CN107540370A - A kind of micropore hercynite raw material and preparation method thereof - Google Patents
A kind of micropore hercynite raw material and preparation method thereof Download PDFInfo
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- CN107540370A CN107540370A CN201710876374.3A CN201710876374A CN107540370A CN 107540370 A CN107540370 A CN 107540370A CN 201710876374 A CN201710876374 A CN 201710876374A CN 107540370 A CN107540370 A CN 107540370A
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Abstract
The present invention relates to a kind of micropore hercynite raw material and preparation method thereof.Its technical scheme is：Under 25 ~ 30 DEG C of water bath conditions, by aluminium dihydrogen phosphate: ammonium hydrogen carbonate: the mass ratio of water is (20 ~ 25): (2 ~ 5): 100, aluminium dihydrogen phosphate, ammonium hydrogen carbonate and water are inserted in container, stirs, obtains mixed solution.The mixed solution: ρ Al is pressed again2O3Micro mist: iron powder: the mass ratio of carbon black is 10: (100 ~ 105): (50 ~ 55): (2 ~ 5), by mixed solution, ρ Al2O3Micro mist, iron powder and carbon black stirring, shaping, obtain being molded compound；Then dry 12 ~ 24 hours, be placed in Muffle furnace under the conditions of 110 ~ 120 DEG C, be incubated 2 ~ 3 hours under the conditions of 1600 ~ 1650 DEG C and in air atmosphere, furnace cooling, crush, micropore hercynite raw material is made.Present invention process is simple and production cost is low；The sintering character of prepared micropore hercynite raw material is good, thermal conductivity factor is small and hercynite high conversion rate.
Description
Technical field
The invention belongs to hercynite technical field.More particularly to a kind of micropore hercynite raw material and its preparation side
Method.
Background technology
Hercynite（FeAl2O4）It is FeO and Al2O3The solid solution formed under the high temperature conditions, there is refractoriness
High, the advantages that intensity is big and resistance to chemical attack is good, it is widely used in the hot industry such as cement, metallurgy, ceramics field.
At present, hercynite is mainly synthesized by sintering process with electric smelting method（The rich preparation for waiting hercynites of Mr. Zhang
[J] silicate is circulated a notice of, 2007,26 (5)：1003~1006）.
Using sintering process synthesizing ferrum-aluminium spinelle, its grain growth is incomplete, and defect is more, especially high-temperature sintering process
In to control climate require it is higher（Fe in reducing atmosphere2+Easily it is changed into simple substance Fe, and Fe in oxidizing atmosphere2+Easily it is transformed into
Fe3+）, thus be difficult to prepare high-purity hercynite；Using electric smelting method synthesizing ferrum-aluminium spinelle, although large-size can be obtained
Crystal grain, but electric smelting method synthesizing ferrum-aluminium spinelle energy consumption is big, and technical process is more complicated（The synthesis of the hercynites such as Li Guohua
And application [J] silicate circulars, 2013,32 (3)：501~505）, thus increase the cost of hercynite.
The content of the invention
It is contemplated that overcome prior art defect, it is therefore an objective to provide the micropore iron that a kind of technique is simple and production cost is low
The preparation method of aluminate raw material.With high conversion rate, the sintering character of the micropore hercynite raw material prepared by this method
Good and thermal conductivity factor is small.
To achieve the above object, the technical solution adopted by the present invention comprises the concrete steps that：
The first step, under 25 ~ 30 DEG C of water bath conditions, aluminium dihydrogen phosphate, ammonium hydrogen carbonate and water are inserted in container, stirring 15 ~ 20
Minute, obtain mixed solution；Wherein, aluminium dihydrogen phosphate: ammonium hydrogen carbonate: the mass ratio of water is (20 ~ 25): (2 ~ 5): 100.
Second step, by the mixed solution, ρ-Al2O3Micro mist, iron powder and carbon black mixing, stir 5 ~ 8 minutes, add mould
Middle shaping, obtain being molded compound；Wherein, the mixed solution: ρ-Al2O3Micro mist: iron powder: the mass ratio of carbon black is 10: (100
~105)∶(50~55)∶(2~5)。
3rd step, the shaping compound added in vacuum drying chamber, dried under the conditions of 110 ~ 120 DEG C 12 ~ 24 small
When, obtain dried shaping compound.
