CN104446459B - Preparation method for the Bubble zirconia insulating product of tungsten sintering intermediate frequency furnace - Google Patents
Preparation method for the Bubble zirconia insulating product of tungsten sintering intermediate frequency furnace Download PDFInfo
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Abstract
The invention belongs to technical field of refractory materials, it is specifically related to the preparation method of a kind of Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace, with Bubble zirconia as aggregate, add electric-melting zirconia powder and chemical method oxygenerating zirconium micropowder, bonding agent is made with water-soluble epoxy resin or water soluble alkyd resin solution, through material mixing, molding with dried, sinter intermediate frequency furnace lining as tungsten, use first through tungsten sintering intermediate frequency furnace.Present invention utilizes the production technology characteristic of tungsten sintering intermediate frequency furnace, high in conjunction with water-soluble epoxy resin or water soluble alkyd resin middle low temperature bond intensity under hydrogen or noble gas, maintain the transformation toughening effect of chemical method oxygenerating zirconium micropowder, improve the thermal shock resistance of goods, improve compressive resistance high, thus extend the service life of tungsten sintering intermediate frequency furnace lining.
Description
Technical field
The invention belongs to technical field of refractory materials, be specifically related to the preparation method of a kind of Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace.
Background technology
Bubble zirconia insulating product is typically used as tungsten sintering intermediate frequency furnace lining.Tungsten sintering intermediate frequency furnace is as a kind of intermittent type gas protecting stove, and furnace type structure is complicated, and liner brick is big, uses temperature to reach more than 2000 DEG C, and tungsten sintering process is with short production cycle, and heating and cooling are frequent.Require that Bubble zirconia insulating product thermal shock resistance is good, be able to take high temperature fluctuation；Compressive resistance is big simultaneously, it is simple to the load-bearing in the production cycle and movement.
Conventional oxidation zirconium hollow ball insulating product is with Bubble zirconia as aggregate, the electric-melting zirconia powder of granularity ＜ 0.044 mm is substrate, bonding agent is made with calcium lignosulfonate solution, through material mixing, molding and dried in shuttle kiln 1700～1800 DEG C of insulation 6～10 h burn till prepared, production cycle is long, and energy resource consumption is high.Being limited by shuttle kiln, shuttle kiln maximum sintering temperature only has 1800 DEG C, and the cold crushing strength that the firing temperature of 1800 DEG C causes Bubble zirconia insulating product is low, only about 20 MPa；Bonding agent is made with calcium lignosulfonate solution, and the middle low temperature bond intensity difference that calcium lignosulfonate is when production process, needing heats up at a slow speed in shuttle kiln burns till, calcium oxide brought into by calcium lignosulfonate simultaneously, cause Bubble zirconia insulating product thermal shock resistance poor, heat is used to only have about 5 times, it is impossible to meet the service life of tungsten sintering intermediate frequency furnace lining.
Summary of the invention
The purpose of the present invention is to propose to a kind of without shuttle kiln firing process, and during tungsten sintering intermediate frequency furnace uses, produce sintering, for the preparation method of the Bubble zirconia insulating product of tungsten sintering intermediate frequency furnace.It is high that Bubble zirconia insulating product prepared by this preparation method has cold crushing strength, uses the feature that heat is many.
To achieve these goals, the technical solution used in the present invention is as follows:
A kind of preparation method of the Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace, raw material components and the percentage by weight of described Bubble zirconia insulating product be: granularity is the Bubble zirconia 55～70% of 0.2～3 mm, the electric-melting zirconia powder 25～44% of granularity ＜ 0.044 mm；The chemical method oxygenerating zirconium micropowder 1～10% of granularity ＜ 5 μm；Add water-soluble epoxy resin or water soluble alkyd resin solution and make bonding agent, addition be the 4～8% of above-mentioned raw materials gross weight, water-soluble epoxy resin or water soluble alkyd resin solid content be 20～60%；Electric-melting zirconia powder is placed in mixing equipment with chemical method oxygenerating zirconium micropowder and mixes, the mixed powder being uniformly mixed；After Bubble zirconia and described bonding agent are stirred moistening, add mixed powder mix homogeneously；Using pressurization vibration mode to prepare the base substrate of required size, after 100～110 DEG C are dried 24～36 hours, cooling obtains required semi-finished product, semi-finished product is used as tungsten and sinters intermediate frequency furnace lining, after tungsten sintering intermediate frequency furnace uses first, obtains described goods；The goods cold crushing strength obtained, more than 30 MPa, uses heat to reach more than 15 times.
