CA2287849A1 - Method for granulating aerogels - Google Patents
Method for granulating aerogels Download PDFInfo
- Publication number
- CA2287849A1 CA2287849A1 CA002287849A CA2287849A CA2287849A1 CA 2287849 A1 CA2287849 A1 CA 2287849A1 CA 002287849 A CA002287849 A CA 002287849A CA 2287849 A CA2287849 A CA 2287849A CA 2287849 A1 CA2287849 A1 CA 2287849A1
- Authority
- CA
- Canada
- Prior art keywords
- aerogels
- aerogel particles
- agglomerates
- mixing apparatus
- gel
- 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.)
- Abandoned
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/14—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic in rotating dishes or pans
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/16—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by suspending the powder material in a gas, e.g. in fluidised beds or as a falling curtain
Abstract
The invention relates to a method for agglomerating aerogel particles.
According to said method, the aerogel particles are placed in a mixing device and mixed thoroughly, a binding agent also being added to said mixing device.
According to said method, the aerogel particles are placed in a mixing device and mixed thoroughly, a binding agent also being added to said mixing device.
Description
26.Ok:T.1999 13:12 LUDERSCHMIDT, S~HUELER & PAPTI'IER ~IR.437 S.18: 35 r ' , ' The object of the present invention is a method of granulating aerogcls.
Auogels, particularly those with a porosity above 60% and a density of less rhea 0.6 glcu.cm display extremely tow thermal conductivity and are therefore used as a heat ink material, as is described in EP-A-0 171 722, as catalysts or as catalyse tamers wd also as adsorption material Fuztbettnore, by virtue of their very low refraction index for solid substances, it is known >'o use them for Cerenkov detectors.
runhermore, by i. ~ reason of Their pazvcular acoustic impedance, the literature describes a possible use as an l; , ~mpedance sulaptazion means, for example in the ultrasound range.
i;
It is also possible for them to be used as carriers for effective substances is pharmacy or agriculture.
Aerogds in the Broader sense, e.g in the sense of "gel with air as the dispersion agent"
are produced by the drying of a suitable gel. The term "aerogel" in this sense ~nbraces aerogels .in the narrower sense, xerogels and cryogds in this respect, a dried gel is ' termed an aerogel in the narrower sense when the liquid of the gel is eliminated at above critical temperature and starting from pressures above critical prescwe. On the other band, if the liquid is elitnmated from the gel under sub~ritical conditions, for example with ' the formation of a liquidlfavour interphase, then the resuhing gel is frequently referred to also as a xerogel When the term aerogels is used in the present invention, these ate acrogels in the broader sense, i.e. in the sense of "gel with air as the dispersion medium".
The term does sot include a~erogels la~own from eaters literature and which are obtainrd for example by precipitation of silicic add (e.g DE 3025437, DD 29b 898) or which occur as pyrogenic silicie acid, e.g. Aerosil"~. Iu these cases, during manufacture, na three-dimensional gel lattice develops which is homogeneous over relatively great distances.
i 25.Ok.T. 1999 i3~ 13 ~uDERSi_HroIDT, SrHUE~ER & PARTrIER r~aR.49' S. 19135 r I~ ' Where aerogels are concerned, it 15 possible basically to difherentiate betweea inorganic and organic aerogels.
lnorg~ic aezogds have already been known since 1931 (S. S. Kistler, Nature 1931, I27, 741 ). Since then, aerngels have been fortltcotntng firotn vanOa9 starting materials. In this respect, for example SiOz-, AhOg-, 'I~Or, ZrOs-, SnO~ , L.i:4-, Ceps-, V~Graerogels and mixtures of these were producal (Ii D. Gasser, P. C. Goswami, Chern Rev, 1989, B9, 765 et seq.) for some yeats~ organic artogels have also been laaown which are derived from the most yvidely diverse starti~ rnntaials, e.g. melamine formaldehyde (R. W. Pekala,1.
Mater, a ' ~~ ' ~Sci. 19$9, 24, 3221).
.
i , T.norganic aerogels can thereby be produced in different ways.
On the one baud, SiOZ aerogels can for exausple be pmdttced by acid hydrolysis and I canda~sation oftara-ethyl arrhosilicau in ethanol. During this process, s gel is produced which oan be dried by super-critical drying while its swcture is maintained.
