CN101423213A - Method for preparing active carbon - Google Patents
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- CN101423213A CN101423213A CNA2007101667205A CN200710166720A CN101423213A CN 101423213 A CN101423213 A CN 101423213A CN A2007101667205 A CNA2007101667205 A CN A2007101667205A CN 200710166720 A CN200710166720 A CN 200710166720A CN 101423213 A CN101423213 A CN 101423213A
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Abstract
The invention provides a novel preparation method of active carbon, aiming at the defects that the existing chemical method used for active carbon production has severe pollution, high energy consumption, excessive sintering loss and little carbon yield; heavy metal remains in finished carbon products; the gas activation method has high requirement on the activation temperature; the temperature in the furnace is not easy to control; the non-uniform activation is caused; and active carbon (such as carbon molecule screen) which is provided with narrow hole distribution and has special application is difficult to prepare, and the like. The method is characterized in that a steam explosion principle is used to carry out low-temperature activation on the active carbonization material; the stream explosion is a process that the solid material is disposed by saturated stream or high-pressure gas for a certain time and then instantly reduced to normal pressure; the stream explosion temperature, pressure, and remaining time are adjusted to carry out the predisposal and the like to the carbonization material, thus gaining high-quality active carbon which has narrow hole distribution, large specific surface area and high carbon yield, and the active carbon with rich micro-pores and large specific surface area is prepared successfully by the semi-coke produced by an indirect-direct vertical furnace by nutlet carbonization material and Fugu coal of northern Shaanxi.
Description
Technical field
A kind of preparation method of active carbon, ownership carbon material sorbent material production field.
Background technology
Gac is a kind of artificial raw material of wood-charcoal material products with highly developed pore texture and very big internal surface area.It mainly is made up of carbon (87%～97%), also contains element and some inorganic minerals such as hydrogen, oxygen, sulphur, nitrogen.The notable attribute of gac is adsorption, and it can adsorb various materials from gas phase or liquid phase, and adsorptive power is very strong.Usually, the pore volume of gac reaches 0.2～1.0cm
2/ g, specific surface area is greater than 400～1000m
2/ g.Compare with the sorbent material (resin, silica gel, zeolite etc.) of other kinds, gac has many uniquenesses and irreplaceable characteristic, promptly highly developed pore texture and huge specific surface area; Contain (or can affix) multiple functional group (to increase active site) on the carbon surface; Has catalytic performance; Stable performance can be used in the environment of differing temps, different pH values, can regenerate.Therefore, the Application of Brand Active Carbon field constantly enlarges.From traditional food, medical decolouring, taste removal be used for smoke mask, to industrial large-scale application (making with extra care, reclaim and separating as solvent, in organic synthesis industry, do catalyzer and carrier, on the national defence science, be used for removing radioactive substance that the nuclear power facility emits etc.), over particularly past 20 years, gac has played important role aspect environment protection; Be used for polished feedwater and sewage disposal, purify air and remove the obnoxious flavour that production is discharged.Gac become produce with life with people closely link to each other, can not short material.The per capita gac demand of some developed countries of west aspect environmental protection reached 300～400g/ (year people).At present, gac year consumption in the whole world surpasses 700,000 t, and with annual 15% speed increase.
Almost any natural or synthetic carbonaceous material as synthesis of organic substance such as the coal of wood material (timber, fruit stone, shell), different metamorphic grade and resol, may be used to produce gac.
The production process of gac mainly comprises the charing and the activation of carbonaceous material.Carbonization process is with the pyrogenous process of carbon raw material secluding air, and reactivation process makes charcoal form the porous microlitic structure exactly, has huge specific surface area.The quality of gac and purposes greatly depend on the reactivation process of gac.
Since basic annals (1909) birth gac industry just beginning, process for preparing activated carbon and equipment just are divided into chemical activation and gas method activation two big classes.The various activation type of furnaces appear in the development surplus 80 year.Technology is ripe gradually, and novel process, new installation, product innovation continue to bring out.But the overwhelming majority still belongs to above-mentioned two major types.
