CN106517189B - A kind of uniform ultra micro mesoporous activated carbon and preparation method thereof for gas separation - Google Patents
A kind of uniform ultra micro mesoporous activated carbon and preparation method thereof for gas separation Download PDFInfo
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- CN106517189B CN106517189B CN201611060108.5A CN201611060108A CN106517189B CN 106517189 B CN106517189 B CN 106517189B CN 201611060108 A CN201611060108 A CN 201611060108A CN 106517189 B CN106517189 B CN 106517189B
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
- C01B3/508—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by selective and reversible uptake by an appropriate medium, i.e. the uptake being based on physical or chemical sorption phenomena or on reversible chemical reactions
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
Abstract
The present invention relates to a kind of uniform ultra micro mesoporous activated carbons and preparation method thereof for gas separation.Its technical solution is to mix semi-coke with mass ratio 1:0.01 ~ 0.2 with KOH, and water, assistant activator is added, and 1 ~ 36h is impregnated, then in N2Lower sequencing is protected to be warming up to 800 DEG C ~ 950 DEG C control thermal decompositions; and it is passed through water and carries out part steam activation 0.5h ~ 1.5h; most afterwards through pickling, be washed to neutrality after drying obtain uniform ultra micro mesoporous activated carbon; aperture integrated distribution is between 0.45 ~ 0.55nm; belong to ultramicropore; microporosity reaches 77cm up to 70% or more, to the adsorption capacity of hydrogen3/ g or more.For the present invention using semi-coke as raw material, cost of material is low, without charing, consumes energy low；Activation method is combined with KOH pretreatment with part steam activation, and KOH dosage is few, has low cost, and low pollution is conducive to the features such as mitigating the corrosion to equipment.Active carbon prepared by the present invention has even aperture distribution, possesses the characteristics such as ultra-microporous extremely abundant, can be applied to the gases separation field such as pressure swing adsorption hydrogen production or hydrogen storage.
Description
Technical field
The invention belongs to functional activity charcoal preparation technical fields.More particularly to a kind of uniform ultramicropore for gas separation
Active carbon and preparation method thereof.
Background technique
Gas absorption isolation technics has many advantages, such as efficient, energy conservation and environmental protection, simple process, being widely used to
The fields such as work, metallurgy, medical and health, environmental protection and bioengineering.The key of adsorption separation technology application is adsorbent, and is lived
Property charcoal be common one of adsorbent, mitigated since it is opposite to the adsorption strength of gas, so that desorption be made to be easier to, therefore
In gas separation process, the active carbon as adsorbent is often more superior than other adsorbents.It is industrial improve gas separation because
The key of element is that adsorbent has uniform ultra-microporous (0.3 ~ 0.5nm) abundant, so preparing uniform ultra-microporous
Active carbon be the key that solve efficient gas isolation technics.
Currently, the technology of preparing of the uniform ultra micro mesoporous activated carbon separated to large-scale production and application in efficient gas is not yet
It breaks through, causes pore-size distribution unreasonable, it is of low quality, and due to that cannot produce in enormous quantities, it is expensive etc., limit activity
Application and popularization of the charcoal in gas separation field.Therefore, comprehensively consider from the performance etc. of raw material sources, cost and product,
The present invention is directed to find a kind of method for preparing uniform ultra micro mesoporous activated carbon, to realize the regulation to activated carbon capillary, make made
Standby uniform ultra micro mesoporous activated carbon has efficient Molecular Sieving Properties, is easy to implement large-scale production, and reduces production and make
Use cost.