Production m~Khods based nn this drying technique are known for example froru EP-A-0 336 076, WO 92103378 or WO 95106617.
The high pressure technique involved itt the super-critical drying of aerogels is however d I
an expensive process and involves a high security risk. Ia addition, however, super-I~ ' i critical drying of aerogels is a very cost-intensive pmduction method.
I
(i Air alterntwive to super-ethical drying is afforded by a ttiethod for the sub-critical drying I of Si41 gels.
i ' The costs involved in aub-critical drying are substantially less by reason of the simpler technolo~r, the lower enet~r costs and the lesser security risk.
' z6.OkT. 1999 i3: i3 LUDERS~=HMIDT. SCNUELER >:~ Pc~RTrIER raR.4S~ S. 2~,'35 The SiO~ gels can for example be obtained by acid hydrolysis oftetra-alknxy silanes in a suitable organic solvent by rt~eans of water. Once the solvent has been exchanged for a I
suitable orgattie solvent, the gel obtained is in a fiutha s<ep reacted with a silylating agent.
The SiOi gel resulting from this can then, from an organic solvent, be dried in air. Thus, aerogels with densities of less than 0.4 g/cu.cm and porosities above 6o°ip can be achieved. The production method based on this drying technique is described in detail in ~10 94125149.
~i ' 4i ;I
Furthermore, the above-described gels can, prior to drying and in the alcohol-aqueous solution, be mixed with tea's-alkoxy stlanes and agcd. in order to increase the gel tattiec strength, as disclosed in WO 92IZO623.
The teCta-alkoxy silanes used as starting materials in the above-described processes do, however, likewise represent an extremely hid cost factor.
A not inconsiderable cost reduction can be achieved by using water-glass as a starting material for the production of SiOz gels To this end, it is possible for example to produce a s~1'cic and from an aqueous water-glass solution with the help of an ion exchange resin.
of eased by the additiop ofa base to produce an SiOz gel.
the silicic acid then being p ycond ~~e~ exchange of the aqueous medium for a suitable organic solvent, it is then possible f 'in a fiuther step to react the resulting gel with a silylating agrnt containing chlorine The i SiOz ge! which is surface modified for example with methyl silyl groups can then and ' ~ likewise from an organic solvent, be dried in air. The production method based on this technique is known from DE-A-43 42 548 i plternati~e methods with regard to the production of an SiOZ uerogel on a basis of water-glass with subsequent sub-critical drying are described in Gcnnasi Patent Application 195 41 715.1 and 195 41 992 8 I
Furthermore, DE-A-195 02 453 describes a use of chlorine-free silylating agents during the production of sub-critically dried aei'ogels.
'~, r 25.OKT.1999 19:13 LI_!DERSCHfIIDT, SCHIJELER x PARTfIER fIR.4.3? 5.21%3S
I.
Auogels, particularly those with a porosity above 60% and a density of less rhea 0.6 glcu.cm display extremely tow thermal conductivity and are therefore used as a heat ink material, as is described in EP-A-0 171 722, as catalysts or as catalyse tamers wd also as adsorption material Fuztbettnore, by virtue of their very low refraction index for solid substances, it is known >'o use them for Cerenkov detectors.
runhermore, by i. ~ reason of Their pazvcular acoustic impedance, the literature describes a possible use as an l; , ~mpedance sulaptazion means, for example in the ultrasound range.
i;
It is also possible for them to be used as carriers for effective substances is pharmacy or agriculture.
Aerogds in the Broader sense, e.g in the sense of "gel with air as the dispersion agent"
are produced by the drying of a suitable gel. The term "aerogel" in this sense ~nbraces aerogels .in the narrower sense, xerogels and cryogds in this respect, a dried gel is ' termed an aerogel in the narrower sense when the liquid of the gel is eliminated at above critical temperature and starting from pressures above critical prescwe. On the other band, if the liquid is elitnmated from the gel under sub~ritical conditions, for example with ' the formation of a liquidlfavour interphase, then the resuhing gel is frequently referred to also as a xerogel When the term aerogels is used in the present invention, these ate acrogels in the broader sense, i.e. in the sense of "gel with air as the dispersion medium".
