CN105435738A - A method of preparing a C/gamma-Fe2O3 composite material from acid-regeneration desilication mud cakes - Google Patents
A method of preparing a C/gamma-Fe2O3 composite material from acid-regeneration desilication mud cakes Download PDFInfo
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- CN105435738A CN105435738A CN201410426016.9A CN201410426016A CN105435738A CN 105435738 A CN105435738 A CN 105435738A CN 201410426016 A CN201410426016 A CN 201410426016A CN 105435738 A CN105435738 A CN 105435738A
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- desilication
- desiliconization
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Abstract
A method of preparing a C/gamma-Fe2O3 composite material from acid-regeneration desilication mud cakes is disclosed. The method includes a) adding water into block desilication mud cakes, pulping under heating, and adding furfuryl alcohol, furfural or starch the mass of which is 2-5 times of that of the desilication mud cakes so as to form desilication mud slurry with food dispersity, b) subjecting the slurry in the step a) to spray drying at 100-120 DEG C to obtain coated desilication mud powder, and c) adding the desilication mud powder obtained in the step b) into a heating furnace, raising the temperature to 600-900 DEG C at a heating speed of 2-5 DEG C/min under inert gas protection, maintaining the temperature for 4-8 h after reaching the target temperature, and cooling inside the furnace to obtain the C/gamma-Fe2O3 composite material. The method of preparing the C/gamma-Fe2O3 composite material from the acid-regeneration desilication mud cakes is provided. The starch, the furfuryl alcohol or the furfural which are cheap are utilized for coating, and then thermal cracking is performed to obtain the magnetic carbon material. The method effectively achieves recovery and reutilization of resources.
Description
Technical field
The present invention relates to a kind of preparation method of composite, be specifically related to the preparation method that the magnetic agraphitic carbon C of tool prepared by trade waste.
Background technology
Material with carbon element is hydrophobic adsorbent, deposits still can play a role in case having water or steam; Material with carbon element is not only applicable to absorption land leakage, also can be used for adsorbed water body leakage; And during for oil removing waterborne, can not sink after absorption.Although carbon has plurality of advantages, in adsorption capacity, being separated complexity, there is limitation in recuperability aspect.
At present, in the cold-rolling process of silicon steel, owing to having the features such as pickling speed is fast, quality good, acid regeneration is easy, chlorohydric acid pickling has become the mainstream technology in strip pickling.Because steel grade itself is containing more Si element, the Si concentration in acid-washing waste acid also can significantly increase.So, for ensureing the iron oxide red quality that acid regeneration unit is produced, pickle liquor enters regeneration technology need set up silica removal device.The process route that usual heavy steel rolling mill uses be by pickle liquor after molten iron flask reaction, add the ammoniacal liquor adjusted to ph of about 20%, then pass into compressed air and generate ferric iron by the SiO in solution
2coated, then add flocculant, by the Fe (OH) generated
3together with SiO
2sedimentation together, to remove the SiO in pickle
2.This process will produce a large amount of desiliconization mud cakes.A large-scale cold rolling steel mill, every year can the desiliconization mud cake of output nearly ten thousand tons, how to dispose the important topic that these desiliconization mud cakes become steel mill's integrated treatment.
Chinese patent application CN200610024039.2 discloses a kind of method that desiliconization mud cake produces iron oxide black, by preparation stoste, prepares the steps such as iron oxide yellow, slurrying, drying, press filtration, oven dry, produces iron oxide black.The method produces iron oxide black, and the added value of iron oxide black is not high, and production process environmental pollution is larger, and need the iron oxide seed crystal price of interpolation also higher, and the economy of whole set process is not strong; In addition, Chinese patent application CN201210359797.5 also discloses a kind of acid regeneration desiliconization mud cake that utilizes and prepares the red method of superfine iron oxide, can with desiliconization mud cake for raw material, and production iron oxide red, can be used for the field such as pigment, paint.What this method was produced is iron oxide red, the added value of iron oxide red is better, but prerequisite is purity reaches requirement, high-purity iron oxide red at least more than 99.3% could for the production of soft magnetic materials, by the iron oxide red that above-mentioned technology is produced, wherein silicone content is uncontrollable to ppm level, and such iron oxide red cannot for the production of soft magnetic products, can only be used for pigment, paint, be there is the not high problem of economy equally.
Summary of the invention
Therefore, the technical problem to be solved in the present invention is that one utilizes regenerated acid desiliconization mud cake to prepare C/ γ-Fe
2o
3the method of composite.
Technical scheme of the present invention is, a kind of acid regeneration desiliconization mud cake prepares C/ γ-Fe
2o
3the method of composite, comprises the following steps:
A, to add water in block desiliconization mud cake, and pull an oar under heating state, add the furfuryl alcohol accounting for desiliconization mud cake 2-5 times of quality, furfural or starch, form dispersed desiliconization material-mud preferably;
B, by the slurry in above-mentioned a after the spraying dry of 100-120 DEG C, obtain coated desiliconization mud powder;
C, the desiliconization mud powder obtained by above-mentioned b are inserted in heating furnace, and under inert gas shielding atmosphere, programming rate is 2-5 DEG C/min, and target temperature is 600-900 DEG C, and after reaching target temperature, insulation 4-8h, obtains C/ γ-Fe with stove cooling
2o
3composite.
