CN106698423A - Method of preparing active coke for desulfurization and denitrification of sintering flue gas by using semi-coke - Google Patents
Method of preparing active coke for desulfurization and denitrification of sintering flue gas by using semi-coke Download PDFInfo
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- CN106698423A CN106698423A CN201710072133.3A CN201710072133A CN106698423A CN 106698423 A CN106698423 A CN 106698423A CN 201710072133 A CN201710072133 A CN 201710072133A CN 106698423 A CN106698423 A CN 106698423A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention discloses a method of preparing active coke for desulfurization and denitrification of sintering flue gas by using semi-coke and belongs to the technical field of energy conservation and emission reduction of sintering production of blast furnace ironmaking. The method can be used for solving the problem that an adsorbent for dry method desulfurization and denitrification of sintering flue gas is high, and meanwhile, the method is capable of expanding the available path of excessive industrial semi-coke. The method disclosed by the invention comprises the following steps: desorbing absorbed water for a selected semi-coke sample, the size fraction of which is less than 5mm; then finely grinding the sample to be smaller than 0.074mm; mixing high-temperature coal tar as an adhesive with the semi-coke sample; and obtaining active coke meeting the desulfurization and denitrification performances (compression strength and removal rate) of the sintering flue gas by virtue of kneading forming, carbonizing and activating. The method is simple in process and low in cost, and the prepared active coke can synergistically treat various pollutants (Sox, NOx, heavy metal, dioxin and the like) in the sintering flue gas, meets the ecological environmental protection program in the 13th Five Year Plan of the state, and has important meaning for the sintering flue gas by virtue of a domesticated active coke technology.
Description
Technical field
It is more particularly to a kind of to use resident's coal gas the present invention relates to blast furnace ironmaking SINTERING PRODUCTION energy-conserving and emission-cutting technology field
The surplus industry semi-coke of one of engineering byproduct is raw material, prepares the burnt method of sintering flue gas desulfurization denitration adsorbent activity.
Technical background
Sintering flue gas be iron and steel enterprise's Air Pollutant Emission main source, mainly comprising sulfur dioxide, nitrogen oxides,
Various pollutions such as particulate matter, bioxin, heavy metal (lead, arsenic, cadmium, chromium, mercury etc.), fluoride and volatile organic matter (VOCs)
Thing, wherein first five influence of kind pollutant to environment are protruded the most, especially sulfur dioxide and nitrogen oxides, and the two is haze master
The important as precursors thing for wanting composition PM2.5 to be formed.《Steel sintering, pelletizing industrial air pollution thing discharge standard》(GB28662-
Etc. 2012) a series of steel industry New emission standards were formally implemented from October 1st, 2012, and were carried out in 1 day January in 2015
Newest discharge standard.Therefore, under new environmental requirement, the control for sintering flue gas pollutant has no longer been simple dedusting
Desulfurization, but need on the basis of the improvement of Single Pollution thing, it is considered to the Collaborative Control of multi-pollutant, so as to realize all pollutions
Factor qualified discharge.So, developing new and effective pollutant purification removing sulfuldioxide just turns into the problem of urgent need to resolve at this stage.
Active carbon adsorption (dry method) flue gases purification is big in Japan, South Korea, Australia by 40 years of researches and improvement
Succeeded in the large-scale steel sintering fume treatment project of Leah and Chinese many families application, be proved to be a kind of and be applied to sintering cigarette
The collaboration of gas multi-pollutant is administered, and can simultaneously realize the advanced technology that changing waste into resources is utilized.But the method produces activated carbon mistake
Journey technique is complex, and cost is larger, is unfavorable for the popularization and application under China's present steel production capacity surplus situation.Such as Mitsui
Coal is formed semicoke by mining company by low temperature distillation (pre- carbonization), mix with binding agent after fine grinding by briquetting, is carbonized again, work
Change and activated carbon is obtained, be directly that raw material carries out low temperature distillation with coal, whole set process is complicated, relatively costly.Patent CN1200876C
The production method of disclosed sintering flue gas desulfurization denitration activated carbon, with coking coal and bituminous coal as raw material proportioning after produce activated carbon,
China's coking coal resource is rare, so the activated carbon of the method for kind production is relatively costly, while bulk density is also smaller.Patent
CN1903717A with lignite and coking coal as raw material, by the way that raw coal is broken, proportioning, grind again be well mixed with binding agent, be carbonized,
Activation obtains activated coke, and the method raw material has used cheap lignite, but coking coal is at most used by weight percentage
30%, cost is still higher, while technical process is relative complex.It is a kind of in flue gas disclosed in patent CN102728322
Activated coke of bioxin absorption and preparation method thereof, solve only the problem of metallurgic waste gas bioxin, and desulphurization denitration need to separately set dress
Put.A kind of simultaneous SO_2 and NO removal catalyst disclosed in patent CN201210462982.7, it is necessary to will sintering flue gas to 300~
500 DEG C could realize denitration, while desulfuration efficiency is relatively low under high temperature, high energy consumption is less economical.