1, chemical activation principle
Zinc chloride and other pharmaceutical chemicals activation method production process of active carbon are called for short chemical method.It is various carbon raw materials are mixed equably (or dipping) with pharmaceutical chemicals after, under suitable temperature, through processes such as charing, activation and recovery pharmaceutical chemicals, rinsing, drying, pulverizing, produces a kind of method of gac.External common chemical medicine has zinc chloride, phosphoric acid, potassium sulphide and rhombspar (CaCO
3MgCO
3), domestic mainly is zinc chloride process, discrete is also used the phosphoric acid method.
Zinc chloride process is directly made raw material with wood chip at home, and charing, activation procedure separate or finish (revolution oven process) together all can.During with zinc chloride process formulation type particle charcoal, plastic phase is finished extrusion molding before charing, and at this moment zinc chloride is not only made activator but also play binding agent.
About the activation of zinc chloride, also not fully aware of so far, it is generally acknowledged that zinc chloride has following effect.
The strong dehydration of zinc chloride makes wooden carbonization temperature significantly reduce (at 150～300 ℃), and changes the thermolysis process, has suppressed the generation of tar, and it is open to help hole, because of tar material can be stopped up hole.Zinc chloride (200 ℃) at a lower temperature can make the xylon swollen, and corrodes wooden inside until producing molten mixture---depolymerization, plasticizing process.Because ZnCI
2732 ℃ of boiling points, 263 ℃ of fusing points, thus under the temperature that essential charing finishes (450 ℃) it be still liquid the existence, do not hinder the rearrangement of carbon molecule, form carbon structure easily, and in charcoal uniform distribution, later on ZnCI
2Reclaim when extracting out, just form flourishing minute aperture.
Zinc chloride process charcoal yield is higher, generally reaches 40% (to the over dry raw material), and 80% carbon forwards gac to, and this is a big characteristic of zinc chloride process.Another characteristic is by regulating the zinc chloride consumption, regulate the pore texture of the gac that produces, as to produce the sugared ratio that solid is considered to be worth doing with solid zinc during with charcoal be that 1:1.6～ratio is adjusted to 1:1.1～1.3, i.e. ZnCl when 2. producing Medicinal Charcoal
2When consumption was big, the aperture was to increasing the change of (it is many to cross Chinese hole) direction.
Simultaneously zinc chloride process has seriously polluted (atmosphere and water body), has heavy-metal residual to influence two big drawbacks such as finished product purposes, uses the producer of this method that the trend of minimizing is arranged.
2, gas method activation principle
It is earlier the charing of carbon containing organic raw material that the gas activation method is produced gac, allows gas activation agent---water vapor, CO then
2, O
2(air) etc. carries out activatory by red-hot charcoal layer and with charcoal generation priming reaction.Activated material is washed refining through sour water, dry back grinding promptly makes powdery carbon.The harder charcoal of the general employing of amorphous pellets charcoal is broken into certain particle size activation back and makes with extra care and get.Typing particle charcoal is that powdered carbon is worn into the extrusion molding of fine powder adding additives, gets through charcoal, activation and whole grain again.
Studies show that, formed the blank of gac microlitic structure during the raw material charing, it is the basic microlitic structure of similar graphite, leave the space between the crystallite, at this moment, because the separating out and decompose of tar material, these spaces are occupied or are stopped up by disorderly " amorphous " charcoal, and the adsorptive capacity of carbonized material is very little as a result.When carrying out (gas method) activation, materials such as the tar in the space at first are removed with disorderly charcoal, have opened the hole of original obturation.At this moment come out in basic crystallite surface, and with the activator effect, take place to burn and lose.It is uneven that crystallite burns mistake, burn the stall degree big with the parallel direction ratio vertical direction of charcoal layer, on the corner and defective locational carbon atom be that carbon on the active site is bigger with the speed of gas reaction, this uneven burning of crystallite is lost the appearance that just causes new hole.In reactivation process subsequently, hole is constantly widened, and the wall between the adjacent micropore is burnt fully and forms bigger hole, causes transitional pore and macropore volumetrical to increase.In a word, these three kinds of processes commonly used are explained the activating mechanism that produces hole in the reactivation process:
(1) opening in original inaccessible hole;
(2) expansion of pre-existent pore, hole wall is burnt mistake;
(3) some structure produces new hole through the selectivity activation.
