CN102560745A - Method for preparing activated carbon fiber material with specific surface area reaching 2500m<2>/g - Google Patents
Method for preparing activated carbon fiber material with specific surface area reaching 2500m<2>/g Download PDFInfo
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- CN102560745A CN102560745A CN2011104276854A CN201110427685A CN102560745A CN 102560745 A CN102560745 A CN 102560745A CN 2011104276854 A CN2011104276854 A CN 2011104276854A CN 201110427685 A CN201110427685 A CN 201110427685A CN 102560745 A CN102560745 A CN 102560745A
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Abstract
The invention relates to a method for preparing an activated carbon fiber material with a specific surface area reaching 2500m<2>/g. the activated carbon fiber material is prepared from a viscose raw material by process steps of anti-inflaming agent spraying treatment, pre-oxidation dehydration treatment, carbonizing treatment, and activating treatment, wherein the prepared activated carbon fiber material has a large amount of porous structures and high specific surface area reaching 2500m<2>/g, and a part of crystals of the material are graphitized. According to the method, the continuous production of the activated carbon fiber material is realized; the specific surface area of the products reaches 2500m<2>/g; the reaction device is convenient, practical, energy-saving, and efficient and is convenient to operate and control.
Description
Technical field
The invention belongs to activated carbon fiber material and make the field, particularly specific area reaches 2500m
2The preparation method of the activated carbon fiber material of/g.
Background technology
Develop rapidly along with human civilization advance and modern industrialization; The generation of a large amount of toxic gases, trade effluent, solid pollutant causes the pollution to the face of land and body of groundwater of extremely serious harm, particularly industrial refuse and blowdown water to existent environment of people; Make the original very freshwater resources of shortage receive severe contamination; A large amount of SO2 gas purgings cause large tracts of land acid rain, and farming and animal husbandry, forestry, building are caused and harm greatly.Excessive emissions CO2 gas causes greenhouse effects, causes glacier, the two poles of the earth to be dissolved; Sea level rise; Global climate is abominable, frequent natural calamity, and all these cause the very big attention of international community; National governments are all with the basic assurance of environmental protection as national sustainable development, and the input of environmental protection is increased year by year.According to statistics, the environmental protection market in the whole world in 1998 is 6,000 hundred million dollars, at present above 1,000,000,000,000 dollars.Toxic gas and industrial city sewage are two big " arch-criminals " that cause environmental pollution; At present toxic gas and simple, effective, the most cheap processing method of industrial city sewage are adopted the active carbon material absorption method exactly, we can say, active carbon has very important effect aspect the protection environment; Be that any other material is all irreplaceable; Simultaneously active carbon also industry and civilian aspect be widely used, Just because of this, the world market is in rising trend always to the demand of active carbon.
Activated carbon fiber (activated carbon fibre; ACF) be at the beginning of 60 generations of 20th century on the basis of high-performance carbon fibre; With carbon fiber after 250 ℃ of-500 ℃ of air pre-oxidation or not melting; Add under the inert gas shielding at 900 ℃ of left and right sides high temperature and to add activated media and developed ACF, 20th century the mid-1970s activated carbon fiber begin suitability for industrialized production in Japan.China realizes that suitability for industrialized production is after 1992.Before this, the material with carbon element that environmental protection and industrial circle are used successively occurred active carbon dust (PAC), grain active carbon (GAC) and with the active carbon particle hot melt stick to glass fibre or organic fiber on fibrous activated carbon (FAC).Different with traditional G AC, PAC, FAC, activated carbon fiber be by pitch fibers or organic fiber through carbonization, activation and obtain, it has highly developed microcellular structure; Pore-size distribution is narrow, and micropore directly is opened on fiber surface, and adsorption capacity is high; Inhale, desorption rate is fast, can conduct electricity, thermal coefficient of expansion is little; Corrosion-resistant, have absorption property and the adsorption dynamics adsorption kinetics property better to do than traditional active carbon.Product has shapes such as endless tow, staple fiber, fibrofelt, cloth, fabric, non-woven, fibrous paper, also can be mixed and made into various goods with other fibers such as fragrant acid amides, glass fibre, ceramic fibre, superabsorbent fiber and ion-exchange fibre etc., also can be made into the high functionality composite; The products made thereby moulding is better; Be difficult for efflorescence, under vibration, can not produce the loosening and too closely knit phenomenon of filling, because particular structure; Compare with traditional active carbon; Its adsorption capacity, absorption and desorption efficient have unrivaled superiority, and ACF also has electric conductivity preferably simultaneously, thereby can be used as electronics and electrode material; Along with the production technology of ACF and technology improve constantly and perfect; Properties of product will be further enhanced, and will have application prospects more in environmental protection and other field, and its economic and social benefit will be very considerable.
