CN107778016A - The method that alumina sol infusion process prepares alumina fibre - Google Patents

The method that alumina sol infusion process prepares alumina fibre Download PDF

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Publication number
CN107778016A
CN107778016A CN201711074769.8A CN201711074769A CN107778016A CN 107778016 A CN107778016 A CN 107778016A CN 201711074769 A CN201711074769 A CN 201711074769A CN 107778016 A CN107778016 A CN 107778016A
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Prior art keywords
alumina
infusion process
process prepares
alumina sol
alumina fibre
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CN201711074769.8A
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王耀斌
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Shaanxi Shengmai Petroleum Co Ltd
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Shaanxi Shengmai Petroleum Co Ltd
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Priority to CN201711074769.8A priority Critical patent/CN107778016A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/48Halides, with or without other cations besides aluminium
    • C01F7/56Chlorides
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/62227Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
    • C04B35/62231Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on oxide ceramics
    • C04B35/62236Fibres based on aluminium oxide

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Ceramic Engineering (AREA)
  • Structural Engineering (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Nonwoven Fabrics (AREA)
  • Inorganic Fibers (AREA)
  • Paper (AREA)

Abstract

The present invention discloses a kind of method that alumina sol infusion process prepares alumina fibre, comprises the following steps:(1)Aluminium powder and mass concentration are mixed for 8% aluminum chloride aqueous solution, the 5h of stirring reaction 3 generates aluminium polychloride under conditions of 80~100 DEG C;(2)It is 95 according to the mass ratio of alundum (Al2O3) and silica:5, aluminium polychloride and hydrosol of silicic acid are mixed, 2 3h are heated to reflux at 100 DEG C, obtain alumina sol;(3)By step(2)After obtained aluminum oxide silica gel microwave reaction 5min, then ultrasonic disperse, obtain maceration extract;(4)By step(3)Obtained maceration extract calcining, you can obtain alumina fibre.The alumina fibre that the present invention is prepared, surface is smooth, and diameter is evenly distributed, and form is good, and intensity is high, and preparation method is simple, and cost is low.