Semi-coke, also known as semicoke, structure are bulk, are the high-volatile bituminous coals of no cohesiveness or weakly caking in middle low temperature item
The solid carbonaceous product for the relatively low volatile that carbonization obtains under part.In recent years, goed deep into people with circular economy concept
The downstream industry chain of the heart, semi-coke industry is gradually expanded, and wherein the activated active carbon for preparing of semi-coke is considered most having development latent
Power.According to statistics, Shenmu County shares 600,000 tons or more of 43 family of semi-coke enterprise, and annual 80000000 tons of Shenmu County's local mine producing coal, wherein
One third is by destructive distillation at semi-coke, and semi-coke market has tended to be saturated.From the point of view of semi-coke nature, it is by low metamorphic grade
Low temperature distillation in coal, fixed 75% or more carbon content, content of ashes less than 10%, in the structure of charcoal containing a large amount of oxygen-containing, sulphur,
Dan Deng functional group, they are that charcoal possesses chemically active material base；In addition to this, semi-coke has higher mechanical strength, retains
Low rank coal possesses the characteristics such as pore structure abundant.
During producing active carbon, to increase specific surface area and regulation pore structure, not according to activation method used
Together, different activators, such as carbon dioxide, water vapour, NaOH, KOH, H are generallyd use3PO4, HNO3, ZnCl2Deng.Wherein using compared with
It is KOH activation method for a kind of widely activation method, the main hydrophilicity for utilizing KOH makees it with hydrophobic carbon surface
Used time, playing the role of pore-creating, (RuLing Tseng, Szu-Kung Tseng, KOH activation are to activated carbon pore structure and suction
The influence of attached performance, colloid and interface science, 2005,287:428-437).As " it is living that a kind of fast activating prepares high-specific surface area
Property charcoal method " (CN103771414A, 2014-05-07) prepare high specific surface micro-pore active carbon using the above method, but
Alkali charcoal ratio used is 1 ~ 4:1, and alkali consumption is larger.KOH activation method has the disadvantage that during production of active carbon
(1) activation yield is lower, and charcoal consumption is larger, and production cost is larger.(2) KOH is rotten to structure of reactor material under hot conditions
Corrosion is strong, and equipment construction cost is high, and service life is short；(3) slurry amount is big, also needs to cause a large amount of using hydrofluoric acid sometimes
The discharge of high concentration basic fluoride waste, causes Heavy environmental pollution.Another method for preparing active carbon is gas activation,
Current widely used activated gas is vapor, is after carbonizing raw material, to contact and react with vapor, in it
Portion forms flourishing gap structure.Because tar and hydrocarbon that raw material generates in carbonization process plug carbide hole
Gap reduces its specific surface area, and activity reduces, therefore is activated using this oxidizing gas of vapor, can not only remove residual
The tar and surface impurity in carbide are stayed in, blocked hole is dredged, at the same time it can also corrode carbide surface, is formed
New pore structure keeps carbide structure more flourishing.However, during steam activation, only with single activation gas
Body, so that the generation of hole is determined by the reactivity of gas and carbon structure, even if controlling different thermal decompositions in activation process
Parameter (activation temperature, activation time etc.), micropore, mesoporous generating process be similar.Therefore it is activated using pure gas
Specific pore structure should not be generated, is difficult significantly to regulate and control pore structure characteristic.
In conclusion the currently used active charcoal preparing process for gas separation, exists and is difficult to effective trim products
Pore-size distribution, high production cost, difficult control of reaction conditions, prouctiveness be low, equipment seriously corroded and seriously polluted etc. asks
Topic.
Summary of the invention
The present invention is directed to overcome prior art defect, it is therefore an objective to provide one kind using semi-coke as raw material, be soaked using low alkali carbon ratio
Stain pre-processes the uniform ultramicropore method for preparation of active carbon combined with part steam activation.The active carbon hole of this method production
Diameter is evenly distributed, and possesses ultra-microporous extremely abundant, can be used for efficient gas separation, have production cost is low, yield is high,
It is low to consume alkali, simple production process, advantages of environment protection.