The maximum characteristics of activated carbon fiber are that adsorption capacity is big, heat-resisting, acid and alkali resistance.ACF is bigger several times to tens times than GAC to organic steam adsorbances such as gasoline, aldehydes, alcohols, phenols, alkene; Inorganic gas there is good adsorption capacity (like NO, NO2, SO2, H2S, HF, HCL etc.); Adsorbance to material in the aqueous solution (like dyestuff, phenol, COD, BOD, oil, volatile phenol, sulfide, iron ion, precious metal ion etc.) is more much higher than GAC, and it also has good adsorption capacity to microorganism, bacterium.Because ACF has the good adsorption ability; The bed of its 3 ~ 4 millimeters thick can be obtained similar effect with the GAC of 20 ~ 100 millimeters thick; The ACF not only adsorption capacity to the high concentration adsorbate is obvious, and is also excellent especially to the adsorption capacity of low concentration adsorbate, as: when toluene gas concentration low to 10ppm when following; ACF can also adsorb it; And GAC adsorbs must be higher than 100ppm the time soon, can be that the content of phenol in the phenol wastewater of 5 ~ 10ppm drops to 0 ~ 0.5ppm with concentration, is that at present known other adsorbent institute is inaccessiable.ACF has special pore structure, makes its absorption and desorption rate than fast many of GAC, PAC.ACF can reach balance in tens of seconds to several minutes to the absorption of gas, when absorption 10% toluene, and fast 4 times of ACF than GAC.When desorb, ACF only needs just desorb fully in 3 minutes, and GAC desorb soon, can reach balance to absorption a few minutes to the dozens of minutes of liquid.Absorption I2, ACF is tens seconds, and GAC is 104 ~ 105 seconds; Both differ 2 ~ 3 one magnitude, therefore available ACF absorption high wind speed contain the variable concentrations organic solvent industrial waste gas, be difficult in the absorption producing and leak suction phenomenon; Help the absorption of ACF single-column, be beneficial to the purified treatment of waste water.
Research work shows that ACF is an efficient physical adsorbent, and the size of its adsorption capacity and its specific area are proportional, in the market can continuous batch the activated carbon product specific area of preparation generally be lower than 2000m
2/ g, main cause is the TENSILE STRENGTH reduction rapidly along with the increase product of specific area, is broken through regular meeting, can't produce continuously; Another reason is that the activation temperature of activation furnace that will make the NACF of high-specific surface area is wanted more than 1100 degree, and common steel shell can subside by Yin Gaowen, so be higher than 2000m
2The continuous preparation of the activated carbon fiber material of/g is difficulty particularly.
Summary of the invention
The objective of the invention is to overcome the prior art defective, provide a kind of continuous specific area to reach 2500m
2/ g activated carbon fiber material preparation method.