The term does sot include a~erogels la~own from eaters literature and which are obtainrd for example by precipitation of silicic add (e.g DE 3025437, DD 29b 898) or which occur as pyrogenic silicie acid, e.g. Aerosil"~. Iu these cases, during manufacture, na three-dimensional gel lattice develops which is homogeneous over relatively great distances.
i 25.Ok.T. 1999 i3~ 13 ~uDERSi_HroIDT, SrHUE~ER & PARTrIER r~aR.49' S. 19135 r I~ ' Where aerogels are concerned, it 15 possible basically to difherentiate betweea inorganic and organic aerogels.
lnorg~ic aezogds have already been known since 1931 (S. S. Kistler, Nature 1931, I27, 741 ). Since then, aerngels have been fortltcotntng firotn vanOa9 starting materials. In this respect, for example SiOz-, AhOg-, 'I~Or, ZrOs-, SnO~ , L.i:4-, Ceps-, V~Graerogels and mixtures of these were producal (Ii D. Gasser, P. C. Goswami, Chern Rev, 1989, B9, 765 et seq.) for some yeats~ organic artogels have also been laaown which are derived from the most yvidely diverse starti~ rnntaials, e.g. melamine formaldehyde (R. W. Pekala,1.
Mater, a ' ~~ ' ~Sci. 19$9, 24, 3221).
.
i , T.norganic aerogels can thereby be produced in different ways.
On the one baud, SiOZ aerogels can for exausple be pmdttced by acid hydrolysis and I canda~sation oftara-ethyl arrhosilicau in ethanol. During this process, s gel is produced which oan be dried by super-critical drying while its swcture is maintained.
Production m~Khods based nn this drying technique are known for example froru EP-A-0 336 076, WO 92103378 or WO 95106617.
The high pressure technique involved itt the super-critical drying of aerogels is however d I
an expensive process and involves a high security risk. Ia addition, however, super-I~ ' i critical drying of aerogels is a very cost-intensive pmduction method.
I
(i Air alterntwive to super-ethical drying is afforded by a ttiethod for the sub-critical drying I of Si41 gels.
i ' The costs involved in aub-critical drying are substantially less by reason of the simpler technolo~r, the lower enet~r costs and the lesser security risk.
' z6.OkT. 1999 i3: i3 LUDERS~=HMIDT. SCNUELER >:~ Pc~RTrIER raR.4S~ S. 2~,'35 The SiO~ gels can for example be obtained by acid hydrolysis oftetra-alknxy silanes in a suitable organic solvent by rt~eans of water. Once the solvent has been exchanged for a I
suitable orgattie solvent, the gel obtained is in a fiutha s<ep reacted with a silylating agent.
The SiOi gel resulting from this can then, from an organic solvent, be dried in air. Thus, aerogels with densities of less than 0.4 g/cu.cm and porosities above 6o°ip can be achieved. The production method based on this drying technique is described in detail in ~10 94125149.
~i ' 4i ;I
Furthermore, the above-described gels can, prior to drying and in the alcohol-aqueous solution, be mixed with tea's-alkoxy stlanes and agcd. in order to increase the gel tattiec strength, as disclosed in WO 92IZO623.
The teCta-alkoxy silanes used as starting materials in the above-described processes do, however, likewise represent an extremely hid cost factor.
A not inconsiderable cost reduction can be achieved by using water-glass as a starting material for the production of SiOz gels To this end, it is possible for example to produce a s~1'cic and from an aqueous water-glass solution with the help of an ion exchange resin.
of eased by the additiop ofa base to produce an SiOz gel.
the silicic acid then being p ycond ~~e~ exchange of the aqueous medium for a suitable organic solvent, it is then possible f 'in a fiuther step to react the resulting gel with a silylating agrnt containing chlorine The i SiOz ge! which is surface modified for example with methyl silyl groups can then and ' ~ likewise from an organic solvent, be dried in air. The production method based on this technique is known from DE-A-43 42 548 i plternati~e methods with regard to the production of an SiOZ uerogel on a basis of water-glass with subsequent sub-critical drying are described in Gcnnasi Patent Application 195 41 715.1 and 195 41 992 8 I
Furthermore, DE-A-195 02 453 describes a use of chlorine-free silylating agents during the production of sub-critically dried aei'ogels.
