Production method of zirconia brick for ultra-high temperature carbon black furnace
阅读说明：本技术 一种特高温炭黑炉用氧化锆砖的生产方法 (Production method of zirconia brick for ultra-high temperature carbon black furnace ) 是由 宋二鹏 宋进朝 孟祥峰 于 2020-12-30 设计创作，主要内容包括：本发明涉及一种特高温炭黑炉用氧化锆砖的生产原料,所述的生产原料由氧化锆粉、Al-2O-3微粉、二氧化锆溶胶和糊精四种物质构成；该生产原料总配比为：以质量计,Al-2O-3微粉占2-4%,二氧化锆溶胶占2.5～3.5%,糊精占1.5～2.0%,余为氧化锆粉。本发明制备的特高温炭黑炉用氧化锆砖具有以下参数性质：ZrO-2≥80%,体积密度≥4.85g/cm～3；常温耐压强度≥35MPa,经高温烧结后耐压强度可达100MPa以上；热膨胀系数(200～1000℃)9.0×10-6(1/℃)。热震稳定性(1100oC-水冷):≥3次。导热系数3～4W/m.K。长期使用温度：2100～2300℃；且氧化锆砖在氧化、还原气氛中都保持稳定。(The invention relates to a raw material for producing zirconia bricks for an ultra-high temperature carbon black furnace, which comprises zirconia powder and Al 2 O 3 The coating consists of four substances, namely micro powder, zirconium dioxide sol and dextrin; the total proportion of the production raw materials is as follows: by mass, Al 2 O 3 2-4% of micro powder, 2.5-3.5% of zirconium dioxide sol, 1.5-2.0% of dextrin and the balance of zirconium oxide powder. The zirconia brick for the ultra-high temperature carbon black furnace prepared by the invention has the following parameter properties: ZrO (ZrO) 2 Not less than 80 percent and volume density not less than 4.85g/cm 3 (ii) a The normal temperature compressive strength is more than or equal to 35MPa, and the compressive strength can reach more than 100MPa after high-temperature sintering; a coefficient of thermal expansion (200 to 1000 ℃) of 9.0X 10-6 (1/. degree. C.). The thermal shock stability (1100 ℃ to water cooling) is more than or equal to 3 times. The thermal conductivity is 3-4W/m.K. Long-term service temperature: 2100-2300 ℃; and the zirconia brick keeps stable in oxidation and reduction atmosphere.)
1. Zirconia brick for ultra-high temperature carbon black furnaceThe production raw material is characterized by comprising zirconia powder and Al2O3Micropowder, zirconium dioxide sol and dextrin.
2. The zirconia brick raw material for production according to claim 1, wherein the raw material comprises the following components in percentage by weight: by mass, Al2O32-4% of micro powder, 2.5-3.5% of zirconium dioxide sol, 1.5-2.0% of dextrin and the balance of zirconium oxide powder.
3. A raw material for zirconia brick according to claim 1 or 2, wherein said Al is2O3The micro powder is rho-Al2O3And (5) micro-powder.
4. The raw material for producing the zirconia brick according to claim 1 or 2, wherein the zirconia sol is a nano zirconia sol having a specific gravity of ρ =1.05 to 1.10g/cm3。
5. The raw material for producing the zirconia brick according to claim 1 or 2, wherein the zirconia powder is composed of yttrium-stabilized zirconia powder and monoclinic electrofused zirconia powder.
6. A raw material for producing a zirconia brick according to claim 5, wherein the monoclinic electrofused zirconia powder has a particle size of 1 μm.
7. A raw material for zirconia brick production according to claim 6, wherein said yttrium-stabilized zirconia powder comprises four kinds of particles: 1-2mm, 0.5-1mm, 0.1-0.5mm, 320 mesh +/-20 mesh; the proportion of the raw materials in the total proportion of the production raw materials is as follows: by mass: 25-45% of yttrium-stabilized zirconia powder with the particle size of 1-2 mm; 10-20% of yttrium-stabilized zirconia powder with the particle size of 0.5-1 mm; 5-20% of yttrium-stabilized zirconia powder with the grain diameter of 0.1-0.5 mm; the yttrium-stabilized zirconia powder with the grain diameter of 320 meshes accounts for 25-35%.
