CN104118876A - Active coke used for flue gas desulfurization as well as preparation method and device of active coke - Google Patents
Active coke used for flue gas desulfurization as well as preparation method and device of active coke Download PDFInfo
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Abstract
The invention discloses an active coke used for flue gas desulfurization. The active coke is prepared by drying, grinding, molding, charring and activating through using raw coal with high metamorphic grade as a main raw material and adding raw coal with low metamorphic grade and coal tar. The active coke comprises the following raw material components by weight percent: 40-70% of raw coal with high metamorphic grade, 20-40% of raw coal with low metamorphic grade and 10-20% of coal tar, wherein dry basis volatile matter content of the raw coal with high metamorphic grade is 5-15%; ash content is 5-15%; the dry basis volatile matter content of the raw coal with high metamorphic grade is 35-45%; and the ash content is 6-20%. Blended coal of coal with high metamorphic grade and coal with low metamorphic grade are used as raw materials of the active coke, complementarity on aspects of raw material price, reactivity, coke preparation yield, and the like of the two coals is utilized, a proper mass ratio of the coal with high metamorphic grade to the coal with low metamorphic grade is (40-70):(20-40), the preparation cost of the active coke is reduced, the process time for carbonization and activation is shortened, and the yield of the active coke is improved.
Description
Technical field
The present invention relates to a kind of flue gas desulfurization activated coke and preparation method thereof and device, belong to material preparation and coal chemical technology.
Background technology
Activated coke desulfurization is the dry method flue gas purification techniques of the physics and chemistry absorption based on porous carbon, has that water loss is little, non-wastewater discharge, sulphur resource utilization reclaim, multiple pollutant is combined and the advantage such as removed.Activated coke desulfurization technology is selected China's arid area flue gases purification and alleviates China's sulphur resource serious unbalance present situation to have important practical significance.
Flue gas desulfurization has the SO that is beneficial to of more flourishing pore texture and some amount conventionally by activated coke
2absorption and the Surface chemical functional group of wood transforming.Coal is abundant, the cheap carbon-rich materials of a kind of reserves, has become main raw material prepared by activated coke.Conventionally, the coal of high metamorphic grade has higher carbon content as hard coal and meager coal, but volatile content and surface functional group are less, chemically reactive is poor, in activated coke preparation process, activated coke yield that high rank coal is produced is high, microvoid structure is flourishing, but needs preparation time long, and cost of material is higher; Low metamorphic grade coal as brown coal in contrast, carbon content is lower, fugitive constituent is high, surface functional group is abundant, chemically reactive is higher, good with activated media reactive behavior in activated coke preparation process, prepare required time shorter, and cost of material is cheap, but productive rate is on the low side and carbonization process in produce a large amount of tar difficulty and put.
At present flue gas desulfurization with the preparation of activated coke raw material used taking bituminous coal and brown coal as main, as Chinese patent " a kind of desulphurizing activated coke and preparation method thereof " (CN102745686A), a kind of method of preparing desulphurizing activated coke taking bituminous coal as raw material is disclosed, the feed coal that the method adopts is datong bitumite, compare hard coal, cheap, the reserves of raw materials used coal enrich.
Chinese patent " a kind of flue gas desulfurization of being prepared by brown coal activated coke and preparation method thereof " (CN101708840B), a kind of method of utilizing separately brown coal to prepare flue gas desulfurization activated coke is disclosed, the method is utilized low value-added brown coal, and the production cost of activated coke has reduced 30-50%.
The ubiquitous deficiency of preparation method of above-mentioned activated coke has: (1) carbonization process can produce a large amount of tar, is difficult to process; (2) productive rate of activated coke is on the low side; (3) system waste heat does not rationally utilize.
Summary of the invention
The object of this invention is to provide flue gas desulfurization activated coke and preparation method thereof and device that a kind of mixed coal taking high rank coal and low rank coal is prepared as raw material, reduce activated coke raw materials cost, reduce the priming reaction time, simultaneously recoverable tar and waste heat.