4th step, the dried shaping compound is placed in Muffle furnace, under the conditions of 1600 ~ 1650 DEG C and air
2 ~ 3 hours are incubated in atmosphere, furnace cooling, is crushed, micropore hercynite raw material is made.
Al (the H of the aluminium dihydrogen phosphate2PO4)3Content >=98wt%.
The NH of the ammonium hydrogen carbonate4HCO3Content >=98wt%.
ρ-the Al2O3The Al of micro mist2O3Content >=98wt%.
Fe contents >=98wt% of the iron powder.
C content >=96wt% of the carbon black.
The vacuum of the vacuum drying chamber is 0.01 ~ 0.02Pa.
Due to being had the positive effect that compared with prior art using above-mentioned technical proposal, the present invention：
1st, raw material sources needed for the present invention are abundant and technique is simple, supported without special installation, and production cost is low.
2nd, the present invention reduces micropore iron using the oxidation-reduction reaction and bulk effect of raw material components to hole miniaturization
The thermal conductivity factor of aluminate raw material, while the control certainly by atmospheric condition in high temperature sintering process and adaptive, increase iron
The conversion ratio of aluminate, and then improve the sintering character of micropore hercynite raw material.
Micropore hercynite raw material prepared by the present invention is after testing：Bulk density is 2.45 ~ 2.70g/cm3；Heat conduction
Coefficient is 2.20 ~ 2.25Wm-1·K-1；The conversion ratio of hercynite is 78 ~ 83%.
Therefore, present invention process is simple and production cost is low；The sintering character of prepared micropore hercynite raw material
Get well, thermal conductivity factor is small and hercynite high conversion rate.
Embodiment
With reference to embodiment, the invention will be further described, not to the limitation of its protection domain.
In present embodiment：
Al (the H of the aluminium dihydrogen phosphate2PO4)3Content >=98wt%.
The NH of the ammonium hydrogen carbonate4HCO3Content >=98wt%.
ρ-the Al2O3The Al of micro mist2O3Content >=98wt%.
Fe contents >=98wt% of the iron powder.
C content >=96wt% of the carbon black.
The vacuum of the vacuum drying chamber is 0.01 ~ 0.02Pa.
Repeated no more in embodiment.
Embodiment 1
A kind of micropore hercynite raw material and preparation method thereof.Preparation method described in the present embodiment comprises the concrete steps that：
The first step, under 25 ~ 30 DEG C of water bath conditions, aluminium dihydrogen phosphate, ammonium hydrogen carbonate and water are inserted in container, stirring 15 ~ 20
Minute, obtain mixed solution；Wherein, aluminium dihydrogen phosphate: ammonium hydrogen carbonate: the mass ratio of water is (20 ~ 22): (2 ~ 4): 100.
Second step, by the mixed solution, ρ-Al2O3Micro mist, iron powder and carbon black mixing, stir 5 ~ 8 minutes, add mould
Middle shaping, obtain being molded compound；Wherein, the mixed solution: ρ-Al2O3Micro mist: iron powder: the mass ratio of carbon black is 10: (100
~102)∶(50~52)∶(2~4)。
3rd step, the shaping compound added in vacuum drying chamber, dried under the conditions of 110 ~ 120 DEG C 12 ~ 24 small
When, obtain dried shaping compound.
4th step, the dried shaping compound is placed in Muffle furnace, under the conditions of 1600 ~ 1620 DEG C and air
2 ~ 3 hours are incubated in atmosphere, furnace cooling, is crushed, micropore hercynite raw material is made.
Micropore hercynite raw material prepared by the present embodiment is after testing：Bulk density is 2.45 ~ 2.55g/cm3；Lead
Hot coefficient is 2.20 ~ 2.22Wm-1·K-1；The conversion ratio of hercynite is 78 ~ 80%.
Embodiment 2
A kind of micropore hercynite raw material and preparation method thereof.Preparation method described in the present embodiment comprises the concrete steps that：
The first step, under 25 ~ 30 DEG C of water bath conditions, aluminium dihydrogen phosphate, ammonium hydrogen carbonate and water are inserted in container, stirring 15 ~ 20
Minute, obtain mixed solution；Wherein, aluminium dihydrogen phosphate: ammonium hydrogen carbonate: the mass ratio of water is (21 ~ 23): (2 ~ 4): 100.