Activated coke is a kind of porous carbonaceous materials, belongs to activated carbon class adsorbent.Activated coke has absorption property, catalytic
Can, and can very easily regenerate, overcome that activated carbon is expensive, mechanical strength is low, the shortcoming of easy crushing.Western China
Contain substantial amounts of jet coal and dross coal, its resident's gas engineering uses shaft furnace gas making, a large amount of semi-cokes of by-product mostly.And semi-coke
Used as the raw material of emerging coal deep processing industry, related syndrome is not yet ripe perfect using technology, also can refer to both at home and abroad
Technical standard, cause a part of semi-coke resource excess, throughout the year pile up cause environmental pollution by the river.If cheap mistake can be used
Surplus industry semi-coke prepares sintering flue gas desulfurization denitration activated coke, can not only solve the pollution problem of semi-coke accumulation, can be with
The production activated coke of low cost is used to sinter various pollutants of fume collaboration treatment.Have to the energy-saving and emission-reduction of iron and steel enterprise important
Directive significance.
The content of the invention
The present invention is for the resources characteristic of semi-coke and the environmental protection pressure of present steel industry, it is therefore intended that invention is a kind of to be used
The surplus industry semi-coke of one of resident's gas engineering byproduct is raw material, prepares sintering flue gas desulfurization denitration adsorbent-activity
Burnt method.Semi-coke is met sintering flue gas desulfurization denitration by series of processes such as milling, proportioning, shaping, charing, activation
The column activated coke of performance (condition), the activated coke can cooperate with treatment sintering various pollutants of fume, so that for production domesticization is lived
Property burnt technology governance sintering flue gas support is provided.
A kind of method that use semi-coke prepares sintering flue gas desulfurization denitration activated coke, it is characterised in that：
Comprise the following steps：
1st, dry：The semi-coke of ＜ 5mm grades that first will be selected according to air-dried moisture in coal assay method (GB/
T212-2008) in drying 2~6 hours at (105~110) DEG C until sample quality is constant, it is therefore an objective to remove the absorption water of semi-coke
For follow-up fine grinding sample preparation is prepared.
2nd, prepared by material strip：Dried semi-coke sample is ground to below 0.074mm with ball mill.In ground raw material
In allocate into 30% high temperature coal-tar be sufficiently stirred for, mediate after, be pressed into a diameter of 8~10mm on mould, length is 13~
15mm material strips, it is therefore an objective to make finished activated Jiao that there is compressive resistance and abundant pore structure higher, be to ensure experimentation
In quality of coke tar used uniformity, first by tar heating to 60 ± 2 DEG C, and should reuse after fully swaying, kneading process
It is to be carried out in 60 ± 2 DEG C of water bath with thermostatic control.
3rd, material strip is dried：The material strip that will be suppressed is at (105~115) DEG C after fully drying standby (>=6 hours).
4th, carbonize：First the shaping material strip of a certain amount of (>=5g) is fitted into middle temperature tube furnace, in N2Protective effect under, rise
Temperature to the temperature of setting is carbonized.
5th, activate：After charing terminates, N is used in middle temperature tube furnace2It is rapidly heated to activation temperature as protective gas, so
After open CO2Flowmeter, activates to sample, afterwards in N2Protection under be cooled to room temperature, obtain finished product column activated coke.
It is then turned on CO2Flowmeter (CO2Flow set is >=90ml/min), after activation (>=85min) terminates, in N2Protection under it is cold
But to room temperature.
6th, pelletize：Seed activity required for finished product column activated coke is made after crushing is burnt.
