CN109569510A - A kind of preparation method of peanut shell base magnetic active carbon - Google Patents
A kind of preparation method of peanut shell base magnetic active carbon Download PDFInfo
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- CN109569510A CN109569510A CN201811479494.0A CN201811479494A CN109569510A CN 109569510 A CN109569510 A CN 109569510A CN 201811479494 A CN201811479494 A CN 201811479494A CN 109569510 A CN109569510 A CN 109569510A
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
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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
- Y02P20/10—Process efficiency
Abstract
A kind of preparation method of peanut shell base magnetic active carbon, method include taking certain mass peanut husk as raw material, the agent of certain mass magnetism are added, by raw material peanut shell and ZnCl2Mass ratio is that the ratio of 1:2 is impregnated in ZnCl2It in solution, stirs evenly, is put into 105 DEG C of baking ovens and dries after time of infusion, weigh certain mass material drying and be placed in resistance furnace activation a period of time under certain vacuum degree and activation temperature.Product is taken out after experiment and boils half an hour in boiling water, after being washed to neutrality with deionized water, is filtered, is dried, grinding up to magnetic active carbon product.This method has many advantages, such as that preparation process is simple, low in cost, energy conservation and environmental protection, and the magnetic active carbon prepared has the advantages that have excellent magnetic characteristics, magnetisable material is not easily to fall off, good adsorption performance.
Description
Technical field
The invention belongs to environmental protection, field of waste resource comprehensive utilization is related to a kind of preparation method of magnetic active carbon
And the magnetic active carbon prepared by this method.
Background technique
Agriculture and forestry organic waste material derives from plant, is mainly made of C, H, O, N etc., is the product of photosynthesis of plant, has
Reproducibility, sustainability.China is an agricultural and forestry production big country, and agricultural are resourceful, and in China, agriculture and forestry organic waste material is in addition to one
Part is used to generate electricity etc. outside recovery energies, and there are also a big chunk abandoned or burnings, are prepared using abandoned biomass
Active carbon not only can reduce environmental pressure, can also increase economic benefit.
Active carbon because its high-specific surface area, pore structure abundant, excellent absorption property are widely used in every field,
Such as medical treatment and pharmacy, Chemical Manufacture, environmental pollution etc..But when active carbon applies to these fields, often there is recycling difficulties
Problem, the method for the recovered carbon of extensive utilization is mainly the precipitation method and floatation at present, these methods can only recycle big
Grain active carbon, but it is bad for the recovering effect of little particle active carbon, and the active carbon for having adsorbed harmful substance will cause water body
Secondary pollution increases environmental pressure.Magnetic separation technology after decades of development, technology relative maturity, but active carbon one
As do not have magnetism, active carbon is assigned into magnetic, make active carbon have magnetism, using magnetic method recovered carbon, this method is not only grasped
Make simply, and the rate of recovery of active carbon is very high, it is possible to prevente effectively from secondary pollution problem of the waste active carbon to water body.But both at home and abroad
It is more complicated to prepare magnetic active carbon inventive technique, high production cost, and magnetisable material is easy to fall off, such as number of patent application
201410596141.4, entitled " preparation method of eucalyptus base magnetic active carbon ", number of patent application 201410145644.X, name
Referred to as " a kind of preparation method of biomass-based magnetic active carbon ".The method for preparing magnetic active carbon of previous patent disclosure
Are as follows: first 400 DEG C of eucalyptus block are carbonized, then eucalyptus charcoal and activator, magnetic agent are mixed in a certain ratio, when impregnating one section
Between after drying to be put into temperature be that 60~120min is activated in 600~900 DEG C of Muffle furnace, washing, dry, grinding obtain eucalyptus base
