction filtration, washing the garden biomass charcoal II by using deionized water until the pH of filtrate is the same as the pH of the deionized water, adding a potassium hydroxide solution, stirring and dipping for 1-2 h, performing suction filtration, washing the garden biomass charcoal II by using the deionized water until the pH of the filtrate is the same as the pH of the deionized water, and drying to obtain the modified garden biomass charcoal.

Description

Garden waste biomass charcoal modification method
Technical Field
The invention relates to the technical field of biomass charcoal modification, in particular to a method for modifying garden waste biomass charcoal.
Background
The garden waste biomass charcoal can be applied to the aspects of water quality purification, soil heavy metal pollution remediation, soil improvement and the like, but has limited adsorption performance. The surface properties of the biomass charcoal can be obviously changed by modification methods such as oxidation, reduction modification and the like, for example, the pores of the biomass charcoal are enriched, the specific surface area is increased, and the number of characteristic functional groups is increased, and the characteristics are favorable for the treatment efficiency of the biomass charcoal in the aspect of water pollution by using an adsorption method; the Wangying research finds that the acid washing treatment can change the surface functional groups of the biomass charcoal, thereby improving the adsorption performance of the biomass charcoal; the Lekun right utilizes KOH to modify spartina alterniflora poles and cotton stalks, and the modified biomass charcoal is rich in micropores and has good adsorption performance on iodine, methylene blue and 2.4-dinitrophenol in water; korean fragrant cloud and the like propose that garden biomass carbon prepared by KOH modification has enlarged BET and developed pore structure; gokce et al found that biomass charcoal modified by nitric acid has a significant influence on the adsorption amount of methylene blue. Therefore, the invention provides a method for modifying garden waste biomass charcoal.
Disclosure of Invention
The invention aims to solve the defect of limited adsorption performance of garden waste biomass charcoal in the prior art, and provides a garden waste biomass charcoal modification method.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for modifying garden waste biomass charcoal comprises the following steps:
s1, adding the garden biomass charcoal into a crusher to be crushed to obtain powder, filtering the powder through a screen with 80 meshes to obtain a screened substance, transferring the non-screened substance back to the crusher to be crushed again until the garden biomass charcoal completely passes through the screen for later use;
s2, pretreatment of garden biomass charcoal: washing and drying garden biomass charcoal to obtain garden biomass charcoal I, stirring and dipping the garden biomass charcoal I with a phosphoric acid solution, performing suction filtration, washing the garden biomass charcoal I with deionized water until the pH of the washed filtrate is the same as that of the deionized water, and drying the garden biomass charcoal I to obtain garden biomass charcoal II for later use;
s3, modification treatment of garden biomass charcoal: stirring and dipping the garden biomass charcoal II in a constant-temperature water bath for 10-12 h by using a ferrous sulfate solution with neutral pH, performing suction filtration, washing the garden biomass charcoal II by using deionized water until the pH of filtrate is the same as that of the deionized water, adding a potassium hydroxide solution, stirring and dipping for 3-5 h, performing suction filtration, washing the garden biomass charcoal II by using the deionized water until the pH of the filtrate is the same as that of the deionized water, and drying to obtain the modified garden biomass charcoal.
Preferably, the mass ratio of the garden biomass charcoal I to the phosphoric acid solution in the step S2 is 1: 2, the phosphoric acid solution has a mass percent concentration of 40 percent and the stirring time is 1-3 h.
Preferably, the conditions for stirring and dipping the ferrous sulfate solution are as follows: the concentration of the ferrous sulfate solution is 1-3 mol/L, the stirring time is 1-2 h, and the mass ratio of the garden biomass charcoal II to the ferrous sulfate solution is 1: 10-1: 20.
preferably, the potassium hydroxide solution is stirred and impregnated under the following conditions: the concentration of the potassium hydroxide is 0.1 mol/L-0.25 mol/L, and the stirring temperature is 30 ℃ to 50 ℃; the mass ratio of the garden biomass charcoal II to the potassium hydroxide solution is 1: 10-1: 20, stirring and dipping for 3-5 h.
Preferably, the garden biomass charcoal is mallotus japonicus fallen leaf biomass charcoal and ligustrum lucidum fallen leaf biomass charcoal.
Preferably, the drying conditions are as follows: the drying temperature is 95 ℃ and the drying time is 12 h.
The invention has the beneficial effects that:
1. according to the invention, through adopting a chemical modification activation method, the pretreated garden biomass charcoal is subjected to modification treatment of a pore structure and oxygen-containing functional groups, the prepared garden biomass charcoal has the advantages of obviously increased pores, increased specific surface area and increased oxygen-containing functional groups, and the removal capability of the modified garden biomass charcoal on the wastewater containing methylene blue is obviously improved.
2. The method has the advantages of simple operation, low cost, low requirement on experimental conditions and good modification effect, and the adsorption removal capacity of the modified methylene blue is enhanced; the method can reduce the adding amount of the garden biomass charcoal in the water treatment process so as to reduce the wastewater treatment cost.
