CN102584262B - Pyrophyllite non-sticky to aluminum and preparation method of pyrophyllite - Google Patents
Pyrophyllite non-sticky to aluminum and preparation method of pyrophyllite Download PDFInfo
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- CN102584262B CN102584262B CN201210006806.2A CN201210006806A CN102584262B CN 102584262 B CN102584262 B CN 102584262B CN 201210006806 A CN201210006806 A CN 201210006806A CN 102584262 B CN102584262 B CN 102584262B
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Abstract
The invention discloses a pyrophyllite non-sticky to aluminum and a preparation method of the pyrophyllite. The preparation method of the pyrophyllite comprises the steps of: preparing a fluorine-containing compound water solution, a calcium-containing compound water solution, a calcium fluoride sol and a calcium fluoride powder body slurry; preparing a sulfate radical-containing compound water solution, a barium-containing compound water solution, a barium sulfate sol and a barium sulfate powder body slurry; preparing a titanium-aluminum compound sol and an aluminum titanate powder body slurry; and respectively carrying out surface coating and heat treatment on the pyrophyllite, and enabling the surface of the pyrophyllite to be coated with a layer of calcium fluoride, barium sulfate or aluminum titanate or 2-3 layers of two or three of the calcium fluoride, the barium sulfate and the aluminum titanate. As the calcium fluoride, the barium sulfate and the aluminum titanate are non-infiltrative to the aluminum, the treated pyrophyllite is non-infiltrative to the aluminum. While the calcium fluoride, the barium sulfate and the aluminum titanate enter in cracks and holes of the pyrophyllite, and the cracks and the holes can be repaired after the calcium fluoride, the barium sulfate and the aluminum titanate are sintered at a high temperature, so that the compression strength of the pyrophyllite is enhanced.
Description
Technical field
The present invention relates to a kind of fire resisting material particle and preparation method thereof, especially relate to a kind of aluminium pyrophyllite and preparation method thereof of not being stained with.
Background technology
Along with the rapid growth of China to the non-ferrous metal demand, coloured smelting factory is constantly adopted new technology and new technology, make the maximization of non-ferrous metallurgical furnace and high efficiency to adapt to requirements of the times, this just makes the working conditions of refractory materials more and more harsh, refractory materials has been proposed to many new requirements, selecting of refractory materials becomes one of key link in production, and in Non Ferrous Melting Furnace, the molten metal contact site all adopts fine and close high quality refractory materials.
Take the metallurgy of aluminium as example, and molten aluminium stove adopts the starting material such as fine and close pyrophyllite commonly used, fused alumina, sintered alumina, and the permeability-reducing admixtures such as external carbon SiClx, aluminium titanates, Calcium Fluoride (Fluorspan), barium sulfate are not only with high costs, and thermal conductivity is high, serious heat loss; If adopt lightweight material and low-cost high silicon raw material are prone to aluminising or react with aluminum melt, it is required that performance is difficult to meet production.If the Calcium Fluoride (Fluorspan) such as the anti-aluminum solutions infiltration of these raw material surface coating one decks or reaction, barium sulfate, aluminium titanates, just can address these problems well.Gently introduce the matter aggregate in this external nonferrous metallurgy as furnace charge, but decrease goods thermal conductivity reduces energy consumption, be conducive to carry out national energy-saving and reduce discharging Major Strategic, and can increase substantially the goods thermal shock performance, and increase the service life, reduce use cost.Aglite surface fluorination calcium, barium sulfate, the metatitanic acid calorize also can increase substantially its compressive strength.
Summary of the invention
The object of the present invention is to provide a kind of aluminium pyrophyllite and preparation method thereof of not being stained with, utilize pyrophyllite, surfacing is Calcium Fluoride (Fluorspan), barium sulfate, aluminium titanates or above the two or above three's laminated coating, and makes it have the method for not being stained with the aluminium characteristic.
For achieving the above object, the technical solution used in the present invention is as follows:
One, a kind of aluminium pyrophyllite of not being stained with: in the pyrophyllite surface coverage, one deck Calcium Fluoride (Fluorspan), barium sulfate or aluminium titanates are arranged, above the two or 2～3 layers of coating of above three.
Described while being coated with one deck, wherein Calcium Fluoride (Fluorspan), barium sulfate or aluminium titanates account for and are not stained with 0.05～50% of aluminium pyrophyllite massfraction; Be coated with Calcium Fluoride (Fluorspan) and barium sulfate when two-layer, internal layer is Calcium Fluoride (Fluorspan), and skin is barium sulfate, and wherein Calcium Fluoride (Fluorspan) and barium sulfate account for and is not stained with 0.05～50% of aluminium pyrophyllite massfraction; Be coated with barium sulfate and aluminium titanates when two-layer, internal layer is aluminium titanates, and skin is barium sulfate, and wherein barium sulfate and aluminium titanates account for and be not stained with 0.05～50% of aluminium pyrophyllite massfraction; Be coated with Calcium Fluoride (Fluorspan) and aluminium titanates when two-layer, internal layer is aluminium titanates, and skin is Calcium Fluoride (Fluorspan), wherein Calcium Fluoride (Fluorspan) and aluminium titanates account for be not stained with aluminium pyrophyllite massfraction 0.05～50%, aluminium titanates accounts for and is not stained with 0.05～50% of aluminium pyrophyllite massfraction; While being coated with three layers, internal layer is that aluminium titanates, middle layer are that Calcium Fluoride (Fluorspan), skin are barium sulfate, and wherein Calcium Fluoride (Fluorspan), barium sulfate and aluminium titanates account for and be not stained with 0.05～50% of aluminium pyrophyllite massfraction.
Two, plant the preparation method who is not stained with the aluminium pyrophyllite, following seven kinds of methods specifically arranged:
1, as follows when not being stained with the step of aluminium pyrophyllite surface coverage when the Calcium Fluoride (Fluorspan) layer is arranged:
(1) batching:
Prepare the fluorochemicals aqueous solution, the calcium containing compound aqueous solution, Calcium Fluoride (Fluorspan) colloidal sol or Calcium Fluoride (Fluorspan) powdery pulp are standby; Its concrete component target is: fluorochemicals aqueous solution massfraction is 2～48%; Calcium containing compound aqueous solution massfraction is 5～55%; In Calcium Fluoride (Fluorspan) colloidal sol, Calcium Fluoride (Fluorspan) colloidal sol massfraction is 5～25%; In the Calcium Fluoride (Fluorspan) powdery pulp, Calcium Fluoride (Fluorspan) massfraction content is 10～30%;
(2) surface coating has following Lung biopsy:
2.1 pyrophyllite is immersed in the fluorochemicals aqueous solution, dries; And then the pyrophyllite that adopts the fluorochemicals aqueous solution to process is immersed in the calcium containing compound aqueous solution again and generates the Calcium Fluoride (Fluorspan) layer, after cleaning, dry;
2.2 the fluorochemicals aqueous solution is sprayed on to the surface of pyrophyllite to moistening, dries; And then the calcium containing compound aqueous solution is sprayed on to the Surface Creation Calcium Fluoride (Fluorspan) that adopts the pyrophyllite that the fluorochemicals aqueous solution processed, after cleaning, dry;
2.3 Calcium Fluoride (Fluorspan) colloidal sol is sprayed on to the surface of pyrophyllite to fully moistening, dries;
2.4 pyrophyllite is immersed in Calcium Fluoride (Fluorspan) colloidal sol, in immersion process, constantly stir, soak time is 0.5～60min, takes out post-drying;
2.5 directly the Calcium Fluoride (Fluorspan) powdery pulp is sprayed on to the surface of pyrophyllite until fully moistening, oven dry gets final product;
(3) thermal treatment:
The pyrophyllite that surface is scribbled to one deck Calcium Fluoride (Fluorspan) is placed in the heat treatment furnace of 800～1200 ℃ and is incubated 1～4 hour, with the stove cooling, completes preparation.
The described fluorine cpd aqueous solution is ammonium fluoride aqueous solution, sodium fluoride aqueous solution or potassium fluoride aqueous solution; The described calcium containing compound aqueous solution is calcium nitrate aqueous solution or calcium chloride water.
2, as follows when not being stained with the step of aluminium pyrophyllite surface coverage when the barium sulfate layer is arranged:
(1) batching:
Prepare containing sulfate radicals compound water solution, the containing barium compound aqueous solution, barium sulfate sol or barium sulfate powdery pulp are standby; Concrete component target is: containing sulfate radicals compound water solution massfraction is 5～42.9%; Containing barium compound aqueous solution massfraction is 3～26%; In barium sulfate sol, the barium sulfate massfraction is: 5～25%; In the barium sulfate powdery pulp, the barium sulfate massfraction is 10～30%;
(2) surface coating has following Lung biopsy:
2.1 pyrophyllite is immersed in the containing sulfate radicals compound water solution, dries; And then the pyrophyllite that adopts the containing sulfate radicals compound water solution to process is immersed in the containing barium compound aqueous solution again and generates the barium sulfate layer, after cleaning, dry;
2.2 the containing sulfate radicals compound water solution is sprayed on to the surface of pyrophyllite to moistening, dries; And then the containing barium compound aqueous solution is sprayed on to the Surface Creation barium sulfate that adopts the pyrophyllite that the containing sulfate radicals compound water solution processed, after cleaning, dry;
2.3 barium sulfate sol is sprayed on to the surface of pyrophyllite to fully moistening, dries;
2.4 pyrophyllite is immersed in barium sulfate sol, in immersion process, constantly stir, soak time is 0.5～60min, takes out post-drying;
2.5 directly the barium sulfate powdery pulp is sprayed on to the surface of pyrophyllite until fully moistening, oven dry gets final product;
(3) thermal treatment
The pyrophyllite that surface is scribbled to one deck barium sulfate is placed in the heat treatment furnace of 600～900 ℃ and is incubated 1～4 hour, with the stove cooling, completes preparation.
Described containing sulfate radicals compound water solution is ammonium sulfate solution, potassium sulfate solution or aqueous sodium persulfate solution; The described containing barium compound aqueous solution is barium nitrate aqueous solution or barium chloride solution.
3, as follows when not being stained with the step of aluminium pyrophyllite surface coverage when the metatitanic acid aluminium lamination is arranged:
(1) batching:
Purchase commercially available or prepare titanium aluminium complex sol and the aluminium titanates powdery pulp is standby; Component target requires as follows:
A titanium aluminium complex sol: Ti
4+concentration is 0.2～0.3mol/L, Al
3+the titanium aluminium complex sol that concentration is 0.2～0.3mol/L; Add the Mg that molar fraction is 1.6～6% in colloidal sol
2+for stablizer; Or add the Mg that molar fraction is 3～5%
2+with the molar fraction Ce that is 0.4～0.8%
4+for stablizer; Or only add the Fe that molar fraction is 1.6～3.3%
3+for stablizer;
B aluminium titanates powdery pulp: consist of the Al that massfraction is 40～50%
2o
3with 50～60% TiO
2; Wherein adding massfraction is that 1～4%MgO is stablizer; Or add the CeO that MgO that massfraction is 1～4% and massfraction are 1～3%
2mixture is stablizer; Or to add massfraction be 3～8%Fe
2o
3for stablizer; Or add the ZrO that massfraction is 0.5～2%
2for stablizer;
(2) surface coating has following two kinds of methods:
2.1 pyrophyllite is immersed in titanium aluminium complex sol or aluminium titanates powdery pulp, in immersion process, constantly stir, soak time is 0.5～60min, takes out post-drying;
2.2 titanium aluminium complex sol or aluminium titanates powdery pulp are sprayed on to the pyrophyllite surface until fully moistening, and oven dry gets final product;
(3) thermal treatment
The heat treatment furnace that the pyrophyllite soaked or sprayed titanium aluminium complex sol and aluminium titanates powdery pulp is placed in to 1250～1450 ℃ is incubated 1～4 hour, with the stove cooling, completes preparation.
4, when not being stained with aluminium pyrophyllite surface coverage when Calcium Fluoride (Fluorspan) and barium sulfate two layers of coatings are arranged:
(1) first pyrophyllite is carried out to the Calcium Fluoride (Fluorspan) coating, its step is as follows:
(1) batching:
Prepare the fluorochemicals aqueous solution, the calcium containing compound aqueous solution, Calcium Fluoride (Fluorspan) colloidal sol or Calcium Fluoride (Fluorspan) powdery pulp are standby; Its concrete component target is: fluorochemicals aqueous solution massfraction is 2～48%; Calcium containing compound aqueous solution massfraction is 5～55%; In Calcium Fluoride (Fluorspan) colloidal sol, Calcium Fluoride (Fluorspan) colloidal sol massfraction is 5～25%; In the Calcium Fluoride (Fluorspan) powdery pulp, Calcium Fluoride (Fluorspan) massfraction content is 10～30%;
(2) surface coating has following Lung biopsy:
2.1 pyrophyllite is immersed in the fluorochemicals aqueous solution, dries; And then the pyrophyllite that adopts the fluorochemicals aqueous solution to process is immersed in the calcium containing compound aqueous solution again and generates the Calcium Fluoride (Fluorspan) layer, after cleaning, dry;
2.2 the fluorochemicals aqueous solution is sprayed on to the surface of pyrophyllite to moistening, dries; And then the calcium containing compound aqueous solution is sprayed on to the Surface Creation Calcium Fluoride (Fluorspan) that adopts the pyrophyllite that the fluorochemicals aqueous solution processed, after cleaning, dry;
2.3 Calcium Fluoride (Fluorspan) colloidal sol is sprayed on to the surface of pyrophyllite to fully moistening, dries;
2.4 pyrophyllite is immersed in Calcium Fluoride (Fluorspan) colloidal sol, in immersion process, constantly stir, soak time is 0.5～60min, takes out post-drying;
2.5 directly the Calcium Fluoride (Fluorspan) powdery pulp is sprayed on to the surface of pyrophyllite until fully moistening, oven dry gets final product;
(3) thermal treatment:
The pyrophyllite that surface is scribbled to one deck Calcium Fluoride (Fluorspan) is placed in the heat treatment furnace of 800～1200 ℃ and is incubated 1～4 hour, with the stove cooling, completes preparation.
