CN103114352A - Preparation method of sol gel of alumina fiber - Google Patents
Preparation method of sol gel of alumina fiber Download PDFInfo
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- CN103114352A CN103114352A CN 201310057784 CN201310057784A CN103114352A CN 103114352 A CN103114352 A CN 103114352A CN 201310057784 CN201310057784 CN 201310057784 CN 201310057784 A CN201310057784 A CN 201310057784A CN 103114352 A CN103114352 A CN 103114352A
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Abstract
The invention discloses a preparation method of sol gel of alumina fiber, and belongs to the field of inorganic fiber. In the method, spinnable sol can be obtained by taking crystallized alumina, deionized water and aluminum powder as major raw materials and taking a filamentization aid as an accessory; and the spinnable sol is subjected to fiber forming, drying and heat treatment process to obtain the alumina fiber. The preparation method disclosed by the invention has the advantages of easily available raw materials, simple technology, convenience in operation and low energy consumption, and can obtain the continuous fiber. The obtained gel fiber is colorless and transparent with gloss, and the surface is smooth without obvious defects; the alumina fiber obtained after the heat treatment at certain temperature has a complete crystal form and grows well; and the fiber surface is dense and uniform and has a good mechanical property.
Description
Technical field
The invention belongs to the Inorganic Non-metallic Materials preparing technical field, particularly a kind of preparation method of alumina fibre.
Technical background
Alumina fibre is a kind of novel high-performance inorganic oxide fibres that grew up in recent years, and it is that a kind of main component is the docrystalline inorfil of aluminium oxide.Alumina fibre has chemical stability, structural stability and excellent high-temperature mechanics, is widely used in the field higher to material requirements.Its raw material is easy to get, and the production path is simple, and is less demanding to production equipment, and inorganicization process need not blanketing with inert gas, can directly carry out in air.With respect to commodity inorfils such as carbon fiber and Nicalon, the production cost of alumina fibre is much lower.In today of economic develop rapidly, aluminium oxide has strategic importance important on preeminent cost performance, military project and huge commercial value.As important strategic materials, the import of alumina fibre is subjected to restriction abroad always, and domestic research to aluminium oxide mainly is confined to staple fibre, aspect continuous alumina fiber, domestic research level is relatively backward, the fiber continuity that obtains and mechanical property do not reach the requirement that relevant departments use, and therefore explore the new preparation technology of alumina fibre, and the performance indications that further improve alumina fibre are the emphasis in the alumina fibre research of present China.In the situation that the staple fibre of this domestic production can't be satisfied the demand again, it is necessary that China researches and develops the aluminium oxide continuous fibers with independent intellectual property right.
Summary of the invention
The sol-gel process for preparing that the purpose of this invention is to provide a kind of alumina fibre.
A kind of sol-gel process for preparing of alumina fibre is characterized in that the method comprises the following steps:
(1) get a certain amount of crystalline aluminum oxide, add deionized water, mix, obtain liquor alumini chloridi;
(2) ratio of aluminium powder in n (AlCl36H2O)/n (Al)=1: 2～1: 4 added in described liquor alumini chloridi, add hot reflux 6～16h in the churned mechanically while in the water bath with thermostatic control of 80～100 ℃, obtain the colloid mother liquor;
(3) will add the fibroblast auxiliary agent in described colloid mother liquor, stir and 40～100 ℃ of concentrated certain hours of constant temperature, obtain the boehmite spinnable colloidal sols of faint yellow transparent colloid form;
(4) with fibroblast under described boehmite spinnable colloidal sols room temperature and dry, obtain gelatinous fibre;
(5) with the heat treatment under 1200 ℃～1400 ℃ heat treatment temperatures of described gelatinous fibre, namely obtain alumina fibre.
Described colloid mother liquor need carry out suction filtration to be processed.
When described fibroblast auxiliary agent was lactic acid, concentration was mass percent 5～20%.
When described fibroblast auxiliary agent was acetic acid, concentration was mass percent 5～40%.
Described mother liquor simmer down to boehmite spinnable colloidal sols required time is 10～12h.
Described fibroblast is 100～350Pas with boehmite sol viscosity.
Described drying is that room temperature is dried 12～36h.
Described heat treatment process is that the heating rate between room temperature～277 ℃ is 0.5～2 ℃/min, insulation 1～3h; Heating rate between 277 ℃～630 ℃ is 0.5～2 ℃/min, insulation 1～3h; 630 ℃ of later heating rates are 2～5 ℃/min, insulation 1～3h.
