CN109320219B - High-performance aluminum-chromium refractory material and manufacturing method and application thereof - Google Patents
High-performance aluminum-chromium refractory material and manufacturing method and application thereof Download PDFInfo
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Abstract
The invention belongs to the field of refractory materials, and particularly relates to a high-performance aluminum-chromium refractory material and a preparation method thereof. The invention takes white corundum particles, fine powder and electric melting chromium oxide as main bodies, adds aluminum chromium slag, alpha alumina micro powder and chromium oxide green or electric melting white corundum fine powder, combines self-made bonding agent and carboxymethyl cellulose, adds additive, and is fired at high temperature. The aluminum-chromium refractory material produced by the technical scheme of the invention has the characteristics of low impurity content, excellent physical properties, good thermal shock resistance and the like, the high-temperature rupture strength is obviously improved, the aluminum-chromium refractory material can be used in various industrial kilns with severe conditions, the cost for producing each ton of high-performance aluminum-chromium refractory material products is obviously reduced, and the effects of cost reduction and efficiency improvement are achieved.
Description
Technical Field
The invention belongs to the field of refractory materials, and particularly relates to a high-performance aluminum-chromium refractory material and a manufacturing method thereof.
Background
Along with the development of high-temperature industry, the requirements on refractory materials are more and more strict, energy conservation, environmental protection and long service life are increasingly emphasized, the high-temperature industry needs a large amount of refractory materials with excellent performance, and the aluminum-chromium refractory material (3-30 percent of chromium oxide) has the characteristics of high-temperature rupture resistance, good thermal shock stability, good erosion resistance and long service life, is particularly suitable for linings of high-temperature and high-pressure kilns, such as Texaco furnaces, carbon black reaction furnaces and other furnace linings, and can also be used as a platform brick for heating furnaces.
The invention only refers to a great deal of good experience, and creatively further improves the high-temperature service performance of the material on the basis of the original aluminum-chromium refractory material, in particular to the improvement of the thermal shock stability and the high-temperature fracture resistance of the material, which is more beneficial to prolonging the service life of the material.
Disclosure of Invention
In order to meet the technical requirements, the invention adopts an additive and a bonding agent mode to adjust the microstructure of the matrix of the aluminum-chromium refractory material product, so as to achieve the purpose of improving the thermal shock stability and the high-temperature strength of the product, and further provides the aluminum-chromium refractory material with more excellent performance and the manufacturing method thereof.
The invention is realized by adopting the following technical scheme.
A high-performance Al-Cr refractory is prepared from aggregate, matrix, binder and additive.
The aggregate comprises the following materials in parts by mass: 40-50 parts of white corundum or tabular corundum particles with the diameter of 1-8mm, 1-20 parts of white corundum or tabular corundum particles with the diameter of 0.01-1mm and 0.5-20 parts of electric melting chromium oxide particles with the diameter of 0.01-2 mm.
Wherein the matrix consists of the following materials in parts by mass: 15-30 parts of aluminum chromium slag powder with 200 meshes, 2-15 parts of white corundum or tabular corundum fine powder with 240 meshes, 1-3 parts of alpha-alumina micro powder with 500 meshes, 0.5-10 parts of electric melting chromium oxide fine powder with 240 meshes and 0.5-5 parts of chromium oxide green with 2-8 mu m.
Wherein the bonding agent is prepared from the following materials in parts by mass: 3-5 parts of self-made aluminum zirconium phosphate-chlorate and 0.5-1.5 parts of carboxymethyl cellulose.
Wherein the additive comprises the following materials in parts by mass: 0.1-0.5 part of alumina short fiber; 1-5 parts of fused zirconia corundum with the grain size of 0.088-0.2mm and 0.5-5 parts of fused zirconia corundum with the grain size of 325 meshes.
Wherein, the white corundum particles and fine powder, the tabular corundum particles and fine powder, and Al in the alpha-alumina micropowder2O3The mass fraction of the component (A) is more than or equal to 99.0 percent.
Wherein the electrofused chromium oxide particles and fine powder are Cr2O3The mass fraction is more than or equal to 99.0 percent.
The aluminum chromium slag powder is obtained by processing a byproduct aluminum chromium slag generated by smelting metal chromium by an aluminothermic process, and the processing method comprises the following steps: grinding the aluminum-chromium slag into fine powder of 200 meshes, filling the fine powder into a flotation machine, adding water, fully stirring, adding a flotation agent oleic acid and sodium hexametaphosphate, wherein the amount of the added oleic acid is 0.05-1.5 percent of that of the aluminum-chromium slag, addingThe sodium hexametaphosphate accounts for 0.5-1.5% of the aluminum chromium slag, and then the sodium hexametaphosphate is dehydrated and washed to reduce metal Al, metal Cr and metal Fe in the original slag2O3、MgO、CaO、SiO2After flotation, the Al content is equal to the impurity content2O380-85% of Cr2O3Between 11-15%.