The object of the invention is realized according to following proposal: a kind of specific area reaches 2500m
2The activated carbon fiber material preparation method of/g,
With the viscose raw material through fire-retardant reagent spray handle, pre-oxidation processed, carbonization and activation processing, form activated carbon fiber material, and the specific area of material reaches 2500m with a large amount of microcellular structures, part crystalline graphiteization
2/ g;
Said fire-retardant reagent spray handle be designed airtight atomized spray soak the prescription formula; Fibrous material is placed in the confined space; Adopt the mode of high-pressure fog evenly to be sprayed at phosphate solution in the viscose acetal fibre; Avoid the inhomogeneous of the liquid waste of solution soaking and content of dispersion that drum extrusion causes, dose is controlled at weight 4-12%;
Said pre-oxidation processed is to utilize low temperature, and general temperature is controlled at 200-300 ℃, and the time of staying is 20-30 minute in body of heater, and the reaction in this process is (NH
4)
3PO
4→ NH
3+ H
3PO
4; [C
6H
10O
5] n → C+H
2O;
The temperature of said carbonization-activation process is controlled at 1000-1200 ℃, and course of reaction is: C+O
2→ CO
2; C+O
2→ CO; C+H
2O → CO; C+H
2O → CO
2; C+CO
2→ CO, carbon is oxidized like this, forms nano aperture;
The key of above-mentioned reaction is the high temperature furnace structure of a kind of uniqueness of invention; Flue adopts thick heat-resistance stainless steel; And adopt T font reinforcement to prevent furnace deformation; The flue upper strata adopts outstanding the drawing of steel structure to prevent that high temperature from subsiding; Flue top is adopted and is covered the extremely light ceramic fiber blanket of one deck alleviating the pressure to flue, and heat insulation effect is fine;
More than the design purpose be to make furnace temperature can be elevated to 1100 ℃, but and long time continuous working, do not produce the stove phenomenon of collapsing; And the furnace insulation performance of this structure is good, and the thermal efficiency is the several times of common seat clay material;
Body of heater of the present invention adopts the automaton of segmentation ladder furnace temperature; The thermocouple sensor thermometric is adopted in temperature control; Carry out the setting and the control of temperature through the intelligent PID temperature control module, the Control for Kiln Temperature segmentation is independently carried out, and can realize that like this thermograde of furnace temperature is freely set and control;
Said activation temperature should be controlled at: entering the mouth is 400-600 ℃, exports to be 700-900 ℃, and the centre is 700-1100 ℃;
Said carbonization-activation technological reaction has been introduced water vapour as oxidant and air-isolation medium, and the mode of movement of the two-way water vapour of high-pressure multi-tube has been invented in design for this reason, arrives any corner of body of heater to guarantee steam, guarantees the even oxide etch of carbon; Water vapour evenly distributes from bottom to top and guarantees that also the viscose material is the activation of floating in activation process simultaneously;
Designed the technology of multipass activation simultaneously, the proportional relation of the specific area of fibrous material and the material soak time in body of heater, if but reduce fibrous material in body of heater hauling speed then can cause the material fracture, produce and be difficult to continuously.And the aperture structure of an activation is difficult to realize the nested structure in hole.
The present invention adopts the activating process of continuous multipass, and each micropore is nested in the last aperture, thereby improves the specific area of material rapidly.
The present invention has realized NACF serialization production, and the product specific area reaches 2500m
2/ g, reaction unit is simple and direct, practical, energy-conservation, efficient, and operation and control are convenient.
Description of drawings
Fig. 1 is the sketch map of the flue of body of heater of the present invention; Wherein, a-vertical view; The b-left view; The c-side view; 1-1: top; 1-2: bottom surface; 1-3: reinforcement; 1-4: suspension ring;
Fig. 2 is a refractory slab view of the present invention, wherein, and 2-1: groove;
Fig. 3 is the cutaway view of one jiao of body of heater overall structure of the present invention; Among the figure, the 3-1 flue; The 3-2 reinforcement; The 3-3 suspension ring; The 3-4 iron shelf; The 3-5 refractory slab; The 3-6 heating wire; The fire-resistant adobe kang platform of 3-7; 3-8 ceramic fibre felt rug; The 3-9 heating wire; The 3-10 ceramic fiber blanket; The 3-11 ceramic fibre is cotton; 3-12 refractory brick;
Fig. 4 is the body of heater temperature control point sensor location drawing of the present invention; Among the figure, the 4-1 flue is inner; 4-2 one warm area; 4-two warm areas; The 4-4 three-temperature-zone; The 4-5 four-temperature region; 4-6 five warm areas; 4-7 six warm areas; 4-8 seven warm areas; 4-9 eight warm areas;
Fig. 5 is a body of heater furnace temperature automatically controlled circuit diagram of the present invention; Among the figure, the 5-1PID temperature controller; 5-2 Power Regulation module; The 5-3 electric heater; The 5-4 temperature sensor;
Fig. 6 is that the medicine sketch map is soaked in body of heater spraying of the present invention; The 6-1 pharmacy jar; 6-2 adjustable constant-flow constant pressure valve; The 6-3 nozzle; The 6-4 spray tank; The former cloth of 6-5 (felt) unreels; The former cloth of 6-6 (felt) rolling;
Fig. 7 is body of heater water vapour pipeline figure of the present invention; The 7-1 flue is inner; The 7-2 air jet pipe; The 7-3 fumarole; 7-4 press water vapor line.
