CN100396631C - Method for producing mullite crystal refractory fiber blanket and its product - Google Patents
Method for producing mullite crystal refractory fiber blanket and its product Download PDFInfo
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- CN100396631C CN100396631C CNB2005100127234A CN200510012723A CN100396631C CN 100396631 C CN100396631 C CN 100396631C CN B2005100127234 A CNB2005100127234 A CN B2005100127234A CN 200510012723 A CN200510012723 A CN 200510012723A CN 100396631 C CN100396631 C CN 100396631C
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Abstract
The present invention relates to a method for producing a mullite crystal refractory fiber blanket and a product thereof. The method comprises the following procedures: producing colloid; producing fiber base substrate-collecting cotton; needling; processing through light burning; processing at high temperature-cutting forming; producing a finished product; or producing the colloid; producing the fiber base substrate-collecting cotton; processing through light burning; needling; processing at high temperature-cutting forming; producing the finished product. Chemical composition is composed of 70 to 72% of Al2O3 and 27 to 29% of SiO2. Overmeasure is permissible impurity, and a fibre crystal phase and a main crystal phase are mullite, the content of which is more than or equal to 60%. The thermal conductivity coefficient is from 0.15 to 0.20 W/m. k at the tapetum fibrosum hot face temperature of 1000 DEG C, and the heater wire change (1400 DEG C *24h) is less than-1%. Compared with the present aluminum silicate fiber blanket, the use temperature of the mullite crystal refractory fiber blanket is enhanced by 150 to 400 DEG C, the use range of the refractory fibrous material is enlarged.
Description
Technical field
The invention belongs to the fire-resistant heat insulating material category, be specifically related to a kind of method for making of mullite crystal refractory fiber blanket and the product that makes thereof.
Background technology
The mullite flame-proof fiber is as the new type high temperature lagging material, has high temperature resistant, anticorrosive, premium properties such as thermal conductivity is low, thermostability and good thermal shock, on the hot industry kiln and high temperature service of industrial sectors such as metallurgy, machinery, oil, chemical industry, electronics, pottery, do furnace lining material and lagging material and use, obtained energy-conservation 5%～40% unusual effect; Reach at aspects such as aerospace guided missile and nuclear power and use in composite reinforcing material, support of the catalyst, all received good effect.Therefore be subjected to people's generally attention, some industrially developed country drop into strength unexpectedly mutually, the exploitation multicrystal mullite refractory fabrics.
But because such fibre technology complexity, production difficulty are big, and thin, short, problems such as fragility is big, easy fracture that fiber exists, domestic this series products can only adopt converted top bundle, wet method goods, hydrostatic profile goods in the use of Industrial Stoves at present, and other finely processed products still belong to blank.This has influenced this series products and has used widening of field, and development and exploitation mullite fiber blanket are very necessary.
Summary of the invention
Purpose of the present invention, be to adopt hydrochloric acid soln, aluminium powder, silicon sol, additive preparation to become colloid, and make the fiber base substrate by getting rid of a technology, the fiber base substrate is through after collecting cotton and drying, light-burned processing through certain temperature, pass through acupuncture again, finally pass through the thermal treatment of certain temperature, again a kind of mullite fiber blanket by being cut into.
The present invention reaches its goal of the invention by following technical solution:
Develop a kind of method for making of mullite crystal refractory fiber blanket, it is characterized in that method for making is divided into glue body, system fiber base substrate---collection is cotton, system needle punched blanket, light-burned processing, pyroprocessing---excision forming step, make finished product, division is as follows:
(1) glue body
1. by weight ratio, concentration 8～15% hydrochloric acid solns: aluminium powder=88～90: 10～12,40～80 ℃ reinforced, and 80～100 ℃ were reacted 1～2 hour, and made first liquid;
2. by weight ratio, first liquid: additive: silicic acid sol=10: 1: 3,50～70 ℃ of reactions 1～4 hour, viscosity 1000～4000mp.s when making 50 ℃, solid content is at 30～40% colloid, and is standby;
Described additive is by weight ratio, soft water: polyvinyl alcohol: lactic acid=10: 1: 10 reacts and made in 1～2 hour at 70～90 ℃;
(2) system fiber base substrate---collection is cotton
The above-mentioned colloid of making, by getting rid of a technology, the rotating speed of control wire swaying roller is at 1000～3000 rev/mins, and forming length is the fiber base substrate of 300～500mm;
The above-mentioned fiber base substrate of making is accumulated as certain thickness by 50～140 ℃ temperature drying and through collecting cotton;
(3) system needle punched blanket
Carry out acupuncture by needle loom, carried out drying 0.5～1.5 hour through 100～350 ℃ temperature again, form needle punched blanket;
(4) light-burned processing
The above-mentioned needle punched blanket of making, through 500～800 ℃, light-burned processing 2～2.5 hours;
(5) pyroprocessing---excision forming
After the light-burned processing, under 1100～1350 ℃, handled 1～4 hour again, at last by being cut into the mullite fiber needle punched blanket of desired size.