Wherein the alumina short fiber is Al2O3The mass fraction is more than or equal to 99 percent, the length is 0.5-2mm, and the diameter is 10-12 mu m.
Wherein the fused zirconia corundum is Zr-40, ZrO2≥40%。
The preparation method of the self-made aluminum zirconium phosphate-chlorate is disclosed.
(1) According to the proportion of humic acid to oxalic acid solution =25:75, adding humic acid into 40% oxalic acid solution, and fully mixing to form emulsion, so as to prepare composite acid solution.
(2) Adding the above complex acid solution to a specific gravity of 1.5kg/cm3In the aluminum dihydrogen phosphate solution of (2), the ratio of aluminum dihydrogen phosphate solution: and (5) uniformly stirring the composite acid solution =8:2 to obtain the aluminum dihydrogen phosphate composite acid solution for later use.
(3) Slowly adding zirconium oxychloride into water at 35-45 deg.C, and stirring until the concentration reaches 33-37% to obtain zirconium oxychloride solution.
(4) Adding the zirconium oxychloride solution and the aluminum-zirconium coupling agent into the aluminum dihydrogen phosphate composite acid solution prepared in the step (2), and mixing the following components in percentage by weight: zirconium oxychloride solution: and (3) preparing an aluminum-zirconium coupling agent =6:3:1, namely, preparing the self-made bonding agent of aluminum zirconium phosphate-chlorate.
Wherein the aluminum-zirconium coupling agent is one or two of LD-139 or TL-6.
A high-performance aluminum-chromium refractory material is prepared by the following specific preparation method.
(1) And (4) preparing premixed powder.
Weighing 5 parts of aluminum chromium slag powder, adding 2-15 parts of 240-mesh white corundum or tabular corundum, 1-3 parts of alpha alumina micro powder, 240-mesh 0.5-10 parts of fused chromium oxide fine powder and 0.5-5 parts of 2-8 mu m chromium oxide green, then adding 1-5 parts of 0.088-0.2mm fused zirconia corundum and 0.5-5 parts of 325-mesh fused zirconia corundum, premixing for 0.5-1h, and fully mixing to obtain premixed powder for later use.
(2) Preparing the aluminum-chromium refractory material molding pug.
Mixing white corundum or tabular corundum particles of 1-8mm in 40-50 weight portions, electrically fused chromium oxide particles of 0.01-1mm in 1-20 weight portions and alumina short fibers of 0.1-0.5 weight portion in a kneading machine for 2-3 min; then adding 3-5 parts of a binding agent of aluminum zirconium phosphate-chlorate and 0.5-1.5 parts of carboxymethyl cellulose, and mixing for 5-8min to fully attach the mixture to the aggregate; adding the rest 10-25 parts of the aluminum chromium slag powder and the premixed powder in the step (1) into a mixing machine, and fully stirring the mixture with aggregate and a binding agent for 15-18min to obtain pug for molding the aluminum chromium refractory material;
the molding pug needs to be used up in 4-6h, if the molding pug is placed for a long time, the moisture in the pug is reduced, the pug which is not used up in the specified time and has reduced moisture can not be used any more, and the molding pug needs to be added into the newly mixed pug according to the proportion of 10-20% for reconfiguration.
(3) And (5) forming and drying.
Pressing and molding the mud for molding the aluminum-chromium refractory material by a hydraulic press or a brick press, and then drying the molded brick body at the temperature of 210 ℃ for 10-12 h; and sorting the dried green bricks for later use.
(4) And (5) firing.
And firing the sorted adobes in a kiln at 1550-.
The invention provides a high-performance aluminum-chromium refractory material, a preparation method and application thereof, and provides a method for improving the high-temperature performance of a product by adjusting a bonding agent and an additive and a method for utilizing floated pure aluminum-chromium slag in a product matrix.
(1) The white corundum and tabular corundum fine powder can ensure the stable structure of the matrix, prevent the over-shrinkage of the material and ensure the alpha-Al2O3The micro powder has the function of promoting the aluminum-chromium solid-phase melting reaction to be carried out as soon as possible with certain activity.
(2) The addition of the electric melting chromium oxide can effectively promote the high-temperature sintering of the material, and the strength and the stability of the material structure are improved through the solid-phase melting reaction of the aluminum oxide and the chromium oxide.
(3) The aluminum chromium slag powder (before flotation) adopted by the invention is a byproduct aluminum chromium slag generated by smelting metal chromium by an aluminothermic method, fully utilizes limited aluminum chromium resources, and can effectively reduce the production cost of the aluminum chromium refractory material.
(4) The aluminum chromium slag powder after flotation has the advantages of low impurity, high structural strength, good acid and alkali resistance and good slag erosion resistance, enhances the high-temperature service performance of the matrix, and can be used under the conditions of high temperature and high pressure.
