CN109399631A - A method of preparing graphitization active carbon - Google Patents
A method of preparing graphitization active carbon Download PDFInfo
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- CN109399631A CN109399631A CN201811411242.4A CN201811411242A CN109399631A CN 109399631 A CN109399631 A CN 109399631A CN 201811411242 A CN201811411242 A CN 201811411242A CN 109399631 A CN109399631 A CN 109399631A
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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
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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
- C01B32/20—Graphite
- C01B32/205—Preparation
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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
The present invention provides a kind of methods for preparing graphitization active carbon; carbon raw material is fed in directly-heated type rotary kiln or directly-heated type shaft kiln under protective atmosphere; carbon raw material successively passes through preheating section, bringing-up section, temperature descending section, then discharges, and graphitization active carbon is prepared.In the bringing-up section; by power electrode in the bringing-up section the carbon raw material and/or its change resulting material (hereafter referred to collectively as material) direct-electrifying in the heating process; by the contact resistance fever heated material between the resistance or material particles or block of the material itself in bringing-up section, and the maximum temperature that the material passes through in directly-heated type rotary kiln or directly-heated type shaft kiln is not less than 800 DEG C.It is an advantage of the invention that the thermal efficiency is high, power consumption is low, good product consistency, process stabilizing, and production capacity is big.
Description
Technical field
The invention belongs to carbon material technical field, it is related to being graphitized the preparation method of active carbon.
Background technique
Active carbon have high specific surface area, flourishing pore structure, surface functional group enrich, have partially electronically conductive property etc. it is excellent
Property is widely used in catalyst preparation, water process, air pollution processing, mineral and the extraction of pharmaceuticals industry, battery, secondary electricity
Pond, super capacitor etc. field, application range are very extensive.
Application recently as active carbon in the fields such as electrode material of battery, secondary cell, super capacitor, to activity
The conduction needs of charcoal improve；It is suitable not only to need when additionally as catalyst carrier or catalyst, in the case where having
Specific surface area and the performances such as pore structure, also there is certain requirement to high temperature resistant, surface texture etc..These are required to activity
Charcoal carries out graphitization processing, to obtain the graphited absorbent charcoal material in part.
Be graphitized the raw material of active carbon, other than active carbon, can also be it is other can be carbonized and activate containing carbon materials
Material, source are very extensive.It can be inorganic carbon material, such as graphite, coal, coke, petroleum coke, carbon black etc.；It can be organic
Object, such as various synthesis high molecular materials and natural macromolecular material, various biological materials such as sugar, starch, cellulose, wood
Quality, protein, polypeptide, fruit stalk, waste etc..Because preparation graphitization active carbon requires heat to 900 DEG C
Even higher temperature when using the material of charcoal non activated as carbon raw material, can be carbonized and activate in passing during heating.
It is existing that active carbon graphitizing method is broadly divided into following three kinds.
Method one is to handle carbon material with graphitizing furnace.Since the graphitization temperature of carbon requires 2500 DEG C or so
Temperature can be generally graphitized with graphitizing furnace.Graphitization temperature is high, need graphited material or workpiece it is hanging or
Surrounding bears excessively high temperature to avoid furnace wall with the worse carbon material support of electric conductivity.Since graphite furnace temperature is high, heating
With cool down it is all slow, feed and withdraw from the time-consuming length of material, it is not easy to the degree of graphitization for controlling active carbon may cause excessively
It is graphitized and destroys completely the pore structure of active carbon.
Another method is that active carbon is heated to 1200 ~ 1900 DEG C, so that activated carbon section is graphitized.Part stone
Inkization is also exactly required by the electrode material of secondary cell, supercapacitor etc..But at such high temperatures, and
It needs to heat several hours under protective atmosphere, the general pushed bat kiln heated using carbon shirt-circuiting furnace and Si-Mo rod.Carbon shirt-circuiting furnace is added with electricity
Hot carbon pipe (and graphite material), then transfers heat to and is heated material, low output, and energy consumption is high.It is rarely used in large-scale industry
Production.Pushed bat kiln yield is not also high, takes up a large area, and power consumption is very high, and matched Elema Si-Mo rod graphite crucible etc. easily consumes
Part is also easily damaged, at high cost.