In order to be obtained, compressive resistance, specific surface area and combination property are optimal and satisfaction sinters flue gas dry desulfurizing denitration requirement
Activated coke, semi-coke of the present invention prepare during activated coke according to its carbonization heating rate control of different charge weights >=5 DEG C/
Min, carburizing temperature is 600 ± 5 DEG C, and carbonization time takes 60min, and activation temperature is 850 ± 5 DEG C, and soak time takes >=90min,
CO2Flow set is >=100ml/min (carbonization heating rate (DEG C/min), soak time (min), CO2Flow (ml/min) with
Charge weight (g) is directly proportional：Carbonization heating rate=charge weight * 1/5+3, soak time=charge weight+80, CO2Flow=loading
Amount * 2+80).
The beneficial effects of the invention are as follows：
(1) it is the raw material of sintering flue gas desulfurization denitration activated coke to use superfluous industry semi-coke, easily obtains and cost is relatively low,
The method that the semi-coke of complete set prepares sintering flue gas desulfurization denitration activated coke is proposed, can " treatment of wastes with processes of wastes against one another ", collaboration treatment
Sintering various pollutants of fume.
(2) coal tar is used to be matched, be sufficiently stirred for, mediated and be pressed into a diameter of 8 with appropriate raw material for binding agent
~10mm, length is the material strip of 13~15mm, can effectively improve the ratio of briquetting of material strip, the final yield rate for ensureing activated coke；
(3) heating rate of use >=5 DEG C/min is in N2Protection under to shaping material strip be carbonized, afterwards using CO2It is right
Material strip after carbonization is activated, and method is simply continuous, it can be ensured that material strip carbonization is uniform, and is taken off with flue gas desulfurization is met
The mechanical strength (compressive resistance) and removal efficiency of nitre performance.
Brief description of the drawings
Fig. 1 is the technology of the present invention route schematic diagram.
Specific embodiment
In order that the object, technical solution and advantage of invention become more apparent, below in conjunction with accompanying drawing to original of the invention
Reason and feature are described, and example is served only for explaining the present invention, is not intended to limit the scope of the present invention.The present embodiment
Technology path it is as shown in Figure 1.Laboratory sample preparation is carried out to semi-coke first, is obtained secondly by carbonization, activation experiment step
Meet the activated coke of sintering flue gas desulfurization denitration performance.
Embodiment 1
Semi-coke raw material is carried out into sample preparation, i.e., the semi-coke raw material of certain ＜ 5mm is taken using quartering, be put into constant temperature and do
The drying 2 hours of (110 DEG C) of dry case.
By dried semi-coke sample using ball mill grinding to below 0.074mm.In ground a certain amount of semi-coke
30% is mixed into sample by weight percentage to be heated to 60 ± 2 DEG C and fully sway uniform high temperature coal-tar, at 60 ± 2 DEG C
Water bath with thermostatic control in be stirred, mediate, after material to be mixed is uniform, a diameter of 8~10mm is squeezed into using mould and jack,
Length is the material strip of 13~15mm.
The material strip that will be suppressed is standby after fully drying 6 hours at 110 DEG C, and the shaping material strip of 5g first is fitted into middle temperature
In tube furnace, in N2Protection under, with the heating rate of 4 DEG C/min rise to 600 ± 5 DEG C charing 60min.
After charing terminates, in N2Protection under be rapidly heated to 850 ± 5 DEG C, Ran Houkai with the heating rate of 25 DEG C/min
Open CO2Flowmeter (90ml/min), activates 85min, activates after terminating in N2Protection under be cooled to room temperature.
Seed activity required for finished product column activated coke is made after crushing is burnt.
The performances such as compressive resistance, the specific surface area (BET) of activated coke of the present invention are further determined, is carried out with merchandise active carbon
Compare, comparative result is as shown in table 1.
The activated coke of table 1 and merchandise active carbon comprehensive comparison result
Embodiment 2
Semi-coke raw material is carried out into sample preparation, i.e., the semi-coke raw material of certain ＜ 5mm is taken using quartering, be put into constant temperature and do
The drying 2 hours of (110 DEG C) of dry case.
