CN110028316B

CN110028316B - Cordierite kiln furniture sagger and preparation method thereof

Info

Publication number: CN110028316B
Application number: CN201910412070.0A
Authority: CN
Inventors: 孙华云
Original assignee: Shandong Vocational College of Industry
Current assignee: Shandong Vocational College of Industry
Priority date: 2019-05-17
Filing date: 2019-05-17
Publication date: 2022-06-03
Anticipated expiration: 2039-05-17
Also published as: CN110028316A

Abstract

A cordierite kiln furniture sagger and a preparation method thereof belong to the technical field of refractory materials. The formula is characterized by comprising the following raw materials in parts by weight: 3-1mm mullite M4710-15 parts, 1-0mm mullite M4710-15 parts, 2-1mm cordierite 16-20 parts, cordierite with particle size less than 150 meshes 7-12 parts, 0.5-0mm sillimanite 8-13 parts, andalusite with particle size less than 200 meshes 7-13 parts, silicon carbide with particle size less than 240 meshes 4-7 parts, leucoderma with particle size less than 240 meshes 5-10 parts, alumina CA370C micro powder 3-6 parts, 0.045mm Suzhou soil 4-6 parts, paper pulp 3.5-5.5 parts, phosphoric acid 0.3-0.6 part and dextrin 0.3-0.6 part. The invention has enough high-temperature refractoriness under load, higher refractoriness and good rapid cooling and heat shock resistance. After the sagger is repeatedly heated and cooled, a certain mechanical strength can be still maintained, and the sagger is not cracked.

Description

Cordierite kiln furniture sagger and preparation method thereof

Technical Field

A cordierite kiln furniture sagger and a preparation method thereof belong to the technical field of refractory materials.

Background

Sagger is a long-term kiln furniture used in kiln, and is a consumable material. The method is widely applied to the industries of ceramics, building materials, chemical industry, metallurgy, glass and the like. Most saggers applied at present are limited in bearing capacity due to heavy weight, and are high in energy consumption, poor in heat penetration performance, easy to crack in the using process, high in breakage rate and short in service life. How to improve the mechanical strength, high-temperature refractoriness under load, rapid cooling and heating resistance, refractoriness and thermal conductivity of the saggar is a problem to be solved urgently at present.

Disclosure of Invention

The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art and provides a cordierite kiln furniture sagger with high use temperature and long service life and a preparation method thereof.

The technical scheme adopted by the invention for solving the technical problem is as follows: the cordierite kiln furniture sagger is characterized by comprising the following raw materials in parts by weight: 3-1mm mullite M4710-15 parts, 1-0mm mullite M4710-15 parts, 2-1mm cordierite 16-20 parts, cordierite with particle size less than 150 meshes 7-12 parts, 0.5-0mm sillimanite 8-13 parts, andalusite with particle size less than 200 meshes 7-13 parts, silicon carbide with particle size less than 240 meshes 4-7 parts, leucoderma with particle size less than 240 meshes 5-10 parts, alumina CA370C micro powder 3-6 parts, 0.045mm Suzhou soil 4-6 parts, paper pulp 3.5-5.5 parts, phosphoric acid 0.3-0.6 part and dextrin 0.3-0.6 part.

The cordierite has the advantages of small thermal expansion coefficient, good thermal shock resistance stability and the like, and is mainly used for the production of ceramic kiln furniture. The linear expansion coefficient of cordierite at 20-1000 deg.C is 1.1-2.0 x 10^-6Per deg.C, silicon carbide 4.7X 10^-6V. mullite 5.3X 10^-6At the same temperature,/° CThe lower expansion coefficients are different, and a thermal expansion coefficient gradient is formed. Cordierite has poor high-temperature performance, instability and a narrow firing range, while mullite has high refractoriness, good high-temperature creep resistance, good spalling resistance and erosion resistance and high-temperature stability. Due to mismatch of thermal expansion coefficients of cordierite and mullite, microcracks are formed on a two-phase interface, and although the material has better thermal shock resistance and high-temperature performance, the service life is still insufficient; the invention adds proper amount of SiC with high heat conductivity coefficient, improves the heat conductivity of the kiln furniture, reduces the temperature difference of each part of the kiln furniture in the rapid cooling and rapid heating process, reduces the thermal stress, improves the thermal shock resistance of the kiln furniture and prolongs the service life.