A kind of acid regeneration desiliconization mud cake according to the present invention prepares C/ γ-Fe
2o
3the method of composite, preferably, heating-up temperature described in step a is 65-95 DEG C.
Further, heating-up temperature described in step a is 75-85 DEG C.
Preferably, heating furnace described in step c is tube furnace.
A kind of acid regeneration desiliconization mud cake according to the present invention prepares C/ γ-Fe
2o
3the method of composite, preferably, inert gas described in step c is selected from the one in nitrogen, argon gas, helium.Further, described inert gas is nitrogen.
Method provided by the invention, can using the higher desiliconization mud cake of iron-holder as template, and by simple polymeric PTC materials, thermal cracking, obtains having recyclable, to realize magnetic water-oil separating C/ γ-Fe
2o
3composite.This composite is a kind of carbon shell parcel, possesses γ-Fe
2o
3the material of kernel, possess good suction-operated to the oil slick in water body, adsorption effect is more than 95%.And can reclaim very easily after using, material possesses regeneration and reuses function.
For furfuryl alcohol, desiliconization mud cake adds water after making beating, adds furfuryl alcohol, and form material-mud, heat up under a shielding gas, the iron hydroxide in desiliconization mud cake can generate γ-Fe
2o
3, and the shell of the Viability charcoal of furfuryl alcohol meeting carbonization, form composite.
The invention has the beneficial effects as follows:
What the technical program provided utilizes acid regeneration desiliconization mud cake to prepare C/ γ-Fe
2o
3the method of composite, do not need acid dissolve or alkali course of dissolution, preparation process environmental pollution is little, raw materials Ye Shi steel mill solid waste, is a kind of eco-friendly friendly process.The technical program technique is simple, is easy to operation, and continuity is strong, and direct thermal cracking obtains magnetic carbon material, can be applicable in water-oil separating, better realizes the problem of resource reclaim recycling.
Accompanying drawing explanation
Fig. 1 is the C/ γ-Fe in the embodiment of the present invention 1
2o
3xRD figure.
Detailed description of the invention
Embodiment 1.
A () adds water in block desiliconization mud cake, and pull an oar under 80 DEG C of heating states, adds the furfuryl alcohol of 5 times of quality desiliconization mud cakes, forms dispersed desiliconization material-mud preferably.
B slurry in above-mentioned (a) after the spraying dry of 110 DEG C, is obtained the desiliconization mud powder that more fluffy furfuryl alcohol is coated by ();
C desiliconization mud powder that above-mentioned (b) obtains by () inserts the N that programming rate is 2.5 DEG C/min
2atmosphere is protected in the tube furnace of 800 DEG C, after insulation 5h, can obtain C/ γ-Fe with stove cooling
2o
3composite.
Embodiment 2.
A () adds water in block desiliconization mud cake, and pull an oar under 80 DEG C of heating states, adds the furfural of 4 times of quality desiliconization mud cakes, forms dispersed desiliconization material-mud preferably.
B slurry in above-mentioned (a) after the spraying dry of 100 DEG C, is obtained the desiliconization mud powder that more fluffy furfural is coated by ();
It is that the N2 atmosphere of 2 DEG C/min is protected in the tube furnace of 700 DEG C that c desiliconization mud powder that above-mentioned (b) obtains by () inserts programming rate, after insulation 6h, can obtain C/ γ-Fe with stove cooling
2o
3composite.
Embodiment 3.
A () adds water in block desiliconization mud cake, and pull an oar under 80 DEG C of heating states, adds the starch of 5 times of quality desiliconization mud cakes, forms dispersed desiliconization material-mud preferably.
B slurry in above-mentioned (a) after the spraying dry of 100-120 DEG C, is obtained the desiliconization mud powder that more fluffy starch is coated by ();
It is that the N2 atmosphere of 2 DEG C/min is protected in the tube furnace of 600 DEG C that c desiliconization mud powder that above-mentioned (b) obtains by () iron oxide inserts programming rate, after insulation 8h, can obtain ultra-fine C/ γ-Fe with stove cooling
2o
3composite.
Embodiment 4.
A () adds water in block desiliconization mud cake, and pull an oar under 75 DEG C of heating states, adds the furfuryl alcohol of 2.5 times of quality desiliconization mud cakes, forms dispersed desiliconization material-mud preferably.
B slurry in above-mentioned (a) after the spraying dry of 100 DEG C, is obtained the desiliconization mud powder that more fluffy furfuryl alcohol is coated by ();
It is that the N2 atmosphere of 2 DEG C/min is protected in the tube furnace of 900 DEG C that c desiliconization mud powder that above-mentioned (b) obtains by () iron oxide inserts programming rate, after insulation 4h, can obtain ultra-fine C/ γ-Fe with stove cooling
2o
3composite.
Embodiment 5.