Drawings
Fig. 1 is a schematic structural diagram of garden biomass of phoenix tree fallen leaves under a scanning electron microscope before modification in the garden waste biomass charcoal modification method provided by the invention;
fig. 2 is a schematic structural diagram of garden biomass of phoenix tree fallen leaves under a scanning electron microscope after modification in the garden waste biomass charcoal modification method provided by the invention;
FIG. 3 is a schematic structural diagram of a garden waste biomass charcoal modification method according to the present invention before and after modification under X-ray diffraction irradiation;
FIG. 4 is a schematic structural diagram of the garden waste biomass charcoal modification method before and after modification under infrared ray diffraction irradiation.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
Example (b): a method for modifying garden waste biomass charcoal comprises the following steps:
s1, adding 100g of the garden biomass charcoal of the fallen leaves of the plane tree into a crusher to be crushed to obtain powder, filtering the powder through a screen with 80 meshes to obtain a screened substance, transferring the non-screened substance back to the crusher to be crushed again until the garden biomass charcoal completely passes through the screen for later use;
s2, pretreatment of garden biomass charcoal: cleaning and drying garden biomass charcoal to obtain garden biomass charcoal I, stirring the garden biomass charcoal I with 200ml of phosphoric acid solution with the mass percentage concentration of 40% for 2 hours, dipping, performing suction filtration, cleaning the garden biomass charcoal I with 1000ml of deionized water until the pH of the cleaned filtrate is the same as the pH of the deionized water, and drying the garden biomass charcoal I to obtain garden biomass charcoal II for later use;
s3, modification treatment of garden biomass charcoal: stirring garden biomass charcoal II in 1500ml of ferrous sulfate solution with neutral pH and concentration of 2mol/L for 1h and dipping for 10h, performing suction filtration, washing the garden biomass charcoal II with deionized water until the pH of filtrate is the same as the pH of the deionized water, adding 1500ml of potassium hydroxide solution with concentration of 0.2mol/L, stirring for 4h, dipping for 2h at the temperature of 40 ℃, performing suction filtration, washing the garden biomass charcoal II with deionized water until the pH of filtrate is the same as the pH of the deionized water, and drying L2h at the temperature of 95 ℃ to obtain the modified garden biomass charcoal.
Observing the structures of the Chinese parasol fallen leaf garden biomass charcoal before and after modification through a scanning electron microscope, as shown in figures 1 and 2:
as shown in fig. 1 and fig. 2, it can be clearly seen through a scanning electron microscope that the unmodified biomass carbon microstructure shows fewer holes and low pore canal connectivity, but the surface of the modified biomass carbon particles of the phoenix tree fallen leaves prepared by the invention has formed a large cellular-like pore structure with different pore diameters, the pore canal connectivity is large, the particle structure has a larger volume than the raw material, and the pores on the particle structure are larger, regular and abundant. The specific surface area of the modified biomass charcoal is greatly improved compared with that before modification, and the specific surface area of the unmodified biomass charcoal obtained by measuring the specific surface area of the biomass charcoal is 121.58m2(g) the specific surface area after modification is 151.49m2The specific surface area increased by 24.40% after modification.
The structures of the biomass charcoal before and after modification in the gardens of the Chinese parasol fallen leaves are observed through X-ray diffraction and infrared ray diffraction, and are shown in figure 3:
as shown in fig. 3, the modified biomass charcoal has more absorption peaks in XRD pattern than unmodified absorption peaks and has higher intensity, the modified biomass charcoal has more distinct diffraction peaks near 26 ° and 44 ° 2 θ respectively, which are (002) plane and (100) plane of turbostratic graphite, and the two diffraction peak intensities are enhanced with modification, because the biomass charcoal tends to amorphous non-crystalline point graphene structure due to chemical modification, the skeleton structural unit of the modified biomass charcoal is similar to amorphous charcoal, the graphite crystallites form the pore walls of the carbonaceous adsorbent, and the gaps between the graphite crystallites become fine pores.
The structures of the biomass charcoal before and after modification in the garden of the fallen leaves of plane tree are observed by infrared diffraction, as shown in figure 4:
as shown in FIG. 4, the FTIR curve of the modified biomass charcoal has partial functional group absorption peaks different from that of the unmodified biomass charcoal, and the modified biomass charcoal has more types of functional groups on the surface, 3403cm-1～3417cm-1A wider absorption peak appears, mainly a stretching vibration area of an O-H bond; 2784cm-1Nearby vibration peaks are generated by C-H stretching vibration; at 1745cm-1the-COO-absorption peak of the nearby B6-K surface is obvious, which shows that the carboxyl content of the biomass charcoal surface is relatively high, the polar organic matter methylene blue can be effectively adsorbed, and the concentration of the carboxyl is 1567cm-1～1623cm-1An absorption peak of C ═ O bond vibration mainly of non-conjugated carbonyl groups or ester groups; at 998cm-1～1060cm-1The modified biomass carbon mainly is a C-O-C bond stretching vibration area, and the analysis shows that the modified biomass carbon contains oxygen-containing groups such as ester, ether, alcohol, phenol and the like, and the functions of the functional groups are not only expressed on the adsorption performance of the biomass carbon, but also on the catalysis effect of the biochar, so that the adsorption rate of the modified biomass carbon is obviously higher than that of the unmodified biomass carbon in the adsorption experiment, the more the oxygen-containing functional groups on the surface of the biomass carbon are, the lower the surface hydrophobicity is, the interaction between the surface functional groups and polar organic pollutant molecules through hydrogen bonds or dipole-dipole effect can be promoted, and the adsorption of the biomass carbon on micromolecules and polar organic pollutants is facilitated.