(5) Phosphoric acid and phosphate (main aluminum dihydrogen phosphate) bonding agents commonly applied in the prior art can only ensure that a semi-finished product of a product has certain strength and forming performance, has stronger bonding strength in the middle and low temperature ranges before the product is sintered, is used as a temporary bonding agent, and does not contribute much in the aspect of high-temperature strength; the self-made aluminum zirconium phosphate-chlorate binding agent can obviously improve the high-temperature strength, particularly the high-temperature rupture strength of the product, so that the product can be applied under the harsh conditions of high temperature and high pressure; the carboxymethyl cellulose organic auxiliary agent is used as a low-temperature temporary plasticizer, and the carboxymethyl cellulose organic auxiliary agent has high viscosity, so that the product has good formability, good moisture retention property on pug, and no negative influence on the fire resistance. The specific actions of the binding agents of the invention are shown below.
Under the action of the aluminum-zirconium coupling agent, the binding agent more tightly bonds materials, the semi-finished product has enough strength, the forming performance of the product is improved, the body density is increased, the porosity is reduced, and the qualification rate of the semi-finished product is improved by about 10%.
Secondly, in the firing process, the high-activity aluminum oxide decomposed by the aluminum dihydrogen phosphate is preferentially subjected to solid-melt reaction with the chromium oxide, so that the interior of the product is more tightly combined, and the high-temperature strength of the product is higher.
And thirdly, zirconium oxide in zirconium oxide and zirconia corundum fine powder decomposed by zirconium oxychloride gradually expands slightly along with the rise of temperature due to different activities, so that microcracks are gradually generated in the matrix, the stress generated by aluminum-chromium solid-phase reaction expansion during sintering is gradually relieved, the aluminum oxide-chromium oxide solid solution is toughened, the increase of the sintering strength of the product is effectively kept, the product is effectively prevented from being loosened or cracked, and the thermal shock property of the product is enhanced.
(6) The addition of the additive fused zirconia corundum enables the refractory product to slightly expand when being fired at high temperature, and microcracks are generated to release the thermal stress in the chrome corundum product, so that the thermal shock stability and the chemical erosion resistance of a material system are further improved.
(7) The alumina microfiber is used in sintered product to form criss-cross stereo network structure and to form anisotropic alumina crystal beam structure in situ, so as to improve the matrix structure and raise the high temperature strength of the product.
(8) The aluminum-chromium refractory material produced by the technical scheme of the invention has the characteristics of low impurity content, excellent physical property, good thermal shock resistance and the like, the high-temperature rupture strength (1400 ℃ x0.5h) of the product is increased from about 8.2MPa to about 14MPa, and the rupture strength is improved by nearly 6MPa, so that the aluminum-chromium refractory product containing aluminum-chromium slag can be used in high-temperature and high-pressure environments, the application range is expanded, and the aluminum-chromium refractory material can be used in various industrial kilns with severe conditions; in addition, the comprehensive qualified rate of the product is improved from 75-85 percent to 90-94 percent at present; in terms of cost, the cost can be reduced by 7% per ton on average; in general, the product has better effect, and also has the effects of increasing production and reducing cost.
Detailed Description
The technical solution of the present invention will be further described with reference to the following specific examples.
Example 1.
A high-performance aluminum-chromium refractory material comprises the following materials in parts by mass: plate corundum: 45 parts of 1-8mm, 15 parts of 0.01-1mm and 10 parts of 240 meshes; electric melting chromic oxide: 0.5 part of 0.01-2mm, 0.5 part of 240 meshes, chromium oxide green: 0.5 part of 2-8 mu m; aluminum chromium slag powder (flotation): 23 portions of 200 meshes; a-alumina: 1.5 portions of 500 meshes; phosphoric acid-zirconium aluminum chlorate solution (self-made): 3 parts, carboxymethyl cellulose (solid): 1.2 parts; electric melting of zirconia corundum: 0.088-0.2mm1.5 parts of fused zirconia corundum: 0.5 part of 325 meshes, alumina short fiber: 0.12 part of 10-12 mu m.
A high-performance aluminum-chromium refractory material is prepared by the following specific preparation method.
(1) And (4) preparing premixed powder.
Weighing 5 parts of aluminum chromium slag powder (flotation), adding 10 parts of 240-mesh plate-shaped corundum, 1.5 parts of alpha alumina micro powder, 240-mesh 0.5 part of fused chromium oxide fine powder and 0.5 part of chromium oxide green with the particle size of 2-8 mu m, then adding 1.5 parts of fused zirconia corundum with the particle size of 0.088-0.2mm and 0.5 part of fused zirconia corundum with the particle size of 325 meshes, then premixing for 0.5h, and fully mixing to obtain premixed powder for later use.
(2) Preparing the aluminum-chromium refractory material molding pug.
