CN1236832A - Process for preparing Al2O3-SiO2 compound fibre - Google Patents

Process for preparing Al2O3-SiO2 compound fibre Download PDF

Info

Publication number
CN1236832A
CN1236832A CN 98109101 CN98109101A CN1236832A CN 1236832 A CN1236832 A CN 1236832A CN 98109101 CN98109101 CN 98109101 CN 98109101 A CN98109101 A CN 98109101A CN 1236832 A CN1236832 A CN 1236832A
Authority
CN
China
Prior art keywords
fibre
spinning solution
alcohol
colloidal sol
spinning
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN 98109101
Other languages
Chinese (zh)
Other versions
CN1059000C (en
Inventor
温月芳
王浩静
王心葵
孙小金
李清
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shanxi Institute of Coal Chemistry of CAS
Original Assignee
Shanxi Institute of Coal Chemistry of CAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shanxi Institute of Coal Chemistry of CAS filed Critical Shanxi Institute of Coal Chemistry of CAS
Priority to CN98109101A priority Critical patent/CN1059000C/en
Publication of CN1236832A publication Critical patent/CN1236832A/en
Application granted granted Critical
Publication of CN1059000C publication Critical patent/CN1059000C/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Abstract

A process for preparing Al2O3-SiO2 compound fibre features that under the existance of organic solvent, the ethyl n-silicate is hydrolyzed by using aluminium sol with polymer structure as acidic catalyst source and water source to obtain spinning liquor whose main component is compound Si-Al solution. Said spinning liquor features high stability, transparency and flowability, simple preparing process, easy operation and high mechanical and high temp performance of Al2O3-SiO2 compound fibre.