The generation of hole and the degree of oxidation of charcoal have confidential relation, and the oxidation of charcoal must consume charcoal.Therefore. loss on ignition commonly used is weighed the activation degree of charcoal, regulates the pore texture of gac, and this is a big characteristic of gas activation method.According to the peaceful viewpoint of Doby, burn the mistake rate less than 50% o'clock, what obtain is the micropore gac; Burn the mistake rate greater than 75% o'clock, what obtain is big mesoporous activated carbon; Burn the mistake rate at 50%～75% o'clock, gac has mixed structure.The yield of gas activation method charcoal is lower, but finished product is purer.
On producing, adopt oxygen-containing gass such as water vapor, stack gas, air, activate with the carbon reaction as activator:
1. steam activation
Carbon with the reaction of water vapor is;
C+H
2O→H
2+CO-131kJ
With the water-gas reaction of carbon gasification, this priming reaction is thermo-negative reaction a---cooling effect, should give heat by the outside, so use superheated vapour more.Heat is reclaimed in flammable reactant gases (water-gas) burning that produces, can the balance heat supply.
Steam activation slowly, steadily can obtain fine activated carbon, adopts at most on producing.
Steam activation is at isolated oxygen, finishes under 750～950 ℃ condition.Oxygen can make carbon surface burn and lose, and reduces the product yield of charcoal, so should reduce entrained air oxygen as far as possible.
2. air (oxygen) activation
Carbon with oxygen reaction is:
C+O
2→ CO
2+ 386.2kJ (below 600 ℃)
2C+O
2→2CO+225.6kJ(800～900℃)
These two reactions are thermopositive reaction, can carry out two kinds of product C O and CO at a lower temperature
2Ratio increasing and increase with temperature.
Because a large amount of heats are emitted in reaction.Normal temps in the wayward stove especially is not easy to avoid local superheating and causes inhomogeneous activation, burns and loses too much, does not generally use separately, is everlasting and infiltrates an amount of water vapor in air-activated dose, utilizes the heat-absorbing action of water-gas reaction to control material layer temperature.
3. stack gas (CO
2) activation
Carbon with the reaction of carbonic acid gas is:
C+CO
2→2CO-170.5kJ(850～1100℃)
This reaction also is thermo-negative reaction, and is more taller than steam activation temperature, generally also do not use separately, often mixes mixed gass such as an amount of air and water vapor and usefulness.
As mentioned above, during with water vapor and Air mixing gas activation, if blending ratio is suitable, can make the relevant weighing apparatus of thermo-negative reaction and thermopositive reaction, make activation temperature stable, activation evenly.In addition, the somebody thinks that the raw material charcoal has various active site, the active site that has be easy to same steam reaction, have be easy to same CO
2The mixed gas activation is adopted in reaction, and the adsorptive power that improves active carbon finished products is good.
The segmentation of employing activation method is also arranged, promptly under 800 ℃, carry out the short period of time activation with water vapor earlier, use air 500～600 ℃ of further activation down then, or use water vapor earlier, then with the stack gas activation, to improve decolorizing ability 800 ℃ of activation.
In order to make structure of activated carbon, chemical structure and absorption property adapt to different industrial uses, promptly possess different adsorption selectivities, multiple manufacture method is arranged.The gas activation method of China's employing at present has 10 unnecessary kinds.Mainly according to classification such as activated gas, the type of furnace, priming reaction beds, as smoldering stove stack gas activation method, saddle stove steam activation method.In addition, also have multitube fluidizing furnace, outer overflow type fluidizing furnace, swirl spouting activation furnace, flint road kiln activation furnace, ramp type activation furnace, venetian blind type activation furnace, mechanical raking activation furnace etc.Activation furnace forward thin layer, reinforcement activation direction develop at present.