Putting 45 parts of tabular corundum particles with the particle size of 1-8mm, 15 parts of tabular corundum particles with the particle size of 0.01-1mm, 0.5 part of electric-melting chromium oxide particles with the particle size of 0.01-2mm and 0.12 part of alumina short fibers into a mixing machine for mixing for 2 min; then adding 3 parts of self-made aluminum zirconium phosphate and 1.2 parts of carboxymethyl cellulose, and mixing for 5min to fully attach the mixture to the aggregate; adding the rest 18 parts of aluminum chromium slag powder and the premixed powder in the step (1) into a mixing machine, and fully stirring the mixture with aggregate and a binding agent for 15min to obtain pug for molding the aluminum chromium refractory material;
note: the molding pug needs to be used up in 4-6h, if the molding pug is placed for a long time, the moisture in the pug is reduced, the pug which is not used up in the specified time and has reduced moisture can not be used any more, and the molding pug needs to be added into the newly mixed pug according to the proportion of 10-20% for reconfiguration.
(3) And (5) forming and drying.
Pressing and molding the mud for molding the aluminum-chromium refractory material by a hydraulic press or a brick press, and then drying the molded brick body for 10 hours at 180 ℃; and sorting the dried green bricks for later use.
(4) And (5) firing.
Firing the selected green bricks in a kiln at 1550 ℃, keeping the temperature for 3h, and taking out of the kiln to obtain the high-performance aluminum-chromium refractory material.
The preparation method of the self-made aluminum zirconium phosphate-chlorate is disclosed.
(1) According to the proportion of humic acid to oxalic acid solution =25:75, adding humic acid into 40% oxalic acid solution, and fully mixing to form emulsion, so as to prepare composite acid solution.
(2) Adding the above complex acid solution to a specific gravity of 1.5kg/cm3The aluminum dihydrogen phosphate solution of (2) is prepared by mixing the following aluminum dihydrogen phosphate solution: and (5) uniformly stirring the composite acid solution =8:2 to obtain the aluminum dihydrogen phosphate composite acid solution for later use.
(3) Slowly adding zirconium oxychloride into water at about 35 ℃, and stirring while adding zirconium oxychloride to reach the concentration of 33 percent to obtain the zirconium oxychloride solution.
(4) Adding the zirconium oxychloride solution and the LD-139 aluminum zirconium coupling agent into the aluminum dihydrogen phosphate composite acid solution prepared in the step (2), and mixing the following components in percentage by weight: zirconium oxychloride solution: LD-139 =6:3:1, namely the self-made aluminum zirconium phosphate-chlorate of the bonding agent.
Comparative example 1.
All the added components and process parameters in the example 1 are kept unchanged, except that the aluminum chromium slag powder after flotation is replaced by aluminum chromium slag without flotation, then the aluminum chromium refractory material with the proportion of 1 in pair is prepared, the performance of the refractory material product prepared by the two technical schemes is detected, and the detection result is shown in the following table.
As can be seen from Table 1, when the aluminum chromium slag is used without flotation, the high-temperature compressive strength and the high-temperature flexural strength are significantly reduced, and therefore, the aluminum chromium slag should be used after flotation.
The embodiment is a high-performance aluminum-chromium refractory material containing about 4% of chromium oxide, only the additive and the bonding agent are different, the difference of product performance indexes is obvious from the table 2, particularly, the high-temperature rupture strength is improved by about 6MPa compared with that of the traditional example 1, the aluminum-chromium slag of the traditional example 3 is not subjected to flotation, the high-temperature rupture strength is lower by about 8MPa, and the aluminum-chromium slag flotation is necessary. The product is applied to a carbon black reaction furnace of a certain company, the service life is prolonged by about 15 percent, and the product performance of the invention is better.
Example 2.
A high-performance aluminum-chromium refractory material comprises the following materials in parts by mass: plate corundum: 45 parts of 1-8mm, 12 parts of 0.01-1mm and 7 parts of 240 meshes; electric melting chromic oxide: 3 parts of 0.01-2mm, 2.5 parts of 240 meshes, chromium oxide green: 2-8 μm 2 parts; aluminum chromium slag powder (flotation): 20 parts of 200 meshes; 1 part of alumina; phosphoric acid-zirconium aluminum chlorate solution (self-made): 3 parts, carboxymethyl cellulose (solid): 1 part; electric melting of zirconia corundum: 0.088-0.2mm1.5 parts of fused zirconia corundum: 325 mesh 2 parts and alumina short fiber 0.2 part.
A high-performance aluminum-chromium refractory material is prepared by the following specific preparation method.
(1) And (4) preparing premixed powder.
Weighing 5 parts of aluminum chromium slag powder (flotation), adding 4 parts of 240-mesh plate-shaped corundum, 1 part of alpha alumina micro powder, 240-mesh 2.5 parts of fused chromium oxide fine powder and 2 parts of chromium oxide green with the particle size of 2-8 mu m, then adding 1.5 parts of fused zirconia corundum with the particle size of 0.088-0.2mm and 2 parts of fused zirconia corundum with the particle size of 325 meshes, then premixing for 0.7h, and fully mixing to obtain premixed powder for later use.