Description

A kind of Al 2O 3-SiO 2The preparation method of composite fibre
The invention belongs to the preparation method of inorganic composite fiber, relate in particular to a kind of Al 2O 3-SiO 2The preparation method of composite fibre.
In the pure alumina fiber, introduce SiO 2Composition can slow down or prevent α-Al well 2O 3The growth of crystal grain, thus reach the purpose that improves alumina fibre mechanical performance and high-temperature behavior, known by people.But it is relatively more difficult usually to add silicide in the alumina fibre presoma.Add organosilicon, be difficult to dissolving; Add inorganic silicon, very easy formation gel.So how to prepare to be suitable for spray silk stable, homogeneous, and the aluminium silicon spinning solution of good fluidity becomes the important step of preparation high-performance alumina fibre.Bp1,445,331 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, therefore, be difficult to apply, day public clear 55-20339 has proposed a kind of with the preparation method of waterglass as the clad aluminum colloidal sol in silicon source, this method is that common waterglass is added the sulfuric acid neutralization, control pH=2-4 placed 12-24 hour, made the silicon gel.Water flush away sodium ion then.This moisture silicon gel is broken into the fine particle of 15-50 μ, under condition of stirring, is distributed in the aluminium colloidal sol, make silicon-aluminum containing colloidal sol.This is that spinning solution is prepared in the silicon source with waterglass, and technology is very complicated, and is not easy to operate.CN10354 79A discloses and has a kind ofly made fresh Ludox with ethyl orthosilicate hydrolysis under hydrochloric acid catalysis, adds the method that the aluminium colloidal sol that contains spinning-aid agent prepares spinning solution.Concrete grammar is, at first spinning-aid agent is added in the polymeric aluminum colloidal sol, then with ethyl orthosilicate in the presence of ethanol, hydrochloric acid is made catalyst, hydrolysis makes fresh Ludox, carries out physical mixed with the above-mentioned polymeric aluminum colloidal sol that contains spinning-aid agent for preparing again, is mixed with spinning solution thus.This method technological operation harshness, condition have discomfort slightly, be easy to generate thixotroping and gel, can't become fine, the spinning solution poor stability, viscosity rises in becoming fine process always, causes the fiber thickness inequality, and owing to the aluminium colloidal sol and the prepared fresh Ludox viscosity that contain spinning-aid agent are all bigger, be unfavorable for the even mixing of two components, promptly silicide is difficult for being uniformly dispersed.In addition, make catalyst, can introduce Cl with HCl -Therefore ion influences the finished fiber quality.
It is even that goal of the invention of the present invention provides a kind of siliceous spinning solution, stable, good fluidity and easy to operate Al 2O 3-SiO 2The preparation method of composite fibre.
Al provided by the invention 2O 3-SiO 2The preparation method of composite fibre comprises the steps:
1.AlCl 36H 2O, metallic aluminium and distilled water under 60-110 ℃ temperature backflow 4-40 hour obtain Al/Cl (mol ratio)=1.5-2.2 after filtration, and polymeric aluminum content is the chlorine oxygen aluminium colloidal sol of the paradigmatic structure of 50-95%;
2. with the chlorine oxygen aluminium colloidal sol of the above-mentioned paradigmatic structure for preparing, silicide, organic solvent and spinning-aid agent obtain spinning solution with certain viscosity through concentrating;
3. spinning solution vacuum removal bubble;
4. the spinning solution that removes behind the bubble becomes fibre to make gelatinous fibre;
5. gelatinous fibre heat treatment is made the compound silica aluminum fiber that adds.
It is characterized in that:
1. spinning solution is prepared by the following method:
A. with Al/Cl (the mol ratio)=1.5-2.2 for preparing, polymeric aluminum content is chlorine oxygen aluminium colloidal sol, ethyl orthosilicate, the alcohol of the paradigmatic structure of 50-95%, presses Al: Si=(5-100): 1 (mol ratio); Alcohol: ethyl orthosilicate=(5-30): 1 (mol ratio) proportioning, under 30-90 ℃ temperature backflow 0.5-40 hour, filter and obtain the compound silicon-aluminum sol that adds;
B. at the compound 10-20% that adds Al weight in this colloidal sol in the silicon-aluminum sol that adds, average degree of polymerization is 1000-3000, and alcoholysis degree is 80-98%, and concentration is the poly-vinyl alcohol solution of 8-10%, and being concentrated into viscosity then is the spinning solution of 15-90 pool;
2. the fine blowing process that adopts on device for spinning of described one-tenth realizes;
3. gelatinous fibre is at 60-100 ℃ of following baking 20-50min, under steam atmosphere, temperature are 200-400 ℃ condition, handles 1-3 hour then, and at last at air atmosphere, temperature is under 850-1400 ℃ the condition, processing 10-50min.
Aforesaid alcohol is C 1-C 4Alcohol, preferably methyl alcohol, ethanol, ethylene glycol, isopropyl alcohol.
The present invention uses the aluminium colloidal sol of paradigmatic structure as acidic catalyst source and water source in the presence of organic solvent with ethyl orthosilicate, hydrolysis makes the compound preparation of spinning solution new technology that silicon-aluminum sol is a main component that adds, the gained spinning solution is stable, transparent, good fluidity, preparing process is simple, and is easy to operate, compare with soluble glass method, saved numerous and diverse gel, washing, therefore operations such as fragmentation, have been simplified and have been added silicon technology, be beneficial to production, compare with ethyl orthosilicate hydrochloric acid hydrolysis method, avoided in adding the silicon process, introducing the chlorine atom, and because the introducing of silicon is to adopt the method for chemical reaction to realize, so the degree of mixing of sial can reach the atom level mixed-level, has advantage simple to operate simultaneously, with the hydrochloric acid hydrolysis method of this method replacement ethyl orthosilicate, the stability of spinning solution, flowability significantly improves, and has guaranteed Al 2O 3-SiO 2The mechanical property of composite fibre and high-temperature behavior.
Embodiment 1
1.120 gram AlCl 36H 2O (analyzing pure), 500 gram distilled water, 100 gram metal aluminium flakes (purity＞99.5%) add in the there-necked flask of 1000ml successively, are 97 ℃ at reflux temperature and reflux 6 hours down, filtration obtains Al/Cl=2.01, and polymeric aluminum content is 86% paradigmatic structure chlorine oxygen aluminum solutions;