Beneficial effect of the present invention is: because boehmite sol adopts the sol-gal process preparation, the method preparation temperature is low, and the time used is short, gained colloidal sol good uniformity, purity is high, stable performance, and this technique is simple to operation, and process conditions require low, are suitable for industrial application.
Description of drawings
Fig. 1 is that the alumina fibre of embodiment 1 preparation amplifies scanning electronic microscope (SEM) picture of 3000 times;
Fig. 2 is that the alumina fibre of embodiment 2 preparations amplifies scanning electronic microscope (SEM) picture of 3000 times.
The specific embodiment
Adopt sol-gal process, make the colloid mother liquor take aluminium chloride, aluminium powder, water as raw material.Fibroblast auxiliary agent lactic acid is added in the colloid mother liquor concentrate, obtain spinnable colloidal sols.The spinnable colloidal sols fibroblast obtains gelatinous fibre, after heat treatment, finally obtains alumina fibre under dry also uniform temperature.
The invention will be further described below in conjunction with drawings and Examples:
Embodiment 1
Get a certain amount of crystalline aluminum oxide, add deionized water, mix, obtain liquor alumini chloridi.Aluminium powder is pressed n (AlCl
36H
2O) ratio of/n (Al)=1: 2 adds in described liquor alumini chloridi, adds hot reflux 12h in the water bath with thermostatic control of 80 ℃ in the churned mechanically while, obtains the colloid mother liquor, then is transferred to carry out suction filtration in the suction filtration device and process.Adding mass percent in the colloid mother liquor is 5% lactic acid fibroblast auxiliary agent, stirs and in the concentrated 12h of 60 ℃ of constant temperature, the viscosity that obtains faint yellow transparent colloid form is 100Pas boehmite spinnable colloidal sols.With fibroblast under boehmite spinnable colloidal sols room temperature and dry 18h, obtain gelatinous fibre.Heating rate between gelatinous fibre heat treatment under 1400 ℃ of heat treatment temperatures, room temperature～277 ℃ is 1 ℃/min, insulation 1h; Heating rate between 277 ℃～630 ℃ is 1 ℃/min, insulation 1h; Heating rate between 630 ℃～1400 ℃ is 2 ℃/min, and insulation 1.5h namely obtains alumina fibre.
Fig. 1 is that the alumina fibre of embodiment 1 preparation amplifies scanning electronic microscope (SEM) picture of 3000 times, can find out fiber surface even compact, free of surface defects.Gained alumina fibre diameter is about 7 μ m, and TENSILE STRENGTH is 5.8cN/dtex, and elongation at break is 12.07%.
Embodiment 2
Get a certain amount of crystalline aluminum oxide, add deionized water, mix, obtain liquor alumini chloridi.Aluminium powder is pressed n (AlCl
36H
2O) ratio of/n (Al)=1: 3 adds in described liquor alumini chloridi, adds hot reflux 10h in the water bath with thermostatic control of 90 ℃ in the churned mechanically while, obtains the colloid mother liquor, then is transferred to carry out suction filtration in the suction filtration device and process.Adding mass percent in the colloid mother liquor is 30% acetic acid fibroblast auxiliary agent, stir and 70 ℃ of concentrated 10h of constant temperature, the viscosity that obtains faint yellow transparent colloid form is 200Pas boehmite spinnable colloidal sols, and fibroblast and at the dry 24h of air at room temperature under room temperature obtains gelatinous fibre.Gelatinous fibre heat treatment under 1200 ℃ of heat treatment temperatures, the heating rate of controlling between room temperature～277 ℃ is 2 ℃/min, insulation 3h; Heating rate between controlling 277 ℃～630 ℃ is 2 ℃/min, insulation 3h; Heating rate between controlling 630 ℃～1200 ℃ is 5 ℃/min, and insulation 2h namely obtains alumina fibre.
Fig. 2 is that the alumina fibre of embodiment 2 preparations amplifies scanning electronic microscope (SEM) picture of 3000 times, and as can be seen from the figure the alumina fibre surface uniform, have a little hole.Gained alumina fibre diameter is about 6 μ m, and TENSILE STRENGTH is 3.8cN/dtex, and elongation at break is 9.07%.