Cordierite is added to form a mullite-cordierite-silicon carbide tissue structure, the expansion coefficient of the structure is smaller than that of the mullite-silicon carbide, and the thermal shock resistance is superior to that of a mullite-silicon carbide material.

M47 is artificially synthesized mullite aggregate calcined at 1580 ℃, the main crystal phase is columnar mullite, and a small amount of glass phase and aluminum titanate are filled in mullite crystal spaces to form a continuous framework structure. The aggregate has low iron content, low porosity, high density and good erosion resistance.

The mullite and the sillimanite are utilized to form a needle-shaped network structure at high temperature, so that the high-temperature stability, the thermal shock resistance and the creep resistance of the product are improved, and the medium-high temperature strength of the kiln furniture is improved.

SiO formed by decomposing andalusite and sillimanite in matrix₂And SiO generated by oxidation of SiC₂Reacts with fine corundum sand powder and alumina micro powder to form a secondary mullite network which is inserted between mullite aggregates, so that the high-temperature stability, creep resistance and thermal shock resistance of the product are further improved.

Based on the physical and chemical properties, the product has corrosion resistance, no slag falling and long service life in the use process, is incomparable with the traditional corundum-mullite, mullite-cordierite and the like, and is an ideal kiln furniture with the use temperature below 1400 ℃.

Preferably, the raw materials comprise the following components in parts by weight: 3-1mm mullite M4712-14 parts, 1-0mm mullite M4712-14 parts, 2-1mm cordierite 17-19 parts, cordierite with a particle size of less than 150 meshes 9-10 parts, 0.5-0mm sillimanite 9-11 parts, andalusite with a particle size of less than 200 meshes 9-10 parts, silicon carbide with a particle size of less than 240 meshes 5.5-6.5 parts, sub-white corundum with a particle size of less than 240 meshes 7-8 parts, alumina CA370C micro powder 4-5 parts, 0.045mm Suzhou soil 4.5-5.6 parts, paper pulp 4.2-5.1 parts, phosphoric acid 0.4-0.5 part, and 0.4-0.5 part of dextrin. Better thermal shock property and strength can be achieved under the preferable raw material proportion.

Preferably, the chemical mass percentage composition of the 3-1mm mullite M47 and the 1-0mm mullite M47 is Al₂O₃50%~50.3%，Fe₂O₃0.82%~0.92%，SiO₂46.8%~47.05%，TiO₂0.91%~0.94%，MgO0.05%~0.07%，CaO0.65%~0.72%，Na₂0.09% -0.11% of O and the balance of impurities.

Preferably, the chemical mass percentage composition of the 2-1mm cordierite and the cordierite with the grain diameter of less than 150 meshes is Al₂O₃34.12%~34.56%，Fe₂O₃0.75%~0.94%，SiO₂48.56%~49.12%，TiO₂0.75% -1.13%, MgO13.11% -13.35% and the balance of impurities.

The preferable composition of mullite and cordierite can be better matched to achieve better thermal shock resistance and high-temperature performance.

More preferably, the chemical mass percentage composition of the 3-1mm mullite M47 and the 1-0mm mullite M47 is Al₂O₃50.20%，Fe₂O₃0.86%，SiO₂47.01%，TiO₂0.93%，MgO 0.06%，CaO 0.69%，Na₂0.11% of O and the balance of impurities; the refractoriness is 1770 ℃.

More preferably, the chemical mass percentage composition of the 2-1mm cordierite and the cordierite with the grain diameter of less than 150 meshes is Al₂O₃34.39%，Fe₂O₃0.88%，SiO₂48.83%，TiO₂0.95 percent, MgO13.23 percent and the balance of impurities; the refractoriness was 1380 ℃.

The more preferred compositions of mullite and cordierite can better match to achieve the best thermal shock resistance and high temperature performance of the present invention.

A preparation method of a cordierite kiln furniture sagger is characterized by comprising the following steps:

1) adding the raw materials into a planetary wet mill according to the proportion, stirring for 20 minutes, uniformly mixing, discharging, and ageing for 12-15 hours;

2) molding by a hydraulic press, controlling the porosity of the wet blank to be 18.5-20.0% and the volume density of the wet blank to be 2.48 g/cm³~2.68g/cm³；

3) Drying the drying holes at 40-110 ℃, wherein the sound is played well without cracks before loading, and the residual water content is 0.45-0.52%;

4) and (3) sintering in a tunnel kiln, wherein the sintering temperature is 1340-1360 ℃, and the sintering time is 6-8 h.