Description

The method that alumina sol infusion process prepares alumina fibre
Technical field
The invention belongs to the preparation field of alumina fibre, and in particular to a kind of alumina sol infusion process prepares aluminum oxide The method of fiber.
Background technology
Alumina fibre due to its excellent chemistry and structural stability, may be used as high temperature thermal insulation material, insulation material, Catalyst carrier, fuel cell barrier film material in pyroreaction, and the strengthening material of resin, metal and ceramic matric composite Material, this causes alumina fibre to turn into the technical fiber with researching value and market prospects.
Because the wellability of alumina fibre and metallic matrix is good, interfacial reaction is smaller, the mechanical property of its composite, Wearability, hardness are improved, and thermal coefficient of expansion reduces.The metal-base composites of alumina fibre enhancing is lived in automobile It is applied in plunger member and rotary gas compressor blade.Again because alumina fibre and resin matrix are well combined, compare glass The elasticity of glass fiber is big, better than the compressive strength of carbon fiber, so aluminum oxide resin composite materials just progressively take in some fields For glass fibre and carbon fiber.
At present, the domestic method for preparing oxide fibre use is mainly sol-gel process.
Fiber prepared by sol-gel process is used for heat-barrier material, and complex process, and variable factor is more whard to control.
Fiber prepared by infusion process is mainly using organic fiber as presoma, after being impregnated in metal salt solution, by washing, Dry, obtain the oxide fibre with some strength after heat treatment, be mainly used in prepare ceramic fibre at present, but prepare Method is complicated, and the fibre strength being prepared is poor, and fiber surface is coarse.
The content of the invention
The defects of for prior art, the present invention provide the side that a kind of alumina sol infusion process prepares alumina fibre Method.
The method that alumina sol infusion process prepares alumina fibre, comprises the following steps:
(1)Aluminium powder and mass concentration are mixed for 8% aluminum chloride aqueous solution, the stirring reaction 3-5h under conditions of 80~100 DEG C Generate aluminium polychloride;
(2)It is 95 according to the mass ratio of alundum (Al2O3) and silica:5, aluminium polychloride and hydrosol of silicic acid are mixed, 2-3h is heated to reflux at 100 DEG C, obtains alumina sol;
(3)By step(2)After obtained aluminum oxide silica gel microwave reaction 5min, then ultrasonic disperse, obtain maceration extract;
(4)By step(3)Obtained maceration extract calcining, you can obtain alumina fibre.
Preferably, step(1)Aluminium powder, the mass ratio of aluminum chloride aqueous solution are(3-5):22.
Preferably, step(3)The power of middle microwave reaction is 200W.
Preferably, step(3)The condition of middle ultrasonic disperse is:It is first ultrasonic under conditions of power 100W, frequency 20Hz 20min, the then ultrasonic 15min under conditions of power 30W, frequency 30.
Preferably, step(4)The condition of middle calcining is:8-10h is calcined at 900-1300 DEG C.
Preferably, step(1)The speed of middle stirring is 3000rpm.
Advantages of the present invention:
The alumina fibre that the present invention is prepared, surface is smooth, and diameter is evenly distributed, and form is good, and intensity is high, and preparation method Simply, cost is low.
Embodiment
Embodiment 1
The method that alumina sol infusion process prepares alumina fibre, comprises the following steps:
(1)Aluminium powder and mass concentration are mixed for 8% aluminum chloride aqueous solution, under conditions of 80 DEG C, mixing speed is Under conditions of 3000rpm, stirring reaction 3h generation aluminium polychlorides;Wherein, aluminium powder, the mass ratio of aluminum chloride aqueous solution are 3: 22;
(2)It is 95 according to the mass ratio of alundum (Al2O3) and silica:5, aluminium polychloride and hydrosol of silicic acid are mixed, 2h is heated to reflux at 100 DEG C, obtains alumina sol;
(3)By step(2)Obtained aluminum oxide silica gel is after microwave reaction 5min under conditions of power is 200W, then carries out ultrasound Scattered, the condition of ultrasonic disperse is:The first ultrasonic 20min under conditions of power 100W, frequency 20Hz, then in power 30W, frequency Ultrasonic 15min, obtains maceration extract under conditions of rate 30;
(4)By step(3)Obtained maceration extract calcines 10h calcinings at 900 DEG C, you can obtains alumina fibre.
Embodiment 2
The method that alumina sol infusion process prepares alumina fibre, comprises the following steps:
(1)Aluminium powder and mass concentration are mixed for 8% aluminum chloride aqueous solution, under conditions of 100 DEG C, mixing speed is Under conditions of 3000rpm, stirring reaction 5h generation aluminium polychlorides;Wherein, aluminium powder, the mass ratio of aluminum chloride aqueous solution are 5: 22;
(2)It is 95 according to the mass ratio of alundum (Al2O3) and silica:5, aluminium polychloride and hydrosol of silicic acid are mixed, 3h is heated to reflux at 100 DEG C, obtains alumina sol;
(3)By step(2)Obtained aluminum oxide silica gel is after microwave reaction 5min under conditions of power is 200W, then carries out ultrasound Scattered, the condition of ultrasonic disperse is:The first ultrasonic 20min under conditions of power 100W, frequency 20Hz, then in power 30W, frequency Ultrasonic 15min, obtains maceration extract under conditions of rate 30;
(4)By step(3)Obtained maceration extract calcines 8h calcinings at 1300 DEG C, you can obtains alumina fibre.
Embodiment 3
The method that alumina sol infusion process prepares alumina fibre, comprises the following steps:
(1)Aluminium powder and mass concentration are mixed for 8% aluminum chloride aqueous solution, under conditions of 90 DEG C, mixing speed is Under conditions of 3000rpm, stirring reaction 4h generation aluminium polychlorides;Wherein, aluminium powder, the mass ratio of aluminum chloride aqueous solution are 4.5: 22;
(2)It is 95 according to the mass ratio of alundum (Al2O3) and silica:5, aluminium polychloride and hydrosol of silicic acid are mixed, 2.5h is heated to reflux at 100 DEG C, obtains alumina sol;
(3)By step(2)Obtained aluminum oxide silica gel is after microwave reaction 5min under conditions of power is 200W, then carries out ultrasound Scattered, the condition of ultrasonic disperse is:The first ultrasonic 20min under conditions of power 100W, frequency 20Hz, then in power 30W, frequency Ultrasonic 15min, obtains maceration extract under conditions of rate 30;
(4)By step(3)Obtained maceration extract calcines 8h calcinings at 1000 DEG C, you can obtains alumina fibre.
Embodiment 4
The method that alumina sol infusion process prepares alumina fibre, comprises the following steps:
(1)Aluminium powder and mass concentration are mixed for 8% aluminum chloride aqueous solution, under conditions of 95 DEG C, mixing speed is Under conditions of 3000rpm, stirring reaction 4.5h generation aluminium polychlorides;Wherein, aluminium powder, the mass ratio of aluminum chloride aqueous solution are 3.5:22;
(2)It is 95 according to the mass ratio of alundum (Al2O3) and silica:5, aluminium polychloride and hydrosol of silicic acid are mixed, 3h is heated to reflux at 100 DEG C, obtains alumina sol;
(3)By step(2)Obtained aluminum oxide silica gel is after microwave reaction 5min under conditions of power is 200W, then carries out ultrasound Scattered, the condition of ultrasonic disperse is:The first ultrasonic 20min under conditions of power 100W, frequency 20Hz, then in power 30W, frequency Ultrasonic 15min, obtains maceration extract under conditions of rate 30;
(4)By step(3)Obtained maceration extract calcines 10h calcinings at 1100 DEG C, you can obtains alumina fibre.