'~, r 25.OKT.1999 19:13 LI_!DERSCHfIIDT, SCHIJELER x PARTfIER fIR.4.3? 5.21%3S
I.
Furthermore, an organofunctiondlisation by means of orgaaofunctionalised silylating agents in the production of sub-critically dried aerogels is described in DF-A-195 3~ I98.
However, on grounds of procedural technology and manufacturing costs, the~
production of aerogel particles on a major industrial scale is limited to particle sizes less than 5 mm a~,nd prefe~bly less than 2 mm.
y~ ~ ~ccording to the particular manner of producing the aerogets, so in prinapte a plurality I
I; ' ~f washing and solvent ~cehange stages are required Since these are diffusion-dependent, the time required is increased by the square of the radius of the gel pardcles_ v Consequently, apawrrt from the drying method, the costs of serogel production also increase quite considerably from the parade size upwards On grounds of cast, the result is an endeavour to produce the srnalJest possible aerogel particles On the other hand, the handling of very small particles is very complicated and thus likewise she costs emailed are unfavourable and nor every industrial application of aerogels is independent of the particle sue.
I
i~, Therefore, from the point of view of handling and fur many applications, larger aerogel '; ~ ' particles are needed or at least advantageous.
y ;
Therefore, the object of the present invention is to provide a method by which small I~ aerogel particles of less than 2 tom can be formed into larger aerogel particles.
I I
This problem is resolved by a method in which the aerogel particles are delivered to a moulding apparatus in which they are compressed In this way, it is particularly simple to form small aerogel panicles into larger aaogel particles.
The binder can be added to the mixing app~rtrus to prior to, during and/or after the addition of the aerogel particles, the subsequent addition beuag prtfetred.
,,, Y
ES.Ok:.T.1999 l3: la LUDER~3CH('1IDT, SCHUELER & PHRT~IER f~IR.43i 5.32%35 ~I , S
T~ ~B~ p~ucles are caused to move so that they rnjoy relative movtment in respect of one another by means of the said mixing apparatus, which is for example an agglomerating plate, a blender or a fluidised bed aryl Adva,rrtageously, the binder is incorporated as an aqueous or non-aqueous solution or suspension or even ~ a melt, for example by spraying The bitrdeT tpsutts in a drawing-tasether of the primarily provided aerogel particles to produce larger agglomerates.
Doting this process, by chemical reaction, rigidi'fication, crystallising out due to n .I ,, evaporation or vaporising of the solverJt, the binder results in a bonding of the mixture '' ~~ srOt~stituerns.
t,~
According to a further advantageous embodiment, the binder is added as a solid ~ubstanoe. Banding rhea takes place by chemical reacrion of the solid substonce with one or more components of the mixture or by the softening of a solid binding agent, e, g, by elev$ted temperatures, resulting in its becoming sticky and boAding the particles of the mixture Another expedient embodiment envisages that in addition to the aerogel particles, also additives and/ot fillers which are present in particulate or fibre form, are added to the ~, , fixing apparatus S ' ~' ' ~ accordance vuith a efe:zed embodiment a ' , , pr , th agglomerates arc separated according to their size. Advantageously, this takes place in that from the granules produced, the target i fraction is screed n~in accordance with the desired granular range_ Crranulates which are too large can possible be cotruninuted, for example with a chopper or a cutter head and screened off so that are they present in the desired ganulaz- rar;ge or may be fed back i to the agglomerating device aft cornminutioa Granules which are too small an poss~'bly be recycled to the agglomerating apparatus.
,~d E6.OKT. i~399 i3: 14 ~UDERSCHrIIDT. SCHUEUER ~ P~RTr~ER rdR. a97 S. 2:35 ,~ , ' 6 i , , ' ~, , Irs accordance with a further embodiment, tde agglomerates are dried prior to being i processed.