The present invention makes full use of the production technology characteristic of tungsten sintering intermediate frequency furnace, is i.e. rapidly heated and is passed through the technological operation feature of protectiveness hydrogen or noble gas, and operation temperature is up to more than 2000 DEG C.The high temperature of more than 2000 DEG C gives the high firing temperature of Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace, makes these goods fully sintered, and cold crushing strength is up to 30 more than MPa.Overcome the defect using shuttle kiln firing temperature low, its maximum sintering temperature only has 1800 DEG C, Bubble zirconia goods cold crushing strength acquired at such a temperature only has 20 MPa, the load-bearing in the production cycle and movement can not be met, decrease the firing process in conventional oxidation zirconium hollow ball insulating product simultaneously, save the energy.The present invention uses water-soluble epoxy resin and water soluble alkyd resin to make bonding agent, gives, under the hydrogen or noble gas of tungsten sintering intermediate frequency furnace, the middle low temperature bond intensity that Bubble zirconia insulating product is high, it is ensured that burning till of Bubble zirconia insulating product.Overcome the defect that conventional oxidation zirconium hollow ball insulating product use calcium lignosulfonate solution to do middle low temperature bond intensity that bonding agent brought is low, this bonding agent is only applicable to shuttle kiln and heats up at a slow speed and burn till, and is not appropriate for the technology characteristics that tungsten sintering intermediate frequency furnace is rapidly heated.The present invention uses water-soluble epoxy resin and water soluble alkyd resin to make bonding agent, such bonding agent does not introduce calcium oxide, the phase transition performance of the chemical method oxygenerating zirconium micropowder that maintenance Bubble zirconia goods are added, this phase transition performance produces toughening effect to Bubble zirconia goods, effectively improve the thermal shock resistance of goods, use heat to reach more than 15 times；And conventional oxidation zirconium hollow ball insulating product uses calcium lignosulfonate solution to make bonding agent, calcium oxide is produced after calcium lignosulfonate pyrolytic, calcium oxide reacts with chemical method oxygenerating zirconium micropowder thus stabilizes chemical method oxygenerating zirconium micropowder, it is made to lose transformation toughening effect, the thermal shock resistance causing conventional articles is deteriorated, and uses heat to only have about 5 times.
A kind of preparation method of the Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace, the CaO+ZrO of Bubble zirconia2+HfO2>=99.4%, CaO:3.8～4.5%.
A kind of preparation method of the Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace, the CaO+ZrO of electric-melting zirconia powder2+HfO2>=99.4%, CaO:3.8～4.5%.
A kind of preparation method of the Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace, the ZrO of chemical method oxygenerating zirconium micropowder2+HfO2≥99.4%。
A kind of preparation method of the Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace, raw material components and percentage by weight be preferably: granularity is the Bubble zirconia 60～65% of 0.2～3 mm, the electric-melting zirconia powder 27～38% of granularity ＜ 0.044 mm；The chemical method oxygenerating zirconium micropowder 2～8% of granularity ＜ 5 μm；Add water-soluble epoxy resin or water soluble alkyd resin solution and make bonding agent, bonding agent addition be the 4～6% of above-mentioned raw materials gross weight, water-soluble epoxy resin or water soluble alkyd resin solid content be 20～50%.
Detailed description of the invention
Bubble zirconia is most preferably mated with piling up by the present invention according to the distribution with continuous sized particles of piling up of discontinuous sized particles, add electric-melting zirconia powder and chemical method oxygenerating zirconium micropowder, make bonding agent with water-soluble epoxy resin or water soluble alkyd resin solution, produce a kind of Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace.In the following embodiments, the CaO+ZrO of Bubble zirconia2+HfO2>=99.4%, CaO:3.8～4.5%；The CaO+ZrO of electric-melting zirconia powder2+HfO2>=99.4%, CaO:3.8～4.5%, granularity ＜ 0.044 mm；The ZrO of chemical method oxygenerating zirconium micropowder2+HfO2>=99.4%, granularity ＜ 5 μm；Electric-melting zirconia powder is placed in mixing equipment with chemical method oxygenerating zirconium micropowder and mixes, the mixed powder being uniformly mixed；After Bubble zirconia and described bonding agent are stirred moistening, add mixed powder mix homogeneously；Using pressurization vibration mode to prepare the base substrate of required size, after 100～110 DEG C are dried 24～36 hours, cooling obtains required semi-finished product, semi-finished product is used as tungsten and sinters intermediate frequency furnace lining, uses first through tungsten sintering intermediate frequency furnace.
Embodiment 1: the preparation method of a kind of Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace.The raw material components of Bubble zirconia insulating product and percentage by weight be: granularity is the Bubble zirconia 60% of 0.2～3 mm, electric-melting zirconia powder 38%, chemical method oxygenerating zirconium micropowder 2%；Bonding agent water-soluble epoxy resin solution addition is above-mentioned raw materials weight 6%, and the solid content of water-soluble epoxy resin solution is 50%.Wherein, described Bubble zirconia granule, by less than or equal to 3 mm, more than 2 mm, less than or equal to 2 mm, more than 1 mm, less than or equal to 1mm, carries out grating, and accounts for the 25% of Bubble zirconia insulating product weight respectively more than 0.2 mm, and 20%, 15%.
The Bubble zirconia insulating product that the present embodiment is obtained, cold crushing strength is 35 MPa, and bulk density is 2.98 g/cm3；Heat is used to reach 15 times.
