CN106955666B - A method of biomass magnetism carbosphere is prepared with agriculture and forestry organic waste material - Google Patents
A method of biomass magnetism carbosphere is prepared with agriculture and forestry organic waste material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 45
- 239000010815 organic waste Substances 0.000 title claims abstract description 45
- 239000002028 Biomass Substances 0.000 title claims abstract description 27
- 230000005389 magnetism Effects 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000002904 solvent Substances 0.000 claims abstract description 35
- 238000002360 preparation method Methods 0.000 claims abstract description 27
- 239000002608 ionic liquid Substances 0.000 claims abstract description 24
- 239000006249 magnetic particle Substances 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 17
- 239000000017 hydrogel Substances 0.000 claims abstract description 11
- 239000002699 waste material Substances 0.000 claims abstract description 10
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 165
- 239000012798 spherical particle Substances 0.000 claims description 18
- 239000011261 inert gas Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- 239000003085 diluting agent Substances 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 10
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- 239000004094 surface-active agent Substances 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 8
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 239000001913 cellulose Substances 0.000 claims description 6
- 229920002678 cellulose Polymers 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 229920000642 polymer Polymers 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- 238000003763 carbonization Methods 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 230000003252 repetitive effect Effects 0.000 claims description 4
- IBZJNLWLRUHZIX-UHFFFAOYSA-N 1-ethyl-3-methyl-2h-imidazole Chemical compound CCN1CN(C)C=C1 IBZJNLWLRUHZIX-UHFFFAOYSA-N 0.000 claims description 3
- 235000017060 Arachis glabrata Nutrition 0.000 claims description 3
- 244000105624 Arachis hypogaea Species 0.000 claims description 3
- 235000010777 Arachis hypogaea Nutrition 0.000 claims description 3
- 235000018262 Arachis monticola Nutrition 0.000 claims description 3
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 3
- 150000001450 anions Chemical class 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 150000001768 cations Chemical class 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000002122 magnetic nanoparticle Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 235000020232 peanut Nutrition 0.000 claims description 3
- 239000001509 sodium citrate Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 3
- 229940038773 trisodium citrate Drugs 0.000 claims description 3
- KAIPKTYOBMEXRR-UHFFFAOYSA-N 1-butyl-3-methyl-2h-imidazole Chemical compound CCCCN1CN(C)C=C1 KAIPKTYOBMEXRR-UHFFFAOYSA-N 0.000 claims description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 2
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims description 2
- 235000007164 Oryza sativa Nutrition 0.000 claims description 2
- 241000353135 Psenopsis anomala Species 0.000 claims description 2
- 240000008042 Zea mays Species 0.000 claims description 2
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims description 2
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 2
- 230000003213 activating effect Effects 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 2
- 235000005822 corn Nutrition 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000010893 paper waste Substances 0.000 claims description 2
- 235000009566 rice Nutrition 0.000 claims description 2
- 239000010907 stover Substances 0.000 claims description 2
- 239000010902 straw Substances 0.000 claims description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims 1
- XLSZMDLNRCVEIJ-UHFFFAOYSA-N methylimidazole Natural products CC1=CNC=N1 XLSZMDLNRCVEIJ-UHFFFAOYSA-N 0.000 claims 1
- DGPIGKCOQYBCJH-UHFFFAOYSA-M sodium;acetic acid;hydroxide Chemical compound O.[Na+].CC([O-])=O DGPIGKCOQYBCJH-UHFFFAOYSA-M 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052799 carbon Inorganic materials 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000001681 protective effect Effects 0.000 abstract description 3
- 238000007493 shaping process Methods 0.000 abstract description 3
- 238000004064 recycling Methods 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 14
- 239000000243 solution Substances 0.000 description 5
- 239000003208 petroleum Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 2
- 229940040526 anhydrous sodium acetate Drugs 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 231100000167 toxic agent Toxicity 0.000 description 2
- 238000003911 water pollution Methods 0.000 description 2
- PBIDWHVVZCGMAR-UHFFFAOYSA-N 1-methyl-3-prop-2-enyl-2h-imidazole Chemical compound CN1CN(CC=C)C=C1 PBIDWHVVZCGMAR-UHFFFAOYSA-N 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- IAZDPXIOMUYVGZ-WFGJKAKNSA-N Dimethyl sulfoxide Chemical group [2H]C([2H])([2H])S(=O)C([2H])([2H])[2H] IAZDPXIOMUYVGZ-WFGJKAKNSA-N 0.000 description 1
- 241000124008 Mammalia Species 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- 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
- B01J20/28002—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 physical properties
- B01J20/28009—Magnetic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
-
- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/32—Spheres
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- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Crystallography & Structural Chemistry (AREA)