In order to avoid the defect of both the above method, existing active carbon graphite technology, generally using catalyzed graphitization
Method.First with the Immesion active carbons such as iron, cobalt, the salt of nickel or alkali metal, alkaline-earth metal or the precursor material of active carbon, so
Be heated to 800 ~ 1200 DEG C of even higher temperature afterwards and keep 1 to several hours, then pickling, washing remove metal or
Metal salt, process flow is long, and pollution is big.These metals or metal salt or alkali have these as graphited catalyst
The graphitization of catalyst, active carbon can carry out at a lower temperature.In addition, some graphitization activated carbon products, especially
When use as catalyst, supporting catalytic active composition is needed, some active ingredients can load to before graphitization
On the precursor material of active carbon or active carbon.
In conclusion even if the graphitization of active carbon is at least all in 900 DEG C or more of temperature using catalyzed graphitization technique
Lower progress, and protective atmosphere is needed, active carbon precursor is activated even if oxidizing atmosphere is added in graphitizing process,
Need to control oxidizing atmosphere additional proportion and flow.Requirement of such technique to equipment is harsher, protective atmosphere
It is required that external heat, high temperature requirement heat transfer efficiency is high, and catalyst may cause to corrode to the metal material of especially heating equipment.Mesh
It is preceding that there is no the methods of practical suitable large-scale industrial production graphitization active carbon.
Summary of the invention
The purpose of the present invention is to provide one kind, low energy consumption, equipment capacity is big, product quality consistency is good, technical process is steady
Fixed graphitization process for preparing activated carbon.By in directly-heated type rotary kiln or directly-heated type shaft kiln with power electrode to carbon raw material or
Its solid material (hereafter referred to collectively as material) direct-electrifying for generating during the reaction of person, by material itself resistance or
Contact resistance between feed particles or block generates heat and heated material under the action of electric current.
The object of the present invention is achieved like this:
A method of graphitization active carbon is prepared, carbon raw material is fed in reacting furnace and is heated, carbon raw material exists in heating process
Reaction generates graphitization active carbon in protective atmosphere, it is characterised in that:
The reacting furnace are as follows: there is burner hearth the electric heating rotary kiln of bringing-up section or shaft kiln (to call directly-heated type rotary kiln and straight in the following text
Hot type shaft kiln), wherein bringing-up section is provided with heating power supply electrode, applied on the material being heated by the electrode voltage to
To the material feed-in electric current being heated, the object being heated is heated using the resistance heating for the material being heated accumulated in bringing-up section
Material；
The heating process are as follows: in directly-heated type rotary kiln or in directly-heated type shaft kiln, the solid material successively passes through
Preheating, heating, cooling, then discharge；In the bringing-up section, by power electrode to the institute in the bringing-up section
The solid material stated and/or its change resulting material (hereafter referred to collectively as material) direct-electrifying in the heating process,
By in bringing-up section material itself resistance or material particles or block between contact resistance generate heat heated material,
And the maximum temperature that the material passes through in directly-heated type rotary kiln or directly-heated type shaft kiln is not less than 800 DEG C；
The air pressure of the protective atmosphere is less than or equal to 2MPa.
Further, the protective atmosphere are as follows: helium, nitrogen, argon gas, ammonia, hydrogen, air, oxygen, titanium dioxide
One of carbon, carbon monoxide or more than one mixture or the protective atmosphere are that the carbon raw material reacts life
At gas or vacuumize；
The carbon raw material are as follows: coal, carbon nanotube, graphene, graphite, carbon black, active carbon, coke, petroleum coke, pitch, biology
One of material, organic polymer, melamine, paraffin, sugar or more than one mixture；
Further, being 10~2000 volts to the voltage of the material direct-electrifying, electric current is 10~100000 amperes.
