CN106975448B - A kind of super-high specific area adsorbent material and preparation method thereof - Google Patents

A kind of super-high specific area adsorbent material and preparation method thereof Download PDF

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CN106975448B
CN106975448B CN201710252640.5A CN201710252640A CN106975448B CN 106975448 B CN106975448 B CN 106975448B CN 201710252640 A CN201710252640 A CN 201710252640A CN 106975448 B CN106975448 B CN 106975448B
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specific surface
adsorbent material
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CN106975448A (en
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陈宝梁
肖欣
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Zhejiang University ZJU
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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
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
    • B01J20/0229—Compounds of Fe
    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/024—Compounds of Zn, Cd, Hg
    • B01J20/0244—Compounds of Zn
    • 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
    • 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
    • B01J2220/4875—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
    • 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

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Abstract

The invention discloses a kind of super-high specific area adsorbent materials and preparation method thereof.The method that object mixes heat together is closed with metal chlorination using waste bagasse, the adsorbent material of superhigh specific surface area is prepared.The material has micropore abundant and central hole structure, has good Adsorption effect to naphthalene, phenanthrene, 1- naphthols, the methylene blue in environment water, while can also remove the toluene gas in room air pollution well.According to the analysis of its preparation process, propose chemical reagent recycles strategy.This method is expected to be applied to the fields such as agricultural wastes resource utilization, indoor air purification, environment water pollutant removal.