(2) Preparing the aluminum-chromium refractory material molding pug.
Putting 45 parts of tabular corundum particles with the particle size of 1-8mm, 12 parts of tabular corundum particles with the particle size of 0.01-1mm, 3 parts of electric melting chromium oxide particles with the particle size of 0.01-2mm and 0.2 part of alumina short fibers into a mixing machine for mixing for 3 min; then adding 3 parts of self-made aluminum zirconium phosphate and 1 part of carboxymethyl cellulose, and mixing for 8min to fully attach the mixture to the aggregate; adding the rest 15 parts of floated aluminum-chromium slag powder and the premixed powder in the step (1) into a mixing machine, and fully stirring the mixture with aggregate and a binding agent for 18min to obtain pug for molding the aluminum-chromium refractory material;
note: the molding pug needs to be used up in 4-6h, if the molding pug is placed for a long time, the moisture in the pug is reduced, the pug which is not used up in the specified time and has reduced moisture can not be used any more, and the molding pug needs to be added into the newly mixed pug according to the proportion of 10-20% for reconfiguration.
(3) And (5) forming and drying.
Pressing and molding the pug for molding the aluminum-chromium refractory material by a hydraulic press or a brick press, and then drying the molded brick body for 10.5 hours at 194 ℃; and sorting the dried green bricks for later use.
(4) And (5) firing.
Firing the sorted adobes in a kiln at 1620 ℃, preserving heat for 2.8h, and taking out of the kiln to obtain the high-performance aluminum-chromium refractory material.
The preparation method of the self-made aluminum zirconium phosphate-chlorate is disclosed.
(1) According to the proportion of humic acid to oxalic acid solution =25:75, adding humic acid into 40% oxalic acid solution, and fully mixing to form emulsion, so as to prepare composite acid solution.
(2) Adding the above complex acid solution to a specific gravity of 1.5kg/cm3The aluminum dihydrogen phosphate solution of (2) is prepared by mixing the following aluminum dihydrogen phosphate solution: and (5) uniformly stirring the composite acid solution =8:2 to obtain the aluminum dihydrogen phosphate composite acid solution for later use.
(3) Slowly adding zirconium oxychloride into water at about 35 ℃, and stirring while adding zirconium oxychloride to reach the concentration of 35% to obtain the zirconium oxychloride solution.
(4) Adding the zirconium oxychloride solution and the TL-6 aluminum zirconium coupling agent into the aluminum dihydrogen phosphate composite acid solution prepared in the step (2), and mixing the following components in percentage by weight: zirconium oxychloride solution: TL-6 =6:3:1, namely the self-made aluminum zirconium phosphate-chlorate of the bonding agent is prepared.
The high-performance aluminum-chromium refractory material containing about 10% of chromium oxide is prepared in the embodiment, only the additive and the bonding agent are different, the difference of the performance indexes of the product is obvious from the table 2, and particularly, the high-temperature rupture strength is improved by about 6MPa compared with that of the traditional example 2, which shows that the product performance of the invention is more excellent.
Example 3.
A high-performance aluminum-chromium refractory material comprises the following materials in parts by mass: plate corundum: 50 parts of 1-8mm, 7 parts of 0.01-1mm and 10 parts of 240 meshes; electric melting chromic oxide: 0.5 part of 0.01-2mm, 10 parts of 240 meshes and 5 parts of chromium oxide green; 30 parts of aluminum chromium slag powder (subjected to flotation); 1 part of alumina; 4 parts of phosphoric acid-aluminum zirconium chlorate solution (self-made) and 1.5 parts of carboxymethyl cellulose; 5 parts of fused zirconia corundum with the grain size of 0.088-0.2mm, 0.5 part of fused zirconia corundum with the grain size of 325 meshes and 0.5 part of alumina short fiber.
A high-performance aluminum-chromium refractory material is prepared by the following specific preparation method.
(1) And (4) preparing premixed powder.
Weighing 5 parts of aluminum chromium slag powder (flotation), adding 10 parts of 240-mesh plate-shaped corundum, 1 part of a alumina micro powder, 240-mesh 10 parts of fused chromium oxide fine powder and 5 parts of chromium oxide green, then adding 5 parts of 0.088-0.2mm fused zirconia corundum and 0.5 part of 325-mesh fused zirconia corundum, premixing for 1h, and fully mixing to obtain premixed powder for later use.
(2) Preparing the aluminum-chromium refractory material molding pug.
