CN111606723A - Corundum-mullite platinum crucible protection bushing and preparation method thereof - Google Patents
Corundum-mullite platinum crucible protection bushing and preparation method thereof Download PDFInfo
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- CN111606723A CN111606723A CN202010450212.5A CN202010450212A CN111606723A CN 111606723 A CN111606723 A CN 111606723A CN 202010450212 A CN202010450212 A CN 202010450212A CN 111606723 A CN111606723 A CN 111606723A
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- mullite
- corundum
- platinum crucible
- bushing
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 229910052863 mullite Inorganic materials 0.000 title claims abstract description 63
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 230000001681 protective effect Effects 0.000 claims abstract description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 49
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 43
- 239000010431 corundum Substances 0.000 claims abstract description 43
- 239000000843 powder Substances 0.000 claims abstract description 37
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 28
- 239000000203 mixture Substances 0.000 claims abstract description 25
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 22
- 239000004568 cement Substances 0.000 claims abstract description 21
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000011159 matrix material Substances 0.000 claims abstract description 17
- 238000001723 curing Methods 0.000 claims abstract description 16
- -1 calcium titanium aluminate Chemical class 0.000 claims abstract description 14
- 150000004645 aluminates Chemical class 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000000654 additive Substances 0.000 claims abstract description 9
- 230000000996 additive effect Effects 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000005245 sintering Methods 0.000 claims abstract description 7
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000011575 calcium Substances 0.000 claims abstract description 3
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 20
- 238000005266 casting Methods 0.000 claims description 13
- 239000002253 acid Substances 0.000 claims description 12
- 239000002131 composite material Substances 0.000 claims description 11
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 7
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 7
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 230000035939 shock Effects 0.000 abstract description 5
- 238000007667 floating Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 description 29
- 239000003921 oil Substances 0.000 description 12
- 239000002245 particle Substances 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 8
- 239000011521 glass Substances 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000011819 refractory material Substances 0.000 description 2
- 239000007767 bonding agent Substances 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000011083 cement mortar Substances 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000006060 molten glass Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000005368 silicate glass Substances 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/06—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture in pot furnaces
- C03B5/08—Glass-melting pots
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
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- 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
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- 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
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
- C04B2235/3222—Aluminates other than alumino-silicates, e.g. spinel (MgAl2O4)
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- 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
- C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
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- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
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Abstract
The invention relates to a corundum mullite platinum crucible protection bushing and a preparation method thereof, wherein the protection bushing comprises aggregate, a matrix and an additive; the aggregate comprises 40-50 parts of mullite and 10-30 parts of calcium titanoaluminate hollow spheres, and the matrix comprises 10-30 parts of corundum fine powder, 5-10 parts of alpha-activated alumina micro powder and 1-5 parts of aluminate cement; the additive comprises a water reducing agent, and the water reducing agent accounts for 0.1-0.7% of the total mass of the aggregate and the matrix. When the protective lining is prepared, the method comprises the following steps of 1, uniformly mixing the calcium titanium aluminate hollow spheres, the aggregate and the additive, uniformly mixing the mixture with mullite, adding water into the mixture, and stirring until the mixture is petal-shaped to obtain a castable; step 3, adding the mixture into a mold under vibration to enable the surface to be flat without bubbles floating upward and without dense water; and 4, demolding after natural curing, drying and sintering, wherein the prepared protective lining has the characteristics of high temperature resistance, good thermal shock stability and long service life.
Description
Technical Field
The invention belongs to the technical field of refractory materials, and particularly relates to a corundum mullite platinum crucible protective bushing and a preparation method thereof.
Background
The crucible used in the development experiment of the silicate glass frit prescription at present mainly comprises a common ceramic crucible, a corundum crucible, a graphite crucible, a platinum crucible and the like, wherein the ceramic crucible is low in price but can only be used under the condition of medium and low temperature, generally is less than about 1450 ℃, and can crack after being used for a long time; the corundum crucible can be melted at high temperature, and the bearing temperature is improved by about 200 ℃ compared with that of a ceramic crucible. For glass melting work, a ceramic crucible or a corundum crucible is very easy to be co-melted with glass, a sample is not easy to take out, and the service life of the crucible is generally only once; although the graphite crucible does not react with glass basically, most of glass melting is an oxidizing atmosphere, the graphite crucible needs to be introduced with a protective atmosphere, and carbon components in the crucible can be melted into the glass after long-time melting, so that the transparency of the glass is affected; the first three kinds of crucibles can be selected as small-scale experimental research, and have large consumption and relatively low price. Compared with the first three types of crucibles, the platinum crucible has the characteristics of high melting point (1773.5 ℃), smooth surface, uniform wall thickness, easy control of temperature field, long service life and the like, so that the platinum crucible is widely used by enterprises or universities.