The method for making of above-mentioned mullite crystal refractory fiber blanket is characterized in that recipe step is as follows:
(1) glue body
1. by weight ratio, concentration 8～15% hydrochloric acid solns: aluminium powder=88～90: 10～12,40～80 ℃ reinforced in batches, and 80～100 ℃ were reacted 1～2 hour, and made first liquid;
2. by weight ratio, first liquid: additive: silicic acid sol=10: 1: 3,50～70 ℃ of reactions 1～4 hour, viscosity 1000～4000mp.s when making 50 ℃, solid content is at 30～40% colloid, and is standby;
Described additive is by weight ratio, soft water: polyvinyl alcohol: lactic acid=10: 1: 10 reacts and made in 1～2 hour at 70～90 ℃;
(2) system fiber base substrate---collection is cotton
The above-mentioned colloid of making, by getting rid of a technology, the rotating speed of control wire swaying roller is at 1000～3000 rev/mins, and forming length is the fiber base substrate of 300～500mm; The above-mentioned fiber base substrate of making carried out drying 0.5～1.5 hour through 100～350 ℃ temperature again by 50～140 ℃ temperature drying and after collecting cotton, being accumulated as certain thickness;
(3) light-burned processing
The above-mentioned fiber base substrate of making, through 500～800 ℃, light-burned processing 2～2.5 hours;
(4) system needle punched blanket
Carry out acupuncture by needle loom, form needle punched blanket;
(5) pyroprocessing---excision forming
After acupuncture is finished, under 1100～1350 ℃, handled 1～4 hour again, at last by being cut into the mullite fiber needle punched blanket of desired size.
The mullite crystal refractory fiber blanket that above-mentioned method for making makes is characterized in that:
(1) its physicals is:
Fibre diameter: 2～6 μ m
φ 〉=0.25mm slag ball content :≤10%
Use temperature: 1500 ℃
Tensile strength: 〉=0.02MPa
The heater wire variation (1400 ℃ * 24h) :≤-1%
Thermal conductivity 0.15～0.20W/mk under 1000 ℃ of the hot-face temperatures
(2) its chemical constitution is: Al
2O
370～72%; SiO
227～29%, surplus is admissible impurity;
(3) its fiber crystalline phase, principal crystalline phase: mullite mullite content 〉=60%.
The method for making of above-mentioned mullite crystal refractory fiber blanket is characterized in that described concentration of hydrochloric acid solution is 9～10%.
This product adopts the X diffractometer to detect, and oikocryst resembles and is mullite, its content 〉=60%.Al in the fiber
2O
3Content is 70～72%, SiO
2Content is 27～30%.Thermal conductivity under 1000 ℃ of this tapetum fibrosum hot-face temperatures is 0.15～0.20W/m.k, heater wire change (1400 ℃ * 24h)＜-1%.
Advantage of the present invention: compare with existing aluminum silicate fiber needle punched blanket, advantage of the present invention is to use the temperature height, improves 150～400 ℃ than present alumina silicate fibre blanket use temperature, thereby has enlarged the use range of refractory fibrous material.
Embodiment
Embodiment one:
With concentration is that 8% hydrochloric acid soln and 90: 12 by weight proportion ratio of aluminium powder evenly join in the reaction ax in batch, and is heated to 60～80 ℃, treat hydrochloric acid soln and aluminium powder add finish after, insulation is 2 hours under 80～100 ℃ temperature, makes first liquid.