The specific embodiment
Below in conjunction with accompanying drawing the present invention is described in more detail:
Furnace binding: in advance with seat clay, brick good fire-resistant a heatable brick bed platform, prefabricated fire-resistant corrosion resistant plate flue as shown in Figure 1 and trough of belt refractory slab as shown in Figure 2; Earlier flue (Fig. 1) is positioned on the fire-resistant adobe kang; Under trough of belt refractory slab insertion flue; Then heating wire is penetrated in the groove of trough of belt refractory slab; Both sides and top with the cotton covering of ceramic fibre flue are attached to heating wire on the ceramic fiber blanket, carry out between the electrical equipment connection heating wire to separate with the ceramic fibre felt rug; Through iron shelf flue is sling, become hanging shape; Cover thick ceramic fiber blanket above again, puzzle with refractory brick on every side and get final product.
Temperature is controlled automatically: adopt the heating wire heating; Through the temperature sensor of eight sections warm areas, the temperature that detects each warm area is as shown in Figure 4, and transmits signals to the PID temperature controller; As requested, set the temperature parameter of each warm area respectively through the PID temperature controller, heating gradient is transferred to the Power Regulation module with signal, and the Power Regulation module is regulated power output according to instruction; Reach the purpose of the accurate temperature control of segmentation, make the activation temperature controllable process, like Fig. 5.
Medicine is soaked in spraying: the mode that medicine is soaked in spraying can be controlled the amount of dispenser, and uniformity consistency is good; Soup is dropped into pharmacy jar, utilize compressed air that soup is extruded nozzle, be sprayed on the former cloth (felt),, between nozzle and pharmacy jar, installed the adjustable constant-flow constant pressure valve additional for the dose that makes ejection does not change with liquid level and pressure oscillation.Nozzle is provided with two rows, and the nozzle location between arrange front-seat and back staggers, and guarantees the uniformity of dispenser, and rolling and the persevering moment damping controller of the device that unreels make the speed of passing through nozzle of former cloth (felt) even, as shown in Figure 6.
Unsteady activation: the 3kg high-pressure steam is sprayed by air jet pipe; Material is suspended on the steam, because many air jet pipe effects, and is uniformly distributed with the fumarole of these a plurality of Three-bearings on the air jet pipe; There is the position of the fumarole on adjacent two air jet pipes to stagger again; Along with at the uniform velocity passing through of material, make the effective and uniformity of activation process, as shown in Figure 7.