Although the platinum crucible is expensive, the thermal conductivity is high (71.4W/mK) and the temperature is reduced quickly, so that the viscosity of molten glass at high temperature is high, the discharging difficulty is increased, the platinum is soft and easy to deform, and the operation is not easy to operate when the platinum is used, but necessary conditions are provided for continuously melting the glass. Therefore, it is necessary to prepare a protective lining of the platinum crucible, which has the function of heat preservation and protects the platinum crucible.
The protective lining of the current platinum crucible is mainly made of mullite refractory material, and the existing mullite lining has the problems of poor thermal shock resistance, easy cracking and easy peeling, and finally short service life.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a corundum mullite platinum crucible protection bushing and a preparation method thereof, and the prepared protection bushing has the characteristics of high temperature resistance, good thermal shock stability and long service life.
The invention is realized by the following technical scheme:
a corundum mullite platinum crucible protection bushing comprises aggregate, a substrate and an additive;
the aggregate comprises 40-50 parts of mullite and 10-30 parts of calcium titanoaluminate hollow spheres by weight, and the matrix comprises 10-30 parts of corundum fine powder, 5-10 parts of alpha-activated alumina micro powder and 1-5 parts of aluminate cement;
the additive comprises a water reducing agent, and the water reducing agent accounts for 0.1-0.7% of the total mass of the aggregate and the matrix.
Preferably, the matrix further comprises not more than 5 parts of silica micropowder.
Preferably, the aluminate cement is Secar71 cement.
Preferably, the water reducing agent is a polycarboxylic acid compound water reducing agent, sodium hexametaphosphate or a mixture of the polycarboxylic acid compound water reducing agent and sodium hexametaphosphate.
A preparation method of a corundum mullite platinum crucible protection bushing is based on any one of the corundum mullite platinum crucible protection bushing and comprises the following steps,
step 1, uniformly mixing a calcium titanium aluminate hollow sphere, aggregate and an additive to obtain an initial castable;
step 2, uniformly mixing the initial castable and mullite to obtain a mixture, adding water into the mixture, and stirring until the obtained mixed system is petal-shaped to obtain a final castable;
step 3, adding the final casting material into a mold corresponding to the platinum crucible protective bushing under the vibration condition, so that the surface of the final casting material is flat, no bubbles float upwards and no dense water phenomenon exists, and a sample to be maintained is obtained;
step 4, naturally curing the sample to be cured for 20-30 h, and then demolding to obtain a preliminarily formed corundum-mullite platinum crucible protective bushing;
and 5, drying and sintering the protective bushing obtained in the step 4 to obtain the corundum mullite platinum crucible protective bushing.
Furthermore, in the step 2, water accounts for 3-5% of the total mass of the initial castable and mullite.
And 3, when the final casting material is added into the mold in the step 3, firstly brushing a layer of oil on the inner wall of the mold.
And further, in the step 5, drying the protective lining obtained in the step 4 at the temperature of 90-110 ℃ for 12-36 h.
And further, in the step 5, the protective lining obtained in the step 4 is dried and then is sintered for 1-6 hours at 1400-1650 ℃.
The corundum mullite platinum crucible protective bushing is obtained by the preparation method of the corundum mullite platinum crucible protective bushing.