2. get 15 gram ethanol, 7.6 gram ethyl orthosilicates, the above-mentioned paradigmatic structure chlorine oxygen aluminium colloidal sol for preparing 200 grams add successively and have in the 500ml there-necked flask of agitating device, reflux 2 hours down at 50 ℃, filter transparently and add silicon clad aluminum colloidal sol;
3. add in the silicon composite sol above-mentioned that to add 35 gram concentration be 10%, the trade mark is 1788 polyvinyl alcohol, stirs down at 60 ℃ and is concentrated into the spinning solution that viscosity is 20 pools (20 ℃);
4. above-mentioned spinning solution normal temperature under vacuum condition outgased 1 hour;
5. on device for spinning, jet to such an extent that add silicon plural gel fiber;
6. the silicon plural gel fiber that adds with above-mentioned winding-up gained toasted 20 minutes down at 80 ℃, handled 2 hours in 360 ℃ the low temperature oven that is connected with water vapour then, at last 950 ℃ of following roastings 40 minutes, got Al 2O 3-SiO 2Composite fibre, fibre property sees Table 1.
Embodiment 2
With embodiment 1 gained Al 2O 3-SiO 2Fiber was 1200 ℃ of following roastings 50 minutes, and the gained fibre property sees Table 1.
Embodiment 3
Al with embodiment 1 gained 2O 3-SiO 2Composite fibre is 1300 ℃ of following roasting half an hour, and the gained fibre property sees Table 1.
Embodiment 4
1. with 120 gram AlCl 36H 2O (analyzing pure), 576 gram distilled water, 120 gram metal aluminium flakes (purity)＞99.5%) add successively in the 1000ml there-necked flask, refluxed 10 hours down at 95 ℃, Al/Cl=2.15 polymeric aluminum content is 89% paradigmatic structure aluminium colloidal sol;
2. get 40 gram ethylene glycol, 22.14 gram ethyl orthosilicates, aluminium colloidal sol 200 gram of above-mentioned paradigmatic structure adds successively and has in the 500ml there-necked flask of agitating device, refluxes 5 hours down at 80 ℃, filters transparently and adds silicon clad aluminum colloidal sol;
3. adding 42 gram concentration are 10% in the silicon clad aluminum solution in above-mentioned adding of preparing, and the trade mark is 1788 polyvinyl alcohol, stirs down at 60 ℃ and is concentrated into the spinning solution that viscosity is 20 pools (20 ℃);
4. above-mentioned spinning solution outgased 1 hour under vacuum condition;
5. the spinning solution after the degassing is jetted to such an extent that add silicon plural gel fiber on device for spinning;
6. above-mentioned winding-up obtains add silicon plural gel fiber and heat-treat by embodiment 1 heat treatment step after, again 1300 ℃ of following roastings 30 minutes, Al 2O 3-SiO 2Composite fibre, fibre property sees Table 1.
Embodiment 5
1. with 120 gram AlCl 36H 2O (analyzing pure), 600 the gram distilled water, 60 the gram metal aluminium flakes (purity)＞99.5%) add successively in the 1000ml there-necked flask, 80 ℃ the reaction 25 hours, filter Al/Cl=1.6, polymeric aluminum content is 57% paradigmatic structure aluminium colloidal sol;
2. get ethyl orthosilicate 3.29 gram, ethanol 10 grams, aluminium colloidal sol 200 grams of the above-mentioned paradigmatic structure for preparing add 500ml successively and have in the there-necked flask of agitating device, are 85 ℃ at reflux temperature and reflux 2 hours down, filter transparently and add silicon clad aluminum colloidal sol;
3. above-mentioned 1788 polyvinyl alcohol, 25 grams that add silicon clad aluminum colloidal sol adding concentration 10% that prepare are concentrated into the spinning solution that viscosity is 20 pools (20 ℃) at 60 ℃;
4. the above-mentioned spinning solution for preparing outgased 1 hour under vacuum condition;
5. on device for spinning, jet gelatinous fibre;
6. above-mentioned gelatinous fibre by embodiment 1 heat treatment step handle Al 2O 3-SiO 2Composite fibre, fibre property sees Table 1.
Example example 6
(pressing the method preparation of CN 1035479A)
1. get 120.7 gram AlCl 36H 2O 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 reflux, refluxed 24 hours down, filter the chlorine oxygen aluminium colloidal sol that obtains Al/Cl=2.0 then in 100 ℃;
2. adding 300 gram concentration and be 3% alcoholysis degree in above-mentioned aluminium colloidal sol is 88%, and average degree of polymerization is 1750 ± 50 polyvinyl alcohol, adds the 0.8ml isobutanol again;
3. get 26.5 gram ethyl orthosilicates and restrain ethanol stirring and dissolving a little, drip hydrochloric acid 0.5 gram of 6N, and add 20ml distilled water, obtain fresh Ludox through hydrolysis in about 10 minutes with 6.5;
4. fresh Ludox is poured in the above-mentioned aluminium colloidal sol into 18 pools when under 85 ℃, being concentrated into viscosity then and being 20 ℃ under stirring condition;
5. on device for spinning, spray Si Dejia silicon plural gel fiber;
6. will spray the gelatinous fibre of silk gained, earlier 60 ℃ of following roastings 30 minutes, in 340 ℃ the processing stove that contains water vapour, handled 20 minutes then, obtain the compound aluminium oxide fibre of green and brown look, obtained siliceous alumina fibre in 30 minutes 1300 ℃ of following roastings at last.Fibre property sees Table 1.
Embodiment 7
By embodiment 6 make after steam treatment and the siliceous alumina fibre that obtained in 30 minutes 850 ℃ of following roastings of compound aluminium oxide fibre.Fibre property sees Table 1.
Table 1 fibre property
Project Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Embodiment 6 Embodiment 7
Fibre composition Al 2O 3-SiO 2(weight ratio) ?100∶5 ?100∶5 ?100∶5 ?100∶15 ?100∶3 ?100∶5 ?100∶5
Average diameter (μ) ????3 ????3 ????3 ????3 ????3 ????2-4 ????2-4
Crystalline phase ????γ ????δγ ????δθ ????δθ ????θα ????δθ ????η
Average crystal grain d (A) ????80 ????140 ????190 ????170 ????390 ????240 ????67
Fibrofelt tensile strength (newton/gram sample) ????40 ????35 ????29 ????20 ????18 ????10.3 ????37
Apparent Good Good Good Good Good Generally Good
The explanation of tabulated data method of testing:
1. X---ray diffraction method records the employing of the average crystal grain of crystalline phase size.
2. average diameter: adopting multiplication factor is the diameter that 1000 times south of the River XSX-2 phase contrast biomicroscope is directly measured every fiber, and the arithmetic mean of instantaneous value of 100 fibre diameters is the average diameter of fiber.
3. alumina fiber blanket tensile strength is carried out on " fibrofelt draws anti-intensity measuring device " designed voluntarily.

