CN103708731B - A kind of nickel slag porous micro crystal material and preparation method thereof - Google Patents

A kind of nickel slag porous micro crystal material and preparation method thereof Download PDF

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CN103708731B
CN103708731B CN201310745768.7A CN201310745768A CN103708731B CN 103708731 B CN103708731 B CN 103708731B CN 201310745768 A CN201310745768 A CN 201310745768A CN 103708731 B CN103708731 B CN 103708731B
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crystal material
micro crystal
porous micro
nickel slag
parent glass
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CN103708731A (en
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曹建尉
王志
杜建亮
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Institute of Process Engineering of CAS
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Abstract

The present invention relates to a kind of nickel slag porous micro crystal material and preparation method thereof, with smelting ferronickel alloy waste residue for primary raw material, with SiO2、CaCO3、Na2CO3、ZnO、K2CO3It is adjuvant Deng additive and clarifier.Porous micro crystal material light weight of the present invention, insulation, wear-resistant, acid-alkali-corrosive-resisting, there is good machinability, can be widely applied to the heat-insulation and heat-preservation of the pipelines in field such as chemical industry, metallurgy, building decoration, oil, mine, machinery, storage tank, heat-exchange system, and the compound heat-insulation system worked under specific condition and sound-proof sound-absorbing system.

Description

A kind of nickel slag porous micro crystal material and preparation method thereof
Technical field
The present invention relates to a kind of porous micro crystal material, espespecially a kind of nickel slag porous micro crystal material utilizing the nickel slag discharged in dilval refining smelting process to prepare and preparation method, purpose is in that provide a kind of lightweight, insulation, wear-resistant, acid-alkali-corrosive-resisting and have the porous material of good machinability, industrial solid castoff nickel slag can be utilized in a large number, and product has excellent physical and mechanical property and stable chemical property.
Background technology
Nickel slag refers to a kind of solid slag of discharge, the granulated slag that the fused mass namely formed in smelting process is formed after Water Quenching in metal smelting nickel and ferronickel process.
The nickel slag discharge capacity of China is huge, and substantial amounts of nickel slag is thrown aside or piles up, and does not only take up a large amount of soil, increases Financial cost, but also surrounding is caused severe contamination, it is therefore necessary to nickel slag is administered and comprehensive utilization of resources.At present, nickel slag as dispensing and composite material produce cement, the gel component of building block and gather materials, the filling in mine material of mine goaf backfill, it addition, various cast stone plate, tubing etc. can be made after also can being fabricated to black glass, black ceramic and high temperature melting.
Utilize nickel slag to prepare the foam pyroceram of high added value, be possible not only to comprehensive utilization nickel slag and reduce environmental pollution, and there is good economic benefit.
Porous micro crystal material is with parent glass, nonmetallic ore etc. for primary raw material, add foaming agent, nucleator and additive etc., mix homogeneously forms batch after crushed, then it is put into batch in special mould to put in electric furnace and heats, through the novel porous microcrystal glass material that the techniques such as preheating, melted, foaming, crystallize, annealing are made.
Porous micro crystal material is heat insulation, the sound absorption of a kind of superior performance, the novel environmental-friendly construction material that moistureproof, fire-proof light is high-strength.Porous micro crystal material is compared with devitrified glass and foam glass, and devitrified glass unit weight is (> 2500kg/m greatly3), it is largely used to building and ornament materials.Foam glass light weight (≤500kg/m3), insulation, but mechanical strength is low, so being suitable for doing insulation material and being unfit to do body of wall load-bearing material.Porous micro crystal material is made up of glassy phase, crystal and pore three part.In the glassy phase matrix being uniform-distribution with a large amount of pore, uniformly dispersing substantial amounts of tiny crystals, makes glass and crystal network link together, forms hyalopilitic texture, substantially increase the mechanical strength of material, it is thus possible to be used for making body of wall load-bearing, decorative heat preservation material.
The construction features of porous micro crystal material itself and material behavior, being doomed porous micro crystal material has many premium properties: (1) is non-hygroscopic, do not absorb water;(2) there is good heat-proof quality, do not burn, can use in-270~900 DEG C of wide temperature range;(3) there is good sound absorbing capabilities;(4) mechanical strength is high, and is prone to process, cut or glue be combined into variously-shaped goods;(5) non-efflorescing cementitious, not aging, nontoxic, "dead" and corrosivity;(6) not by rat eaten insect bite and microbiologic(al) corrosion;(7) there is good chemical stability, all of chemical erosion beyond the fluoric acid of resistance to dehydrogenation.