In sum, the gac activation method is the gordian technique of decision quality of activated carbon, and different activation methods has the different characteristics and the scope of application.Chemical activation such as zinc chloride process have seriously polluted (atmosphere and water body), have heavy-metal residual to influence two big drawbacks such as finished product purposes in the charcoal finished product, day by day reduce in the world at present and adopt.Gas activation method activation temperature is had relatively high expectations, steam activation is at isolated oxygen, under 750～950 ℃ condition, finish, it is strong endothermic reaction, must the outside infeed overheated steam and keep high temperature, some factories often feed a certain amount of air and burn the part charcoal and keep activation temperature, and it is higher to consume energy, cause to burn and lose too much, the charcoal yield is few.Temperature is wayward in the stove, especially is not easy to avoid local superheating and causes inhomogeneous activation, particularly is not easy to control the gac such as the carbon molecular sieve that obtain the narrower special purpose of pore distribution.
Patent characteristic
According to above-mentioned situation, we invent a kind of novel absorbent charcoal preparation method, it is characterized in that adopting the quick-fried principle of vapour that the gac carbonized material is carried out low-temperature activation, regulate the quick-fried temperature of vapour, pressure and carbonized material is carried out pre-treatment etc., thereby obtain the high quality active carbon of the different purposes that pore distribution is narrow, specific surface area big, the charcoal yield is high.
The quick-fried process of vapour is steam explosion (steam explosion) process, and it is with solid materials, and moment was reduced to non-pressurized process after particularly lignocellulosic material was handled certain hour with saturation steam or high pressure gas.Nineteen twenty-eight, the W.H.Mason of the U.S. has at first invented the steam explosion technology, and this technology used the saturated steam of 7～8MPa to carry out steam explosion as medium at that time, was used for the research of fiberboard preparation.
The steam explosion technology starts from nineteen twenty-six the earliest, is interrupter method production at that time, mainly is to be used to produce beaver board.Since the seventies in 20th century, this technology also is widely used in the production of animal-feed and extracts ethanol and speciality chemical from lumber fibre.After the eighties, this technology has very big development, and the use field also progressively enlarges, and continuous steam explosion method production technology and equipment have occurred, the continuous steam explosion method Processes and apparatus of promptly Canadian StakeTechnology company exploitation, and produce many patents.The later stage eighties, Stake Technology company is applied to the pulping and paper-making field with this technology, it and the joint research of Quebec, CAN university, at first a large amount of steam explosion tests has been carried out to many non-wood fibrous raw materials in poplar, back, obtained good effect.On this basis, developed steam explosion pulping technique and equipment, and be used to produce the animal-feed technical elements at pulping waste liquor deep research is also arranged.
At home, the investigator also began the steam explosion technology is studied in the eighties in 20th century, and was applied to fields such as slurrying, feed, starter, lignocellulosic material pre-treatment.The Zhan Huaiyu of South China Science ﹠ Engineering University, yellow doing strong etc. are adopted the slurrying of steam explosion technology to poplar, bagasse, mao bamboon respectively.The Lai Wenheng of Beijing Forestry University, Pan Ding as etc. the steam explosions of 3 kinds of fast setation white poplars, birch, Pinus massoniana Lamb, wheat straw etc. handled done research, and inquired into the principal element that influences quick-fried broken power.The Chen Hongzhang of Chinese Academy Of Sciences Process Engineering Research Institute, Li Zuohu etc. have then done research to the processing of the steam explosions of wheat straw, hemp, herbal medicine, tobacco etc., have analyzed and inquired into broken process and the principle of steam explosion.Also the degumming effect of the performance that steam exploded wheat straw is starched, hemp, Chinese medicine extraction ratio of effective constituents etc. are studied.It is the feedstock production xylo-oligosaccharide with the stalk that Chen Hongzhang etc. also utilize the steam explosion technology, and applies for multinomial related invention patent.The big vast maple of Nanjing Forestry University, Dan Gu etc. have also done trial in this respect.Zhejiang is shouldered the Chen Yu of university and is then utilized steam explosion technical finesse wheat straw to be applied to the manufacturing of microbiological degradation and non-glue fibre board as, Ouyang Pingkai of Nanjing University of Chemical Technology etc.The research that the Shao Ziqiang of Beijing Institute of Technology adopts steam explosion technical finesse pure cellulose to be used to improve the chemical reaction performance.
The steam explosion technology is used for gac activation does not appear in the newspapers, and we are used for the carbonized material activation of process for preparing active carbon with this technology, and have carried out preliminary study, and succeed, and makes successfully that micropore is abundant, the big (2000m of specific surface area
2/ g) gac.