Preferably, the porosity of the wet blank in the step 2) is 19-19.5%, and the volume density of the wet blank is 2.53 g/cm³~2.60g/cm³。

Preferably, the drying temperature in the step 3) is 50-60 ℃, and the residual moisture is 0.48-0.50%.

Preferably, the firing temperature in the step 4) is 1350 ℃ and the firing time is 7 hours.

Compared with the prior art, the invention has the beneficial effects that:

(1) sufficient room-temperature mechanical strength. The sagger is not damaged when carrying and loading the sagger to bear weight.

(2) Sufficient high temperature refractoriness under load. The firing temperature of the sagger is higher than that of the contained product by more than 50-100 ℃, so that the sagger is prevented from softening and deforming at the firing temperature of the product.

(3) Higher refractoriness. The sintering temperature of the product is higher than that of the filled product by more than 300 ℃.

(4) Good resistance to rapid cooling and rapid heating. After the sagger is repeatedly heated and cooled, a certain mechanical strength can be still maintained, and the sagger is not cracked. The cordierite sagger has good thermal stability and long service life. It is especially suitable for roller kilns of ceramics, glass, metallurgy, chemical industry and other rapid sintering.

(5) Good heat-conducting property and low heat storage property.

Detailed Description

The invention is further illustrated by the following specific examples, of which example 1 is the best mode of practice.

Example 1

1) Adding the raw materials into a planetary wet mill according to the proportion and stirring for 20 minutes; the raw materials comprise the following components in parts by weight: 3-1mm mullite M4713 parts, 1-0mm mullite M4713 parts, 2-1mm cordierite 18 parts, cordierite with the grain size of less than 150 meshes 9.5 parts, 0.5-0mm sillimanite 10 parts, andalusite with the grain size of less than 200 meshes 9.5 parts, silicon carbide with the grain size of less than 240 meshes 6 parts, sub-white corundum with the grain size of less than 240 meshes 7.5 parts, alumina CA370C micro powder 4.5 parts, 0.045mm Suzhou soil 5 parts, paper pulp 4.5 parts, phosphoric acid 0.45 part and dextrin 0.45 part; the chemical mass percentage composition of the 3-1mm mullite M47 and the 1-0mm mullite M47 is Al₂O₃50.20%，Fe₂O₃0.86%，SiO₂47.01%，TiO₂0.93%，MgO 0.06%，CaO 0.69%，Na₂0.11% of O and the balance of impurities; the refractoriness is 1770 ℃; the chemical mass percentage composition of 2-1mm cordierite and cordierite with grain diameter less than 150 meshes is Al₂O₃34.39%，Fe₂O₃0.88%，SiO₂48.83%，TiO₂0.95 percent, MgO13.23 percent and the balance of impurities; the refractoriness is 1380 ℃; uniformly mixing, discharging and ageing for 13 hours;

2) molding by a hydraulic press, controlling the porosity of the wet blank to be 19 percent and the volume density of the wet blank to be 2.56g/cm³；

3) Drying at 55 deg.C, making sound before loading, and residual water content of 0.49%;

4) and (4) sintering in a tunnel kiln at 1350 ℃ for 7 h.

Example 2

1, adding the raw materials into a planetary wet mill according to the proportion and stirring for 20 minutes; the raw materials comprise the following components in parts by weight: 3-1mm mullite M4714 parts, 1-0mm mullite M4712 parts, 2-1mm cordierite 19 parts, cordierite with the grain size of less than 150 meshes 9 parts, 0.5-0mm sillimanite 11 parts, andalusite with the grain size of less than 200 meshes 9 parts, silicon carbide with the grain size of less than 240 meshes 6.5 parts, sub-white corundum with the grain size of less than 240 meshes 7 parts, alumina CA370C micro powder 5 parts, 0.045mm Suzhou soil 4.5 parts, paper pulp 5.1 parts, phosphoric acid 0.4 part and dextrin 0.5 part; the chemical mass percentage composition of the 3-1mm mullite M47 and the 1-0mm mullite M47 is Al₂O₃50.20%，Fe₂O₃0.86%，SiO₂47.01%，TiO₂0.93%，MgO 0.06%，CaO 0.69%，Na₂0.11% of O and the balance of impurities; the refractoriness is 1770 ℃; the chemical mass percentage composition of 2-1mm cordierite and cordierite with grain diameter less than 150 meshes is Al₂O₃34.39%，Fe₂O₃0.88%，SiO₂48.83%，TiO₂0.95 percent, MgO13.23 percent and the balance of impurities; the refractoriness is 1380 ℃; uniformly mixing, discharging and ageing for 14 hours;

2) molding by a hydraulic press, controlling the porosity of the wet blank to be 19.5 percent and the volume density of the wet blank to be 2.60g/cm³；

3) Drying at 60 deg.C in drying hole, making sound before loading, and residual water content of 0.50%;

4) and (4) sintering in a tunnel kiln at 1350 ℃ for 7 h.