Porous micro crystal material is mainly used in: the load bearing wall of (1) building, ceiling, enclosure wall, internal partition wall;(2) cryogenic piping, equipment, container and storage tank;(3) gentle high-temperature pipe, equipment in;(4) deep fat and heated bitumen storage tank;(5) petrochemical industry, sulfuration production process;(6) fluid heat transfer system;(7) compressor, the sound insulation of Ventilator Room and sound-absorbing wall;(8) the compound heat-insulation system worked under specific condition.
In sum, yet there are no report utilizes nickel slag to prepare porous micro crystal material, the present invention utilizes nickel slag to prepare porous micro crystal material for primary raw material, both can dissolve in a large number nickel slag, alleviate its pollution to soil and environment, the high value added product of low cost can be produced again, there is significant economy, environmental and social benefits.
Summary of the invention
It is an object of the invention to big argument, recycling nickel slag, by the production technology cleaned, preparing light thermal-insulation, wear-resistant corrosion-resistant, porous micro crystal material that intensity is higher, this kind of porous micro crystal material can have different colors, and can be cut into different shapes according to actual needs.
In order to achieve the above object, the present invention is realized by scheme in detail below.
A kind of nickel slag porous micro crystal material, it is made up of parent glass, foaming agent, foam stabilizer, modifying ingredients and coloring agent, wherein parent glass accounts for the 85.0-90.0% of gross weight, foaming agent accounts for the 3.0-10.0% of gross weight, foam stabilizer accounts for the 2.0-6.0% of gross weight, modifying ingredients accounts for the 0-5.0% of gross weight, and coloring agent accounts for the 0-2.0% of gross weight.
The raw material of described parent glass is made up of nickel slag, additive and clarifier of fluxing, and wherein nickel slag accounts for the 50.0-76.0% of gross weight, and additive accounts for the 20.0-27.0% of gross weight, and clarifier of fluxing accounts for the 5.0-8.0% of gross weight;Described additive is SiO2、CaCO3、Na2CO3、CaF2、ZnO、Al2O3、BaCO3、K2CO3、MgO、NaNO3In five kinds or more than five kinds or all, the weight ratio between them is 15-20:7-11:6-13:0-15:0-6:7-12:0-3:1-4:0-2:0-7;Described clarifier of fluxing is CeO2、Na2O、NH4NO3And Na2SO4In one or more, the weight ratio between them is 0-4:0-7:2-5:0-15.
The main chemical compositions of described nickel slag is 0.1-0.6%Na2O、17.0-24.0%MgO、3.0-5.0%Al2O3、50.0-53.0%SiO2、12.0-15.0%CaO、0.05-0.15%TiO2、0.9-2.0%Cr2O3、0.3-0.7%MnO、4.0-10.0%Fe2O3, all the other compositions be CuO, ZnO, SrO, content is respectively less than 0.01%.
Described additive can also by containing SiO2、CaO、Na2O、CaF2、ZnO、Al2O3、BaO、K2The mineral of O, MgO, industrial chemicals, mine tailing, waste residue provide;Described mine tailing includes gangue or adopting iron ore tailings;Described waste residue includes blast furnace slag, phosphorus slag or boron mud.
Described foaming agent is SiC, carbon dust (C), calcium carbonate (CaCO3), MnO2、Fe2O3In one or more or all, the weight ratio between them is 2-5:0-3:0-2:0-3:0-1.
Described foam stabilizer be in sodium phosphate, phosphoric acid, sodium dihydrogen phosphate, magnesium phosphate one or more or all, the weight ratio between them is 1-6:0-2:0-3:0-4.
Described modifying ingredients be in Borax, boric acid, sodium nitrate, prodan, sodium carbonate or magnesium carbonate one or more or all, the weight ratio between them is 2-5:0-3:0-2:0-5:0-3:0-2.
Add according to actual needs and obtain porous micro crystal material containing what the coloring agent of Fe, Mn, Cu, Cr, Co, Ni, Ti coloring ion made different colours.
The moulding of described nickel slag porous micro crystal material is tabular or cylindrical shape or Curved, or other shape any processed according to actual needs.