(2) again pyrophyllite is carried out to the barium sulfate coating, its step is as follows:
(1) batching:
Prepare containing sulfate radicals compound water solution, the containing barium compound aqueous solution, barium sulfate sol or barium sulfate powdery pulp are standby; Concrete component target is: containing sulfate radicals compound water solution massfraction is 5～42.9%; Containing barium compound aqueous solution massfraction is 3～26%; In barium sulfate sol, the barium sulfate massfraction is: 5～25%; In the barium sulfate powdery pulp, the barium sulfate massfraction is 10～30%;
(2) surface coating has following Lung biopsy:
2.1 pyrophyllite is immersed in the containing sulfate radicals compound water solution, dries; And then the pyrophyllite that adopts the containing sulfate radicals compound water solution to process is immersed in the containing barium compound aqueous solution again and generates the barium sulfate layer, after cleaning, dry;
2.2 the containing sulfate radicals compound water solution is sprayed on to the surface of pyrophyllite to moistening, dries; And then the containing barium compound aqueous solution is sprayed on to the Surface Creation barium sulfate that adopts the pyrophyllite that the containing sulfate radicals compound water solution processed, after cleaning, dry;
2.3 barium sulfate sol is sprayed on to the surface of pyrophyllite to fully moistening, dries;
2.4 pyrophyllite is immersed in barium sulfate sol, in immersion process, constantly stir, soak time is 0.5～60min, takes out post-drying;
2.5 directly the barium sulfate powdery pulp is sprayed on to the surface of pyrophyllite until fully moistening, oven dry gets final product;
(3) thermal treatment
The pyrophyllite that surface is scribbled to one deck barium sulfate is placed in the heat treatment furnace of 600～900 ℃ and is incubated 1～4 hour, with the stove cooling, completes preparation.
5, when not being stained with aluminium pyrophyllite surface coverage when Calcium Fluoride (Fluorspan) and two layers of coating of aluminium titanates are arranged:
(1) first pyrophyllite is carried out to the aluminium titanates coating, its step is as follows:
(1) batching:
Purchase commercially available or prepare titanium aluminium complex sol and the aluminium titanates powdery pulp is standby; Component target requires as follows:
A titanium aluminium complex sol: Ti
4+concentration is 0.2～0.3mol/L, Al
3+the titanium aluminium complex sol that concentration is 0.2～0.3mol/L; Add the Mg that molar fraction is 1.6～6% in colloidal sol
2+for stablizer; Or add the Mg that molar fraction is 3～5%
2+with the molar fraction Ce that is 0.4～0.8%
4+for stablizer; Or only add the Fe that molar fraction is 1.6～3.3%
3+for being stablizer;
B aluminium titanates powdery pulp: consist of the Al that massfraction is 40～50%
2o
3with 50～60% TiO
2; Wherein adding massfraction is that 1～4%MgO is stablizer; Or add the CeO that MgO that massfraction is 1～4% and massfraction are 1～3%
2mixture is stablizer; Or to add massfraction be 3～8%Fe
2o
3for stablizer; Or add the ZrO that massfraction is 0.5～2%
2for stablizer;
(2) surface coating has following two kinds of methods:
2.1 pyrophyllite is immersed in titanium aluminium complex sol or aluminium titanates powdery pulp, in immersion process, constantly stir, soak time is 0.5～60min, takes out post-drying;
2.2 titanium aluminium complex sol or aluminium titanates powdery pulp are sprayed on to the pyrophyllite surface until fully moistening, and oven dry gets final product;
(3) thermal treatment
The heat treatment furnace that the pyrophyllite soaked or sprayed titanium aluminium complex sol and aluminium titanates powdery pulp is placed in to 1250～1450 ℃ is incubated 1～4 hour, with the stove cooling, completes preparation.
(2) again pyrophyllite is carried out to the Calcium Fluoride (Fluorspan) coating, its step is as follows:
(1) batching:
Prepare the fluorochemicals aqueous solution, the calcium containing compound aqueous solution, Calcium Fluoride (Fluorspan) colloidal sol or Calcium Fluoride (Fluorspan) powdery pulp are standby; Its concrete component target is: fluorochemicals aqueous solution massfraction is 2～48%; Calcium containing compound aqueous solution massfraction is 5～55%; In Calcium Fluoride (Fluorspan) colloidal sol, Calcium Fluoride (Fluorspan) colloidal sol massfraction is 5～25%; In the Calcium Fluoride (Fluorspan) powdery pulp, Calcium Fluoride (Fluorspan) massfraction content is 10～30%;
(2) surface coating has following Lung biopsy:
2.1 pyrophyllite is immersed in the fluorochemicals aqueous solution, dries; And then the pyrophyllite that adopts the fluorochemicals aqueous solution to process is immersed in the calcium containing compound aqueous solution again and generates the Calcium Fluoride (Fluorspan) layer, after cleaning, dry;
2.2 the fluorochemicals aqueous solution is sprayed on to the surface of pyrophyllite to moistening, dries; And then the calcium containing compound aqueous solution is sprayed on to the Surface Creation Calcium Fluoride (Fluorspan) that adopts the pyrophyllite that the fluorochemicals aqueous solution processed, after cleaning, dry;
2.3 Calcium Fluoride (Fluorspan) colloidal sol is sprayed on to the surface of pyrophyllite to fully moistening, dries;
2.4 pyrophyllite is immersed in Calcium Fluoride (Fluorspan) colloidal sol, in immersion process, constantly stir, soak time is 0.5～60min, takes out post-drying;
2.5 directly the Calcium Fluoride (Fluorspan) powdery pulp is sprayed on to the surface of pyrophyllite until fully moistening, oven dry gets final product;
(3) thermal treatment:
The pyrophyllite that surface is scribbled to one deck Calcium Fluoride (Fluorspan) is placed in the heat treatment furnace of 800～1200 ℃ and is incubated 1～4 hour, with the stove cooling, completes preparation.
6, when not being stained with aluminium pyrophyllite surface coverage when aluminium titanates and two layers of coating of Calcium Fluoride (Fluorspan) are arranged:
(1) first pyrophyllite is carried out to the aluminium titanates coating, its step is as follows:
(1) batching:
Purchase commercially available or prepare titanium aluminium complex sol and the aluminium titanates powdery pulp is standby; Component target requires as follows:
A titanium aluminium complex sol: Ti
4+concentration is 0.2～0.3mol/L, Al
3+the titanium aluminium complex sol that concentration is 0.2～0.3mol/L; Add the Mg that molar fraction is 1.6～6% in colloidal sol
2+for stablizer; Or add the Mg that molar fraction is 3～5%
2+with the molar fraction Ce that is 0.4～0.8%
4+for stablizer; Or only add the Fe that molar fraction is 1.6～3.3%
3+for being stablizer;
B aluminium titanates powdery pulp: consist of the Al that massfraction is 40～50%
2o
3with 50～60% TiO
2; Wherein adding massfraction is that 1～4%MgO is stablizer; Or add the CeO that MgO that massfraction is 1～4% and massfraction are 1～3%
2mixture is stablizer; Or to add massfraction be 3～8%Fe
2o
3for stablizer; Or add the ZrO that massfraction is 0.5～2%
2for stablizer;
(2) surface coating has following two kinds of methods:
2.1 pyrophyllite is immersed in titanium aluminium complex sol or aluminium titanates powdery pulp, in immersion process, constantly stir, soak time is 0.5～60min, takes out post-drying;
2.2 titanium aluminium complex sol or aluminium titanates powdery pulp are sprayed on to the pyrophyllite surface until fully moistening, and oven dry gets final product;
(3) thermal treatment
The heat treatment furnace that the pyrophyllite soaked or sprayed titanium aluminium complex sol and aluminium titanates powdery pulp is placed in to 1250～1450 ℃ is incubated 1～4 hour, with the stove cooling, completes preparation.
(2) again pyrophyllite is carried out to the Calcium Fluoride (Fluorspan) coating, its step is as follows:
(1) batching:
Prepare the fluorochemicals aqueous solution, the calcium containing compound aqueous solution, Calcium Fluoride (Fluorspan) colloidal sol or Calcium Fluoride (Fluorspan) powdery pulp are standby; Its concrete component target is: fluorochemicals aqueous solution massfraction is 2～48%; Calcium containing compound aqueous solution massfraction is 5～55%; In Calcium Fluoride (Fluorspan) colloidal sol, Calcium Fluoride (Fluorspan) colloidal sol massfraction is 5～25%; In the Calcium Fluoride (Fluorspan) powdery pulp, Calcium Fluoride (Fluorspan) massfraction content is 10～30%;
(2) surface coating has following Lung biopsy:
2.1 pyrophyllite is immersed in the fluorochemicals aqueous solution, dries; And then the pyrophyllite that adopts the fluorochemicals aqueous solution to process is immersed in the calcium containing compound aqueous solution again and generates the Calcium Fluoride (Fluorspan) layer, after cleaning, dry;
2.2 the fluorochemicals aqueous solution is sprayed on to the surface of pyrophyllite to moistening, dries; And then the calcium containing compound aqueous solution is sprayed on to the Surface Creation Calcium Fluoride (Fluorspan) that adopts the pyrophyllite that the fluorochemicals aqueous solution processed, after cleaning, dry;
2.3 Calcium Fluoride (Fluorspan) colloidal sol is sprayed on to the surface of pyrophyllite to fully moistening, dries;
2.4 pyrophyllite is immersed in Calcium Fluoride (Fluorspan) colloidal sol, in immersion process, constantly stir, soak time is 0.5～60min, takes out post-drying;
2.5 directly the Calcium Fluoride (Fluorspan) powdery pulp is sprayed on to the surface of pyrophyllite until fully moistening, oven dry gets final product;
(3) thermal treatment:
The pyrophyllite that surface is scribbled to one deck Calcium Fluoride (Fluorspan) is placed in the heat treatment furnace of 800～1200 ℃ and is incubated 1～4 hour, with the stove cooling, completes preparation.
7, when not being stained with aluminium pyrophyllite surface coverage when Calcium Fluoride (Fluorspan), barium sulfate, three layers of compound coating of aluminium titanates are arranged:
(1) first aluminium titanates is carried out in the pyrophyllite surface and apply, its step is as follows:
(1) batching:
Purchase commercially available or prepare titanium aluminium complex sol and the aluminium titanates powdery pulp is standby; Component target requires as follows:
A titanium aluminium complex sol: Ti
4+concentration is 0.2～0.3mol/L, Al
3+the titanium aluminium complex sol that concentration is 0.2～0.3mol/L; Add the Mg that molar fraction is 1.6～6% in colloidal sol
2+for stablizer; Or add the Mg that molar fraction is 3～5%
2+with the molar fraction Ce that is 0.4～0.8%
4+for stablizer; Or only add the Fe that molar fraction is 1.6～3.3%
3+for being stablizer;
B aluminium titanates powdery pulp: consist of the Al that massfraction is 40～50%
2o
3with 50～60% TiO
2; Wherein adding massfraction is that 1～4%MgO is stablizer; Or add the CeO that MgO that massfraction is 1～4% and massfraction are 1～3%
2mixture is stablizer; Or to add massfraction be 3～8%Fe
2o
3for stablizer; Or add the ZrO that massfraction is 0.5～2%
2for stablizer;
(2) surface coating has following two kinds of methods:
2.1 pyrophyllite is immersed in titanium aluminium complex sol or aluminium titanates powdery pulp, in immersion process, constantly stir, soak time is 0.5～60min, takes out post-drying;
2.2 titanium aluminium complex sol or aluminium titanates powdery pulp are sprayed on to the pyrophyllite surface until fully moistening, and oven dry gets final product;
(3) thermal treatment
The heat treatment furnace that the pyrophyllite soaked or sprayed titanium aluminium complex sol and aluminium titanates powdery pulp is placed in to 1250～1450 ℃ is incubated 1～4 hour, with the stove cooling, completes preparation.
(2) covered aluminum titanate coatings and formed calcium fluoride coating again, its step is as follows:
(1) batching:
Prepare the fluorochemicals aqueous solution, the calcium containing compound aqueous solution, Calcium Fluoride (Fluorspan) colloidal sol or Calcium Fluoride (Fluorspan) powdery pulp are standby; Its concrete component target is: fluorochemicals aqueous solution massfraction is 2～48%; Calcium containing compound aqueous solution massfraction is 5～55%; In Calcium Fluoride (Fluorspan) colloidal sol, Calcium Fluoride (Fluorspan) colloidal sol massfraction is 5～25%; In the Calcium Fluoride (Fluorspan) powdery pulp, Calcium Fluoride (Fluorspan) massfraction content is 10～30%;
(2) surface coating has following Lung biopsy:
2.1 pyrophyllite is immersed in the fluorochemicals aqueous solution, dries; And then the pyrophyllite that adopts the fluorochemicals aqueous solution to process is immersed in the calcium containing compound aqueous solution again and generates the Calcium Fluoride (Fluorspan) layer, after cleaning, dry;
2.2 the fluorochemicals aqueous solution is sprayed on to the surface of pyrophyllite to moistening, dries; And then the calcium containing compound aqueous solution is sprayed on to the Surface Creation Calcium Fluoride (Fluorspan) that adopts the pyrophyllite that the fluorochemicals aqueous solution processed, after cleaning, dry;
2.3 Calcium Fluoride (Fluorspan) colloidal sol is sprayed on to the surface of pyrophyllite to fully moistening, dries;
2.4 pyrophyllite is immersed in Calcium Fluoride (Fluorspan) colloidal sol, in immersion process, constantly stir, soak time is 0.5～60min, takes out post-drying;
2.5 directly the Calcium Fluoride (Fluorspan) powdery pulp is sprayed on to the surface of pyrophyllite until fully moistening, oven dry gets final product;
(3) thermal treatment:
The pyrophyllite that surface is scribbled to one deck Calcium Fluoride (Fluorspan) is placed in the heat treatment furnace of 800～1200 ℃ and is incubated 1～4 hour, with the stove cooling, completes preparation.
(3) be coated with the pyrophyllite formation barium sulfate coating of aluminium titanates and calcium fluoride coating, its step is as follows:
(1) batching:
Prepare containing sulfate radicals compound water solution, the containing barium compound aqueous solution, barium sulfate sol or barium sulfate powdery pulp are standby; Concrete component target is: containing sulfate radicals compound water solution massfraction is 5～42.9%; Containing barium compound aqueous solution massfraction is 3～26%; In barium sulfate sol, the barium sulfate massfraction is: 5～25%; In the barium sulfate powdery pulp, the barium sulfate massfraction is 10～30%;
(2) surface coating has following Lung biopsy:
2.1 pyrophyllite is immersed in the containing sulfate radicals compound water solution, dries; And then the pyrophyllite that adopts the containing sulfate radicals compound water solution to process is immersed in the containing barium compound aqueous solution again and generates the barium sulfate layer, after cleaning, dry;
2.2 the containing sulfate radicals compound water solution is sprayed on to the surface of pyrophyllite to moistening, dries; And then the containing barium compound aqueous solution is sprayed on to the Surface Creation barium sulfate that adopts the pyrophyllite that the containing sulfate radicals compound water solution processed, after cleaning, dry;
2.3 barium sulfate sol is sprayed on to the surface of pyrophyllite to fully moistening, dries;
2.4 pyrophyllite is immersed in barium sulfate sol, in immersion process, constantly stir, soak time is 0.5～60min, takes out post-drying;
2.5 directly the barium sulfate powdery pulp is sprayed on to the surface of pyrophyllite until fully moistening, oven dry gets final product;
(3) thermal treatment
The pyrophyllite that surface is scribbled to one deck barium sulfate is placed in the heat treatment furnace of 600～900 ℃ and is incubated 1～4 hour, with the stove cooling, completes preparation.