Putting 50 parts of tabular corundum particles with the particle size of 1-8mm, 7 parts of tabular corundum particles with the particle size of 0.01-1mm, 0.5 part of electric melting chromium oxide particles with the particle size of 0.01-2mm and 0.5 part of alumina short fibers into a mixing machine for mixing for 2.5 min; then adding 4 parts of self-made aluminum zirconium phosphate and 1.5 parts of carboxymethyl cellulose, and mixing for 6min to fully attach the mixture to the aggregate; and adding the rest 25 parts of floated aluminum chromium slag powder and the premixed powder in the step (1) into a mixing machine, and fully stirring the mixture with aggregate and a binding agent for 16min to obtain the pug for molding the aluminum chromium refractory material.
Note: the molding pug needs to be used up in 4-6h, if the molding pug is placed for a long time, the moisture in the pug is reduced, the pug which is not used up in the specified time and has reduced moisture can not be used any more, and the molding pug needs to be added into the newly mixed pug according to the proportion of 10-20% for reconfiguration.
(3) And (5) forming and drying.
Pressing and molding the mud for molding the aluminum-chromium refractory material by a hydraulic press or a brick press, and then drying the molded brick body for 12 hours at 200 ℃; and sorting the dried green bricks for later use.
(4) And (5) firing.
Firing the sorted adobes in a kiln at 1750 ℃, keeping the temperature for 2h, and taking out of the kiln to obtain the high-performance aluminum-chromium refractory material.
The preparation method of the self-made aluminum zirconium phosphate-chlorate is disclosed.
(1) According to the proportion of humic acid to oxalic acid solution =25:75, adding humic acid into 40% oxalic acid solution, and fully mixing to form emulsion, so as to prepare composite acid solution.
(2) Adding the above complex acid solution to a specific gravity of 1.5kg/cm3The aluminum dihydrogen phosphate solution of (2) is prepared by mixing the following aluminum dihydrogen phosphate solution: and (5) uniformly stirring the composite acid solution =8:2 to obtain the aluminum dihydrogen phosphate composite acid solution for later use.
(3) Slowly adding zirconium oxychloride into water at about 40 ℃, and stirring while adding zirconium oxychloride to reach the concentration of 37 percent to obtain the zirconium oxychloride solution.
(4) Adding the zirconium oxychloride solution and the TL-6 aluminum zirconium coupling agent into the aluminum dihydrogen phosphate composite acid solution prepared in the step (2), and mixing the following components in percentage by weight: zirconium oxychloride solution: TL-6 =6:3:1, namely the self-made aluminum zirconium phosphate-chlorate of the bonding agent is prepared.
Example 4.
A high-performance aluminum-chromium refractory material comprises the following materials in parts by mass: plate corundum: 40 parts of 1-8mm, 20 parts of 0.01-1mm and 15 parts of 240 meshes; electric melting chromic oxide: 6 parts of 0.01-2mm, 3 parts of 240 meshes and 1.3 parts of chromium oxide green; 21 parts of aluminum chromium slag powder (subjected to flotation); 1.4 parts of a-alumina; 4 parts of phosphoric acid-aluminum zirconium chlorate solution (self-made) and 0.8 part of carboxymethyl cellulose; 2 parts of fused zirconia corundum with the diameter of 0.088-0.2mm, 1.1 parts of fused zirconia corundum with the mesh size of 325 and 0.25 part of alumina short fiber.
A high-performance aluminum-chromium refractory material is prepared by the following specific preparation method.
(1) And (4) preparing premixed powder.
Weighing 5 parts of aluminum chromium slag powder (flotation), adding 15 parts of 240-mesh plate-shaped corundum, 1.4 parts of alpha alumina micro powder, 240-mesh 3 parts of fused chromium oxide fine powder and 1.3 parts of chromium oxide green, then adding 2 parts of 0.088-0.2mm fused zirconia corundum and 1.1 parts of 325-mesh fused zirconia corundum, then premixing for 0.75h, and fully mixing to obtain premixed powder for later use.
(2) Preparing the aluminum-chromium refractory material molding pug.
Mixing 40 parts of tabular corundum particles with the particle size of 1-8mm, 20 parts of tabular corundum particles with the particle size of 0.01-1mm, 6 parts of electrofused chromium oxide particles with the particle size of 0.01-2mm and 0.25 part of alumina short fibers in a mixing machine for 2.5 min; then adding 4 parts of self-made aluminum zirconium phosphate and 0.8 part of carboxymethyl cellulose, and mixing for 5min to fully attach the mixture to the aggregate; and adding the remaining 16 parts of floated aluminum chromium slag powder and the premixed powder in the step (1) into a mixing machine, and fully stirring the mixture with aggregate and a binding agent for 18min to obtain the pug for molding the aluminum chromium refractory material.
Note: the molding pug needs to be used up in 4-6h, if the molding pug is placed for a long time, the moisture in the pug is reduced, the pug which is not used up in the specified time and has reduced moisture can not be used any more, and the molding pug needs to be added into the newly mixed pug according to the proportion of 10-20% for reconfiguration.
(3) And (5) forming and drying.