A kind of preparation method of nickel slag porous micro crystal material,
First preparing parent glass, then pulverized by parent glass and mix homogeneously with foaming agent, foam stabilizer, modifying ingredients and coloring agent, load die for molding, after molding, kiln kiln roasting sent into by biscuit and mould, obtains porous micro crystal material, specifically comprises the following steps that
(1) prepared by parent glass
1. dispensing: nickel slag and various adjuvant are pulverized, then crosses 40 mesh sieves, and various adjuvants refer to additive and clarifier of fluxing;Accounting for the nickel slag of gross weight 55.0-65.0% according to composition proportion accurate weighing, account for the additive of gross weight 20.0-27.0%, account for the clarifier of fluxing of gross weight 5.0-8.0%, wherein additive is SiO2、CaCO3、Na2CO3、CaF2、ZnO、Al2O3、BaCO3、K2CO3、MgO、NaNO3In five kinds or more than five kinds or all, the weight ratio between them is 15-20:7-11:6-13:0-15:0-6:7-12:0-3:1-4:0-2:0-7;Described clarifier of fluxing is CeO2、Na2O、NH4NO3And Na2SO4In one or more, the weight ratio between them is 0-4:0-7:2-5:0-15.;Clear agent of fluxing is CeO2、Na2O、NH4NO3And Na2SO4In one or more or all, the weight ratio between them is 0-4:0-7:2-5:0-15.Various raw materials put into batch mixer or agitator, it is possible to additionally incorporate the water of raw material gross weight 1.0-6.0%, stir, make parent glass batch.
The main chemical compositions of nickel slag is 0.1-0.6%Na2O、17.0-24.0%MgO、3.0-5.0%Al2O3、50.0-53.0%SiO2、12.0-15.0%CaO、0.05-0.15%TiO2、0.9-2.0%Cr2O3、0.3-0.7%MnO、4.0-10.0%Fe2O3, other composition be surplus.
Or additive and clarifier of fluxing are pulverized, then crosses 40 mesh sieves, account for the additive of gross weight 20.0-27.0wt% according to composition proportion accurate weighing, account for the clarifier of fluxing of gross weight 5.0-8.0wt%;Additive is sufficiently mixed with clarifier of fluxing, forms uniform adjuvant batch;
Additionally, the raw-material additive of parent glass also can by containing SiO2、CaO、Na2O、CaF2、ZnO、Al2O3、BaO、K2The mineral of O, MgO, industrial chemicals, mine tailing (gangue, adopting iron ore tailings), waste residue (blast furnace slag, phosphorus slag, boron mud) provide.
2. fusing: parent glass batch is melted within the scope of 1450-1560 DEG C 1.0-6.0h, makes glass melts, then at 1350-1500 DEG C of scope inside holding 1.0-3.0h, homogenizing, fining glass liquid, obtain the high temp glass melt of molten state.
Or adjuvant batch is put in the hot nickel slag of the high temperature accounting for gross weight 55.0-65.0wt%, 2.0-4.0h is melted within the scope of 1460-1560 DEG C, make glass melts, then at 1350-1500 DEG C of scope inside holding 1.0-3.0h, homogenizing, fining glass liquid, obtain the high temp glass melt of molten state;
3. cooling: vitreous humour is by rolling basis of formation glass plate;Maybe the vitreous humour of clarification is poured into molding in the steel die preheated, obtains parent glass block;Or by dry after vitreous humour direct-water-quenching, obtain parent glass pellet.
4. powder process: by parent glass plate (block, pellet) pulverizing, ball milling, obtain parent glass powder.
(2) preparation of nickel slag porous micro crystal material
First, according to the raw material ratio accurate weighing parent glass powder of porous micro crystal material, foaming agent, foam stabilizer, modifying ingredients and coloring agent, parent glass accounts for the 85.0-90.0% of gross weight, foaming agent accounts for the 3.0-10.0% of gross weight, foam stabilizer accounts for the 2.0-6.0% of gross weight, modifying ingredients accounts for the 0-5.0% of gross weight, and coloring agent accounts for the 0-2.0% of gross weight.Wherein foaming agent is SiC, carbon dust (C), calcium carbonate (CaCO3), MnO2、Fe2O3In one or more or all, the weight ratio between them is 2-5:0-3:0-2:0-3:0-1.Foam stabilizer be in sodium phosphate, phosphoric acid, sodium dihydrogen phosphate, magnesium phosphate one or more or all, the weight ratio between them is 1-6:0-2:0-3:0-4.Modifying ingredients be in Borax, boric acid, sodium nitrate, prodan, sodium carbonate, magnesium carbonate one or more or all, the weight ratio between them is 2-5:0-3:0-2:0-5:0-3:0-2.Coloring agent color according to actual needs can add the coloring agent containing coloring ions such as Fe, Mn, Cu, Cr, Co, Ni, Ti.