8. The method for manufacturing zirconia bricks for ultra-high temperature carbon black furnaces according to the raw materials for production of claim 7, wherein the method comprises the following parameters and steps:
the total proportion of production raw materials is as follows:
by mass: 25-45% of yttrium-stabilized zirconia powder with the particle size of 1-2 mm;
10-20% of yttrium-stabilized zirconia powder with the particle size of 0.5-1 mm;
5-20% of yttrium-stabilized zirconia powder with the grain diameter of 0.1-0.5 mm;
25-35% of yttrium-stabilized zirconia powder with the grain size of 320 meshes +/-20 meshes;
Al2O3the micro powder accounts for 2 to 4 percent;
the zirconium dioxide sol accounts for 2.5-3.5%;
dextrin accounts for 1.5-2.0%;
the process flow comprises the following steps:
(1) fine powder premixing:
accurately weighing 320-mesh +/-20-mesh yttrium-stabilized zirconia powder, 1-micron monoclinic fused zirconia powder and rho-Al according to the total proportion of production raw materials2O3Mixing the micro powder and dextrin in a pre-mixer for 30min, and discharging for later use;
(2) mixing the aggregate:
accurately weighing 1-2mm, 0.5-1mm and 0.1-0.5mm yttrium-stabilized zirconia particles according to the formula amount, adding the yttrium-stabilized zirconia particles into a wet mill, dry-mixing for 2-3 min, adding 2/3 amount of nano zirconia sol solution, mixing for 5-10 min,
then adding the fine powder obtained after premixing in the step (1), mixing for 3-5 min, then adding the remaining 1/3-amount nano zirconium dioxide sol solution, finally mixing for 15-25 min, and discharging;
(3) molding: molding the pug obtained in the step (2) by adopting a friction press;
(4) drying: drying the green brick formed in the step (3) at 120 ℃ for 12-24 hours;
(5) and (3) firing: and (4) firing the dried green brick in the step (4) at the temperature of 1800-1850 ℃.
9. The method of claim 8, wherein in step (3), the press is 315t, 630t or 1000 t.
10. The method according to claim 8, wherein in the step (5), the sintering holding time is 8-12 hours.
Technical Field
The invention belongs to the technical field of a production method of a zirconia brick for an extra-high temperature carbon black furnace, and particularly relates to the technical field of production raw materials and production methods of the zirconia brick for the extra-high temperature carbon black furnace.
Background
The carbon black is produced by high-temperature cracking natural gas or heavy oil in a carbon black reaction furnace. The carbon black reaction furnace consists of five parts, namely a combustion chamber, a throat pipe, a reaction section, a quenching section and a retention section. In the process of producing the carbon black, the temperature of a combustion section in a carbon black reaction furnace is usually 1600-1700 ℃; the throat pipe and the reaction section are high-temperature areas, and the working temperature is up to 1900-; moving speed of hot air flow in furnaceThe diameter of the throat pipe is as large as 340-370 m.s, and the end of the throat pipe is the maximum of the whole furnace-1. In addition, the ash generated after pyrolysis of fuel and raw material contains oxides and compounds of elements such as V, Ni, Na, Ca, S, etc., and has a great corrosive effect on the substrate material. The furnace lining is subject to the scouring and erosion action of high-temperature flue gas, and is easy to be peeled off and corroded and damaged.
At present, ZrO has been produced2Reports on the research and application of the components introduced into the carbon black reaction furnace lining refractory. Adopts Al2O3-Cr2O3Is or at Al2O3-Cr2O3Introducing a certain amount of ZrO into the system2The material is used as the lining of the high-temperature section of the reaction furnace and is more used in the United states and some countries in Western Europe. In Al2O3-Cr2O3Introduction of ZrO into the system2The purpose is to improve the thermal shock resistance and chemical erosion resistance of the system material and prolong the service life of the furnace lining material. Pure ZrO used as lining of high-temperature carbon black reaction furnace2The quality product is a new product developed and used in recent years. Pure ZrO developed in Japan using CaO or MgO as stabilizer2The brick is tried in the inner linings of a combustion chamber, a throat pipe section, a reaction section and a cooling section of a high-grade carbon black reaction furnace, and the product is found to have poor thermal shock resistance and ZrO under the reducing atmosphere of about 1600 DEG C2Failure problems caused by reaction with C to form ZrC.
Disclosure of Invention
The invention aims to solve the defects of the problems and provides a method for producing zirconia bricks for an ultra-high temperature carbon black furnace.