Magnetic active carbon.In eucalyptus charcoal: K2CO3: FeCl3Mass ratio is 1:1.5:1, and dip time is 7 hours, activation temperature 800
DEG C, activation time is when being 60min, the magnetic active carbon methylene blue adsorption value that is prepared is 400.05mg/g, iodine sorption value
For 655.627mg/g, saturation magnetization 28.67emu/g.The technical method of the latter patent disclosure are as follows: discard agricultural
It is added to together with iron precursor in polyhydric alcohol solutions after the processing of object acid in 270 DEG C~280 DEG C condition lower limit oxygen pyrolysis or hydro-thermal
Charing obtains magnetic bio carbon matrix, and wherein iron precursor ferric acetyl acetonade or 180 DEG C of carbonyl iron resolve into magnetic Nano material
Fe3O4Back loading is on biological carbon matrix, and then magnetic nanoparticle is made in 500 DEG C of sintering under nitrogen protection.It is prepared
Magnetic nanoparticle specific surface area is up to 130.34m2/ g, hole volume product are up to 0.1522cm3/g.Both the above method is all
Magnetic active carbon is prepared using " two-step method ", and the temperature that the method preparation process of previous patent needs is very high, not only prepares
Complex process, and high preparation temperature considerably increases production cost, and absorption property is also undesirable.The latter patent system is for magnetic
Property active carbon method preparation magnetic nanoparticle specific surface area and pore volume it is all smaller.For another example number of patent application is
200910077154.X, title are as follows: prepare magnetic described in a kind of " preparation method of magnetic active carbon and the magnetic active carbon " patent
Property active carbon method are as follows: first by coal raw materials, magnetic additive, binder and surfactant be sufficiently mixed resulting mixture,
It is press-formed and dries, then the molding after drying is subjected to charing process in 400~700 DEG C of temperature, carbide is made, then
Carbide activation is prepared into magnetic active carbon at a temperature of 700~1000 DEG C, the method use binders, be easy to cause stifled
Hole, and then the absorption property of active carbon is reduced, iodine number is 700mg/g or so.
In conclusion preparing magnetic active carbon at present is primarily present preparation temperature height；It is not economical enough；Preparation process is multiple
It is miscellaneous；The problems such as magnetic active carbon magnetic property of preparation is bad, and magnetisable material is easy to fall off and absorption property is bad.Although at present
There is research invention one-step method to prepare magnetic active carbon, but need to be carried out at hydro-thermal to generate magnetisable material in the preparation material stage
Reason, joined such as sodium hydroxide alkaline reagent, keeps the material preparation stage complicated and increases preparation cost.
Summary of the invention
The shortcomings that in view of existing technologies, using simpler preparation process, step activation magnetizes peanut to the present invention under vacuum
Shell prepares magnetic active carbon, it is therefore an objective to it is further simplified preparation process, it is energy saving, and preparation cost is reduced, it is steady to prepare magnetic property
Determine, magnetisable material is not easily to fall off, good adsorption performance magnetic active carbon.
The invention is realized by the following technical scheme:
1) by the washing of discarded peanut shell, it is dry, be crushed it is spare after 40 mesh molecular sieves.
2) it weighs certain mass peanut shell powder to be placed in a beaker, adds certain mass magnetism agent Fe2O3Powder.
3) certain mass activator ZnCl is taken2It is dissolved in the water, by ZnCl obtained2Solution is poured into equipped with peanut shell powder
It in the beaker of magnetic agent powder, stirs, impregnates 12~36 hours.
4) raw material after dipping is put into 105 DEG C of baking ovens and is dried.
5) it takes drying material in certain mass step 4 to be placed in self-control resistance furnace, controls 10~50kPa of vacuum degree, setting
400~600 DEG C of activation temperature, activate 0~120min.It is taken out after cooling, is crushed, is put into boiling water and boils 30min, use deionized water
It washs repeatedly, until the aqueous solution pH after washing is about 7.It is put into ground 200 mesh molecular sieve after drying in 120 DEG C of baking ovens, i.e.,
Magnetic active carbon is made.
