CN105540751B - A kind of preparation method of Fe-C method filler - Google Patents
A kind of preparation method of Fe-C method filler Download PDFInfo
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- CN105540751B CN105540751B CN201510922227.6A CN201510922227A CN105540751B CN 105540751 B CN105540751 B CN 105540751B CN 201510922227 A CN201510922227 A CN 201510922227A CN 105540751 B CN105540751 B CN 105540751B
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- greasy filth
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- 239000000945 filler Substances 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 68
- 229910017112 Fe—C Inorganic materials 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 73
- 238000005097 cold rolling Methods 0.000 claims abstract description 36
- 229910052742 iron Inorganic materials 0.000 claims abstract description 31
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000002817 coal dust Substances 0.000 claims abstract description 17
- 239000011261 inert gas Substances 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000000197 pyrolysis Methods 0.000 claims abstract description 5
- 239000003960 organic solvent Substances 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 18
- 239000003245 coal Substances 0.000 claims description 17
- 239000011324 bead Substances 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000003610 charcoal Substances 0.000 claims description 8
- 239000004519 grease Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000005868 electrolysis reaction Methods 0.000 claims description 6
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 6
- 239000011707 mineral Substances 0.000 claims description 6
- 239000012798 spherical particle Substances 0.000 claims description 6
- 239000004094 surface-active agent Substances 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 5
- 235000019871 vegetable fat Nutrition 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229910000831 Steel Inorganic materials 0.000 abstract description 8
- 239000010959 steel Substances 0.000 abstract description 8
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 229910052799 carbon Inorganic materials 0.000 abstract description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 abstract description 3
- 239000002351 wastewater Substances 0.000 description 10
- 238000004939 coking Methods 0.000 description 8
- 239000000839 emulsion Substances 0.000 description 7
- 239000000843 powder Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000009303 advanced oxidation process reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000002468 redox effect Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 235000019197 fats Nutrition 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- XEEYBQQBJWHFJM-OUBTZVSYSA-N iron-52 Chemical compound [57Fe] XEEYBQQBJWHFJM-OUBTZVSYSA-N 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention discloses a kind of preparation methods of Fe-C method filler, it is using cold rolling greasy filth and coal dust as raw material, carries out destructive distillation under inert gas shielding after mixing, obtains the activated carbon of Fe2O3 doping to get Fe-C method filler；The mass ratio of the cold rolling greasy filth and coal dust is 1：（20~50）, cold rolling greasy filth is mainly the mixture of micron iron powder or nanometer iron powder and organic solvent.The present invention is to be fired to survive with iron-containing active carbon particle using the common coal dust of steel industry and cold rolling greasy filth, with micron order iron and reduction ferrous components, and Fe-C method filler particles are formed with pore-creating phenomenon, it is at low cost so as to improve the reaction efficiency of primary battery.
Description
Technical field
The invention belongs to metallurgical environmental protection fields, and in particular to a kind of preparation method of Fe-C method filler.
Background technology
In waste water treatment process, broad spectrum activity of the advanced oxidation processes because of its degradation efficiency height and to organism kinds becomes
Handle the method first of used water difficult to degradate.And in advanced oxidation processes, Fe-C method is a kind of efficient treatment process, place
The principle of reason is mainly by forming iron charcoal primary battery, and primary battery aoxidizes the hardly degraded organic substance in waste water, so as to reach
The organic matter purpose into degrading waste water.And in Fe-C method treatment process, efficient electricity charcoal primary battery particle is processing
The key of efficiency.At present, Fe-C method filler particles are mainly made by the way that iron powder is doped in activated carbon, such
Inner electrolysis filler particles its prepare it is simple, but its because of iron powder the inhomogeneities in charcoal particle, so as to cause its reaction efficiency low
Under.
Invention content
The technical problems to be solved by the invention be for the above-mentioned prior art in deficiency, a kind of Fe-C method is provided
The preparation method of filler is to be fired to survive with iron-containing activated carbon using the common coal dust of steel industry and cold rolling greasy filth
Particle has micron order iron and reduction ferrous components, and forms pore-creating phenomenon to Fe-C method filler particles, so as to improve original
The reaction efficiency of battery, it is at low cost.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is as follows：
A kind of preparation method of Fe-C method filler is using cold rolling greasy filth and coal dust as raw material, after mixing lazy
Destructive distillation is carried out under property gas shield, obtains the activated carbon of Fe2O3 doping to get Fe-C method filler；The cold rolling greasy filth and coal dust
Mass ratio be 1：（20~50）, cold rolling greasy filth is mainly the mixture of micron iron powder or nanometer iron powder and organic solvent.
