CN107376836A - A kind of preparation method of ature of coal magnetic-particle activated carbon - Google Patents
A kind of preparation method of ature of coal magnetic-particle activated carbon Download PDFInfo
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Abstract
A kind of preparation method of ature of coal magnetic-particle activated carbon, activates and produces the ature of coal magnetic-particle activated carbon at high temperature after coal particle is mixed with ferrocene.The preparation method of the present invention greatly reduces the use of chemical reagent, realizes green production, and technique is simple, and cost is cheap, and obtained product has high added value, is with a wide range of applications.
Description
Technical field
The invention belongs to technical field of active carbon, and in particular to a kind of preparation side of ature of coal magnetic-particle activated carbon granule
Method, especially the high anthracite of inexpensive carbon content is prepared by catalysis, the load of ferrocene and has magnetic graininess work
Property charcoal.
Background technology
Activated carbon is a kind of sorbing material of loose structure, has abundant pore structure, and specific surface area is big, environmental protection,
It is widely used in the industries such as medicine, food, chemical industry.It can be good at only by the processing in activated carbon later stage, modification
Change color, recycling design and rare metal of waste gas and sewage, removing food and medicament etc..The recycling of activated carbon is to make
Extension, and the major issue solved is needed at present, existing method includes filtration method, sedimentation, magnetic method.Its
Middle magnetic method can the recovery of selectivity have magnetic activated carbon, will not be restricted by activated carbon granule size, it is convenient real
It is existing.Therefore, magnetic active carbon is one of focus of research.Activated carbon, which prepares conventional raw material, wood chip, sludge, rice husk, coal etc.,
Wherein coal mass active carbon has the advantages that big hardness, Stability Analysis of Structures, easily regenerates, be cheap, has fairly good application prospect.
The preparation technology of ature of coal magnetic active carbon generally includes to be molded, carbonize, activate and magnetize four parts, is become according to coal
The difference of matter degree need to carry out coal blending and prepare desired carbon content to reach activated carbon, need adhesive during kneading；Activation process
Need to add the catalyst such as hydrogen-oxygen potassium, zinc chloride in order that pore structure is more abundant；Magnetic history needs to add containing ferromagnetic
Salting liquid and some surfactants, all in all processing step is numerous and diverse, and additive easily causes environmental pollution more, prepares cost
Also it is higher.
Directly magnetized the most succinctly using active carbon finished products, but cost of material greatly improves, and common methods have dipping
Method, mixing method, bonding method and Magnetic reagent method, these methods are required for adding surfactant, acid-base solution and magnetisable material etc.
Reacted.As CN 101818338A disclose the method that non-palladium activation method prepares nickel radical magnetic active carbon, the invention is saved into
Type, charing, activation stage, directly powdered activated carbon is impregnated in chitosan acetic acid solution, nickel plating is magnetized, from whole magnetic
Property activated carbon preparation process from the point of view of, only belong to magnetized spot, not inherently simplify magnetic active carbon preparation technology,
The use of additive is reduced, opposite cost increase, easily causes environmental pollution, while magnetisable material easily blocks pore structure, drop
The absorption property of low activity charcoal.
With going deep into for research, the preparation method of coal base magnetic active carbon updates simplification, as CN 101497028A are public
A kind of preparation method of magnetic active carbon and the magnetic active carbon are opened.The invention is by coal raw materials, magnetic additive, binding agent
Magnetic active carbon is made with carbonizing, activating again after surfactant mixed-forming.Although the invention by magnetic history with activity
Charcoal preparation process is combined, and simplifies technique to a certain extent, but the additive such as catalyst, adhesive, Magnetic reagent does not have still
Reduce, the pollution to environment is still present, and the material such as various iron, manganese, nickel or cobalt that the kneading and compacting stage adds is not easy to merge, and makes
Easily there is the problems such as loose, broken in the magnetic active carbon short texture being prepared, application process.And for example CN
105457594A discloses a kind of preparation method of hydrophilic magnetic active carbon, and the invention is first by feed coal, magnetisable material, binding agent
With surfactant be sufficiently mixed shaping, charing, then add methanol, glyceride, 20wt% ammoniacal liquor, manganese nitrate, chloroform,
A series of additive treating carbides such as nitric acid, bromine water, are finally activated.Although the invention improves activated carbon to a certain extent
Specific surface area, but magnetic efficiency is general, and substantial amounts of additive, which adds, to be prepared cost, produces substantial amounts of pollutant, and is added
Add treatment process complicated, be not suitable for industrial production.