Containing sulfate radicals compound water solution described in method 1～7 is ammonium sulfate solution, potassium sulfate solution or aqueous sodium persulfate solution; The described containing barium compound aqueous solution is barium nitrate aqueous solution or barium chloride solution; The described fluorine cpd aqueous solution is ammonium fluoride aqueous solution, sodium fluoride aqueous solution or potassium fluoride aqueous solution; The described calcium containing compound aqueous solution is calcium nitrate aqueous solution or calcium chloride water.
The beneficial effect that the present invention has is:
Adopt surface coating Calcium Fluoride (Fluorspan), barium sulfate, the method for aluminium titanates is carried out surface modification.Calcium Fluoride (Fluorspan), barium sulfate and aluminium titanates are attached to the surface of pyrophyllite, and enter gap, in crackle and hole, dry rear Calcium Fluoride (Fluorspan), barium sulfate, aluminium titanates is distributed in the pyrophyllite surface, gap and intergranule.Calcium Fluoride (Fluorspan) under the condition of being heated, barium sulfate, aluminium titanates pyrophyllite sintering.Due to Calcium Fluoride (Fluorspan), barium sulfate, aluminium titanates has not imbibition characteristic of pair aluminium, thereby treated pyrophyllite does not infiltrate aluminium.And Calcium Fluoride (Fluorspan), barium sulfate, aluminium titanates enters among pyrophyllite crackle and hole, energy mended crack and hole after high temperature sintering, thereby the compressive strength of raising pyrophyllite.
The accompanying drawing explanation
Fig. 1 is not stained with the graphic representation of aluminium pyrophyllite.
Fig. 2 be one deck coating arranged be not stained with aluminium pyrophyllite part sectioned view.
Fig. 3 be two layers of coating are arranged be not stained with aluminium pyrophyllite part sectioned view.
Fig. 4 be three layers of coating are arranged be not stained with aluminium pyrophyllite part sectioned view.
In figure: 1, pyrophyllite particle in irregular shape, 2, pyrophyllite matrix, 3, Calcium Fluoride (Fluorspan), barium sulfate or metatitanic acid coating, 4 and 5 is Calcium Fluoride (Fluorspan) and barium sulfate combination coating, aluminium titanates and Calcium Fluoride (Fluorspan) combination coating or aluminium titanates and barium sulfate combination coating, 6, aluminum titanate coatings, 7, calcium fluoride coating, 8 barium sulfate coatings.
Embodiment
Embodiment 1:(soaks)
First configure the fluorochemicals aqueous solution and the calcium containing compound aqueous solution, pyrophyllite is immersed in the fluorochemicals aqueous solution, the pyrophyllite that to process through the fluorochemicals aqueous solution again after oven dry is immersed in the calcium containing compound aqueous solution, Surface Creation Calcium Fluoride (Fluorspan), after washing and drying, put into High Temperature Furnaces Heating Apparatus thermal treatment, thermal treatment temp is 800～1200 ℃, soaking time is 1～4 hour, finally obtains the pyrophyllite surface and is covered with one deck Calcium Fluoride (Fluorspan).Specific embodiments is in Table 1.Agalmatolite before untreated distributes as Fig. 1, and wherein 1 is agalmatolite.Its sectional view of pyrophyllite that adopts the method gained to have calcium fluoride coating is as Fig. 2, and wherein 1 is the pyrophyllite matrix, and the 3rd, calcium fluoride coating
When the calcium nitrite reactant aqueous solution that the sodium fluoride aqueous solution that pyrophyllite employing massfraction is 2% and massfraction are 5% precipitates coating, Calcium Fluoride (Fluorspan) quality percentage composition 0.05%;
When pyrophyllite adopts the calcium nitrate aqueous solution reaction precipitation coating that sodium fluoride aqueous solution that massfraction is 3.8% and massfraction are 45%, Calcium Fluoride (Fluorspan) quality percentage composition 1.5%;
When the calcium nitrite reactant aqueous solution that the sodium fluoride aqueous solution that pyrophyllite employing massfraction is 2.5% and massfraction are 20% precipitates coating, Calcium Fluoride (Fluorspan) quality percentage composition 0.08%;
When pyrophyllite adopts the calcium chloride water reaction precipitation coating that sodium fluoride aqueous solution that massfraction is 3.8% and massfraction are 42%, Calcium Fluoride (Fluorspan) quality percentage composition 1.2%;
When pyrophyllite adopts the chlorine calcium nitrate aqueous solution reaction precipitation coating that ammonium fluoride aqueous solution that massfraction is 25% and massfraction are 55%, Calcium Fluoride (Fluorspan) quality percentage composition 15%;
When the Calcium hydrogen carbonate calcium reactant aqueous solution that the ammonium fluoride aqueous solution that pyrophyllite employing massfraction is 20% and massfraction are 13% precipitates coating, Calcium Fluoride (Fluorspan) quality percentage composition 8%;
When the Calcium hydrogen carbonate reactant aqueous solution that the ammonium fluoride aqueous solution that pyrophyllite employing massfraction is 15% and massfraction are 13% precipitates coating, Calcium Fluoride (Fluorspan) quality percentage composition 7%;
When pyrophyllite adopts the calcium chloride water reaction precipitation coating that ammonium fluoride aqueous solution that massfraction is 10% and massfraction are 30%, Calcium Fluoride (Fluorspan) quality percentage composition 12%;
When the Calcium hydrogen carbonate reactant aqueous solution that the potassium fluoride aqueous solution that pyrophyllite employing massfraction is 48% and massfraction are 5% precipitates coating, Calcium Fluoride (Fluorspan) quality percentage composition 6%;
When the calcium nitrite reactant aqueous solution that the potassium fluoride aqueous solution that pyrophyllite employing massfraction is 39% and massfraction are 45% precipitates coating, Calcium Fluoride (Fluorspan) quality percentage composition 14%;
When pyrophyllite adopts the calcium nitrate aqueous solution reaction precipitation coating that potassium fluoride aqueous solution that massfraction is 30% and massfraction are 35%, Calcium Fluoride (Fluorspan) quality percentage composition 12%;
When pyrophyllite adopts the calcium chloride water reaction precipitation coating that potassium fluoride aqueous solution that massfraction is 20% and massfraction are 20%, Calcium Fluoride (Fluorspan) quality percentage composition 10%;
The modification of table 1 precipitator method is not stained with the aluminium pyrophyllite and is processed under differing temps
Embodiment 2 (spraying)
First configure the fluorochemicals aqueous solution and the calcium containing compound aqueous solution, the fluorochemicals aqueous solution is sprayed on to the pyrophyllite skin drying, and then it is extremely moistening that the calcium containing compound aqueous solution is sprayed on to the pyrophyllite surface that sprayed the fluorochemicals aqueous solution, reaction generates the Calcium Fluoride (Fluorspan) precipitation, washing is dried, and puts into High Temperature Furnaces Heating Apparatus thermal treatment, and thermal treatment temp is 800～1200 ℃, soaking time is 1～4 hour, finally obtains the pyrophyllite surface and is covered with one deck Calcium Fluoride (Fluorspan).Specific embodiments is in Table 2.Agalmatolite before untreated distributes as Fig. 1, and wherein 1 is agalmatolite.Its sectional view of pyrophyllite that adopts the method gained to have calcium fluoride coating is as Fig. 2, and wherein 2 is pyrophyllite matrixes, and the 3rd, calcium fluoride coating
While after the calcium nitrite aqueous solution spraying reaction that the sodium fluoride aqueous solution that pyrophyllite employing massfraction is 2% and massfraction are 5%, generating coating, Calcium Fluoride (Fluorspan) quality percentage composition 0.08%;
While after the calcium nitrate aqueous solution spraying reaction that the sodium fluoride aqueous solution that pyrophyllite employing massfraction is 3.8% and massfraction are 45%, generating coating, Calcium Fluoride (Fluorspan) quality percentage composition 2.3%;
While after the calcium nitrite aqueous solution spraying reaction that the sodium fluoride aqueous solution that pyrophyllite employing massfraction is 2.5% and massfraction are 20%, generating coating, Calcium Fluoride (Fluorspan) quality percentage composition 0.78%;
While after the calcium chloride water spraying reaction that the sodium fluoride aqueous solution that pyrophyllite employing massfraction is 3.8% and massfraction are 42%, generating coating, Calcium Fluoride (Fluorspan) quality percentage composition 1.5%;
While after the chlorine calcium nitrate aqueous solution spraying reaction that the ammonium fluoride aqueous solution that pyrophyllite employing massfraction is 25% and massfraction are 55%, generating coating, Calcium Fluoride (Fluorspan) quality percentage composition 23%;
While after the Calcium hydrogen carbonate calcium aqueous solution spraying reaction that the ammonium fluoride aqueous solution that pyrophyllite employing massfraction is 20% and massfraction are 13%, generating coating, Calcium Fluoride (Fluorspan) quality percentage composition 10%;
While after the Calcium hydrogen carbonate aqueous solution spraying reaction that the ammonium fluoride aqueous solution that pyrophyllite employing massfraction is 15% and massfraction are 13%, generating coating, Calcium Fluoride (Fluorspan) quality percentage composition 9%;
While after the calcium chloride water spraying reaction that the ammonium fluoride aqueous solution that pyrophyllite employing massfraction is 10% and massfraction are 30%, generating coating, Calcium Fluoride (Fluorspan) quality percentage composition 15%;
While after the Calcium hydrogen carbonate aqueous solution spraying reaction that the potassium fluoride aqueous solution that pyrophyllite employing massfraction is 48% and massfraction are 5%, generating coating, Calcium Fluoride (Fluorspan) quality percentage composition 8%;
While after the calcium nitrite aqueous solution spraying reaction that the potassium fluoride aqueous solution that pyrophyllite employing massfraction is 39% and massfraction are 45%, generating coating, Calcium Fluoride (Fluorspan) quality percentage composition 120%;
While after the calcium nitrate aqueous solution spraying reaction that the potassium fluoride aqueous solution that pyrophyllite employing massfraction is 30% and massfraction are 35%, generating coating, Calcium Fluoride (Fluorspan) quality percentage composition 17%;
While after the calcium chloride water spraying reaction that the potassium fluoride aqueous solution that pyrophyllite employing massfraction is 20% and massfraction are 20%, generating coating, Calcium Fluoride (Fluorspan) quality percentage composition 13%;
The modification of table 2 precipitator method is not stained with the aluminium pyrophyllite and is processed under differing temps
Embodiment 3:(spraying)
By commercial or prepare calcium fluoride powder system form slurry, in slurry, the Calcium Fluoride (Fluorspan) massfraction is 10%, 15%, 18%, 22%, 26%, 30%, be sprayed on the pyrophyllite surface to fully moistening, dry, be placed in High Temperature Furnaces Heating Apparatus thermal treatment 1～4 hour, thermal treatment temp is 800 ℃～1200 ℃.Specific embodiments is in Table 3.Agalmatolite before untreated distributes as Fig. 1, and wherein 1 is agalmatolite.Its sectional view of pyrophyllite that adopts the method gained to have calcium fluoride coating is as Fig. 2, and wherein 2 is pyrophyllite matrixes, and the 3rd, calcium fluoride coating
The method of the Calcium Fluoride (Fluorspan) powdery pulp that employing is 10% at pyrophyllite surface spraying massfraction generates coating, Calcium Fluoride (Fluorspan) Calcium Fluoride (Fluorspan) quality percentage composition 13%;
The method of the Calcium Fluoride (Fluorspan) powdery pulp that employing is 15% at pyrophyllite surface spraying massfraction generates coating, Calcium Fluoride (Fluorspan) Calcium Fluoride (Fluorspan) quality percentage composition 18%;
The method of the Calcium Fluoride (Fluorspan) powdery pulp that employing is 18% at pyrophyllite surface spraying massfraction generates coating, Calcium Fluoride (Fluorspan) Calcium Fluoride (Fluorspan) quality percentage composition 27%;
The method of the Calcium Fluoride (Fluorspan) powdery pulp that employing is 22% at pyrophyllite surface spraying massfraction generates coating, Calcium Fluoride (Fluorspan) Calcium Fluoride (Fluorspan) quality percentage composition 35%;
The method of the Calcium Fluoride (Fluorspan) powdery pulp that employing is 26% at pyrophyllite surface spraying massfraction generates coating, Calcium Fluoride (Fluorspan) Calcium Fluoride (Fluorspan) quality percentage composition 41%;
The method of the Calcium Fluoride (Fluorspan) powdery pulp that employing is 30% at pyrophyllite surface spraying massfraction generates coating, Calcium Fluoride (Fluorspan) Calcium Fluoride (Fluorspan) quality percentage composition 50%;
Table 3 is not stained with the aluminium pyrophyllite and is processed under differing temps
Commercial Calcium Fluoride (Fluorspan) colloidal sol is configured to the Calcium Fluoride (Fluorspan) colloidal sol of various solubility, in colloidal sol, the Calcium Fluoride (Fluorspan) massfraction is 5%, 15%, 25%, be sprayed on aluminium calcium hollow ball surface to fully moistening or aluminium calcium hollow ball is immersed in Calcium Fluoride (Fluorspan) colloidal sol, dry, be placed in High Temperature Furnaces Heating Apparatus thermal treatment 1～4 hour, thermal treatment temp is 800 ℃～1200 ℃.Specific embodiments is in Table 4.Agalmatolite before untreated distributes as Fig. 1, and wherein 1 is agalmatolite.Its sectional view of pyrophyllite that adopts the method gained to have calcium fluoride coating is as Fig. 2, and wherein 2 is pyrophyllite matrixes, and the 3rd, calcium fluoride coating
Table 4 Calcium Fluoride (Fluorspan) colloidal sol is processed aluminium calcium hollow ball
Embodiment 5:(soaks)
First configure containing sulfate radicals compound water solution and the containing barium compound aqueous solution, pyrophyllite is immersed in the containing sulfate radicals compound water solution, the pyrophyllite that to process through the containing sulfate radicals compound water solution again after oven dry is immersed in the containing barium compound aqueous solution, make it Surface Creation barium sulfate, after washing and drying, put into High Temperature Furnaces Heating Apparatus thermal treatment, thermal treatment temp is 600～900 ℃, soaking time is 1～4 hour, finally obtains the pyrophyllite surface and is covered with one deck barium sulfate.Specific embodiments is in Table 5.Agalmatolite before untreated distributes as Fig. 1, and wherein 1 is agalmatolite.Its sectional view of pyrophyllite that adopts the method gained to have the barium sulfate coating is as Fig. 2, and wherein 2 is pyrophyllite matrixes, and the 3rd, the barium sulfate coating
When pyrophyllite adopts the barium nitrate aqueous solution reaction precipitation coating that ammonium sulfate solution that massfraction is 42.9% and massfraction are 5%, barium sulfate quality percentage composition 8%;