Then, below raw material mixing and ball milling to 180 orders, reach Homogeneous phase mixing, form porous micro crystal material raw material stand-by.
(3) molding
First, releasing agent (1-3:1-5 mixing pressed by aluminium oxide and waterglass) being brushed on heat-resisting die surface, then, the raw material mixed is loaded die for molding, the bulk density making base substrate is 0.5-1.0g/cm3
(4) burn till
First, base substrate is sent into together with mould kiln, with the programming rate of 8-20 DEG C/min, be warming up to 950-1250 DEG C, be incubated 10-30min, then be cooled to less than 600 DEG C and be incubated 0-4.0h, formation cellular glass;Then, it is warming up to 650-800 DEG C with the programming rate of 5-20 DEG C/min, is incubated 2.0-6.0h coring then the programming rate with 5-15 DEG C/min, is warming up to 780-940 DEG C, be incubated 2.0-4.0h crystallization, obtain porous micro crystal material.
Or base substrate is sent into together with mould kiln, with the programming rate of 5-20 DEG C/min, is warming up to 950-1250 DEG C, be incubated 20-45min, then be cooled to less than 600 DEG C and be incubated 0-4.0h, obtain porous micro crystal material.
The profile of described nickel slag porous micro crystal material is tabular or cylindrical shape or Curved, or other shape any processed according to actual needs.
Beneficial effects of the present invention and advantage are in that:
(1) can comprehensive utilization of resources nickel slag effectively
The present invention foam pyroceram with nickel slag for main material production high added value, nickel slag volume in the parent glass raw material of porous micro crystal material can regulate within the scope of 55.0-65.0wt.%, it is possible not only to reduce the production cost of porous micro crystal material, it is also possible to alleviate the industrial solid castoff pollution to environment.
(2) porous micro crystal material is excellent physical and mechanical property and chemical stability
1. lightweight, high insulating effect
Porous micro crystal material internal structure is based on closo pore, average pore size 0.2-3.0mm, density≤0.9g/cm3, heat preservation and insulation is excellent, heat conductivity≤0.15W/m K.
2. mechanical strength is high, wear-resistant corrosion-resistant
Porous micro crystal material comprcssive strength >=10.0MPa, wearability≤2.3 × 10-3g/cm2, acid-alkali-corrosive-resisting (acid resistance k≤0.05%, alkali resistance k≤0.03%).
3. machinable function admirable
Porous micro crystal material according to actual needs, can be cut into different size and shape.
(3) hot nickel slag and cold conditions nickel slag resource utilization process
The present invention not only provides the technique utilizing cold conditions nickel slag to produce porous micro crystal material, herein in connection with the actual discharge process of the hot nickel slag of high temperature, it is provided that a kind of technique directly utilizing high-temperature molten-state nickel slag production porous micro crystal material.
(4) porous micro crystal material single firing process
The present invention through once-firing, can complete the processes such as melted, the foaming of porous material, crystallization, annealing.
Accompanying drawing explanation
Fig. 1 is the preparation technology of cold conditions nickel slag parent glass of the present invention;
Fig. 2 is the preparation technology of the hot nickel slag parent glass of the present invention;
Fig. 3 is the preparation technology of the porous micro crystal material of the present invention.
Detailed description of the invention
The present invention is discussed in detail below in conjunction with drawings and the specific embodiments.But below example is only limitted to explain the present invention, and protection scope of the present invention should include the full content of claim, is not limited only to the present embodiment.And the present invention is by example below, those skilled in the art are able to be fully achieved all the elements that the claims in the present invention record.
Embodiment 1
(1) preparation of parent glass
Cold conditions nickel slag and various adjuvant are pulverized, then crosses 40 mesh sieves, according to 60.0 kilograms of cold conditions nickel slags of composition proportion accurate weighing, 8.0 kilograms of calcium carbonate, 9.0 kilograms of aluminium sesquioxide, 18.0 kilograms of silicon dioxide, 9.0 kilograms of sodium carbonate, 3.0 kg of potassium carbonate.Various raw materials put into batch mixer or agitator, it is possible to additionally incorporate the water of raw material gross weight 5.0%, stir, make parent glass batch.Parent glass batch is melted within the scope of 1485-1520 DEG C 2.0-4.0h, makes glass melts, then at 1350-1370 DEG C of scope inside holding 1.0-3.0h, homogenizing, fining glass liquid, obtain the high temp glass melt (as shown in Figure 1) of molten state.