Compared with the prior art, the invention has the following beneficial technical effects:
the corundum-mullite quality protection lining sleeve provided by the invention can provide a certain content of Al by designing the specific content of mullite to be 40-50% by mass2O3The introduced calcium titanium aluminate hollow sphere is an excellent refractory heat-insulating material, 10-30% by mass of the calcium titanium aluminate hollow sphere can reduce the heat conductivity of a protective lining and enhance the heat-insulating effect, the corundum fine powder is used as a matched substrate raw material and is also a main raw material, 10-30% by mass of corundum fine powder and 5-10% by mass of α -activated alumina micro powder can be filled in a gap between aggregate and the calcium titanium aluminate hollow sphere and are beneficial to improving the volume density of the castable after high-temperature calcination and solid-phase reaction, 1-5% by mass of aluminate cement is used as a bonding agent to combine the raw material components and accelerate the solidification of the castable, a water reducing agent accounts for 0.1-0.7% of the total mass of the main materials, the interface energy of the raw material component particles can be reduced, the coagulation of mullite ions can be destroyed, the fluidity of the castable is improved, the sample is easy to form during pouring, and the water consumption required by the castable can be reduced, so that the corundum fine powder and the corundum formed by the corundum have the characteristics of high-temperature resistance, high-temperature strength, the final high alumina ceramic crucible protective lining, high alumina linear strength and high platinum linear shrinkage rate, and high apparent porosity and high linear shrinkage rate of the mullite crucible, and high temperatureHas the advantages of good thermal shock stability and long service life.
Furthermore, the silicon powder with the weight not more than 5 parts can improve the volume density, and simultaneously has the function of a water reducing agent, so that the water consumption is reduced, and the fluidity of the mixture is improved.
The preparation method of the corundum-mullite protective bushing comprises the steps of uniformly mixing 40-50 parts of mullite, 10-30 parts of calcium titanium aluminate hollow spheres, 10-30 parts of corundum fine powder, 10-30 parts of alpha-active alumina micro powder, 1-5 parts of aluminate cement and a water reducing agent accounting for 0.1% -0.7% of the total mass of the raw materials, adding water to obtain a petal-shaped castable, and obtaining the corundum-mullite platinum crucible protective bushing after vibration molding, natural curing, drying and firing.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
The invention relates to a corundum mullite platinum crucible protective bushing and a preparation method thereof, wherein the corundum mullite platinum crucible protective bushing comprises the following raw materials in percentage by mass: the water reducing agent is prepared by using 40-50% of mullite (with the grain diameter of 0-5 mm), 10-30% of calcium titanium aluminate hollow spheres (with the grain diameter of 0-1 mm), 10-30% of corundum fine powder (with the grain diameter of 0-1 mm), 5-10% of alpha-activated alumina micro powder, 0-5% of silicon micro powder and 1-5% of aluminate cement as raw materials, and the added raw materials are 0.1-0.7% of the total mass of the main materials.
Wherein the aluminate cement is Secar71 cement.
The water reducing agent is one or a mixture of a polycarboxylic acid composite water reducing agent and sodium hexametaphosphate.
The preparation method of the corundum mullite platinum crucible protective lining comprises the following steps of uniformly mixing the raw materials, adding 3-5% of water by mass, uniformly stirring, casting, vibrating and forming to obtain the corundum mullite platinum crucible protective lining,
step 1, premixing the substrate,
accurately weighing the titanium-calcium aluminate hollow spheres, the fine corundum powder, the alpha-activated alumina micro powder, the silicon micro powder, the aluminate cement and the water reducing agent according to the proportion, then pouring the weighed materials into a three-dimensional mixer (without limitation on model) for mixing for 25-35 min without the requirement of sequence, and uniformly mixing for later use;
step 2, forming a casting material,
pouring mullite particles and the matrix premixed uniformly in the step 1 into a stirring pot, uniformly mixing by using a paste mixer (with unlimited model), then mixing a small amount of the materials for many times according to conditions, so that the materials are easily mixed uniformly, adding water with the mass fraction of 3% -5% of the raw materials while stirring, continuously mixing the materials until the raw materials are uniformly attached to the wall of the stirring pot, and forming the shape of a petal, wherein a low-speed gear of equipment is generally selected, the stirring speed is 135-145 rpm, the stirring time is 3-18 min, and the shape is continuously changed due to the longer time, and the stirring is stopped at the moment, so that the mixture not only has certain fluidity, but also is not easy to generate the water-tight phenomenon in the vibration forming process;
step 3, vibration molding is carried out,
placing a forming die coated with oil inside on a cement mortar vibrating table (model is not limited) for fixing, gradually adding the casting material in the step 2 into a die corresponding to the platinum crucible protective lining while vibrating, continuously vibrating after the die is filled until the surface of the casting material is flat, no air bubbles float upwards and no water sealing phenomenon exists, and then floating water in the casting material; the mould is coated with oil to facilitate demoulding, and a layer of oil is brushed, so that the oil quantity does not influence the experiment, and common oil can be used;
step 4, the natural curing is carried out,
naturally curing the protective lining sample formed by vibration in the step 3 with a mold for 20-30 h, then demolding, cleaning the mold, and oiling and curing;
and step 5, drying the mixture,
putting the protective lining sample obtained in the step 4 into a vacuum drying oven, and drying for 12-36 hours at 90-110 ℃;
and step 6, sintering the mixture,
and (4) placing the dried sample in the step (5) into a muffle furnace to be sintered at 1400-1650 ℃, heating to a target temperature, and then keeping the temperature for 1-6 h, wherein the heating rate can be set to be 2-10 ℃/min.
