CN108483993A - A kind of preparation method of the fire retardant man-made stone containing magnesium aluminate spinel - Google Patents
A kind of preparation method of the fire retardant man-made stone containing magnesium aluminate spinel Download PDFInfo
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- CN108483993A CN108483993A CN201810325700.6A CN201810325700A CN108483993A CN 108483993 A CN108483993 A CN 108483993A CN 201810325700 A CN201810325700 A CN 201810325700A CN 108483993 A CN108483993 A CN 108483993A
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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
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/10—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B26/12—Condensation polymers of aldehydes or ketones
- C04B26/122—Phenol-formaldehyde condensation polymers
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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
- C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
- C04B22/0093—Aluminates
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00017—Aspects relating to the protection of the environment
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/28—Fire resistance, i.e. materials resistant to accidental fires or high temperatures
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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
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
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- Chemical & Material Sciences (AREA)
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- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
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Abstract
The preparation method of the present invention relates to a kind of fire retardant man-made stone containing magnesium aluminate spinel, the nano magnalium spinelle MgAl2O4With special structure, good inorganic nanometer oxide material can be used as, it is added in talcum powder/phenolic resin/quartz, improve the heat resistance and intensity of artificial stone, the ageing time for reducing artificial stone can keep non-degradable for a long time under high temperature action, and can also keep preferable flame retardant effect, increase carbon left, greatly improves LOI loss on ignition indexes.
Description
Technical field
The present invention relates to a kind of preparation methods of the fire retardant man-made stone comprising nano magnalium spinelle, belong to construction material neck
Domain.
Background technology
With the promotion of people's living standard, the improvement of living conditions, interior decoration industry is grown rapidly, decoration material
Dosage is very big, wherein stone material be it is a kind of most generally use, one of most basic building materials are widely used in ground, metope and table top
Mat formation.Lithotome cost of winning is high, pollution is big, and contains a large amount of naturally occurring radioactive substances, to human health damage compared with
Greatly.With the continuous development of Material Field, the performance of artificial stone material is gradually improved, close to be even more than lithotome,
Increasingly received by market and user, is widely used in cabinet, bathroom, ground, wall decoration.But current artificial stone
Material still has that intensity is low, abrasion-resistant surface is poor, flame-proof heat-resistant performance is not strong, the disadvantage of surface gloss difference.
Invention content
For many deficiencies existing for existing artificial stone, the present invention provides a kind of fire retardant man-made stone containing magnesium aluminate spinel
Preparation method, be prepared in accordance with the following steps:
(1)Prepare compound magnesium aluminate spinel MgAl2O4;
(2)By 70-90 parts of talcum powder, 50-60 parts of phenolic resin, 6-10 parts of boron trifluoride, 10-20 parts of white carbon, crushed crude pearlite
25-30 parts last, 5-15 parts of melamine, 5-15 parts of triethyl phosphate, 5-15 parts of hydroxyapatite, 5-15 parts of mica sheet, quartz
50-70 parts, 5-10 parts of molecular sieve SBA-15 and step(1)Obtained MgAl2O4 10-20 parts of mixing, pour into homogenizer,
It first uses 1000 revs/min of speed to stir at room temperature 30 minutes, is then stirred with 3000 revs/min of speed at 50 DEG C
The batch mixing stirred evenly is discharged, is uniformly taped against on making sheet mold by 30min, and then making sheet mold is placed in vacuum environment and is done
Dry curing molding, the artificial stone blank being removed from the molds after solidification carries out fixed thick, polishing to blank, polishing treatment is hindered
Fire artificial stone.
Wherein, the step(1)Middle MgAl2O4Preparation method be:0.02molMg (NO are weighed respectively3)2· 6H2O、
0.04molAl(NO3)3 9H2O is dissolved in 50ml deionization oedema, matches to obtain mixing salt solution, takes 0.04molNa2CO3、
0.06molNaOH is dissolved in 50ml deionized waters, and then quickly stirring, is added aqueous slkali by salting liquid, pH is made to be maintained at 9-11,
It is uniformly mixed, precipitation is filtered, deionized water is washed till neutrality, 8-10h is dried in 80-100 DEG C of baking oven, then at 800-1000 DEG C
Muffle kiln roasting 4-6h.