When pyrophyllite adopts the barium nitrate aqueous solution reaction precipitation coating that ammonium sulfate solution that massfraction is 30% and massfraction are 3%, barium sulfate quality percentage composition 3%;
When pyrophyllite adopts the barium nitrate aqueous solution reaction precipitation coating that ammonium sulfate solution that massfraction is 20% and massfraction are 7%, barium sulfate quality percentage composition 5%;
When pyrophyllite adopts the barium chloride solution reaction precipitation coating that aqueous sodium persulfate solution that massfraction is 16% and massfraction are 26%, barium sulfate quality percentage composition 15%;
When pyrophyllite adopts the barium nitrate aqueous solution reaction precipitation coating that aqueous sodium persulfate solution that massfraction is 12% and massfraction are 15%, barium sulfate quality percentage composition 12%;
When pyrophyllite adopts the barium nitrate aqueous solution reaction precipitation coating that aqueous sodium persulfate solution that massfraction is 10% and massfraction are 10%, barium sulfate quality percentage composition 7%;
When pyrophyllite adopts the barium nitrate aqueous solution reaction precipitation coating that potassium sulfate solution that massfraction is 10% and massfraction are 8%, barium sulfate quality percentage composition 6%;
When pyrophyllite adopts the barium nitrate aqueous solution reaction precipitation coating that ammonium sulfate solution that massfraction is 8% and massfraction are 6%, barium sulfate quality percentage composition 1.6%;
When pyrophyllite adopts the barium nitrate aqueous solution reaction precipitation coating that ammonium sulfate solution that massfraction is 5% and massfraction are 8%, barium sulfate quality percentage composition 1.3%;
While after the barium nitrate aqueous solution spraying reaction that the ammonium sulfate solution that pyrophyllite employing massfraction is 42.9% and massfraction are 5%, generating coating, barium sulfate quality percentage composition 9%;
The modification of table 5 precipitator method is not stained with the aluminium pyrophyllite and is processed under differing temps
Embodiment 6 (spraying)
First configure containing sulfate radicals compound water solution and the containing barium compound aqueous solution, the containing sulfate radicals compound water solution is sprayed on to the pyrophyllite skin drying, and then it is extremely moistening that the containing barium compound aqueous solution is sprayed on to the pyrophyllite surface that sprayed the containing sulfate radicals compound water solution, reaction generates barium sulfate precipitate, washing is dried, and puts into High Temperature Furnaces Heating Apparatus thermal treatment, and thermal treatment temp is 600～900 ℃, soaking time is 1～4 hour, and the surface that finally obtains pyrophyllite is covered with one deck barium sulfate.Specific embodiments is in Table 5.Agalmatolite before untreated distributes as Fig. 1, and wherein 1 is agalmatolite.Its sectional view of pyrophyllite that has the barium sulfate coating with the method gained is as Fig. 2, and wherein 2 is pyrophyllite matrixes, and the 3rd, the barium sulfate coating
While after the barium nitrate aqueous solution spraying reaction that the ammonium sulfate solution that pyrophyllite employing massfraction is 30% and massfraction are 3%, generating coating, barium sulfate quality percentage composition 4%;
While after the barium nitrate aqueous solution spraying reaction that the ammonium sulfate solution that pyrophyllite employing massfraction is 20% and massfraction are 7%, generating coating, barium sulfate quality percentage composition 6%;
While after the barium chloride solution spraying reaction that the aqueous sodium persulfate solution that pyrophyllite employing massfraction is 16% and massfraction are 26%, generating coating, barium sulfate quality percentage composition 17%;
While after the barium nitrate aqueous solution spraying reaction that the aqueous sodium persulfate solution that pyrophyllite employing massfraction is 12% and massfraction are 15%, generating coating, barium sulfate quality percentage composition 14%;
While after the barium nitrate aqueous solution spraying reaction that the aqueous sodium persulfate solution that pyrophyllite employing massfraction is 10% and massfraction are 10%, generating coating, barium sulfate quality percentage composition 9%;
While after the barium nitrate aqueous solution spraying reaction that the potassium sulfate solution that pyrophyllite employing massfraction is 10% and massfraction are 8%, generating coating, barium sulfate quality percentage composition 8%;
While after the barium nitrate aqueous solution spraying reaction that the ammonium sulfate solution that pyrophyllite employing massfraction is 8% and massfraction are 6%, generating coating, barium sulfate quality percentage composition 2.7%;
While after the barium nitrate aqueous solution spraying reaction that the ammonium sulfate solution that pyrophyllite employing massfraction is 5% and massfraction are 8%, generating coating, barium sulfate quality percentage composition 2.3%;
The modification of table 6 precipitator method is not stained with the aluminium pyrophyllite and is processed under differing temps
Embodiment 7:(spraying)
By commercial or prepare blaue fixe system form slurry, in slurry, the barium sulfate massfraction is 10%, 15%, 18%, 22%, 26%, 30% is sprayed on the pyrophyllite surface to fully moistening, dry, be placed in High Temperature Furnaces Heating Apparatus thermal treatment 1～4 hour, thermal treatment temp is 600 ℃～900 ℃.Specific embodiments is in Table 6.Agalmatolite before untreated distributes as Fig. 1, and wherein 1 is agalmatolite.Its sectional view of pyrophyllite that has the barium sulfate coating with the method gained is as Fig. 2, and wherein 2 is pyrophyllite matrixes, and the 3rd, the barium sulfate coating
The method of the barium sulfate powdery pulp that employing is 10% at pyrophyllite surface spraying massfraction generates coating, barium sulfate quality percentage composition 13%;
The method of the barium sulfate powdery pulp that employing is 15% at pyrophyllite surface spraying massfraction generates coating, barium sulfate quality percentage composition 18%;
The method of the barium sulfate powdery pulp that employing is 18% at pyrophyllite surface spraying massfraction generates coating, barium sulfate quality percentage composition 27%;
The method of the barium sulfate powdery pulp that employing is 22% at pyrophyllite surface spraying massfraction generates coating, barium sulfate quality percentage composition 35%;
The method of the barium sulfate powdery pulp that employing is 26% at pyrophyllite surface spraying massfraction generates coating, barium sulfate quality percentage composition 41%;
The method of the barium sulfate powdery pulp that employing is 30% at pyrophyllite surface spraying massfraction generates coating, barium sulfate quality percentage composition 50%;
Table 7 is not stained with the aluminium pyrophyllite and is processed under differing temps
Commercial barium sulfate sol is configured to the barium sulfate sol of various solubility, in colloidal sol, the barium sulfate massfraction is 5%, 15%, 25%, be sprayed on fire resisting material particle surface to fully moistening or fire resisting material particle is immersed in barium sulfate sol, dry, be placed in High Temperature Furnaces Heating Apparatus thermal treatment 1～4 hour, thermal treatment temp is 600 ℃～900 ℃.Specific embodiments is in Table 8.Agalmatolite before untreated distributes as Fig. 1, and wherein 1 is agalmatolite.Its sectional view of pyrophyllite that has the barium sulfate coating with the method gained is as Fig. 2, and wherein 2 is pyrophyllite matrixes, and the 3rd, the barium sulfate coating.
Table 8 barium sulfate sol is processed aluminium calcium hollow ball
Embodiment 9 (titanium aluminium complex sol),
First prepare titanium aluminium complex sol: Ti
4+concentration is 0.2～0.3mol/L, Al
3+the titanium aluminium complex sol that concentration is 0.2～0.3mol/L; Add the Mg that molar fraction is 1.6～6% in colloidal sol
2+for stablizer; Or add the Mg that molar fraction is 3～5%
2+with the molar fraction Ce that is 0.4～0.8%
4+for stablizer; Or only add the Fe that molar fraction is 1.6～3.3%
3+for stablizer.Pyrophyllite is put into to colloidal sol to be soaked 0.5～60min or colloidal sol is sprayed on to the pyrophyllite surface to the surface wettability post-drying, then put into High Temperature Furnaces Heating Apparatus thermal treatment, thermal treatment temp is 1250～1450 ℃, soaking time 1～4 hour, obtain not being stained with the aluminium pyrophyllite, specific embodiments is in Table 9.Agalmatolite before untreated distributes as Fig. 1, and wherein 1 is agalmatolite.Its sectional view of pyrophyllite that has aluminum titanate coatings with the method gained is as Fig. 2, and wherein 2 is pyrophyllite matrixes, and the 3rd, aluminum titanate coatings.
Pyrophyllite is immersed in containing Ti
4+concentration is 0.2mol/L, Al
3+concentration is 0.3mol/L, the Mg that is 1.6% containing mass percent
2+titanium aluminium colloidal sol generate coating, aluminium titanates quality percentage composition is 3.9%;
Pyrophyllite is soaked containing Ti
4+concentration is 0.25mol/L, Al
3+concentration is 0.25mol/L, the Mg that is 3% containing mass percent
2+, mass percent is 0.8%Ce
4+titanium aluminium colloidal sol in generate coating, aluminium titanates quality percentage composition is 3.9%;
Pyrophyllite is soaked containing Ti
4+concentration is 0.3mol/L, Al
3+concentration is 0.25mol/L, the Fe that is 1.6% containing mass percent
3+titanium aluminium colloidal sol generate coating, aluminium titanates quality percentage composition is 4.9%;
Will be containing Ti
4+concentration is 0.2mol/L, Al
3+concentration is 0.3mol/L, the Fe that is 1.6% containing mass percent
3+titanium aluminium colloidal sol be sprayed on pyrophyllite and generate coating, aluminium titanates quality percentage composition is 4.5%;
Will be containing Ti
4+concentration is 0.25mol/L, Al
3+concentration is 0.25mol/L, the Mg that is 5% containing mass percent
2+titanium aluminium colloidal sol be sprayed on pyrophyllite and generate coating, aluminium titanates quality percentage composition is 5.3%;
Will be containing Ti
4+concentration is 0.3mol/L, Al
3+concentration is 0.25mol/L, the Fe that is 3.3% containing mass percent
3+titanium aluminium colloidal sol be sprayed on pyrophyllite and generate coating, aluminium titanates quality percentage composition is 5.9%;
The sol-gel modified aluminium pyrophyllite of not being stained with of table 9 titanium aluminium is processed under differing temps
Embodiment 10 (aluminium titanates powder),
Now prepare the aluminium titanates powdery pulp: get the raw materials ready by the requirement of aluminium titanates quality mark, consist of the Al that massfraction is 40～50%
2o
3with 50～60% TiO
2; Wherein adding massfraction is that 1～4%MgO is stablizer; Or add the CeO that MgO that massfraction is 1～4% and massfraction are 1～3%
2mixture is stablizer; Or to add massfraction be 3～8%Fe
2o
3for stablizer; Or add the ZrO that massfraction is 0.5～2%
2for stablizer.It is dry after pyrophyllite is soaked to 0.5～60min in aluminium titanates powder slurry, or the aluminium titanates powdery pulp is sprayed on pyrophyllite to dry after surface wettability, put into High Temperature Furnaces Heating Apparatus thermal treatment, thermal treatment temp is 1250～1450 ℃, soaking time 1～4 hour, obtain surface containing aluminium titanates be not stained with the aluminium pyrophyllite, specific embodiments is in Table 10.Agalmatolite before untreated distributes as Fig. 1, and wherein 1 is agalmatolite.Its sectional view of pyrophyllite that has aluminum titanate coatings with the method gained is as Fig. 2, and wherein 2 is pyrophyllite matrixes, and the 3rd, aluminum titanate coatings
Pyrophyllite is immersed in to the Al that mass percent is 40%
2o
3, the TiO that mass percent is 60%
2, the aluminium titanates powdery pulp of the MgO that molecular fraction is 4%, aluminium titanates quality percentage composition is 38%;
Pyrophyllite is immersed in to the Al that mass percent is 42%
2o
3, the TiO that mass percent is 58%
2, the Fe that molecular fraction is 8%
2o
3the aluminium titanates powdery pulp make coating, aluminium titanates quality percentage composition is 40%
Pyrophyllite is immersed in to the Al that mass percent is 43%
2o
3, the TiO that mass percent is 57%
2, the ZrO that molecular fraction is 0.5%
2the aluminium titanates powdery pulp make coating, aluminium titanates quality percentage composition is 45%
Pyrophyllite is soaked to the Al that mass percent is 45%
2o
3, the TiO that mass percent is 55%
2, the MgO that molecular fraction is 4%, the CeO that molecular fraction is 1%
2the aluminium titanates powdery pulp make coating, aluminium titanates quality percentage composition is 47%;
The Al that is 42% by mass percent
2o
3, the TiO that mass percent is 58%
2, the Fe that molecular fraction is 3%
2o
3the aluminium titanates powdery pulp be sprayed on the pyrophyllite surface and make coating, aluminium titanates quality percentage composition is 50%;
The Al that is 45% by mass percent
2o
3, the TiO that mass percent is 55%
2, the ZrO that molecular fraction is 2%
2the aluminium titanates powdery pulp be sprayed on the pyrophyllite surface and make coating, aluminium titanates quality percentage composition is 49%;
The Al that is 43% by mass percent
2o
3, the TiO that mass percent is 57%
2, the MgO that molecular fraction is 1%, the CeO that molecular fraction is 2%
2the aluminium titanates powdery pulp be sprayed on the pyrophyllite surface and make coating, aluminium titanates quality percentage composition is 46%;
The Al that is 44% by mass percent
2o
3, the TiO that mass percent is 56%
2, the MgO that molecular fraction is 1%, the CeO that molecular fraction is 2%
2the aluminium titanates powdery pulp be sprayed on the pyrophyllite surface and make coating, aluminium titanates quality percentage composition is 43%;
Table 10 aluminium titanates powdery pulp modified surface is not stained with the aluminium pyrophyllite and is processed under differing temps
Embodiment 11. (in the pyrophyllite appearance, forming successively Calcium Fluoride (Fluorspan) and barium sulfate two-layer compound coating)
One of: by embodiment 1 and embodiment 5, carry out successively,
Two: by embodiment 1 and embodiment 6, carry out successively,
Three: by embodiment 1 and embodiment 7, carry out successively,
Four: by embodiment 1 and embodiment 8, carry out successively
Five: by embodiment 2 and embodiment 5, carry out successively,
Six: by embodiment 2 and embodiment 6, carry out successively,
Seven: by embodiment 2 and embodiment 7, carry out successively,
Eight: by embodiment 2 and embodiment 8, carry out successively
Nine: by embodiment 3 and embodiment 5, carry out successively,
Ten: by embodiment 3 and embodiment 6, carry out successively,
11: by embodiment 3 and embodiment 7, carry out successively,
12: by embodiment 3 and embodiment 8, carry out successively
13: by embodiment 4 and embodiment 5, carry out successively,
14: by embodiment 4 and embodiment 6, carry out successively,
15: by embodiment 4 and embodiment 7, carry out successively,
16: by embodiment 4 and embodiment 8, carry out successively.
