CN109053159A - A method of cooperate with processing magnesite to prepare high density magnesium zirconia block using microwave outfield - Google Patents
A method of cooperate with processing magnesite to prepare high density magnesium zirconia block using microwave outfield Download PDFInfo
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- CN109053159A CN109053159A CN201811018494.0A CN201811018494A CN109053159A CN 109053159 A CN109053159 A CN 109053159A CN 201811018494 A CN201811018494 A CN 201811018494A CN 109053159 A CN109053159 A CN 109053159A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/03—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
- C04B35/04—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
- C04B35/043—Refractories from grain sized mixtures
- C04B35/0435—Refractories from grain sized mixtures containing refractory metal compounds other than chromium oxide or chrome ore
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
- C04B2235/3248—Zirconates or hafnates, e.g. zircon
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
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- Manufacturing & Machinery (AREA)
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- Inorganic Compounds Of Heavy Metals (AREA)
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Abstract
The present invention is disclosed a kind of cooperateed with using microwave outfield and handles magnesite preparation high density magnesium zirconia block method, natural magnesite can be obtained into highdensity magnesium zirconia refractory after the processing of the methods of broken, multistage roasting, aquation, levigate, microwave cooperating processing and addition zircon using this method, using its bulk density of magnesium zirconia block obtained by the present invention up to 3.4g/cm3More than.And the raw materials used in the present invention is relatively inexpensive and is easy to get, and the relatively easy easy realization of production procedure can effectively reduce production cost.And any toxic or harmful substance will not be produced in production process, can effectively guarantee the green of production link and process with it is innoxious, be easy to industrial production.
Description
Technical field
The invention belongs to technical field of refractory materials, be related to it is a kind of prepared using microwave outfield collaboration processing magnesite it is highly dense
Spend the method for magnesium zirconia block.
Background technique
Magnesite has itself content of magnesium height as production one of magnesia and the essential mineral raw material of magnesium metal,
The inherent advantages such as his impurity element is relatively fewer.Currently, the various magnesium that are prepared as a raw material for production with magnisite and
Magnesium salts product has been widely used for the fields such as metallurgy, resistance to material, chemical industry, building and new material.
In terms of preparing refractory material, when directly preparing magnesia or high magnesia brick using magnesite, since magnesium carbonate is dividing
In solution preocess, the porosity of material itself can be increase accordingly, so that the bulk density of its own is corresponding to consistency to be reduced, and right
Production technology and condition require relatively high.The general high magnesia brick or magnesia, volume for directly magnesite being utilized to prepare is close
Degree does not exceed 3.2g/cm3, and the properties such as magnesia itself crystal structure also fire proofed wood prepared by single use magnesia
Expect that thermal shock performance is also relatively poor, is also easy to produce slight crack etc. in actual use, and then influence production.Therefore, at present in life
Produce in corresponding magnesia refractories often that other elements make it react production knot in sintering procedure with magnesia into its raw material
The relative complex magnesia composite refractory of structure promotes itself original anti-thermal shock and erosion-resisting characteristics, and then promotes material itself
Service life.Wherein the most representative is exactly magnesium chromium matter composite refractory.
But in magnesite-chrome brick production process, pollution of the chromium to ecological environment around inevitably will cause, and
And the thermal coefficient of MgO-CaO coating material in use is relatively large, not only will increase the heat dissipation pressure during materials'use,
Also result in the waste of its a large amount of heat.In recent years, with the new refractory material pressure of environmental protection and exploration substitution magnesite-chrome brick
It is constantly promoted, promoting relevant industries and researcher to develop as early as possible, one kind is novel, environmentally friendly, refractoriness is high and has higher
The novel refractory of heat preservation property.
Based on the above background, there are some investigators to propose and develop it is a kind of using zirconium oxide substitution chromium oxide give birth to
Produce the correlation technique of magnesium zirconia block, but it substantially passes through electric-melting magnesium and zirconium oxide analysis is pure etc. is prepared, production cost phase
To higher, production technology is relative complex, is also not suitable for large-scale industrial production and practical application.