Example 3

1) Adding the raw materials into a planetary wet mill according to the proportion and stirring for 20 minutes; the raw materials comprise the following components in parts by weight: 3-1mm mullite M4712 parts, 1-0mm mullite M4714 parts, 2-1mm cordierite 17 parts, cordierite with the grain size of less than 150 meshes 10 parts, 0.5-0mm sillimanite 9 parts, andalusite with the grain size of less than 200 meshes 10 parts, silicon carbide with the grain size of less than 240 meshes 5.5 parts, sub-white corundum with the grain size of less than 240 meshes 8 parts, alumina CA370C micro powder 4 parts, 0.045mm Suzhou soil 5.6 parts, paper pulp 4.2 parts, phosphoric acid 0.5 part and dextrin 0.4 part; the chemical mass percentage composition of the 3-1mm mullite M47 and the 1-0mm mullite M47 is Al₂O₃50.20%，Fe₂O₃0.86%，SiO₂47.01%，TiO₂0.93%，MgO 0.06%，CaO 0.69%，Na₂0.11% of O and the balance of impurities; the refractoriness is 1770 ℃; the chemical mass percentage composition of 2-1mm cordierite and cordierite with grain diameter less than 150 meshes is Al₂O₃34.39%，Fe₂O₃0.88%，SiO₂48.83%，TiO₂0.95 percent, MgO13.23 percent and the balance of impurities; the refractoriness is 1380 ℃; uniformly mixing, discharging and ageing for 13 hours;

2) molding by a hydraulic press, controlling the porosity of the wet blank to be 19 percent and the volume density of the wet blank to be 2.53 g/cm³；

3) Drying at 50 deg.C in drying hole, making sound before loading, and residual water content of 0.48%;

4) and (4) sintering in a tunnel kiln at 1350 ℃ for 7 h.

Example 4

1) Adding the raw materials into a planetary wet mill according to the proportion and stirring for 20 minutes; the raw materials comprise the following components in parts by weight: 3-1mm mullite M4715 parts, 1-0mm mullite M4710 parts, 2-1mm cordierite 20 parts, cordierite with particle size less than 150 meshes 7 parts, 0.5-0mm sillimanite 13 parts, andalusite with particle size less than 200 meshes 7 parts, silicon carbide with particle size less than 240 meshes 7 parts, sub-white corundum with particle size less than 240 meshes 5 parts, alumina CA370C micro powder 6 parts, 0.045mm Suzhou soil 4 parts, paper pulp 5.5 parts, phosphoric acid 0.3 part and dextrin 0.6 part. The chemical mass percentage composition of the 3-1mm mullite M47 and the 1-0mm mullite M47 is Al₂O₃50.3%，Fe₂O₃0.82%，SiO₂47.05%，TiO₂0.91%，MgO0.07%，CaO0.65%，Na₂0.11% of O and the balance of impurities. The chemical mass percentage composition of 2-1mm cordierite and cordierite with grain diameter less than 150 meshes is Al₂O₃34.56%，Fe₂O₃0.75%，SiO₂49.12%，TiO₂0.75%, MgO13.35% and the balance of impurities. Uniformly mixing, discharging and ageing for 12 hours;

2) molding by a hydraulic press, controlling the porosity of the wet blank to be 18.5 percent and the volume density of the wet blank to be 2.48 g/cm³；

3) Drying at 40 deg.C in drying hole, making sound before loading, and residual water content of 0.45%;

4) sintering at 1340 ℃ for 6 h.