CN 101972629A disclose the preparation method and its coal base magnetic active carbon of a kind of coal base magnetic active carbon, should
Invention prepares magnetic active carbon using coal includes coal dust deliming, the preparation of Magnetic reagent, catalyzing and carbonizing, the several steps of activation, from original
Material angle sees that useful raw materials scope is wide, but deliming process adds Feedstock treating cost, and processing step is still numerous and diverse, it is difficult to implement
Degree is big, and it is molten to prepare dodecyl sodium sulfate, ferric chloride solution, ammoniacal liquor, sodium hydroxide solution or potassium hydroxide that Magnetic reagent is used
Liquid is big for environment pollution, cost is high, and the activator (potassium hydroxide or sodium hydroxide) that follow-up charing, activation process are used increases again
Cost and the pollution to environment.CN 102614830A disclose a kind of preparation method of coal base manganese magnetic active carbon, the invention
Magnetic reagent is made in electrolytic manganese residues, although waste reclamation additive is not reduced, technique is not also substantially simplified.CN
The magnetic active carbon that 103736457A discloses a kind of preparation method of magnetic active carbon and prepared by this method, the invention utilize
Abandoned biomass and Magnetic reagent mixed pyrolysis obtain magnetic active carbon, although production technology has been simplified, raw material needs early stage
Impregnated with zinc chloride, need laurate, lauryl sodium sulfate as surfactant and acid, alkali soluble during preparation Magnetic reagent
Liquid adjusts pH value, and cost is high and easily causes environmental pollution, although the abandoned biomass cost of selection is low, structure is not steady enough
Fixed, obtained magnetic active carbon is easily loose, damaged.
Ature of coal magnetic active carbon at home and abroad gradually expanded in market development space in recent years, in order to improve coal mass active carbon
Market value, suitable for the use in each field, prepare Stability Analysis of Structures using simple, green method, pore structure is enriched, easily divides
From, recovery magnetic active carbon it is most important.
The content of the invention
Therefore, it is an object of the invention to provide a kind of preparation method of ature of coal magnetic-particle activated carbon, this method is significantly
Reduce the use of chemical reagent, realize green production, and technique is simple, cost is cheap, and obtained product has high added value,
It is with a wide range of applications.
For the above-mentioned purpose, the present invention adopts the following technical scheme that：
A kind of preparation method of ature of coal magnetic-particle activated carbon, including it is as follows：In height after coal particle is mixed with ferrocene
Activated under temperature and produce the ature of coal magnetic-particle activated carbon.
Raw material of the present invention can select the coal of low cost, and the raw coal particle of appropriate particle size is obtained by simple pretreatment,
Addition ferrocene is heat-treated, and a step completes the preparation of magnetic active carbon, ferrocene (C10H10Fe) play during the course of the reaction
Two kinds of effects of catalysis and load.
This invention simplifies the preparation technology of activated carbon, only activates a procedure under air by adding ferrocene
Magnetic active carbon particle is prepared, that is, eliminates chemical treatment and the kneading and compacting of raw material, again do not have to repeatedly add catalyst,
Activating agent, Magnetic reagent etc., not only simplify production technology, reduce preparation cost, also greatly alleviate problem of environmental pollution,
Green production, green product are just really accomplished.The present invention realizes the maximization of resource to product again from raw material to preparation technology
Utilize, high added value, the magnetic-particle activated carbon of recyclable regeneration meet the Resources Strategy target in China, effectively raise me
The economic benefit and social benefit of state, have responded the Strategy for economic development of China's green economy.
Preferably, the raw material of the coal particle is anthracite, preferably high corruption degree, high-carbon contain, measure ash content and wave
The anthracite that hair point is low, cost is low.
