CN1014043B - Method for preparing compound aluminium oxide fibre - Google Patents
Method for preparing compound aluminium oxide fibreInfo
- Publication number
- CN1014043B CN1014043B CN 87101912 CN87101912A CN1014043B CN 1014043 B CN1014043 B CN 1014043B CN 87101912 CN87101912 CN 87101912 CN 87101912 A CN87101912 A CN 87101912A CN 1014043 B CN1014043 B CN 1014043B
- Authority
- CN
- China
- Prior art keywords
- spinning solution
- aluminium oxide
- colloidal sol
- oxide fibre
- fiber
- Prior art date
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Abstract
The present invention provides a preparing method of silicon containing alumina fiber, which comprises the steps as follows: AlCl3.6H2O, aluminum and water or aluminum, hydrochloric acid and water are mixed to prepare aluminium oxychloride collosol in which the atomic ratio of Al to Cl is 1.5: 2.1; polyvinyl alcohol and an ethyl orthosilicate alcoholic solution are mixed for hydrolyzation to prepare fresh silicasol; the aluminium oxychloride collosol and the fresh silicasol are mixed with the alcohol from C2 to C8 to prepare a spinning solution; the spinning solution is injected by compressed air to prepare precursor fiber; the precursor fiber is baked at low temperature of 60 to 100 DEG C, heated with water vapor at 300 to 400 DEG C, and roasted at high temperature of 850 to 1300 DEG C to prepare silicon containing alumina fiber. The present invention has the advantages of easy acquisition of silicide as raw material, simple preparation technology of the spinning solution, and high quality of fiber, and thus, the present invention can be widely used for preparing silicon containing alumina fiber in different function.
Description
The present invention relates to the preparation method of inorganic fibre, specifically belong to the preparation method of siliceous compound aluminium oxide fibre.
Sapphire whisker is the novel light inorganic materials that the seventies grows up.Because it has high temperature resistant, low heat conductivity and high chemical resistance of concrete ability, thereby is widely used in aerospace, nuclear power and large-scale metallurgical stove, forging furnace liner, lagging material or hot antidetonation, sound-proof material etc.; Because it has high outside surface, therefore low endoporus resistance is suitable for doing the support of the catalyst of diffusion controlled reaction especially.The alumina short fibre metal-base composites that the eighties grows up have light weight, high temperature resistant, resistance to wear, antifatigue and low thermal expansivity and cheap, be a kind of up-and-coming strongthener therefore.
As everyone knows, the sapphire whisker precursor is heated to 1000～1100 ℃ when heat-treating, can the α phase transformation take place and cause fiber itself to be pulverized, in preparation aluminum oxide spinning solution process, need to add second component for this reason, in the sapphire whisker heat treatment process, stablize the aluminum oxide crystalline phase, prevent α phase transformation or grain growth and cause fiber to be pulverized or intensity reduces.Usually adopt and contain the inhibitor of compounds such as p, Ca, Mg, La, Si as sapphire whisker α phase transformation or grain growth.Wherein more effective composition is SiO
2, but the adding silicide is then difficult unusually in aluminium colloidal sol, if add inorganic silicon in aluminium colloidal sol, very easy gel can't spray silk; If add organosilicon, then can't dissolve.So, how to prepare the stable siliceous spinning solution that is suitable for spraying silk, become the key of preparation sapphire whisker.For this reason, some feasible methods have been found in the continuous effort of personnel after deliberation, as: Bp 1,445,331 disclose the method that adds the water-soluble poly siloxanes in a kind of chlorine oxygen aluminium colloidal sol, but this compound is synthetic complicated, be difficult for obtaining, cost is also high, should not promote the use of.Public clear 55-20239 of day has proposed a kind of with the preparation method of water glass as the compound aluminium oxide fibre in silicide source, this method adds common water glass in the sulfuric acid and control pH=2～4, placed 12～24 hours, make the silicon gel, water flush away sodium ion then, this moisture silicon gel is broken into 15～50 μ fine particles, under condition of stirring, is distributed to then in the chlorine oxygen aluminium colloidal sol, make siliceous spinning solution.Spinning solution behind the interpolation polyvinyl alcohol slowly is heated to 500 ℃ through the compound aluminium oxide fibre precursor of centrifugal spinning gained from room temperature, removes the fugitive constituent in the fiber precursor, is warming up to 1200 ℃ of following roastings and gets compound aluminium oxide fibre in about 20 minutes.This method is the source preparation spinning solution of silicide with water glass, and technology is very complicated, and is not easy to operate, therefore also can influence the quality of finished fiber.The siliceous aluminum oxide spinning solution of existing preparation method is perhaps because the restriction of suitable silicide raw material perhaps owing to the blending process complexity, has influenced the compound aluminium oxide fibre industrial expansion.