Claims (3)

1. Al 2O 3-SiO 2Composite fibre, the preparation method comprises the steps:
(1) AlCl 36H 2O, metallic aluminium and distilled water under 60-110 ℃ temperature backflow 4-40 hour obtain Al/Cl (mol ratio)=1.5-2.2 after filtration, and polymeric aluminum content is the chlorine oxygen aluminium colloidal sol of the paradigmatic structure of 50-95%;
(2) with the chlorine oxygen aluminium colloidal sol of the above-mentioned paradigmatic structure for preparing, silicide, organic solvent and spinning-aid agent are through concentrating the spinning solution that obtains having certain viscosity;
(3) spinning solution vacuum removal bubble;
(4) spinning solution that removes behind the bubble becomes fibre to make gelatinous fibre;
(5) gelatinous fibre heat treatment is made the compound silica aluminum fiber that adds.
It is characterized in that:
(1) spinning solution is prepared by the following method:
A. with Al/Cl (the mol ratio)=1.5-2.2 for preparing, polymeric aluminum content is chlorine oxygen aluminium colloidal sol, ethyl orthosilicate, the alcohol of the paradigmatic structure of 50-95%, presses Al: Si=(5-100): 1 (mol ratio); Ethanol: ethyl orthosilicate=(5-30): 1 (mol ratio) proportioning, under 30-90 ℃ temperature backflow 0.5-40 hour, filter and obtain the compound silicon-aluminum sol that adds;
B. at the compound 10-20% that adds Al weight in this colloidal sol in the silicon-aluminum sol that adds, average degree of polymerization is 1000-3000, and alcoholysis degree is 80-98%, and concentration is the poly-vinyl alcohol solution of 8-10%, and being concentrated into viscosity then is the spinning solution of 15-90 pool;
(2) the fine blowing process that adopts on device for spinning of described one-tenth realizes;
(3) gelatinous fibre is at 60-100 ℃ of following baking 20-50min, under steam atmosphere, temperature are 200-400 ℃ condition, handles 1-3 hour then, and at last at air atmosphere, temperature is under 850-1400 ℃ the condition, processing 10-50min.
2. a kind of Al according to claim 1 2O 3-SiO 2The preparation method of composite fibre is characterized in that described alcohol is C 1-C 4Alcohol.
3. a kind of Al according to claim 1 2O 3-SiO 2The preparation method of composite fibre is characterized in that described alcohol preferably methyl alcohol, ethanol, ethylene glycol, isopropyl alcohol.
CN98109101A 1998-05-22 1998-05-22 Process for preparing Al2O3-SiO2 compound fibre Expired - Fee Related CN1059000C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN98109101A CN1059000C (en) 1998-05-22 1998-05-22 Process for preparing Al2O3-SiO2 compound fibre