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- Processing Of Solid Wastes (AREA)
- Soil Conditioners And Soil-Stabilizing Materials (AREA)
Abstract
A method of biomass magnetism carbosphere being prepared with agriculture and forestry organic waste material, is related to a kind of method for preparing magnetic carbosphere.The present invention is that have burn into pollute equipment to solve current active carbon preparation, prepare complexity, the difficult technical problem of high production cost, recycling.The present invention: one, agriculture and forestry organic waste material powder is prepared；Two, hydrogel sphere is prepared；Three, it is carbonized.It itself is renewable resource and raw material is cheap and easy to get the invention has the advantages that the present invention uses agriculture and forestry organic waste material as raw material, this is to turn waste into wealth；Select ionic liquid as solvent, it is environmentally protective to may be reused；One step of product shaping process is extracted from biomass to complete, and redissolution process, simple and convenient is precipitated without biomass；Product is spherical in shape, easy to use；It may be reused in product added with magnetic particle.
Description
Technical field
The present invention relates to a kind of methods for preparing magnetic carbosphere.
Background technique
With the development of society, people are more and more for the demand of the energy and resource, however traditional mineral and fossil
Fuel source has been not enough to maintain the development of society, and people are huge by the sight trend of purchasing nature reserves of concern, and can be again
Raw biomass resource.Wherein agriculture and forestry organic waste material has a large amount of agriculture and forestry organic waste material to be produced every year by the concern of people
Come, is dropped to cause the waste of vast resources, and improperly processing will cause a large amount of pollution, if can be by this
A little agriculture and forestry organic waste materials are converted to product can be to make great contribution for social sustainable development.
Water pollution has become the problem of vital importance that the mankind have to face, and oil leak is one of them.From people
The problem of class begins to use petroleum, and petroleum is revealed occurs repeatedly.The toxic compounds such as contained benzene and toluene are bled into sea in petroleum
Behind ocean, these toxic compounds have also quickly entered food chain, and from low algae, to higher mammal, none can escape by luck.
Petroleum is adsorbed by active carbon, processing Oil spills problem is one of solution.But existing active carbon preparation is deposited
It is insufficient in following several respects: (1) that the catalyst such as soda acid being added in preparation process, have corrosion to equipment, while causing largely to pollute；
(2) preparation flow is complicated, high production cost；(3) raw material of most of high grade activated carbon is timber and coal；(4) work prepared
Property charcoal absorption after recycle it is difficult.
Summary of the invention
The present invention is that have burn into pollute equipment to solve current active carbon preparation, prepare complexity, production cost
Technical problem high, recycling is difficult, and a kind of method with agriculture and forestry organic waste material preparation biomass magnetism carbosphere is provided.
A kind of method with agriculture and forestry organic waste material preparation biomass magnetism carbosphere of the invention carries out according to the following steps:
One, prepare agriculture and forestry organic waste material powder: agriculture and forestry organic waste material cleaned up to and is cut into block, temperature be 70 DEG C~
Dry 6h under conditions of 105 DEG C~for 24 hours, dry block agriculture and forestry organic waste material is then ground into 30 mesh~300 mesh with pulverizer
Agriculture and forestry organic waste material powder；
Two, it 1., by agriculture and forestry organic waste material powder is added in ionic liquid, is stirred under conditions of temperature is 60 DEG C~100 DEG C
4h~for 24 hours is mixed, whole filtrates are collected by filtration, surfactant, Fe are added into whole filtrates3O4Magnetic particle and diluent, so
The stirring 4h~for 24 hours under conditions of temperature is 40 DEG C~60 DEG C afterwards, obtains mixed liquor；
2., mixed liquor poured into the syringe with syringe needle, mixed liquor is injected into solvent a with syringe, in solvent a
It is middle to form multiple spherical particles, spherical particle is collected in solvent a；
3., spherical particle is immersed in 1h~2h in solvent b, collect spherical particle in solvent b；
4., by step 2 3. repetitive operation 3 times~5 times, obtain hydrogel sphere；
The mass ratio of the agriculture and forestry organic waste material powder and ionic liquid is (1~15): 100；The ionic liquid and
The mass ratio of surfactant is 50:(1~5)；The ionic liquid and Fe3O4The mass ratio of magnetic particle be 50:(1~
10)；The mass ratio of the ionic liquid and diluent is 5:(3~10)；The size of the syringe needle is 0.45mm × 15mm；
Three, the hydrogel sphere for preparing step 2 dry 4h~12h under conditions of temperature is 15 DEG C~50 DEG C, then exists
With 3 DEG C/min~10 DEG C/min heating rate from room temperature to 500 DEG C~1000 DEG C under inert gas shielding, in indifferent gas
Carbonization 1h~3h, under inert gas protection furnace cooling are given birth under conditions of body protection and temperature are 500 DEG C~1000 DEG C
Changing of magnetism carbosphere.