The technical solution adopted by the present invention carries out as follows:
Step 1: using semi-coke as raw material, first by the KOH for accounting for 1 ~ 20wt% of raw material semi-coke, account for the work of 1 ~ 12wt% of raw material semi-coke
Change auxiliary agent and water is mixed, is configured to maceration extract, wherein the quality of water is 0.8 ~ 1.2 times of raw material semi-coke；Semi-coke is added again
Enter 1 ~ 36h of normal temperature dipping in maceration extract, pre-feed is made；
Step 2: pre-feed made from step 1 is moved into tube furnace, in N2Control thermal decomposition is carried out under protective atmosphere,
Wherein N2The flow of protective atmosphere is 150 ~ 300ml/min；The control thermal decomposition is first by tube furnace with 3 ~ 8 DEG C/min
Heating rate is warming up to 350 ~ 400 DEG C, keeps the temperature 0.5 ~ 1.5 h, then 800 are continuously heating to the heating rate of 3 ~ 8 DEG C/min ~
950 DEG C of progress part steam activations；The part steam activation be under the conditions of 800 ~ 950 DEG C of temperature into reaction tube
Water flow is introduced, wherein the flow of water is 1 ~ 5ml/min, water flow is closed after activating 0.5 ~ 1.5h, finally in N2It is cold under protective atmosphere
But to room temperature, uniform ultramicropore activated carbon crude product is made；
Step 3: uniform ultramicropore activated carbon crude product made from step 2 is washed with 5% HCl solution, is filtered,
And it is washed repeatedly with distilled water to neutrality and uniform ultra micro mesoporous activated carbon is made then in 110 DEG C of 12 h of freeze-day with constant temperature；
The aperture integrated distribution of the uniform ultra micro mesoporous activated carbon of the preparation belongs to ultramicropore between 0.45 ~ 0.55nm,
Specific surface area reaches 840m2/ g or more, for microporosity up to 70% or more, hydrogen sorption capacity reaches 77cm3/ g or more.
The semi-coke raw material is by the destructive distillation under middle cryogenic conditions of the high-volatile bituminous coal of no cohesiveness or weakly caking
It is pyrolyzed the solid carbonaceous product of obtained relatively low volatile.
The assistant activator is by 1 ~ 30% hydrogen peroxide, KNO3, 1 ~ 5wt% neopelex ethanol solution composition,
4:5:3 ratio is prepared in mass ratio.
The determination condition of the maximum adsorption capacity of the hydrogen is 25 DEG C, adsorptive pressure 11.4MPa.
Due to the adoption of the above technical scheme, the present invention has following technical effect that compared with prior art
(1) present invention is using semi-coke as raw material, in alkali charcoal than being only (0.01 ~ 0.2): carrying out under conditions of 1 to raw material semi-coke
Dipping, control thermal decomposition is carried out under the vapor atmosphere of part, uniform ultra micro mesoporous activated carbon is made.Since semi-coke itself possesses one
Fixed pore structure, surface oxygen-containing functional group rich in, the K in dipping process+It can be in OH—Under lubricating action easily into
Enter semi-coke pore interior.As temperature rises to 350 ~ 400 DEG C, KOH is in a molten state, and KOH reacts with carbon, makes fragrant knot
Branched carbon atoms and KOH in structure are combined into-C-OK structure, which easily decomposes at higher temperatures and leave micropore, is conducive to
The development of pore structure, increases porosity.KOH dosage is very small in preparation process, not only effectively reduces cost, it is often more important that
The corrosion of equipment and materials can be slowed down, simultaneously because alkali charcoal, than small, carbon source loadings, which increase, also significantly to be mentioned conducive to equipment capacity
It is high.
(2) method that the present invention is thermally decomposed using the control of the control rate of heat addition, temperature and time condition, selection exist
0.5 ~ 1.5 h is kept the temperature at a temperature of 350 ~ 400 DEG C, guarantees that KOH can immerse inside charcoal particle in the molten state, with aromatic structure
In branched carbon atoms be combined into-C-OK structure, the structure can with temperature increase gradually decompose and leave micropore, be conducive to
Uniform ultra-microporous development.