Example 1
Weighing and preparing the following raw materials in percentage by mass: 50 percent of mullite, 10 percent of calcium titanium aluminate hollow spheres, 30 percent of corundum fine powder, 5 percent of alpha-activated alumina micro powder and 5 percent of Secar71 cement are taken as raw materials, and a polycarboxylic acid composite water reducing agent accounting for 0.5 percent of the total mass of the raw materials is added.
The preparation method of the corundum mullite platinum crucible protective bushing specifically comprises the following steps,
step 1, premixing the substrate,
pouring the titanium calcium aluminate hollow spheres, the corundum fine powder, the alpha-activated alumina micro powder, the Secar71 cement and the polycarboxylic acid composite water reducing agent into a three-dimensional mixer (with unlimited models) to be mixed for 30min without the requirement of sequence, and uniformly mixing for later use;
step 2, forming a casting material,
pouring mullite particles and the uniformly premixed matrix into a stirring pot, uniformly mixing by using a pure slurry stirrer (the model is not limited), then stirring a small amount of mullite particles and the matrix while adding water with the mass fraction of 5% of the raw materials for continuous mixing, and stopping stirring until the raw materials are uniformly adhered to the wall of the stirring pot and are in a petal shape, wherein the mixture has certain fluidity;
step 3, vibration molding is carried out,
placing a forming die coated with oil inside on a mortar vibrating table (model is not limited) for fixing, gradually adding the uniformly mixed castable into the die (while vibrating and changing adding), and continuously vibrating after the die is filled until the surface of the castable is flat, no bubbles float upwards and no dense water phenomenon exists; the mould is oiled to facilitate demoulding, and the oil quantity does not influence the experiment;
step 4, natural curing, namely, naturally curing the protective lining sample formed by vibration for 24 hours with a mold, then demolding, cleaning the mold, and oiling and curing;
and step 5, drying the mixture,
putting the demoulded protective lining sample into a vacuum drying oven to be dried for 24 hours at the temperature of 110 ℃;
and step 6, sintering the mixture,
and (3) putting the dried sample into a muffle furnace to be sintered at 1600 ℃, heating to the target temperature, and then preserving heat for 3h, wherein the heating rate is 5 ℃/min.
Example 2
Weighing and preparing the following raw materials in percentage by mass: 50 percent of mullite, 20 percent of calcium titanium aluminate hollow spheres, 10 percent of corundum fine powder, 10 percent of alpha-activated alumina fine powder, 5 percent of silicon fine powder and 5 percent of Secar71 cement are taken as raw materials, and a polycarboxylic acid composite water reducing agent with the total mass of 0.5 percent of the raw materials is added. The preparation method is the same as that of example 1.
Example 3
Weighing and preparing the following raw materials in percentage by mass: the water reducer is prepared from 40% of mullite, 30% of calcium titanium aluminate hollow spheres, 20% of corundum fine powder, 5% of alpha-activated alumina fine powder and 5% of Secar71 cement, and is added with 0.5% of polycarboxylic acid composite water reducer based on the total mass of the raw materials. The preparation method is the same as that of example 1.
Example 4
Weighing and preparing the following raw materials in percentage by mass: the material comprises 45% of mullite, 15% of calcium titanium aluminate hollow spheres, 15% of corundum fine powder, 6% of alpha-activated alumina fine powder, 1% of silicon fine powder and 3% of Secar71 cement, and sodium hexametaphosphate accounting for 0.1% of the total mass of the material.
