CN109320219A - A kind of high-performance aluminum chrome refractory and preparation method thereof and application - Google Patents

A kind of high-performance aluminum chrome refractory and preparation method thereof and application Download PDF

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CN109320219A
CN109320219A CN201811343210.5A CN201811343210A CN109320219A CN 109320219 A CN109320219 A CN 109320219A CN 201811343210 A CN201811343210 A CN 201811343210A CN 109320219 A CN109320219 A CN 109320219A
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aluminium
parts
added
chrome
powder
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CN109320219B (en
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王树山
谷慧鹏
王珏
张海峰
王利
付伟
金耀东
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Liaoning Zhongmei High-Temperature Materials Co Ltd
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Liaoning Zhongmei High-Temperature Materials Co Ltd
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Abstract

The invention belongs to fire resisting material fields, and in particular to a kind of high-performance aluminum chrome refractory and preparation method thereof.The present invention is based on white fused alumina particle and fine powder, electric smelting chromium oxide, addition aluminium chromium slag, alpha-aluminium oxide micro mist, chrome oxide green or fused white corundum fine powder, is combined with making bonding agent and carboxymethyl cellulose by oneself, additive is added, fires through high temperature.The aluminium chrome refractory produced using technical solution of the present invention, it is low with impurity content, physical property is excellent, the features such as thermal shock resistance is good, high temperature break resistant intensity significantly improves, it can be used in the harsh Industrial Stoves of various conditions, and produce high-performance aluminum chrome refractory goods cost per ton to significantly reduce, play the role of cost efficiency.

Description

A kind of high-performance aluminum chrome refractory and preparation method thereof and application
Technical field
The invention belongs to fire resisting material fields more particularly to a kind of high-performance aluminum chrome refractory and preparation method thereof.
Background technique
With the development of hot industry, the requirement to refractory material is more and more harsher, and energy-saving and environmental protection, long-life are increasingly heavy Depending on getting up, the refractory material that hot industry needs largely to have excellent properties, and aluminium chrome refractory (chromium oxide 3-30%) High with the anti-folding of high temperature, good thermal shock stability, erosion-resisting characteristics are good, the feature of service life length, especially suitable for high temperature, high pressure kiln Liner, such as Texaco stove, black reactor inner lining of furnace, it is also possible to make heating furnace platform brick.
Technical literature, patent there are many have carried out detailed report to the excellent characteristics of aluminium chrome refractory and application Road, which is not described herein again, and the present invention only uses for reference its big measured experience, creative into one on the basis of primary aluminum chromium refractory material Step improves the applied at elevated temperature performance of material, in particular to the raising of material thermal shock resistance and high temperature fracture resistance is more conducive to Materials'use life-time dilatation.
Summary of the invention
To realize above-mentioned technical requirements, the present invention is that aluminium chrome refractory is adjusted using additive and bonding agent mode The microstructure of article substrate achievees the purpose that improve product thermal shock resistance and elevated temperature strength, and then proposes a kind of performance more Excellent aluminium chrome refractory and preparation method thereof.
The present invention is implemented with the following technical solutions.
A kind of high-performance aluminum chrome refractory, is made of aggregate, matrix, bonding agent and additive.
Wherein, aggregate is made of following mass parts material: 40-50 part of white fused alumina or plate diamond spar particle 1-8mm, 1-20 part of 0.01-1mm, electric smelting chrome oxide particle 0.01-2mm 0.5-20 part.
Wherein, matrix is made of following mass parts material: 15-30 parts of 200 mesh of aluminium chromium slag powder, white fused alumina or plate diamond spar are thin 2-15 part of 240 mesh of powder, 1-3 part of 500 mesh of Alpha-alumina micro mist, 0.5-10 part of 240 mesh of electric smelting chromium oxide fine powder, chromium oxide Green 2~8 μm of 0.5-5 part.
Wherein, bonding agent is made of following mass parts material: self-control phosphoric acid -3-5 parts of aluminium chlorate zirconium, carboxymethyl cellulose 0.5-1.5 parts.
Wherein, additive is made of following mass parts material: 0.1-0.5 parts of alumina short fibre；Fused zirconia 1-5 part of 0.088-0.2mm, 0.5-5 part of 325 mesh of fused zirconia.
Wherein, the Al in the white fused alumina particle and fine powder, plate diamond spar particle and fine powder, Alpha-alumina micro mist2O3's Mass fraction >=99.0%.
Wherein, the electric smelting chrome oxide particle and fine powder, Cr2O3Mass fraction >=99.0%.