Or various adjuvants are pulverized, then crosses 40 mesh sieves, according to 8.0 kilograms of calcium carbonate of composition proportion accurate weighing, 9.0 kilograms of aluminium sesquioxide, 18.0 kilograms of silicon dioxide, 9.0 kilograms of sodium carbonate, 3.0 kg of potassium carbonate.Various adjuvants put into batch mixer or agitator, it is possible to additionally incorporate the water of adjuvant gross weight 5.0%, stir, make parent glass batch adjuvant, are joined by parent glass batch adjuvant in 60.0 kilograms of hot nickel slags of high temperature.Within the scope of 1485-1520 DEG C, melt 2.0-4.0h, make glass melts, then at 1350-1370 DEG C of scope inside holding 1.0-3.0h, homogenizing, fining glass liquid, obtain the high temp glass melt (as shown in Figure 2) of molten state.
Vitreous humour is by rolling basis of formation glass plate;Maybe the vitreous humour of clarification is poured into molding in the steel die preheated, obtains parent glass block;Or by dry after vitreous humour direct-water-quenching, obtain parent glass pellet.By parent glass plate (block, pellet) pulverizing, ball milling, obtain parent glass powder.
(2) preparation (as shown in Figure 3) of nickel slag porous micro crystal material
First, according to the raw material ratio of porous micro crystal material, accurate weighing 85.0% parent glass powder, 6.0% foaming agent, 4.0% foam stabilizer, 4.0% modifying ingredients and 1.0% coloring agent.Wherein foaming agent is SiC, carbon dust (C), MnO2、Fe2O3, the weight ratio between them is 5:1:2:1.Foam stabilizer is sodium phosphate, magnesium phosphate, and the weight ratio between them is 4:1.Modifying ingredients is Borax, boric acid, and the weight ratio between them is 3:1.Coloring agent color according to actual needs can add the coloring agent containing coloring ions such as Fe, Mn, Cu, Cr, Co, Ni, Ti.
Then, below raw material mixing and ball milling to 180 orders, reach Homogeneous phase mixing, form porous micro crystal material raw material stand-by.
(3) molding
First, releasing agent is brushed on heat-resisting die surface, then, the crystallite foam glass raw material mixed is loaded die for molding.
(4) burn till
First, base substrate is sent into together with mould kiln, with the programming rate of 15 DEG C/min, be warming up to 1180 DEG C, be incubated 20min, then be cooled to less than 500 DEG C and be incubated 3.0h, formation foam glass;Then, it is warming up to 650 DEG C with the programming rate of 15 DEG C/min, is incubated 2.0h coring then the programming rate with 8 DEG C/min, is warming up to 920 DEG C, be incubated 3.0h crystallization, obtain porous micro crystal material.
The density of this porous micro crystal material is 0.70g/cm3, average bubble diameter 0.9mm, heat conductivity 0.08W/m K, comprcssive strength 12MPa, acid resistance k=0.05%, alkali resistance k=0.03%.
Embodiment 2
(1) preparation of parent glass
Cold conditions nickel slag and various adjuvant are pulverized, then 40 mesh sieves are crossed, according to 55.0 kilograms of cold conditions nickel slags of composition proportion accurate weighing, 8.0 kilograms of calcium carbonate, 2.0 kilograms of calcium fluoride, 9.0 kilograms of aluminium sesquioxide, 2.0 kilograms of sodium nitrates, 1.0 kilograms of brium carbonates, 18.0 kilograms of silicon dioxide, 9.0 kilograms of sodium carbonate, 3.0 kg of potassium carbonate..Various raw materials put into batch mixer or agitator, it is possible to additionally incorporate the water of raw material gross weight 5.0%, stir, make parent glass batch.Parent glass batch is melted within the scope of 1470-1500 DEG C 2.0-4.0h, makes glass melts, then at 1300-1350 DEG C of scope inside holding 1.0-3.0h, homogenizing, fining glass liquid, obtain the high temp glass melt (as shown in Figure 1) of molten state.
Or various adjuvants are pulverized, then crosses 40 mesh sieves, according to 8.0 kilograms of calcium carbonate of composition proportion accurate weighing, 2.0 kilograms of calcium fluoride, 9.0 kilograms of aluminium sesquioxide, 2.0 kilograms of sodium nitrates, 1.0 kilograms of brium carbonates, 18.0 kilogram silicon dioxide, 9.0 kilograms of sodium carbonate, 3.0 kg of potassium carbonate.Various adjuvants put into batch mixer or agitator, it is possible to additionally incorporate the water of adjuvant gross weight 5.0%, stir, make parent glass batch adjuvant, are joined by parent glass batch adjuvant in 55.0 kilograms of hot nickel slags of high temperature.Within the scope of 1470-1500 DEG C, melt 2.0-4.0h, make glass melts, then at 1300-1350 DEG C of scope inside holding 1.0-3.0h, homogenizing, fining glass liquid, obtain the high temp glass melt (as shown in Figure 2) of molten state.