By dried semi-coke sample using ball mill grinding to below 0.074mm.In ground a certain amount of semi-coke
30% is mixed into sample by weight percentage to be heated to 60 ± 2 DEG C and fully sway uniform high temperature coal-tar, at 60 ± 2 DEG C
Water bath with thermostatic control in be stirred, mediate, after material to be mixed is uniform, a diameter of 8~10mm is squeezed into using mould and jack,
Length is the material strip of 13~15mm.
The material strip that will be suppressed is standby after fully drying 6 hours at 110 DEG C, during first the shaping material strip of 10g is fitted into
In warm tube furnace, in N2Protection under, with the heating rate of 5 DEG C/min rise to 600 ± 5 DEG C charing 60min.
After charing terminates, in N2Protection under be rapidly heated to 850 ± 5 DEG C, Ran Houkai with the heating rate of 25 DEG C/min
Open CO2Flowmeter (100ml/min), activates 90min, activates after terminating in N2Protection under be cooled to room temperature.
Seed activity required for finished product column activated coke is made after crushing is burnt.
The performances such as compressive resistance, the specific surface area (BET) of activated coke of the present invention are further determined, is carried out with merchandise active carbon
Compare, comparative result is as shown in table 2.
The activated coke of table 2 and merchandise active carbon comprehensive comparison result
Embodiment 3
Semi-coke raw material is carried out into sample preparation, i.e., the semi-coke raw material of certain ＜ 5mm is taken using quartering, be put into constant temperature and do
The drying 2 hours of (110 DEG C) of dry case.
By dried semi-coke sample using ball mill grinding to below 0.074mm.In ground a certain amount of semi-coke
30% is mixed into sample by weight percentage to be heated to 60 ± 2 DEG C and fully sway uniform high temperature coal-tar, at 60 ± 2 DEG C
Water bath with thermostatic control in be stirred, mediate, after material to be mixed is uniform, a diameter of 8~10mm is squeezed into using mould and jack,
Length is the material strip of 13~15mm.
The material strip that will be suppressed is standby after fully drying 6 hours at 110 DEG C, during first the shaping material strip of 15g is fitted into
In warm tube furnace, in N2Protection under, with the heating rate of 6 DEG C/min rise to 600 ± 5 DEG C charing 60min.
After charing terminates, in N2Protection under be rapidly heated to 850 ± 5 DEG C, Ran Houkai with the heating rate of 25 DEG C/min
Open CO2Flowmeter (110ml/min), activates 95min, activates after terminating in N2Protection under be cooled to room temperature.
Seed activity required for finished product column activated coke is made after crushing is burnt.
The performances such as compressive resistance, the specific surface area (BET) of activated coke of the present invention are further determined, is carried out with merchandise active carbon
Compare, comparative result is as shown in table 3.
The activated coke of table 3 and merchandise active carbon comprehensive comparison result
Embodiment 4
Semi-coke raw material is carried out into sample preparation, i.e., the semi-coke raw material of certain ＜ 5mm is taken using quartering, be put into constant temperature and do
The drying 2 hours of (110 DEG C) of dry case.
By dried semi-coke sample using ball mill grinding to below 0.074mm.In ground a certain amount of semi-coke
30% is mixed into sample by weight percentage to be heated to 60 ± 2 DEG C and fully sway uniform high temperature coal-tar, at 60 ± 2 DEG C
Water bath with thermostatic control in be stirred, mediate, after material to be mixed is uniform, a diameter of 8~10mm is squeezed into using mould and jack,
Length is the material strip of 13~15mm.
The material strip that will be suppressed is standby after fully drying 6 hours at 110 DEG C, during first the shaping material strip of 30g is fitted into
In warm tube furnace, in N2Protection under, with the heating rate of 9 DEG C/min rise to 600 ± 5 DEG C charing 60min.
After charing terminates, in N2Protection under be rapidly heated to 850 ± 5 DEG C, Ran Houkai with the heating rate of 25 DEG C/min
Open CO2Flowmeter (140ml/min), activates 110min, activates after terminating in N2Protection under be cooled to room temperature.
Seed activity required for finished product column activated coke is made after crushing is burnt.
The performances such as compressive resistance, the specific surface area (BET) of activated coke of the present invention are further determined, is carried out with merchandise active carbon
Compare, comparative result is as shown in table 4.
The activated coke of table 4 and merchandise active carbon comprehensive comparison result
Preferred embodiments of the invention are the foregoing is only, is not intended to limit the invention, it is all in theory of the invention and original
Within then, any modification, equivalent substitution and improvements done should be included within the scope of the present invention.