Wherein, the aluminium chromium slag powder is the aluminium chromium slag powder through flotation, is by that will be produced by aluminothermic process metal smelting chromium Byproduct aluminium chromic wastes disposal after obtain, processing method are as follows: aluminium chromium slag is first worn into 200 mesh fine powders, is fitted into flotation device, adds Water is sufficiently stirred, and flotation agent oleic acid, calgon is added, wherein the 0.05-1.5% that oleic acid amount is aluminium chromium slag is added, is added Calgon amount is the 0.5-1.5% of aluminium chromium slag, is then dehydrated washing again, reduce metal Al in original slag, metal Cr, Fe2O3、MgO、CaO、SiO2Equal impurity contents, after flotation, Al therein2O3In 80-85%, Cr2O3Between 11-15%.
Wherein, the alumina short fibre, Al2O3Mass fraction >=99%, length 0.5-2mm, 10-12 μm of diameter.
Wherein, the fused zirconia is Zr-40, ZrO2≥40%。
Wherein, self-control phosphoric acid-aluminium chlorate zirconium preparation method.
(1) in humic acid: oxalic acid solution=25:75 ratio, it is to fill in 40% oxalic acid solution that humic acid, which is added to concentration, Divide mixing, forms emulsion, Compound-acid solution is made.
(2) above-mentioned Compound-acid solution is added to specific gravity is 1.5kg/cm3Phosphate dihydrogen aluminum solution in, by biphosphate Aluminum solutions: Compound-acid solution=8:2 is stirred evenly, spare at aluminium dihydrogen phosphate Compound-acid solution.
(3) zirconium oxychloride is slowly added in 35-45 DEG C or so of water, is added while stirring, concentration reaches 33-37% or so Until, zirconyl chloride solution.
(4) the aluminium dihydrogen phosphate Compound-acid solution prepared in (2) is added in above-mentioned zirconyl chloride solution and aluminum-zirconium coupling agent In, by aluminium dihydrogen phosphate Compound-acid solution: zirconyl chloride solution: the configuration of aluminum-zirconium coupling agent=6:3:1, bonding agent make phosphorus by oneself Acid-aluminium chlorate zirconium.
Wherein, the aluminum-zirconium coupling agent is one or both of LD-139 or TL-6.
A kind of high-performance aluminum chrome refractory, specific preparation method are as follows.
(1) preparation of premixed powder.
5 parts of aluminium chromium slag powder are weighed, 240 mesh white fused aluminas or 2-15 parts of plate diamond spar, 1-3 parts of a alumina powder, electric smelting are added 0.5-10 parts of 240 mesh of chromium oxide fine powder, 2~8 μm of chrome oxide green 0.5-5 part, add fused zirconia 0.088-0.2mm's 1-5 parts, then 0.5-5 part of 325 mesh of fused zirconia premixes 0.5-1h, mixes well to obtain premixed powder, spare.
(2) preparation of aluminium chrome refractory molding pug.
Take 40-50 part, 1-20 part of 0.01-1mm, electric smelting chrome oxide particle of white fused alumina or plate diamond spar particle 1-8mm 0.5-20 part of 0.01-2mm and 0.1-0.5 parts of alumina short fibres, which are put into muller, to be mixed, duration 2-3min；Then Bonding agent phosphoric acid -3-5 parts of aluminium chlorate zirconium, 0.5-1.5 parts of carboxymethyl cellulose is added, mixes 5-8min, is sufficiently adhering to it In aggregate；The premixed powder in remaining 10-25 parts of aluminium chromium slag powder and (1) is added in muller again, with aggregate and bonding agent It is sufficiently stirred, duration 15-18min is to get aluminium chrome refractory molding pug；
Molding need to be finished with pug in 4-6h, if standing time will lead to moisture in pug long and reduce, without at the appointed time The pug that the moisture content that is finished reduces cannot be further continued for carrying out using need to be added in the ratio of 10-20% in newly mixed pug again Configuration.
(3) shaping and drying.
By the molding of aluminium chrome refractory with pug by hydraulic press or brick machine compression moulding, then form brick body in 180-210 DEG C of dry 10-12h；Adobe after drying is sorted, it is spare.
(4) it is burnt into.
Adobe after sorting is burnt into kiln, firing temperature is 1550-1750 DEG C, keeps the temperature kiln discharge after 2-3h, is made one Kind high-performance aluminum chrome refractory.
A kind of high-performance aluminum chrome refractory proposed by the present invention and preparation method thereof and application, propose by knot The adjustment of mixture and additive improves the method for product high-temperature behavior and the purified aluminum chromium slag after flotation utilizes in article substrate The beneficial effect of method.
(1) white fused alumina, plate diamond spar fine powder can guarantee the stable structure of matrix, prevent crossing for material from shrinking, α-Al2O3 The effect of micro mist is that there is certain activity the reaction of aluminium chromium solid phase fusion to be promoted to carry out as early as possible for it.
(2) addition of electric smelting chromium oxide can effectively facilitate its high temperature firing, and anti-by aluminium oxide, chromium oxide solid phase fusion The intensity and stability of material structure should be increased.