The raw material used is the anthracite of low cost, and carbon content is high, and ash content and volatile matter are relatively low, have degree of metamorphism it is high,
The advantages such as Stability Analysis of Structures, hardness is big, compared with the prior art, the present invention need not carry out the place of deliming processing and chemical agent
Reason, processing is convenient, and operation difficulty is small, cost-effective, will not cause the pollution problem of chemical agent；Also, Coal Stkucture By Using is steady
Fixed, hardness is big, and the magnetic active carbon pore structure being prepared is abundant and firm, and cracky, is not easy to recycling.
In a preferred embodiment, component content is as follows in anthracite raw material：Ash content 5-10%, volatile matter 5-12%, moisture
1-5%, fixed carbon 70-90%, preferably ash content 7.05%, volatile matter 8.97%, moisture 2.53%, fixed carbon 81.45%.
Preferably, the particle diameter of the coal particle is 60-80 mesh, for example, 65 mesh, 70 mesh, 75 mesh etc..It can be passed through by anthracite
Obtained after crossing broken, grinding through screening.Feed coal grain diameter 60-80 mesh (0.2-0.3mm), it ensure that the ratio surface of activated carbon
Product and reactivity, are easy to the recycling of activated carbon repeatedly.
Preferably, the coal particle pre-wash and drying.
Preferably, it is to be dried more than 10 hours at 100-150 DEG C to dry, and is dried 24 hours preferably at 120 DEG C.
Preferably, the mass ratio of coal particle and ferrocene is 1:3-3:1, for example, 1:3、1:2、1:1、2:1、3:1 etc., it is excellent
Elect 0.5-2 as:1.
Preferably, the time that coal particle mixes with ferrocene is 30-90 minutes, for example, 30min, 45min, 60min,
75min, 90min etc., preferably 60min.
Preferably, activation is carried out in confined conditions.It can be carried out in resistance furnace.
Preferably, the atmosphere of activation is air atmosphere.
Preferably, activate at 800-1200 DEG C, for example, 820 DEG C, 850 DEG C, 890 DEG C, 930 DEG C, 980 DEG C, 1050 DEG C,
1100 DEG C, 1150 DEG C etc. it is lower carry out 1-5 hours, for example, 1.2 hours, 1.7 hours, 2.1 hours, 2.5 hours, 3.2 hours,
3.8 hours, 4.5 hours etc., 2-3 hours are carried out preferably at 1000 DEG C.Ferrocene play the role of it is combustion-supporting, 100 DEG C just can show
Distillation is write, feed coal is eaten into erosion in the environment of ferrocene and forms preliminary pore structure, with the rise of temperature, ferrocene decomposes
And react to obtain ferroso-ferric oxide with the organic matter on coal surface and some gas organic matters continue to promote feed coal pore structure
Formed, while ferroso-ferric oxide completes load on the surface of coal.
After activation terminates after the activated carbon cooling made from, wash to neutrality, dry repeatedly using deionized water, such as
Dried 24 hours at 120 DEG C.
Preferably, the preparation method comprises the following steps：
(1) it is well mixed after particle diameter is dried for the coal particle of 60-80 mesh with ferrocene with mass ratio 0.3-4；
(2) mixture obtained by step (2) is activated into 1-5 hours at 800-1200 DEG C；
(3) activation cools down after terminating, washs, is drying to obtain the ature of coal magnetic-particle activated carbon.
Preferably, the preparation method comprises the following steps：
(1) take anthracite to carry out coarse crushing and screening, carry out in small, broken bits to the anthracite of bulky grain and sieve, collection cut size exists
The smokeless coal particle of 60-80 mesh (0.2-0.3mm)；
(2) the smokeless coal particle in step 1) is subjected to ion, is dried 24 hours at 120 DEG C and obtain feed coal
Grain；
(3) feed coal obtained in step 2) is uniformly mixed with ferrocene, incorporation time is 30-90 minutes, feed coal
Mass ratio with ferrocene is：1:2；1:1；2:1；
(4) it will be put in the mixed uniformly feed coal of ferrocene in resistance furnace, and be warming up to 1000 DEG C in confined conditions, lived
Change 2 hours；Ferrocene plays the role of combustion-supporting, just can significantly be distilled at 100 DEG C, feed coal is eaten into erosion shape in the environment of ferrocene
Into preliminary pore structure, with the rise of temperature, ferrocene decomposes and reacts to obtain four oxidations three with the organic matter on coal surface
Iron and some gas organic matters continue to promote the formation of feed coal pore structure, while ferroso-ferric oxide is completed to bear on the surface of coal
Carry.