I
,;
.I
, ~I
,, (, a , ~ , i i ' a I
~i , ') i '
However, on grounds of procedural technology and manufacturing costs, the~
production of aerogel particles on a major industrial scale is limited to particle sizes less than 5 mm a~,nd prefe~bly less than 2 mm.
y~ ~ ~ccording to the particular manner of producing the aerogets, so in prinapte a plurality I
I; ' ~f washing and solvent ~cehange stages are required Since these are diffusion-dependent, the time required is increased by the square of the radius of the gel pardcles_ v Consequently, apawrrt from the drying method, the costs of serogel production also increase quite considerably from the parade size upwards On grounds of cast, the result is an endeavour to produce the srnalJest possible aerogel particles On the other hand, the handling of very small particles is very complicated and thus likewise she costs emailed are unfavourable and nor every industrial application of aerogels is independent of the particle sue.
I
i~, Therefore, from the point of view of handling and fur many applications, larger aerogel '; ~ ' particles are needed or at least advantageous.
y ;
Therefore, the object of the present invention is to provide a method by which small I~ aerogel particles of less than 2 tom can be formed into larger aerogel particles.
I I
This problem is resolved by a method in which the aerogel particles are delivered to a moulding apparatus in which they are compressed In this way, it is particularly simple to form small aerogel panicles into larger aaogel particles.
The binder can be added to the mixing app~rtrus to prior to, during and/or after the addition of the aerogel particles, the subsequent addition beuag prtfetred.
,,, Y
ES.Ok:.T.1999 l3: la LUDER~3CH('1IDT, SCHUELER & PHRT~IER f~IR.43i 5.32%35 ~I , S
T~ ~B~ p~ucles are caused to move so that they rnjoy relative movtment in respect of one another by means of the said mixing apparatus, which is for example an agglomerating plate, a blender or a fluidised bed aryl Adva,rrtageously, the binder is incorporated as an aqueous or non-aqueous solution or suspension or even ~ a melt, for example by spraying The bitrdeT tpsutts in a drawing-tasether of the primarily provided aerogel particles to produce larger agglomerates.
Doting this process, by chemical reaction, rigidi'fication, crystallising out due to n .I ,, evaporation or vaporising of the solverJt, the binder results in a bonding of the mixture '' ~~ srOt~stituerns.
t,~
According to a further advantageous embodiment, the binder is added as a solid ~ubstanoe. Banding rhea takes place by chemical reacrion of the solid substonce with one or more components of the mixture or by the softening of a solid binding agent, e, g, by elev$ted temperatures, resulting in its becoming sticky and boAding the particles of the mixture Another expedient embodiment envisages that in addition to the aerogel particles, also additives and/ot fillers which are present in particulate or fibre form, are added to the ~, , fixing apparatus S ' ~' ' ~ accordance vuith a efe:zed embodiment a ' , , pr , th agglomerates arc separated according to their size. Advantageously, this takes place in that from the granules produced, the target i fraction is screed n~in accordance with the desired granular range_ Crranulates which are too large can possible be cotruninuted, for example with a chopper or a cutter head and screened off so that are they present in the desired ganulaz- rar;ge or may be fed back i to the agglomerating device aft cornminutioa Granules which are too small an poss~'bly be recycled to the agglomerating apparatus.
,~d E6.OKT. i~399 i3: 14 ~UDERSCHrIIDT. SCHUEUER ~ P~RTr~ER rdR. a97 S. 2:35 ,~ , ' 6 i , , ' ~, , Irs accordance with a further embodiment, tde agglomerates are dried prior to being i processed.
I
,;
.I
, ~I
,, (, a , ~ , i i ' a I
~i , ') i '
Claims (9)
1. A method for the granulation of aerogel particles in which the aerogel particles are fed into a mixing apparatus and are thoroughly mixed and a binder is added to the mixing apparatus.
claims
claims
2. A method according to claim 1, characterised in that the aerogel particles are presented to the mixing apparatus and the binder is then added
3. A method according to claim 1 or 2, characterised in that the binder is incorporated as an aqueous of non-aqueous solution, as a suspension, as a melt or as a solid substance.
4. A method according to at least one of the preceding claims, characterised in that in addition to the aerogel particles, also additives and/or fillers are fed into the mixing apparatus.
5. A method according to at least one of the preceding claims, characterised in that the agglomerates are separated according to their size.
6. A method according to claim 5, characterised in that the agglomerates which are below the desired granular range are fed back to the mixing apparatus.