With the viscose raw material through fire-retardant reagent spray handle, pre-oxidation processed, carbonization and activation processing, form activated carbon fiber material, and the specific area of material reaches 2500m with a large amount of microcellular structures, part crystalline graphiteization
2/ g;
Fire-retardant reagent spray handle be designed airtight atomized spray soak the prescription formula; Fibrous material is placed in the confined space; Adopt the mode of high-pressure fog evenly to be sprayed at phosphate solution in the viscose acetal fibre; Avoid the inhomogeneous of the liquid waste of solution soaking and content of dispersion that drum extrusion causes, dose is controlled at 4-12% (Wt%); The pre-oxidation processed is to utilize low temperature, and general temperature is controlled at 200-300 ℃, and the time of staying is 20-30 minute in body of heater, and the reaction in this process is (NH
4)
3PO
4→ NH
3+ H
3PO
4; [C
6H
10O
5] n → C+H
2O; The temperature of carbonization-activation process is controlled at 1000-1200 ℃, and course of reaction is: C+O
2→ CO
2; C+O
2→ CO; C+H
2O → CO; C+H
2O → CO
2; C+CO
2→ CO, carbon is oxidized like this, forms nano aperture; The key of this reaction is the high temperature furnace structure of a kind of uniqueness of invention; Flue adopts the thick heat-resistance stainless steel of 10mm; And adopt T font reinforcement to prevent furnace deformation; The flue upper strata adopts outstanding the drawing of steel structure to prevent that high temperature from subsiding, and the flue top is adopted and covered the extremely light ceramic fiber blanket of one deck alleviating the pressure to flue, and heat insulation effect is fine; More than the design purpose be to make furnace temperature can be elevated to 1100 ℃, but and long time continuous working, do not produce the stove phenomenon of collapsing; And the furnace insulation performance of this structure is good, and the thermal efficiency is the several times of common seat clay material;
Body of heater of the present invention adopts the automaton of segmentation ladder furnace temperature; The thermocouple sensor thermometric is adopted in temperature control; Carry out the setting and the control of temperature through the intelligent PID temperature control module, the Control for Kiln Temperature segmentation is independently carried out, and can realize that like this thermograde of furnace temperature is freely set and control; Activation temperature should be controlled at: entering the mouth is 400-600 ℃, exports to be 700-900 ℃, and the centre is 700-1100 ℃; The carbonization-activation technological reaction has been introduced water vapour as oxidant and air-isolation medium, and the mode of movement of the two-way water vapour of high-pressure multi-tube has been invented in design for this reason, arrives any corner of body of heater to guarantee steam, guarantees the even oxide etch of carbon; Water vapour evenly distributes from bottom to top and guarantees that also the viscose material is the activation of floating in activation process simultaneously;
Designed the technology of multipass activation simultaneously, the proportional relation of the specific area of fibrous material and the material soak time in body of heater, if but reduce fibrous material in body of heater hauling speed then can cause the material fracture, produce and be difficult to continuously.And the aperture structure of an activation is difficult to realize the nested structure in hole.
The present invention adopts the activating process of continuous multipass, and each micropore is nested in the last aperture, thereby improves the specific area of material rapidly.
Claims (10)
1. a specific area reaches 2500m
2The preparation method of the activated carbon fiber material of/g; With the viscose raw material through fire-retardant reagent spray handle, pre-oxidation processed, carbonization and activation processing; Formation has the activated carbon fiber material of a large amount of microcellular structures, part crystalline graphiteization, and the specific area of material reaches 2500m
2/ g.
2. specific area according to claim 1 reaches 2500m
2The preparation method of the activated carbon fiber material of/g; It is characterized in that fire-retardant reagent spray handle adopt airtight atomized spray soak the prescription formula; Fibrous material is placed in the confined space; Adopt the mode of high-pressure fog that phosphate solution evenly is sprayed in the viscose acetal fibre, dose is controlled at weight ratio 4-12%.
3. specific area according to claim 1 reaches 2500m
2The preparation method of the activated carbon fiber material of/g is characterized in that the pre-oxidation processed is to utilize low temperature in closed furnace body, to carry out, and temperature is controlled at 200-300 ℃, and the time of staying is 20-30 minute in body of heater.
4. specific area according to claim 1 reaches 2500m
2The preparation method of the activated carbon fiber material of/g is characterized in that the temperature of carbonization, activation process is controlled at 1000-1200 ℃.
5. specific area according to claim 1 reaches 2500m
2The preparation method of the activated carbon fiber material of/g; The high temperature furnace structure that it is characterized in that the activation carbonization is: flue adopts heat-resistance stainless steel to make; Flue adopts T font reinforcement to prevent furnace deformation; Its upper strata adopts outstanding the drawing of steel structure to prevent that high temperature from subsiding, and the flue top covers one deck light ceramics fibrofelt alleviating the pressure to flue, and heat insulation effect is fine.
6. specific area according to claim 1 reaches 2500m
2The preparation method of the activated carbon fiber material of/g; It is characterized in that body of heater adopts segmentation ladder furnace temperature automaton; The thermocouple sensor thermometric is adopted in temperature control; Carry out the setting and the control of temperature through the intelligent PID temperature control module, the Control for Kiln Temperature segmentation is independently carried out, and realizes that the thermograde of furnace temperature is freely set and control.