(5) after activation terminates, sample furnace cooling is waited, granular activated carbon is collected, is washed with deionized water to neutrality,
Dried 24 hours at 120 DEG C and produce the ature of coal magnetic-particle activated carbon.
Coal-based granular activated carbon standard GB/T 7702.1-7702.14-87 be can refer to obtained activated carbon in step 5)
Particle carries out methylene blue adsorption number detection.
Beneficial effects of the present invention are as follows：
1), it is of the invention raw coal particle after pretreatment is uniformly mixed with ferrocene after hot place is carried out directly in resistance furnace
Reason, preparation technology simplify, and additive is largely reduced.Compared with prior art, step is simple, it is not necessary to coal blending kneading, it is not necessary to
With Magnetic reagent impregnated raw material coal, it is not required that separately plus catalyst is carbonized and activated.The present invention is by magnetic additive with being catalyzed
Agent is replaced with a kind of material of ferrocene, in heat treatment process can catalysed promoted activated carbon structure formation, and can complete iron
The load of magnetisable material.
2), method technique of the invention is simple, easy to operate, only needs to add ferrocene in preparation process, avoids Magnetic reagent
Prepare, the largely reuse of chemical agents in catalyst activation procedure, avoid the environmental pollution that production is brought, it is cost-effective,
And by the mixing of ferrocene and feed coal, heat treatment, the load of ferroso-ferric oxide is completed during being generated in aperture, is kept away
The problem of pore structure is blocked is exempted from.
3), the magnetic active carbon that this method is prepared is tested through application, has good adsorptivity and recycling
Effect.Magnetic active carbon specific surface area prepared by the present invention reaches 300m2/ more than g, reach as high as 1300m2/ g or so, total pore volume
Product reaches 0.3cm3/ more than g, reach as high as 0.8cm3/ more than g, meet activated carbon standard；Saturation magnetization reaches
More than 0.28emu/g, 1.2emu/g or so is reached as high as, coercivity reaches more than 89Oe, reaches as high as 288Oe or so, hardness
Greatly, recycling number can reach more than 10 times；There is no the use of chemical solution in preparation process, it is cost-effective, avoid
Environmental pollution, it is truly realized green production.
Brief description of the drawings
Fig. 1 is the XRD of ature of coal magnetic-particle activated carbon prepared by embodiment 1；
Fig. 2 is the ESEM of ature of coal magnetic-particle activated carbon prepared by embodiment 1；
Fig. 3 is the hysteresis curve of ature of coal magnetic-particle activated carbon prepared by embodiment 1.
Embodiment
The present invention will be further described with reference to the accompanying drawings and examples.
Embodiment 1
The raw material prepared using Ningxia anthratite as magnetic-particle activated carbon.
Smokeless Coal pretreatment：Ningxia anthratite is obtained into thin of anthracite through jaw crusher coarse crushing and ball mill are in small, broken bits
Grain, then sieved with moto-vibro screen, smokeless coal particle of the collection cut size between 0.2-0.3mm, removal of impurities is cleaned with deionized water,
It is placed in 120 DEG C of air dry oven and dries the raw material coal particle that acquisition in 24 hours prepares magnetic active carbon.
It is 1 that obtained raw material coal particle, which will be pre-processed, according to coal and ferrocene mass ratio:2, take feed coal 2g, ferrocene
Uniformly mixing is placed in closed resistance furnace 4g after 40 minutes, is heated to 1000 DEG C, is incubated 2 hours；Collect furnace cooling
Activated carbon sample be washed with deionized to neutrality, be placed in air dry oven and dried 24 hours at 120 DEG C, it is final to obtain
Magnetic active carbon particle.