By said program, the component in the cold rolling greasy filth is by mass percentage：Mineral grease 20 ~ 30%, vegetable oil
Fat 10 ~ 20%, iron 40 ~ 57%, surfactant 3 ~ 5%, water 10 ~ 20%.In metallurgical cold-rolling process, in order to be cooled down to steel billet
And lubrication, a large amount of emulsion can be used, and emulsion is after a period of time has passed, because contaminated, is purified, and leads to
It is often that it is filtered by magnetic bar filter, what is filtered down from magnetic bar filter is largely containing grease and iron filings
The mixed pollutants of mixed pollutants, this grease and iron filings are commonly referred to as cold rolling greasy filth.
By said program, the preferred bottle coal powder of coal dust, coal particle size is 100 ~ 300 microns.Bottle coal is that China has been verified
Occupy one of coal of large percentage in coking coal reserves, degree of metamorphism is low, and volatile matter is higher, and cohesiveness is generally weaker than gas fertilizer
Coal, rich coal, 1/3 coking coal and coking coal etc., the ratio occupied in practical coal blending is few.
By said program, the inert gas is nitrogen or rare gas.
By said program, the pyrolysis temperature is 800 ~ 900 DEG C.
The preparation method of above-mentioned Fe-C method filler, specifically comprises the following steps：
1）It is 1 according to the mass ratio of cold rolling greasy filth and coal dust：（20~50）The two is sufficiently mixed uniformly；
2）Under inert gas shielding, by step 1）Gained mixture is heated to 800 ~ 900 DEG C, keeps the temperature more than 1.5h；
3）Under inert gas shielding, by step 2）Products therefrom is cooled to room temperature, obtain the activated carbon of doping iron to get
To Fe-C method filler.
Another preparation method of above-mentioned Fe-C method filler, it is more economical quick, specifically comprise the following steps：
1）It is 1 according to the mass ratio of cold rolling greasy filth and coal dust：（20~50）The two is sufficiently mixed uniformly；
2）By step 1）After gained mixture is heated to 100 DEG C, inert gas shielding is passed through, is continuously heating to 800 ~ 900
DEG C, 1.5 ~ 3h is kept the temperature, is then maintained under inert gas shielding, is cooled to 100 DEG C, then stops being passed through inert gas, cool down
Room temperature obtains the activated carbon of doping iron to get to Fe-C method filler.
By said program, the Fe-C method filler is crushed to required grain shape, as Fe-C method filler
Grain.Under normal conditions, it is contemplated that the specific surface area of spherical particle is bigger, and the Fe-C method filler is generally prepared as required
Grain size is spherical particle, as Fe-C method filler bead.
Fe-C method filler of the present invention has higher redox effect for primary battery, in oxidable waste water
Hardly degraded organic substance.
Compared with prior art, the beneficial effects of the invention are as follows：
1）The present invention is carried out using the greasy filth of the common coal dust of steel industry and the generation of cold-rolling pickling section magnetic bar filter
Firing is survived with iron-containing active carbon particle, i.e. Fe-C method filler, and the greasy filth on magnetic bar filter is mainly micron iron
Such substance is doped in coal dust by the mixture of powder or nanometer iron powder and organic solvent, can make activated carbon obtained
Grain has micron order iron and reduction ferrous components, and the evenly property of the iron in Fe-C method filler particles, has very high oxidation
Reduction effect.
2）Fe-C method filler of the present invention is gasified at high temperature using the oil content contained by cold rolling greasy filth volatilizees this
One characteristic forms pore-creating phenomenon to Fe-C method filler particles, increases the reaction specific surface area of Fe-C method filler, solution
The certainly conventional iron charcoal electrolysis underdeveloped problem of primary battery pore structure, so as to improve the reaction efficiency of primary battery, so as to fulfill
Fe-C method primary battery efficiency maximizes.
3）The present invention prepares iron using the greasy filth that the common coal dust of steel industry and cold-rolling pickling section magnetic bar filter generate
Charcoal Inner electrolysis filler is to solve ferrum-carbon internal electrolysis processing high concentrated organic wastewater key point of high cost, can make to be originally used for
The cold rolling greasy filth of danger wastes becomes the raw material for generating efficient Fe-C method primary battery, realizes dangerous waste recycling.
Description of the drawings
Fig. 1 is the shape appearance figure of micron iron in cold rolling greasy filth.
Fig. 2 is the energy spectrum diagram of cold rolling greasy filth.
Fig. 3 is the microscopic appearance figure of Fe-C method filler prepared by the present invention.
Fig. 4 is the pictorial diagram of Fe-C method filler bead prepared by the present invention.
Fig. 5 is Fe-C method filler bead prepared by the present invention and comparison filler to coking high concentrated organic wastewater COD
Removing is compared.