Pressing and molding the pug for molding the aluminum-chromium refractory material by a hydraulic press or a brick press, and then drying the molded brick body for 11 hours at 205 ℃; and sorting the dried green bricks for later use.
(4) And (5) firing.
Firing the sorted adobes in a kiln at 1620 ℃, preserving heat for 3h, and taking out of the kiln to obtain the high-performance aluminum-chromium refractory material.
The preparation method of the self-made aluminum zirconium phosphate-chlorate is disclosed.
(1) According to the proportion of humic acid to oxalic acid solution =25:75, adding humic acid into 40% oxalic acid solution, and fully mixing to form emulsion, so as to prepare composite acid solution.
(2) Adding the above complex acid solution to a specific gravity of 1.5kg/cm3The aluminum dihydrogen phosphate solution of (2) is prepared by mixing the following aluminum dihydrogen phosphate solution: and (5) uniformly stirring the composite acid solution =8:2 to obtain the aluminum dihydrogen phosphate composite acid solution for later use.
(3) Slowly adding zirconium oxychloride into water at about 40 ℃, and stirring while adding zirconium oxychloride to reach the concentration of 36 percent to obtain the zirconium oxychloride solution.
(4) Adding the zirconium oxychloride solution and the LD-139 aluminum zirconium coupling agent into the aluminum dihydrogen phosphate composite acid solution prepared in the step (2), and mixing the following components in percentage by weight: zirconium oxychloride solution: LD-139 =6:3:1, namely the self-made aluminum zirconium phosphate-chlorate of the bonding agent.
The results of the tests performed on the articles of the examples and the conventional examples are shown in the following table.
Apparent porosity, volume density, normal-temperature compressive strength, high-temperature folding resistance and the like are detected according to national standards, thermal shock stability is detected according to smelting standards, and data of conventional performance index detection are shown in the table.
The conventional examples in the table refer to: and under the condition of keeping other raw materials consistent and preparation process consistent, the aluminum phosphate binding agent and the product produced without aluminum chromium slag floatation are used.
Comparison of data from the table: compared with the traditional product (Cr)2O34 percent and 10 percent), the self-made bonding agent and the additive obviously improve the high-temperature performance of the product, in particular the high-temperature rupture strength index is improved by one grade, which reaches more than 14MPa, and the high-temperature rupture strength self-made bonding agent and the additive can be completely applied to a high-temperature high-pressure kiln with the temperature of more than 1400 ℃ and the pressure of 8.5 MPa. In addition, from the conventional product, the high-temperature rupture strength of the sample using the unrefined aluminum-chromium slag is only about 6MPa, which shows that the high-temperature strength of the product is greatly influenced by the purification and non-purification of the aluminum-chromium slag, and the purification of the aluminum-chromium slag is necessary.
The high-performance aluminum-chromium refractory material product produced by the method has excellent thermal shock stability and high-temperature rupture strength, can be used in various industrial kilns under severe conditions, is environment-friendly, saves energy, reduces consumption and has higher cost performance; in addition, the comprehensive qualified rate of the product is improved from 75-85% to 90-94% at present; in terms of cost, the cost can be reduced by 7% per ton on average; in general, the product has better effect, and also has the effects of increasing production and reducing cost.
Claims (1)
1. An aluminum-chromium refractory material is characterized by comprising aggregate, a matrix, a bonding agent and an additive:
the aggregate comprises the following materials in parts by mass: 40-50 parts of white corundum or tabular corundum particles with the diameter of 1-8mm, 1-20 parts of 0.01-1mm and 0.5-20 parts of electric melting chromium oxide particles with the diameter of 0.01-2 mm;
wherein the matrix consists of the following materials in parts by mass: 15-30 parts of aluminum chromium slag powder with 200 meshes, 2-15 parts of white corundum or tabular corundum fine powder with 240 meshes, 1-3 parts of alpha-alumina micro powder with 500 meshes, 0.5-10 parts of electric melting chromium oxide fine powder with 240 meshes and 0.5-5 parts of chromium oxide green with 2-8 mu m;
wherein the bonding agent is prepared from the following materials in parts by mass: 3-5 parts of self-made aluminum zirconium phosphate-chlorate and 0.5-1.5 parts of carboxymethyl cellulose;
wherein the additive comprises the following materials in parts by mass: 0.1-0.5 part of alumina short fiber; 1-5 parts of fused zirconia corundum with the grain size of 0.088-0.2mm and 0.5-5 parts of fused zirconia corundum with the grain size of 325 meshes;