Wherein, the preparation process of the SBA-15 molecular sieves is:Under conditions of 35-40 DEG C, by three block surface-active
Agent P123 is dissolved in appropriate amount of deionized water, and ethyl orthosilicate (TEOS), hydrochloric acid (HCl) are added thereto, stirs to continuing vigorous
For 24 hours, it is packed into 100-180 DEG C of crystallization in polytetrafluoroethylene (PTFE) bottle for 24 hours, to be filtered, washed and dried, 5-8h is finally calcined at 550 DEG C, so
After be filtered, washed and dried, obtained white powder is SBA-15, and the molar ratio of each raw material is about TEOS:P123:HCl:
H2O=1:0.017:5.88:136.
Wherein, step(2)Middle dry solidification forming temperature is 50-65 DEG C, preferably 55-60 DEG C.
Wherein, magnesium aluminate spinel average grain diameter is 20-65nm, preferably 25-45nm.
Beneficial effects of the present invention:
Phosphorus and phosphorus-containing compound fire retardant are listed as three big flame-retardant systems with halogen system, inorganic system.Triethyl phosphate, hydroxyapatite
The flame retardant effect of equal phosphorus series compounds is preferable, because the metaphosphoric acid generated when burning can be grouped to stable poly state, becomes combustion
The protective layer for burning point, can completely cut off the contact by combustion things with oxygen.The phosphoric acid and poly-metaphosphoric acid of generation are all then strong acid, are had very strong
Dehydration property, polymer dehydration carbonization can be made, and charring layer is formed in polymer surfaces, reach starvation and prevent burning
Purpose.
Melamine has the advantages that Halogen, low toxicity, low cigarette, and nitrogenous flame ratardant is preferable in the flame retardant effect of polyester plastics,
It is especially combined with phosphorus flame retardant, Intumscent Flame Retardant System can be formed, by the synergistic effect of the two, can be greatly improved
The flame retardant effect of polyalkenylesters hydrocarbon artificial stone.The application uses melamine and is applied in combination with triethyl phosphate, hydroxyapatite,
And the ratio of three is adjusted, so that three is played synergistic effect, forms Intumscent Flame Retardant System, experiments have shown that, three(Melamine
Amine:Triethyl phosphate:Hydroxyapatite)Best mass ratio is 1:1:1, flame retardant effect can be greatly improved.Nano inorganic oxygen
Compound is the good selection of fire retardant, such as nano magnesia, and nano zine oxide etc. all can serve as nano inorganic oxide resistance
Combustion agent is added in polyene ester material.Due to nano effect, Preparing Organic-inorganic Nano Hybrid Material have more conventional polymer/
Filler compound is incomparable a little, for example density is small, high mechanical strength, inspiratory and permeability, especially heat-resisting
Property and anti-flammability can be greatly improved.Further, some scholars study the clays class laminar silicic acids such as concave convex rod, montmorillonite
The flame retardant property of salt nanocomposite, above-mentioned inorganic material have different degrees of flame retardant effect.Perovskite structure oxide
ABO3 has unique optics, electricity and magnetic performance, is widely used in terms of biological agent ceramics, has thermal stability
It is good, at low cost, absorption oxygen can be carried out according to B selections, A, B atom, which can be mentioned, adjusts Lattice Oxygen quantity and activity.Mesh
It is preceding that resistance is used as using the more excellent nano-perovskite material of structure or similar polymetallic metal composite oxide not yet
Combustible material.
The aerial burning of high-molecular compound is a kind of very fierce oxidation reaction, belongs to chain reaction course.
It is proliferated a large amount of active hydroxyl free radicals in combustion process, when hydroxyl free radical and high-molecular compound meet, generates hydrocarbon
Compound free radical and water, in the presence of oxygen, hydrocarbon radical decomposition, and form new hydroxyl free radical.So
Cycle, makes combustion reaction constantly continue.The mechanism of action of fire retardant is more complicated, including many factors, but mainly by adopting
Burn cycle is prevented with either physically or chemically.
The present invention uses magnesium aluminate spinel as inorganic nano flame retardant constituent for the first time, by itself and molecular sieve SBA-15 and point
Polyene material is added in spar together, is mixed to form fire-retardant compounding agent, moreover it is possible to which the intensity for further increasing complex material compensates for point
The defect of flexible difference, forms hard and soft complementation in son sieve material, and inorganic material is carried out skeletonizing or intercalation, forms spatial stability
Structure controls the migration rate of space charge, improves charge movement rate, is conducive to capture or detrapping, avoids charge
Polymerization improves flame retardant property to avoid making the artificial stone materials such as its aging, the inflammable usually problem, increases intensity, increases
Add carbon left, it is ageing-resistant to improve LOI indexes.