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN98109101A CN1059000C (en) 1998-05-22 1998-05-22 Process for preparing Al2O3-SiO2 compound fibre

Publications (2)

Publication Number Publication Date
CN1236832A true CN1236832A (en) 1999-12-01
CN1059000C CN1059000C (en) 2000-11-29

Family

ID=5219896

Family Applications (1)

Application Number Title Priority Date Filing Date
CN98109101A Expired - Fee Related CN1059000C (en) 1998-05-22 1998-05-22 Process for preparing Al2O3-SiO2 compound fibre

Country Status (1)

Country Link
CN (1) CN1059000C (en)

Cited By (12)

* Cited by examiner, † Cited by third party
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)
CN101213330B (en) * 2005-05-31 2012-06-06 帝人株式会社 Ceramic fibre and manufacturing method thereof
CN101381225B (en) * 2008-10-10 2013-04-24 厦门大学 Continuous aluminium oxide base ceramic fibre preparation method
CN104005115A (en) * 2014-06-17 2014-08-27 山东大学 Method for preparing aluminum oxide ceramic fibers
CN104169476A (en) * 2012-01-31 2014-11-26 霓佳斯株式会社 Inorganic fiber and process for manufacturing same
CN105603578A (en) * 2015-12-31 2016-05-25 东华大学 Method for preparing high-specific-surface-area continuous SiO2 porous fiber through natural drying method
CN105603577A (en) * 2015-12-31 2016-05-25 东华大学 Method for preparing continuous SiO2/nanocrystalline metal aerogel fiber with catalytic performance by adding nanocrystalline metal in situ
CN108539147A (en) * 2018-03-21 2018-09-14 同济大学 A kind of preparation method and application of lithium ion battery negative material SiO@Al@C
CN108585948A (en) * 2018-03-19 2018-09-28 山东大学 A kind of method that aluminium oxide base ceramic fibre surface is modified
CN109023591A (en) * 2018-10-11 2018-12-18 厦门大学 A kind of α-Al2O3The preparation method of continuous fiber
CN111139552A (en) * 2020-01-14 2020-05-12 山东鲁阳浩特高技术纤维有限公司 Preparation method of alumina short fiber
CN111304917A (en) * 2020-04-13 2020-06-19 江苏鼎峰石油科技有限公司 Amphiphilic high-temperature-resistant silicon-based fiber plugging agent and preparation method thereof

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5423727A (en) * 1977-07-22 1979-02-22 Toshiba Monofrax Production of polycrystalline oxidized fiber
CN1014043B (en) * 1987-03-13 1991-09-25 中国科学院山西煤炭化学研究所 Method for preparing compound aluminium oxide fibre
CN1022619C (en) * 1988-01-16 1993-11-03 湖南省陶瓷研究所 Albite porcelain
JPH10243375A (en) * 1997-03-03 1998-09-11 Hitachi Ltd System for selecting program

Cited By (18)