Summary of the invention
In order to solve the above technical problems, the present invention provides it is a kind of using microwave outfield collaboration processing magnesite prepare it is highly dense
The method of magnesium zirconia block is spent, the initial material of the inventive method is natural crystal, and production technology is also relatively easy, is easily applied to
Actual magnesium zirconia block production.
The present invention provide it is a kind of using microwave outfield cooperate with processing magnesite preparation high density magnesium zirconia block method, including with
Lower step:
Step 1: magnesite and zircon being crushed and ground respectively；
Step 2: the magnesite powder for handling acquisition in step 1 being placed in Muffle furnace and is roasted, the complete of magnesium carbonate is promoted
It is complete to decompose, primary light-magnesite powder is made；
Step 3: light calcined magnesia being carried out by hydration process using aquation method, is placed in ball mill and carries out ball-milling treatment；
Step 4: the aquation mud that step 3 is obtained is sent into vacuum microwave reaction dress after being packed into clay pot or silica crucible
Set that microwave dehydration under interior vacuumized is dry and the second decomposition processing of magnesium hydroxide, vacuum microwave reaction unit it is anti-
Answering power is 3000W, and reaction time 40-60min, vacuum degree need to be in 20KPa or more, and collaboration processing weight of material is in 10Kg every time
Below；
Step 5: after product is completely cooling after the reaction in step 4, in obtained active oxidation magnesium powder and step 1
The zircon of acquisition carries out mix, and zircon additive amount is 5%-10%；
Step 6: the mixed material prepared in step 5 being pressed, while still to sample after the completion of compacting
Pressure maintaining processing is carried out, is demoulded later, sample to be fired is made；
Step 7: sample to be fired being sent into high temperature furnace and is finally fired, is taken after the completion of sample firing and cooling
Out, high density magnesium zirconia block is obtained.
In the method for the invention for cooperateing with processing magnesite preparation high density magnesium zirconia block using microwave outfield, the step
Magnesite is ground to 100 mesh in 1, and zircon is ground to 200 mesh.
In the method for the invention for cooperateing with processing magnesite preparation high density magnesium zirconia block using microwave outfield, the step
Maturing temperature in 2 is 850 DEG C, and calcining time is 2 hours.
In the method for the invention for cooperateing with processing magnesite preparation high density magnesium zirconia block using microwave outfield, the step
Ball-milling Time is 8-12 hours in 3.
In the method for the invention for cooperateing with processing magnesite preparation high density magnesium zirconia block using microwave outfield, the step
Press power generates variation according to required compacting specimen size in 6, and in the range of 15MPa-500MPa, pressure maintaining handles the time as 5-10
Minute.
In the method for the invention for cooperateing with processing magnesite preparation high density magnesium zirconia block using microwave outfield, the step
Firing temperature in 7 is 1600 DEG C, the firing time 3 hours, and with the lifting/lowering temperature of 5 DEG C/min in heating and temperature-fall period
Speed is fired.
A kind of method cooperateing with processing magnesite preparation high density magnesium zirconia block using microwave outfield of the invention at least has
Below the utility model has the advantages that
(1) the raw materials used present invention is natural minerals, it is not necessarily to any secondary synthesis product, it is relatively inexpensive and be easy to get, it is raw
The relatively easy easy realization of process is produced, production cost can be effectively reduced.
(2) compared with the additive selected by the other methods of additive added by the present invention, additive of the invention is
Natural crystal product, and any toxic or harmful substance will not be produced in production process, can effectively guarantee production link and
Process green with it is innoxious.
(3) reasons such as the present invention uses roasting, aquation, levigate and microwave drying and the modified collaboration processing mode decomposed
The activity for the magnesia that change means directly prepare magnesite is constantly promoted with granularity.Make its own physical property and chemistry
Performance is pure closer to magnesia analysis, and then promotes sample final mass.
