CN104446459A - Preparation method of zirconium oxide hollow sphere heat-insulating product for tungsten-molybdenum sintering medium-frequency furnace - Google Patents
Preparation method of zirconium oxide hollow sphere heat-insulating product for tungsten-molybdenum sintering medium-frequency furnace Download PDFInfo
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Abstract
The invention belongs to the technical field of fireproof materials, and particularly relates to a preparation method of a zirconium oxide hollow sphere heat-insulating product for a tungsten-molybdenum sintering medium-frequency furnace. The preparation method comprises the following steps of: taking a zirconium oxide hollow sphere as an aggregate, and adding electric melting zirconium oxide powder and zirconium oxide micropowder prepared through a chemical method; taking a water-soluble epoxy resin solution or a water-soluble alkyd resin solution as a bonding agent, and blending, forming and drying to serve as a liner of the tungsten-molybdenum sintering medium-frequency furnace; firstly using for the tungsten-molybdenum sintering medium-frequency furnace. The preparation method disclosed by the invention can be used for improving the thermal shock resistant property of the product and enhancing the compression strength by utilizing the characteristics of a production process of the tungsten-molybdenum sintering medium-frequency furnace, combining with high bonding strength of water-soluble epoxy resin or water-soluble alkyd resin under hydrogen or inert gas at medium and low temperature and keeping the transformation toughening effect of the zirconium oxide micropowder prepared through the chemical method, thereby prolonging the service life of the liner of the tungsten-molybdenum sintering medium-frequency furnace.
Description
Technical field
The invention belongs to technical field of refractory materials, be specifically related to a kind of preparation method of the 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 large, and use temperature reaches 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 strength is large simultaneously, is convenient to the load-bearing in the production cycle and movement.
Conventional oxidation zirconium hollow ball insulating product take Bubble zirconia as aggregate, the electric-melting zirconia powder of granularity < 0.044 mm is matrix, bonding agent is made with calcium lignosulfonate solution, after batch mixing, shaping and drying, in shuttle kiln, 1700 ~ 1800 DEG C of insulation 6 ~ 10 h burn till obtained, production cycle is long, and energy consumption is high.Limit 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 has about 20 MPa; Bonding agent is made with calcium lignosulfonate solution, and calcium lignin sulphonate when production process in low temperature bond intensity difference, needing heats up at a slow speed in shuttle kiln burns till, calcium oxide brought into by calcium lignin sulphonate simultaneously, cause Bubble zirconia insulating product thermal shock resistance poor, use heat to only have about 5 times, the work-ing life of tungsten sintering intermediate frequency furnace lining can not be met.
Summary of the invention
The object of the invention is to propose one without shuttle kiln firing process, and in the use procedure of tungsten sintering intermediate frequency furnace, 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, feed composition and the weight percent of described Bubble zirconia insulating product are: granularity is the electric-melting zirconia powder 25 ~ 44% of Bubble zirconia 55 ~ 70%, granularity < 0.044 mm of 0.2 ~ 3 mm; The chemical method oxygenerating zirconium micro mist 1 ~ 10% of granularity < 5 μm; Add water-soluble epoxy resin or water soluble alkyd resin solution makes bonding agent, add-on is 4 ~ 8% of above-mentioned raw materials gross weight, and water-soluble epoxy resin or water soluble alkyd resin solid content are 20 ~ 60%; Electric-melting zirconia powder is placed in mixing equipment with chemical method oxygenerating zirconium micro mist and mixes, the powder mix be uniformly mixed; Bubble zirconia and described bonding agent are stirred after soaking, then add powder mix and mix; Adopt pressurization vibration mode to prepare the base substrate of desired size, cool after 24 ~ 36 hours through 100 ~ 110 DEG C of dryings and obtain required work in-process, work in-process are used as tungsten sintering intermediate frequency furnace lining, after tungsten sintering intermediate frequency furnace uses first, obtain described goods; The goods cold crushing strength obtained is greater 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, and be namely rapidly heated and pass into the technological operation feature of protectiveness hydrogen or rare gas element, service temperature is up to more than 2000 DEG C.The high temperature of more than 2000 DEG C gives for the high firing temperature of the Bubble zirconia insulating product of tungsten sintering intermediate frequency furnace, and make these goods fully sintered, cold crushing strength is up to 30 more than MPa.Overcome the defect adopting shuttle kiln firing temperature low, its maximum sintering temperature only has 1800 DEG C, Bubble zirconia goods cold crushing strength obtained 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 adopts water-soluble epoxy resin and water soluble alkyd resin to make bonding agent, give under the tungsten sintering hydrogen of intermediate frequency furnace or rare gas element Bubble zirconia insulating product high in low temperature bond intensity, ensure that burning till of Bubble zirconia insulating product.Overcome the defect that conventional oxidation zirconium hollow ball insulating product adopt calcium lignosulfonate solution to do middle low temperature bond intensity that bonding agent brings is low, this bonding agent is only applicable to shuttle kiln and heats up at a slow speed and burn till, and is not suitable for the technology characteristics that tungsten sintering intermediate frequency furnace is rapidly heated.The present invention adopts water-soluble epoxy resin and water soluble alkyd resin to make bonding agent, such bonding agent does not introduce calcium oxide, maintain the phase transition performance of the chemical method oxygenerating zirconium micro mist that Bubble zirconia goods add, 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 adopts calcium lignosulfonate solution to make bonding agent, calcium oxide is produced after calcium lignin sulphonate pyrolytic decomposition, calcium oxide and chemical method oxygenerating zirconium micro mist react thus stabilize chemical method oxygenerating zirconium micro mist, it is made to lose transformation toughening effect, cause the thermal shock resistance of conventional articles to be deteriorated, use heat only to have about 5 times.