Fig. 1 is the XRD of ature of coal magnetic-particle activated carbon prepared by embodiment 1, shows the magnetic activity being prepared
Charcoal has the crystal structure of ferroso-ferric oxide, shows that ferroso-ferric oxide has been combined with activated carbon；Fig. 2 is prepared by embodiment 1
Ature of coal magnetic-particle activated carbon ESEM, can it is shown that the pore structure figure for the magnetic active carbon particle being prepared
Intuitively to see abundant pore structure；The magnetic hysteresis that the magnetic active carbon particle that embodiment 1 is prepared is shown in Fig. 3 is returned
Line chart, change with the change of applied field strengths, coercivity and remanent magnetism be present, belong to typical ferromagnetic material, it was demonstrated that system
Standby obtained activated carbon has magnetic.
Magnetic active carbon specific surface area manufactured in the present embodiment is 1263.542m2/ g, total hole volume 0.825cm3/g；It is full
It is 0.766emu/g, coercivity 288.052Oe with the intensity of magnetization.
Embodiment 2：
The raw material prepared using Ningxia anthratite as magnetic-particle activated carbon.
Smokeless Coal pretreatment will pre-process obtained raw material coal particle according to coal and ferrocene mass ratio with embodiment 1
For 1:1, taking feed coal 3g, ferrocene 3g, uniformly mixing is placed in closed resistance furnace after 40 minutes, is heated to 1000 DEG C,
Insulation 2 hours；The activated carbon sample for collecting furnace cooling is washed with deionized to neutrality, is placed in air dry oven 120
Dried 24 hours at DEG C, it is final to obtain magnetic active carbon particle.
Magnetic active carbon specific surface area manufactured in the present embodiment is 761.443m2/ g, total hole volume 0.453cm3/g；It is full
It is 0.526emu/g, coercivity 160.217Oe with the intensity of magnetization.
Embodiment 3：
The raw material prepared using Ningxia anthratite as magnetic-particle activated carbon.
Smokeless Coal pretreatment will pre-process obtained raw material coal particle according to coal and ferrocene mass ratio with embodiment 1
For 2:1, taking feed coal 4g, ferrocene 2g, uniformly mixing is placed in closed resistance furnace after 40 minutes, is heated to 1000 DEG C,
Insulation 2 hours；The activated carbon sample for collecting furnace cooling is washed with deionized to neutrality, is placed in air dry oven 120
Dried 24 hours at DEG C, it is final to obtain magnetic active carbon particle.
Magnetic active carbon specific surface area manufactured in the present embodiment is 624.271m2/ g, total hole volume 0.326cm3/g；It is full
It is 0.496emu/g, coercivity 108.257Oe with the intensity of magnetization.
Embodiment 4：
The raw material prepared using Ningxia anthratite as magnetic-particle activated carbon.
Smokeless Coal pretreatment will pre-process obtained raw material coal particle according to coal and ferrocene mass ratio with embodiment 1
For 1:3, taking feed coal 1.5g, ferrocene 4.5g, uniformly mixing is placed in closed resistance furnace after 45 minutes, is heated to 800
DEG C, it is incubated 5 hours；The activated carbon sample for collecting furnace cooling is washed with deionized to neutrality, is placed in air dry oven
Dried 24 hours at 120 DEG C, it is final to obtain magnetic active carbon particle.
Magnetic active carbon specific surface area manufactured in the present embodiment is 956.327m2/ g, total hole volume 0.654cm3/g；It is full
It is 1.748emu/g, coercivity 90.233Oe with the intensity of magnetization.
Embodiment 5：
The raw material prepared using Ningxia anthratite as magnetic-particle activated carbon.
Smokeless Coal pretreatment will pre-process obtained raw material coal particle according to coal and ferrocene mass ratio with embodiment 1
For 3:1, taking feed coal 4.5g, ferrocene 1.5g, uniformly mixing is placed in closed resistance furnace after 45 minutes, is heated to
1200 DEG C, it is incubated 1 hour；The activated carbon sample for collecting furnace cooling is washed with deionized to neutrality, is placed in air dry oven
In dried 24 hours at 120 DEG C, it is final to obtain magnetic active carbon particle.
Magnetic active carbon specific surface area manufactured in the present embodiment is 316.772m2/ g, total hole volume 0.265cm3/g；It is full
It is 0.285emu/g, coercivity 89.603Oe with the intensity of magnetization.