(4) the used microwave drying of the present invention and the modified microwave cooperating treatment process decomposed are to the light-burned oxidation after aquation
Magnesium powder is handled.In early period, due to the fuel factor of microwave, so that the hydrone in microwave processing process is due to absorbing microwave
Energy and the volatilization that constantly heats up, and under the action of vacuum, evaporation and the available quick discharge of vapor to distil out,
Accelerate drying process.Dry magnesium hydrate powder is obtained after complete volatilization again because being divided the effects of non-thermal effect
Solution, finally obtains active oxidation magnesium powder, and in microwave processing process, due to the fuel factor of microwave and non-thermal effect etc. again
Influence factor is but also the connecting keys such as cluster between the self structure of finally obtained magnesium powder, macromolecular are absorbing microwave energy mistake
Occur to be broken even secondary depolymerization in journey, and then its own structure is caused to form certain defect, and it is added in mixing process
The zircon entered then carries out this filling to defect caused by it in subsequent compression moulding and high temperature sintering procedure, so that magnesia
Reacting between additive is more abundant, while consistency also relatively available promotion.
(5) using high density magnesium zirconia block prepared by the present invention, the final volume density of product is up to 3.4g/cm3
More than.
Detailed description of the invention
Fig. 1 is a kind of flow chart of method that processing magnesite preparation high density magnesium zirconia block is cooperateed with using microwave outfield.
Specific embodiment
For conciser statement implementer's method of the invention, Fig. 1 provides the present invention using at the collaboration of microwave outfield
Manage the key link techniqueflow schematic diagram of the method for magnesite preparation high density magnesium zirconia block.Preparation of the invention as described in Figure 1
The method of high density magnesium zirconia block the following steps are included:
Step 1 is broken and grinds: magnesite and zircon being crushed and ground respectively；
When it is implemented, since natural crystal granularity is relatively large, directly carry out production can seriously affect product quality with
The material firing time, therefore ore need to be subjected to simple milled processed, wherein magnesite is ground to 100 mesh, zircon grinding
To 200 mesh.
The light-burned decomposition of step 2 magnesite: the magnesite powder for handling acquisition in step 1 being placed in Muffle furnace and is roasted,
Promote the complete decomposition of magnesium carbonate, primary light-magnesite powder is made；
When it is implemented, maturing temperature is 850 DEG C, calcining time is 2 hours.
Step 3 aquation is levigate: light calcined magnesia being carried out hydration process using aquation method, is placed in ball mill and carries out ball
Mill processing；
When it is implemented, light calcined magnesia is carried out using aquation method to promote light calcined magnesia activity itself and granularity
Hydration process, and as carrying out ball-milling treatment in ball mill, so that magnesia sufficiently aquation can generate magnesium hydroxide, and
In mechanical milling process, the granularity of material also can be conducive to promote final product quality, Ball-milling Time is 8-12 hours by levigate again.
The processing of step 4 microwave cooperating: the aquation mud that step 3 is obtained is sent into very after being packed into clay pot or silica crucible
The second decomposition processing of microwave dehydration drying and magnesium hydroxide under being vacuumized in empty microwave reaction device, vacuum microwave
The reaction power of reaction unit is 3000W, reaction time 40-60min, and vacuum degree need to cooperate with every time processed material in 20KPa or more
Expect weight in 10Kg or less；
Step 5 mixing: after product cools down completely after the reaction in step 4, obtained active oxidation magnesium powder and step
The zircon obtained in rapid 1 carries out mix, and zircon additive amount is 5%-10%；
Step 6 compression moulding: the mixed material prepared in step 5 is pressed, while after the completion of compacting
Pressure maintaining processing still is carried out to sample, is demoulded later, sample to be fired is made；
When it is implemented, press power generates variation according to required compacting specimen size, in the range of 15MPa-500MPa, protect
The pressure processing time is 5-10 minutes.
Step 7 high temperature sintering: sample to be fired being sent into high temperature furnace and is finally fired, firing temperature 1600
DEG C, the firing time 3 hours, and be fired in heating and temperature-fall period with the lifting/lowering temperature speed of 5 DEG C/min, to sample
It fires and is taken out after the completion of cooling, obtain high density magnesium zirconia block.
Illustrate the implementation process of this method below by embodiment.
Embodiment 1
The selected magnesite of this implementation and zircon ingredient are distinguished shown in following Tables 1 and 2.