Agalmatolite before untreated distributes as Fig. 1, and wherein 1 is agalmatolite.Its sectional view of pyrophyllite that has Calcium Fluoride (Fluorspan) and barium sulfate two-layer compound coating with the method gained is as Fig. 3, and wherein 2 is pyrophyllite matrixes, and the 4th, calcium fluoride coating, the 5th, barium sulfate coating
Embodiment 12. (in the pyrophyllite appearance, forming successively aluminium titanates and Calcium Fluoride (Fluorspan) two-layer compound coating)
One of: by embodiment 9 and embodiment 1, carry out successively,
Two: by embodiment 9 and embodiment 2, carry out successively,
Three: by embodiment 9 and embodiment 3, carry out successively,
Four: by embodiment 9 and embodiment 4, carry out successively
Five: by embodiment 10 and embodiment 1, carry out successively,
Six: by embodiment 10 and embodiment 2, carry out successively,
Seven: by embodiment 10 and embodiment 3, carry out successively,
Eight: by embodiment 10 and embodiment 4, carry out successively
Nine: by embodiment 11 and embodiment 1, carry out successively,
Ten: by embodiment 11 and embodiment 2, carry out successively,
11: by embodiment 11 and embodiment 3, carry out successively,
12: by embodiment 11 and embodiment 4, carry out successively
Agalmatolite before untreated distributes as Fig. 1, and wherein 1 is agalmatolite.Its sectional view of pyrophyllite that has aluminium titanates and Calcium Fluoride (Fluorspan) two-layer compound coating with the method gained is as Fig. 3, and wherein 2 is pyrophyllite matrixes, and the 4th, aluminum titanate coatings, the 5th, calcium fluoride coating
Embodiment 13. (in the pyrophyllite appearance, forming successively aluminium titanates and barium sulfate two-layer compound coating)
One of: by embodiment 9 and embodiment 5, carry out successively,
Two: by embodiment 9 and embodiment 6, carry out successively,
Three: by embodiment 9 and embodiment 7, carry out successively,
Four: by embodiment 9 and embodiment 8, carry out successively
Five: by embodiment 10 and embodiment 5, carry out successively,
Six: by embodiment 10 and embodiment 6, carry out successively,
Seven: by embodiment 10 and embodiment 7, carry out successively,
Eight: by embodiment 10 and embodiment 8, carry out successively
Agalmatolite before untreated distributes as Fig. 1, and wherein 1 is agalmatolite.Its sectional view of pyrophyllite that has aluminium titanates and barium sulfate two-layer compound coating with the method gained is as Fig. 3, and wherein 2 is pyrophyllite matrixes, and the 4th, aluminum titanate coatings, the 5th, barium sulfate coating
Embodiment 14. (appearance forms aluminium titanates, Calcium Fluoride (Fluorspan) and three layers of compound coating of barium sulfate successively on the pyrophyllite surface)
One of: by embodiment 9, embodiment 1 be, embodiment 5 carries out successively,
Two: by embodiment 9, embodiment 1 be, embodiment 6 carries out successively,
Three: by embodiment 9, embodiment 1 be, embodiment 7 carries out successively,
Four: by embodiment 9, embodiment 1 be, embodiment 8 carries out successively,
Five: by embodiment 9, embodiment 2 be, embodiment 5 carries out successively,
Six: by embodiment 9, embodiment 2 be, embodiment 6 carries out successively,
Seven: by embodiment 9, embodiment 2 be, embodiment 7 carries out successively,
Eight: by embodiment 9, embodiment 2 be, embodiment 8 carries out successively,
Nine: by embodiment 9, embodiment 3 be, embodiment 5 carries out successively,
Ten: by embodiment 9, embodiment 3 be, embodiment 6 carries out successively,
11: by embodiment 9, embodiment 3 be, embodiment 7 carries out successively,
12: by embodiment 9, embodiment 3 be, embodiment 8 carries out successively,
13: by embodiment 9, embodiment 4 be, embodiment 5 carries out successively,
14: by embodiment 9, embodiment 4 be, embodiment 6 carries out successively,
15: by embodiment 9, embodiment 4 be, embodiment 7 carries out successively,
16: by embodiment 9, embodiment 4 be, embodiment 8 carries out successively,
Agalmatolite before untreated distributes as Fig. 1, and wherein 1 is agalmatolite.Its sectional view of pyrophyllite that has aluminium titanates, Calcium Fluoride (Fluorspan) and three layers of compound coating of barium sulfate with the method gained is as Fig. 4, and wherein 2 is pyrophyllite matrixes, and the 6th, aluminum titanate coatings, the 7th, calcium fluoride coating, the 8th, barium sulfate coating.
Claims (11)
1. be not stained with the aluminium pyrophyllite for one kind, it is characterized in that: in the pyrophyllite surface coverage, one deck Calcium Fluoride (Fluorspan), barium sulfate or aluminium titanates are arranged, wherein Calcium Fluoride (Fluorspan), barium sulfate or aluminium titanates account for and are not stained with 0.05～50% of aluminium pyrophyllite massfraction; The step of its preparation method is as follows:
When not being stained with, the step of aluminium pyrophyllite surface coverage when the Calcium Fluoride (Fluorspan) layer is arranged is as follows:
(1) batching:
Prepare the fluorochemicals aqueous solution, the calcium containing compound aqueous solution, Calcium Fluoride (Fluorspan) colloidal sol or Calcium Fluoride (Fluorspan) powdery pulp are standby; Its concrete component target is: fluorochemicals aqueous solution massfraction is 2～48%; Calcium containing compound aqueous solution massfraction is 5～55%; In Calcium Fluoride (Fluorspan) colloidal sol, the Calcium Fluoride (Fluorspan) massfraction is 5～25%; In the Calcium Fluoride (Fluorspan) powdery pulp, Calcium Fluoride (Fluorspan) massfraction content is 10～30%;
(2) surface coating has following Lung biopsy:
2.1 pyrophyllite is immersed in the fluorochemicals aqueous solution, dries; And then the pyrophyllite that adopts the fluorochemicals aqueous solution to process is immersed in the calcium containing compound aqueous solution again and generates the Calcium Fluoride (Fluorspan) layer, after cleaning, dry;
2.2 the fluorochemicals aqueous solution is sprayed on to the surface of pyrophyllite to moistening, dries; And then the calcium containing compound aqueous solution is sprayed on to the Surface Creation Calcium Fluoride (Fluorspan) that adopts the pyrophyllite that the fluorochemicals aqueous solution processed, after cleaning, dry;
2.3 Calcium Fluoride (Fluorspan) colloidal sol is sprayed on to the surface of pyrophyllite to fully moistening, dries;
2.4 pyrophyllite is immersed in Calcium Fluoride (Fluorspan) colloidal sol, in immersion process, constantly stir, soak time is 0.5 ~ 60min, takes out post-drying;
2.5 directly the Calcium Fluoride (Fluorspan) powdery pulp is sprayed on to the surface of pyrophyllite until fully moistening, oven dry gets final product;
(3) thermal treatment:
The pyrophyllite that surface is scribbled to one deck Calcium Fluoride (Fluorspan) is placed in the heat treatment furnace of 800～1200 ℃ and is incubated 1～4 hour, with the stove cooling, completes preparation;
The described fluorine cpd aqueous solution is ammonium fluoride aqueous solution, sodium fluoride aqueous solution or potassium fluoride aqueous solution; The described calcium containing compound aqueous solution is calcium nitrate aqueous solution or calcium chloride water;
When not being stained with, the step of aluminium pyrophyllite surface coverage when the barium sulfate layer is arranged is as follows:
(1) batching:
Prepare containing sulfate radicals compound water solution, the containing barium compound aqueous solution, barium sulfate sol or barium sulfate powdery pulp are standby; Concrete component target is: containing sulfate radicals compound water solution massfraction is 5～42.9%; Containing barium compound aqueous solution massfraction is 3～26%; In barium sulfate sol, the barium sulfate massfraction is: 5～25%; In the barium sulfate powdery pulp, the barium sulfate massfraction is 10～30%;
(2) surface coating has following Lung biopsy:
2.1 pyrophyllite is immersed in the containing sulfate radicals compound water solution, dries; And then the pyrophyllite that adopts the containing sulfate radicals compound water solution to process is immersed in the containing barium compound aqueous solution again and generates the barium sulfate layer, after cleaning, dry;
2.2 the containing sulfate radicals compound water solution is sprayed on to the surface of pyrophyllite to moistening, dries; And then the containing barium compound aqueous solution is sprayed on to the Surface Creation barium sulfate that adopts the pyrophyllite that the containing sulfate radicals compound water solution processed, after cleaning, dry;
2.3 barium sulfate sol is sprayed on to the surface of pyrophyllite to fully moistening, dries;
2.4 pyrophyllite is immersed in barium sulfate sol, in immersion process, constantly stir, soak time is 0.5 ~ 60min, takes out post-drying;
2.5 directly the barium sulfate powdery pulp is sprayed on to the surface of pyrophyllite until fully moistening, oven dry gets final product;
(3) thermal treatment
The pyrophyllite that surface is scribbled to one deck barium sulfate is placed in the heat treatment furnace of 600～900 ℃ and is incubated 1～4 hour, with the stove cooling, completes preparation;
Described containing sulfate radicals compound water solution is ammonium sulfate solution, potassium sulfate solution or aqueous sodium persulfate solution; The described containing barium compound aqueous solution is barium nitrate aqueous solution or barium chloride solution;
When not being stained with, the step of aluminium pyrophyllite surface coverage when the metatitanic acid aluminium lamination is arranged is as follows:
(1) batching:
Purchase commercially available or prepare titanium aluminium complex sol and the aluminium titanates powdery pulp is standby; Component target requires as follows:
A titanium aluminium complex sol: Ti
4+concentration is 0.2 ~ 0.3mol/L, Al
3+the titanium aluminium complex sol that concentration is 0.2～0.3mol/L; Add the Mg that molar fraction is 1.6～6% in colloidal sol
2+for stablizer; Or add the Mg that molar fraction is 3～5%
2+with the molar fraction Ce that is 0.4～0.8%
4+for stablizer; Or only add the Fe that molar fraction is 1.6～3.3%
3+for stablizer;
B aluminium titanates powdery pulp: consist of the Al that massfraction is 40～50%
2o
3with 50～60% TiO
2; Wherein adding massfraction is that 1～4%MgO is stablizer; Or add the CeO that MgO that massfraction is 1～4% and massfraction are 1～3%
2mixture is stablizer; Or to add massfraction be 3～8% Fe
2o
3for stablizer; Or add the ZrO that massfraction is 0.5～2%
2for stablizer;
(2) surface coating has following two kinds of methods:
2.1 pyrophyllite is immersed in titanium aluminium complex sol or aluminium titanates powdery pulp, in immersion process, constantly stir, soak time is 0.5 ~ 60min, takes out post-drying;
2.2 titanium aluminium complex sol or aluminium titanates powdery pulp are sprayed on to the pyrophyllite surface until fully moistening, and oven dry gets final product;
(3) thermal treatment
The heat treatment furnace that the pyrophyllite soaked or sprayed titanium aluminium complex sol or aluminium titanates powdery pulp is placed in to 1250～1450 ℃ is incubated 1～4 hour, with the stove cooling, completes preparation.