Claims (4)
1. a kind of method that use semi-coke prepares sintering flue gas desulfurization denitration activated coke, it is characterised in that：
Preparation process is as follows：
1) dry：The semi-coke of ＜ 5mm grades that will be selected according to air-dried moisture in GB/T212-2008 coals assay method in
2~6 hours are dried at 105~110 DEG C until sample quality is constant；
2) prepared by material strip：Dried semi-coke sample is ground to below 0.074mm with ball mill, is matched somebody with somebody in ground raw material
Enter 30% high temperature coal-tar be sufficiently stirred for, mediate after, a diameter of 8~10mm is pressed on mould, length is 13~15mm
Material strip；
3) material strip is dried：The material strip that will be suppressed standby, drying time >=6 hour after fully drying at 105~115 DEG C；
4) carbonize：First the shaping material strip of a certain amount of (>=5g) is fitted into middle temperature tube furnace, in N2Protective effect under, be warming up to
The temperature of setting is carbonized.
5) activate：After charing terminates, N is used in middle temperature tube furnace2It is rapidly heated to activation temperature, Ran Houkai as protective gas
Open CO2Flowmeter, activates to sample, afterwards in N2Protection under be cooled to room temperature, obtain finished product column activated coke.Then
Open CO2Flowmeter；CO2Flow set is >=90ml/min, soak time >=85min；After end, in N2Protection under cool down
To room temperature；
6) pelletize：Seed activity required for finished product column activated coke is made after crushing is burnt.
2. the method that use semi-coke according to claim 1 prepares sintering flue gas desulfurization denitration activated coke, its feature exists
In：According to different charge weights during semi-coke preparation activated coke, carbonization heating rate is controlled in >=5 DEG C/min, carbonization temperature
It is 600 ± 5 DEG C to spend, and carbonization time takes 60min, and activation temperature is 850 ± 5 DEG C, and soak time takes >=90min；CO2Flow set
It is >=100ml/min；Carbonization heating rate (DEG C/min), soak time (min), CO2Flow (ml/min) and charge weight (g) into
Direct ratio：Carbonization heating rate=charge weight * 1/5+3, soak time=charge weight+80, CO2Flow=charge weight * 2+80.
3. the method that use semi-coke according to claim 1 prepares sintering flue gas desulfurization denitration activated coke, its feature exists
In：Step 2) high temperature coal-tar is to be heated to 60 ± 2 DEG C, and reuse after fully swaying.
4. the method that use semi-coke according to claim 1 prepares sintering flue gas desulfurization denitration activated coke, its feature exists
In：Step 2) kneading process carried out in 60 ± 2 DEG C of water bath with thermostatic control.
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Cited By (5)
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|---|---|---|---|---|
| CN107915224A (en) * | 2018-01-02 | 2018-04-17 | 陕西煤业化工集团神木天元化工有限公司 | The method of activated carbon and the activated carbon of acquisition are prepared using semi-coke small powder and coal tar |
| CN108516545A (en) * | 2018-04-03 | 2018-09-11 | 宁夏廷远活性炭有限公司 | A kind of production technology producing activated coke using semi-coke |
| CN109179407A (en) * | 2018-09-21 | 2019-01-11 | 西安建筑科技大学 | A kind of semi-coke base activated coke and preparation method thereof |
| 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 |
| CN114426276A (en) * | 2020-10-29 | 2022-05-03 | 宝武炭材料科技有限公司 | Preparation method of columnar activated coke for desulfurization and denitrification |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107915224A (en) * | 2018-01-02 | 2018-04-17 | 陕西煤业化工集团神木天元化工有限公司 | The method of activated carbon and the activated carbon of acquisition are prepared using semi-coke small powder and coal tar |
| CN108516545A (en) * | 2018-04-03 | 2018-09-11 | 宁夏廷远活性炭有限公司 | A kind of production technology producing activated coke using semi-coke |
| CN109179407A (en) * | 2018-09-21 | 2019-01-11 | 西安建筑科技大学 | A kind of semi-coke base activated coke and preparation method thereof |
| CN114426276A (en) * | 2020-10-29 | 2022-05-03 | 宝武炭材料科技有限公司 | Preparation method of columnar activated coke for desulfurization and denitrification |
| 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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