As previously mentioned, formed the blank of gac microlitic structure during the raw material charing, it is the basic microlitic structure of similar graphite, leave the space between the crystallite, at this moment, because the separating out and decompose of tar material, these spaces are occupied or are stopped up by disorderly " amorphous " charcoal, and the adsorptive capacity of carbonized material is very little as a result.
When carrying out the quick-fried activation of vapour, at first carbonized material is carried out the steam pressurising, under certain temperature, pressure condition, steam has been full of in the hole of carbonized material, stop certain hour, steam carries out swelling and ramollescence to tar in the hole etc., treats unexpected decompression, and the energy dispose procedure of physics is finished in steam and carbonized material acting in conjunction.Vapour phase medium ejection moment rapid expansion in the carbonized material, high temperature liquid water in the carbonized material and the rapid bumping of remollescent tar form flash distillation simultaneously, utilize vapour phase saturation steam and high temperature liquid water or the acting in conjunction of tar two media, the adiabatic expansion process that moment finishes, externally acting is gone out the tamper in the carbonized material hole, the hole is enlarged, voidage increases, and specific surface area increases, and has realized the activation of carbonized material.
The quick-fried reactivation process of vapour is divided into two stages, at first is vapor phase pulping, and high pressure steam is penetrated into the hole in the carbonized material, and, tamper coal-tar middle oil to the carbonized material hole and hole wall carry out swelling with softening, even carry out gasification reaction.Next is quick-fried broken process, utilize the multiple medium acting in conjunction of vapour phase saturation steam, high temperature liquid water, tar and gasification reactant in carbonized material, the adiabatic expansion process that moment finishes, externally acting, tamper in the carbonized material hole is gone out, and the hole is enlarged, and voidage increases, specific surface area increases, and has realized the activation of carbonized material.
Can think, have in steam explosion reactivation process that thermosol expands, effects such as gasification and mechanical breaking.
(1) during thermosol expanded effect steam explosion process, hot high pressure steam entered in the carbonized material, and infiltrates the hole of carbonized material inside.Because the combined action of water vapour and heat makes the softening swelling of lower-molecular substance in the carbonized material hole.
(2) reaction of water vapour and carbon takes place in pneumatolysis when temperature is higher, and the duct is enlarged.
When (3) mechanical breaking acts on high pressure steam release, the hot steam molecule that has infiltrated hole inside in the mode of air-flow from coming out than the high speed abrupt release of blind hole crack, hole inner and around high speed moment of hot steam flow, make carbonized material generation mechanical breaking to a certain extent, the blind hole road is opened, and pore is enlarged.Simultaneously also can produce new crack.
By carbonized material is carried out pre-treatment, as broken, alkali lye impregnating, the steam regulation temperature and pressure, the residence time, release speed can effectively be controlled the hole size and the pore distribution of gac, realizes the directed gac of producing different purposes.
Patent example 1
Employing is through the fruit stone carbonized material of the tube furnace charing (800 ℃) of indirect heating, will be after screening, fragmentation less than the carbonized material adding steam explosion container of 3mm greater than 1mm, encloses container carries out steam pressurising (2.5MPa), open a plurality of steam escape valves on the steam explosion container behind the stop certain hour (10 minutes) simultaneously, the steam explosion container is reduced pressure suddenly, vapour phase medium ejection moment rapid expansion in the carbonized material, gas and solid materials pour holding tank and carry out the inertia gas solid separation, obtain high-specific surface area (3000m after the cyclone dust removal
2/ g) indefinite form gac.
Patent example 2
Adopt Fugu, northern Shensi coal through between-semicoke that straight Hybrid Heating upright furnace is produced, will be after screening, fragmentation less than the carbonized material adding steam explosion container of 6mm greater than 3mm, encloses container carries out steam pressurising (2.5MPa), open a plurality of steam escape valves on the steam explosion container behind the stop certain hour (10 minutes) simultaneously, the steam explosion container is reduced pressure suddenly, vapour phase medium ejection moment rapid expansion in the carbonized material, gas and solid materials pour holding tank and carry out the inertia gas solid separation, obtain high-specific surface area (2200m after the cyclone dust removal
2/ g) indefinite form gac.