The present invention be using rich cellulose-containing agriculture and forestry organic waste material as raw material, with environmentally protective lyate ion liquid,
And surfactant and magnetic particle are added thereto, it instills in solvent after shaping by washing, drying, then in inert gas
Middle carbonization treatment finally obtains biomass magnetism carbosphere.
The invention has the advantages that the present invention uses agriculture and forestry organic waste material as raw material, it itself is renewable resource and original
Expect cheap and easy to get, this is to turn waste into wealth；Select ionic liquid as solvent, it is environmentally protective to may be reused；It is mentioned from biomass
The completion of one step of product shaping process is got, redissolution process, simple and convenient is precipitated without biomass；Product is spherical in shape, is easy to make
With；It may be reused in product added with magnetic particle.
Preparation method of the invention has good operability, and resource reutilization can be not only carried out to agriculture and forestry organic waste material, but also
Water pollution problems can be solved with product.
Detailed description of the invention
Fig. 1 is the photo in kind for testing the hydrogel sphere biomass magnetism carbosphere of step 2 preparation；
Fig. 2 is the photo in kind for testing the biomass magnetism carbosphere of a preparation；
Fig. 3 is the low power number stereoscan photograph for testing the biomass magnetism carbosphere of a preparation；
Fig. 4 is the high magnification numbe stereoscan photograph for testing the biomass magnetism carbosphere of a preparation.
Specific embodiment
Specific embodiment 1: present embodiment is a kind of side for preparing biomass magnetism carbosphere with agriculture and forestry organic waste material
Method specifically carries out according to the following steps:
One, prepare agriculture and forestry organic waste material powder: agriculture and forestry organic waste material cleaned up to and is cut into block, temperature be 70 DEG C~
Dry 6h under conditions of 105 DEG C~for 24 hours, dry block agriculture and forestry organic waste material is then ground into 30 mesh~300 mesh with pulverizer
Agriculture and forestry organic waste material powder；
Two, it 1., by agriculture and forestry organic waste material powder is added in ionic liquid, is stirred under conditions of temperature is 60 DEG C~100 DEG C
4h~for 24 hours is mixed, whole filtrates are collected by filtration, surfactant, Fe are added into whole filtrates3O4Magnetic particle and diluent, so
The stirring 4h~for 24 hours under conditions of temperature is 40 DEG C~60 DEG C afterwards, obtains mixed liquor；
2., mixed liquor poured into the syringe with syringe needle, mixed liquor is injected into solvent a with syringe, in solvent a
It is middle to form multiple spherical particles, spherical particle is collected in solvent a；
3., spherical particle is immersed in 1h~2h in solvent b, collect spherical particle in solvent b；
4., by step 2 3. repetitive operation 3 times~5 times, obtain hydrogel sphere；
The mass ratio of the agriculture and forestry organic waste material powder and ionic liquid is (1~15): 100；The ionic liquid and
The mass ratio of surfactant is 50:(1~5)；The ionic liquid and Fe3O4The mass ratio of magnetic particle be 50:(1~
10)；The mass ratio of the ionic liquid and diluent is 5:(3~10)；The size of the syringe needle is 0.45mm × 15mm；
Three, the hydrogel sphere for preparing step 2 dry 4h~12h under conditions of temperature is 15 DEG C~50 DEG C, then exists
With 3 DEG C/min~10 DEG C/min heating rate from room temperature to 500 DEG C~1000 DEG C under inert gas shielding, in indifferent gas
Carbonization 1h~3h, under inert gas protection furnace cooling are given birth under conditions of body protection and temperature are 500 DEG C~1000 DEG C
Changing of magnetism carbosphere.