Second step, by the mixed solution, ρ-Al2O3Micro mist, iron powder and carbon black mixing, stir 5 ~ 8 minutes, add mould
Middle shaping, obtain being molded compound；Wherein, the mixed solution: ρ-Al2O3Micro mist: iron powder: the mass ratio of carbon black is 10: (101
~103)∶(51~53)∶(2~4)。
3rd step, the shaping compound added in vacuum drying chamber, dried under the conditions of 110 ~ 120 DEG C 12 ~ 24 small
When, obtain dried shaping compound.
4th step, the dried shaping compound is placed in Muffle furnace, under the conditions of 1610 ~ 1630 DEG C and air
2 ~ 3 hours are incubated in atmosphere, furnace cooling, is crushed, micropore hercynite raw material is made.
Micropore hercynite raw material prepared by the present embodiment is after testing：Bulk density is 2.50 ~ 2.60g/cm3；Lead
Hot coefficient is 2.21 ~ 2.23Wm-1·K-1；The conversion ratio of hercynite is 79 ~ 81%.
Embodiment 3
A kind of micropore hercynite raw material and preparation method thereof.Preparation method described in the present embodiment comprises the concrete steps that：
The first step, under 25 ~ 30 DEG C of water bath conditions, aluminium dihydrogen phosphate, ammonium hydrogen carbonate and water are inserted in container, stirring 15 ~ 20
Minute, obtain mixed solution；Wherein, aluminium dihydrogen phosphate: ammonium hydrogen carbonate: the mass ratio of water is (22 ~ 24): (3 ~ 5): 100.
Second step, by the mixed solution, ρ-Al2O3Micro mist, iron powder and carbon black mixing, stir 5 ~ 8 minutes, add mould
Middle shaping, obtain being molded compound；Wherein, the mixed solution: ρ-Al2O3Micro mist: iron powder: the mass ratio of carbon black is 10: (102
~104)∶(52~54)∶(3~5)。
3rd step, the shaping compound added in vacuum drying chamber, dried under the conditions of 110 ~ 120 DEG C 12 ~ 24 small
When, obtain dried shaping compound.
4th step, the dried shaping compound is placed in Muffle furnace, under the conditions of 1620 ~ 1640 DEG C and air
2 ~ 3 hours are incubated in atmosphere, furnace cooling, is crushed, micropore hercynite raw material is made.
Micropore hercynite raw material prepared by the present embodiment is after testing：Bulk density is 2.55 ~ 2.65g/cm3；Lead
Hot coefficient is 2.22 ~ 2.24Wm-1·K-1；The conversion ratio of hercynite is 80 ~ 82%.
Embodiment 4
A kind of micropore hercynite raw material and preparation method thereof.Preparation method described in the present embodiment comprises the concrete steps that：
The first step, under 25 ~ 30 DEG C of water bath conditions, aluminium dihydrogen phosphate, ammonium hydrogen carbonate and water are inserted in container, stirring 15 ~ 20
Minute, obtain mixed solution；Wherein, aluminium dihydrogen phosphate: ammonium hydrogen carbonate: the mass ratio of water is (23 ~ 25): (3 ~ 5): 100.
Second step, by the mixed solution, ρ-Al2O3Micro mist, iron powder and carbon black mixing, stir 5 ~ 8 minutes, add mould
Middle shaping, obtain being molded compound；Wherein, the mixed solution: ρ-Al2O3Micro mist: iron powder: the mass ratio of carbon black is 10: (103
~105)∶(53~55)∶(3~5)。
3rd step, the shaping compound added in vacuum drying chamber, dried under the conditions of 110 ~ 120 DEG C 12 ~ 24 small
When, obtain dried shaping compound.
4th step, the dried shaping compound is placed in Muffle furnace, under the conditions of 1630 ~ 1650 DEG C and air
2 ~ 3 hours are incubated in atmosphere, furnace cooling, is crushed, micropore hercynite raw material is made.