For achieving the above object, the present invention adopts following technical scheme:
A kind of flue gas desulfurization activated coke, taking high metamorphic grade raw coal as main raw material, allocates low metamorphic grade raw coal and coal tar into, after drying, abrasive dust, moulding, charing and activation, makes; Feed composition and proportioning are: high metamorphic grade raw coal 40-70%, low metamorphic grade raw coal 20-40%, coal tar 10-20%; Dry base volatile content in described high metamorphic grade raw coal is 5-15%, ash oontent 5-15%, and surplus is moisture and fixed carbon; Dry base volatile content 35-45% in described low metamorphic grade raw coal, ash oontent 6-20%, surplus is moisture and fixed carbon, above-described content is all in quality percentage composition.
Described high metamorphic grade raw coal is hard coal or meager coal, and low metamorphic grade raw coal is brown coal;
The present invention also provides the preparation method of this activated coke, comprises the following steps:
(1) low metamorphic grade raw coal is broken into the coal cinder that granularity is less than 5cm, the water content being dried in coal cinder is 10-15%;
(2) grind to form 100-300 object coal dust by high metamorphic grade raw coal with through step (1) low metamorphic grade raw coal after treatment;
(3) get by mass percentage the high metamorphic grade coal dust of 40-70% and the low metamorphic grade coal dust of 20-40%, and to add mass percent be the binding agent of 10-20%, mix, under the pressure of 20-80MPa, be squeezed into cylindrical pellet, particle diameter 5-10mm, length is 10-50mm;
(4) particle after moulding is carried out to charing and make carbonized material, carbonization temperature is 450-700 DEG C, temperature rise rate 5-15 DEG C/min, carbonization time 30-180min, charing atmosphere is nitrogen or rare gas element, after charing, flue gas obtains crude tar oil after condensation, and crude tar oil makes coal tar after dehydration, uses as the binding agent of step (3);
(5) activate to passing into activation gas in carbonized material, activation temperature 800-1000 DEG C, soak time 5-120min, is prepared into flue gas desulfurization activated coke.
In step (1), the desiccant thermal source of low metamorphic grade raw coal is hot flue gas and the micro-wave energy after step (5) activating process;
In step (1), first low metamorphic grade raw coal adopts hot flue gas after step (5) activating process as thermal source, is heated to 100 DEG C and keep 1-10min from room temperature; Then adopt hot flue gas and microwave combined heating.
In step (5), described activation gas is the mixed gas of water vapour and oxygen, and wherein oxygen volume content is 0-8%;
The device that flue gas desulfurization of the present invention is prepared by activated coke, comprises for the first crusher of broken low metamorphic grade raw coal with for the second crusher of the high metamorphic grade raw coal of fragmentation; The discharge end of described the first crusher is connected with drying machine, the top of described drying machine and be parallel on the drying machine both sides outer wall of feedstock direction and be equipped with microwave generator, the discharge end of drying machine be connected for the first pulverizing mill that grinds low metamorphic grade raw coal; The discharge end of described the second crusher be connected for the second pulverizing mill that grinds high metamorphic grade raw coal; The discharge end of described the first pulverizing mill and the second pulverizing mill is all connected with mixing and blending machine, described mixing and blending machine is connected with compacting shape machine, the discharge end of described compacting shape machine is connected with the feed end of charring furnace, the discharge end of described charring furnace respectively by pipeline and condenser for flue gas after condensation charing be connected for the activation furnace that activates carbonized material, the exit end of described condenser is connected with tar water eliminator, and the exit end of described tar water eliminator is connected with mixing and blending machine; The exit end of described activation furnace is connected with drying machine by pipeline.
Described drying machine is that belt transmits tunnel furnace or chain grate furnace or rotary kiln.
Described charring furnace is fixed bed or rotary kiln reactor.
Described activation furnace is fixed bed or rotary kiln reactor.
Beneficial effect of the present invention:
(1) the present invention adopts the coal blending of high rank coal and low metamorphic grade coal as activated coke raw materials, utilize the complementarity of these two kinds of coals at aspects such as cost of material, reactive behavior and coke yields processed, selecting the quality proportioning that high metamorphic grade raw coal and low metamorphic grade raw coal are suitable is (40-70): (20-40), reduce activated coke preparation cost, shorten charing and required process time of activation, improved the productive rate of activated coke.
