CN102180684A - Industrially-synthesized magnesium-iron-aluminum compound spinel and synthetic method thereof - Google Patents
Industrially-synthesized magnesium-iron-aluminum compound spinel and synthetic method thereof Download PDFInfo
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- CN102180684A CN102180684A CN 201110055798 CN201110055798A CN102180684A CN 102180684 A CN102180684 A CN 102180684A CN 201110055798 CN201110055798 CN 201110055798 CN 201110055798 A CN201110055798 A CN 201110055798A CN 102180684 A CN102180684 A CN 102180684A
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- aluminium composite
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- synthetic magnesium
- iron aluminium
- composite spinelle
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Abstract
The invention relates to an industrially-synthesized magnesium-iron-aluminum compound spinel and a synthetic method thereof, belonging to the technical field of refractory materials. The compound spinel comprises the following chemical components in percentage by weight: 25-45 percent of Fe2O3, 35-55 percent of Al2O3, 0-30 percent of MgO and 0-5 percent of ZrO2. The synthetic method comprises the following steps of: preparing materials, blanking and sintering, wherein an industrial kiln is taken as a sintering kiln, and the temperature is raised freely below 600 DEG C; and transferring into a reducing atmosphere in the process of raising the temperature from 600 DEG C to 1,200 DEG C, preserving heat at the sintering temperature between 600 DEG C and 1,200 DEG C for 3-8 hours when the CO concentration is over 10,000 PPm, preserving the reducing atmosphere, lowering the temperature to 800-600 DEG C and naturally cooling to room temperature. The synthetic method is simple in synthetic process, convenient for industrial control and easy for mass production.
Description
Technical field
The present invention relates to a kind of industrialization synthetic magnesium iron aluminium composite spinelle and synthetic method, belong to technical field of refractory materials.
Background technology
The researchist of magnesium company (RHI) difficult to understand adopts electric smelting method industrialization manufacturing to synthesize high-purity hercynite, has higher production efficiency.
Adopt the nitrogen protection synthesizing ferrous aluminum spinel, can only burn till by electric furnace, small scale, efficient are low.
Report is arranged: under laboratory condition, 1550 ℃ and CO/ (CO+CO in electric furnace
2+ O
2) be under 10% the reducing atmosphere condition, can obtain the higher hercynite of synthetic ratio.But this firing atmosphere condition is actual cannot the realization in the industrial combustion kiln, because gas is removed CO, CO in the kiln
2, O
2Also has a large amount of N outward
2And H
2O gas, CO/ (CO+CO
2+ O
2) be that 10% reducing atmosphere firing condition is difficult to reach, there is greatly difficulty in the industrially scalable manufacturing.
Summary of the invention
The object of the present invention is to provide a kind of industrialization synthetic magnesium iron aluminium composite spinelle and synthetic method, synthesis technique is simple, is convenient to Industry Control, is easy to large-scale production.
Industrialization synthetic magnesium iron aluminium composite spinelle of the present invention, its chemical weight percentage composition is:
Fe
2O
3?25～45％、Al
2O
3?35～55％、MgO?0～30％、ZrO
2?0～5％。
Its XRD spectral line shows that main crystalline phase is FeOAl
2O
3, account for 85-99%; Paracrystalline phase is MgOAl
2O
3, MgOFe
2O
3Account for 1～15% and the ZrO of 0-4.7%
2, and the glassy phase of 0-2%.
Synthetic method comprises batching, base and burns till that its burning kiln is Industrial Stoves, and rapid and natural heats up before 600 ℃; 600-1200 ℃ of temperature-rise period transfers reducing atmosphere to, and CO concentration reaches more than the 10000PPm, firing temperature 1500-1600 ℃ following soaking time 3-8 hour, keep reducing atmosphere to cooling to 600-800 ℃, be cooled to room temperature naturally.
Wherein:
Batching adds the wedding agent of batching gross weight 1～6%, base through being crushed to meso-position radius below 20 microns.
Batching is a raw material with iron containing compounds, commercial alumina, magnesium-containing compound, carbon compound and zirconium-containing compound.
Commercial alumina, granularity are crossed the 0.2mm sieve.
Iron containing compounds is FeO, Fe
2O
3With a kind of or several combination arbitrarily in the roll scale, granularity is crossed the 0.2mm sieve.
Magnesium-containing compound is for being magnesite clinker among the MgO or a kind of or combination in the caustic-calcined magnesite, and granularity is crossed the 0.2mm sieve.