(3) the aluminium chromium slag powder (before flotation) that the present invention uses, is byproduct aluminium chromium caused by aluminothermic process metal smelting chromium Slag takes full advantage of limited aluminium chromium resource, can be effectively reduced the production cost of aluminium chrome refractory.
(4) the aluminium chromium slag powder after flotation, because its impurity is low, structural strength is big, antiacid alkali resistance is good, slag-resistant aggressivity It is good, the applied at elevated temperature performance of matrix is enhanced, can be used under high-temperature and high-pressure conditions.
(5) phosphoric acid, phosphate (major phosphate aluminum dihydrogen) bonding agent often applied in the prior art only can guarantee product Semi-finished product have some strength and processability, product sintering before in, in low temperature range have stronger bond strength, make For interim combination agent use, and contributed in terms of elevated temperature strength little；And the present invention makes phosphoric acid-aluminium chlorate zirconium bonding agent by oneself, The elevated temperature strength of product, especially high temperature break resistant intensity can be significantly improved, enables product under high temperature and pressure harsh conditions Application；It is aided with carboxymethyl cellulose organic additive as low temperature transient plasticizer, because its stickiness is big, makes product molding It is good, there is good moisture retention to pug, and will not adversely affect to fire resistance.Bonding agent of the invention specifically acts on Show the following.
1. under the action of aluminum-zirconium coupling agent, bonding agent material is combined it is closer, semi-finished product have sufficient intensity, And the processability of product is improved, the close increase of body, the porosity reduce, and the qualification rate of semi-finished product improves 10% or so.
2. being in sintering procedure, the high-activity aluminium oxide that aluminium dihydrogen phosphate decomposes is preferential and chromium oxide is admittedly molten reacts, and makes Product internal combustion it is even closer, the elevated temperature strength of product is bigger.
3. be in zirconium oxide and fused alumina zirconia fine powder that zirconium oxychloride decomposes zirconium oxide with temperature raising, because it is active different by Microdilatancy is walked, micro-crack is gradually generated in matrix, because of the stress that the expansion of aluminium chromium solid phase reaction generates when gradually alleviating firing, is increased Tough alumina chromia solid solution, effectively keeps the increase of product sintering strength, effectively prevent product loose or crack, Enhance the thermal shock resistance of product.
(6) addition of additive fused zirconia, its microdilatancy when making refractory product high temperature firing, generating micro-crack makes chromium Thermal stress in corundum products wins an acquittal, and further improves the thermal shock resistance and resistance to chemical attack of material system.
(7) aluminium oxide microfibre is commonly used in the structural strength and thermal shock resistance that product is improved in castable, the present invention It is used in burnt product, forms criss-cross dimensional network structure using it, cross network is formed in situ in sintering process The anisotropic brilliant binding structure of aluminium oxide, improve the matrix structure of product, increase the elevated temperature strength of product.
(8) using the aluminium chrome refractory of technical solution of the present invention production, have impurity content low, physical property It is excellent, the features such as thermal shock resistance is good, the high temperature break resistant intensity (1400 DEG C of x0.5h) of product from original 8.2MPa or so increase to Present 14MPa or so improves nearly 6MPa, so that the aluminium chromium refractory product of the chromium slag containing aluminium, can also be used in high temperature and pressure In environment, its application range is expanded, can be used in the harsh Industrial Stoves of various conditions；In addition, product comprehensive qualified rate 90%-94% till now is improved from 75%-85%；It is averagely per ton to can reduce cost 7% in terms of cost；In general Not only make product effect more preferable, also acts as the effect of volume increase drop originally.
Specific embodiment
Below in conjunction with specific embodiment, further description of the technical solution of the present invention.
Embodiment 1.
A kind of high-performance aluminum chrome refractory is made of following mass parts material: plate diamond spar: 45 parts of 1-8mm, 15 parts of 0.01-1mm, 10 parts of 240 mesh；Electric smelting chromium oxide: 0.5 part of 0.01-2mm, 0.5 part of 240 mesh, chrome oxide green: 0.5 part of 2-8 μm；Aluminium chromium slag powder (flotation): 23 parts of 200 mesh；A- aluminium oxide: 1.5 parts of 500 mesh；Phosphoric acid-aluminium chlorate zirconium liquid (self-control): 3 parts, carboxymethyl cellulose (solid): 1.2 parts；Fused zirconia: 0.088-0.2mm1.5 parts, fused zirconia: 325 0.5 part of mesh, alumina short fibre: 10-12 μm 0.12 part.
A kind of high-performance aluminum chrome refractory, specific preparation method are as follows.
(1) preparation of premixed powder.
Weigh 5 parts of aluminium chromium slag powder (flotation), 10 parts of 240 mesh plate diamond spar of addition, 1.5 parts of a alumina powder, electric smelting oxidation 0.5 part of 240 mesh of chromium fine powder, 0.5 part of 2~8 μm of chrome oxide green, add 1.5 parts of fused zirconia 0.088-0.2mm, electricity 0.5 part of molten 325 mesh of fused alumina zirconia, then premixes 0.5h, mixes well to obtain premixed powder, spare.