Further, the reacting furnace is the electric heating rotary kiln that Chinese patent CN103335513A is disclosed.
Further, being provided with preheating section before the bringing-up section of the reacting furnace and/or after the bringing-up section
It is provided with temperature descending section, material is preheated and/or is cooled down.
Further, one kind or more no more than 10 times of carbon molal quantity in carbon raw material is added in the carbon raw material
Kind inorganic compound.
Compared with the prior art, the invention has the following beneficial effects:
1) apply direct current or alternating voltage directly into material with electrode and be passed through electric current, material accumulation, which is got up, itself has one
Fixed resistance, the resistance generate heat under the function of current, eliminate diabatic process of the heat from heater element to material, avoid pair
Fire resisting material of furnace body and the nondistinctive heating of material, heat utilization ratio is high, and power consumption is low.And it avoids and is caused because of thermal transmission requirement
Make the limitation of material accumulation thinner thickness, furnace cavity utilization rate improves, and productivity improves, but also directly-heated type rotary kiln or straight
Hot type vertical kiln device can be done smaller.
2) it due to carrying out heating reaction by the way of to the heating of raw material direct-electrifying, avoids using Elema, silicon molybdenum
The resistance heating elements such as stick or molybdenum filament and crucible.Easy to operate, cost is relatively low.
3) when graphitizing process carries out in directly-heated type rotary kiln, material obtain it is lasting stir, further improve anti-
Heat and mass transfer process during answering, so that the reaction time is short, the thermal efficiency is high, and uniform in quality is stablized, and material is in directly-heated type
Traveling can be continuously moved inside rotary kiln and directly-heated type shaft kiln, be convenient for large-scale industrial production, good product consistency.
4) due in directly-heated type rotary kiln and having preheating section in directly-heated type shaft kiln, a heating section and a cooling section can pass through control
Revolving speed or discharging speed the control material of directly-heated type rotary kiln processed can be accurately controlled in the residence time of each temperature section
The degree of graphitization of active carbon.
Specific embodiment
Illustrate specific technical solution of the invention now in conjunction with embodiment.Following embodiment only illustrates skill of the invention
Art scheme reliable and effective can be realized, but technical solution of the invention is not limited in following embodiment.
Embodiment 1
By 1.0 tons of coal quality column-shaped active carbons, it is added in directly-heated type rotary kiln with the speed of 100kg/h.Directly-heated type rotary kiln is continuous
It rotates, piles with solid material between positive and negative electrode in directly-heated type rotary kiln, pass through the direct current of 1500A or friendship between positive and negative anodes
Galvanic electricity stream.Material successively passes through warming-up section (namely preheating section), the high temperature section (namely bringing-up section) between rotary kiln positive and negative electrode,
Temperature descending section discharging.Rotary kiln discharge end is passed through nitrogen, nitrogen flow 20Nm3/ h, reaction end gas are withdrawn from from rotary kiln feed end, object
Material is in rotary kiln internal stops 8h.1650 DEG C of high temperature section maximum temperature in rotary kiln.Products obtained therefrom is through X-ray powder diffraction point
Analysis has apparent graphite diffraction maximum.