For a preparation method for the Bubble zirconia insulating product of tungsten sintering intermediate frequency furnace, the CaO+ZrO of Bubble zirconia
2+ HfO
2>=99.4%, CaO:3.8 ~ 4.5%.
For a preparation method for the Bubble zirconia insulating product of tungsten sintering intermediate frequency furnace, the CaO+ZrO of electric-melting zirconia powder
2+ HfO
2>=99.4%, CaO:3.8 ~ 4.5%.
For a preparation method for the Bubble zirconia insulating product of tungsten sintering intermediate frequency furnace, the ZrO of chemical method oxygenerating zirconium micro mist
2+ HfO
2>=99.4%.
A kind of preparation method of the Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace, feed composition and weight percent be preferably: granularity is the electric-melting zirconia powder 27 ~ 38% of Bubble zirconia 60 ~ 65%, granularity < 0.044 mm of 0.2 ~ 3 mm; The chemical method oxygenerating zirconium micro mist 2 ~ 8% of granularity < 5 μm; Add water-soluble epoxy resin or water soluble alkyd resin solution makes bonding agent, bonding agent add-on is 4 ~ 6% of above-mentioned raw materials gross weight, and water-soluble epoxy resin or water soluble alkyd resin solid content are 20 ~ 50%.
Embodiment
The present invention carries out optimum matching according to the distribution of the continuous sized particles of heap sum of discontinuous sized particles and accumulation to Bubble zirconia, add electric-melting zirconia powder and chemical method oxygenerating zirconium micro mist, 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 zirconia
2+ HfO
2>=99.4%, CaO:3.8 ~ 4.5%; The CaO+ZrO of electric-melting zirconia powder
2+ HfO
2>=99.4%, CaO:3.8 ~ 4.5%, granularity < 0.044 mm; The ZrO of chemical method oxygenerating zirconium micro mist
2+ HfO
2>=99.4%, granularity < 5 μm; Electric-melting zirconia powder is placed in mixing equipment with chemical method oxygenerating zirconium micro mist and mixes, the powder mix be uniformly mixed; Bubble zirconia and described bonding agent are stirred after soaking, then add powder mix and mix; Adopt pressurization vibration mode to prepare the base substrate of desired size, cool after 24 ~ 36 hours through 100 ~ 110 DEG C of dryings and obtain required work in-process, work in-process are used as tungsten sintering intermediate frequency furnace lining, use first through tungsten sintering intermediate frequency furnace.
Embodiment 1: a kind of preparation method of the Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace.The feed composition of Bubble zirconia insulating product and weight percent are: granularity is the Bubble zirconia 60% of 0.2 ~ 3 mm, electric-melting zirconia powder 38%, chemical method oxygenerating zirconium micro mist 2%; Bonding agent water-soluble epoxy resin solution add-on is above-mentioned raw materials weight 6%, and the solid content of water-soluble epoxy resin solution is 50%.Wherein, described Bubble zirconia particle, by being less than or equal to 3 mm, being greater than 2 mm, is less than or equal to 2 mm, is greater than 1 mm, be less than or equal to 1mm, is greater than 0.2 mm and carries out grating, and account for 25%, 20% of Bubble zirconia insulating product weight respectively, 15%.
The Bubble zirconia insulating product that the present embodiment obtains, cold crushing strength is 35 MPa, and volume density is 2.98 g/cm
3; Heat is used to reach 15 times.