The artificial stone of the present invention due to using dimension stone of magnesia alumina spinel for the first time, using its advantage space structure, and and SBA-
15 molecular sieves are compound, and a part can generate more inorganic nano flame-retardant composition, remove from and be individually added into inorganic nano magnesia
Equal inorganic anti-flaming materials, another part can utilize the skeleton structure of space omission and SBA-15 molecular sieves, optimize polymeric material
The carbon-forming performance of material improves LOI indexes, and the organic backbone in SBA-15 molecular sieves can be further multiple with polyene material
It closes, is conducive to comprehensive covering of fire proofing, greatly improves flame retardant property.Aging can be substantially reduced, the resistance to of artificial stone is improved
High temperature, use intensity and resistance to flame retardant property.
The application has studied including composite material MgAl2O4With molecular sieve SBA-15 to the fire-retardant and power of quartzy composite material
Performance is learned, by thering are limited oxygen index, vertical combustion and mechanical property tests to measure, it is known that composite material combination property is excellent, property
Energy stabilization, oxygen index (OI) height, good flame retardation effect, effect are lasting, cheap;It is non-toxic by non-volatile, smog is small, the compound resistance
Combustible material has fire-retardant, suppression cigarette and the function of reducing toxic gas concurrently, and being a kind of non-environmental-pollution fire proofing has commercial Application
Foreground.
Specific implementation mode
The present invention will be further described in detail with reference to the specific embodiments.
Embodiment 1
(1)Prepare compound magnesium aluminate spinel MgAl2O4:
(a)MgAl2O4It prepares:0.02molMg (NO are weighed respectively3)2· 6H2O、0.04molAl(NO3)3 ·9H2O is dissolved in
50ml deionization oedema matches to obtain mixing salt solution, 0.04molNa2CO3,0.06molNaOH is taken to be dissolved in 50ml deionized waters,
Then quickly stirring, is added aqueous slkali by salting liquid, PH is made to be maintained at 9-11, is uniformly mixed, and precipitation is filtered, deionization washing
To neutrality.8h is dried in 80 DEG C of baking ovens.Then in 800 DEG C of Muffle kiln roasting 4-6h.
(b) prepared by SBA-15:Under conditions of 40 DEG C, three block surfactant P123 is dissolved in appropriate amount of deionized water,
Ethyl orthosilicate (TEOS), hydrochloric acid (HCl) are added thereto, stirs to continuing vigorous for 24 hours, is packed into 120 in polytetrafluoroethylene (PTFE) bottle
DEG C crystallization for 24 hours, is filtered, washed and dried, and 6h is finally calcined at 550 DEG C, is then filtered, washed and dried, obtained white powder
End is SBA-15, spare;
(2)By 70 parts of talcum powder, 50 parts of phenolic resin, 6 parts of boron trifluoride, 10 parts of white carbon, 25 parts of perlite powder, trimerization
5 parts of cyanamide, 5 parts of triethyl phosphate, 5 parts of hydroxyapatite, 5 parts of mica sheet, 50 parts of quartz, 5 parts of molecular sieve SBA-15 and above-mentioned
The MgAl that step obtains2O4 10 parts of mixing, pour into homogenizer, first use 1000 revs/min of speed stirring 30 at room temperature
Minute, 30min is then stirred with 3000 revs/min of speed at 50 DEG C, the batch mixing stirred evenly is discharged, making sheet is uniformly taped against
On mold, making sheet mold is then placed in vacuum environment the dry solidification at 50 DEG C and is molded, after being removed from the molds solidification
Artificial stone blank carries out fixed thick, polishing to blank, polishing treatment obtains fire retardant man-made stone.
Embodiment 2
(1)Prepare compound magnesium aluminate spinel MgAl2O4:
(a)MgAl2O4It prepares:Weigh respectively 0.02molMg (NO3) 2 6H2O, 0.04molAl (NO3) 3 9H2O be dissolved in 50ml
Deionization oedema matches to obtain mixing salt solution, takes 0.04molNa2CO3,0.06molNaOH to be dissolved in 50ml deionized waters, then
Quickly stirring, is added aqueous slkali by salting liquid, PH is made to be maintained at 9-11, is uniformly mixed, and precipitation is filtered, during deionized water is washed till
Property.10h is dried in 100 DEG C of baking ovens.Then in 800 DEG C of Muffle kiln roasting 4h.