The technical improvement anticipates: partial stabilization of ZrO2The high-temperature-resistant ZrO addition agent can improve the compressive strength and the thermal shock resistance of the product by adding a proper amount of additive and firing at high temperature, is used in a high-temperature and ultrahigh-temperature reducing atmosphere of a reaction furnace, and avoids ZrO at about 1600 DEG C2Reacts with C to form ZrC-induced erosion. However, what additives can meet the technical expectations of the present invention becomes a technical problem to be solved. In particular, the addition of additives does not lead to a too high, preferably even and better reduction of the energy consumption in the production step.
In view of the above, the present invention is achieved as follows.
The invention relates to a raw material for producing zirconia bricks for an ultra-high temperature carbon black furnace, which comprises zirconia powder and Al2O3Micropowder, zirconium dioxide sol and dextrin.
Further, the total proportion of the production raw materials is as follows: by mass, Al2O32-4% of micro powder, 2.5-3.5% of zirconium dioxide sol, 1.5-2.0% of dextrin and the balance of zirconium oxide powder.
Further, Al according to the present invention2O3The micro powder is rho-Al2O3And (5) micro-powder.
Further, the zirconium dioxide sol is nano zirconium dioxide sol, and the specific gravity of the zirconium dioxide sol is rho = 1.05-1.10 g/cm3. The nano zirconium dioxide sol has two functions: a binder and a filler.
Furthermore, the zirconia powder of the invention is composed of yttrium-stabilized zirconia powder and monoclinic electric melting zirconia powder.
Further, the monoclinic electric melting zirconia powder has the grain diameter of 1 mu m.
Further, the yttrium-stabilized zirconia powder of the present invention comprises four particle sizes: 1-2mm, 0.5-1mm, 0.1-0.5mm, 320 mesh +/-20 mesh; the proportion of the raw materials in the total proportion of the production raw materials is as follows: by mass: 25-45% of yttrium-stabilized zirconia powder with the particle size of 1-2 mm; 10-20% of yttrium-stabilized zirconia powder with the particle size of 0.5-1 mm; 5-20% of yttrium-stabilized zirconia powder with the grain diameter of 0.1-0.5 mm; the yttrium-stabilized zirconia powder with the grain diameter of 320 meshes +/-20 meshes accounts for 25-35 percent. The four kinds of yttrium-stabilized zirconia powder with different particle sizes are used, so that the critical strength is increased, the stability is enhanced, and the method is energy-saving and environment-friendly.
The yttrium-stabilized zirconia powder of the invention comprises four particle sizes: 1-2mm, 0.5-1mm, 0.1-0.5mm, 320 mesh +/-20 mesh; wherein:
1-2mm is more than 1mm and less than or equal to 2 mm;
0.5-1mm is more than or equal to 0.5mm and less than or equal to 1 mm;
0.1-0.5mm is more than or equal to 0.1mm and less than 0.5 mm;
the 320 meshes +/-20 meshes are carried out according to the international mesh standard, and the particle size of 300 meshes is 0.050 mm.
The method for manufacturing the zirconia brick for the ultra-high temperature carbon black furnace by using the production raw materials is characterized by comprising the following parameters and steps:
the total proportion of production raw materials is as follows:
by mass: 25-45% of yttrium-stabilized zirconia powder with the particle size of 1-2 mm;
10-20% of yttrium-stabilized zirconia powder with the particle size of 0.5-1 mm;
5-20% of yttrium-stabilized zirconia powder with the grain diameter of 0.1-0.5 mm;
25-35% of yttrium-stabilized zirconia powder with the grain size of 320 meshes +/-20 meshes;
Al2O3the micro powder accounts for 2 to 4 percent;
the zirconium dioxide sol accounts for 2.5-3.5%;
dextrin accounts for 1.5-2.0%;
the process flow comprises the following steps:
(1) fine powder premixing:
accurately weighing 320-mesh +/-20-mesh yttrium-stabilized zirconia powder, 1-micron monoclinic fused zirconia powder and rho-Al according to the total proportion of production raw materials2O3Mixing the micro powder and dextrin in a pre-mixer for 30min, and discharging for later use;
(2) mixing the aggregate:
accurately weighing 1-2mm, 0.5-1mm and 0.1-0.5mm yttrium-stabilized zirconia particles according to the formula amount, adding the yttrium-stabilized zirconia particles into a wet mill, dry-mixing for 2-3 min, adding 2/3 amount of nano zirconia sol solution, mixing for 5-10 min,
then adding the fine powder obtained after premixing in the step (1), mixing for 3-5 min, then adding the remaining 1/3-amount nano zirconium dioxide sol solution, finally mixing for 15-25 min, and discharging;
(3) molding: molding the pug obtained in the step (2) by adopting a friction press;
(4) drying: drying the green brick formed in the step (3) at 120 ℃ for 12-24 hours;
(5) and (3) firing: and (4) firing the dried green brick in the step (4) at the temperature of 1800-1850 ℃. Aiming at the traditional sintering process standard of 1750-1800 ℃, the invention only increases 50 ℃ on the basis of the prior art, and can meet the requirement of all production raw materials on the total proportion to produce the zirconia brick for the ultra-high temperature carbon black furnace, which has the parameter property recorded in the beneficial effect of the invention.