The object of the present invention is to provide a kind of silicide raw material to be easy to get, siliceous preparation of spinning solution technology is simple, easy to operate, the preparation method of the siliceous compound aluminium oxide fibre that thermal effectiveness is good.
The preparation method of compound aluminium oxide fibre provided by the invention may further comprise the steps:
1) AlCl
3, 6H
2O, metallic aluminium and water or metallic aluminium, hydrochloric acid and water are 80～110 ℃ of down widely different streams 15～120 hours at reflux temperature, make the Al/Cl(atomic ratio after filtration)=1.5～2.1 chlorine oxygen aluminium colloidal sol,
2) add spinning-aid agent, silicide, defoamer in the above-mentioned chlorine oxygen aluminium colloidal sol for preparing, through the concentrated spinning solution that obtains certain viscosity,
3) above-mentioned spinning solution becomes fibre to make the compound aluminium oxide fibre precursor,
4) thermal treatment of compound aluminium oxide fibre,
Characteristics of the present invention are:
1) spinning solution is prepared as follows:
A, in the chlorine oxygen aluminium colloidal sol of the Al/Cl=1.5 for preparing～2.1, add earlier Al in this aluminium colloidal sol
2O
3The mean polymerisation degree of the 2-10% of weight is 1000～3000, and alcoholysis degree is 80～98% polyvinyl alcohol spinning-aid agent, and the concentration of polyvinyl alcohol solution is 1～5%,
Add 0.1～1.5%(with Al in b, the above-mentioned spinning solution
2O
3Weight is benchmark) defoamer C
2～C
8Alcohol,
C, in the presence of hydrochloric acid and water, separate the fresh silicon sol that obtains with the tetraethoxy after the alcohol dissolving and add in the above-mentioned aluminium colloidal sol that contains spinning-aid agent, be concentrated into viscosity 10～50 pools then, adjust the proportioning of silicon sol and aluminium colloidal sol, make SiO in the spinning solution of gained
2/ Al
2O
3(weight) 3～15%,
2) said one-tenth method for fiber is a blowing process: with the above-mentioned spinning solution that is concentrated into 10～50 pools (20 ℃ time), put into the liquid tank of band shower nozzle after the filtration, liquid stream that sprays by at least one nozzle under pressurized air pushes and the high velocity air that sprays from least one gas jet are 25 ℃～40 ℃ of room temperatures, relative humidity be 40～80% times and stream jet the compound aluminium oxide fibre precursor
3) the sapphire whisker precursor of winding-up gained toasted 20～30 minutes down at 60～100 ℃ earlier, low temperature (300～400 ℃) was handled 15～30 minutes under water vapour atmosphere then, high temperature (850～1300 ℃) roasting 20～40 minutes under oxidizing atmosphere at last.
It is the silicon raw material with the tetraethoxy that the present invention studies successful, C
2～C
8Alcohol is the preparation of spinning solution novel process of principal feature as defoamer, gained spinning solution good stability, and the silicide raw material is easy to get, and blending process is simple, and is easy to operate.
The chlorine oxygen aluminium colloidal sol available metal aluminium powder that the present invention relates to, metal aluminum shot or aluminium bits directly and hydrochloric acid reaction make, but the also compound of aluminium, for example: AlCl
3, 6H
2O, Al(NO
3)
39H
2O or Al
2(So
4)
318H
2O, metallic aluminium and water are formulated, and aluminum compound is with AlCl
36H
2O is best, and the purity of metallic aluminium is high more, and fiber fineness height, quality are good, but the time of preparation aluminium colloidal sol is also long, and cost is also high, and the purity of selecting for use usually is 98.5～99.5%.