(b) prepared by SBA-15:Under conditions of 40 DEG C, three block surfactant P123 is dissolved in appropriate amount of deionized water,
Ethyl orthosilicate (TEOS), hydrochloric acid (HCl) are added thereto, stirs to continuing vigorous for 24 hours, is packed into 120 in polytetrafluoroethylene (PTFE) bottle
DEG C crystallization for 24 hours, is filtered, washed and dried, and 6h is finally calcined at 550 DEG C, is then filtered, washed and dried, obtained white powder
End is SBA-15, spare;
(2)By 80 parts of talcum powder, 55 parts of phenolic resin, 8 parts of boron trifluoride, 15 parts of white carbon, 28 parts of perlite powder, trimerization
10 parts of cyanamide, 10 parts of triethyl phosphate, 10 parts of hydroxyapatite, 10 parts of mica sheet, quartz 60 parts, 8 parts of molecular sieve SBA-15 and
The MgAl that above-mentioned steps obtain2O415 parts of mixing, pour into homogenizer, first 1000 revs/min of speed are used to stir at room temperature
It mixes 30 minutes, 30min is then stirred with 3000 revs/min of speed at 50 DEG C, the batch mixing stirred evenly is discharged, is uniformly taped against
On making sheet mold, then making sheet mold is placed in vacuum environment and is molded in 60 DEG C of dry solidifications, after being removed from the molds solidification
Artificial stone blank, fixed thick, polishing is carried out to blank, polishing treatment obtains fire retardant man-made stone.
Embodiment 3
(1)Prepare compound magnesium aluminate spinel MgAl2O4;
(a)MgAl2O4It prepares:0.02molMg (NO3) is weighed respectively2 6H2O、0.04molAl(NO3) 3 9H2O are dissolved in 50ml and go
Ion oedema matches to obtain mixing salt solution, takes 0.04molNa2CO3,0.06molNaOH to be dissolved in 50ml deionized waters, then soon
Speed stirring, is added aqueous slkali by salting liquid, PH is made to be maintained at 9-11, is uniformly mixed, and precipitation is filtered, during deionized water is washed till
Property.10h is dried in 80 DEG C of baking ovens.Then in 800 DEG C of Muffle kiln roasting 6h.
(b) prepared by SBA-15:Under conditions of 40 DEG C, three block surfactant P123 is dissolved in appropriate amount of deionized water,
Ethyl orthosilicate (TEOS), hydrochloric acid (HCl) are added thereto, stirs to continuing vigorous for 24 hours, is packed into 120 in polytetrafluoroethylene (PTFE) bottle
DEG C crystallization for 24 hours, is filtered, washed and dried, and 6h is finally calcined at 550 DEG C, is then filtered, washed and dried, obtained white powder
End is SBA-15, spare;
(2)By 90 parts of talcum powder, 60 parts of phenolic resin, 10 parts of boron trifluoride, 20 parts of white carbon, 30 parts of perlite powder, trimerization
15 parts of cyanamide, 15 parts of triethyl phosphate, 15 parts of hydroxyapatite, 15 parts of mica sheet, quartzy 70 parts, 10 parts of molecular sieve SBA-15
The MgAl obtained with above-mentioned steps2O420 parts of mixing, pour into homogenizer, first use 1000 revs/min of speed at room temperature
Then stirring 30 minutes stirs 30min at 50 DEG C with 3000 revs/min of speed, the batch mixing stirred evenly is discharged, and uniformly spreads
Onto making sheet mold, then making sheet mold is placed in vacuum environment and is molded in 65 DEG C of dry solidifications, solidification is removed from the molds
Artificial stone blank afterwards carries out fixed thick, polishing to blank, polishing treatment obtains fire retardant man-made stone.
Comparative example 1
It is added without nano magnalium spinelle, other experiment parameters are the same as embodiment 1.
Comparative example 2
SBA-15 materials are added without, other experiment parameters are the same as embodiment 1.
Comparative example 3
The magnesium aluminate spinel of the present invention is replaced using concave convex rod, other experiment parameters are the same as embodiment 1.
Comparative example 4
The SBA-15 for replacing the present invention is sieved using common molecular, other experiment parameters are the same as embodiment 1.