When injecting mixed liquor into solvent a with syringe in the step of present embodiment two, every injection is once drop mixed liquor
A spherical particle can be obtained in solvent a, so the amount for needing to be added dropwise mixed liquor determines according to actual needs；Solvent a's
As long as amount can accommodate spherical particle, particular/special requirement is not done.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: agricultural described in step 1
Waste is rich cellulose-containing product waste material.It is other same as the specific embodiment one.
Specific embodiment 3: present embodiment is unlike specific embodiment two: the richness is cellulose-containing
Product waste material is peanut shell, melon seed cases, corn stover, rice straw, sawdust, branch, throwaway chopsticks or waste paper.Other and tool
Body embodiment two is identical.
Specific embodiment 4: the present embodiment is different from the first embodiment in that: Fe described in step 23O4
The preparation method of magnetic particle is:
By the anhydrous FeCl of 4mmol3It being added in the diethylene glycol (DEG) of 50mL, stirring 40min~50min forms clear solution,
Then the trisodium citrate of 1.6mmol is added, be heated to 80 DEG C and stirs 30min formation clear solution, is then added
The anhydrous sodium acetate of 12.0mmol is stirred for 30min, is then transferred in the stainless steel autoclave of polytetrafluoroethyllining lining and carries out
Sealing, keeps the temperature 6h at 240 DEG C for autoclave, obtains Fe3O4Magnetic nanoparticle.It is other same as the specific embodiment one.
Specific embodiment 5: the present embodiment is different from the first embodiment in that: ion described in step 2
Cation is 1- ethyl-3-methylimidazole, 1- butyl -3- methylimidazole or 1- allyl -3- methylimidazole, anion in liquid
For F1-、Cl1-、Br1-、BF4 1-、PF6 1-Or OAc1-.It is other same as the specific embodiment one.
Specific embodiment 6: the present embodiment is different from the first embodiment in that: surface described in step 2
Activating agent is hexadecyltrimethylammonium chloride, cetyl trimethylammonium bromide, block polymer P123 or block polymer
F127.It is other same as the specific embodiment one.
Specific embodiment 7: the present embodiment is different from the first embodiment in that: dilution described in step 2
Agent is dimethyl sulfoxide, n,N-Dimethylformamide or n,N-dimethylacetamide.It is other same as the specific embodiment one.
Specific embodiment 8: the present embodiment is different from the first embodiment in that: solvent a described in step 2
For the mixture of one or more of methanol, ethyl alcohol, acetone and chloroform, solvent b is identical as solvent a.It is other with it is specific
Embodiment one is identical.
Specific embodiment 9: the present embodiment is different from the first embodiment in that: inertia described in step 2
Gas is nitrogen or argon gas.It is other same as the specific embodiment one.
Effect of the invention is verified by following tests:
Test one: this test be it is a kind of with agriculture and forestry organic waste material prepare biomass magnetism carbosphere method, specifically press with
What lower step carried out:
One, it prepares agriculture and forestry organic waste material powder: agriculture and forestry organic waste material is cleaned up to and is cut into block, in item at a temperature of 90 °C
Dry block agriculture and forestry organic waste material, is then ground into the agriculture and forestry organic waste material powder of 100 mesh by dry 12h with pulverizer under part；
Two, it 1., by agriculture and forestry organic waste material powder is added in ionic liquid, stirs 6h, mistake under conditions of temperature is 80 DEG C
Whole filtrates are collected in filter, and surfactant, Fe are added into whole filtrates3O4Then magnetic particle and diluent are 50 in temperature
12h is stirred under conditions of DEG C, obtains mixed liquor；
2., mixed liquor poured into the syringe with syringe needle, mixed liquor is injected into solvent a with syringe, in solvent a
It is middle to form multiple spherical particles, spherical particle is collected in solvent a；
3., spherical particle is immersed in 1h in solvent b, collect spherical particle in solvent b；
4., by step 2 3. repetitive operation 3 times, obtain hydrogel sphere；
The mass ratio of the agriculture and forestry organic waste material powder and ionic liquid is 1:10；The ionic liquid and surface-active
The mass ratio of agent is 10:1；The ionic liquid and Fe3O4The mass ratio of magnetic particle is 50:3；The ionic liquid and
The mass ratio of diluent is 1:1；The size of the syringe needle is 0.45mm × 15mm；
Three, the hydrogel sphere for preparing step 2 dry 8h under conditions of temperature is 15 DEG C, is then protected in inert gas
With the heating rate of 5 DEG C/min from room temperature to 750 DEG C under shield, under conditions of inert gas shielding and temperature are 750 DEG C
Be carbonized 1h, and furnace cooling under inert gas protection obtains biomass magnetism carbosphere.