In the preparation spinning solution process, often need to add the water-soluble polymer organic polymer, with stability and the spinning property of improving spinning solution.Preferably select for use straight chain to gather the hydroxy kind organic polymer, for example polyoxyethylene glycol, polyethylene oxide, polyvinyl alcohol etc., wherein with the polyvinyl alcohol effect for well, selecting the polymerization degree usually for use is 1000～3000, alcoholysis degree is that 80～98% polyvinyl alcohol is as spinning-aid agent.It is that 88% polymerization degree is 1750 ± 50 polyvinyl alcohol that the present invention recommends to select alcoholysis degree for use, and the content of recommendation is 6～8%, and the concentration of polyvinyl alcohol solution is 2～4%.
Because tetraethoxy is water insoluble,, can select C for use so need to prepare fresh silicon sol as solvent with alcohol
1～C
Alcohol, wherein ethanol is the most commonly used, and the required mineral acid of hydrolysis is dilute hydrochloric acid preferably.
If aluminium colloidal sol directly mixes with silicon sol, certainly will cause gel, can not become fine, so spinning-aid agent must join in the aluminium colloidal sol prior to silicon sol.
The present invention adopts the fine method of jetting into, is 10～50 pools during 20 ℃ of the viscosity of the spinning solution that it is suitable, preferably selects 15～30 pools for use.The above-mentioned spinning solution for preparing can be concentrated into required viscosity by methods such as for example underpressure distillation or direct stirring evaporations, and the present invention selects the method for direct stirring evaporation for use.
The spinning solution that the present invention relates to, its SiO
2/ Al
2O
3(weight ratio) is controlled at 3～15% usually, and preferably 5～8%.Cross lowly, can not control Al effectively
2O
3Grain growth, too high, easily generate mullite structure, cause fibre strength to descend.
Be the aeration quality of fiber in the spinning solution after preventing to concentrate, so need to add a small amount of defoamer to remove the bubble that may exist in spinning solution, the present invention recommends C
2～C
Alcohol is preferably selected isopropylcarbinol for use, and suitable amount is that the 0.2-1.5%(of spinning solution is with Al
2O
3Weight is benchmark), add the stability that a spot of alcohol compound also can improve spinning solution in the spinning solution, also can add a small amount of Glacial acetic acid in the spinning solution, reduce the surface tension of spinning solution, be beneficial to fibre, reduce the slag ball of fiber.
Test shows, adds for example Al in spinning solution
2O
30.2～5%MgO of weight can improve the intensity of compound aluminium oxide fibre.
Centrifugal spinning, blowing process etc. all are to produce the effective ways of compound aluminium oxide fibre, and centrifuging output is big, but the equipment cost height.The present invention adopts blowing process to become fine, and the prior art owned by France of jetting normally is expressed to material in the high velocity air by one or more holes and goes, and air flow line is the traffic direction along the material that squeezes out.Under the effect of air-flow, the material that squeezes out is blown to fiber precursor.Fluid jetting head of the present invention can be with one or more nozzles, its quantity depends mainly on the output of fiber, nozzle bore can be different shape, the present invention adopts circle hole shape, the big I in aperture in very large range changes, the present invention selects 0.2～4mm for use, preferably select 0.4～1.0mm for use, spinning solution can adopt the pressurized air extruding to be emitted into fibre in the liquid tank, the size of air pressure depends mainly on the viscosity of spinning solution, the size of nozzle, the output of fiber, can select in a big way, the present invention selectes 1～4kg/cm
2The main effect of high velocity air is to make the liquid stream drawing-off from the liquid jet ejection to become fiber and dehydration typing rapidly, so gas line speed size should adapt with the liquid stream of ejection, and the flow of air-flow is decided by the size and the quantity of gas jet simultaneously, and the selected gas line speed of the present invention is 50～200 meter per seconds.Gas jet can be that the aperture is the circular hole of 0.2～0.8mm, also can be that width is the slit of 0.5～1.5mm, the quantity of nozzle can equate with the quantity of liquid jet, and, gas jet should be established in position, make air-flow concentrate on liquid side of flowing down that liquid jet pushes out or liquid stream near.It is consistent with the liquid flow path direction that the direction of air-flow should keep, or have a certain degree, and the present invention adopts 20～60 °.