Specific detection
Detect the tensile strength (σ t/MPa) of above-mentioned anti-aging artificial stone, elongation at break (δ/ %), carbon left, hardness, LOI refer to
Then above-mentioned anti-aging artificial stone is carried out hot air aging by number all over the world by 250 DEG C × 30, then detect tensile strength and keep
Rate (E1/ %) and elongation at break conservation rate (E2/ %), concrete outcome is shown in Table 1.
The each Testing index of 1 artificial stone of table
Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | |
Carbon left, wt% | 18.6 | 196 | 20.1 | 1.19 | 2.1 | 4.4 | 1.5 |
Hardness, ShoreA | 96 | 95 | 95 | 84 | 75 | 76 | 72 |
Tensile strength, MPa | 52 | 50 | 48 | 45 | 35 | 46 | 43 |
Elongation at break % | 550 | 521 | 500 | 380 | 395 | 420 | 405 |
LOI | 39.3 | 37.5 | 39.0 | 19.1 | 20.1 | 25.1 | 27.4 |
250 DEG C × 30 days, LOI | 33.8 | 34.1 | 33.5 | 14.3 | 11.2 | 10.5 | 12.7 |
250 DEG C × 30 days, E1/ % | 97.4 | 95.3 | 97.6 | 77.5 | 72.5 | 73.6 | 80.3 |
250 DEG C × 30 days, E2/ % | 90.7 | 90.5 | 94.0 | 62.9 | 61.9 | 62.5 | 70.4 |
There are the above results to can be seen that by the way that magnesium aluminate spinel and molecular sieve SBA-15 is added, advantageously reduces insulating materials
The density of LDPE/EVA/PVC systems improves the heat resistance and intensity of insulating materials, reduces the ageing time of insulating materials, improves
LOI indexes have good anti-flammability, improve carbon left, can keep under high temperature action for a long time(250 DEG C × 30 days)It does not drop
Solution, and by for a long time(250 DEG C × 30 days)Still have higher LOI indexes, flame retardant property still preferable.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those skilled in the art within the technical scope disclosed by the invention, can without the variation that creative work is expected or
It replaces, should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be limited with claims
Subject to fixed protection domain.
Claims (3)
1. a kind of preparation method of the fire retardant man-made stone containing magnesium aluminate spinel, which is characterized in that be prepared in accordance with the following steps:
(1)Prepare compound magnesium aluminate spinel MgAl2O4, magnesium aluminate spinel average grain diameter is about 20-65nm;
(2)By 70-90 parts of talcum powder, 50-60 parts of phenolic resin, 6-10 parts of boron trifluoride, 10-20 parts of white carbon, crushed crude pearlite
25-30 parts last, 5-15 parts of melamine, 5-15 parts of triethyl phosphate, 5-15 parts of hydroxyapatite, 5-15 parts of mica sheet, quartz
50-70 parts, 5-10 parts of molecular sieve SBA-15 and step(1)Obtained MgAl2O4 10-20 parts of mixing, pour into homogenizer,
It first uses 1000 revs/min of speed to stir at room temperature 30 minutes, is then stirred with 3000 revs/min of speed at 50 DEG C
The batch mixing stirred evenly is discharged, is uniformly taped against on making sheet mold by 30min, and then making sheet mold is placed in vacuum environment and is done
Dry curing molding, the artificial stone blank being removed from the molds after solidification carries out fixed thick, polishing to blank, polishing treatment is hindered
Fire artificial stone;
The step(1)Middle MgAl2O4Preparation method be:0.02mol Mg (NO are weighed respectively3)2· 6H2O、0.04mol Al
(NO3)3· 9H2O is dissolved in 50ml deionized waters, is matched to obtain mixing salt solution, is taken 0.04mol Na2CO3, 0.06mol NaOH it is molten
In 50ml deionized waters, then quickly stirring, is added aqueous slkali by salting liquid, pH is made to be maintained at 9-11, is uniformly mixed, will sink
It forms sediment and filters, deionized water is washed till neutrality, 8-10h is dried in 80-100 DEG C of baking oven, then in 800-1000 DEG C of Muffle kiln roasting
4-6h。
2. preparation method as claimed in claim 1 or 2, which is characterized in that step(2)Middle dry solidification forming temperature is 50-
65℃。
3. preparation method as claimed in claim 1 or 2, which is characterized in that step(2)Middle dry solidification forming temperature is 55-
60℃。
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CN106007480B (en) | 2018-08-07 |
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