(3) in the selection of activation method, the present invention is used with minute quantity KOH dipping, the preparation of part vapor activation
Uniform ultra micro mesoporous activated carbon.KOH has pore-creating, erosion and catalytic action to raw material, but KOH dosage is few, overcomes because using
The shortcomings that corrosion to equipment caused by alkali activates and the pollution to environment, while using N2With the mixed atmosphere of vapor, water
The dosage of steam is few, reduces reactivity, so that charcoal is avoided that excessive ablation occurs, led to the collapsing of microporous wall, and also overcomed
Specific pore structure should not be generated using pure gas activation and be difficult significantly to regulate and control the problem of ultramicropore structure.
(4) the aperture integrated distribution of active carbon prepared by the present invention belongs to ultramicropore between 0.45 ~ 0.55nm, compares table
Area reaches 840m2/ g or more, for microporosity up to 70% or more, the maximum adsorption capacity of hydrogen reaches 77cm3/ g or more.
(5) it is that raw material prepares uniform ultra micro mesoporous activated carbon that the present invention, which can also select industrial waste Ramsbottom carbon powder, itself
Possess microcellular structure abundant, there is high fixed carbon content height, specific resistance, chemical activity height, containing ash content is low, aluminium is low, sulphur is low, phosphorus
Low characteristic belongs to the carbon source with certain degree of graphitization.And Ramsbottom carbon powder is a kind of trade waste, is raw material system by it
Standby ultra micro mesoporous activated carbon, comprehensive utilization turn waste into wealth, realize the resource utilization of Ramsbottom carbon powder, solve active carbon preparation
Raw material problem, saved cost.
Therefore the present invention have production cost is low, alkali consumption is few, to equipment corrosion less, production process it is controllable and environmental-friendly
The features such as, the active carbon of preparation with uniform ultra-microporous, with large specific surface area and smaller mean pore sizes, narrow hole
It is distributed and is possessed the ability of good adsorbent hydrogen, can be applied to gas separation, especially suitable for using pressure swing adsorption from coal gas
Middle separation hydrogen.
Detailed description of the invention
Fig. 1 is the graph of pore diameter distribution of the uniform ultra micro mesoporous activated carbon for gas separation prepared by embodiment 1.
Fig. 2 is the N of the uniform ultra micro mesoporous activated carbon for gas separation prepared by embodiment 12Adsorption/desorption curve.
Fig. 3 is the TEM figure of the uniform ultra micro mesoporous activated carbon for gas separation prepared by embodiment 1.
Fig. 4 is the absorption etc. of the pressure-variable adsorption hydrogen of the uniform ultra micro mesoporous activated carbon for gas separation prepared by embodiment 1
Warm line chart.
Specific embodiment
The present invention is described further below with reference to embodiment, not limiting of its scope.
Embodiment 1
A kind of uniform ultra micro mesoporous activated carbon and preparation method thereof for gas separation, includes the following steps:
Step 1: raw material semi-coke is ground, 150 ~ 200 meshes are crossed, it is dry, Ramsbottom carbon powder is obtained, raw material semi-coke will be accounted for
The KOH of 15wt%, the assistant activator for accounting for raw material semi-coke 5wt% and water are mixed, and maceration extract is configured to, and wherein the quality of water is former
0.8 times of semi-coke of material；Normal temperature dipping in maceration extract is added in semi-coke again and for 24 hours, pre-feed is made；
Step 2: pre-feed made from step 1 is moved into tube furnace, in N2Control thermal decomposition is carried out under protective atmosphere,
Wherein N2The flow of protective atmosphere is 200 ~ 250ml/min；The control thermal decomposition is first by tube furnace with 4 ~ 6 DEG C/min
Heating rate is warming up to 370 DEG C, keeps the temperature 1 h, then be continuously heating to 900 DEG C with the heating rate of 4 ~ 6 DEG C/min, is passed through water,
The flow of middle water is 2ml/min, stops being passed through water after activating 1h, finally in N2It is cooled to room temperature under protective atmosphere, is made uniform
Ultramicropore activated carbon crude product；
Step 3: uniform ultramicropore activated carbon crude product made from step 2 is washed with 5% HCl solution, is filtered,
And uniform ultra micro mesoporous activated carbon is made then in 110 DEG C of 12 h of freeze-day with constant temperature with distilled water repeated flushing to neutrality；
As a result: the iodine sorption value of active carbon obtained by the present embodiment is 888.1mg/g, specific surface area 840.5m2/ g, micropore
Rate is 70.4%.Graph of pore diameter distribution and N2Adsorption/desorption curve is as shown in Figure 1, 2, and TEM schemes the suction as shown in figure 3, pressure-variable adsorption hydrogen
Attached isollaothermic chart is as shown in Figure 4.As Fig. 1,2 it is found that active carbon prepared by the invention based on ultramicropore, pore-size distribution collection
In, the channel of transport gas is provided with a small amount of mesoporous.