Add carbon compound, keep the reducing atmosphere of material internal in the sintering process, carbon compound is a kind of or several combination arbitrarily in graphite, carbon black, refinery coke, the hard coal etc., and granularity is crossed the 0.2mm sieve.
Zirconium-containing compound is zirconium silicate, zirconium white etc.
Wedding agent is a kind of or several combination arbitrarily in spent pulping liquor, starch, dextrin, resin, polyvinyl alcohol and the methylcellulose gum.
Batching is pulverized can adopt dry grinding, adopts compression moulding mode base; Or the employing wet grinding, through filter mud, mixing, vacuumize and squeeze base mode base.
Compared with prior art, the present invention has following beneficial effect:
Among the present invention, burning till and being warming up to 600 ℃ of later enforcement atmosphere is reducing atmosphere, and oxygen partial pressure is low, the Fe in the iron oxide
3+To change Fe into
2+, and then form the FeOAl of stable existence with aluminum oxide
2O
3Owing to the composition reason of raw material, remove and form FeOAl
2O
3Also may form other 2 kinds of spinel MgOAl outward
2O
3, MgOFe
2O
3Or its mixture, because the existence of above-mentioned composite spinelle, avoided iron between different valence state, to change and the volume effect that causes, avoided in the raw material free Fe and compound thereof, Al
2O
3, new chemical reaction takes place between the magnesia and the volumetric expansion that causes, product performance are stable.
Product ferro-magnesium-aluminum spinelle of the present invention is used to make the magnesia-hercynite brick of chromium-less, can satisfy the requirement of cement sectors technical development.
Technology of the present invention is simple, burns till by the direct method realization reduction of controlling the concentration of CO, is convenient to Industry Control, is easy to large-scale production.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment
Batching adopts iron cpd, commercial alumina, magnesium-containing compound, carbon compound, contains Zirconium oxide and wedding agent, whole mistake 80 mesh sieves of raw material, and batching satisfies the chemical ingredients composition requirement of product: Fe
2O
325～45%, Al
2O
335～55%, MgO0～30%, ZrO
20～5%.Wedding agent is a kind of in spent pulping liquor, starch, dextrin, resin, polyvinyl alcohol and the methylcellulose gum, tests respectively, and add-on is 1～6% of the batching gross weight, selects to add 3%, 4%, 4.5% and 6% respectively and tests.
Batching is through grinding, or dry grinding or wet-milling all can, can on 400-1200 ton pressing machine, suppress base, or it is mixing after vacuumize and squeeze mud and extrude base, 110 ℃ of dryings to add an amount of moisture content.
Industrial Stoves heat up before 600 ℃ naturally; 600-1200 ℃ of temperature-rise period transfers reducing atmosphere to, adopts respectively firing temperature 1500-1600 ℃ of following soaking time and tests in 5,6 hours, keeps reducing atmosphere to cooling to 600-800 ℃, is cooled to room temperature naturally.Grog is ferro-magnesium-aluminum spinelle, is used to make the magnesia-hercynite brick of chromium-less.
The specific embodiment parameter list
Claims (9)
1. industrialization synthetic magnesium iron aluminium composite spinelle is characterized in that its chemical weight percentage composition is:
Fe
2O
3?25～45％、Al
2O
3?35～55％、MgO?0～30％、ZrO
2?0～5％。
2. industrialization synthetic magnesium iron aluminium composite spinelle according to claim 1 is characterized in that its XRD spectral line shows that main crystalline phase is FeOAl
2O
3, account for 85-99%; Paracrystalline phase is MgOAl
2O
3, MgOFe
2O
3Account for 1～15% and the ZrO of 0-4.7%
2, and the glassy phase of 0-2%.
3. the method for the synthetic magnesium iron aluminium composite spinelle of the described industrialization of claim 1 comprises batching, base and burns till, and it is characterized in that burning kiln is Industrial Stoves, freely heats up before 600 ℃; 600-1200 ℃ of temperature-rise period transfers reducing atmosphere to, and CO concentration reaches more than the 10000PPm, firing temperature 1500-1600 ℃ following soaking time 3-8 hour, keep reducing atmosphere to cooling to 800-600 ℃, be cooled to room temperature naturally.
4. the method for the synthetic magnesium iron aluminium composite spinelle of industrialization according to claim 3 is characterized in that batching through being crushed to meso-position radius below 20 microns, adds the wedding agent of batching gross weight 1～6%, base.