(2) preparation of aluminium chrome refractory molding pug.
Take 45 parts of plate diamond spar particle 1-8mm, 15 parts of 0.01-1mm, electric smelting chrome oxide particle 0.01-2mm 0.5 Part and 0.12 part of alumina short fibre, which are put into muller, to be mixed, duration 2min；Then self-control phosphoric acid-aluminium chlorate zirconium is added 3 parts, 1.2 parts of carboxymethyl cellulose mix 5min, are sufficiently adhering to it in aggregate；Again by remaining 18 parts of aluminium chromium slag powder and (1) premixed powder in is added in muller, is sufficiently stirred with aggregate and bonding agent, duration 15min is resistance to get aluminium chromium matter Pug is used in fiery material molding；
Note: molding need to be finished with pug in 4-6h, if standing time will lead to moisture in pug long and reduce, not in the stipulated time The pug that the moisture content that is inside finished reduces cannot be further continued for carrying out using need to be added in weight in newly mixed pug in the ratio of 10-20% New configuration.
(3) shaping and drying.
By the molding of aluminium chrome refractory with pug by hydraulic press or brick machine compression moulding, then form brick body in 180 DEG C of dry 10h；Adobe after drying is sorted, it is spare.
(4) it is burnt into.
Adobe after sorting is burnt into kiln, firing temperature is 1550 DEG C, keeps the temperature kiln discharge after 3h, a kind of high-performance is made Aluminium chrome refractory.
Wherein, self-control phosphoric acid-aluminium chlorate zirconium preparation method.
(1) in humic acid: oxalic acid solution=25:75 ratio, it is to fill in 40% oxalic acid solution that humic acid, which is added to concentration, Divide mixing, forms emulsion, Compound-acid solution is made.
(2) above-mentioned Compound-acid solution is added to specific gravity is 1.5kg/cm3Phosphate dihydrogen aluminum solution, by aluminium dihydrogen phosphate Solution: Compound-acid solution=8:2 is stirred evenly, spare at aluminium dihydrogen phosphate Compound-acid solution.
(3) zirconium oxychloride is slowly added in 35 DEG C or so of water, is added while stirring, concentration up to 33%, oxychlorination Zirconium solution.
(4) it is compound that above-mentioned zirconyl chloride solution and LD-139 aluminum-zirconium coupling agent are added to the aluminium dihydrogen phosphate prepared in (2) In acid solution, by aluminium dihydrogen phosphate Compound-acid solution: zirconyl chloride solution: LD-139=6:3:1 configuration, bonding agent self-control Phosphoric acid-aluminium chlorate zirconium.
Comparative example 1.
The ingredient of additions all in embodiment 1 is remained unchanged with technological parameter, only the aluminium chromium slag powder after flotation is replaced It changes the aluminium chromium slag without flotation into, is then prepared into the aluminium chrome refractory of comparative example 1, two above technical solution is made It obtains fire resistive material product and carries out performance detection, testing result see the table below.
From table 1 it follows that crushing strength under high temperature and the anti-folding of high temperature are strong in the case that aluminium chromium slag is not just applied through flotation Degree is substantially reduced, so, aluminium chromium slag uses after answering flotation.
The embodiment is the high-performance aluminum chrome refractory containing chromium oxide 4% or so, and only additive, bonding agent are different, Obvious from product properties index difference from the point of view of table 2, especially high temperature break resistant intensity is than conventional example 1, raising 6MPa or so, conventional case Sub 3 aluminium chromium slags are not through anti-some more low difference 8MPa of folding of flotation high temperature or so, it will be seen that aluminium chromium slag flotation is necessary.This project product In certain company's black reactor application, service life improves 15% or so, illustrates that properties of product of the invention are more preferable.
Embodiment 2.
A kind of high-performance aluminum chrome refractory is made of following mass parts material: plate diamond spar: 45 parts of 1-8mm, 12 parts, 7 parts of 240 mesh of 0.01-1mm；Electric smelting chromium oxide: 0.01-2mm3 parts, 2.5 parts of 240 mesh, chrome oxide green: 2-8 μm 2 parts； Aluminium chromium slag powder (flotation): 200 20 parts of mesh；1 part of a- aluminium oxide；Phosphoric acid-aluminium chlorate zirconium liquid (self-control): 3 parts, carboxymethyl cellulose (solid): 1 part；Fused zirconia: 1.5 parts of 0.088-0.2mm, fused zirconia: 325 2 parts of mesh, alumina short fibre 0.2 Part.
A kind of high-performance aluminum chrome refractory, specific preparation method are as follows.
(1) preparation of premixed powder.