A () adds water in block desiliconization mud cake, and pull an oar under 80 DEG C of heating states, adds the furfural of 5 times of quality desiliconization mud cakes, forms dispersed desiliconization material-mud preferably.
B slurry in above-mentioned (a) after the spraying dry of 120 DEG C, is obtained the desiliconization mud powder that more fluffy furfural is coated by ();
It is that the N2 atmosphere of 4 DEG C/min is protected in the tube furnace of 700 DEG C that c desiliconization mud powder that above-mentioned (b) obtains by () iron oxide inserts programming rate, after insulation 8h, can obtain ultra-fine C/ γ-Fe with stove cooling
2o
3composite.
Embodiment 6
A () adds water in block desiliconization mud cake, and pull an oar under 85 DEG C of heating states, adds the furfural of 2 times of quality desiliconization mud cakes, forms dispersed desiliconization material-mud preferably.
B slurry in above-mentioned (a) after the spraying dry of 120 DEG C, is obtained the desiliconization mud powder that more fluffy furfuryl alcohol is coated by ();
It is that the argon atmosphere of 5 DEG C/min is protected in the tube furnace of 800 DEG C that c desiliconization mud powder that above-mentioned (b) obtains by () iron oxide inserts programming rate, after insulation 8h, can obtain ultra-fine C/ γ-Fe with stove cooling
2o
3composite.
The present invention utilizes regenerated acid desiliconization mud cake to prepare C/ γ-Fe by providing one
2o
3the method of composite, after utilizing cheap starch, furfural or furfuryl alcohol coated, thermal cracking obtains magnetic carbon material, effectively achieves resource reclaim recycling.
Claims (6)
1. an acid regeneration desiliconization mud cake prepares C/ γ-Fe
2o
3the method of composite, is characterized in that: comprise the following steps:
A, to add water in block desiliconization mud cake, and pull an oar under heating state, add the furfuryl alcohol accounting for desiliconization mud cake 2-5 times of quality, furfuryl alcohol or starch, form dispersed desiliconization material-mud preferably;
B, by the slurry in above-mentioned a after the spraying dry of 100-120 DEG C, obtain coated desiliconization mud powder;
C, the desiliconization mud powder obtained by above-mentioned b are inserted in heating furnace, and under inert gas shielding atmosphere, programming rate is 2-5 DEG C/min, and target temperature is 600-900 DEG C, and after reaching target temperature, insulation 4-8h, obtains C/ γ-Fe with stove cooling
2o
3composite.
2. a kind of acid regeneration desiliconization mud cake according to claim 1 prepares C/ γ-Fe
2o
3the method of composite, is characterized in that, heating-up temperature described in step a is 65-95 DEG C.
3. a kind of acid regeneration desiliconization mud cake according to claim 2 prepares C/ γ-Fe
2o
3the method of composite, is characterized in that, heating-up temperature described in step a is 75-85 DEG C.
4. a kind of acid regeneration desiliconization mud cake according to claim 1 prepares C/ γ-Fe
2o
3the method of composite, is characterized in that, heating furnace described in step c is tube furnace.
5. a kind of acid regeneration desiliconization mud cake according to claim 1 prepares C/ γ-Fe
2o
3the method of composite, is characterized in that, inert gas described in step c is selected from the one in nitrogen, argon gas, helium.
6. a kind of acid regeneration desiliconization mud cake according to claim 5 prepares C/ γ-Fe
2o
3the method of composite, is characterized in that, inert gas described in step c is nitrogen.
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|---|---|---|---|
| CN201410426016.9A CN105435738B (en) | 2014-08-27 | 2014-08-27 | A kind of acid regeneration desiliconization mud cake preparation C/ γ-Fe2O3The method of composite material |
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|---|---|---|---|
| CN201410426016.9A CN105435738B (en) | 2014-08-27 | 2014-08-27 | A kind of acid regeneration desiliconization mud cake preparation C/ γ-Fe2O3The method of composite material |
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| CN105435738B CN105435738B (en) | 2018-10-02 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030100445A1 (en) * | 2001-11-28 | 2003-05-29 | Toshiya Ueda | Photocatalytic active carbon, colored photocatalytic active carbon, coloring active carbon, and deodorant and adsorption product using them |
| CN1807263A (en) * | 2006-02-21 | 2006-07-26 | 上海宝齐氧化铁有限公司 | Method for producing iron oxide black using desilicified mud cake |
-
2014
- 2014-08-27 CN CN201410426016.9A patent/CN105435738B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030100445A1 (en) * | 2001-11-28 | 2003-05-29 | Toshiya Ueda | Photocatalytic active carbon, colored photocatalytic active carbon, coloring active carbon, and deodorant and adsorption product using them |
| CN1807263A (en) * | 2006-02-21 | 2006-07-26 | 上海宝齐氧化铁有限公司 | Method for producing iron oxide black using desilicified mud cake |
Non-Patent Citations (1)
| Title |
|---|
| 邱介山等: ""淀粉基碳包覆铁纳米胶囊的合成及其磁学性能"", 《新型炭材料》 * |
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