Embodiment 2: the preparation method of a kind of Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace.The raw material components of Bubble zirconia insulating product and percentage by weight be: granularity is the Bubble zirconia 65% of 0.2～3 mm, electric-melting zirconia powder 31%, chemical method oxygenerating zirconium micropowder 4%；Bonding agent water soluble alkyd resin solution and water-soluble epoxy resin solution addition are respectively above-mentioned raw materials gross weight 3%, and the solid content of water-soluble epoxy resin solution is 25%, and the solid content of water soluble alkyd resin solution is 25%.Wherein, described Bubble zirconia granule, by less than or equal to 3 mm, more than 2 mm, less than or equal to 2 mm, more than 1 mm, less than or equal to 1mm, carries out grating, and accounts for the 20% of Bubble zirconia insulating product weight respectively more than 0.2 mm, and 25%, 20%.
The Bubble zirconia insulating product that the present embodiment is obtained, cold crushing strength is 32 MPa, uses heat to reach 17 times.
Embodiment 3: the preparation method of a kind of Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace.The raw material components of Bubble zirconia insulating product and percentage by weight be: granularity is the Bubble zirconia 65% of 0.2～3 mm, electric-melting zirconia powder 27%, chemical method oxygenerating zirconium micropowder 8%；Bonding agent water soluble alkyd resin solution is above-mentioned raw materials gross weight 4%, and the solid content of water soluble alkyd resin solution is 20%.Wherein, described Bubble zirconia granule, by less than or equal to 3 mm, more than 2 mm, less than or equal to 2 mm, more than 1 mm, less than or equal to 1mm, carries out grating, and accounts for the 25% of Bubble zirconia insulating product weight respectively more than 0.2 mm, and 15%, 25%.
The Bubble zirconia insulating product that the present embodiment is obtained, cold crushing strength is 37 MPa, uses heat to reach 18 times.
Claims (5)
1. the preparation method for the Bubble zirconia insulating product of tungsten sintering intermediate frequency furnace, raw material components and the percentage by weight of described Bubble zirconia insulating product be: granularity is the Bubble zirconia 55～70% of 0.2～3 mm, the electric-melting zirconia powder 25～44% of granularity ＜ 0.044 mm；The chemical method oxygenerating zirconium micropowder 1～10% of granularity ＜ 5 μm；It is characterized in that: the CaO+ZrO of Bubble zirconia2+HfO2>=99.4%, CaO:3.8～4.5%；Described Bubble zirconia insulating product is additionally added water-soluble epoxy resin or water soluble alkyd resin solution makees bonding agent, addition be the 4～8% of above-mentioned raw materials gross weight, water-soluble epoxy resin or water soluble alkyd resin solid content be 20～60%；Electric-melting zirconia powder is placed in mixing equipment with chemical method oxygenerating zirconium micropowder and mixes, the mixed powder being uniformly mixed；After Bubble zirconia and described bonding agent are stirred moistening, add mixed powder mix homogeneously；Using pressurization vibration mode to prepare the base substrate of required size, after 100～110 DEG C are dried 24～36 hours, cooling obtains required semi-finished product, semi-finished product is used as tungsten and sinters intermediate frequency furnace lining, after tungsten sintering intermediate frequency furnace uses first, obtains described goods；The goods cold crushing strength obtained, more than 30 MPa, uses heat to reach more than 15 times.
The preparation method of Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace the most according to claim 1, it is characterised in that: raw material components and percentage by weight be: granularity is the Bubble zirconia 60～65% of 0.2～3 mm；The electric-melting zirconia powder 27～38% of granularity ＜ 0.044 mm；The chemical method oxygenerating zirconium micropowder 2～8% of granularity ＜ 5 μm.
The preparation method of the Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace the most according to claim 1, it is characterised in that: the solid content of bonding agent solution is 20～50%.
The preparation method of the Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace the most according to claim 1 and 2, it is characterised in that: the CaO+ZrO of electric-melting zirconia powder2+HfO2>=99.4%, CaO:3.8～4.5%.
The preparation method of the Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace the most according to claim 1 and 2, it is characterised in that: the ZrO of chemical method oxygenerating zirconium micropowder2+HfO2≥99.4%。
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| CN104788108B (en) * | 2015-04-09 | 2016-09-14 | 中钢集团洛阳耐火材料研究院有限公司 | A kind of zirconium oxide fiber board and preparation method |
| CN107827456B (en) * | 2017-12-10 | 2021-03-12 | 湖南仁海科技材料发展有限公司 | Preparation method of zirconia hollow sphere heat insulation product |
| CN109535984A (en) * | 2018-12-27 | 2019-03-29 | 中钢集团洛阳耐火材料研究院有限公司 | A kind of superhigh temperature infra-red radiation heat preservation energy-saving coating |
| CN110937896A (en) * | 2019-12-11 | 2020-03-31 | 郑州利晟保温材料有限公司 | Preparation method of zirconia light brick |
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