(2) tar carbonization process being produced reclaims as the burnt binding agent of system and uses, and has solved coal tar and has disposed difficult problem.
(3) in reactivation process, being added in of appropriate oxygen (0-8%) avoided in the situation of the excessive ablation of carbon that uncontrollable combustion reactions causes, greatly shorten soak time, after activation, flue gas can be used for the dry of low metamorphic grade raw coal, has saved the energy.
Brief description of the drawings
Fig. 1 is the structure drawing of device of preparing by activated coke for flue gas desulfurization of the present invention;
Wherein, 1-the first crusher, 2-drying machine, 3-microwave generator, 4-the first coal pulverizer, 5-the second crusher, 6-the second coal pulverizer, 7-mixing and blending machine, 8-compacting shape machine, 9-charring furnace, 10-condenser, 11-tar water eliminator, 12-activation furnace.
Embodiment
The present invention is further illustrated in conjunction with the embodiments, should be noted that following explanation is only in order to explain the present invention, does not limit its content.
The high metamorphic grade coal adopting in embodiment is coal A and coal B, and low metamorphic grade coal is coal C and coal D, and wherein coal A is hard coal, and coal B is meager coal, and coal C and coal D are brown coal.The coal analysis result of these four kinds of raw coal is shown as table 1.
The technical analysis result of table 1. feed coal
Note: M
arfor moisture as received coal, A
dfor dry base ash content, V
dfor dry base fugitive constituent.
Embodiment 1
As shown in Figure 1, flue gas desulfurization is as follows by the concrete preparation process of activated coke: coal C is broken for to the coal cinder that particle diameter is less than 5cm through the first crusher 1, send into drying machine 2 inner dryings, the thermal source of Dryly use is heat of activation flue gas and micro-wave energy, microwave generator 3 is arranged on the top of drying machine 2 and is parallel on the drying machine both sides outer wall of feedstock direction, after coal C is dry, its moisture is reduced to 12%, and the coal cinder of coal C after dry is entered to the first coal pulverizer 4, and wearing into granularity is 200 object coal dusts; Coal A becomes through the second crusher 5 coal cinder that particle diameter is less than 5cm, then through the second coal pulverizer 6, wearing into granularity is 200 object coal dusts; Coal A, coal C and coal tar after abrasive dust mix in mixing agitator 7 according to the ratio of mass percent 65%, 20% and 15%, compound is in compacting shape machine 8, under the pressure of 60MPa, be squeezed into diameter 8mm, length is the particle of 15mm, then enter in charring furnace 9 and complete carbonization process, in carbonization process, pass into N
2550 DEG C of carbonization temperatures, 5 DEG C/min of temperature rise rate, carbonization time is 90min, charing flue gas is in pipeline is sent into condenser 10, charing flue gas after the condensation cleaning of footpath is discharged, and the crude tar oil that condensation obtains passes through tar water eliminator 11 again, obtains coal tar and sends in mixing agitator 7 as activated coke processed tamanori; Carbonized material enters in activation furnace 12 and activates, in reactivation process, in activation furnace, pass into activation gas, activation gas is water vapour and oxygen mixed gas, wherein oxygen volume content is 1%, 850 DEG C of activation temperatures, soak time 30min, obtains activated coke product, productive rate is 60%, produces heat of activation flue gas dry for coal C in pipeline is sent into drying machine 2.
Wherein, the drying means of coal C is: the hot flue gas that adopts activating process to produce can be used as thermal source, and dry for coal C is heated to 100 DEG C and keep 5 minutes by it from room temperature, adopt afterwards hot flue gas and microwave combined heating, it is 12% that coal C is dried to moisture content.The power of microwave heating determines according to coal C water content and drying treatment amount, according to being 0.5-1.5KW micro-wave energy/(kg dehydrating amount/h).
Drying machine 2 in the present embodiment is belt transmission tunnel furnace, and charring furnace 9 is fixed bed, and activation furnace 12 is rotary kiln reactor.