Further, in step (3) of the method of the present invention, the press is 315t, 630t or 1000 t.
Further, in the step (5), the sintering and heat preservation time is 8-12 hours.
The invention has the beneficial effects that the invention adopts nano zirconium dioxide sol as a binder, zirconia bricks are used in the reaction section of the ultra-high temperature carbon black furnace and the throat, and sintering aids such as superfine zirconia, alumina micropowder and the like are added to the zirconia bricks to be sintered at the high temperature of 1850 ℃. The zirconia brick of the extra-high temperature carbon black furnace produced by the invention can meet the use requirements of the high temperature section of the relevant special carbon black furnace. The zirconia brick for the ultra-high temperature carbon black furnace prepared by the invention has the following parameter properties: ZrO (ZrO)2Not less than 80 percent and volume density not less than 4.85g/cm3(ii) a The normal temperature compressive strength is more than or equal to 35MPa, and the compressive strength can reach more than 100MPa after high-temperature sintering; a coefficient of thermal expansion (200 to 1000 ℃) of 9.0X 10-6 (1/. degree. C.). The thermal shock stability (1100 ℃ to water cooling) is more than or equal to 3 times. The thermal conductivity is 3-4W/m.K. Long-term service temperature: 2100-2300 ℃; and the zirconia brick keeps stable in oxidation and reduction atmosphere.
The invention is further explained below with reference to specific embodiments.
Detailed Description
The invention relates to a raw material for producing zirconia bricks for an ultra-high temperature carbon black furnace, which comprises zirconia powder and Al2O3Micropowder, zirconium dioxide sol and dextrin.
Further, the total proportion of the production raw materials is as follows: by mass, Al2O32-4% of micro powder, 2.5-3.5% of zirconium dioxide sol, 1.5-2.0% of dextrin and the balance of zirconium oxide powder.
Further, the present invention isThe Al is2O3The micro powder is rho-Al2O3And (5) micro-powder.
Further, the zirconium dioxide sol is nano zirconium dioxide sol, and the specific gravity of the zirconium dioxide sol is rho = 1.05-1.10 g/cm3. The nano zirconium dioxide sol has two functions: a binder and a filler.
Furthermore, the zirconia powder of the invention is composed of yttrium-stabilized zirconia powder and monoclinic electric melting zirconia powder.
Further, the monoclinic electric melting zirconia powder has the grain diameter of 1 mu m.
Further, the yttrium-stabilized zirconia powder of the present invention comprises four particle sizes: 1-2mm, 0.5-1mm, 0.1-0.5mm, 320 mesh +/-20 mesh; the proportion of the raw materials in the total proportion of the production raw materials is as follows: by mass: 25-45% of yttrium-stabilized zirconia powder with the particle size of 1-2 mm; 10-20% of yttrium-stabilized zirconia powder with the particle size of 0.5-1 mm; 5-20% of yttrium-stabilized zirconia powder with the grain diameter of 0.1-0.5 mm; the yttrium-stabilized zirconia powder with the grain diameter of 320 meshes +/-20 meshes accounts for 25-35 percent. The four kinds of yttrium-stabilized zirconia powder with different particle sizes are used, so that the critical strength is increased, the stability is enhanced, and the method is energy-saving and environment-friendly.