Fig. 6 is the Fe-C method filler bead prepared through the present invention, treated that coking high concentration is organic for comparison filler
UV- ~ VIS scanning figures of waste water.
Specific embodiment
Further detailed description is done to the present invention, but the embodiment invented is without being limited thereto with reference to embodiment.
Cold rolling greasy filth is steel industry in the steel bad operation of rolling, from the bad fine particle iron to come off of steel（Micron order is very
To nanoscale）It is mingled in emulsion, the later stage in the purification process of emulsion, is adsorbed by magnetic bar filter, main
Ingredient is mainly mineral grease 20 ~ 30%, vegetable fat 10 ~ 20%, iron 40 ~ 57%, surfactant 3 ~ 5%, water 10 ~ 20%.
Embodiment 1
A kind of preparation method of Fe-C method filler, specifically comprises the following steps：
1）50g greasy filth is taken to be placed in the high-volatile bottle coal powder of 2000g from the magnetic bar filter of cold-rolling emulsion workshop section
In, the two is sufficiently mixed mixing using blender；Component in the cold rolling greasy filth is by mass percentage：Mineral grease
22%, vegetable fat 15%, iron 40%, surfactant 3%, water 20%；The grain size of high-volatile bottle coal powder is at 90 ~ 150 microns；
2）By step 1）Gained mixture is put into heating furnace heating, after temperature reaches 100 DEG C, is passed through into heating furnace
N2, continue to heat heating furnace, until temperature rises to 900 DEG C, heating furnace kept the temperature at 900 DEG C；After keeping the temperature 2h,
Heating furnace is heated in stopping, continuing logical N2, furnace temperature is made to be cooled to 100 DEG C；After furnace temperature is cooled to 100 DEG C, stop being passed through
Nitrogen until heating furnace cools down room temperature, obtains the activated carbon of doping iron to get to Fe-C method filler；
3）By step 2）It is spherical particle that gained Fe-C method filler, which is crushed to required grain size, as Fe-C method
Filler bead.
Embodiment 2
A kind of preparation method of Fe-C method filler, specifically comprises the following steps：
1）50g greasy filth is taken to be placed in the high-volatile bottle coal of 1000g from the magnetic bar filter of cold-rolling emulsion workshop section,
The two is sufficiently mixed mixing using blender；Component in the cold rolling greasy filth is by mass percentage：Mineral grease
30%, vegetable fat 10%, iron 40%, surfactant 5%, water 15%；The grain size of high-volatile bottle coal powder is at 100 ~ 200 microns；
2）By step 1）Gained mixture is put into heating furnace, and N is passed through into heating furnace2It is protected, temperature rises to 800 DEG C
After kept the temperature；After keeping the temperature 1.5h, N is kept2In the case of being continually fed into, furnace temperature is made gradually to be cooled to room temperature, obtain doping iron
Activated carbon to get to Fe-C method filler；
3）By step 2）It is spherical particle that gained Fe-C method filler, which is crushed to required grain size, as Fe-C method
Filler bead.
Embodiment 3
A kind of preparation method of Fe-C method filler, specifically comprises the following steps：
1）50g greasy filth is taken to be placed in the high-volatile bottle coal of 2500g from the magnetic bar filter of cold-rolling emulsion workshop section,
The two is sufficiently mixed mixing using blender；Component in the cold rolling greasy filth is by mass percentage：Mineral grease
20%, vegetable fat 10%, iron 57%, surfactant 3%, water 15%；The grain size of high-volatile bottle coal powder is at 200 ~ 300 microns；
2）By step 1）Gained mixture is put into heating furnace heating, after temperature reaches 100 DEG C, is passed through into heating furnace
N2, continue to heat heating furnace, until temperature rises to 850 DEG C, heating furnace kept the temperature at 850 DEG C；After keeping the temperature 3h,
Heating furnace is heated in stopping, continuing logical N2, furnace temperature is made to be cooled to 100 DEG C；After furnace temperature is cooled to 100 DEG C, stop being passed through
Nitrogen until heating furnace cools down room temperature, obtains the activated carbon of doping iron to get to Fe-C method filler；
3）By step 2）It is spherical particle that gained Fe-C method filler, which is crushed to required grain size, as Fe-C method
Filler bead.
Fig. 1 is the shape appearance figure of the scanning electron microscope of cold rolling greasy filth, and cold rolling greasy filth can be shown from figure mainly by two phase compositions,
Organic matter and iron part including black, and the fineness of iron particle is in the micron-scale.
Fig. 2 is the scanning electron microscope energy spectrum diagram of cold rolling greasy filth, it can be seen that：The essential element of cold rolling greasy filth is iron element and carbon.