2. be not stained with the aluminium pyrophyllite for one kind, it is characterized in that: in the pyrophyllite surface coverage, two layers of Calcium Fluoride (Fluorspan) or barium sulfate or aluminium titanates are arranged, be coated with Calcium Fluoride (Fluorspan) and barium sulfate when two-layer, internal layer is Calcium Fluoride (Fluorspan), skin is barium sulfate, and wherein Calcium Fluoride (Fluorspan) and barium sulfate account for and is not stained with 0.05～50% of aluminium pyrophyllite massfraction; Be coated with barium sulfate and aluminium titanates when two-layer, internal layer is aluminium titanates, and skin is barium sulfate, and wherein barium sulfate and aluminium titanates account for and be not stained with 0.05 ~ 50% of aluminium pyrophyllite massfraction; Be coated with Calcium Fluoride (Fluorspan) and aluminium titanates when two-layer, internal layer is aluminium titanates, and skin is Calcium Fluoride (Fluorspan), wherein Calcium Fluoride (Fluorspan) and aluminium titanates account for be not stained with aluminium pyrophyllite massfraction 0.05～50%, aluminium titanates accounts for and is not stained with 0.05～50% of aluminium pyrophyllite massfraction; The step of its preparation method is as follows: not being stained with aluminium pyrophyllite surface coverage has more than Calcium Fluoride (Fluorspan), barium sulfate, aluminium titanates when the two two layers of coatings combines, and following three kinds of methods are arranged:
1. when not being stained with aluminium pyrophyllite surface coverage when Calcium Fluoride (Fluorspan) and barium sulfate two layers of coatings are arranged:
(i) first pyrophyllite is carried out to the Calcium Fluoride (Fluorspan) coating, its step is as follows:
(1) batching:
Prepare the fluorochemicals aqueous solution, the calcium containing compound aqueous solution, Calcium Fluoride (Fluorspan) colloidal sol or Calcium Fluoride (Fluorspan) powdery pulp are standby; Its concrete component target is: fluorochemicals aqueous solution massfraction is 2～48%; Calcium containing compound aqueous solution massfraction is 5～55%; In Calcium Fluoride (Fluorspan) colloidal sol, the Calcium Fluoride (Fluorspan) massfraction is 5～25%; In the Calcium Fluoride (Fluorspan) powdery pulp, Calcium Fluoride (Fluorspan) massfraction content is 10～30%;
(2) surface coating has following Lung biopsy:
2.1 pyrophyllite is immersed in the fluorochemicals aqueous solution, dries; And then the pyrophyllite that adopts the fluorochemicals aqueous solution to process is immersed in the calcium containing compound aqueous solution again and generates the Calcium Fluoride (Fluorspan) layer, after cleaning, dry;
2.2 the fluorochemicals aqueous solution is sprayed on to the surface of pyrophyllite to moistening, dries; And then the calcium containing compound aqueous solution is sprayed on to the Surface Creation Calcium Fluoride (Fluorspan) that adopts the pyrophyllite that the fluorochemicals aqueous solution processed, after cleaning, dry;
2.3 Calcium Fluoride (Fluorspan) colloidal sol is sprayed on to the surface of pyrophyllite to fully moistening, dries;
2.4 pyrophyllite is immersed in Calcium Fluoride (Fluorspan) colloidal sol, in immersion process, constantly stir, soak time is 0.5 ~ 60min, takes out post-drying;
2.5 directly the Calcium Fluoride (Fluorspan) powdery pulp is sprayed on to the surface of pyrophyllite until fully moistening, oven dry gets final product;
(3) thermal treatment:
The pyrophyllite that surface is scribbled to one deck Calcium Fluoride (Fluorspan) is placed in the heat treatment furnace of 800～1200 ℃ and is incubated 1～4 hour, with the stove cooling, completes preparation;
(ii) again pyrophyllite is carried out to the barium sulfate coating, its step is as follows:
(1) batching:
Prepare containing sulfate radicals compound water solution, the containing barium compound aqueous solution, barium sulfate sol or barium sulfate powdery pulp are standby; Concrete component target is: containing sulfate radicals compound water solution massfraction is 5～42.9%; Containing barium compound aqueous solution massfraction is 3～26%; In barium sulfate sol, the barium sulfate massfraction is: 5～25%; In the barium sulfate powdery pulp, the barium sulfate massfraction is 10～30%;
(2) surface coating has following Lung biopsy:
2.1 pyrophyllite is immersed in the containing sulfate radicals compound water solution, dries; And then the pyrophyllite that adopts the containing sulfate radicals compound water solution to process is immersed in the containing barium compound aqueous solution again and generates the barium sulfate layer, after cleaning, dry;
2.2 the containing sulfate radicals compound water solution is sprayed on to the surface of pyrophyllite to moistening, dries; And then the containing barium compound aqueous solution is sprayed on to the Surface Creation barium sulfate that adopts the pyrophyllite that the containing sulfate radicals compound water solution processed, after cleaning, dry;
2.3 barium sulfate sol is sprayed on to the surface of pyrophyllite to fully moistening, dries;
2.4 pyrophyllite is immersed in barium sulfate sol, in immersion process, constantly stir, soak time is 0.5 ~ 60min, takes out post-drying;
2.5 directly the barium sulfate powdery pulp is sprayed on to the surface of pyrophyllite until fully moistening, oven dry gets final product;
(3) thermal treatment
The pyrophyllite that surface is scribbled to one deck barium sulfate is placed in the heat treatment furnace of 600～900 ℃ and is incubated 1～4 hour, with the stove cooling, completes preparation;
2. when not being stained with aluminium pyrophyllite surface coverage when Calcium Fluoride (Fluorspan) and two layers of coating of aluminium titanates are arranged:
(i) first pyrophyllite is carried out to the aluminium titanates coating, its step is as follows:
(1) batching:
Purchase commercially available or prepare titanium aluminium complex sol and the aluminium titanates powdery pulp is standby; Component target requires as follows:
A titanium aluminium complex sol: Ti
4+concentration is 0.2 ~ 0.3mol/L, Al
3+the titanium aluminium complex sol that concentration is 0.2～0.3mol/L; Add the Mg that molar fraction is 1.6～6% in colloidal sol
2+for stablizer; Or add the Mg that molar fraction is 3～5%
2+with the molar fraction Ce that is 0.4～0.8%
4+for stablizer; Or only add the Fe that molar fraction is 1.6～3.3%
3+for being stablizer;
B aluminium titanates powdery pulp: consist of the Al that massfraction is 40～50%
2o
3with 50～60% TiO
2; Wherein adding massfraction is that 1～4%MgO is stablizer; Or add the CeO that MgO that massfraction is 1～4% and massfraction are 1～3%
2mixture is stablizer; Or to add massfraction be 3～8% Fe
2o
3for stablizer; Or add the ZrO that massfraction is 0.5～2%
2for stablizer;
(2) surface coating has following two kinds of methods:
2.1 pyrophyllite is immersed in titanium aluminium complex sol or aluminium titanates powdery pulp, in immersion process, constantly stir, soak time is 0.5 ~ 60min, takes out post-drying;
2.2 titanium aluminium complex sol or aluminium titanates powdery pulp are sprayed on to the pyrophyllite surface until fully moistening, and oven dry gets final product;
(3) thermal treatment
The heat treatment furnace that the pyrophyllite soaked or sprayed titanium aluminium complex sol or aluminium titanates powdery pulp is placed in to 1250～1450 ℃ is incubated 1～4 hour, with the stove cooling, completes preparation;
(ii) again pyrophyllite is carried out to the Calcium Fluoride (Fluorspan) coating, its step is as follows:
(1) batching:
Prepare the fluorochemicals aqueous solution, the calcium containing compound aqueous solution, Calcium Fluoride (Fluorspan) colloidal sol or Calcium Fluoride (Fluorspan) powdery pulp are standby; Its concrete component target is: fluorochemicals aqueous solution massfraction is 2～48%; Calcium containing compound aqueous solution massfraction is 5～55%; In Calcium Fluoride (Fluorspan) colloidal sol, the Calcium Fluoride (Fluorspan) massfraction is 5～25%; In the Calcium Fluoride (Fluorspan) powdery pulp, Calcium Fluoride (Fluorspan) massfraction content is 10～30%;
(2) surface coating has following Lung biopsy:
2.1 pyrophyllite is immersed in the fluorochemicals aqueous solution, dries; And then the pyrophyllite that adopts the fluorochemicals aqueous solution to process is immersed in the calcium containing compound aqueous solution again and generates the Calcium Fluoride (Fluorspan) layer, after cleaning, dry;
2.2 the fluorochemicals aqueous solution is sprayed on to the surface of pyrophyllite to moistening, dries; And then the calcium containing compound aqueous solution is sprayed on to the Surface Creation Calcium Fluoride (Fluorspan) that adopts the pyrophyllite that the fluorochemicals aqueous solution processed, after cleaning, dry;
2.3 Calcium Fluoride (Fluorspan) colloidal sol is sprayed on to the surface of pyrophyllite to fully moistening, dries;
2.4 pyrophyllite is immersed in Calcium Fluoride (Fluorspan) colloidal sol, in immersion process, constantly stir, soak time is 0.5 ~ 60min, takes out post-drying;
2.5 directly the Calcium Fluoride (Fluorspan) powdery pulp is sprayed on to the surface of pyrophyllite until fully moistening, oven dry gets final product;
(3) thermal treatment:
The pyrophyllite that surface is scribbled to one deck Calcium Fluoride (Fluorspan) is placed in the heat treatment furnace of 800～1200 ℃ and is incubated 1～4 hour, with the stove cooling, completes preparation;
3. when not being stained with aluminium pyrophyllite surface coverage when aluminium titanates and two layers of coating of Calcium Fluoride (Fluorspan) are arranged:
(i) first pyrophyllite is carried out to the aluminium titanates coating, its step is as follows:
(1) batching:
Purchase commercially available or prepare titanium aluminium complex sol and the aluminium titanates powdery pulp is standby; Component target requires as follows:
A titanium aluminium complex sol: Ti
4+concentration is 0.2 ~ 0.3mol/L, Al
3+the titanium aluminium complex sol that concentration is 0.2～0.3mol/L; Add the Mg that molar fraction is 1.6～6% in colloidal sol
2+for stablizer; Or add the Mg that molar fraction is 3～5%
2+with the molar fraction Ce that is 0.4～0.8%
4+for stablizer; Or only add the Fe that molar fraction is 1.6～3.3%
3+for being stablizer;
B aluminium titanates powdery pulp: consist of the Al that massfraction is 40～50%
2o
3with 50～60% TiO
2; Wherein adding massfraction is that 1～4%MgO is stablizer; Or add the CeO that MgO that massfraction is 1～4% and massfraction are 1～3%
2mixture is stablizer; Or to add massfraction be 3～8% Fe
2o
3for stablizer; Or add the ZrO that massfraction is 0.5～2%
2for stablizer;
(2) surface coating has following two kinds of methods:
2.1 pyrophyllite is immersed in titanium aluminium complex sol or aluminium titanates powdery pulp, in immersion process, constantly stir, soak time is 0.5 ~ 60min, takes out post-drying;
2.2 titanium aluminium complex sol or aluminium titanates powdery pulp are sprayed on to the pyrophyllite surface until fully moistening, and oven dry gets final product;
(3) thermal treatment
The heat treatment furnace that the pyrophyllite soaked or sprayed titanium aluminium complex sol or aluminium titanates powdery pulp is placed in to 1250～1450 ℃ is incubated 1～4 hour, with the stove cooling, completes preparation;
(ii) again pyrophyllite is carried out to the Calcium Fluoride (Fluorspan) coating, its step is as follows:
(1) batching:
Prepare the fluorochemicals aqueous solution, the calcium containing compound aqueous solution, Calcium Fluoride (Fluorspan) colloidal sol or Calcium Fluoride (Fluorspan) powdery pulp are standby; Its concrete component target is: fluorochemicals aqueous solution massfraction is 2～48%; Calcium containing compound aqueous solution massfraction is 5～55%; In Calcium Fluoride (Fluorspan) colloidal sol, the Calcium Fluoride (Fluorspan) massfraction is 5～25%; In the Calcium Fluoride (Fluorspan) powdery pulp, Calcium Fluoride (Fluorspan) massfraction content is 10～30%;
(2) surface coating has following Lung biopsy:
2.1 pyrophyllite is immersed in the fluorochemicals aqueous solution, dries; And then the pyrophyllite that adopts the fluorochemicals aqueous solution to process is immersed in the calcium containing compound aqueous solution again and generates the Calcium Fluoride (Fluorspan) layer, after cleaning, dry;
2.2 the fluorochemicals aqueous solution is sprayed on to the surface of pyrophyllite to moistening, dries; And then the calcium containing compound aqueous solution is sprayed on to the Surface Creation Calcium Fluoride (Fluorspan) that adopts the pyrophyllite that the fluorochemicals aqueous solution processed, after cleaning, dry;
2.3 Calcium Fluoride (Fluorspan) colloidal sol is sprayed on to the surface of pyrophyllite to fully moistening, dries;
2.4 pyrophyllite is immersed in Calcium Fluoride (Fluorspan) colloidal sol, in immersion process, constantly stir, soak time is 0.5 ~ 60min, takes out post-drying;
2.5 directly the Calcium Fluoride (Fluorspan) powdery pulp is sprayed on to the surface of pyrophyllite until fully moistening, oven dry gets final product;
(3) thermal treatment:
The pyrophyllite that surface is scribbled to one deck Calcium Fluoride (Fluorspan) is placed in the heat treatment furnace of 800～1200 ℃ and is incubated 1～4 hour, with the stove cooling, completes preparation;
Described containing sulfate radicals compound water solution is ammonium sulfate solution, potassium sulfate solution or aqueous sodium persulfate solution; The described containing barium compound aqueous solution is barium nitrate aqueous solution or barium chloride solution; The described fluorine cpd aqueous solution is ammonium fluoride aqueous solution, sodium fluoride aqueous solution or potassium fluoride aqueous solution; The described calcium containing compound aqueous solution is calcium nitrate aqueous solution or calcium chloride water.
3. be not stained with the aluminium pyrophyllite for one kind, it is characterized in that: in the pyrophyllite surface coverage, three layers of Calcium Fluoride (Fluorspan), barium sulfate and aluminium titanates are arranged, internal layer is that aluminium titanates, middle layer are that Calcium Fluoride (Fluorspan), skin are barium sulfate, wherein Calcium Fluoride (Fluorspan), barium sulfate and aluminium titanates account for and are not stained with 0.05～50% of aluminium pyrophyllite massfraction, and the step of its preparation method is as follows:
(i) first aluminium titanates is carried out in the pyrophyllite surface and apply, its step is as follows:
(1) batching:
Purchase commercially available or prepare titanium aluminium complex sol and the aluminium titanates powdery pulp is standby; Component target requires as follows:
A titanium aluminium complex sol: Ti
4+concentration is 0.2 ~ 0.3mol/L, Al
3+the titanium aluminium complex sol that concentration is 0.2～0.3mol/L; Add the Mg that molar fraction is 1.6～6% in colloidal sol
2+for stablizer; Or add the Mg that molar fraction is 3～5%
2+with the molar fraction Ce that is 0.4～0.8%
4+for stablizer; Or only add the Fe that molar fraction is 1.6～3.3%
3+for being stablizer;
B aluminium titanates powdery pulp: consist of the Al that massfraction is 40～50%
2o
3with 50～60% TiO
2; Wherein adding massfraction is that 1～4%MgO is stablizer; Or add the CeO that MgO that massfraction is 1～4% and massfraction are 1～3%
2mixture is stablizer; Or to add massfraction be 3～8% Fe
2o
3for stablizer; Or add the ZrO that massfraction is 0.5～2%
2for stablizer;
(2) surface coating has following two kinds of methods:
2.1 pyrophyllite is immersed in titanium aluminium complex sol or aluminium titanates powdery pulp, in immersion process, constantly stir, soak time is 0.5 ~ 60min, takes out post-drying;
2.2 titanium aluminium complex sol or aluminium titanates powdery pulp are sprayed on to the pyrophyllite surface until fully moistening, and oven dry gets final product;
(3) thermal treatment
The heat treatment furnace that the pyrophyllite soaked or sprayed titanium aluminium complex sol or aluminium titanates powdery pulp is placed in to 1250～1450 ℃ is incubated 1～4 hour, with the stove cooling, completes preparation;
(ii) covered aluminum titanate coatings and formed calcium fluoride coating again, its step is as follows:
(1) batching:
Prepare the fluorochemicals aqueous solution, the calcium containing compound aqueous solution, Calcium Fluoride (Fluorspan) colloidal sol or Calcium Fluoride (Fluorspan) powdery pulp are standby; Its concrete component target is: fluorochemicals aqueous solution massfraction is 2～48%; Calcium containing compound aqueous solution massfraction is 5～55%; In Calcium Fluoride (Fluorspan) colloidal sol, the Calcium Fluoride (Fluorspan) massfraction is 5～25%; In the Calcium Fluoride (Fluorspan) powdery pulp, Calcium Fluoride (Fluorspan) massfraction content is 10～30%;
(2) surface coating has following Lung biopsy:
2.1 pyrophyllite is immersed in the fluorochemicals aqueous solution, dries; And then the pyrophyllite that adopts the fluorochemicals aqueous solution to process is immersed in the calcium containing compound aqueous solution again and generates the Calcium Fluoride (Fluorspan) layer, after cleaning, dry;
2.2 the fluorochemicals aqueous solution is sprayed on to the surface of pyrophyllite to moistening, dries; And then the calcium containing compound aqueous solution is sprayed on to the Surface Creation Calcium Fluoride (Fluorspan) that adopts the pyrophyllite that the fluorochemicals aqueous solution processed, after cleaning, dry;
2.3 Calcium Fluoride (Fluorspan) colloidal sol is sprayed on to the surface of pyrophyllite to fully moistening, dries;
2.4 pyrophyllite is immersed in Calcium Fluoride (Fluorspan) colloidal sol, in immersion process, constantly stir, soak time is 0.5 ~ 60min, takes out post-drying;
2.5 directly the Calcium Fluoride (Fluorspan) powdery pulp is sprayed on to the surface of pyrophyllite until fully moistening, oven dry gets final product;
(3) thermal treatment:
The pyrophyllite that surface is scribbled to one deck Calcium Fluoride (Fluorspan) is placed in the heat treatment furnace of 800～1200 ℃ and is incubated 1～4 hour, with the stove cooling, completes preparation;
(iii) the pyrophyllite that has been coated with aluminium titanates and calcium fluoride coating forms the barium sulfate coating, and its step is as follows:
(1) batching:
Prepare containing sulfate radicals compound water solution, the containing barium compound aqueous solution, barium sulfate sol or barium sulfate powdery pulp are standby; Concrete component target is: containing sulfate radicals compound water solution massfraction is 5～42.9%; Containing barium compound aqueous solution massfraction is 3～26%; In barium sulfate sol, the barium sulfate massfraction is: 5～25%; In the barium sulfate powdery pulp, the barium sulfate massfraction is 10～30%;
(2) surface coating has following Lung biopsy:
2.1 pyrophyllite is immersed in the containing sulfate radicals compound water solution, dries; And then the pyrophyllite that adopts the containing sulfate radicals compound water solution to process is immersed in the containing barium compound aqueous solution again and generates the barium sulfate layer, after cleaning, dry;
2.2 the containing sulfate radicals compound water solution is sprayed on to the surface of pyrophyllite to moistening, dries; And then the containing barium compound aqueous solution is sprayed on to the Surface Creation barium sulfate that adopts the pyrophyllite that the containing sulfate radicals compound water solution processed, after cleaning, dry;
2.3 barium sulfate sol is sprayed on to the surface of pyrophyllite to fully moistening, dries;
2.4 pyrophyllite is immersed in barium sulfate sol, in immersion process, constantly stir, soak time is 0.5 ~ 60min, takes out post-drying;
2.5 directly the barium sulfate powdery pulp is sprayed on to the surface of pyrophyllite until fully moistening, oven dry gets final product;
(3) thermal treatment
The pyrophyllite that surface is scribbled to one deck barium sulfate is placed in the heat treatment furnace of 600～900 ℃ and is incubated 1～4 hour, with the stove cooling, completes preparation;
Described containing sulfate radicals compound water solution is ammonium sulfate solution, potassium sulfate solution or aqueous sodium persulfate solution; The described containing barium compound aqueous solution is barium nitrate aqueous solution or barium chloride solution; The described fluorine cpd aqueous solution is ammonium fluoride aqueous solution, sodium fluoride aqueous solution or potassium fluoride aqueous solution, and the described calcium containing compound aqueous solution is calcium nitrate aqueous solution or calcium chloride water.