Example 5

1) Adding the raw materials into a planetary wet mill according to the proportion and stirring for 20 minutes; the raw materials comprise the following components in parts by weight: 3-1mm mullite M4710 parts, 1-0mm mullite M4715 parts, 2-1mm cordierite 16 parts, cordierite with the grain size of less than 150 meshes 12 parts, 0.5-0mm sillimanite 8 parts, andalusite with the grain size of less than 200 meshes 13 parts, silicon carbide with the grain size of less than 240 meshes 4 parts, sub-white corundum with the grain size of less than 240 meshes 10 parts, alumina CA370C micro powder 3 parts, 0.045mm Suzhou soil 6 parts, paper pulp 3.5 parts, phosphoric acid 0.6 part and dextrin 0.3 part. 3-The chemical mass percentage composition of the 1mm mullite M47 and the 1-0mm mullite M47 is Al₂O₃50%，Fe₂O₃0.92%，SiO₂46.8%，TiO₂0.94%，MgO0.05%，CaO0.72%，Na₂0.09% of O and the balance of impurities. The chemical mass percentage composition of 2-1mm cordierite and cordierite with grain diameter less than 150 meshes is Al₂O₃34.12%，Fe₂O₃0.94%，SiO₂48.56%，TiO₂1.13%, MgO13.11% and the balance impurities. Uniformly mixing, discharging, and ageing the mixture for 15 hours; (ii) a

2) Molding by a hydraulic press, controlling the porosity of the wet blank to be 20.0 percent and the volume density of the wet blank to be 2.68g/cm³；

3) Drying at 110 deg.C, making sound before loading, and residual water content of 0.52%;

4) and firing is carried out at a temperature of 1360 ℃ for 7 h.

Comparative example 1

The process and the raw material ratio are the same as the example 1, except that the amount of the mullite M473-1mm mullite M47 in the raw material is 26 parts, and the grain diameter is 1-0 mm.

Comparative example 2

The process and the raw material ratio were the same as in example 1, except that 40 parts of cordierite was used as the raw material.

Comparative example 3

The process and the raw material ratio are the same as those of the example 1, except that the usage amount of cordierite in the raw materials is 27 parts, and the grain diameter is less than 150 meshes.

Comparative example 4

The process and the raw material ratio are the same as the example 1, except that the amount of the sillimanite in the raw materials is 4 parts, and the amount of the andalusite in the raw materials is 20 parts.

Comparative example 5

The process and the raw material ratio were the same as example 1, except that no silicon carbide was used in the raw material.

Comparative example 6

The process and the raw material ratio are the same as the example 1, except that the raw materials comprise 0.5 part of paper pulp, 5 parts of phosphoric acid and 0.3 part of dextrin.

Appearance of the finished products of examples 1 to 5: the appearance of the finished product after burning is slightly yellowish. And (3) sounding: the sound is played and the steel is crisp.

The results of the performance tests of the examples and the comparisons are shown in tables 1 to 4.

TABLE 1

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TABLE 2

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TABLE 3

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TABLE 4

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The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.

Claims

1. A cordierite kiln furniture sagger is characterized by comprising the following raw materials in parts by weight: 3-1mm mullite M4713 parts, 1-0mm mullite M4713 parts, 2-1mm cordierite 18 parts, cordierite with the grain size of less than 150 meshes 9.5 parts, 0.5-0mm sillimanite 10 parts, andalusite with the grain size of less than 200 meshes 9.5 parts, silicon carbide with the grain size of less than 240 meshes 6 parts, sub-white corundum with the grain size of less than 240 meshes 7.5 parts, alumina CA370C micro powder 4.5 parts, 0.045mm Suzhou soil 5 parts, paper pulp 4.5 parts, phosphoric acid 0.45 part and dextrin 0.45 part; chemical mass hundreds of 3-1mm mullite M47 and 1-0mm mullite M47The composition of the component is Al₂O₃50.20%，Fe₂O₃0.86%，SiO₂47.01%，TiO₂0.93%，MgO 0.06%，CaO 0.69%，Na₂0.11% of O and the balance of impurities; the fire resistance is 1770 ℃; the chemical mass percentage composition of 2-1mm cordierite and cordierite with grain diameter less than 150 meshes is Al₂O₃34.39%，Fe₂O₃0.88%，SiO₂48.83%，TiO₂0.95 percent, MgO13.23 percent and the balance of impurities; the refractoriness is 1380 ℃;

the preparation method of the cordierite kiln furniture sagger comprises the following steps:

1) adding the raw materials into a planetary wet mill according to the proportion and stirring for 20 minutes; uniformly mixing, discharging and ageing for 13 hours;

2) molding by a hydraulic press, and controlling the porosity of the wet blank to be 19% and the volume density of the wet blank to be 2.56g/cm 3;

4) and (4) firing in a tunnel kiln at 1350 ℃ for 7 h.