Embodiment 2
Coal D is broken for to the coal cinder that particle diameter is less than 5cm through the first crusher 1, send into drying machine 2 inner dryings, the thermal source of Dryly use is heat of activation flue gas and micro-wave energy, microwave generator 3 is arranged on the top of drying machine 2 and is parallel on the drying machine both sides outer wall of feedstock direction, after coal D is dry, its moisture is reduced to 14%, the coal cinder of coal D after dry is entered to the first coal pulverizer 4, and wearing into granularity is 250 object coal dusts, coal A becomes through the second crusher 5 coal cinder that particle diameter is less than 5cm, then through the second coal pulverizer 6, wearing into granularity is 250 object coal dusts, coal A after abrasive dust, coal D and coal tar are according to mass percent 50%, 30% and 20% ratio mixes in mixing agitator 7, compound is in compacting shape machine 8, under the pressure of 70MPa, be squeezed into diameter 9mm, length is the particle of 15mm, then enter in charring furnace 9 and complete carbonization process, in carbonization process, pass into helium, 600 DEG C of carbonization temperatures, 5 DEG C/min of temperature rise rate, carbonization time is 60min, charing flue gas is in pipeline is sent into condenser 10, charing flue gas after the condensation cleaning of footpath is discharged, the crude tar oil that condensation obtains passes through tar water eliminator 11 again, obtaining coal tar sends in mixing agitator 7 as activated coke processed tamanori, carbonized material enters in activation furnace 12 and activates, in reactivation process, in activation furnace, pass into activation gas, activation gas is water vapour, 900 DEG C of activation temperatures, soak time 120min, obtain activated coke product, productive rate is 55%, produces heat of activation flue gas dry for coal D in pipeline is sent into drying machine 2.
Wherein, the drying means of coal D is: the hot flue gas that adopts activating process to produce can be used as thermal source, and dry for coal D is heated to 100 DEG C and keep 10 minutes by it from room temperature, adopt afterwards hot flue gas and microwave combined heating, it is 14% that coal C is dried to moisture content.The power of microwave heating determines according to coal D water content and drying treatment amount, according to being 0.5-1.5KW micro-wave energy/(kg dehydrating amount/h).
Drying machine 2 in the present embodiment is chain grate furnace, and charring furnace 9 is rotary kiln reactor, and activation furnace 12 is fixed bed.
Embodiment 3
Coal C is broken for to the coal cinder that particle diameter is less than 5cm through the first crusher 1, send into drying machine 2 inner dryings, the thermal source of Dryly use is heat of activation flue gas and micro-wave energy, microwave generator 3 is arranged on the top of drying machine 2 and is parallel on the drying machine both sides outer wall of feedstock direction, after coal C is dry, its moisture is reduced to 12%, the coal cinder of coal C after dry is entered to the first coal pulverizer 4, and wearing into granularity is 200 object coal dusts, coal B becomes through the second crusher 5 coal cinder that particle diameter is less than 5cm, then through the second coal pulverizer 6, wearing into granularity is 200 object coal dusts, coal B after abrasive dust, coal C and coal tar are according to mass percent 45%, 35% and 20% ratio mixes in mixing agitator 7, compound is in compacting shape machine 8, under the pressure of 80MPa, be squeezed into diameter 10mm, length is the particle of 20mm, then enter in charring furnace 9 and complete carbonization process, in carbonization process, pass into nitrogen, 500 DEG C of carbonization temperatures, 8 DEG C/min of temperature rise rate, carbonization time is 120min, charing flue gas is in pipeline is sent into condenser 10, charing flue gas after the condensation cleaning of footpath is discharged, the crude tar oil that condensation obtains passes through tar water eliminator 11 again, obtaining coal tar sends in mixing agitator 7 as activated coke processed tamanori, carbonized material enters in activation furnace 12 and activates, in reactivation process, in activation furnace, pass into activation gas, activation gas is water vapour and oxygen, wherein oxygen volume content is 2%, 950 DEG C of activation temperatures, soak time 20min, obtains activated coke product, productive rate is 50%, produces heat of activation flue gas dry for coal C in pipeline is sent into drying machine 2.
Wherein, the drying means of coal C is with embodiment 1.
Drying machine 2 in the present embodiment is rotary kiln, and charring furnace 9 is rotary kiln reactor, and activation furnace 12 is fixed bed.