Agriculture and forestry organic waste material described in step 1 is rich cellulose-containing product waste material, is peanut shell；
Fe described in step 23O4The preparation method of magnetic particle is:
By the anhydrous FeCl of 4mmol3It being added in the diethylene glycol (DEG) of 50mL, stirring 40min~50min forms clear solution,
Then the trisodium citrate of 1.6mmol is added, be heated to 80 DEG C and stirs 30min formation clear solution, is then added
The anhydrous sodium acetate of 12.0mmol is stirred for 30min, is then transferred in the stainless steel autoclave of polytetrafluoroethyllining lining and carries out
Sealing, keeps the temperature 6h at 240 DEG C for autoclave, obtains Fe3O4Magnetic nanoparticle.
Cation is 1- ethyl-3-methylimidazole, anion F in ionic liquid described in step 21-；
Surfactant described in step 2 is block polymer P123；
Diluent described in step 2 is N,N-dimethylformamide；
Solvent a described in step 2 is ethyl alcohol, and solvent b is identical as solvent a；
Inert gas described in step 2 is nitrogen.
Fig. 1 is the photo in kind for testing the hydrogel sphere biomass magnetism carbosphere of step 2 preparation, can be with from figure
Find out that the gel microballon size of preparation is more uniform, spherical uniform, color is pale brown, this is because wherein containing Fe3O4Magnetic particle
Reason.
Fig. 2 is the photo in kind for testing the biomass magnetism carbosphere of a preparation, as can be seen from the figure tests a preparation
Carbosphere size it is more uniform, it is spherical uniformly.
Fig. 3 is the low power number stereoscan photograph for testing the biomass magnetism carbosphere of a preparation, as can be seen from the figure
The carbon ball of one preparation of test has certain pore structure.
Fig. 4 is the high magnification numbe stereoscan photograph for testing the biomass magnetism carbosphere of a preparation, can be seen that examination in figure
Small particle there are many testing in the carbon ball of a preparation, these particles are Fe 3 O 4 magnetic particles, and magnetic particle is in carbon ball
Inside it is uniformly distributed.