5 parts of aluminium chromium slag powder (flotation) are weighed, 4 parts of 240 mesh plate diamond spar, 1 part of a alumina powder, electric smelting chromium oxide are added 2.5 parts of 240 mesh of fine powder, 2 parts of 2~8 μm of chrome oxide green, add 1.5 parts of fused zirconia 0.088-0.2mm, electric smelting zirconium 2 parts of 325 mesh of corundum, then premix 0.7h, mix well to obtain premixed powder, spare.
(2) preparation of aluminium chrome refractory molding pug.
Take 45 parts of plate diamond spar particle 1-8mm, 12 parts of 0.01-1mm, 3 parts of electric smelting chrome oxide particle 0.01-2mm It is put into muller and is mixed with 0.2 part of alumina short fibre, duration 3min；Then self-control phosphoric acid-aluminium chlorate zirconium 3 is added Part, 1 part of carboxymethyl cellulose mix 8min, are sufficiently adhering to it in aggregate；Again by the aluminium chromium slag after remaining 15 parts of flotation Premixed powder in powder and (1) is added in muller, is sufficiently stirred with aggregate and bonding agent, duration 18min is to get aluminium chromium Pug is used in fire resistant materials molding；
Note: molding need to be finished with pug in 4-6h, if standing time will lead to moisture in pug long and reduce, not in the stipulated time The pug that the moisture content that is inside finished reduces cannot be further continued for carrying out using need to be added in weight in newly mixed pug in the ratio of 10-20% New configuration.
(3) shaping and drying.
By the molding of aluminium chrome refractory with pug by hydraulic press or brick machine compression moulding, then form brick body in 194 DEG C of dry 10.5h；Adobe after drying is sorted, it is spare.
(4) it is burnt into.
Adobe after sorting is burnt into kiln, firing temperature is 1620 DEG C, keeps the temperature kiln discharge after 2.8h, a kind of high property is made It can aluminium chrome refractory.
Wherein, self-control phosphoric acid-aluminium chlorate zirconium preparation method.
(1) in humic acid: oxalic acid solution=25:75 ratio, it is to fill in 40% oxalic acid solution that humic acid, which is added to concentration, Divide mixing, forms emulsion, Compound-acid solution is made.
(2) above-mentioned Compound-acid solution is added to specific gravity is 1.5kg/cm3Phosphate dihydrogen aluminum solution, by aluminium dihydrogen phosphate Solution: Compound-acid solution=8:2 is stirred evenly, spare at aluminium dihydrogen phosphate Compound-acid solution.
(3) zirconium oxychloride is slowly added in 35 DEG C or so of water, is added while stirring, concentration up to 35%, oxychlorination Zirconium solution.
(4) the aluminium dihydrogen phosphate Compound-acid prepared in (2) is added in above-mentioned zirconyl chloride solution and TL-6 aluminum-zirconium coupling agent In solution, by aluminium dihydrogen phosphate Compound-acid solution: zirconyl chloride solution: TL-6=6:3:1 configuration, bonding agent make by oneself phosphorus Acid-aluminium chlorate zirconium.
The high-performance aluminum chrome refractory containing chromium oxide 10% or so is made in the embodiment, and only additive, bonding agent be not Together, obvious from product properties index difference from the point of view of table 2, especially high temperature break resistant intensity improves 6MPa or so, explanation than conventional example 2 Properties of product of the invention are more superior.
Embodiment 3.
A kind of high-performance aluminum chrome refractory is made of following mass parts material: plate diamond spar: 50 parts of 1-8mm, 7 parts, 10 parts of 240 mesh of 0.01-1mm；Electric smelting chromium oxide: 0.5 part, 10 parts of 240 mesh of 0.01-2mm, 5 parts of chrome oxide green；Aluminium chromium 30 parts of ground-slag (flotation)；1 part of a- aluminium oxide；Phosphoric acid -4 parts of aluminium chlorate zirconium liquid (self-control), 1.5 parts of carboxymethyl cellulose；Electric smelting zirconium 5 parts of corundum 0.088-0.2mm, 0.5 part of 325 mesh of fused zirconia, 0.5 part of alumina short fibre.
A kind of high-performance aluminum chrome refractory, specific preparation method are as follows.
(1) preparation of premixed powder.
5 parts of aluminium chromium slag powder (flotation) are weighed, 10 parts of 240 mesh plate diamond spar, 1 part of a alumina powder, electric smelting chromium oxide are added 10 parts of 240 mesh of fine powder, 5 parts of chrome oxide green add 5 parts of fused zirconia 0.088-0.2mm, 325 purpose of fused zirconia 0.5 part, 1h is then premixed, mixes well to obtain premixed powder, it is spare.
(2) preparation of aluminium chrome refractory molding pug.