Micropore hercynite raw material manufactured in the present embodiment is after testing：Bulk density is 2.60 ~ 2.70g/cm3；Heat conduction
Coefficient is 2.23 ~ 2.25Wm-1·K-1；The conversion ratio of hercynite is 81 ~ 83%.
Present embodiment has the positive effect that compared with prior art：
1st, raw material sources needed for present embodiment are abundant and technique is simple, supported without special installation, and production cost is low.
2nd, present embodiment is dropped using the oxidation-reduction reaction and bulk effect of raw material components to hole miniaturization
The thermal conductivity factor of humble hole hercynite raw material, at the same by high temperature sintering process atmospheric condition from control with it is adaptive
Should, increase the conversion ratio of hercynite, and then improve the sintering character of micropore hercynite raw material.
Micropore hercynite raw material prepared by present embodiment is after testing：Bulk density is 2.45 ~ 2.70g/
cm3；Thermal conductivity factor is 2.20 ~ 2.25Wm-1·K-1；The conversion ratio of hercynite is 78 ~ 83%.
Therefore, present embodiment technique is simple and production cost is low；Prepared micropore hercynite raw material
Sintering character is good, thermal conductivity factor is small and hercynite high conversion rate.
Claims (8)
1. a kind of preparation method of micropore hercynite raw material, it is characterised in that the preparation method comprises the concrete steps that：
The first step, under 25 ~ 30 DEG C of water bath conditions, aluminium dihydrogen phosphate, ammonium hydrogen carbonate and water are inserted in container, stirring 15 ~ 20
Minute, obtain mixed solution；Wherein, aluminium dihydrogen phosphate: ammonium hydrogen carbonate: the mass ratio of water is (20 ~ 25): (2 ~ 5): 100；
Second step, by the mixed solution, ρ-Al2O3Micro mist, iron powder and carbon black mixing, stir 5 ~ 8 minutes, add mould in into
Type, obtain being molded compound；Wherein, the mixed solution: ρ-Al2O3Micro mist: iron powder: the mass ratio of carbon black is 10: (100 ~
105)∶(50~55)∶(2~5)；
3rd step, by it is described shaping compound add vacuum drying chamber in, under the conditions of 110 ~ 120 DEG C dry 12 ~ 24 hours, obtain
To dried shaping compound；
4th step, the dried shaping compound is placed in Muffle furnace, under the conditions of 1600 ~ 1650 DEG C and air atmosphere
Middle insulation 2 ~ 3 hours, furnace cooling, is crushed, and micropore hercynite raw material is made.
2. the preparation method of micropore hercynite raw material according to claim 1, it is characterised in that the biphosphate
Al (the H of aluminium2PO4)3Content >=98wt%.
3. the preparation method of micropore hercynite raw material according to claim 1, it is characterised in that the ammonium hydrogen carbonate
NH4HCO3Content >=98wt%.
4. the preparation method of micropore hercynite raw material according to claim 1, it is characterised in that the ρ-Al2O3It is micro-
The Al of powder2O3Content >=98wt%.
5. the preparation method of micropore hercynite raw material according to claim 1, it is characterised in that the Fe of the iron powder
Content >=98wt%.
6. the preparation method of micropore hercynite raw material according to claim 1, it is characterised in that the C of the carbon black contains
Amount >=96wt%.
7. the preparation method of micropore hercynite raw material according to claim 1, it is characterised in that the vacuum drying
The vacuum of case is 0.01 ~ 0.02Pa.
A kind of 8. micropore hercynite raw material, it is characterised in that the micropore hercynite raw material be according to claim 1 ~
Micropore hercynite raw material prepared by the preparation method of micropore hercynite raw material any one of 7.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115108848A (en) * | 2022-07-20 | 2022-09-27 | 浙江锦诚新材料股份有限公司 | Iron-aluminum spinel brick and preparation method thereof |
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2017
- 2017-09-25 CN CN201710876374.3A patent/CN107540370A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115108848A (en) * | 2022-07-20 | 2022-09-27 | 浙江锦诚新材料股份有限公司 | Iron-aluminum spinel brick and preparation method thereof |
| CN115108848B (en) * | 2022-07-20 | 2023-04-11 | 浙江锦诚新材料股份有限公司 | Iron-aluminum spinel brick and preparation method thereof |
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Application publication date: 20180105 |