For obtaining quality precursor preferably, suitable temperature and the relative humidity of control is crucial.Usually select 25～40 ℃ of room temperatures for use, the relative humidity scope that adapts therewith is 40～80%.Temperature is low excessively, and relative humidity is too high, causes material dehydration rapidly, and the fiber precursor that forms of winding-up is with good adherence of together, and the slag ball is many; The temperature height, relative humidity is low, and then because dehydration is too fast, spinning nozzle is easily stifled.
The present invention adopts comparison demulcent condition part to remove the moisture content of composite alumina precursor, so that colloid fiber does not have subsurface defect and bubble formation, thereby can guarantee the intensity of fibrous finished product.The present invention toasts down at 60～100 ℃ can remove 6～10% moisture content in 20～30 minutes; Then under higher temperature in the presence of water vapor the fiber precursor hydrolysis remove partly chlorine and water, the present invention regulates dechlorination speed and dechlorination amount by control water vapor thermal treatment temp and treatment time, is not destroyed to keep the precursor structure.The water vapor thermal treatment temp is at 300～400 ℃, and the treatment time is 15～30 minutes, and may command dechlorination amount is 50～90%.Dechlorination is too fast, and the dechlorination amount is excessive, can cause the fiber embrittlement.Fiber after water vapor thermal treatment was 850～1300 ℃ of following roastings 20～40 minutes.The fiber surface area of handling under higher maturing temperature is little, and linear shrinkage ratio is low, can be used as high temperature material or metal composite; Low maturing temperature is handled the fiber of gained down, and surface-area is big.
The invention provides a kind of silicon sol made from tetraethoxy, polyvinyl alcohol is a spinning-aid agent, C
2～C
8Alcohol is the preparation of spinning solution novel process of characteristics for defoamer.Therefore compare with soluble glass method, saved the operations such as fragmentation of numerous and diverse gel, washing, gel, simplified and add silicon technology, easy to operate, be beneficial to production.The silicon sol that this law obtains with teos hydrolysis replaces the silicon gel of soluble glass method, has added the good C of effect in addition again
2～C
8The alcohol defoamer obviously improves the stability of the spinning solution that is mixed with and flow characteristics, thereby has improved the quality and the performance of compound aluminium oxide fibre.The present invention adopts low temperature dewatering, the water vapor protection method of low-temperature heat treatment down, has guaranteed that effectively the fiber precursor structure is not destroyed in dehydration, the dechlorination process, thereby has guaranteed the intensity (seeing Table) of fibrous finished product.
Embodiment 1
1. get 120.7 gram AlCl
36H
2The O(chemical pure) is dissolved in the 400ml distilled water, pour into and be added with in the round-bottomed flasks that purity is 99.5% metallic aluminium bits, 67.7 grams, add 1000ml distilled water again, on common widely different stream device in 100 ℃ of widely different streams 24 hours down, filter the chlorine oxygen aluminium colloidal sol that obtains Al/Cl=2.0 then
2. adding 300 gram concentration and be 3% alcoholysis degree in above-mentioned aluminium colloidal sol is 88%, and mean polymerisation degree is 1750 ± 50 polyvinyl alcohol (Beijing Organic Chemical Plant), adds 0.8ml isopropylcarbinol (Beijing Chemical Plant, chemical reagent) again,
3. (white crane chemical plant, Shanghai contains SiO to get 26.5 gram tetraethoxys
228.4%),, drip hydrochloric acid 0.5 gram of 6N, and add 20ml distilled water, obtain fresh silicon sol through hydrolysis in about 10 minutes with 6.5 gram alcohol (chemical pure) stirring and dissolving a little,
4. fresh silicon sol is poured under agitation condition in the above-mentioned aluminium colloidal sol, 18 pools when under 85 ℃, being concentrated into viscosity then and being 20 ℃,
5. the spinning solution that is mixed with by above-mentioned steps is put into the liquid tank of band shower nozzle, with 1kg/cm
2The pressurized air of (gauge pressure) is 0.5 millimeter nozzle ejection by 5 apertures with spinning solution, with the high velocity air from corresponding 5 gas spouts be 25 ℃ in temperature, relative temperature be 60% time and stream jet the composite alumina precursor, each gas spout is long 2mm, the slit of wide 1mm, gas velocity is 70 meter per seconds, and air flow line becomes 30 ° of angles approximately with the liquid flow path direction of ejection
6. will the jet moisture compound aluminium oxide fibre precursor of gained, toasted 30 minutes down at 60 ℃ earlier, in 340 ℃ the processing stove that contains water vapor, handled 20 minutes then, obtain the compound aluminium oxide fibre of green and brown look, obtained pure white softness in 30 minutes 1300 ℃ of following roastings at last, diameter is even, has the siliceous sapphire whisker of glossy, and test result sees Table
Embodiment 2
Add 3.5 gram MgCl in the chlorine oxygen aluminium colloidal sol that makes by embodiment 1 earlier
2, 6H
2O(Beijing Chemical Plant, chemical reagent), press embodiment 1 identical method, step, condition then, maturing temperature is 1000 ℃, obtains softness, pure white, even, has the sapphire whisker that contains magnesium, silicon of silky lustre.