Take 50 parts of plate diamond spar particle 1-8mm, 7 parts of 0.01-1mm, 0.5 part of electric smelting chrome oxide particle 0.01-2mm It is put into muller and is mixed with 0.5 part of alumina short fibre, duration 2.5min；Then self-control phosphoric acid-aluminium chlorate zirconium 4 is added Part, 1.5 parts of carboxymethyl cellulose mix 6min, are sufficiently adhering to it in aggregate；Again by the aluminium chromium after remaining 25 parts of flotation Premixed powder in ground-slag and (1) is added in muller, is sufficiently stirred with aggregate and bonding agent, duration 16min is to get aluminium Pug is used in chrome refractory molding.
Note: molding need to be finished with pug in 4-6h, if standing time will lead to moisture in pug long and reduce, not provided The pug that the moisture content that is finished in time reduces cannot be further continued for carrying out using need to be added in newly mixed pug in the ratio of 10-20% In reconfigure.
(3) shaping and drying.
By the molding of aluminium chrome refractory with pug by hydraulic press or brick machine compression moulding, then form brick body in 200 DEG C of dry 12h；Adobe after drying is sorted, it is spare.
(4) it is burnt into.
Adobe after sorting is burnt into kiln, firing temperature is 1750 DEG C, keeps the temperature kiln discharge after 2h, a kind of high-performance is made Aluminium chrome refractory.
Wherein, self-control phosphoric acid-aluminium chlorate zirconium preparation method.
(1) in humic acid: oxalic acid solution=25:75 ratio, it is to fill in 40% oxalic acid solution that humic acid, which is added to concentration, Divide mixing, forms emulsion, Compound-acid solution is made.
(2) above-mentioned Compound-acid solution is added to specific gravity is 1.5kg/cm3Phosphate dihydrogen aluminum solution, by aluminium dihydrogen phosphate Solution: Compound-acid solution=8:2 is stirred evenly, spare at aluminium dihydrogen phosphate Compound-acid solution.
(3) zirconium oxychloride is slowly added in 40 DEG C or so of water, is added while stirring, concentration up to 37%, oxychlorination Zirconium solution.
(4) the aluminium dihydrogen phosphate Compound-acid prepared in (2) is added in above-mentioned zirconyl chloride solution and TL-6 aluminum-zirconium coupling agent In solution, by aluminium dihydrogen phosphate Compound-acid solution: zirconyl chloride solution: TL-6=6:3:1 configuration, bonding agent make by oneself phosphorus Acid-aluminium chlorate zirconium.
Embodiment 4.
A kind of high-performance aluminum chrome refractory is made of following mass parts material: plate diamond spar: 40 parts of 1-8mm, 20 parts, 15 parts of 240 mesh of 0.01-1mm；Electric smelting chromium oxide: 6 parts, 3 parts of 240 mesh of 0.01-2mm, 1.3 parts of chrome oxide green；Aluminium chromium 21 parts of ground-slag (flotation)；1.4 parts of a- aluminium oxide；Phosphoric acid -4 parts of aluminium chlorate zirconium liquid (self-control), 0.8 part of carboxymethyl cellulose；Electric smelting 2 parts of fused alumina zirconia 0.088-0.2mm, 1.1 parts of 325 mesh of fused zirconia, 0.25 part of alumina short fibre.
A kind of high-performance aluminum chrome refractory, specific preparation method are as follows.
(1) preparation of premixed powder.
Weigh 5 parts of aluminium chromium slag powder (flotation), 15 parts of 240 mesh plate diamond spar of addition, 1.4 parts of a alumina powder, electric smelting oxidation 3 parts of 240 mesh of chromium fine powder, 1.3 parts of chrome oxide green add 2 parts of fused zirconia 0.088-0.2mm, 325 mesh of fused zirconia 1.1 parts, then premix 0.75h, mix well to obtain premixed powder, it is spare.
(2) preparation of aluminium chrome refractory molding pug.
Take 40 parts of plate diamond spar particle 1-8mm, 20 parts of 0.01-1mm, 6 and of electric smelting chrome oxide particle 0.01-2mm 0.25 part of alumina short fibre is put into muller and is mixed, duration 2.5min；Then self-control phosphoric acid-aluminium chlorate zirconium 4 is added Part, 0.8 part of carboxymethyl cellulose mix 5min, are sufficiently adhering to it in aggregate；Again by the aluminium chromium after remaining 16 parts of flotation Premixed powder in ground-slag and (1) is added in muller, is sufficiently stirred with aggregate and bonding agent, duration 18min is to get aluminium Pug is used in chrome refractory molding.
Note: molding need to be finished with pug in 4-6h, if standing time will lead to moisture in pug long and reduce, not provided The pug that the moisture content that is finished in time reduces cannot be further continued for carrying out using need to be added in newly mixed pug in the ratio of 10-20% In reconfigure.
(3) shaping and drying.
By the molding of aluminium chrome refractory with pug by hydraulic press or brick machine compression moulding, then form brick body in 205 DEG C of dry 11h；Adobe after drying is sorted, it is spare.
(4) it is burnt into.