Adopt this first liquid 100Kg, add additive 10Kg then, add acidic silicasol 30Kg again, be warming up to 70 ℃ and concentrate, concentrate after 1 hour, make the colloid of viscosity 1000mp.s (50 ℃ time),
Additive is by weight ratio, soft water: polyvinyl alcohol: lactic acid=10: 1: 10 reacts and made in 2 hours at 70～80 ℃;
Adopting the solid content in the colloid that above-mentioned technology makes is 30%, is added to colloid in the wire swaying roller then and adjusts wire swaying roller rotating speed to 1000 rev/min to form length be the fiber base substrate of 300-400mm.This fiber base substrate by 50～100 ℃ temperature drying after and be accumulated as certain thickness after, carry out acupuncture by needle loom, and then carry out drying after 1.5 hours through 100～250 ℃ temperature, through 500～600 ℃ light-burned processing 2.5 hours, again through handling under 1100～1350 ℃ the temperature 1～2 hour, at last by being cut into the mullite fiber needle punched blanket of certain size.
This product adopts the X diffractometer to detect, and oikocryst resembles and is mullite, its content 78.5%.Al in the fiber
2O
3Content is 71%, SiO
2Content is 28.5%, and surplus is admissible impurity.Thermal conductivity under 1000 ℃ of this mullite fiber blanket hot-face temperatures is 0.18W/m.k, heater wire change (1400 ℃ * 24h) be-0.9%.
Embodiment two:
With concentration is that 15% hydrochloric acid soln and 88: 10 by weight proportion ratio of aluminium powder evenly join in the reaction ax in batch, and is heated to 40～60 ℃, treat hydrochloric acid soln and aluminium powder add finish after, insulation is 1 hour under 80～100 ℃ temperature, makes first liquid.
Adopt this first liquid 100Kg, add additive 10Kg then, add acidic silicasol 30Kg again, be warming up to 50 ℃ and concentrate, concentrate after 4 hours, make the colloid of viscosity 4000mp.s (50 ℃ time),
Additive is by weight ratio, soft water: polyvinyl alcohol: lactic acid=10: 1: 10 reacts and made in 1 hour at 80～90 ℃;
Adopting the solid content in the colloid that above-mentioned technology makes is 40%, is added to colloid in the wire swaying roller then and adjusts wire swaying roller rotating speed to 3000 rev/min to form length be the fiber base substrate of 400-500mm.This fiber base substrate by 100～140 ℃ temperature drying after and be accumulated as certain thickness after, carry out acupuncture by needle loom, and then carry out drying after 0.5 hour through 250～350 ℃ temperature, through 600～800 ℃ light-burned processing 2 hours, again through handling under 1100～1350 ℃ the temperature 3～4 hours, at last by being cut into the mullite fiber needle punched blanket of certain size.
This product adopts the X diffractometer to detect, and oikocryst resembles and is mullite, its content 78.5%.Al in the fiber
2O
3Content is 72%, SiO
2Content is 27.5%, and surplus is admissible impurity.Thermal conductivity under 1000 ℃ of this mullite fiber blanket hot-face temperatures is 0.15W/m.k, heater wire change (1400 ℃ * 24h) be-0.8%.
Embodiment three:
With concentration is that 8% hydrochloric acid soln and 90: 12 by weight proportion ratio of aluminium powder evenly join in the reaction ax in batch, and is heated to 60～80 ℃, treat hydrochloric acid soln and aluminium powder add finish after, insulation is 2 hours under 80～100 ℃ temperature, makes first liquid.
Adopt this first liquid 100Kg, add additive 10Kg then, add acidic silicasol 30Kg again, be warming up to 70 ℃ and concentrate, concentrate after 1 hour, make the colloid of viscosity 1000mp.s (50 ℃ time),
Additive is by weight ratio, soft water: polyvinyl alcohol: lactic acid=10: 1: 10 reacts and made in 2 hours at 70～80 ℃;
Adopting the solid content in the colloid that above-mentioned technology makes is 30%, is added to colloid in the wire swaying roller then and adjusts wire swaying roller rotating speed to 1000 rev/min to form length be the fiber base substrate of 300-400mm.This fiber base substrate by 50～100 ℃ temperature drying after and be accumulated as certain thickness after, and then carried out drying 1.5 hours through 100～250 ℃ temperature; Through 500～600 ℃ light-burned processing 2.5 hours; Carry out acupuncture by needle loom and form needle punched blanket; Again through handling under 1100～1350 ℃ the temperature 1～2 hour, at last by being cut into the mullite fiber needle punched blanket of certain size.