Claims (4)
1. a kind of method with agriculture and forestry organic waste material preparation biomass magnetism carbosphere, it is characterised in that prepared and given birth to agriculture and forestry organic waste material
The method of changing of magnetism carbosphere carries out according to the following steps:
One, it prepares agriculture and forestry organic waste material powder: agriculture and forestry organic waste material is cleaned up to and is cut into block, be 70 DEG C~105 DEG C in temperature
Under conditions of dry 6h~for 24 hours, dry block agriculture and forestry organic waste material is then ground into the agricultural of 30 mesh~300 mesh with pulverizer
Waste powder；Agriculture and forestry organic waste material described in step 1 is rich cellulose-containing product waste material；
Two, it 1., by agriculture and forestry organic waste material powder is added in ionic liquid, stirs 4h under conditions of temperature is 60 DEG C~100 DEG C
~for 24 hours, whole filtrates are collected by filtration, surfactant, Fe are added into whole filtrates3O4Magnetic particle and diluent, then exist
Temperature stirs 4h~for 24 hours under conditions of being 40 DEG C~60 DEG C, obtains mixed liquor；
2., mixed liquor poured into the syringe with syringe needle, inject mixed liquor into solvent a with syringe, the shape in solvent a
At multiple spherical particles, spherical particle is collected in solvent a；
3., spherical particle is immersed in 1h~2h in solvent b, collect spherical particle in solvent b；
4., by step 2 3. repetitive operation 3 times~5 times, obtain hydrogel sphere；
The mass ratio of the agriculture and forestry organic waste material powder and ionic liquid is (1~15): 100；The ionic liquid and surface
The mass ratio of activating agent is 50:(1~5)；The ionic liquid and Fe3O4The mass ratio of magnetic particle is 50:(1~10)；Institute
The mass ratio of the ionic liquid and diluent stated is 5:(3~10)；The size of the syringe needle is 0.45mm × 15mm；
Solvent a described in step 2 is the mixture of one or more of methanol, ethyl alcohol, acetone and chloroform, solvent b
It is identical as solvent a；
Cation is 1- ethyl-3-methylimidazole, 1- butyl -3- methylimidazole or 1- alkene in ionic liquid described in step 2
Propyl -3- methylimidazole, anion F1-、Cl1-、Br1-、BF4 1-、PF6 1-Or OAc1-；
Surfactant described in step 2 is hexadecyltrimethylammonium chloride, cetyl trimethylammonium bromide, block
Polymer P 123 or block polymer F127；
Diluent described in step 2 is dimethyl sulfoxide, n,N-Dimethylformamide or n,N-dimethylacetamide；
Three, the hydrogel sphere for preparing step 2 dry 4h~12h under conditions of temperature is 15 DEG C~50 DEG C, then in inertia
With 3 DEG C/min~10 DEG C/min heating rate from room temperature to 500 DEG C~1000 DEG C under gas shield, protected in inert gas
Carbonization 1h~3h, under inert gas protection furnace cooling obtain biomass under conditions of shield and temperature are 500 DEG C~1000 DEG C
Magnetic carbosphere.
2. a kind of method with agriculture and forestry organic waste material preparation biomass magnetism carbosphere according to claim 1, feature exist
In the described cellulose-containing product waste material of richness be peanut shell, it is melon seed cases, corn stover, rice straw, sawdust, branch, primary
Property chopsticks or waste paper.
3. a kind of method with agriculture and forestry organic waste material preparation biomass magnetism carbosphere according to claim 1, feature exist
Fe described in step 23O4The preparation method of magnetic particle is:
By the anhydrous FeCl of 4mmol3Be added in the diethylene glycol (DEG) of 50mL, stirring 40min~50min formed clear solution, then plus
The trisodium citrate for entering 1.6mmol is heated to 80 DEG C and stirs 30min formation clear solution, the nothing of 12.0mmol is then added
Water sodium acetate is stirred for 30min, is then transferred in the stainless steel autoclave of polytetrafluoroethyllining lining and is sealed, by autoclave
6h is kept the temperature at 240 DEG C, obtains Fe3O4Magnetic nanoparticle.
4. a kind of method with agriculture and forestry organic waste material preparation biomass magnetism carbosphere according to claim 1, feature exist
Inert gas described in step 2 is nitrogen or argon gas.
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| CN108355615B (en) * | 2018-03-10 | 2020-12-25 | 扬州工业职业技术学院 | Preparation method of ionic liquid modified corncob-based material and application of ionic liquid modified corncob-based material in degradation of pesticide residues in soil |
| CN109160666A (en) * | 2018-10-09 | 2019-01-08 | 中国石油集团川庆钻探工程有限公司 | A kind of fracturing outlet liquid process for reclaiming |
| CN109437193A (en) * | 2018-12-26 | 2019-03-08 | 济南大学 | A method of active carbon is prepared based on litter decoration |
| CN109755623A (en) * | 2019-02-28 | 2019-05-14 | 山东理工大学 | A kind of direct carbon solid oxide fuel cell group of micro-tubular based on melon seed cases derivatived fuel |
| CN110828838B (en) * | 2019-11-22 | 2022-02-11 | 河北师范大学 | Preparation method of palladium-based catalyst with particle size larger than 10 microns and snowflake ball morphology |
| CN115382547B (en) * | 2022-09-09 | 2024-03-15 | 四川农业大学 | Iron-carbon microsphere composite catalyst for Fenton-like system, and preparation method and application thereof |
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