Claims (8)
1. the sol-gel process for preparing of an alumina fibre, is characterized in that, the method comprises the following steps:
(1) get a certain amount of crystalline aluminum oxide, add deionized water, mix, obtain liquor alumini chloridi;
(2) ratio of aluminium powder in n (AlCl36H2O)/n (Al)=1: 2～1: 4 added in described liquor alumini chloridi, add hot reflux 6～16h in the churned mechanically while in the water bath with thermostatic control of 80～100 ℃, obtain the colloid mother liquor;
(3) will add the fibroblast auxiliary agent in described colloid mother liquor, stir and 40～100 ℃ of concentrated certain hours of constant temperature, obtain the boehmite spinnable colloidal sols of faint yellow transparent colloid form;
(4) with fibroblast under described boehmite spinnable colloidal sols room temperature and dry, obtain gelatinous fibre;
(5) with the heat treatment under 1200 ℃～1400 ℃ heat treatment temperatures of described gelatinous fibre, namely obtain alumina fibre.
2. preparation method according to claim 1 is characterized in that: in step (2), described colloid mother liquor need carry out suction filtration to be processed.
3. preparation method according to claim 1, it is characterized in that: in step (3), when described fibroblast auxiliary agent was lactic acid, concentration was mass percent 5～20%.
4. preparation method according to claim 3, it is characterized in that: in step (3), when described fibroblast auxiliary agent was acetic acid, concentration was mass percent 5～40%.
5. preparation method according to claim 1, it is characterized in that: in step (3), described mother liquor simmer down to boehmite spinnable colloidal sols required time is 10～12h.
6. preparation method according to claim 1, it is characterized in that: in step (3), described fibroblast is 100～350Pas with boehmite sol viscosity.
7. preparation method according to claim 1, it is characterized in that: in step (4), described drying is that room temperature is dried 12～36h.
8. preparation method according to claim 1 is characterized in that: in step (5), described heat treatment process is that the heating rate between room temperature～277 ℃ is 0.5～2 ℃/min, insulation 1～3h; Heating rate between 277 ℃～630 ℃ is 0.5～2 ℃/min, insulation 1～3h; 630 ℃ of later heating rates are 2～5 ℃/min, insulation 1～3h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104086201A (en) * | 2014-07-22 | 2014-10-08 | 南京理工宇龙新材料科技有限公司 | High-purity alumina fiber and preparation method thereof |
| CN106458623A (en) * | 2014-05-25 | 2017-02-22 | 王胜国 | Method and apparatus for producing alumina monohydrate and sol gel abrasive grain |
| CN109422919A (en) * | 2017-09-05 | 2019-03-05 | 张家港市五湖新材料技术开发有限公司 | A kind of preparation method of aluminium oxide-chitosan aerogel composite |
| CN109939664A (en) * | 2019-04-16 | 2019-06-28 | 天津工业大学 | A kind of multiple dimensioned preparation method for receiving micrometer alumina fiber photocatalyst carrier |
| CN109987929A (en) * | 2019-04-16 | 2019-07-09 | 天津工业大学 | A kind of preparation method of the multiple dimensioned alumina fibre of needle prick shape of fluorine induced growth |
-
2013
- 2013-02-25 CN CN 201310057784 patent/CN103114352A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106458623A (en) * | 2014-05-25 | 2017-02-22 | 王胜国 | Method and apparatus for producing alumina monohydrate and sol gel abrasive grain |
| CN104086201A (en) * | 2014-07-22 | 2014-10-08 | 南京理工宇龙新材料科技有限公司 | High-purity alumina fiber and preparation method thereof |
| CN109422919A (en) * | 2017-09-05 | 2019-03-05 | 张家港市五湖新材料技术开发有限公司 | A kind of preparation method of aluminium oxide-chitosan aerogel composite |
| CN109939664A (en) * | 2019-04-16 | 2019-06-28 | 天津工业大学 | A kind of multiple dimensioned preparation method for receiving micrometer alumina fiber photocatalyst carrier |
| CN109987929A (en) * | 2019-04-16 | 2019-07-09 | 天津工业大学 | A kind of preparation method of the multiple dimensioned alumina fibre of needle prick shape of fluorine induced growth |
| CN109987929B (en) * | 2019-04-16 | 2021-07-27 | 天津工业大学 | Preparation method of fluorine-induced-growth needle-punched multi-scale alumina fiber |
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Application publication date: 20130522 |