1 magnesite chemical component (wt/%) of table
2 zircon chemical component (wt/%) of table
Firstly, ore is ground, wherein magnesite is ground to 100 mesh, and zircon is ground to 200 mesh.Later
Ground zircon being given over to subsequent spare, magnesite is placed in Muffle furnace and is roasted, firing temperature is 850 DEG C,
Firing time 2 hours.The light-magnesite powder after roasting is subjected to aquation and ball-milling treatment 10 hours later.By sample after ball milling
After being stood, being precipitated obtained aquation mud be packed into after clay or silica crucible be sent into vacuum microwave reaction unit take out it is true
The second decomposition processing of microwave dehydration drying and magnesium hydroxide under empty, reaction power 3000W, reaction time 40min,
Vacuum degree need to be controlled in 30KPa or so.After product cools down completely after reacting, obtained active oxidation magnesium powder and zircon
Carry out mix.Its zircon additive amount is 5%.The material mixed is pressed later, is pressed into diameter 2cm
Magnesium zirconia block, press power is set as 15MPa, and carries out pressure maintaining 5min processing to sample in pressing process, is taken off later
Mould.Sample is sent directly into high temperature furnace and is fired after demoulding, firing temperature be 1600 DEG C, the firing time 3 hours, and
It is fired in heating and temperature-fall period with the lifting/lowering temperature speed of 5 DEG C/min.The taking-up after the completion of sample is fired and is cooling.
It is measured later by bulk density of the method for GB/T2999-2002 to the magnesium zirconia block after taking-up, final magnesium zirconia block
Bulk density is 3.41g/cm3。
Embodiment 2
The selected magnesite of this implementation and zircon ingredient are distinguished shown in Tables 1 and 2 as above.
Firstly, ore is ground, wherein magnesite is ground to 100 mesh, and zircon is ground to 200 mesh.Later
Ground zircon being given over to subsequent spare, magnesite is placed in Muffle furnace and is roasted, firing temperature is 850 DEG C,
Firing time 2 hours.The light-magnesite powder after roasting is subjected to aquation and ball-milling treatment 10 hours later.By sample after ball milling
After being stood, being precipitated obtained aquation mud be packed into after clay or silica crucible be sent into vacuum microwave reaction unit take out it is true
The second decomposition processing of microwave dehydration drying and magnesium hydroxide under empty, reaction power 3000W, reaction time 50min,
Vacuum degree need to be controlled in 30KPa or so.After product cools down completely after reacting, obtained active oxidation magnesium powder and zircon
Carry out mix.Its zircon additive amount is 10%.The material mixed is pressed later, is pressed into diameter
The magnesium zirconia block of 5cm, press power are set as 200MPa, and in pressing process to sample carry out pressure maintaining 8min processing, it is laggard
Row demoulding.Sample is sent directly into high temperature furnace and is fired after demoulding, firing temperature be 1600 DEG C, the firing time 3 hours, and
It is fired in heating and temperature-fall period with the lifting/lowering temperature speed of 5 DEG C/min.It is taken after the completion of sample firing and cooling
Out.It is measured later by bulk density of the method for GB/T2999-2002 to the magnesium zirconia block after taking-up, final magnesium zirconium
Brick bulk density is 3.46g/cm3。
The foregoing is merely presently preferred embodiments of the present invention, the thought being not intended to limit the invention, all of the invention
Within spirit and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (6)
1. it is a kind of using microwave outfield cooperate with processing magnesite preparation high density magnesium zirconia block method, which is characterized in that including with
Lower step:
Step 1: magnesite and zircon being crushed and ground respectively；
Step 2: the magnesite powder for handling acquisition in step 1 being placed in Muffle furnace and is roasted, dividing completely for magnesium carbonate is promoted
Primary light-magnesite powder is made in solution；
Step 3: light calcined magnesia being carried out by hydration process using aquation method, is placed in ball mill and carries out ball-milling treatment；
Step 4: the aquation mud that step 3 is obtained is sent into vacuum microwave reaction unit after being packed into clay pot or silica crucible
The second decomposition processing of microwave dehydration drying and magnesium hydroxide under being vacuumized, the reaction function of vacuum microwave reaction unit
Rate is 3000W, reaction time 40-60min, vacuum degree need in 20KPa or more, every time collaboration processing weight of material 10Kg with
Under；
Step 5: after product cools down completely after the reaction in step 4, obtained active oxidation magnesium powder is obtained with step 1
Zircon carry out mix, zircon additive amount be 5%-10%；
Step 6: the mixed material prepared in step 5 being pressed, while still sample is carried out after the completion of compacting
Pressure maintaining processing, is demoulded later, sample to be fired is made；
Step 7: sample to be fired is sent into high temperature furnace and is finally fired, the taking-up after the completion of sample is fired and is cooling,
Obtain high density magnesium zirconia block.