Embodiment 2: a kind of preparation method of the Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace.The feed composition of Bubble zirconia insulating product and weight percent are: granularity is the Bubble zirconia 65% of 0.2 ~ 3 mm, electric-melting zirconia powder 31%, chemical method oxygenerating zirconium micro mist 4%; Bonding agent water soluble alkyd resin solution and water-soluble epoxy resin solution add-on 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 particle, by being less than or equal to 3 mm, being greater than 2 mm, is less than or equal to 2 mm, is greater than 1 mm, be less than or equal to 1mm, is greater than 0.2 mm and carries out grating, and account for 20%, 25% of Bubble zirconia insulating product weight respectively, 20%.
The Bubble zirconia insulating product that the present embodiment obtains, cold crushing strength is 32 MPa, uses heat to reach 17 times.
Embodiment 3: a kind of preparation method of the Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace.The feed composition of Bubble zirconia insulating product and weight percent are: granularity is the Bubble zirconia 65% of 0.2 ~ 3 mm, electric-melting zirconia powder 27%, chemical method oxygenerating zirconium micro mist 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 particle, by being less than or equal to 3 mm, being greater than 2 mm, is less than or equal to 2 mm, is greater than 1 mm, be less than or equal to 1mm, is greater than 0.2 mm and carries out grating, and account for 25%, 15% of Bubble zirconia insulating product weight respectively, 25%.
The Bubble zirconia insulating product that the present embodiment obtains, cold crushing strength is 37 MPa, uses heat to reach 18 times.
Claims (7)
1. the preparation method for the Bubble zirconia insulating product of tungsten sintering intermediate frequency furnace, it is characterized in that: feed composition and the weight percent of described Bubble zirconia insulating product are: granularity is the electric-melting zirconia powder 25 ~ 44% of Bubble zirconia 55 ~ 70%, granularity < 0.044 mm of 0.2 ~ 3 mm; The chemical method oxygenerating zirconium micro mist 1 ~ 10% of granularity < 5 μm; Add water-soluble epoxy resin or water soluble alkyd resin solution makes bonding agent, add-on is 4 ~ 8% of above-mentioned raw materials gross weight, and water-soluble epoxy resin or water soluble alkyd resin solid content are 20 ~ 60%; Electric-melting zirconia powder is placed in mixing equipment with chemical method oxygenerating zirconium micro mist and mixes, the powder mix be uniformly mixed; Bubble zirconia and described bonding agent are stirred after soaking, then add powder mix and mix; Adopt pressurization vibration mode to prepare the base substrate of desired size, cool after 24 ~ 36 hours through 100 ~ 110 DEG C of dryings and obtain required work in-process, work in-process are used as tungsten sintering intermediate frequency furnace lining, after tungsten sintering intermediate frequency furnace uses first, obtain described goods; The goods cold crushing strength obtained is greater than 30 MPa, uses heat to reach more than 15 times.
2. the preparation method of the Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace according to claim 1, is characterized in that: feed composition and weight percent are: 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 micro mist 2 ~ 8% of granularity < 5 μm.
3. the preparation method of the Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace according to claim 1 and 2, it is characterized in that: described bonding agent is the one in water-soluble epoxy resin and water soluble alkyd resin solution, or the wherein combination solution of two kinds.
4. the preparation method of the Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace according to claim 1, is characterized in that: the solid content of bonding agent solution is 20 ~ 50%.
5. the preparation method of the Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace according to claim 1 and 2, is characterized in that: the CaO+ZrO of Bubble zirconia
2+ HfO
2>=99.4%, CaO:3.8 ~ 4.5%.
6. the preparation method of the Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace according to claim 1 and 2, is characterized in that: the CaO+ZrO of electric-melting zirconia powder
2+ HfO
2>=99.4%, CaO:3.8 ~ 4.5%.
7. the preparation method of the Bubble zirconia insulating product for tungsten sintering intermediate frequency furnace according to claim 1 and 2, is characterized in that: the ZrO of chemical method oxygenerating zirconium micro mist
2+ HfO
2>=99.4%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104788108A (en) * | 2015-04-09 | 2015-07-22 | 中钢集团洛阳耐火材料研究院有限公司 | Zirconia fiber board and preparation method |
| CN107827456A (en) * | 2017-12-10 | 2018-03-23 | 湖南仁海科技材料发展有限公司 | A kind of preparation method of Bubble zirconia insulating 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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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104788108A (en) * | 2015-04-09 | 2015-07-22 | 中钢集团洛阳耐火材料研究院有限公司 | Zirconia fiber board and preparation method |
| CN107827456A (en) * | 2017-12-10 | 2018-03-23 | 湖南仁海科技材料发展有限公司 | A kind of preparation method of Bubble zirconia insulating product |
| CN107827456B (en) * | 2017-12-10 | 2021-03-12 | 湖南仁海科技材料发展有限公司 | A kind of preparation method of zirconia hollow ball 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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