Description

A kind of super-high specific area adsorbent material and preparation method thereof
Technical field
The invention belongs to field of material preparation, particularly with regard in the preparation and preparation process of high-specific surface area material Recycle
Background technique
The carbon material of high-specific surface area is always the important directions of material science and Research of Environmental Sciences, catalysis load, The research fields such as Adsorption of pollutant have important potential using value in battery power, environment water.Traditional life Although the carbon materials such as object carbon, charcoal, coal ash are cheap but specific surface area is not high enough, and activator used in process for preparing active carbon It is difficult to reuse mostly.And some novel high-specific surface area material (such as graphene, class grapheme material, the organic bones of metal Frame etc.), the cost of raw material, preparation cost are expensive, and preparation process can produce a large amount of waste waste liquid；And in water body easily Reunion, the easily unstability such as collapsing, significantly limit the application of these materials in the actual environment.It is discarded in agricultural production Object material is a kind of cheap biomass material abundant, and bagasse used in the present invention is exactly a kind of agriculture waste goods and materials abundant Source, from the point of view of worldwide, China produced 1.14 hundred million tons in 2007, and India then produces 2.7 hundred million tons of sugarcanes every year Slag.These waste biomass materials how are made full use of to prepare with high-performance, high economic value added and the carbon that can be applied Material becomes important research direction.
Summary of the invention
It is an object of the invention to realize the resource utilization of agricultural wastes, that is, utilize existing agricultural wastes --- The carbon material of superhigh specific surface area is prepared by step activation carbonization for bagasse.The specific surface area of the material is up to 1500 ~3000m2/ g, and there is micropore abundant and central hole structure, molecular structure is class graphene-structured, and in water body It can be stabilized, it is fabulous to the Adsorption effect of armaticity organic pollutant.
The purpose of the present invention is realized by following technological means:
The super-high specific area adsorbent material is closed after object mixes heat together and is being passed through with metal chlorination using bagasse as raw material Excessively high warm solution obtains adsorbent material, and adsorbent material has micropore and central hole structure and lamellar structure is the graphene knot of single layer Structure.
Another object of the present invention is to provide a kind of preparation methods of super-high specific area adsorbent material, utilize FeCl3 Intercalation and catalyzed graphitization and ZnCl2Pore-creating activation, common carbonization obtains superhigh specific surface area carbon material.Its Specific step is as follows:
Remove skin sugarcane and FeCl3And ZnCl2Water-bath heat together, after dry, heating pyrolysis obtains mineral under protective gas atmosphere Compound carbon material removes mineral compound on carbon material after cooling with acid again, is freeze-dried to obtain with superelevation ratio The adsorbent material of surface area.
Preferably, the temperature of water-bath heat together is 50~100 DEG C, heat together duration is preferably two days or more.
Preferably, it can be N that protection gas, which is,2, the inert gases such as argon gas.
Preferably, the heating rate of pyrolytic process is 2~20 DEG C/min, pyrolysis temperature is 600~1000 DEG C.
Preferably, sugarcane, FeCl3And ZnCl2Ratio be 1:1~10:1~10；The acid is preferably 0.1~ The hydrochloric acid of 2mol/L.
Moreover, as shown in Figure 1, the achievable circulation benefit such as used reagent and acid-leached product during the preparation process With, and a large amount of imflammable gas generated during the preparation process can also be collected.It specifically recycles and is divided into three aspects: First is that can be to the FeCl obtained after pickling3And ZnCl2It is recycled with hydrochloric acid；Second is that can be produced to during water-bath Raw HCl gas is recycled；Third is that (mainly can include to the biomass cracking gases for the generation that is carbonized in preparation process CH4, CO, H2Deng) and pickling during imflammable gas (the mainly H that generates2) recycled.
The present invention closes the method that object mixes heat together with metal chlorination using waste bagasse, and superelevation specific surface is prepared Long-pending adsorbent material.The material has micropore abundant and central hole structure, to naphthalene, phenanthrene, the 1- naphthols, methylene in environment water Indigo plant has good Adsorption effect, while can also remove the toluene gas in room air pollution well.According to its system The analysis of standby process, propose chemical reagent recycles strategy.This method can be applied to agricultural wastes recycling benefit With, fields such as indoor air purification, environment water pollutant removal.
Detailed description of the invention
The preparation process of Fig. 1 superhigh specific surface area carbon material and its recycle schematic diagram；
The nitrogen adsorption desorption curve of Fig. 2 embodiment 1；
The scanning electron microscopic observation of Fig. 3 embodiment 1；
The scanning electron microscopic observation of Fig. 4 embodiment 1；
The transmission electron microscope observing of Fig. 5 embodiment 1；
The transmission electron microscope observing of Fig. 6 embodiment 1；
The atomic force microscope observation of Fig. 7 embodiment 1.
Specific embodiment
Below by drawings and examples, the present invention will be further elaborated, preferably so as to those skilled in the art Understand essence of the invention.
Embodiment 1
Present embodiment has synthesized the carbon material of high-specific surface area.Detailed process is as follows: taking blocky peeling sugarcane and FeCl3 And ZnCl2(mass ratio: 1:8:3) water-bath heat together two days or more at a temperature of 80 DEG C, after dry, in N2It heats up under protective gas atmosphere Pyrolysis obtains the compound carbon material of mineral, and heating rate is 5 DEG C/min, and pyrolysis temperature is 900 DEG C.It is used again after natural cooling The mineral of the hydrochloric acid removal composite material of 2mol/L, are freeze-dried to obtain the adsorbent material with high-specific surface area.It obtains The yield of carbon material be about 14%.
Present implementation simple process, raw materials used cheap, environmental pollution is small, and equipment is simple.Preparation process Chemical reagent can be realized and be recycled, and be expected to be applied to be engineered to utilize waste material.The carbon being prepared in the present embodiment The specific surface area of material is up to 2280m2/g.To the adsorbance difference of typical environmental contaminants naphthalene, phenanthrene, naphthols, methylene blue Up to 615.84mg/g, 431.16mg/g, 2040.07mg/g and 474.74mg/g, much higher than the other materials reported at present Adsorption levels.
The nitrogen adsorption desorption curve of carbon material manufactured in the present embodiment such as Fig. 2, the carbon material is to nitrogen as seen from the figure The adsorbance (under normal pressure) of gas is up to 2866.2mg/g, can be with by the calculating of Brunauer-Emmett-Teller model The specific surface area for obtaining the carbon material is up to 2280m2/g.The scanning electron microscope image for the carbon material that Fig. 3 and Fig. 4 are shown, The carbon material central hole structure abundant it can be seen from the two figures.Fig. 5 and Fig. 6 is the transmission electron microscope observing figure of carbon material, by The figure can see the class graphene-structured on its microcellular structure and its surface.Fig. 7 is the atomic force microscopy of high-specific surface area material Structure observation, material shows the graphene sheet layer structure of 400 ran sizes as seen from the figure, and its height is 1nm or so is the structure of single-layer graphene.
Embodiment 2
Present embodiment has synthesized the carbon material of high-specific surface area.Detailed process is as follows: taking blocky peeling sugarcane and FeCl3 And ZnCl2(mass ratio: 3:24:2) water-bath heat together two days or more at a temperature of 80 DEG C, after dry, in N2It heats up under protective gas atmosphere Pyrolysis obtains the compound carbon material of mineral, and heating rate is 5 DEG C/min, and pyrolysis temperature is 900 DEG C.It is used again after natural cooling The mineral of the hydrochloric acid removal composite material of 2mol/L, are freeze-dried to obtain the adsorbent material with high-specific surface area.
Embodiment 3
Present embodiment has synthesized the carbon material of high-specific surface area.Detailed process is as follows: taking blocky peeling sugarcane and FeCl3 And ZnCl2(mass ratio: 1:8:3) water-bath heat together two days or more at a temperature of 80 DEG C, after dry, in N2It heats up under protective gas atmosphere Pyrolysis obtains the compound carbon material of mineral, and heating rate is 20 DEG C/min, and pyrolysis temperature is 900 DEG C.It is used again after natural cooling The mineral of the hydrochloric acid removal composite material of 2mol/L, are freeze-dried to obtain the adsorbent material with high-specific surface area.
Embodiment 4
Present embodiment has synthesized the carbon material of high-specific surface area.Detailed process is as follows: taking blocky peeling sugarcane and FeCl3 And ZnCl2(mass ratio: 1:8:3) water-bath heat together two days or more at a temperature of 100 DEG C, after dry, in N2It heats up under protective gas atmosphere Pyrolysis obtains the compound carbon material of mineral, and heating rate is 5 DEG C/min, and pyrolysis temperature is 900 DEG C.It is used again after natural cooling The mineral of the hydrochloric acid removal composite material of 2mol/L, are freeze-dried to obtain the adsorbent material with high-specific surface area.
Embodiment 5
Present embodiment has synthesized the carbon material of high-specific surface area.Detailed process is as follows: taking blocky peeling sugarcane and FeCl3 And ZnCl2(mass ratio: 1:1:1) water-bath heat together two days or more at 50 °C, after dry, in N2It heats up under protective gas atmosphere Pyrolysis obtains the compound carbon material of mineral, and heating rate is 2 DEG C/min, and pyrolysis temperature is 600 DEG C.It is used again after natural cooling The mineral of the hydrochloric acid removal composite material of 0.1mol/L, are freeze-dried to obtain the adsorbent material with high-specific surface area.
Embodiment 6
Present embodiment has synthesized the carbon material of high-specific surface area.Detailed process is as follows: taking blocky peeling sugarcane and FeCl3 And ZnCl2(mass ratio: 1:10:10) water-bath heat together two days or more at 50 °C, after dry, in N2It is risen under protective gas atmosphere Warm solution obtains the compound carbon material of mineral, and heating rate is 20 DEG C/min, and pyrolysis temperature is 1000 DEG C.After natural cooling Again with the mineral of the hydrochloric acid removal composite material of 1mol/L, it is freeze-dried to obtain the adsorbent material with high-specific surface area.
The specific surface area of the obtained carbon material of 1 preceding four kind of embodiment of table preparation
Embodiment Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4
Specific surface area (m2g-1) 2280 952.2 1239 1035
Table 1 shows the specific surface area for the carbon material that Examples 1 to 4 prepares.It should be pointed out that above-described Embodiment is a kind of preferable scheme of the invention, and so it is not intended to limiting the invention.Common skill in relation to technical field Art personnel can also make a variety of changes and modification without departing from the spirit and scope of the present invention.Therefore all to take The mode of equivalent substitution or equivalent transformation technical solution obtained, falls within the scope of protection of the present invention.