Vitreous humour is by rolling basis of formation glass plate;Maybe the vitreous humour of clarification is poured into molding in the steel die preheated, obtains parent glass block;Or by dry after vitreous humour direct-water-quenching, obtain parent glass pellet.By parent glass plate (block, pellet) pulverizing, ball milling, obtain parent glass powder.
(2) preparation (as shown in Figure 3) of nickel slag porous micro crystal material
First, according to the raw material ratio of porous micro crystal material, accurate weighing 87.0% parent glass powder, 4.5% foaming agent, 5.0% foam stabilizer, 2.5% modifying ingredients and 0.5% coloring agent.Wherein foaming agent is SiC, carbon dust (C), MnO2, the weight ratio between them is 5:1:1.Foam stabilizer is sodium phosphate, magnesium phosphate, and the weight ratio between them is 5:1.Modifying ingredients is Borax, boric acid, prodan, and the weight ratio between them is 4:2:1.Coloring agent color according to actual needs can add the coloring agent containing coloring ions such as Fe, Mn, Cu, Cr, Co, Ni, Ti.
Then, below raw material mixing and ball milling to 180 orders, reach Homogeneous phase mixing, form porous micro crystal material raw material stand-by.
(3) molding
First, releasing agent is brushed on heat-resisting die surface, then, the crystallite foam glass raw material mixed is loaded die for molding.
(4) burn till
First, base substrate is sent into together with mould kiln, with the programming rate of 15 DEG C/min, be warming up to 1150 DEG C, be incubated 15min, then be cooled to less than 500 DEG C and be incubated 4.0h, formation foam glass;Then, it is warming up to 735 DEG C with the programming rate of 15 DEG C/min, is incubated 3.5h coring then the programming rate with 5 DEG C/min, is warming up to 840 DEG C, be incubated 2.0h crystallization, obtain porous micro crystal material.
The density of this porous micro crystal material is 0.63g/cm3, average bubble diameter 1.7mm, heat conductivity 0.11W/m K, comprcssive strength 10.3MPa, acid resistance k=0.04%, alkali resistance k=0.03%.
Embodiment 3
(1) preparation of parent glass
Cold conditions nickel slag and various adjuvant are pulverized, then crosses 40 mesh sieves, according to 65.0 kilograms of cold conditions nickel slags of composition proportion accurate weighing, 7.0 kilograms of calcium carbonate, 8.5 kilograms of aluminium sesquioxide, 15.5 kilograms of silicon dioxide, 9.0 kilograms of sodium carbonate, 3.5 kg of potassium carbonate, 2.0 kilograms of sodium nitrates, 0.5 kilogram of zinc oxide.Various raw materials put into batch mixer or agitator, it is possible to additionally incorporate the water of raw material gross weight 5.0%, stir, make parent glass batch.Parent glass batch is melted within the scope of 1485-1520 DEG C 2.0-4.0h, makes glass melts, then at 1350-1370 DEG C of scope inside holding 1.0-3.0h, homogenizing, fining glass liquid, obtain the high temp glass melt (as shown in Figure 1) of molten state.
Or various adjuvants are pulverized, then crosses 40 mesh sieves, according to 7.0 kilograms of calcium carbonate of composition proportion accurate weighing, 8.5 kilograms of aluminium sesquioxide, 15.5 kilograms of silicon dioxide, 9.0 kilograms of sodium carbonate, 3.5 kg of potassium carbonate, 1.5 kilograms of sodium nitrates, 0.5 kilogram of zinc oxide.Various adjuvants put into batch mixer or agitator, it is possible to additionally incorporate the water of adjuvant gross weight 5.0%, stir, make parent glass batch adjuvant, are joined by parent glass batch adjuvant in 65.0 kilograms of hot nickel slags of high temperature.Within the scope of 1485-1520 DEG C, melt 2.0-4.0h, make glass melts, then at 1350-1370 DEG C of scope inside holding 1.0-3.0h, homogenizing, fining glass liquid, obtain the high temp glass melt (as shown in Figure 2) of molten state.