The present invention has the advantage that one, under vacuum conditions compared with the technical matters for preparing magnetic active carbon in the past
It is lower to prepare activation temperature required for magnetic active carbon, can effectively save the energy, reduces production cost, and want to equipment
It asks and is relatively low, the pernicious gas in reaction process can be collected, and pollution environment is avoided；Two, by peanut shell directly with work
Agent, magnetic agent are mixed with dipping, and simplify magnetic active carbon preparation process, magnetic agent is stronger in conjunction with biomass, makes to generate
Magnetic active carbon magnetic property it is more preferable, magnetic agent be Fe2O3, cost is lower with respect to other magnetic agent.Three, raw material peanut shell is
A kind of agricultural wastes, abundance are cheap.Four, not only absorption property is excellent for the magnetic active carbon prepared through the invention
It is good, and magnetic property is also satisfactory.
Detailed description of the invention
Fig. 1 (a)~(d) respectively represents the magnetic hysteresis tropic for the magnetic active carbon that Examples 1 to 4 is prepared.
Fig. 2 (a)~(d) respectively represents the Magneto separate effect photo for the magnetic active carbon that Examples 1 to 4 is prepared.
Specific embodiment
Embodiment 1
10g peanut shell powder is weighed, magnetic agent Fe is added2O31g；Weigh 20gZnCl2, add 40ml water to dissolve, by ZnCl2
Solution pours into the beaker equipped with peanut shell powder and magnetic agent, is sufficiently stirred, and is uniformly mixed raw material.Burning is tamping with preservative film
Rim of a cup is placed 24 hours；Raw material is put into 105 DEG C of baking ovens after 24 hours and is dried.12g drying material is taken to be placed in self-control resistance furnace
Device activation, 450 DEG C of activation temperature of setting, control system pressure are 10kPa, activation time 60min, take out, smash after cooling
It is broken, 30min is boiled in boiling water, is washed repeatedly with deionized water, until when aqueous solution pH is 7, filtering, in 120 DEG C of electric heating air blast
It is dried in drying box, ground 200 mesh molecular sieve, magnetic active carbon is made.Being detected magnetic activated carbon-iodine adsorptive value is
920.34mg/g, methylene blue adsorption value 366.18mg/g, saturation magnetization 8.96emu/g, remanent magnetism 1.16emu/
G, coercivity 99.56Oe.
Embodiment 2
10g peanut shell powder is weighed, magnetic agent Fe is added2O31g；Weigh 20gZnCl2, add 40ml water to dissolve, by ZnCl2
Solution pours into the beaker equipped with peanut shell powder and magnetic agent, is sufficiently stirred, and is uniformly mixed raw material.Burning is tamping with preservative film
Rim of a cup is placed 24 hours；Raw material is put into 105 DEG C of baking ovens after 24 hours and is dried.12g drying material is taken to be placed in self-control resistance furnace
Device activation, 450 DEG C of activation temperature of setting, control system pressure are 10kPa, activation time 30min, take out, smash after cooling
It is broken, 30min is boiled in boiling water, is washed repeatedly with deionized water, until when aqueous solution pH is 7, filtering, in 120 DEG C of electric heating air blast
It is dried in drying box, ground 200 mesh molecular sieve, magnetic active carbon is made.Being detected magnetic activated carbon-iodine adsorptive value is
989.41mg/g, methylene blue adsorption value 365.1mg/g, saturation magnetization 7.12emu/g, 0.91emu/g, coercivity
For 108.16Oe.