Claims (7)

1. a kind of preparation method of super-high specific area adsorbent material characterized by comprising press the quality of 1:1 ~ 10:1 ~ 10 Than removing skin sugarcane and FeCl3And ZnCl2Water-bath heat together two days or more at a temperature of 50 ~ 100 DEG C, after dry, in protective gas atmosphere Lower heating pyrolysis obtains the compound carbon material of mineral, and the heating rate of pyrolytic process is 2 ~ 20 DEG C/min, and pyrolysis temperature is 600 ~ 1000℃；It is freeze-dried to obtain again with mineral compound on acid removal carbon material with superhigh specific surface area after cooling Adsorbent material, adsorbent material has micropore and central hole structure and lamellar structure is the graphene-structured of single layer.
2. the preparation method of super-high specific area adsorbent material as described in claim 1, which is characterized in that the ratio of adsorbent material Surface area is 1500 ~ 3000m2/g。
3. the preparation method of super-high specific area adsorbent material as described in claim 1, which is characterized in that protection gas is inertia Gas.
4. the preparation method of superhigh specific surface area material as described in claim 1, which is characterized in that the acid be 0.1 ~ The hydrochloric acid of 2mol/L.
5. the preparation method of superhigh specific surface area material as claimed in claim 4, which is characterized in that what is obtained after pickling FeCl3And ZnCl2It is recycled with hydrochloric acid.
6. the preparation method of superhigh specific surface area material as claimed in claim 4, which is characterized in that generated to during water-bath HCl gas recycled.
7. the preparation method of superhigh specific surface area material as described in claim 1, which is characterized in that being carbonized in preparation process The imflammable gas generated during the biomass cracking gases of generation and pickling is recycled.
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CN110368896B (en) * 2019-06-04 2020-08-07 中国地质大学（武汉） Ultrahigh-specific-surface-area carbon-based functional material and preparation method and application thereof
CN111154503A (en) * 2020-01-09 2020-05-15 复旦大学 Method for reducing high toxic substances in biochar

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