Claims (5)
1. preparation method of active carbon, it is characterized in that the carbonized material that utilizes prior art to produce adopts the quick-fried technology of vapour, moment was reduced to non-pressurized process after soon the solid carbonized material was handled certain hour with saturation steam or high pressure gas, the gac carbonized material is carried out low-temperature activation, the gac that the preparation micropore is abundant, specific surface area is bigger.
2. the described carbonized material of claim 1 comprises the carbonized material of wooden, ature of coal, macromolecular material and the preparation of all carbon raw materials.
3. the quick-fried technology of the described vapour of claim 1 comprises interval type and the quick-fried process of continous way vapour.
4. the described carbonized material of claim 1 can pass through processing such as fragmentation, screening, steeping liq and promotes the quick-fried activation effect of vapour.
5. the described gac of claim 1 comprises different purposes, difform gac and carbonaceous molecular sieve.
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|---|---|---|---|
| CNA2007101667205A CN101423213A (en) | 2007-10-30 | 2007-10-30 | Method for preparing active carbon |
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|---|---|---|---|
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| CN106629712A (en) * | 2016-12-30 | 2017-05-10 | 中南大学 | Method for preparing activated carbon from mixture of coal and biomass |
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|---|---|---|---|---|
| CN102872794A (en) * | 2012-09-04 | 2013-01-16 | 常州大学 | Composite adsorption material for removing bromate from water and preparation method for adsorption material |
| CN103665961A (en) * | 2013-12-16 | 2014-03-26 | 山东源根石油化工有限公司 | Preparation method of modified nanometer titanium dioxide through steam explosion and coating |
| CN103665961B (en) * | 2013-12-16 | 2015-06-03 | 山东源根石油化工有限公司 | Preparation method of modified nanometer titanium dioxide through steam explosion and coating |
| CN104445184A (en) * | 2014-12-08 | 2015-03-25 | 柳州东侯生物能源科技有限公司 | Recycling method of nutshells |
| CN104445184B (en) * | 2014-12-08 | 2017-01-11 | 柳州东侯生物能源科技有限公司 | Recycling method of nutshells |
| CN107572518A (en) * | 2016-07-04 | 2018-01-12 | 现代自动车株式会社 | Method for preparing activated carbon |
| CN107572518B (en) * | 2016-07-04 | 2021-07-13 | 现代自动车株式会社 | Method for producing activated carbon |
| CN106517188A (en) * | 2016-11-04 | 2017-03-22 | 江苏竹溪活性炭有限公司 | Preparing method for coal-based active carbon for controlling environmental protection and control |
| CN106517188B (en) * | 2016-11-04 | 2019-02-19 | 江苏竹溪活性炭有限公司 | Environment protection treating active carbon from coal preparation method |
| CN106629712B (en) * | 2016-12-30 | 2019-03-15 | 中南大学 | A method of active carbon is prepared using the mixture of coal and biomass |
| CN106629712A (en) * | 2016-12-30 | 2017-05-10 | 中南大学 | Method for preparing activated carbon from mixture of coal and biomass |
| CN106672965A (en) * | 2017-01-05 | 2017-05-17 | 新疆弘瑞达纤维有限公司 | Method for preparing high-surface-area multi-stage porous carbon with cotton straws |
| CN108658581A (en) * | 2018-06-29 | 2018-10-16 | 界首市东城群海彩陶工作室 | A kind of preparation method of ancient painted pottery pug |
| CN110734059A (en) * | 2018-07-19 | 2020-01-31 | 深圳市环球绿地新材料有限公司 | kinds of activated carbon with low specific surface area, its preparation method and application |
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| CN111333070A (en) * | 2020-03-10 | 2020-06-26 | 天津科技大学 | Method for utilizing all components of sunflower disc raw material |
| CN111333070B (en) * | 2020-03-10 | 2022-09-16 | 天津科技大学 | Method for utilizing whole components of sunflower disc raw material |
| CN111943194A (en) * | 2020-08-18 | 2020-11-17 | 湖州民强炭业有限公司 | Preparation method of coconut shell carbon molecular sieve for methane purification |
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