7. specific area according to claim 1 reaches 2500m
2The preparation method of the activated carbon fiber material of/g is characterized in that the activation temperature inlet is 400-600 ℃, exports to be 700-900 ℃ of degree, and the centre is 700-1100 ℃.
8. specific area according to claim 1 reaches 2500m
2The preparation method of the activated carbon fiber material of/g; The technological reaction that it is characterized in that activation, carbonization has been introduced water vapour as oxidant and air-isolation medium; Adopt the mode of movement of the two-way water vapour of high-pressure multi-tube; To guarantee that steam arrives any corner of body of heater, guarantees the even oxide etch of carbon.
9. specific area according to claim 1 reaches 2500m
2The preparation method of the activated carbon fiber material of/g is characterized in that the water vapour of activation, carbonization evenly distributes from bottom to top, guarantees that the viscose material is the activation of floating in activation process.
10. specific area according to claim 1 reaches 2500m
2The preparation method of the activated carbon fiber material of/g is characterized in that the technology of the employing multipass activation of activation carbonization, and each micropore is nested in the last aperture, thereby improves the specific area of material rapidly.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103320904A (en) * | 2013-06-20 | 2013-09-25 | 中国科学院理化技术研究所 | Steam activation preparation method and preparation device of microporous activated carbon fibers |
| CN103521194A (en) * | 2013-08-30 | 2014-01-22 | 蚌埠德美过滤技术有限公司 | Surface polymer modified wood charcoal adsorbing agent and preparation method thereof |
| CN104567407A (en) * | 2015-01-06 | 2015-04-29 | 辽宁伊菲科技股份有限公司 | Heat preservation reinforcing technique for large horizontal atmosphere sintering furnace |
| CN104944424A (en) * | 2015-06-29 | 2015-09-30 | 宁夏宝塔石化科技实业发展有限公司 | Preparation method of activated carbon material with specific area of 2300 m<2>/g |
| CN105170181A (en) * | 2015-09-25 | 2015-12-23 | 天津工业大学 | Method for optimizing catalytic performance of carbon/titanium dioxide composite fiber membrane |
| CN105483361A (en) * | 2016-01-27 | 2016-04-13 | 中达电通股份有限公司 | Temperature control method in heat treatment technology |
| CN107262029A (en) * | 2017-06-14 | 2017-10-20 | 昆明理工大学 | A kind of high flame retardant carbon-supported catalyst and preparation method thereof |
| CN109082880A (en) * | 2018-07-05 | 2018-12-25 | 王伟霞 | Functional activity carbon fiber, preparation method and applications |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103320904A (en) * | 2013-06-20 | 2013-09-25 | 中国科学院理化技术研究所 | Steam activation preparation method and preparation device of microporous activated carbon fibers |
| CN103320904B (en) * | 2013-06-20 | 2015-03-18 | 中国科学院理化技术研究所 | Steam activation preparation method and preparation device of microporous activated carbon fibers |
| CN103521194A (en) * | 2013-08-30 | 2014-01-22 | 蚌埠德美过滤技术有限公司 | Surface polymer modified wood charcoal adsorbing agent and preparation method thereof |
| CN104567407A (en) * | 2015-01-06 | 2015-04-29 | 辽宁伊菲科技股份有限公司 | Heat preservation reinforcing technique for large horizontal atmosphere sintering furnace |
| CN104944424A (en) * | 2015-06-29 | 2015-09-30 | 宁夏宝塔石化科技实业发展有限公司 | Preparation method of activated carbon material with specific area of 2300 m<2>/g |
| CN105170181A (en) * | 2015-09-25 | 2015-12-23 | 天津工业大学 | Method for optimizing catalytic performance of carbon/titanium dioxide composite fiber membrane |
| CN105483361A (en) * | 2016-01-27 | 2016-04-13 | 中达电通股份有限公司 | Temperature control method in heat treatment technology |
| CN107262029A (en) * | 2017-06-14 | 2017-10-20 | 昆明理工大学 | A kind of high flame retardant carbon-supported catalyst and preparation method thereof |
| CN109082880A (en) * | 2018-07-05 | 2018-12-25 | 王伟霞 | Functional activity carbon fiber, preparation method and applications |
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