This product adopts the X diffractometer to detect, and oikocryst resembles and is mullite, its content 78.5%.Al in the fiber
2O
3Content is 71%, SiO
2Content is 28.5%, and surplus is admissible impurity.Thermal conductivity under 1000 ℃ of this mullite fiber blanket hot-face temperatures is 0.18W/m.k, heater wire change (1400 ℃ * 24h) be-0.9%.
Embodiment four:
With concentration is that 15% hydrochloric acid soln and 88: 10 by weight proportion ratio of aluminium powder evenly join in the reaction ax in batch, and is heated to 40～60 ℃, treat hydrochloric acid soln and aluminium powder add finish after, insulation is 1 hour under 80～100 ℃ temperature, makes first liquid.
Adopt this first liquid 100Kg, add additive 10Kg then, add acidic silicasol 30Kg again, be warming up to 50 ℃ and concentrate, concentrate after 4 hours, make the colloid of viscosity 4000mp.s (50 ℃ time),
Additive is by weight ratio, soft water: polyvinyl alcohol: lactic acid=10: 1: 10 reacts and made in 1 hour at 80～90 ℃;
Adopting the solid content in the colloid that above-mentioned technology makes is 40%, is added to colloid in the wire swaying roller then and adjusts wire swaying roller rotating speed to 3000 rev/min to form length be the fiber base substrate of 400-500mm.This fiber base substrate by 50～100 ℃ temperature drying after and be accumulated as certain thickness after, and then carried out drying 0.5 hour through 200～350 ℃ temperature; Through 600～800 ℃ light-burned processing 2 hours; Carry out acupuncture by needle loom and form needle punched blanket; Again through handling under 1100～1350 ℃ the temperature 2～4 hours, at last by being cut into the mullite fiber needle punched blanket of certain size.
This product adopts the X diffractometer to detect, and oikocryst resembles and is mullite, its content 78.5%.Al in the fiber
2O
3Content is 71.2%, SiO
2Content is 28.3%, and surplus is admissible impurity.Thermal conductivity under 1000 ℃ of this mullite fiber blanket hot-face temperatures is 0.15W/m.k, heater wire change (1400 ℃ * 24h) be-0.9%.
Embodiment five
With concentration is that 9% hydrochloric acid soln and 90: 12 by weight proportion ratio of aluminium powder evenly join in the reaction ax in batch, and is heated to 60～80 ℃, treat hydrochloric acid soln and aluminium powder add finish after, insulation is 2 hours under 80～100 ℃ temperature, makes first liquid.
Adopt this first liquid 100Kg, add additive 10Kg then, add acidic silicasol 30Kg again, be warming up to 70 ℃ and concentrate, concentrate after 1 hour, make the colloid of viscosity 1000mp.s (50 ℃ time),
Additive is by weight ratio, soft water: polyvinyl alcohol: lactic acid=10: 1: 10 reacts and made in 2 hours at 70～80 ℃;
Adopting the solid content in the colloid that above-mentioned technology makes is 30%, is added to colloid in the wire swaying roller then and adjusts wire swaying roller rotating speed to 1000 rev/min to form length be the fiber base substrate of 300-400mm.This fiber base substrate by 50～100 ℃ temperature drying after and be accumulated as certain thickness after, carry out acupuncture by needle loom, and then carry out drying after 1.5 hours through 100～250 ℃ temperature, through 500～600 ℃ light-burned processing 2.5 hours, again through handling under 1100～1350 ℃ the temperature 1～2 hour, at last by being cut into the mullite fiber needle punched blanket of certain size.
This product adopts the X diffractometer to detect, and oikocryst resembles and is mullite, its content 78.5%.Al in the fiber
2O
3Content is 71%, SiO
2Content is 28.5%, and surplus is admissible impurity.Thermal conductivity under 1000 ℃ of this mullite fiber blanket hot-face temperatures is 0.18W/m.k, heater wire change (1400 ℃ * 24h) be-0.9%.