Embodiment 2
A kind of uniform ultra micro mesoporous activated carbon and preparation method thereof for gas separation, includes the following steps:
Step 1: industrial waste Ramsbottom carbon powder is ground, 150 ~ 200 meshes are crossed, it is dry, Ramsbottom carbon powder is obtained, raw material will be accounted for
The KOH of semi-coke 10wt%, the assistant activator for accounting for raw material semi-coke 10wt% and water are mixed, and are configured to maceration extract, wherein the matter of water
Amount is 1.2 times of raw material semi-coke；Normal temperature dipping 18h in maceration extract is added in semi-coke again, pre-feed is made；
Step 2: pre-feed made from step 1 is moved into tube furnace, in N2Control thermal decomposition is carried out under protective atmosphere,
Wherein N2The flow of protective atmosphere is 200ml/min；The control thermal decomposition is first by tube furnace with the heating of 4 ~ 6 DEG C/min
Rate is warming up to 350 DEG C, keep the temperature 1h, then be continuously heating to 950 DEG C with the heating rate of 4 ~ 6 DEG C/min, be passed through water, wherein water
Flow is 5ml/min, stops being passed through water after activating 0.5h, finally in N2It is cooled to room temperature under protective atmosphere, uniform ultra micro is made
Mesoporous activated carbon crude product；
Step 3: uniform ultramicropore activated carbon crude product made from step 2 is washed with 5% HCl solution, is filtered,
And uniform ultra micro mesoporous activated carbon is made then in 110 DEG C of 12 h of freeze-day with constant temperature with distilled water repeated flushing to neutrality；
The iodine sorption value of active carbon obtained by the present embodiment is 804.1mg/g, specific surface area 692.2m2/ g, microporosity are
64.2%。
Embodiment 3
A kind of uniform ultra micro mesoporous activated carbon and preparation method thereof for gas separation, includes the following steps:
Step 1: industrial waste Ramsbottom carbon powder is ground, 150 ~ 200 meshes are crossed, it is dry, Ramsbottom carbon powder is obtained, raw material will be accounted for
The KOH of semi-coke 5wt%, the assistant activator for accounting for raw material semi-coke 10wt% and water are mixed, and are configured to maceration extract, wherein the quality of water
It is 1.2 times of raw material semi-coke；Normal temperature dipping 12h in maceration extract is added in semi-coke again, pre-feed is made；
Step 2: pre-feed made from step 1 is moved into tube furnace, in N2Control thermal decomposition is carried out under protective atmosphere,
Wherein N2The flow of protective atmosphere is 300ml/min；The control thermal decomposition is first by tube furnace with the heating of 4 ~ 6 DEG C/min
Rate is warming up to 400 DEG C, keep the temperature 1h, then be continuously heating to 800 DEG C with the heating rate of 4 ~ 6 DEG C/min, be passed through water, wherein water
Flow is 1ml/min, stops being passed through water after activating 1h, finally in N2It is cooled to room temperature under protective atmosphere, uniform ultramicropore is made
Activated carbon crude product；
Step 3: uniform ultramicropore activated carbon crude product made from step 2 is washed with 5% HCl solution, is filtered,
And uniform ultra micro mesoporous activated carbon is made then in 110 DEG C of 12 h of freeze-day with constant temperature with distilled water repeated flushing to neutrality；
The iodine sorption value of active carbon obtained by the present embodiment is 754.1mg/g, specific surface area 619.2m2/ g, microporosity are