Vitreous humour is by rolling basis of formation glass plate;Maybe the vitreous humour of clarification is poured into molding in the steel die preheated, obtains parent glass block;Or by dry after vitreous humour direct-water-quenching, obtain parent glass pellet.By parent glass plate (block, pellet) pulverizing, ball milling, obtain parent glass powder.
(2) preparation (as shown in Figure 3) of nickel slag porous micro crystal material
First, according to the raw material ratio of porous micro crystal material, accurate weighing 90.0% parent glass powder, 4.0% foaming agent, 3.0% foam stabilizer, 2.7% modifying ingredients and 0.3% coloring agent.Wherein foaming agent is SiC, carbon dust (C), calcium carbonate (CaCO3), the weight ratio between them is 5:1:1.Foam stabilizer is sodium phosphate, sodium dihydrogen phosphate, magnesium phosphate, and the weight ratio between them is 4:1:1.Modifying ingredients is Borax, sodium nitrate, prodan, and the weight ratio between them is 5:1:3.Coloring agent color according to actual needs can add the coloring agent containing coloring ions such as Fe, Mn, Cu, Cr, Co, Ni, Ti.
Then, below raw material mixing and ball milling to 180 orders, reach Homogeneous phase mixing, form porous micro crystal material raw material stand-by.
(3) molding
First, releasing agent is brushed on heat-resisting die surface, then, the crystallite foam glass raw material mixed is loaded die for molding.
(4) burn till
First, base substrate is sent into together with mould kiln, with the programming rate of 18 DEG C/min, be warming up to 1160 DEG C, be incubated 20min, then be cooled to less than 500 DEG C and be incubated 3.0h, formation foam glass;Then, it is warming up to 650 DEG C with the programming rate of 10 DEG C/min, is incubated 3.0h coring then the programming rate with 7 DEG C/min, is warming up to 920 DEG C, be incubated 2.0h crystallization, obtain porous micro crystal material.
The density of this porous micro crystal material is 0.66g/cm3, average bubble diameter 1.2mm, heat conductivity 0.95W/m K, comprcssive strength 11.0MPa, acid resistance k=0.04%, alkali resistance k=0.025%.
In a word, the porous micro crystal material light weight of the present invention, insulation, wear-resistant, acid-alkali-corrosive-resisting, there is good machinability, can be widely applied to the heat-insulation and heat-preservation of the pipelines in field such as chemical industry, metallurgy, building decoration, oil, mine, machinery, storage tank, heat-exchange system, and the compound heat-insulation system worked under specific condition and sound-proof sound-absorbing system.
It should be noted that according to the various embodiments described above of the present invention, those skilled in the art are the four corners that can realize independent claims of the present invention and appurtenance completely, it is achieved process and the same the various embodiments described above of method;And non-elaborated part of the present invention belongs to techniques well known.
The above; being only part detailed description of the invention of the present invention, but protection scope of the present invention is not limited thereto, any those skilled in the art are in the technical scope that the invention discloses; the change that can readily occur in or replacement, all should be encompassed within protection scope of the present invention.

Claims (6)

1. a nickel slag porous micro crystal material, it is characterized in that: be made up of parent glass, foaming agent, foam stabilizer, modifying ingredients and coloring agent, wherein parent glass accounts for the 85.0-90.0% of gross weight, foaming agent accounts for the 3.0-10.0% of gross weight, foam stabilizer accounts for the 2.0-6.0% of gross weight, modifying ingredients accounts for the 0-5.0% of gross weight, and coloring agent accounts for the 0-2.0% of gross weight;
The raw material of described parent glass is made up of nickel slag, additive and clarifier of fluxing, and wherein nickel slag accounts for the 55.0-65.0% of gross weight, and additive accounts for the 20.0-27.0% of gross weight, and clarifier of fluxing accounts for the 5.0-8.0% of gross weight;Described additive is SiO2、CaCO3、Na2CO3、CaF2、ZnO、Al2O3、BaCO3、K2CO3、MgO、NaNO3In five kinds or more than five kinds or all, the weight ratio between them is 15-20:7-11:6-13:0-15:0-6:7-12:0-3:1-4:0-2:0-7;Described clarifier of fluxing is CeO2、Na2O、NH4NO3And Na2SO4In one or more, the weight ratio between them is 0-4:0-7:2-5:0-15;
The main chemical compositions of described nickel slag is 0.1-0.6%Na2O, 17.0-24.0%MgO, 3.0-5.0%Al2O3, 50.0-53.0%SiO2, 12.0-15.0%CaO, 0.05-0.15%TiO2, 0.9-2.0%Cr2O3, 0.3-0.7%MnO, 4.0-10.0%Fe2O3, all the other compositions be CuO, ZnO, SrO, content is respectively less than 0.01%;
Described foaming agent is SiC, carbon dust (C), calcium carbonate (CaCO3)、MnO2、Fe2O3In one or more or all, the weight ratio between them is 2-5:0-3:0-2:0-3:0-1.