Fig. 3 is the shape appearance figure of Fe-C method filler bead prepared by the present invention, it can be seen that the Fe-C method filler is small
Ball has abundant pore structure, so as to larger specific surface area.
Fe-C method filler bead prepared by the present invention and commercially available filler be made primary battery to coking wastewater at
Reason, as a result as shown in Figure 5 and Figure 6, it is known that：On processing coking high concentrated organic wastewater, the Fe-C method of the invention prepared
Filler bead is much higher than commercially available common Inner electrolysis filler to the removal rate of COD, can reach 86%；It is prepared through the present invention
Fe-C method filler bead treated coking wastewater, result is more excellent, has higher redox effect, more effectively
Hardly degraded organic substance in ground oxidized waste water.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, replacement, combine, simplification, should be
Equivalent substitute mode, is included within protection scope of the present invention.
Claims (9)
1. a kind of preparation method of Fe-C method filler, it is characterised in that it is the mixing using cold rolling greasy filth and coal dust as raw material
Destructive distillation is carried out under inert gas shielding after uniformly, obtains the activated carbon of Fe2O3 doping to get Fe-C method filler；The cold rolling
The mass ratio of greasy filth and coal dust is 1：（20~50）, cold rolling greasy filth is mainly the mixed of micron iron powder or nanometer iron powder and organic solvent
Close object.
A kind of 2. preparation method of Fe-C method filler according to claim 1, it is characterised in that the cold rolling greasy filth
In component be by mass percentage：Mineral grease 20 ~ 30%, vegetable fat 10 ~ 20%, iron 40 ~ 57%, surfactant 3 ~
5%, water 10 ~ 20%.
3. the preparation method of a kind of Fe-C method filler according to claim 1, it is characterised in that the coal dust is gas
Coal.
A kind of 4. preparation method of Fe-C method filler according to claim 1, it is characterised in that the inert gas
For nitrogen or rare gas.
A kind of 5. preparation method of Fe-C method filler according to claim 1, it is characterised in that the pyrolysis temperature
It is 800 ~ 900 DEG C.
6. the preparation method of a kind of Fe-C method filler according to claim 1, it is characterised in that include the following steps：
1）It is 1 according to the mass ratio of cold rolling greasy filth and coal dust：（20~50）The two is sufficiently mixed uniformly；
2）Under inert gas shielding, by step 1）Gained mixture is heated to 800 ~ 900 DEG C, keeps the temperature more than 1.5h；
3）Under inert gas shielding, by step 2）Products therefrom is cooled to room temperature, and obtains the activated carbon of doping iron to get to iron
Charcoal Inner electrolysis filler.
7. the preparation method of a kind of Fe-C method filler according to claim 1, it is characterised in that include the following steps：
1）It is 1 according to the mass ratio of cold rolling greasy filth and coal dust：（20~50）The two is sufficiently mixed uniformly；
2）By step 1）After gained mixture is heated to 100 DEG C, inert gas shielding is passed through, is continuously heating to 800 ~ 900 DEG C, is protected
1.5 ~ 3h of temperature, is then maintained under inert gas shielding, is cooled to 100 DEG C, then stops being passed through inert gas, is cooled to room
Temperature obtains the activated carbon of doping iron to get to Fe-C method filler.
8. the preparation method of a kind of Fe-C method filler according to claim 1, it is characterised in that electric in the iron charcoal
Solution filler is crushed to required grain shape, as Fe-C method filler particles.
9. the preparation method of a kind of Fe-C method filler according to claim 8, it is characterised in that electric in the iron charcoal
Solution filler is prepared into the spherical particle of required grain size, as Fe-C method filler bead.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510922227.6A CN105540751B (en) | 2015-12-11 | 2015-12-11 | A kind of preparation method of Fe-C method filler |
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| CN201510922227.6A CN105540751B (en) | 2015-12-11 | 2015-12-11 | A kind of preparation method of Fe-C method filler |
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| CN105540751A CN105540751A (en) | 2016-05-04 |
| CN105540751B true CN105540751B (en) | 2018-06-26 |
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| CN104495988A (en) * | 2014-12-02 | 2015-04-08 | 刘达苏 | Production method of spherical iron-carbon micro-electrolysis filler |
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| CN104495988A (en) * | 2014-12-02 | 2015-04-08 | 刘达苏 | Production method of spherical iron-carbon micro-electrolysis filler |
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Effective date of registration: 20170719 Address after: 430083, Gate No. 2, Qingshan District, Hubei, Wuhan Applicant after: WUHAN IRON AND STEEL Co.,Ltd. Address before: 430080 Wuhan, Hubei Friendship Road, No. 999, Wuchang Applicant before: WUHAN IRON AND STEEL (GROUP) Corp. |
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