wherein, the Al in the white corundum particles and fine powder, the tabular corundum particles and fine powder and the alpha-alumina micro powder2O3The mass fraction is more than or equal to 99.0 percent;
electrofused chromium oxide particles and fine powder, Cr thereof2O3The mass fraction is more than or equal to 99.0 percent;
the alumina short fiber, Al2O3The mass fraction is more than or equal to 99 percent, the length is 0.5-2mm, and the diameter is 10-12 mu m;
the fused zirconia corundum is Zr-40, ZrO2≥40%；
The aluminum chromium slag powder is floated aluminum chromium slag powder obtained by treating a byproduct aluminum chromium slag generated by smelting metal chromium by an aluminothermic method, wherein Al is contained in the aluminum chromium slag powder2O3Between 80 and 85 percent of Cr2O3Between 11-15%;
the specific flotation process of the aluminum chromium slag comprises the following steps: grinding the aluminum-chromium slag into fine powder of 200 meshes, filling the fine powder into a flotation machine, adding water, fully stirring, adding a flotation agent oleic acid and sodium hexametaphosphate, wherein the amount of the added oleic acid is 0.05-1.5 percent of that of the aluminum-chromium slag, the amount of the added sodium hexametaphosphate is 0.5-1.5 percent of that of the aluminum-chromium slag, then dehydrating and washing to reduce metal Al, metal Cr and metal Fe in the raw slag2O3、MgO、CaO、SiO2The content of impurities;
the preparation method of the self-made aluminum zirconium phosphate comprises the following steps:
(1) adding humic acid into oxalic acid solution with the concentration of 40% according to the proportion of humic acid to oxalic acid solution =25:75, and fully mixing to form emulsion to prepare composite acid solution;
(2) adding the above complex acid solution to a specific gravity of 1.5kg/cm3In the aluminum dihydrogen phosphate solution of (2), the ratio of aluminum dihydrogen phosphate solution: 2, uniformly stirring the composite acid solution =8:2 to obtain a composite acid solution of aluminum dihydrogen phosphate for later use;
(3) slowly adding zirconium oxychloride into water at 35-45 deg.C, stirring and adding until the concentration reaches 33-37% to obtain zirconium oxychloride solution;
(4) adding the zirconium oxychloride solution and the aluminum-zirconium coupling agent into the aluminum dihydrogen phosphate composite acid solution prepared in the step (2), and mixing the following components in percentage by weight: zirconium oxychloride solution: preparing an aluminum-zirconium coupling agent =6:3:1, namely, preparing a bonding agent self-made aluminum zirconium phosphate-chlorate; wherein the aluminum-zirconium coupling agent is one or two of LD-139 or TL-6;
the preparation method of the aluminum-chromium refractory material comprises the following steps:
(1) preparation of premixed flour
Weighing 5 parts of aluminum chromium slag powder, adding 2-15 parts of 240-mesh white corundum or tabular corundum, 1-3 parts of alpha alumina micropowder, 240-mesh 0.5-10 parts of fused chromium oxide fine powder and 0.5-5 parts of 2-8 mu m chromium oxide green, then adding 1-5 parts of 0.088-0.2mm fused zirconia corundum and 0.5-5 parts of 325-mesh fused zirconia corundum, premixing for 0.5-1h, and fully mixing to obtain premixed powder for later use;
(2) preparation of aluminium-chromium refractory material forming pug
Mixing white corundum or tabular corundum particles of 1-8mm in 40-50 weight portions, electrically fused chromium oxide particles of 0.01-1mm in 1-20 weight portions and alumina short fibers of 0.1-0.5 weight portion in a kneading machine for 2-3 min; then adding 3-5 parts of a binding agent of aluminum zirconium phosphate-chlorate and 0.5-1.5 parts of carboxymethyl cellulose, and mixing for 5-8min to fully attach the mixture to the aggregate; adding the rest 10-25 parts of the aluminum chromium slag powder and the premixed powder in the step (1) into a mixing machine, and fully stirring the mixture with aggregate and a binding agent for 15-18min to obtain pug for molding the aluminum chromium refractory material;
(3) drying the formed product
Pressing and molding the mud for molding the aluminum-chromium refractory material by a hydraulic press or a brick press, and then drying the molded brick body at the temperature of 210 ℃ for 10-12 h; sorting the dried green bricks for later use;
(4) firing into
And firing the sorted adobes in a kiln at 1550-.
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| CN102557683A (en) * | 2011-12-23 | 2012-07-11 | 中钢集团洛阳耐火材料研究院有限公司 | Aluminum chrome refractory material |
| CN103274713A (en) * | 2013-06-28 | 2013-09-04 | 上海智环建设工程有限公司 | High-aluminum ramming material adopting zirconium oxychloride as additive |
| CN103755361A (en) * | 2013-12-20 | 2014-04-30 | 中钢集团洛阳耐火材料研究院有限公司 | Aluminum-chromium-silicon fireproof material |
| CN103740284A (en) * | 2014-01-06 | 2014-04-23 | 武汉双虎涂料有限公司 | High temperature-resistant composite inorganic binder, as well as preparation method and application thereof |
| CN108101516A (en) * | 2018-01-15 | 2018-06-01 | 中钢集团洛阳耐火材料研究院有限公司 | A kind of alumina-silica Cr refractory product and preparation method thereof |
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