Embodiment 2
The sawdust of 2% nickel nitrate is impregnated with by 1.0 tons to be added in directly-heated type shaft kiln with certain speed.Directly-heated type shaft kiln burner hearth is high
Spend 6m, burner hearth internal diameter 60cm.The both ends of burner hearth middle section 3m long are provided with positive and negative electrode, to the material feed-in in this section
The electric current of 1000A.For burner hearth bottom with the speed continuous discharge of 50kg/h, roof of the furnace is continuous or is intermittently added raw material to maintain
Material position.Material successively passes through warming-up section (namely preheating section), the high temperature section (namely bringing-up section) between rotary kiln positive and negative electrode, drop
Temperature section discharging.The discharge end of directly-heated type shaft kiln is passed through nitrogen, nitrogen flow 20Nm3/ h, reaction end gas is from the top of directly-heated type shaft kiln
It withdraws from, material is in kiln internal stops 8h.1000 DEG C of maximum temperature of directly-heated type shaft kiln bringing-up section.Products obtained therefrom spreads out through X-ray powder
Analysis is penetrated, there is apparent graphite diffraction maximum, BET tests specific surface area 877m2/g。
Claims (6)
1. a kind of method for preparing graphitization active carbon, carbon raw material is fed in reacting furnace and is heated, carbon raw material in heating process
Reaction generates graphitization active carbon in protective atmosphere, it is characterised in that:
The reacting furnace are as follows: there is burner hearth the electric heating rotary kiln of bringing-up section or shaft kiln (to call directly-heated type rotary kiln and straight in the following text
Hot type shaft kiln), wherein bringing-up section is provided with heating power supply electrode, applied on the material being heated by the electrode voltage to
To the material feed-in electric current being heated, the object being heated is heated using the resistance heating for the material being heated accumulated in bringing-up section
Material；
The heating process are as follows: in directly-heated type rotary kiln or in directly-heated type shaft kiln, the solid material successively passes through
Preheating, heating, cooling, then discharge；In the bringing-up section, by power electrode to the institute in the bringing-up section
The solid material stated and/or its change resulting material (hereafter referred to collectively as material) direct-electrifying in the heating process,
By in bringing-up section material itself resistance or material particles or block between contact resistance generate heat heated material,
And the maximum temperature that the material passes through in directly-heated type rotary kiln or directly-heated type shaft kiln is not less than 800 DEG C；
The air pressure of the protective atmosphere is less than or equal to 2MPa.
2. the method for preparation graphitization active carbon according to claim 1, it is characterised in that: the protective atmosphere are as follows: helium
One of gas, nitrogen, argon gas, ammonia, hydrogen, air, oxygen, carbon dioxide, carbon monoxide or more than one mixture,
Either the protective atmosphere is the gas or vacuumize that the carbon raw material reaction generates；
The carbon raw material are as follows: coal, carbon nanotube, graphene, graphite, carbon black, active carbon, coke, petroleum coke, pitch, biology
One of material, organic polymer, melamine, paraffin, sugar or more than one mixture.
3. the method for preparation graphitization active carbon as claimed in any of claims 1 to 2, it is characterised in that: to institute
The voltage for the material direct-electrifying stated is 10~2000 volts, and electric current is 10~100000 amperes.
4. the method for preparation graphitization active carbon as claimed in any of claims 1 to 3, it is characterised in that: described
Reacting furnace be Chinese patent CN103335513A disclose electric heating rotary kiln.
5. the method for preparation graphitization active carbon as claimed in any of claims 1 to 4, it is characterised in that: in institute
It is provided with preheating section before the bringing-up section for the reacting furnace stated and/or is provided with temperature descending section after the bringing-up section, material is carried out
Preheating and/or cooling.
6. the method for preparation graphitization active carbon as claimed in any of claims 1 to 5, it is characterised in that: in institute
In the carbon raw material stated, one or more inorganic compounds no more than 10 times of carbon molal quantity in carbon raw material are added.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201811411242.4A CN109399631A (en) | 2018-11-24 | 2018-11-24 | A method of preparing graphitization active carbon |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811411242.4A CN109399631A (en) | 2018-11-24 | 2018-11-24 | A method of preparing graphitization active carbon |
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| CN109399631A true CN109399631A (en) | 2019-03-01 |
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| CN201811411242.4A Pending CN109399631A (en) | 2018-11-24 | 2018-11-24 | A method of preparing graphitization active carbon |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113441110A (en) * | 2021-08-13 | 2021-09-28 | 成都中科普瑞净化设备有限公司 | Method for preparing adsorbent for adsorbing and separating carbon monoxide |
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2018
- 2018-11-24 CN CN201811411242.4A patent/CN109399631A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113441110A (en) * | 2021-08-13 | 2021-09-28 | 成都中科普瑞净化设备有限公司 | Method for preparing adsorbent for adsorbing and separating carbon monoxide |
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Application publication date: 20190301 |