2. nickel slag porous micro crystal material according to claim 1, it is characterised in that: described foam stabilizer be in sodium phosphate, phosphoric acid, sodium dihydrogen phosphate, magnesium phosphate one or more or all, the weight ratio between them is 1-6:0-2:0-3:0-4.
3. nickel slag porous micro crystal material according to claim 1, it is characterized in that: described modifying ingredients be in Borax, boric acid, sodium nitrate, prodan, sodium carbonate or magnesium carbonate one or more or all, the weight ratio between them is 2-5:0-3:0-2:0-5:0-3:0-2.
4. nickel slag porous micro crystal material according to claim 1, it is characterised in that: add according to actual needs and obtain porous micro crystal material containing what the coloring agent of Fe, Mn, Cu, Cr, Co, Ni, Ti coloring ion made different colours.
5. nickel slag porous micro crystal material according to claim 1, it is characterised in that: the moulding of described nickel slag porous micro crystal material is tabular or cylindrical shape or Curved, or other shape any processed according to actual needs.
6. prepare the method for nickel slag porous micro crystal material described in claim 1 for one kind, it is characterized in that: first prepare parent glass, then parent glass is pulverized and mix homogeneously with foaming agent, foam stabilizer, modifying ingredients and coloring agent, load and mould is sent into kiln kiln roasting, obtain porous micro crystal material, specifically comprise the following steps that
(1) prepared by parent glass
1. dispensing: nickel slag, additive and clarifier of fluxing are pulverized, then 40 mesh sieves are crossed, the nickel slag of raw material gross weight 55.0-65.0wt% is accounted for according to composition proportion accurate weighing, account for the additive of raw material gross weight 20.0-27.0wt%, accounting for the clarifier of fluxing of raw material gross weight 5.0-8.0wt%, various raw materials put into batch mixer or agitator, it is possible to additionally incorporate the water of raw material gross weight 1.0-6.0%, stir, make parent glass batch;
2. fusing: parent glass batch is melted within the scope of 1450-1560 DEG C 1.0-6.0h, makes glass melts, then at 1350-1500 DEG C of scope inside holding 1.0-3.0h, homogenizing, fining glass liquid, obtain the high temp glass melt of molten state;
3. cooling: vitreous humour is by rolling basis of formation glass plate;Maybe the vitreous humour of clarification is poured into molding in the steel die preheated, obtains parent glass block;Or by dry after vitreous humour direct-water-quenching, obtain parent glass pellet;
4. powder: parent glass plate or parent glass block or parent glass pellet are pulverized, ball milling, obtains parent glass powder;
(2) prepared by nickel slag porous micro crystal material
1. first, according to the raw material ratio accurate weighing parent glass powder of nickel slag porous micro crystal material, foaming agent, foam stabilizer and modifying ingredients;Then, below they mixing and ball milling to 180 orders, reach Homogeneous phase mixing, form foam pyroceram raw material stand-by;
2. molding
First, releasing agent and aluminium oxide and waterglass being mixed brushing by a certain percentage on heat-resisting die surface, then, the porous micro crystal material raw material that will mix loads die for molding, and the bulk density making base substrate is 0.5-1.0g/cm3
3. burn till
First, base substrate is sent into together with mould kiln, with the programming rate of 8-20 DEG C/min, be warming up to 950-1250 DEG C, be incubated 10-30min, then be cooled to less than 600 DEG C and be incubated 0-4.0h, formation foam glass;Then, it is warming up to 650-800 DEG C with the programming rate of 5-20 DEG C/min, is incubated 2.0-6.0h coring then the programming rate with 5-15 DEG C/min, is warming up to 780-940 DEG C, be incubated 2.0-4.0h crystallization, obtain porous micro crystal material;Or base substrate is sent into together with mould kiln, with the programming rate of 5-20 DEG C/min, is warming up to 950-1250 DEG C, be incubated 20-45min, then be cooled to less than 600 DEG C and be incubated 0-4.0h, obtain porous micro crystal material.
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