Embodiment six
With concentration is that 10% hydrochloric acid soln and 88: 10 by weight proportion ratio of aluminium powder evenly join in the reaction ax in batch, and is heated to 40～60 ℃, treat hydrochloric acid soln and aluminium powder add finish after, insulation is 1 hour under 80～100 ℃ temperature, makes first liquid.
Adopt this first liquid 100Kg, add additive 10Kg then, add acidic silicasol 30Kg again, be warming up to 50 ℃ and concentrate, concentrate after 4 hours, make the colloid of viscosity 4000mp.s (50 ℃ time),
Additive is by weight ratio, soft water: polyvinyl alcohol: lactic acid=10: 1: 10 reacts and made in 1 hour at 80～90 ℃;
Adopting the solid content in the colloid that above-mentioned technology makes is 40%, is added to colloid in the wire swaying roller then and adjusts wire swaying roller rotating speed to 3000 rev/min to form length be the fiber base substrate of 400-500mm.This fiber base substrate by 50～100 ℃ temperature drying after and be accumulated as certain thickness after, and then carried out drying 0.5 hour through 200～350 ℃ temperature; Through 600～800 ℃ light-burned processing 2 hours; Carry out acupuncture by needle loom and form needle punched blanket; Again through handling under 1100～1350 ℃ the temperature 2～4 hours, at last by being cut into the mullite fiber needle punched blanket of certain size.
This product adopts the X diffractometer to detect, and oikocryst resembles and is mullite, its content 78.5%.Al in the fiber
2O
3Content is 70.5%, SiO
2Content is 29%, and surplus is admissible impurity.Thermal conductivity under 1000 ℃ of this mullite fiber blanket hot-face temperatures is 0.15W/m.k, heater wire change (1400 ℃ * 24h) be-0.8%.
Claims (4)
1. excision forming step that the method for making of a mullite crystal refractory fiber blanket is characterized in that method for making is divided into glue body, system fiber base substrate---collection is cotton, system needle punched blanket, light-burned processing, pyroprocessing---makes finished product, and division is as follows:
(1) glue body
1. by weight ratio, concentration 8～15% hydrochloric acid solns: aluminium powder=88～90: 10～12,40～80 ℃ reinforced, and 80～100 ℃ were reacted 1～2 hour, and made first liquid;
2. by weight ratio, first liquid: additive: silicic acid sol=10: 1: 3,50～70 ℃ of reactions 1～4 hour, viscosity 1000～4000mp.s when making 50 ℃, solid content is at 30～40% colloid, and is standby;
Described additive is by weight ratio, soft water: polyvinyl alcohol: lactic acid=10: 1: 10 reacts and made in 1～2 hour at 70～90 ℃;
(2) system fiber base substrate---collection is cotton
The above-mentioned colloid of making, by getting rid of a technology, the rotating speed of control wire swaying roller is at 1000～3000 rev/mins, and forming length is the fiber base substrate of 300～500mm;
The above-mentioned fiber base substrate of making is accumulated as certain thickness by 50～140 ℃ temperature drying and through collecting cotton;
(3) system needle punched blanket
Carry out acupuncture by needle loom, carried out drying 0.5～1.5 hour through 100～350 ℃ temperature again, form needle punched blanket;
(4) light-burned processing
The above-mentioned needle punched blanket of making, through 500～800 ℃, light-burned processing 2～2.5 hours;
(5) pyroprocessing---excision forming
After the light-burned processing, under 1100～1350 ℃, handled 1～4 hour again, at last by being cut into the mullite crystal refractory fiber blanket finished product of desired size.