Embodiment 3
The compound aluminium oxide fibre after water vapor thermal treatment that makes by embodiment 1 obtained pure white softness in 30 minutes 850 ℃ of following roastings, and diameter is even, is rich in gloss, the siliceous sapphire whisker that tensile strength is fabulous.
Embodiment 4
Get 89.5 gram AlCl
36H
2O is dissolved in the distilled water of 300ml, pour into and be added with at the bottom of the gardens that purity is 99.5% metallic aluminium bits, 47.0 grams in the flask, add 1000ml distilled water again and on common widely different stream device, descended widely different streams 24 hours at 100 ℃, filtration obtains the chlorine oxygen aluminium colloidal sol of Al/Cl=1.9, below pure white, soft by obtaining under embodiment 1 identical method, step, the condition, evenly and have a siliceous sapphire whisker of glossy.
Embodiment 5
1. getting 80.0 gram purity is that 99.5% aluminium bits are put into there-necked flask adding 340ml distilled water, other gets 38% concentrated hydrochloric acid, 130ml, with slowly being added dropwise to behind the distilled water diluting of equivalent in the flask and reactive aluminum, after question response relaxed, intensification was boiled, widely different stream 22 hours, obtain the chlorine oxygen aluminium colloidal sol of Al/Cl=1.80 after filtration
2. adding 300 gram concentration and be 4% alcoholysis degree in above-mentioned aluminium colloidal sol is 98%, mean polymerisation degree is 1750 ± 50 polyvinyl alcohol (Red Star chemical plant, Beijing), add the 1ml isopropylcarbinol again, obtained the siliceous sapphire whisker similar by resulting compound aluminium oxide fibre after water vapor thermal treatment under embodiment 1 identical method, step, the condition in 20 minutes 1100 ℃ of following roastings then with embodiment 1,4.
The explanation of tabular data testing method:
1. crystallization phases and average crystal grain size are to adopt the X-ray diffraction method to record,
Linear shrinkage ratio be fiber in the data of 1500 ℃ of following calcinations after two hours,
3. specific surface area is to adopt BET static capacity absorption method (2500 absorption instrument) to record,
4. mean diameter: using magnification is the diameter that 380～630 times optical readings microscope is directly measured every fiber, and the arithmetical av of 100 Fibre diameters is average fibre diameter.
5. the slag ball is meant that diameter is greater than the non-fibrous material of 0.07mm in the sample, and slag ball content is represented with the percentage ratio that the slag ball weight accounts for original sample weight.
Put into mortar after sample drying weighed, add less water, be ground into pasty state, utilize the elutriation method to make slag ball and fiber separation with the pestle of being with rubber tip.The oven dry of slag ball is sieved, and weighs greater than the slag ball of 0.07mm in the cut-off footpath, and calculating can get slag ball content in the fiber sample.