7. A method according to claim 5, characterised in that the agglomerates which are above the desired granular range are comminuted
8. A method according to claim 7, characterised in that the comminuted and/or the agglomerates which are below the desired granular range are fed to the mixing apparatus
9. A method according to at least one of the preceding claims, characterised in that the agglomerates are dried further to processing.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19718740A DE19718740A1 (en) | 1997-05-02 | 1997-05-02 | Process for the granulation of aerogels |
| DE19718740.4 | 1997-05-02 | ||
| PCT/EP1998/002519 WO1998050144A1 (en) | 1997-05-02 | 1998-04-29 | Method for granulating aerogels |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA2287849A1 true CA2287849A1 (en) | 1998-11-12 |
Family
ID=7828544
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA002287849A Abandoned CA2287849A1 (en) | 1997-05-02 | 1998-04-29 | Method for granulating aerogels |
Country Status (8)
| Country | Link |
|---|---|
| US (1) | US6481649B1 (en) |
| EP (1) | EP0979141A1 (en) |
| JP (1) | JP2001523162A (en) |
| KR (1) | KR20010012153A (en) |
| CN (1) | CN1126592C (en) |
| CA (1) | CA2287849A1 (en) |
| DE (1) | DE19718740A1 (en) |
| WO (1) | WO1998050144A1 (en) |
Families Citing this family (32)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19648798C2 (en) * | 1996-11-26 | 1998-11-19 | Hoechst Ag | Process for the production of organically modified aerogels by surface modification of the aqueous gel (without prior solvent exchange) and subsequent drying |
| US6702949B2 (en) | 1997-10-24 | 2004-03-09 | Microdiffusion, Inc. | Diffuser/emulsifier for aquaculture applications |
| US7128278B2 (en) | 1997-10-24 | 2006-10-31 | Microdiffusion, Inc. | System and method for irritating with aerated water |
| US6386751B1 (en) | 1997-10-24 | 2002-05-14 | Diffusion Dynamics, Inc. | Diffuser/emulsifier |
| US7654728B2 (en) | 1997-10-24 | 2010-02-02 | Revalesio Corporation | System and method for therapeutic application of dissolved oxygen |
| US8034749B2 (en) * | 2002-12-31 | 2011-10-11 | Baker Hughes Incorporated | Aerogels effective to reduce drilling fluid density |
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| US20060084707A1 (en) * | 2004-10-15 | 2006-04-20 | Aspen Aerogels, Inc. | Methods for manufacture of aerogels |
| WO2008044873A1 (en) * | 2006-10-10 | 2008-04-17 | Korea Institute Of Industrial Technology | Method for preparing permanently hydrophobic aerogel and permanently hydrophobic aerogel prepared by using the method |
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| MX2010011856A (en) | 2008-05-01 | 2011-02-15 | Revalesio Corp | Compositions and methods for treating digestive disorders. |
| US8815292B2 (en) | 2009-04-27 | 2014-08-26 | Revalesio Corporation | Compositions and methods for treating insulin resistance and diabetes mellitus |
| KR20130114581A (en) | 2010-05-07 | 2013-10-18 | 레발레시오 코퍼레이션 | Compositions and methods for enhancing physiological performance and recovery time |
| JP2013533320A (en) | 2010-08-12 | 2013-08-22 | レバレジオ コーポレイション | Compositions and methods for treating tauopathy |
| US8697766B2 (en) * | 2011-02-24 | 2014-04-15 | Basf Se | Process for producing pulverulent porous materials |
| EP2581216A1 (en) | 2011-10-12 | 2013-04-17 | Dow Global Technologies LLC | Panel with fire barrier |