4. a kind of preparation method who is not stained with the aluminium pyrophyllite according to claim 1, is characterized in that, when not being stained with, the step of aluminium pyrophyllite surface coverage when the Calcium Fluoride (Fluorspan) layer is arranged is as follows:
(1) batching:
Prepare the fluorochemicals aqueous solution, the calcium containing compound aqueous solution, Calcium Fluoride (Fluorspan) colloidal sol or Calcium Fluoride (Fluorspan) powdery pulp are standby; Its concrete component target is: fluorochemicals aqueous solution massfraction is 2～48%; Calcium containing compound aqueous solution massfraction is 5～55%; In Calcium Fluoride (Fluorspan) colloidal sol, the Calcium Fluoride (Fluorspan) massfraction is 5～25%; In the Calcium Fluoride (Fluorspan) powdery pulp, Calcium Fluoride (Fluorspan) massfraction content is 10～30%;
(2) surface coating has following Lung biopsy:
2.1 pyrophyllite is immersed in the fluorochemicals aqueous solution, dries; And then the pyrophyllite that adopts the fluorochemicals aqueous solution to process is immersed in the calcium containing compound aqueous solution again and generates the Calcium Fluoride (Fluorspan) layer, after cleaning, dry;
2.2 the fluorochemicals aqueous solution is sprayed on to the surface of pyrophyllite to moistening, dries; And then the calcium containing compound aqueous solution is sprayed on to the Surface Creation Calcium Fluoride (Fluorspan) that adopts the pyrophyllite that the fluorochemicals aqueous solution processed, after cleaning, dry;
2.3 Calcium Fluoride (Fluorspan) colloidal sol is sprayed on to the surface of pyrophyllite to fully moistening, dries;
2.4 pyrophyllite is immersed in Calcium Fluoride (Fluorspan) colloidal sol, in immersion process, constantly stir, soak time is 0.5 ~ 60min, takes out post-drying;
2.5 directly the Calcium Fluoride (Fluorspan) powdery pulp is sprayed on to the surface of pyrophyllite until fully moistening, oven dry gets final product;
(3) thermal treatment:
The pyrophyllite that surface is scribbled to one deck Calcium Fluoride (Fluorspan) is placed in the heat treatment furnace of 800～1200 ℃ and is incubated 1～4 hour, with the stove cooling, completes preparation.
5. a kind of preparation method who is not stained with the aluminium pyrophyllite according to claim 1 is characterized in that:
The described fluorine cpd aqueous solution is ammonium fluoride aqueous solution, sodium fluoride aqueous solution or potassium fluoride aqueous solution; The described calcium containing compound aqueous solution is calcium nitrate aqueous solution or calcium chloride water.
6. a kind of preparation method who is not stained with the aluminium pyrophyllite according to claim 1, is characterized in that, when not being stained with, the step of aluminium pyrophyllite surface coverage when the barium sulfate layer is arranged is as follows:
(1) batching:
Prepare containing sulfate radicals compound water solution, the containing barium compound aqueous solution, barium sulfate sol or barium sulfate powdery pulp are standby; Concrete component target is: containing sulfate radicals compound water solution massfraction is 5～42.9%; Containing barium compound aqueous solution massfraction is 3～26%; In barium sulfate sol, the barium sulfate massfraction is: 5～25%; In the barium sulfate powdery pulp, the barium sulfate massfraction is 10～30%;
(2) surface coating has following Lung biopsy:
2.1 pyrophyllite is immersed in the containing sulfate radicals compound water solution, dries; And then the pyrophyllite that adopts the containing sulfate radicals compound water solution to process is immersed in the containing barium compound aqueous solution again and generates the barium sulfate layer, after cleaning, dry;
2.2 the containing sulfate radicals compound water solution is sprayed on to the surface of pyrophyllite to moistening, dries; And then the containing barium compound aqueous solution is sprayed on to the Surface Creation barium sulfate that adopts the pyrophyllite that the containing sulfate radicals compound water solution processed, after cleaning, dry;
2.3 barium sulfate sol is sprayed on to the surface of pyrophyllite to fully moistening, dries;
2.4 pyrophyllite is immersed in barium sulfate sol, in immersion process, constantly stir, soak time is 0.5 ~ 60min, takes out post-drying;
2.5 directly the barium sulfate powdery pulp is sprayed on to the surface of pyrophyllite until fully moistening, oven dry gets final product;
(3) thermal treatment
The pyrophyllite that surface is scribbled to one deck barium sulfate is placed in the heat treatment furnace of 600～900 ℃ and is incubated 1～4 hour, with the stove cooling, completes preparation.
7. a kind of preparation method who is not stained with the aluminium pyrophyllite according to claim 6, it is characterized in that: described containing sulfate radicals compound water solution is ammonium sulfate solution, potassium sulfate solution or aqueous sodium persulfate solution; The described containing barium compound aqueous solution is barium nitrate aqueous solution or barium chloride solution.
8. a kind of preparation method who is not stained with the aluminium pyrophyllite according to claim 1, is characterized in that, when not being stained with, the step of aluminium pyrophyllite surface coverage when the metatitanic acid aluminium lamination is arranged is as follows:
(1) batching:
Purchase commercially available or prepare titanium aluminium complex sol and the aluminium titanates powdery pulp is standby; Component target requires as follows:
A titanium aluminium complex sol: Ti
4+concentration is 0.2 ~ 0.3mol/L, Al
3+the titanium aluminium complex sol that concentration is 0.2～0.3mol/L; Add the Mg that molar fraction is 1.6～6% in colloidal sol
2+for stablizer; Or add the Mg that molar fraction is 3～5%
2+with the molar fraction Ce that is 0.4～0.8%
4+for stablizer; Or only add the Fe that molar fraction is 1.6～3.3%
3+for stablizer;
B aluminium titanates powdery pulp: consist of the Al that massfraction is 40～50%
2o
3with 50～60% TiO
2; Wherein adding massfraction is that 1～4%MgO is stablizer; Or add the CeO that MgO that massfraction is 1～4% and massfraction are 1～3%
2mixture is stablizer; Or to add massfraction be 3～8% Fe
2o
3for stablizer; Or add the ZrO that massfraction is 0.5～2%
2for stablizer;
(2) surface coating has following two kinds of methods:
2.1 pyrophyllite is immersed in titanium aluminium complex sol or aluminium titanates powdery pulp, in immersion process, constantly stir, soak time is 0.5 ~ 60min, takes out post-drying;
2.2 titanium aluminium complex sol or aluminium titanates powdery pulp are sprayed on to the pyrophyllite surface until fully moistening, and oven dry gets final product;
(3) thermal treatment
The heat treatment furnace that the pyrophyllite soaked or sprayed titanium aluminium complex sol or aluminium titanates powdery pulp is placed in to 1250～1450 ℃ is incubated 1～4 hour, with the stove cooling, completes preparation.
9. a kind of preparation method who is not stained with the aluminium pyrophyllite according to claim 2, is characterized in that, not being stained with aluminium pyrophyllite surface coverage has more than Calcium Fluoride (Fluorspan), barium sulfate, aluminium titanates when the two two layers of coatings combines, and following three kinds of methods are arranged:
1. when not being stained with aluminium pyrophyllite surface coverage when Calcium Fluoride (Fluorspan) and barium sulfate two layers of coatings are arranged:
(i) first pyrophyllite is carried out to the Calcium Fluoride (Fluorspan) coating, its step is as follows:
(1) batching:
Prepare the fluorochemicals aqueous solution, the calcium containing compound aqueous solution, Calcium Fluoride (Fluorspan) colloidal sol or Calcium Fluoride (Fluorspan) powdery pulp are standby; Its concrete component target is: fluorochemicals aqueous solution massfraction is 2～48%; Calcium containing compound aqueous solution massfraction is 5～55%; In Calcium Fluoride (Fluorspan) colloidal sol, the Calcium Fluoride (Fluorspan) massfraction is 5～25%; In the Calcium Fluoride (Fluorspan) powdery pulp, Calcium Fluoride (Fluorspan) massfraction content is 10～30%;
(2) surface coating has following Lung biopsy:
2.1 pyrophyllite is immersed in the fluorochemicals aqueous solution, dries; And then the pyrophyllite that adopts the fluorochemicals aqueous solution to process is immersed in the calcium containing compound aqueous solution again and generates the Calcium Fluoride (Fluorspan) layer, after cleaning, dry;
2.2 the fluorochemicals aqueous solution is sprayed on to the surface of pyrophyllite to moistening, dries; And then the calcium containing compound aqueous solution is sprayed on to the Surface Creation Calcium Fluoride (Fluorspan) that adopts the pyrophyllite that the fluorochemicals aqueous solution processed, after cleaning, dry;
2.3 Calcium Fluoride (Fluorspan) colloidal sol is sprayed on to the surface of pyrophyllite to fully moistening, dries;
2.4 pyrophyllite is immersed in Calcium Fluoride (Fluorspan) colloidal sol, in immersion process, constantly stir, soak time is 0.5 ~ 60min, takes out post-drying;
2.5 directly the Calcium Fluoride (Fluorspan) powdery pulp is sprayed on to the surface of pyrophyllite until fully moistening, oven dry gets final product;
(3) thermal treatment:
The pyrophyllite that surface is scribbled to one deck Calcium Fluoride (Fluorspan) is placed in the heat treatment furnace of 800～1200 ℃ and is incubated 1～4 hour, with the stove cooling, completes preparation;
(ii) again pyrophyllite is carried out to the barium sulfate coating, its step is as follows:
(1) batching:
Prepare containing sulfate radicals compound water solution, the containing barium compound aqueous solution, barium sulfate sol or barium sulfate powdery pulp are standby; Concrete component target is: containing sulfate radicals compound water solution massfraction is 5～42.9%; Containing barium compound aqueous solution massfraction is 3～26%; In barium sulfate sol, the barium sulfate massfraction is: 5～25%; In the barium sulfate powdery pulp, the barium sulfate massfraction is 10～30%;
(2) surface coating has following Lung biopsy:
2.1 pyrophyllite is immersed in the containing sulfate radicals compound water solution, dries; And then the pyrophyllite that adopts the containing sulfate radicals compound water solution to process is immersed in the containing barium compound aqueous solution again and generates the barium sulfate layer, after cleaning, dry;
2.2 the containing sulfate radicals compound water solution is sprayed on to the surface of pyrophyllite to moistening, dries; And then the containing barium compound aqueous solution is sprayed on to the Surface Creation barium sulfate that adopts the pyrophyllite that the containing sulfate radicals compound water solution processed, after cleaning, dry;
2.3 barium sulfate sol is sprayed on to the surface of pyrophyllite to fully moistening, dries;
2.4 pyrophyllite is immersed in barium sulfate sol, in immersion process, constantly stir, soak time is 0.5 ~ 60min, takes out post-drying;
2.5 directly the barium sulfate powdery pulp is sprayed on to the surface of pyrophyllite until fully moistening, oven dry gets final product;
(3) thermal treatment
The pyrophyllite that surface is scribbled to one deck barium sulfate is placed in the heat treatment furnace of 600～900 ℃ and is incubated 1～4 hour, with the stove cooling, completes preparation;
2. when not being stained with aluminium pyrophyllite surface coverage when Calcium Fluoride (Fluorspan) and two layers of coating of aluminium titanates are arranged:
(i) first pyrophyllite is carried out to the aluminium titanates coating, its step is as follows:
(1) batching:
Purchase commercially available or prepare titanium aluminium complex sol and the aluminium titanates powdery pulp is standby; Component target requires as follows:
A titanium aluminium complex sol: Ti
4+concentration is 0.2 ~ 0.3mol/L, Al
3+the titanium aluminium complex sol that concentration is 0.2～0.3mol/L; Add the Mg that molar fraction is 1.6～6% in colloidal sol
2+for stablizer; Or add the Mg that molar fraction is 3～5%
2+with the molar fraction Ce that is 0.4～0.8%
4+for stablizer; Or only add the Fe that molar fraction is 1.6～3.3%
3+for being stablizer;
B aluminium titanates powdery pulp: consist of the Al that massfraction is 40～50%
2o
3with 50～60% TiO
2; Wherein adding massfraction is that 1～4%MgO is stablizer; Or add the CeO that MgO that massfraction is 1～4% and massfraction are 1～3%
2mixture is stablizer; Or to add massfraction be 3～8% Fe
2o
3for stablizer; Or add the ZrO that massfraction is 0.5～2%
2for stablizer;
(2) surface coating has following two kinds of methods:
2.1 pyrophyllite is immersed in titanium aluminium complex sol or aluminium titanates powdery pulp, in immersion process, constantly stir, soak time is 0.5 ~ 60min, takes out post-drying;
2.2 titanium aluminium complex sol or aluminium titanates powdery pulp are sprayed on to the pyrophyllite surface until fully moistening, and oven dry gets final product;
(3) thermal treatment
The heat treatment furnace that the pyrophyllite soaked or sprayed titanium aluminium complex sol or aluminium titanates powdery pulp is placed in to 1250～1450 ℃ is incubated 1～4 hour, with the stove cooling, completes preparation;
(ii) again pyrophyllite is carried out to the Calcium Fluoride (Fluorspan) coating, its step is as follows:
(1) batching:
Prepare the fluorochemicals aqueous solution, the calcium containing compound aqueous solution, Calcium Fluoride (Fluorspan) colloidal sol or Calcium Fluoride (Fluorspan) powdery pulp are standby; Its concrete component target is: fluorochemicals aqueous solution massfraction is 2～48%; Calcium containing compound aqueous solution massfraction is 5～55%; In Calcium Fluoride (Fluorspan) colloidal sol, the Calcium Fluoride (Fluorspan) massfraction is 5～25%; In the Calcium Fluoride (Fluorspan) powdery pulp, Calcium Fluoride (Fluorspan) massfraction content is 10～30%;