2. special as described in claim 1 using the method for microwave outfield collaboration processing magnesite preparation high density magnesium zirconia block
Sign is that magnesite is ground to 100 mesh in the step 1, and zircon is ground to 200 mesh.
3. special as described in claim 1 using the method for microwave outfield collaboration processing magnesite preparation high density magnesium zirconia block
Sign is that the maturing temperature in the step 2 is 850 DEG C, and calcining time is 2 hours.
4. special as described in claim 1 using the method for microwave outfield collaboration processing magnesite preparation high density magnesium zirconia block
Sign is that Ball-milling Time is 8-12 hours in the step 3.
5. special as described in claim 1 using the method for microwave outfield collaboration processing magnesite preparation high density magnesium zirconia block
Sign is that press power generates variation according to required compacting specimen size in the step 6, in the range of 15MPa-500MPa, protects
The pressure processing time is 5-10 minutes.
6. special as described in claim 1 using the method for microwave outfield collaboration processing magnesite preparation high density magnesium zirconia block
Sign is, the firing temperature in the step 7 is 1600 DEG C, the firing time 3 hours, and with 5 in heating and temperature-fall period
DEG C/the lifting/lowering temperature speed of min is fired.
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Cited By (5)
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| CN109534698A (en) * | 2019-02-01 | 2019-03-29 | 东北大学 | A method of extra light calcined magnesia is prepared using magnesite microwave activation |
| WO2020155244A1 (en) * | 2019-02-01 | 2020-08-06 | 东北大学 | Method for preparing high-density magnesia by using microwave sintering of magnesite |
| CN112341218A (en) * | 2020-11-05 | 2021-02-09 | 中民驰远实业有限公司 | Method for preparing high-performance magnesium-zirconium composite ceramic tile by spark plasma sintering |
| CN115572080A (en) * | 2022-11-09 | 2023-01-06 | 营口菱镁化工集团有限公司 | Preparation method of feed-grade magnesium oxide |
| CN115959890A (en) * | 2023-01-09 | 2023-04-14 | 营口鼎盛实业有限公司 | Preparation method of modified magnesia refractory material |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109534698A (en) * | 2019-02-01 | 2019-03-29 | 东北大学 | A method of extra light calcined magnesia is prepared using magnesite microwave activation |
| CN109534698B (en) * | 2019-02-01 | 2020-08-04 | 东北大学 | Method for preparing high-activity magnesium oxide by using magnesite through microwave activation |
| WO2020155245A1 (en) * | 2019-02-01 | 2020-08-06 | 东北大学 | Method for using magnesite microwave activation to prepare highly reactive magnesium oxide |
| WO2020155244A1 (en) * | 2019-02-01 | 2020-08-06 | 东北大学 | Method for preparing high-density magnesia by using microwave sintering of magnesite |
| CN112341218A (en) * | 2020-11-05 | 2021-02-09 | 中民驰远实业有限公司 | Method for preparing high-performance magnesium-zirconium composite ceramic tile by spark plasma sintering |
| CN112341218B (en) * | 2020-11-05 | 2022-04-12 | 中民驰远实业有限公司 | Method for preparing high-performance magnesium-zirconium composite ceramic tile by spark plasma sintering |
| CN115572080A (en) * | 2022-11-09 | 2023-01-06 | 营口菱镁化工集团有限公司 | Preparation method of feed-grade magnesium oxide |
| CN115572080B (en) * | 2022-11-09 | 2024-01-16 | 营口菱镁化工集团有限公司 | Preparation method of feed-grade magnesium oxide |
| CN115959890A (en) * | 2023-01-09 | 2023-04-14 | 营口鼎盛实业有限公司 | Preparation method of modified magnesia refractory material |
| CN115959890B (en) * | 2023-01-09 | 2023-08-25 | 营口鼎盛实业有限公司 | Preparation method of modified magnesia refractory material |
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