6. alumina fiber blanket tensile strength is carried out on " the fibrefelt tensile strength determinator " that design voluntarily.Method is: neatly cut fiber sample 0.5 gram of 6 centimetres of 5 cm x, be clipped on the two ends anchor clamps of " drawing strong instrument ".Each is wide 5 centimetres for anchor clamps, and long 1.5 centimetres is 3 centimetres so sample bears the length of pulling force, wide 5 centimetres.After opening " drawing strong instrument ", fiber sample begins evenly stressed, and the instrument upper spring extends gradually.When pulling force increases to a certain limit and causes sample and rupture suddenly, read spring elongation millimeter, calculate fibrefelt tensile strength in view of the above.
By table as seen, adopt the most performance index of compound aluminium oxide fibre of the said method preparation of the present invention close with the Saffil fiber, its grain growth speed of embodiment 4 gained fibers then is considerably slower than the Saffil fiber, and tensile strength is also apparently higher than the Saffil fiber.At present, the performance of Saffil fiber and quality are generally acknowledged that by international therefore, fiber provided by the present invention is a kind of more satisfactory siliceous complex fiber material.
By embodiment 2 as seen, add the intensity that small amounts magnesium can improve compound aluminium oxide fibre.
By embodiment 3 as seen, resulting fiber under lower maturing temperature, its specific surface area is big, is a kind of porous material, is specially adapted to the carrier as the catalyzer of diffusion controlled reaction.
Table compound aluminium oxide fibre performance relatively
＊
Project implementation example 1 embodiment 2 embodiment 3 embodiment 4 embodiment 5 SAEFIL
Fiber
Fibrous 5
5 5 7 5 5
(SiO
2)/(Al
2O
3) heavy % (MgO0.5)/(Al
2O
3)
Mean diameter
2～4 2～4 2～4 2～4 3～5 3
μ
Slag ball content
% 2.4 2.0 2.4 2.3 2.5 1.9
Crystallization phases δ, θ η δ, θ δ, θ θ, α
Average crystal grain
240 67 190 248 542
- d（
）
Specific surface
65
Rice
2/ gram
Fibrefelt
Tensile strength 10.3 25.6 37 20 10.8 9.8
Newton/gram sample
Linear shrinkage ratio
% 1.1 1.2 1.1 1.8
* the SAFFIL fiber is Britain's business men product sapphire whisker, handles through 1300 ℃ of calcinations half an hour.
Claims (5)
1, a kind of preparation method of compound aluminium oxide fibre may further comprise the steps:
(1) AlCl, 6H
2O, metallic aluminium and water or metallic aluminium, hydrochloric acid and water reflux temperature are 30～110 ℃ and refluxed 15～120 hours down, obtain the chlorine oxygen aluminium colloidal sol of Al/Cl (atomic ratio)=1.5～2.1 after filtration,
(2) add spinning-aid agent, silicide, a small amount of defoamer in the above-mentioned chlorine oxygen aluminium colloidal sol for preparing, then through the concentrated spinning solution that obtains having certain viscosity,
(3) above-mentioned spinning solution becomes fibre to make the compound aluminium oxide fibre precursor,
(4) thermal treatment of composite alumina precursor,
It is characterized in that:
(1) spinning solution is prepared as follows:
A) in the chlorine oxygen aluminium colloidal sol of the Al/Cl=1.5 for preparing～2.1, add Al in this aluminium colloidal sol earlier
2O
32～10% mean polymerisation degree of weight is 1000～3000, and alcoholysis degree is 80～98% polyvinyl alcohol spinning-aid agent, and the concentration of polyvinyl alcohol solution is 1～5%,
B) add 0.1～1.5% (with Al in the above-mentioned spinning solution
2O
3Weight is benchmark) defoamer C
2～C
8Alcohol,
C) add in the above-mentioned aluminium colloidal sol that contains spinning-aid agent with the fresh silicon sol that hydrolysis obtains in the presence of hydrochloric acid and water of the tetraethoxy after the alcohol dissolving, being concentrated into viscosity then is 10～50 pools, and the proportioning of adjustment silicon sol and aluminium colloidal sol makes SiO in the spinning solution of gained
8/ Al
2O
3(weight) is 3～15%,
(2) said one-tenth method for fiber is a blowing process: with the above-mentioned spinning solution that is concentrated into 10～50 pools (20 ℃ time), put into the liquid tank of band shower nozzle after the filtration, liquid stream that sprays by at least one nozzle under pressurized air pushes and the high velocity air that sprays from least one gas jet are 25～40 ℃ of room temperatures, relative humidity be 40～80% times and stream jet the compound aluminium oxide fibre precursor
(3) the compound aluminium oxide fibre precursor of winding-up gained toasted 20～30 minutes down at 60～100 ℃ earlier, low temperature (300 ℃～400 ℃) was handled 15～30 minutes under water vapour atmosphere then, high temperature (850～1300 ℃) roasting 20～40 minutes under oxidizing atmosphere at last.