The preparation method of the corundum mullite platinum crucible protective bushing specifically comprises the following steps,
step 1, premixing the substrate,
pouring the titanium calcium aluminate hollow spheres, the corundum fine powder, the alpha-activated alumina micro powder, the Secar71 cement and the polycarboxylic acid composite water reducing agent into a three-dimensional mixer (with unlimited models) to be mixed for 30min without the requirement of sequence, and uniformly mixing for later use;
step 2, forming a casting material,
pouring mullite particles and the uniformly premixed matrix into a stirring pot, uniformly mixing by using a pure slurry stirrer (the model is not limited), then stirring a small amount of mullite particles and the matrix while adding water with the mass fraction of 3% of the raw materials for continuous mixing, and stopping stirring until the raw materials are uniformly adhered to the wall of the stirring pot and are in a petal shape, wherein the mixture has certain fluidity;
step 3, vibration molding is carried out,
placing a forming die coated with oil inside on a mortar vibrating table (model is not limited) for fixing, gradually adding the uniformly mixed castable into the die (while vibrating and changing adding), and continuously vibrating after the die is filled until the surface of the castable is flat, no bubbles float upwards and no dense water phenomenon exists; the mould is oiled to facilitate demoulding, and the oil quantity does not influence the experiment;
step 4, natural curing, namely, naturally curing the protective lining sample formed by vibration for 20 hours with a mold, then demolding, cleaning the mold, and oiling and curing;
and step 5, drying the mixture,
putting the demoulded protective lining sample into a vacuum drying oven to be dried for 36 hours at the temperature of 90 ℃;
and step 6, sintering the mixture,
and (3) placing the dried sample into a muffle furnace to be sintered at 1400 ℃, heating to a target temperature, and then preserving heat for 6h, wherein the heating rate is 10 ℃/min.
Example 5
Weighing and preparing the following raw materials in percentage by mass: the composite water reducing agent is prepared from 48% of mullite, 25% of calcium titanium aluminate hollow spheres, 25% of corundum fine powder, 8% of alpha-activated alumina micro powder, 3% of silicon micro powder and 1% of Secar71 cement, and a mixture of 0.7% of total mass of raw materials of a polycarboxylic acid composite water reducing agent and sodium hexametaphosphate in a ratio of 1: 1.
The preparation method of the corundum mullite platinum crucible protective bushing specifically comprises the following steps,
step 1, premixing the substrate,
pouring the titanium calcium aluminate hollow spheres, the corundum fine powder, the alpha-activated alumina micro powder, the Secar71 cement and the polycarboxylic acid composite water reducing agent into a three-dimensional mixer (with unlimited models) to be mixed for 30min without the requirement of sequence, and uniformly mixing for later use;
step 2, forming a casting material,
pouring mullite particles and the uniformly premixed matrix into a stirring pot, uniformly mixing by using a pure slurry stirrer (the model is not limited), then stirring a small amount of mullite particles and the matrix while adding water with the mass fraction of 4% of the raw materials for continuous mixing, and stopping stirring until the raw materials are uniformly adhered to the wall of the stirring pot to form a petal shape, wherein the mixture has certain fluidity;
step 3, vibration molding is carried out,
placing a forming die coated with oil inside on a mortar vibrating table (model is not limited) for fixing, gradually adding the uniformly mixed castable into the die (while vibrating and changing adding), and continuously vibrating after the die is filled until the surface of the castable is flat, no bubbles float upwards and no dense water phenomenon exists; the mould is oiled to facilitate demoulding, and the oil quantity does not influence the experiment;
step 4, natural curing, namely, naturally curing the protective lining sample formed by vibration for 30 hours with a mold, then demolding, cleaning the mold, and oiling and curing;
and step 5, drying the mixture,
putting the demoulded protective lining sample into a vacuum drying oven to be dried for 12 hours at the temperature of 100 ℃;
and step 6, sintering the mixture,
and (3) putting the dried sample into a muffle furnace to be sintered at 1650 ℃, heating to the target temperature, and then preserving heat for 1h at the heating rate of 2 ℃/min.
The properties of the crucibles obtained in examples 1 to 3 are shown in Table 1.
TABLE 1 Properties of crucible bushing obtained in example
Based on four groups of data of volume density, apparent porosity, linear shrinkage and compressive strength, the thermal shock resistance of the crucible protective bushing can be improved by using the raw material particle grading and forming mode specially used by the invention, and finally, the crucible protective bushing is prevented from being easy to crack and peel, so that the effect of prolonging the service life of the protective bushing is achieved.