Embodiment 3
10g peanut shell powder is weighed, magnetic agent Fe is added2O30.6g；Weigh 20g ZnCl2, add 40ml water to dissolve, it will
ZnCl2Solution pours into the beaker equipped with peanut shell powder and magnetic agent, is sufficiently stirred, and is uniformly mixed raw material.Use preservative film
Beaker mouth is tamping to place 24 hours；Raw material is put into 105 DEG C of baking ovens after 24 hours and is dried.12g drying material is taken to be placed in self-control
The activation of resistance furnace apparatus, 450 DEG C of activation temperature of setting, control system pressure are 10kPa, activation time 60min, are taken after cooling
Out, it smashs to pieces, 30min is boiled in boiling water, washed repeatedly with deionized water, until when aqueous solution pH is 7, filtering, in 120 DEG C of electric heating
It is dried in air dry oven, ground 200 mesh molecular sieve, magnetic active carbon is made.Being detected magnetic activated carbon-iodine adsorptive value is
1050.83mg/g, methylene blue adsorption value 365.64mg/g, saturation magnetization 2.59emu/g, remanent magnetism 0.25emu/
G, coercivity 80.56Oe.
Embodiment 4
10g peanut shell powder is weighed, magnetic agent Fe is added2O31.2g；Weigh 20g ZnCl2, add 40ml water to dissolve, it will
ZnCl2Solution pours into the beaker equipped with peanut shell powder and magnetic agent, is sufficiently stirred, and is uniformly mixed raw material.Use preservative film
Beaker mouth is tamping to place 24 hours；Raw material is put into 105 DEG C of baking ovens after 24 hours and is dried.12g drying material is taken to be placed in self-control
The activation of resistance furnace apparatus, 450 DEG C of activation temperature of setting, control system pressure are 10kPa, activation time 60min, are taken after cooling
Out, it smashs to pieces, 30min is boiled in boiling water, washed repeatedly with deionized water, until when aqueous solution pH is 7, filtering, in 120 DEG C of electric heating
It is dried in air dry oven, ground 200 mesh molecular sieve, magnetic active carbon is made.Being detected magnetic activated carbon-iodine adsorptive value is
909.39mg/g, methylene blue adsorption value 349.89mg/g, saturation magnetization 8.98emu/g, remanent magnetism 1.12emu/
G, coercivity 115.64Oe.
Claims (6)
1. a kind of preparation method of peanut shell base magnetic active carbon, it is characterised in that prepared using peanut shell as one step of raw material magnetic living
Property charcoal, includes the following steps:
It 1) will be spare after the washing of discarded peanut shell, dry, crushing；
2) certain mass peanut shell powder is weighed, the magnetic agent of certain mass ratio is added thereto.
3) certain mass activator ZnCl is weighed2, it is dissolved in a certain amount of water, obtained solution A.
4) solution A in step 3 is poured into step 2 peanut shell powder, magnetic agent, activator and peanut shell powder is mixed
Uniformly, it after time of infusion, dries in an oven, obtains raw material B；
5) it takes certain mass raw material B to be put into homemade activation device, certain activation temperature, certain vacuum degree, activation one is set
It fixes time.After reaction, it after temperature of charge drops to room temperature, takes out product and is crushed, boiled in boiling water a period of time, washing is extremely
When solution is neutral, then dries and grind to get product magnetic active carbon.
2. according to the method described in claim 1, its characterization method, is in 2) that magnetic agent is Fe2O3。
3. according to the method described in claim 1, its characterization method, is in 4) that dip time is 12~36 hours.
4. according to the method described in claim 1, its characterization method, is in 5) that system pressure is 10kPa~50kPa.
5. according to the method described in claim 1, its characterization method, is in 5) that activation temperature is 400 DEG C~600 DEG C.
6. according to the method described in claim 1, its characterization method, is in 5) that activation time is 0min~120min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110713184A (en) * | 2019-11-28 | 2020-01-21 | 湖南省格林森炭业股份有限公司 | Secondary processing method of activated carbon |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110713184A (en) * | 2019-11-28 | 2020-01-21 | 湖南省格林森炭业股份有限公司 | Secondary processing method of activated carbon |
| CN110713184B (en) * | 2019-11-28 | 2024-04-05 | 湖南省格林森炭业股份有限公司 | Secondary processing method of activated carbon |
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Application publication date: 20190405 |