Adobe after sorting is burnt into kiln, firing temperature is 1620 DEG C, keeps the temperature kiln discharge after 3h, a kind of high-performance is made Aluminium chrome refractory.
Wherein, self-control phosphoric acid-aluminium chlorate zirconium preparation method.
(1) in humic acid: oxalic acid solution=25:75 ratio, it is to fill in 40% oxalic acid solution that humic acid, which is added to concentration, Divide mixing, forms emulsion, Compound-acid solution is made.
(2) above-mentioned Compound-acid solution is added to specific gravity is 1.5kg/cm3Phosphate dihydrogen aluminum solution, by aluminium dihydrogen phosphate Solution: Compound-acid solution=8:2 is stirred evenly, spare at aluminium dihydrogen phosphate Compound-acid solution.
(3) zirconium oxychloride is slowly added in 40 DEG C or so of water, is added while stirring, concentration up to 36%, oxychlorination Zirconium solution.
(4) it is compound that above-mentioned zirconyl chloride solution and LD-139 aluminum-zirconium coupling agent are added to the aluminium dihydrogen phosphate prepared in (2) In acid solution, by aluminium dihydrogen phosphate Compound-acid solution: zirconyl chloride solution: LD-139=6:3:1 configuration, bonding agent self-control Phosphoric acid-aluminium chlorate zirconium.
The product of embodiment and conventional case is detected, as a result see the table below.
Anti- folding of apparent porosity, bulk density, cold crushing strength, high temperature etc. is detected by national standard, and thermal shock resistance is pressed The detection of smelting mark, the data such as table of conventional performance index detection.
Conventional case in table refers to: keeping that other raw materials are consistent, under preparation process unanimous circumstances, combine using aluminum phosphate Agent and the product produced without flotation aluminium chromium slag.
The data comparison from table: product produced by the invention (Cr compared with conventional articles2O3Content is 4% and 10%), from Bonding agent and additive processed significantly improve the high-temperature behavior of product, especially high temperature break resistant intensity index and improve a shelves It is secondary, 14MPa or more is reached, can be applied on 1400 DEG C or more, the high temperature and pressure kiln of 8.5MPa completely.In addition, being made from tradition From the point of view of product, using the high temperature break resistant intensity only 6MPa or so for the aluminium chromium slag sample not purified, illustrates the purification of aluminium chromium slag and do not purify The elevated temperature strength of product is influenced also very greatly, the purification of aluminium chromium slag is necessary.
High-performance aluminum chrome refractory product produced by the invention is anti-with very excellent thermal shock resistance and high temperature Intensity is rolled over, can be used in the harsh Industrial Stoves of various conditions, environmental protection, energy conservation, consumption reduction cost performance with higher；In addition, should Product comprehensive qualified rate also improves 90%-94% till now from 75%-85%；It is averagely per ton to can reduce in terms of cost Cost 7%；Not only make product effect more preferable in general, also acts as the effect of volume increase drop originally.

Claims (10)

1. a kind of high-performance aluminum chrome refractory, is made of aggregate, matrix, bonding agent and additive:
Wherein, aggregate is made of following mass parts material: white fused alumina or 40-50 part of plate diamond spar particle 1-8mm, 0.01-1mm 1-20 part, electric smelting chrome oxide particle 0.01-2mm 0.5-20 part；
Wherein, matrix is made of following mass parts material: 15-30 parts of 200 mesh of aluminium chromium slag powder, white fused alumina or plate diamond spar fine powder 2-15 part of 240 mesh, 1-3 part of 500 mesh of Alpha-alumina micro mist, 0.5-10 part of 240 mesh of electric smelting chromium oxide fine powder, chrome oxide green 2~8 μm 0.5-5 part；
Wherein, bonding agent is made of following mass parts material: self-control phosphoric acid -3-5 parts of aluminium chlorate zirconium, carboxymethyl cellulose 0.5- 1.5 part；
Wherein, additive is made of following mass parts material: 0.1-0.5 parts of alumina short fibre；Fused zirconia 0.088- 1-5 part of 0.2mm, 0.5-5 part of 325 mesh of fused zirconia.
2. high-performance aluminum chrome refractory according to claim 1, wherein white fused alumina particle and fine powder, plate diamond spar Al in particle and fine powder, Alpha-alumina micro mist2O3Mass fraction >=99.0%.
3. high-performance aluminum chrome refractory according to claim 1, wherein electric smelting chrome oxide particle and fine powder, Cr2O3Mass fraction >=99.0%.
4. high-performance aluminum chrome refractory according to claim 1, wherein the alumina short fibre, Al2O3Matter Amount score >=99%, length 0.5-2mm, 10-12 μm of diameter.
5. high-performance aluminum chrome refractory according to claim 1, wherein fused zirconia Zr-40, ZrO2≥ 40%。
6. high-performance aluminum chrome refractory according to claim 1, wherein aluminium chromium slag powder is the aluminium chromium slag through flotation Powder is the aluminium chromium slag after flotation by will obtain after byproduct aluminium chromic wastes disposal caused by aluminothermic process metal smelting chromium Powder, Al therein2O3In 80-85%, Cr2O3Between 11-15%.