* Cited by examiner, † Cited by third party
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)
CN101213330B (en) * 2005-05-31 2012-06-06 帝人株式会社 Ceramic fibre and manufacturing method thereof
CN101381225B (en) * 2008-10-10 2013-04-24 厦门大学 Continuous aluminium oxide base ceramic fibre preparation method
CN104169476A (en) * 2012-01-31 2014-11-26 霓佳斯株式会社 Inorganic fiber and process for manufacturing same
US9302947B2 (en) 2012-01-31 2016-04-05 Nichias Corporation Inorganic fiber and process for manufacturing same
CN104169476B (en) * 2012-01-31 2016-10-05 霓佳斯株式会社 Inorfil and manufacture method thereof
CN104005115A (en) * 2014-06-17 2014-08-27 山东大学 Method for preparing aluminum oxide ceramic fibers
CN104005115B (en) * 2014-06-17 2016-05-04 山东大学 A kind of preparation method of ceramic alumina fiber
CN105603577A (en) * 2015-12-31 2016-05-25 东华大学 Method for preparing continuous SiO2/nanocrystalline metal aerogel fiber with catalytic performance by adding nanocrystalline metal in situ
CN105603578A (en) * 2015-12-31 2016-05-25 东华大学 Method for preparing high-specific-surface-area continuous SiO2 porous fiber through natural drying method
CN108585948A (en) * 2018-03-19 2018-09-28 山东大学 A kind of method that aluminium oxide base ceramic fibre surface is modified
CN108539147A (en) * 2018-03-21 2018-09-14 同济大学 A kind of preparation method and application of lithium ion battery negative material SiO@Al@C
CN108539147B (en) * 2018-03-21 2021-01-12 同济大学 Preparation method and application of lithium ion battery negative electrode material SiO @ Al @ C
CN109023591A (en) * 2018-10-11 2018-12-18 厦门大学 A kind of α-Al2O3The preparation method of continuous fiber
CN111139552A (en) * 2020-01-14 2020-05-12 山东鲁阳浩特高技术纤维有限公司 Preparation method of alumina short fiber
CN111139552B (en) * 2020-01-14 2022-07-22 山东鲁阳浩特高技术纤维有限公司 Preparation method of alumina short fiber
CN111304917A (en) * 2020-04-13 2020-06-19 江苏鼎峰石油科技有限公司 Amphiphilic high-temperature-resistant silicon-based fiber plugging agent and preparation method thereof
CN111304917B (en) * 2020-04-13 2022-05-27 江苏鼎峰石油科技有限公司 Amphiphilic high-temperature-resistant silicon-based fiber plugging agent and preparation method thereof

Also Published As

Publication number Publication date
CN1059000C (en) 2000-11-29

Similar Documents

Publication Publication Date Title
CN1059000C (en) Process for preparing Al2O3-SiO2 compound fibre
CN1101725C (en) Method for producing organically modified, permanently hydrophobic aerogels
CN102875811A (en) Preparation method for phenyl vinyl MQ silicone resin
CN1699166A (en) Nano organic solvent silicasol and preparation method thereof
CN113999397B (en) Preparation method and application of low-cost liquid polycarbosilane
CN108484963A (en) A kind of atmosphere pressure desiccation prepares the method for phenolic aldehyde aeroge and phenolic aldehyde aeroge obtained
CN1172937C (en) Process for preparingsilicon oligomer solution and organopolysiloxane film formed from the solution
CN1232435A (en) Process for producing organically modified aerogels
US20060216219A1 (en) Aerogel monolith with improved strength
JP2000264620A (en) Production of hydrophobic aerogel
CN1120801C (en) Dual-pore molecular sieve and its preparing process
CN1092143C (en) Process for synthesizing hydrophobic medium porous molecular sieve
CN1014043B (en) Method for preparing compound aluminium oxide fibre
CN1759135A (en) Organic siloxane resins and insulating film using the same
CN111153481A (en) Preparation method and application of covalent bond type silicon-aluminum flocculating agent
CN1059001C (en) Process for preparing spinning liquid as precursor of Al2O3-SiO2 compound fibre
CN1115308C (en) Method for fabricating silica glass
CN1208248C (en) Preparation method of mesopore aluminium containing molecular sieve
CN1796278A (en) Method for preparing silicon-aluminum molecular sieve in EUO structure
CN1246224C (en) Preparation method of high titanium content mesoppore molecular sieve
CN1765903A (en) Epoxy-silsesquioxanes preparation method
CN115215348B (en) Preparation method of vermicular mesoporous silica
CN115073958B (en) Paint additive with antibacterial and antiviral functions and preparation method and application thereof
CN1257948C (en) Organic-inorganic hybrid paint and its preparing method
CN116102977B (en) Transparent hydrophilic anti-fog coating with silicon-doped carbonized polymer dots as construction elements and preparation method thereof

Legal Events

Date Code Title Description
C06 Publication
C10 Entry into substantive examination
PB01 Publication
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
C19 Lapse of patent right due to non-payment of the annual fee
CF01 Termination of patent right due to non-payment of annual fee
REG Reference to a national code

Ref country code: HK

Ref legal event code: GR

Ref document number: 1039287

Country of ref document: HK