The yttrium-stabilized zirconia powder of the invention comprises four particle sizes: 1-2mm, 0.5-1mm, 0.1-0.5mm, 320 mesh +/-20 mesh;
wherein:
1-2mm is more than 1mm and less than or equal to 2 mm;
0.5-1mm is more than or equal to 0.5mm and less than or equal to 1 mm;
0.1-0.5mm is more than or equal to 0.1mm and less than 0.5 mm;
the 320 meshes +/-20 meshes are carried out according to the international mesh standard, and the particle size of 300 meshes is 0.050 mm.
The method for manufacturing the zirconia brick for the ultra-high temperature carbon black furnace by using the production raw materials is characterized by comprising the following parameters and steps:
the total proportion of production raw materials is as follows:
by mass: 25-45% of yttrium-stabilized zirconia powder with the particle size of 1-2 mm;
10-20% of yttrium-stabilized zirconia powder with the particle size of 0.5-1 mm;
5-20% of yttrium-stabilized zirconia powder with the grain diameter of 0.1-0.5 mm;
25-35% of yttrium-stabilized zirconia powder with the grain size of 320 meshes +/-20 meshes;
Al2O3the micro powder accounts for 2 to 4 percent;
the zirconium dioxide sol accounts for 2.5-3.5%;
dextrin accounts for 1.5-2.0%;
the process flow comprises the following steps:
(1) fine powder premixing:
accurately weighing 320-mesh +/-20-mesh yttrium-stabilized zirconia powder, 1-micron monoclinic fused zirconia powder and rho-Al according to the total proportion of production raw materials2O3Mixing the micro powder and dextrin in a pre-mixer for 30min, and discharging for later use;
(2) mixing the aggregate:
accurately weighing 1-2mm, 0.5-1mm and 0.1-0.5mm yttrium-stabilized zirconia particles according to the formula amount, adding the yttrium-stabilized zirconia particles into a wet mill, dry-mixing for 2-3 min, adding 2/3 amount of nano zirconia sol solution, mixing for 5-10 min,
then adding the fine powder obtained after premixing in the step (1), mixing for 3-5 min, then adding the remaining 1/3-amount nano zirconium dioxide sol solution, finally mixing for 15-25 min, and discharging;
(3) molding: molding the pug obtained in the step (2) by adopting a friction press;
(4) drying: drying the green brick formed in the step (3) at 120 ℃ for 12-24 hours;
(5) and (3) firing: and (4) firing the dried green brick in the step (4) at the temperature of 1800-1850 ℃. Aiming at the traditional sintering process standard of 1750-1800 ℃, the invention only increases 50 ℃ on the basis of the prior art, and can meet the requirement of all production raw materials on the total proportion to produce the zirconia brick for the ultra-high temperature carbon black furnace, which has the parameter property recorded in the beneficial effect of the invention.
Further, in step (3) of the method of the present invention, the press is 315t, 630t or 1000 t.
Further, in the step (5), the sintering and heat preservation time is 8-12 hours.
Since the formulation of the present invention falls within the numerical range, the examples are not exhaustive, and only some extreme counter examples and effects are described to show the reliability of the technical gist of the present invention.
1) The zirconia powder of the invention adopts yttrium-stabilized zirconia powder with the grain diameter of 1-2mm, the roughness is stronger after sample mixing, and the later volume density and the compressive strength do not reach the standard.
2) The zirconia powder of the invention adopts the yttrium stabilized zirconia powder with the grain diameter of 320 meshes +/-20 meshes, the roughness is stronger after the sample is mixed, the later-stage volume density and the compressive strength reach the standards, but the sintering temperature is increased too high, and the energy consumption is higher.
3) The fine powder premixing and the aggregate mixing are reversely adjusted, so that the density distribution of the unit volume of the produced zirconia brick is not uniform, and the compressive strength is not up to the standard.
4) The production raw materials are sintered at the traditional temperature of 1750-1800 ℃ after being mixed in total, and the compressive strength after being sintered does not reach the standard; the firing temperature is insufficient, and the thermal expansion coefficient and the thermal shock stability of the product do not reach the standard.
The technical parameters of the invention, more test steps and results, and the limitation of the contents are not provided for all, and the complete technical scheme of the invention is subject to the scope of the invention published in the specification.
The above description is only a part of the specific embodiments of the present invention (the protection scope of the present invention is defined by the numerical range of the present invention and other technical points), and the details or common sense of the technical solutions are not described herein too much. It should be noted that the above-mentioned embodiments do not limit the present invention in any way, and all technical solutions obtained by means of equivalent substitution or equivalent transformation for those skilled in the art are within the protection scope of the present invention. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.