2, the preparation method of compound aluminium oxide fibre as claimed in claim 1 when it is characterized in that preparing spinning solution, should add Al in the aluminium colloidal sol earlier in chlorine oxygen aluminium colloidal sol
2O
36～8% alcoholysis degree of weight is 88%, and the polymerization degree is 17.50 ± 50 polyvinyl alcohol spinning-aid agent.
3, the preparation method of compound aluminium oxide fibre as claimed in claim 1 is characterized in that SiO in the said spinning solution
2/ Al
2O
3(weight) is 5～8%.
4, the preparation method of compound aluminium oxide fibre as claimed in claim 1 is characterized in that said defoamer is an isopropylcarbinol.
5, the preparation method of compound aluminium oxide fibre as claimed in claim 1 is characterized in that adding 0.2～5%(again with Al in addition in the spinning solution
2O
3Weight is benchmark) MgO.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 87101912 CN1014043B (en) | 1987-03-13 | 1987-03-13 | Method for preparing compound aluminium oxide fibre |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 87101912 CN1014043B (en) | 1987-03-13 | 1987-03-13 | Method for preparing compound aluminium oxide fibre |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1035479A CN1035479A (en) | 1989-09-13 |
| CN1014043B true CN1014043B (en) | 1991-09-25 |
Family
ID=4813679
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 87101912 Expired CN1014043B (en) | 1987-03-13 | 1987-03-13 | Method for preparing compound aluminium oxide fibre |
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| Country | Link |
|---|---|
| CN (1) | CN1014043B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100405030C (en) * | 2004-02-19 | 2008-07-23 | 德清县延炜耐火材料厂 | Splash-proof tube (Vagcor) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1059000C (en) * | 1998-05-22 | 2000-11-29 | 中国科学院山西煤炭化学研究所 | Process for preparing Al2O3-SiO2 compound fibre |
| CN1059001C (en) * | 1998-05-22 | 2000-11-29 | 中国科学院山西煤炭化学研究所 | Process for preparing spinning liquid as precursor of Al2O3-SiO2 compound fibre |
| EP2034151B1 (en) * | 2001-05-25 | 2015-02-25 | Ibiden Co., Ltd. | Holding seal material and manufacturing method thereof |
| CN101185817B (en) * | 2007-12-12 | 2010-12-08 | 天津工业大学 | Method for preparing nano alumina fiber film material |
| CN106350899B (en) * | 2016-08-24 | 2019-01-11 | 南京理工大学 | A kind of preparation method of hollow aluminum fiber |
| CN109133075B (en) * | 2018-08-31 | 2020-09-15 | 贺州市骏鑫矿产品有限责任公司 | Production method of potassium feldspar |
| CN109825899B (en) * | 2019-03-05 | 2021-06-25 | 山东大学 | Method for directly preparing mesoporous silicon-magnesium composite oxide fiber through electrostatic spinning |
| CN110078486A (en) * | 2019-04-29 | 2019-08-02 | 江苏辉迈粉体科技有限公司 | A kind of preparation method of quartz fibre |
| CN113862832A (en) * | 2021-11-11 | 2021-12-31 | 国装新材料技术(江苏)有限公司 | Continuous alumina fiber, preparation method thereof and heat-insulation protective fabric |
-
1987
- 1987-03-13 CN CN 87101912 patent/CN1014043B/en not_active Expired
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100405030C (en) * | 2004-02-19 | 2008-07-23 | 德清县延炜耐火材料厂 | Splash-proof tube (Vagcor) |
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| Publication number | Publication date |
|---|---|
| CN1035479A (en) | 1989-09-13 |
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