Embodiment 4
Coal D is broken for to the coal cinder that particle diameter is less than 5cm through the first crusher 1, send into drying machine 2 inner dryings, the thermal source of Dryly use is heat of activation flue gas and micro-wave energy, microwave generator 3 is arranged on the top of drying machine 2 and is parallel on the drying machine both sides outer wall of feedstock direction, after coal D is dry, its moisture is reduced to 14%, the coal cinder of coal D after dry is entered to the first coal pulverizer 4, and wearing into granularity is 300 object coal dusts, coal B becomes through the second crusher 5 coal cinder that particle diameter is less than 5cm, then through the second coal pulverizer 6, wearing into granularity is 300 object coal dusts, coal B after abrasive dust, coal D and coal tar are according to mass percent 70%, 20% and 10% ratio mixes in mixing agitator 7, compound is in compacting shape machine 8, under the pressure of 80MPa, be squeezed into diameter 5mm, length is the particle of 15mm, then enter in charring furnace 9 and complete carbonization process, in carbonization process, pass into nitrogen, 500 DEG C of carbonization temperatures, 5 DEG C/min of temperature rise rate, carbonization time is 150min, charing flue gas is in pipeline is sent into condenser 10, charing flue gas after the condensation cleaning of footpath is discharged, the crude tar oil that condensation obtains passes through tar water eliminator 11 again, obtaining coal tar sends in mixing agitator 7 as activated coke processed tamanori, carbonized material enters in activation furnace 12 and activates, in reactivation process, in activation furnace, pass into activation gas, activation gas is water vapour and oxygen mixed gas, wherein oxygen volume content is 5%, 800 DEG C of activation temperatures, soak time 10min, obtains activated coke product, productive rate is 52%, produces heat of activation flue gas dry for coal D in pipeline is sent into drying machine 2.
Wherein, the drying means of coal D is with embodiment 2.
Drying machine 2 in the present embodiment is rotary kiln, and charring furnace 9 is rotary kiln reactor, and activation furnace 12 is rotary kiln reactor.
Activated coke performance measurement:
Activated coke sample to the embodiment of the present invention 1 to 4 preparation carries out Performance Detection, and wherein Sulfur capacity adopts MT/T998-2006 standard, and other index all, taking GB/T7702.1-7702.22-1997 standard as according to carrying out the detection of correlated performance index, the results are shown in Table 2.
Table 2 activated coke the performance test results
| ? | Sulfur capacity mg/g | Bulk specific gravity | Iodine number mg/g | Ultimate compression strength N/cm 2 | Point of ignition DEG C |
| Embodiment 1 | 50.6 | 555 | 607 | 436 | 400 |
| Embodiment 2 | 45.7 | 503 | 524 | 440 | 405 |
| Embodiment 3 | 52.3 | 530 | 670 | 398 | 394 |
| Embodiment 4 | 59.2 | 570 | 735 | 478 | 435 |
As can be seen from Table 2: the features such as it is moderate that the activated coke for desulfuration of preparing by technical scheme of the present invention has bulk specific gravity, and ultimate compression strength is good, wear-resistant, and Sulfur capacity is high, good in oxidation resistance.
Claims (10)
1. a flue gas desulfurization activated coke, is characterized in that, taking high metamorphic grade raw coal as main raw material, allocates low metamorphic grade raw coal and coal tar into, after drying, abrasive dust, moulding, charing and activation, makes; Feed composition and proportioning are: high metamorphic grade raw coal 40-70%, low metamorphic grade raw coal 20-40%, coal tar 10-20%; Dry base volatile content in described high metamorphic grade raw coal is 5-15%, ash oontent 5-15%; Dry base volatile content 35-45% in described low metamorphic grade raw coal, ash oontent 6-20%, above-described content is all in quality percentage composition.
2. a kind of flue gas desulfurization activated coke as claimed in claim 1, is characterized in that, described high metamorphic grade raw coal is hard coal or meager coal, and low metamorphic grade raw coal is brown coal.