7. high-performance aluminum chrome refractory according to claim 1, wherein the specific floatation process of aluminium chromium slag are as follows: first Aluminium chromium slag is worn into 200 mesh fine powders, is fitted into flotation device, adds water, be sufficiently stirred, flotation agent oleic acid, calgon is added, It is middle that the 0.05-1.5% that oleic acid amount is aluminium chromium slag is added, the 0.5-1.5% that calgon amount is aluminium chromium slag is added, is then dehydrated again Washing reduces metal Al, metal Cr, Fe in former slag2O3、MgO、CaO、SiO2Equal impurity contents.
8. high-performance aluminum chrome refractory according to claim 1, wherein the self-control phosphoric acid-aluminium chlorate zirconium, system Preparation Method are as follows:
(1) in humic acid: oxalic acid solution=25:75 ratio, it is sufficiently to mix in 40% oxalic acid solution that humic acid, which is added to concentration, It closes, forms emulsion, Compound-acid solution is made；
(2) above-mentioned Compound-acid solution is added to specific gravity is 1.5kg/cm3Phosphate dihydrogen aluminum solution in, it is molten by aluminium dihydrogen phosphate Liquid: Compound-acid solution=8:2 is stirred evenly, spare at aluminium dihydrogen phosphate Compound-acid solution；
(3) zirconium oxychloride is slowly added in 35-45 DEG C or so of water, is added while stirring, until concentration reaches 33-37% or so, Zirconyl chloride solution；
(4) above-mentioned zirconyl chloride solution and aluminum-zirconium coupling agent are added in the aluminium dihydrogen phosphate Compound-acid solution prepared in (2), are pressed Aluminium dihydrogen phosphate Compound-acid solution: zirconyl chloride solution: the configuration of aluminum-zirconium coupling agent=6:3:1, bonding agent make phosphoric acid-chlorine by oneself Sour aluminium zirconium；
Wherein, the aluminum-zirconium coupling agent is one or both of LD-139 or TL-6.
9. a kind of preparation method of high-performance aluminum chrome refractory:
(1) preparation of premixed powder
5 parts of aluminium chromium slag powder are weighed, 240 mesh white fused aluminas or 2-15 parts of plate diamond spar, 1-3 parts of a alumina powder, electric smelting oxidation are added 0.5-10 parts of 240 mesh of chromium fine powder, 2~8 μm of chrome oxide green 0.5-5 part, add the 1-5 of fused zirconia 0.088-0.2mm Part, then 0.5-5 part of 325 mesh of fused zirconia premixes 0.5-1h, mixes well to obtain premixed powder, spare；
(2) preparation of aluminium chrome refractory molding pug
Take 40-50 part of white fused alumina or plate diamond spar particle 1-8mm, 1-20 part of 0.01-1mm, electric smelting chrome oxide particle 0.01- 0.5-20 part of 2mm and 0.1-0.5 parts of alumina short fibres, which are put into muller, to be mixed, duration 2-3min；Then it is added Bonding agent phosphoric acid -3-5 parts of aluminium chlorate zirconium, 0.5-1.5 parts of carboxymethyl cellulose mix 5-8min, it are made to be sufficiently adhering to aggregate In；The premixed powder in remaining 10-25 parts of aluminium chromium slag powder and (1) is added in muller again, is carried out with aggregate and bonding agent It is sufficiently stirred, duration 15-18min is to get aluminium chrome refractory molding pug；
(3) shaping and drying
By the molding of aluminium chrome refractory with pug by hydraulic press or brick machine compression moulding, brick body is then formed in 180- 210 DEG C of dry 10-12h；Adobe after drying is sorted, it is spare；
(4) it is burnt into
Adobe after sorting is burnt into kiln, firing temperature is 1550-1750 DEG C, keeps the temperature kiln discharge after 2-3h, is made a kind of high Performance aluminium chrome refractory.
10. the preparation method of high-performance aluminum chrome refractory according to claim 9, wherein the aluminium chromium matter fire resisting Material molding need to be finished with pug in 4-6h, if standing time will lead to moisture in pug long and reduce, without at the appointed time The pug that the moisture content that is finished reduces cannot be further continued for carrying out using need to be added in the ratio of 10-20% in newly mixed pug again Configuration.
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CN112745108A (en) * 2020-12-07 2021-05-04 北京金隅通达耐火技术有限公司 High-density chromium corundum brick for hazardous waste disposal rotary kiln
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CN114956786A (en) * 2022-06-23 2022-08-30 攀钢集团攀枝花钢铁研究院有限公司 Preparation method for producing calcium aluminate-aluminum-chromium brick by using vanadium iron slag as raw material
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