XRD, ESEM, the hysteresis curve of above-described embodiment products obtained therefrom are shown to be had with the products obtained therefrom of embodiment 1
Similar performance.
Comparative example
The raw material prepared using Ningxia anthratite as magnetic-particle activated carbon.
Smokeless Coal pretreatment will pre-process obtained raw material coal particle according to coal and sodium hydroxide quality with embodiment 1
Than for 1:2, taking feed coal 2g, sodium hydroxide 4g, uniformly mixing is placed in closed resistance furnace after 45 minutes, is heated to
1000 DEG C, it is incubated 2 hours；The activated carbon sample for collecting furnace cooling is washed with deionized to neutrality, is placed in air dry oven
In at 120 DEG C dry 24 hours, finally obtain activated carbon granule.
Magnetic active carbon specific surface area prepared by this comparative example is 65.240m2/ g, total hole volume 0.0254cm3/g；It is full
It is 0emu/g, coercivity 0Oe with the intensity of magnetization.
It can just be attained the results expected it can be seen that the present invention uses coal particle to prepare activated carbon granule with ferrocene for raw material.
Obviously, above-described embodiment is only intended to clearly illustrate example, and is not the restriction to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of change or
Change.There is no necessity and possibility to exhaust all the enbodiments.And the obvious change thus extended out or
Among changing still in the protection domain of the invention.
Claims (10)
1. a kind of preparation method of ature of coal magnetic-particle activated carbon, it is characterised in that in height after coal particle is mixed with ferrocene
Activated under temperature and produce the ature of coal magnetic-particle activated carbon.
2. preparation method according to claim 1, it is characterised in that the raw material of the coal particle is anthracite, is preferably
High corruption degree, high-carbon contain, measures ash content and volatile matter is low, cost is low anthracite.
3. preparation method according to claim 1 or 2, it is characterised in that the particle diameter of the coal particle is 60-80 mesh.
4. according to the preparation method described in claim any one of 1-3, it is characterised in that the coal particle pre-wash is simultaneously done
It is dry.
5. preparation method according to claim 4, it is characterised in that dry be at 100-150 DEG C dry 10 hours with
On.
6. according to the preparation method described in claim any one of 1-5, it is characterised in that the mass ratio of coal particle and ferrocene is
1:3-3:1, preferably 0.5-2:1；
Preferably, the time that coal particle mixes with ferrocene is 30-90 minutes, preferably 60 minutes.
7. according to the preparation method described in claim any one of 1-6, it is characterised in that activation is carried out in confined conditions.
8. according to the preparation method described in claim any one of 1-7, it is characterised in that the atmosphere of activation is air atmosphere.
9. according to the preparation method described in claim any one of 1-8, it is characterised in that activation carries out 1- at 800-1200 DEG C
5 hours, 2-3 hours are carried out preferably at 1000 DEG C.
10. according to the preparation method described in claim any one of 1-9, it is characterised in that the preparation method includes following step
Suddenly：
(1) with ferrocene with mass ratio 1 after particle diameter is dried for the coal particle of 60-80 mesh:3-3:1 mixing 30-90 minutes；
(2) mixture obtained by step (2) is activated into 1-5 hours at 800-1200 DEG C；
(3) activation cools down after terminating, washs, is drying to obtain the ature of coal magnetic-particle activated carbon.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108187616A (en) * | 2017-12-29 | 2018-06-22 | 刘威林 | A kind of special magnetic charcoal of gold and silver and its manufacturing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108187616A (en) * | 2017-12-29 | 2018-06-22 | 刘威林 | A kind of special magnetic charcoal of gold and silver and its manufacturing method |
| CN110918052A (en) * | 2019-10-28 | 2020-03-27 | 安徽省通源环境节能股份有限公司 | Preparation process of magnetic livestock bone carbonized particle adsorbent |
| CN113753894A (en) * | 2021-09-30 | 2021-12-07 | 山西华青环保股份有限公司 | Preparation method of ferroferric oxide loaded active carbon |
| CN114768765A (en) * | 2022-05-12 | 2022-07-22 | 太原理工大学 | Preparation method of brown coal-based magnetic activated carbon and wastewater treatment method |
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