3. the preparation method of flue gas desulfurization use activated coke described in claim 1, is characterized in that, comprises the following steps:
(1) low metamorphic grade raw coal is broken into the coal cinder that granularity is less than 5cm, the water content being dried in coal cinder is 10-15%;
(2) grind to form 100-300 object coal dust by high metamorphic grade raw coal with through step (1) low metamorphic grade raw coal after treatment;
(3) get by mass percentage the high metamorphic grade coal dust of 40-70% and the low metamorphic grade coal dust of 20-40%, and to add mass percent be the binding agent of 10-20%, mix, under the pressure of 20-80MPa, be squeezed into cylindrical pellet, particle diameter 5-10mm, length is 10-50mm;
(4) particle after moulding is carried out to charing and make carbonized material, carbonization temperature is 450-700 DEG C, temperature rise rate 5-15 DEG C/min, carbonization time 30-180min, charing atmosphere is nitrogen or rare gas element, after charing, flue gas obtains crude tar oil after condensation, and crude tar oil makes coal tar after dehydration, uses as the binding agent of step (3);
(5) activate to passing into activation gas in carbonized material, activation temperature 800-1000 DEG C, soak time 5-120min, is prepared into flue gas desulfurization activated coke.
4. the preparation method of activated coke for flue gas desulfurization as claimed in claim 3, is characterized in that, in step (1), the desiccant thermal source of low metamorphic grade raw coal is hot flue gas and the micro-wave energy after step (5) activating process.
5. the preparation method of activated coke for flue gas desulfurization as claimed in claim 3, it is characterized in that, in step (1), first low metamorphic grade raw coal adopts hot flue gas after step (5) activating process as thermal source, is heated to 100 DEG C and keep 1-10min from room temperature; Then adopt hot flue gas and microwave combined heating.
6. the preparation method of activated coke for flue gas desulfurization as claimed in claim 3, is characterized in that, in step (5), described activation gas is the mixed gas of water vapour and oxygen, and wherein oxygen volume content is 0-8%.
7. the device by activated coke preparation method for flue gas desulfurization described in claim 3, is characterized in that, comprises for the first crusher of broken low metamorphic grade raw coal with for the second crusher of the high metamorphic grade raw coal of fragmentation; The discharge end of described the first crusher is connected with drying machine, the top of described drying machine and be parallel on the drying machine both sides outer wall of feedstock direction and be equipped with microwave generator, the discharge end of drying machine be connected for the first pulverizing mill that grinds low metamorphic grade raw coal; The discharge end of described the second crusher be connected for the second pulverizing mill that grinds high metamorphic grade raw coal; The discharge end of described the first pulverizing mill and the second pulverizing mill is all connected with mixing and blending machine, described mixing and blending machine is connected with compacting shape machine, the discharge end of described compacting shape machine is connected with the feed end of charring furnace, the discharge end of described charring furnace respectively by pipeline and condenser for flue gas after condensation charing be connected for the activation furnace that activates carbonized material, the exit end of described condenser is connected with tar water eliminator, and the exit end of described tar water eliminator is connected with mixing and blending machine; The exit end of described activation furnace is connected with drying machine by pipeline.
8. device as claimed in claim 7, is characterized in that, described drying machine is that belt transmits tunnel furnace or chain grate furnace or rotary kiln.
9. device as claimed in claim 7, is characterized in that, described charring furnace is fixed bed or rotary kiln reactor.
10. device as claimed in claim 7, is characterized in that, described activation furnace is fixed bed or rotary kiln reactor.
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| CN108927111A (en) * | 2018-08-08 | 2018-12-04 | 国家能源投资集团有限责任公司 | The device for making of powdered activated coke and the reparation technology of powdered activated coke |
| CN110791305A (en) * | 2019-11-11 | 2020-02-14 | 山东大学 | Method and system for preparing active coke by co-pyrolysis of biomass and coal |
| CN111924841A (en) * | 2020-07-17 | 2020-11-13 | 中冶南方都市环保工程技术股份有限公司 | Method for recycling active coke desulfurization and denitrification waste coke |
| CN112456489A (en) * | 2020-11-11 | 2021-03-09 | 中冶南方都市环保工程技术股份有限公司 | Preparation method of active coke |
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