| DE102015207939A1 (en) | 2015-04-29 | 2016-11-03 | Wacker Chemie Ag | Process for the preparation of organically modified aerogels |
| DE102015207944A1 (en) | 2015-04-29 | 2016-11-03 | Wacker Chemie Ag | Process for the preparation of organically modified aerogels |
| DE102015211812A1 (en) | 2015-06-25 | 2016-12-29 | Wacker Chemie Ag | Economical process for the production of organically modified lyo- or aerogels |
| CN108147401B (en) * | 2018-01-12 | 2019-11-15 | 昂星新型碳材料常州有限公司 | The preparation method of graphene aerogel powder |
| CN111183113B (en) | 2018-02-14 | 2023-03-24 | 株式会社Lg化学 | Method for producing hydrophobic silica aerogel particles |
| CN110077079B (en) * | 2019-05-29 | 2020-12-29 | 浙江康廷电子科技有限公司 | Composite structure of aerogel and PET (polyethylene terephthalate) base material and preparation process thereof |
| WO2023148082A1 (en) | 2022-02-03 | 2023-08-10 | Empa Eidgenössische Materialprüfungs- Und Forschungsanstalt | Binder-free bulk silica aerogel material, method of producing the same and uses thereof |
Family Cites Families (76)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE296898C (en) | ||||
| DE261581C (en) | 1912-01-17 | 1913-06-25 | Krupp Ag | Impact detonator with a delay that can be switched on and off |
| US2093454A (en) | 1934-10-01 | 1937-09-21 | Samuel S Kistler | Method of producing aerogels |
| US2385217A (en) | 1942-10-09 | 1945-09-18 | Socony Vacuum Oil Co Inc | Gel pellets |
| GB607234A (en) | 1946-01-15 | 1948-08-27 | Standard Oil Dev Co | Improved process for the preparation of gel particles |
| NL74665C (en) | 1949-04-07 | |||
| GB682574A (en) | 1950-05-04 | 1952-11-12 | Dow Corning Ltd | Improvements in or relating to silica compositions |
| US2680696A (en) | 1951-02-14 | 1954-06-08 | Du Pont | Method of esterifying the surface of a silica substrate having a reactive silanol surface |
| US2786042A (en) | 1951-11-23 | 1957-03-19 | Du Pont | Process for preparing sols of colloidal particles of reacted amorphous silica and products thereof |
| US2886460A (en) | 1954-09-14 | 1959-05-12 | Du Pont | Organophilic and hydrophilic composition |
| GB783868A (en) | 1954-10-06 | 1957-10-02 | Midland Silicones Ltd | A process of preparing hydrophobic organo-silicon powders |
| US3015645A (en) | 1954-10-06 | 1962-01-02 | Dow Corning | Silica powders |
| US2978298A (en) | 1956-09-04 | 1961-04-04 | Gen Electric | Process for producing hydrophobic aerogels |
| US3122520A (en) | 1959-10-05 | 1964-02-25 | Dow Corning | Method of making silicone rubber fillers |
| US3024126A (en) | 1960-06-15 | 1962-03-06 | Dow Corning | Method of treating reinforcing silica |
| DE1667078B2 (en) | 1967-10-31 | 1979-07-19 | W.R. Grace & Co., New York, N.Y. (V.St.A.) | Process for the preparation of spherical silica hydrogels |
| SE319161B (en) | 1968-01-30 | 1970-01-12 | Fosfatbolaget Ab | |
| US3794713A (en) | 1968-08-06 | 1974-02-26 | Nat Petro Chem | Preparation of silica gels |
| DE2103243C3 (en) | 1971-01-25 | 1979-01-11 | Basf Ag, 6700 Ludwigshafen | Process and device for the production of largely spherical, silica-containing hydrogels |
| US4101443A (en) | 1976-06-01 | 1978-07-18 | Union Carbide Corporation | Transient antifoam compositions |
| US4101442A (en) | 1976-06-01 | 1978-07-18 | Union Carbide Corporation | Non-aqueous antifoam compositions |
| US4190457A (en) | 1978-06-09 | 1980-02-26 | Phillips Petroleum Co. | Preparation of inorganic xerogels |
| CS208879B1 (en) | 1979-07-09 | 1981-10-30 | Ivan Novak | Preparation method of silicic acid xerogel with high volumen of pores |