Claims (10)
1. A corundum-mullite platinum crucible protection bushing is characterized by comprising aggregate, a matrix and an additive;
the aggregate comprises 40-50 parts of mullite and 10-30 parts of calcium titanoaluminate hollow spheres by weight, and the matrix comprises 10-30 parts of corundum fine powder, 5-10 parts of alpha-activated alumina micro powder and 1-5 parts of aluminate cement;
the additive comprises a water reducing agent, and the water reducing agent accounts for 0.1-0.7% of the total mass of the aggregate and the matrix.
2. The corundum-mullite platinum crucible protective sleeve as claimed in claim 1, wherein said matrix further comprises not more than 5 parts of silica micropowder.
3. The corundum-mullite platinum crucible protective bushing as claimed in claim 1, wherein said aluminate cement is Secar71 cement.
4. The corundum-mullite platinum crucible protective bushing as claimed in claim 1, wherein the water reducing agent is a polycarboxylic acid composite water reducing agent, sodium hexametaphosphate or a mixture of the polycarboxylic acid composite water reducing agent and sodium hexametaphosphate.
5. A method for preparing a corundum mullite platinum crucible protection bushing, which is characterized in that the corundum mullite platinum crucible protection bushing based on any one of claims 1-4 comprises the following steps,
step 1, uniformly mixing a calcium titanium aluminate hollow sphere, aggregate and an additive to obtain an initial castable;
step 2, uniformly mixing the initial castable and mullite to obtain a mixture, adding water into the mixture, and stirring until the obtained mixed system is petal-shaped to obtain a final castable;
step 3, adding the final casting material into a mold corresponding to the platinum crucible protective bushing under the vibration condition, so that the surface of the final casting material is flat, no bubbles float upwards and no dense water phenomenon exists, and a sample to be maintained is obtained;
step 4, naturally curing the sample to be cured for 20-30 h, and then demolding to obtain a preliminarily formed corundum-mullite platinum crucible protective bushing;
and 5, drying and sintering the protective bushing obtained in the step 4 to obtain the corundum mullite platinum crucible protective bushing.
6. The method for preparing a corundum-mullite platinum crucible protective bushing as claimed in claim 5, wherein in step 2, water accounts for 3% -5% of the total mass of the initial castable and mullite.
7. The method for preparing a corundum-mullite platinum crucible protective bushing as claimed in claim 5, wherein in step 3, when the final castable is added into the mold, a layer of oil is brushed on the inner wall of the mold.
8. The method for preparing a corundum-mullite platinum crucible protective bushing according to claim 5, wherein in the step 5, the protective bushing obtained in the step 4 is dried at 90-110 ℃ for 12-36 h.
9. The method for preparing the corundum-mullite platinum crucible protective bushing according to claim 5, wherein in the step 5, the protective bushing obtained in the step 4 is dried and then is fired at 1400-1650 ℃ for 1-6 h.
10. The corundum mullite platinum crucible protective bushing obtained by the preparation method of the corundum mullite platinum crucible protective bushing as claimed in any one of claims 5 to 9.
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| CN101955364A (en) * | 2010-10-21 | 2011-01-26 | 淄博鲁铭高温材料科技有限公司 | Method for producing corundum-mullite sagger |
| CN107382328A (en) * | 2017-06-06 | 2017-11-24 | 浙江德清炜烨新材料有限公司 | A kind of corundum-mullite castable and preparation method thereof |
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| CN108774071A (en) * | 2018-06-21 | 2018-11-09 | 华北理工大学 | A kind of air pipe of blast furnace castable and preparation method thereof |
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| CN101955364A (en) * | 2010-10-21 | 2011-01-26 | 淄博鲁铭高温材料科技有限公司 | Method for producing corundum-mullite sagger |
| CN108610063A (en) * | 2016-12-09 | 2018-10-02 | 宝山钢铁股份有限公司 | High-performance mullite thermal insulation fire-resistant pouring material |
| CN107382328A (en) * | 2017-06-06 | 2017-11-24 | 浙江德清炜烨新材料有限公司 | A kind of corundum-mullite castable and preparation method thereof |
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