(2) surface coating has following Lung biopsy:
2.1 pyrophyllite is immersed in the fluorochemicals aqueous solution, dries; And then the pyrophyllite that adopts the fluorochemicals aqueous solution to process is immersed in the calcium containing compound aqueous solution again and generates the Calcium Fluoride (Fluorspan) layer, after cleaning, dry;
2.2 the fluorochemicals aqueous solution is sprayed on to the surface of pyrophyllite to moistening, dries; And then the calcium containing compound aqueous solution is sprayed on to the Surface Creation Calcium Fluoride (Fluorspan) that adopts the pyrophyllite that the fluorochemicals aqueous solution processed, after cleaning, dry;
2.3 Calcium Fluoride (Fluorspan) colloidal sol is sprayed on to the surface of pyrophyllite to fully moistening, dries;
2.4 pyrophyllite is immersed in Calcium Fluoride (Fluorspan) colloidal sol, in immersion process, constantly stir, soak time is 0.5 ~ 60min, takes out post-drying;
2.5 directly the Calcium Fluoride (Fluorspan) powdery pulp is sprayed on to the surface of pyrophyllite until fully moistening, oven dry gets final product;
(3) thermal treatment:
The pyrophyllite that surface is scribbled to one deck Calcium Fluoride (Fluorspan) is placed in the heat treatment furnace of 800～1200 ℃ and is incubated 1～4 hour, with the stove cooling, completes preparation;
3. when not being stained with aluminium pyrophyllite surface coverage when aluminium titanates and two layers of coating of Calcium Fluoride (Fluorspan) are arranged:
(i) first pyrophyllite is carried out to the aluminium titanates coating, its step is as follows:
(1) batching:
Purchase commercially available or prepare titanium aluminium complex sol and the aluminium titanates powdery pulp is standby; Component target requires as follows:
A titanium aluminium complex sol: Ti
4+concentration is 0.2 ~ 0.3mol/L, Al
3+the titanium aluminium complex sol that concentration is 0.2～0.3mol/L; Add the Mg that molar fraction is 1.6～6% in colloidal sol
2+for stablizer; Or add the Mg that molar fraction is 3～5%
2+with the molar fraction Ce that is 0.4～0.8%
4+for stablizer; Or only add the Fe that molar fraction is 1.6～3.3%
3+for being stablizer;
B aluminium titanates powdery pulp: consist of the Al that massfraction is 40～50%
2o
3with 50～60% TiO
2; Wherein adding massfraction is that 1～4%MgO is stablizer; Or add the CeO that MgO that massfraction is 1～4% and massfraction are 1～3%
2mixture is stablizer; Or to add massfraction be 3～8% Fe
2o
3for stablizer; Or add the ZrO that massfraction is 0.5～2%
2for stablizer;
(2) surface coating has following two kinds of methods:
2.1 pyrophyllite is immersed in titanium aluminium complex sol or aluminium titanates powdery pulp, in immersion process, constantly stir, soak time is 0.5 ~ 60min, takes out post-drying;
2.2 titanium aluminium complex sol or aluminium titanates powdery pulp are sprayed on to the pyrophyllite surface until fully moistening, and oven dry gets final product;
(3) thermal treatment
The heat treatment furnace that the pyrophyllite soaked or sprayed titanium aluminium complex sol or aluminium titanates powdery pulp is placed in to 1250～1450 ℃ is incubated 1～4 hour, with the stove cooling, completes preparation;
(ii) again pyrophyllite is carried out to the Calcium Fluoride (Fluorspan) coating, its step is as follows:
(1) batching:
Prepare the fluorochemicals aqueous solution, the calcium containing compound aqueous solution, Calcium Fluoride (Fluorspan) colloidal sol or Calcium Fluoride (Fluorspan) powdery pulp are standby; Its concrete component target is: fluorochemicals aqueous solution massfraction is 2～48%; Calcium containing compound aqueous solution massfraction is 5～55%; In Calcium Fluoride (Fluorspan) colloidal sol, the Calcium Fluoride (Fluorspan) massfraction is 5～25%; In the Calcium Fluoride (Fluorspan) powdery pulp, Calcium Fluoride (Fluorspan) massfraction content is 10～30%;
(2) surface coating has following Lung biopsy:
2.1 pyrophyllite is immersed in the fluorochemicals aqueous solution, dries; And then the pyrophyllite that adopts the fluorochemicals aqueous solution to process is immersed in the calcium containing compound aqueous solution again and generates the Calcium Fluoride (Fluorspan) layer, after cleaning, dry;
2.2 the fluorochemicals aqueous solution is sprayed on to the surface of pyrophyllite to moistening, dries; And then the calcium containing compound aqueous solution is sprayed on to the Surface Creation Calcium Fluoride (Fluorspan) that adopts the pyrophyllite that the fluorochemicals aqueous solution processed, after cleaning, dry;
2.3 Calcium Fluoride (Fluorspan) colloidal sol is sprayed on to the surface of pyrophyllite to fully moistening, dries;
2.4 pyrophyllite is immersed in Calcium Fluoride (Fluorspan) colloidal sol, in immersion process, constantly stir, soak time is 0.5 ~ 60min, takes out post-drying;
2.5 directly the Calcium Fluoride (Fluorspan) powdery pulp is sprayed on to the surface of pyrophyllite until fully moistening, oven dry gets final product;
(3) thermal treatment:
The pyrophyllite that surface is scribbled to one deck Calcium Fluoride (Fluorspan) is placed in the heat treatment furnace of 800～1200 ℃ and is incubated 1～4 hour, with the stove cooling, completes preparation.
10. a kind of preparation method who is not stained with the aluminium pyrophyllite according to claim 9, is characterized in that, described containing sulfate radicals compound water solution is ammonium sulfate solution, potassium sulfate solution or aqueous sodium persulfate solution; The described containing barium compound aqueous solution is barium nitrate aqueous solution or barium chloride solution; The described fluorine cpd aqueous solution is ammonium fluoride aqueous solution, sodium fluoride aqueous solution or potassium fluoride aqueous solution; The described calcium containing compound aqueous solution is calcium nitrate aqueous solution or calcium chloride water.
11. a kind of preparation method who is not stained with the aluminium pyrophyllite according to claim 3, is characterized in that, when not being stained with aluminium pyrophyllite surface coverage when Calcium Fluoride (Fluorspan), barium sulfate, three layers of compound coating of aluminium titanates are arranged:
(i) first aluminium titanates is carried out in the pyrophyllite surface and apply, its step is as follows:
(1) batching:
Purchase commercially available or prepare titanium aluminium complex sol and the aluminium titanates powdery pulp is standby; Component target requires as follows:
A titanium aluminium complex sol: Ti
4+concentration is 0.2 ~ 0.3mol/L, Al
3+the titanium aluminium complex sol that concentration is 0.2～0.3mol/L; Add the Mg that molar fraction is 1.6～6% in colloidal sol
2+for stablizer; Or add the Mg that molar fraction is 3～5%
2+with the molar fraction Ce that is 0.4～0.8%
4+for stablizer; Or only add the Fe that molar fraction is 1.6～3.3%
3+for being stablizer;
B aluminium titanates powdery pulp: consist of the Al that massfraction is 40～50%
2o
3with 50～60% TiO
2; Wherein adding massfraction is that 1～4%MgO is stablizer; Or add the CeO that MgO that massfraction is 1～4% and massfraction are 1～3%
2mixture is stablizer; Or to add massfraction be 3～8% Fe
2o
3for stablizer; Or add the ZrO that massfraction is 0.5～2%
2for stablizer;
(2) surface coating has following two kinds of methods:
2.1 pyrophyllite is immersed in titanium aluminium complex sol or aluminium titanates powdery pulp, in immersion process, constantly stir, soak time is 0.5 ~ 60min, takes out post-drying;
2.2 titanium aluminium complex sol or aluminium titanates powdery pulp are sprayed on to the pyrophyllite surface until fully moistening, and oven dry gets final product;
(3) thermal treatment
The heat treatment furnace that the pyrophyllite soaked or sprayed titanium aluminium complex sol or aluminium titanates powdery pulp is placed in to 1250～1450 ℃ is incubated 1～4 hour, with the stove cooling, completes preparation;
(ii) covered aluminum titanate coatings and formed calcium fluoride coating again, its step is as follows:
(1) batching:
Prepare the fluorochemicals aqueous solution, the calcium containing compound aqueous solution, Calcium Fluoride (Fluorspan) colloidal sol or Calcium Fluoride (Fluorspan) powdery pulp are standby; Its concrete component target is: fluorochemicals aqueous solution massfraction is 2～48%; Calcium containing compound aqueous solution massfraction is 5～55%; In Calcium Fluoride (Fluorspan) colloidal sol, the Calcium Fluoride (Fluorspan) massfraction is 5～25%; In the Calcium Fluoride (Fluorspan) powdery pulp, Calcium Fluoride (Fluorspan) massfraction content is 10～30%;
(2) surface coating has following Lung biopsy:
2.1 pyrophyllite is immersed in the fluorochemicals aqueous solution, dries; And then the pyrophyllite that adopts the fluorochemicals aqueous solution to process is immersed in the calcium containing compound aqueous solution again and generates the Calcium Fluoride (Fluorspan) layer, after cleaning, dry;
2.2 the fluorochemicals aqueous solution is sprayed on to the surface of pyrophyllite to moistening, dries; And then the calcium containing compound aqueous solution is sprayed on to the Surface Creation Calcium Fluoride (Fluorspan) that adopts the pyrophyllite that the fluorochemicals aqueous solution processed, after cleaning, dry;
2.3 Calcium Fluoride (Fluorspan) colloidal sol is sprayed on to the surface of pyrophyllite to fully moistening, dries;
2.4 pyrophyllite is immersed in Calcium Fluoride (Fluorspan) colloidal sol, in immersion process, constantly stir, soak time is 0.5 ~ 60min, takes out post-drying;
2.5 directly the Calcium Fluoride (Fluorspan) powdery pulp is sprayed on to the surface of pyrophyllite until fully moistening, oven dry gets final product;
(3) thermal treatment:
The pyrophyllite that surface is scribbled to one deck Calcium Fluoride (Fluorspan) is placed in the heat treatment furnace of 800～1200 ℃ and is incubated 1～4 hour, with the stove cooling, completes preparation;
(iii) the pyrophyllite that has been coated with aluminium titanates and calcium fluoride coating forms the barium sulfate coating, and its step is as follows:
(1) batching:
Prepare containing sulfate radicals compound water solution, the containing barium compound aqueous solution, barium sulfate sol or barium sulfate powdery pulp are standby; Concrete component target is: containing sulfate radicals compound water solution massfraction is 5～42.9%; Containing barium compound aqueous solution massfraction is 3～26%; In barium sulfate sol, the barium sulfate massfraction is: 5～25%; In the barium sulfate powdery pulp, the barium sulfate massfraction is 10～30%;
(2) surface coating has following Lung biopsy:
2.1 pyrophyllite is immersed in the containing sulfate radicals compound water solution, dries; And then the pyrophyllite that adopts the containing sulfate radicals compound water solution to process is immersed in the containing barium compound aqueous solution again and generates the barium sulfate layer, after cleaning, dry;
2.2 the containing sulfate radicals compound water solution is sprayed on to the surface of pyrophyllite to moistening, dries; And then the containing barium compound aqueous solution is sprayed on to the Surface Creation barium sulfate that adopts the pyrophyllite that the containing sulfate radicals compound water solution processed, after cleaning, dry;
2.3 barium sulfate sol is sprayed on to the surface of pyrophyllite to fully moistening, dries;
2.4 pyrophyllite is immersed in barium sulfate sol, in immersion process, constantly stir, soak time is 0.5 ~ 60min, takes out post-drying;
2.5 directly the barium sulfate powdery pulp is sprayed on to the surface of pyrophyllite until fully moistening, oven dry gets final product;
(3) thermal treatment
The pyrophyllite that surface is scribbled to one deck barium sulfate is placed in the heat treatment furnace of 600～900 ℃ and is incubated 1～4 hour, with the stove cooling, completes preparation;
Described containing sulfate radicals compound water solution is ammonium sulfate solution, potassium sulfate solution or aqueous sodium persulfate solution; The described containing barium compound aqueous solution is barium nitrate aqueous solution or barium chloride solution; The described fluorine cpd aqueous solution is ammonium fluoride aqueous solution, sodium fluoride aqueous solution or potassium fluoride aqueous solution, and the described calcium containing compound aqueous solution is calcium nitrate aqueous solution or calcium chloride water.
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| CN101045828A (en) * | 2006-07-03 | 2007-10-03 | 张义纲 | Phosphate film-coated powder and preparation method thereof |
| CN101734935A (en) * | 2009-12-24 | 2010-06-16 | 中钢集团洛阳耐火材料研究院有限公司 | Aluminium liquid infiltration-resistant high-aluminum plastic material and preparation method |
| CN101734928A (en) * | 2009-12-24 | 2010-06-16 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of fused silica refractory casting material unwetted by aluminum liquid |
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| US20100270520A1 (en) * | 2007-05-14 | 2010-10-28 | Hi-Van Corporation | Carbon/aluminum complex compound and carbon/aluminum complex compound-coated inorganic compound |
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| CN101045828A (en) * | 2006-07-03 | 2007-10-03 | 张义纲 | Phosphate film-coated powder and preparation method thereof |
| CN101734935A (en) * | 2009-12-24 | 2010-06-16 | 中钢集团洛阳耐火材料研究院有限公司 | Aluminium liquid infiltration-resistant high-aluminum plastic material and preparation method |
| CN101734928A (en) * | 2009-12-24 | 2010-06-16 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of fused silica refractory casting material unwetted by aluminum liquid |
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