Putting 50mL of methylene blue solution with the initial concentration of 5mg/L into a conical flask, adding 20mg of unmodified and modified garden biomass charcoal, placing the mixture on an oscillator for oscillation (30 ℃, 150r/min and 40min), filtering the mixture by using a microporous filter membrane (0.45mm) to obtain the methylene blue solution after adsorption, measuring the absorbance of the methylene blue solution, and calculating to obtain the removal rates of the unmodified and modified biomass charcoal to the methylene blue, wherein the removal rates are respectively 56-61% and 78-83%, so that the removal rate of the modified biomass charcoal to the methylene blue can be obviously improved.
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 person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (6)

1. A modification method of garden waste biomass charcoal is characterized by comprising the following steps:
s1, adding the garden biomass charcoal into a crusher to be crushed to obtain powder, filtering the powder through a screen with 80 meshes to obtain a screened substance, transferring the non-screened substance back to the crusher to be crushed again until the garden biomass charcoal completely passes through the screen for later use;
s2, pretreatment of garden biomass charcoal: washing and drying garden biomass charcoal to obtain garden biomass charcoal I, stirring and dipping the garden biomass charcoal I with a phosphoric acid solution, performing suction filtration, washing the garden biomass charcoal I with deionized water until the pH of the washed filtrate is the same as that of the deionized water, and drying the garden biomass charcoal I to obtain garden biomass charcoal II for later use;
s3, modification treatment of garden biomass charcoal: stirring and dipping the garden biomass charcoal II in a constant-temperature water bath for 10-12 h by using a ferrous sulfate solution with neutral pH, performing suction filtration, washing the garden biomass charcoal II by using deionized water until the pH of filtrate is the same as that of the deionized water, adding a potassium hydroxide solution, stirring and dipping for 3-5 h, performing suction filtration, washing the garden biomass charcoal II by using the deionized water until the pH of the filtrate is the same as that of the deionized water, and drying to obtain the modified garden biomass charcoal.
2. The method for modifying the garden waste biomass charcoal according to claim 1, wherein the mass ratio of the garden biomass charcoal I to the phosphoric acid solution in the step S2 is 1: 2, the phosphoric acid solution has a mass percent concentration of 40 percent and the stirring time is 1-3 h.
3. The method for modifying the garden waste biomass charcoal according to claim 1, wherein the conditions for stirring and soaking the ferrous sulfate solution are as follows: the concentration of the ferrous sulfate solution is 1-3 mol/L, the stirring time is 1-2 h, and the mass ratio of the garden biomass charcoal II to the ferrous sulfate solution is 1: 10-1: 20.
4. the method for modifying the garden waste biomass charcoal according to claim 1, wherein the potassium hydroxide solution is stirred and soaked under the following conditions: the concentration of the potassium hydroxide is 0.1 mol/L-0.25 mol/L, and the stirring temperature is 30 ℃ to 50 ℃; the mass ratio of the garden biomass charcoal II to the potassium hydroxide solution is 1: 10-1: 20, stirring and dipping for 3-5 h.
5. The method for modifying the garden waste biomass charcoal as claimed in claim 1, wherein the garden biomass charcoal is a phoenix tree fallen leaf biomass charcoal and a privet fallen leaf biomass charcoal.
6. The method for modifying the biomass charcoal of the garden waste according to claim 1, wherein the drying conditions are as follows: the drying temperature is 95 ℃ and the drying time is 12 h.
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Publication number Priority date Publication date Assignee Title
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CN106348294A (en) * 2016-11-09 2017-01-25 南阳师范学院 Preparation method of deciduous leaf activated carbon
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CN101708845A (en) * 2009-11-20 2010-05-19 中南林业科技大学 Method for manufacturing active carbon by using rice hulls and stalks as main raw materials
CN101780954A (en) * 2010-01-22 2010-07-21 核工业西南勘察设计研究院有限公司 Carbon material with high surface activity and preparation method thereof
CN105854804A (en) * 2016-05-20 2016-08-17 昆明理工大学 Method for modifying activated carbon
CN106348294A (en) * 2016-11-09 2017-01-25 南阳师范学院 Preparation method of deciduous leaf activated carbon
CN107555414A (en) * 2017-09-15 2018-01-09 佛山科学技术学院 A kind of garden waste biomass carbon and its production and use

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