5. the method for the synthetic magnesium iron aluminium composite spinelle of industrialization according to claim 3 is characterized in that batching is a raw material with iron containing compounds, commercial alumina, magnesium-containing compound, carbon compound and zirconium-containing compound.
6. the method for the synthetic magnesium iron aluminium composite spinelle of industrialization according to claim 5 is characterized in that commercial alumina, and granularity is crossed the 0.2mm sieve.
7. the method for the synthetic magnesium iron aluminium composite spinelle of industrialization according to claim 5 is characterized in that iron containing compounds is FeO, Fe
2O
3Or a kind of or several combination arbitrarily in the roll scale, granularity is crossed the 0.2mm sieve.
8. the method for the synthetic magnesium iron aluminium composite spinelle of industrialization according to claim 5 is characterized in that magnesium-containing compound is magnesite clinker among the MgO or a kind of or combination in the caustic-calcined magnesite, and granularity is crossed the 0.2mm sieve.
9. the method for the synthetic magnesium iron aluminium composite spinelle of industrialization according to claim 5 is characterized in that wedding agent is a kind of or several combination arbitrarily in spent pulping liquor, starch, dextrin, resin, polyvinyl alcohol and the methylcellulose gum.
Priority Applications (1)
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|---|---|---|---|
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|---|---|---|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102557687A (en) * | 2012-01-05 | 2012-07-11 | 武汉科技大学 | FeAl2O4-Al2O3 composite powder and method for preparing FeAl2O4-Al2O3 composite powder under reducing atmosphere |
| CN105819877A (en) * | 2014-07-16 | 2016-08-03 | 山国强 | Novel environment-friendly blast furnace stemming |
| CN106631119A (en) * | 2016-12-28 | 2017-05-10 | 河南和成无机新材料股份有限公司 | High-strength lightweight microporous spinel and preparation method thereof and high temperature resistant brick |
| CN107522485A (en) * | 2017-08-24 | 2017-12-29 | 浙江科屹耐火材料有限公司 | A kind of spinel fibre oxidation Zr refractory material and its preparation technology |
| CN108603102A (en) * | 2016-02-19 | 2018-09-28 | 尼卡石油科技有限公司 | Ceramsite propping agent and its manufacturing method |
| CN110981462A (en) * | 2019-12-30 | 2020-04-10 | 武汉科技大学 | Porous periclase-magnesium-iron-aluminum composite spinel ceramic material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101973771A (en) * | 2010-09-29 | 2011-02-16 | 淄博市鲁中耐火材料有限公司 | Ferrous aluminum and magnesium system refractory raw material and preparation method thereof |
-
2011
- 2011-03-09 CN CN 201110055798 patent/CN102180684A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101973771A (en) * | 2010-09-29 | 2011-02-16 | 淄博市鲁中耐火材料有限公司 | Ferrous aluminum and magnesium system refractory raw material and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 《武汉科技大学学报》 20090228 杨斌 原位合成方镁石-铁铝尖晶石材料的烧结工艺及性能研究 86-89 1-2 第32卷, 第1期 2 * |
| 《耐火材料》 20101031 马淑龙等 添加MgO对铁铝尖晶石合成和烧结的影响 334-337 1-9 第44卷, 第5期 2 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102557687A (en) * | 2012-01-05 | 2012-07-11 | 武汉科技大学 | FeAl2O4-Al2O3 composite powder and method for preparing FeAl2O4-Al2O3 composite powder under reducing atmosphere |
| CN105819877A (en) * | 2014-07-16 | 2016-08-03 | 山国强 | Novel environment-friendly blast furnace stemming |
| CN108603102A (en) * | 2016-02-19 | 2018-09-28 | 尼卡石油科技有限公司 | Ceramsite propping agent and its manufacturing method |
| CN106631119A (en) * | 2016-12-28 | 2017-05-10 | 河南和成无机新材料股份有限公司 | High-strength lightweight microporous spinel and preparation method thereof and high temperature resistant brick |
| CN107522485A (en) * | 2017-08-24 | 2017-12-29 | 浙江科屹耐火材料有限公司 | A kind of spinel fibre oxidation Zr refractory material and its preparation technology |
| CN107522485B (en) * | 2017-08-24 | 2020-09-01 | 马长江 | Spinel fiber reinforced zirconia refractory material and preparation process thereof |
| CN110981462A (en) * | 2019-12-30 | 2020-04-10 | 武汉科技大学 | Porous periclase-magnesium-iron-aluminum composite spinel ceramic material and preparation method thereof |
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Application publication date: 20110914 |