59.2%。
Claims (5)
1. a kind of preparation method of the uniform ultra micro mesoporous activated carbon for gas separation, which is characterized in that specifically according to the following steps
It completes:
Step 1: using semi-coke as raw material, first the KOH for accounting for 1 ~ 20wt% of raw material semi-coke, the activation for accounting for 1 ~ 12wt% of raw material semi-coke are helped
Agent and water are mixed, and maceration extract is configured to, and wherein the quality of water is 0.8 ~ 1.2 times of raw material semi-coke；Semi-coke is added again and is soaked
Pre-feed is made in 1 ~ 36h of normal temperature dipping in stain liquid；
Step 2: pre-feed made from step 1 is moved into tube furnace, in N2Control thermal decomposition is carried out under protective atmosphere, wherein
N2The flow of protective atmosphere is 150 ~ 300ml/min；The control thermal decomposition is first by tube furnace with the heating of 3 ~ 8 DEG C/min
Rate is warming up to 350 ~ 400 DEG C, keeps the temperature 0.5 ~ 1.5 h, then be continuously heating to 800 ~ 950 DEG C with the heating rate of 3 ~ 8 DEG C/min
Carry out part steam activation；The part steam activation is to introduce under the conditions of 800 ~ 950 DEG C of temperature into reaction tube
Water flow, wherein the flow of water is 1 ~ 5ml/min, water flow is closed after activating 0.5 ~ 1.5h, finally in N2It is cooled under protective atmosphere
Uniform ultramicropore activated carbon crude product is made in room temperature；
Step 3: being washed, being filtered to uniform ultramicropore activated carbon crude product made from step 2 with 5% HCl solution, it is used in combination
Distilled water washs repeatedly to neutrality and uniform ultra micro mesoporous activated carbon is made then in 110 DEG C of 12 h of freeze-day with constant temperature；
The aperture integrated distribution of the uniform ultra micro mesoporous activated carbon of the preparation belongs to ultramicropore, compares table between 0.45 ~ 0.55nm
Area reaches 840m2/ g or more, for microporosity up to 70% or more, hydrogen sorption capacity reaches 77cm3/ g or more.
2. the preparation method of the uniform ultra micro mesoporous activated carbon according to claim 1 for gas separation, which is characterized in that
The semi-coke raw material is that carbonization obtains under middle cryogenic conditions by the high-volatile bituminous coal of no cohesiveness or weakly caking
Relatively low volatile solid carbonaceous product.
3. the preparation method of the uniform ultra micro mesoporous activated carbon according to claim 1 for gas separation, which is characterized in that
The assistant activator is by 1 ~ 30% hydrogen peroxide, KNO3, 1 ~ 5wt% neopelex ethanol solution composition, in mass ratio
4:5:3 ratio is prepared.
4. the preparation method of the uniform ultra micro mesoporous activated carbon according to claim 1 for gas separation, which is characterized in that
The determination condition of the maximum adsorption capacity of the hydrogen is 25 DEG C, adsorptive pressure 11.4MPa.
5. a kind of uniform ultra micro mesoporous activated carbon for gas separation, which is characterized in that the uniform ultra micro mesoporous activated carbon is root
According to uniformly super prepared by preparation method of any one of the claim 1 ~ 4 for the uniform ultra micro mesoporous activated carbon of gas separation
Microporous activated carbon.
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