2. method for making according to the described mullite crystal refractory fiber blanket of claim 1 is characterized in that recipe step is as follows:
(1) glue body
1. by weight ratio, concentration 8～15% hydrochloric acid solns: aluminium powder=88～90: 10～12,40～80 ℃ reinforced in batches, and 80～100 ℃ were reacted 1～2 hour, and made first liquid;
2. by weight ratio, first liquid: additive: silicic acid sol=10: 1: 3,50～70 ℃ of reactions 1～4 hour, viscosity 1000～4000mp.s when making 50 ℃, solid content is at 30～40% colloid, and is standby;
Described additive is by weight ratio, soft water: polyvinyl alcohol: lactic acid=10: 1: 10
At 70～90 ℃, react and made in 1～2 hour;
(2) system fiber base substrate---collection is cotton
The above-mentioned colloid of making, by getting rid of a technology, the rotating speed of control wire swaying roller is at 1000～3000 rev/mins, and forming length is the fiber base substrate of 300～500mm; The above-mentioned fiber base substrate of making carried out drying 0.5～1.5 hour through 100～350 ℃ temperature again by 50～140 ℃ temperature drying and after collecting cotton, being accumulated as certain thickness;
(3) light-burned processing
The above-mentioned fiber base substrate of making, through 500～800 ℃, light-burned processing 2～2.5 hours;
(4) system needle punched blanket
Carry out acupuncture by needle loom, form needle punched blanket;
(5) pyroprocessing---excision forming
After acupuncture is finished, under 1100～1350 ℃, handled 1～4 hour again, at last by being cut into the mullite crystal refractory fiber blanket finished product of desired size.
3. the mullite crystal refractory fiber blanket that makes according to the described method for making of claim 1 is characterized in that:
(1) its physicals is:
Fibre diameter: 2～6 μ m
ф 〉=0.25mm slag ball content :≤10%
Use temperature: 1500 ℃
Tensile strength: 〉=0.02MPa
Heater wire changes, 1400 ℃ * 24h :≤-1%
Thermal conductivity 0.15～0.20W/mk under 1000 ℃ of the hot-face temperatures
(2) its chemical constitution is: Al
2O
370～72%; SiO
227～29%, surplus is admissible impurity;
(3) its fiber crystalline phase, principal crystalline phase: mullite mullite content 〉=60%.
4. according to the method for making of the described mullite crystal refractory fiber blanket of claim 1, it is characterized in that described concentration of hydrochloric acid solution is 9～10%.
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| CNB2005100127234A CN100396631C (en) | 2005-08-05 | 2005-08-05 | Method for producing mullite crystal refractory fiber blanket and its product |
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| CNB2005100127234A CN100396631C (en) | 2005-08-05 | 2005-08-05 | Method for producing mullite crystal refractory fiber blanket and its product |
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| CN102465358B (en) * | 2010-11-19 | 2014-02-19 | 山东鲁阳股份有限公司 | Method for preparing polycrystal mullite fibers |
| CN102182014B (en) * | 2011-01-26 | 2014-03-12 | 武汉鑫友泰光电科技有限公司 | Preparation method of light quartz fiber felt |
| CN103225130A (en) * | 2012-12-30 | 2013-07-31 | 河北联合大学 | Method for preparing mullite nanofibers by combination of non-hydrolytic sol-gel technology and electrostatic spinning technology |
| CN105734833B (en) * | 2016-02-04 | 2018-03-16 | 河北国美新型建材有限公司 | A kind of alumina silicate gets rid of filament fibre board and preparation method thereof |
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| CN108251966B (en) * | 2018-01-05 | 2018-12-11 | 航天特种材料及工艺技术研究所 | A kind of mullite fiber precast body and preparation method thereof |
| CN108385270A (en) * | 2018-04-26 | 2018-08-10 | 山东鲁阳浩特高技术纤维有限公司 | A kind of alumina fibre composite module and preparation method thereof |
| CN111039690B (en) * | 2019-12-26 | 2022-04-15 | 山东鲁阳浩特高技术纤维有限公司 | Alumina fiber composite module and preparation method thereof |
| CN111455554B (en) * | 2020-04-07 | 2021-07-23 | 山东鲁阳浩特高技术纤维有限公司 | Alumina fiber blanket and preparation method thereof |
| CN111270411B (en) * | 2020-04-07 | 2021-08-06 | 山东鲁阳浩特高技术纤维有限公司 | Preparation method of alumina fiber blanket |
| CN113846424B (en) * | 2021-09-26 | 2022-11-15 | 航天特种材料及工艺技术研究所 | Mullite fiber needled felt and preparation method thereof |
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| CN1749190A (en) | 2006-03-22 |
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