Claims (6)

1. the method that alumina sol infusion process prepares alumina fibre, it is characterised in that:Comprise the following steps:
(1)Aluminium powder and mass concentration are mixed for 8% aluminum chloride aqueous solution, the stirring reaction 3-5h under conditions of 80~100 DEG C Generate aluminium polychloride;
(2)It is 95 according to the mass ratio of alundum (Al2O3) and silica:5, aluminium polychloride and hydrosol of silicic acid are mixed, 2-3h is heated to reflux at 100 DEG C, obtains alumina sol;
(3)By step(2)After obtained aluminum oxide silica gel microwave reaction 5min, then ultrasonic disperse, obtain maceration extract;
(4)By step(3)Obtained maceration extract calcining, you can obtain alumina fibre.
2. the method that alumina sol infusion process prepares alumina fibre according to claim 1, it is characterised in that:Step (1)Aluminium powder, the mass ratio of aluminum chloride aqueous solution are(3-5):22.
3. the method that alumina sol infusion process prepares alumina fibre according to claim 1, it is characterised in that:Step (3)The power of middle microwave reaction is 200W.
4. the method that alumina sol infusion process prepares alumina fibre according to claim 1, it is characterised in that:Step (3)The condition of middle ultrasonic disperse is:The first ultrasonic 20min under conditions of power 100W, frequency 20Hz, then in power 30W, frequency Ultrasonic 15min under conditions of rate 30.
5. the method that alumina sol infusion process prepares alumina fibre according to claim 1, it is characterised in that:Step (4)The condition of middle calcining is:8-10h is calcined at 900-1300 DEG C.
6. the method that alumina sol infusion process prepares alumina fibre according to claim 1, it is characterised in that:Step (1)The speed of middle stirring is 3000rpm.
CN201711074769.8A 2017-11-06 2017-11-06 The method that alumina sol infusion process prepares alumina fibre Withdrawn CN107778016A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111218731A (en) * 2019-12-26 2020-06-02 山东鲁阳浩特高技术纤维有限公司 Sol for preparing alumina fiber and preparation method thereof
CN112320828A (en) * 2020-10-14 2021-02-05 中纳电子科技连云港有限公司 Method for preparing nano macroporous low-density spherical alumina by acid-base electrochemical double-string method
CN113522304A (en) * 2021-08-04 2021-10-22 安徽科浦环保科技有限公司 Preparation method of wide-temperature selective trapping reduction denitration material
CN113956026A (en) * 2021-11-29 2022-01-21 福建师范大学泉港石化研究院 Preparation method of boron-doped aluminum silicate ceramic long fiber
CN116332665A (en) * 2023-03-08 2023-06-27 航天特种材料及工艺技术研究所 Preparation method of alumina fiber reinforced alumina ceramic matrix composite material containing low-mode interface

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111218731A (en) * 2019-12-26 2020-06-02 山东鲁阳浩特高技术纤维有限公司 Sol for preparing alumina fiber and preparation method thereof
CN111218731B (en) * 2019-12-26 2023-02-03 山东鲁阳浩特高技术纤维有限公司 Sol for preparing alumina fiber and preparation method thereof
CN112320828A (en) * 2020-10-14 2021-02-05 中纳电子科技连云港有限公司 Method for preparing nano macroporous low-density spherical alumina by acid-base electrochemical double-string method
CN113522304A (en) * 2021-08-04 2021-10-22 安徽科浦环保科技有限公司 Preparation method of wide-temperature selective trapping reduction denitration material
CN113956026A (en) * 2021-11-29 2022-01-21 福建师范大学泉港石化研究院 Preparation method of boron-doped aluminum silicate ceramic long fiber
CN116332665A (en) * 2023-03-08 2023-06-27 航天特种材料及工艺技术研究所 Preparation method of alumina fiber reinforced alumina ceramic matrix composite material containing low-mode interface

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