| DE2951577A1 (en) * | 1979-12-21 | 1981-07-02 | Grünzweig + Hartmann und Glasfaser AG, 6700 Ludwigshafen | METHOD FOR PRODUCING HEAT-INSULATING BODIES AND DEVICE FOR IMPLEMENTING THE METHOD |
| US4344800A (en) | 1980-06-03 | 1982-08-17 | Dow Corning Corporation | Method for producing hydrophobic reinforcing silica fillers and fillers obtained thereby |
| DE3329016A1 (en) | 1983-08-11 | 1985-02-28 | Basf Ag, 6700 Ludwigshafen | METHOD FOR PRODUCING POLYMERISATES OF ETHYLENE BY MEANS OF A SILICONE XEROGEL / CHROMTRIOXIDE CATALYST |
| DE3429671A1 (en) | 1984-08-11 | 1986-02-20 | Basf Ag, 6700 Ludwigshafen | METHOD FOR PRODUCING AEROGELS |
| JPS6169867A (en) | 1984-09-13 | 1986-04-10 | Mitsubishi Rayon Co Ltd | Resin composition containing fine silica particle |
| US4649037A (en) | 1985-03-29 | 1987-03-10 | Allied Corporation | Spray-dried inorganic oxides from non-aqueous gels or solutions |
| FR2584698B1 (en) * | 1985-07-15 | 1990-05-18 | Rhone Poulenc Spec Chim | PROCESS FOR THE PREPARATION OF SPHEROIDAL SILICA PARTICLES |
| US5215733A (en) | 1986-04-25 | 1993-06-01 | Unilever Patent Holdings B.V. | Manufacture of silica gels using shear to reduce the particle size prior to washing with a hydrocyclone |
| US4888369A (en) | 1987-01-21 | 1989-12-19 | Himont Incorporated | Polypropylene composition resistant to high energy radiation, and radiation sterilized articles therefrom |
| FR2613708B1 (en) | 1987-04-13 | 1990-10-12 | Rhone Poulenc Chimie | HYDROPHOBIC PRECIPITATION SILICA, ITS PREPARATION PROCESS AND ITS APPLICATION TO THE REINFORCEMENT OF SILICON ELASTOMERS |
| US4950502A (en) | 1987-09-10 | 1990-08-21 | Dow Corning Corporation | Method of hydrophobing silica |
| US5001183A (en) | 1987-09-10 | 1991-03-19 | Dow Corning Corporation | Method of hydrophobing silica |
| US4873218A (en) | 1988-05-26 | 1989-10-10 | The United States Department Of Energy | Low density, resorcinol-formaldehyde aerogels |
| JPH02152196A (en) | 1988-12-03 | 1990-06-12 | Osaka Prefecture | Distributed el element |
| DE3914850A1 (en) | 1989-05-05 | 1990-11-08 | Basf Ag | THERMAL INSULATING MATERIAL BASED ON PIGMENT-BASED SILICONE ACULATE ARRAY |
| WO1992003378A1 (en) | 1990-08-23 | 1992-03-05 | United States Department Of Energy | A METHOD FOR PRODUCING METAL OXIDE AEROGELS HAVING DENSITIES LESS THAN 0.02 g/cm?3¿ |
| US5409683A (en) | 1990-08-23 | 1995-04-25 | Regents Of The University Of California | Method for producing metal oxide aerogels |
| JP2646150B2 (en) | 1990-08-27 | 1997-08-25 | 出光興産 株式会社 | Water repellent silica sol and method for producing the same |
| US5674962A (en) | 1990-11-30 | 1997-10-07 | Mitsubishi Rayon Company Ltd. | Toner resin |
| US5081163A (en) | 1991-04-11 | 1992-01-14 | The United States Of America As Represented By The Department Of Energy | Melamine-formaldehyde aerogels |
| NO912006D0 (en) | 1991-05-24 | 1991-05-24 | Sinvent As | PROCEDURE FOR THE MANUFACTURE OF A SILICA-AEROGEL-LIKE MATERIAL. |
| DE4201306A1 (en) | 1992-01-20 | 1993-07-22 | Basf Ag | MOLDED PARTS OR PANELS FROM SILICA AEROGELS |
| US5565142A (en) | 1992-04-01 | 1996-10-15 | Deshpande; Ravindra | Preparation of high porosity xerogels by chemical surface modification. |
| DE4231749A1 (en) | 1992-09-23 | 1994-03-24 | Basf Ag | Process for the preparation of a supported catalyst for the polymerization of alpha-olefins |
| US5420168A (en) | 1993-04-01 | 1995-05-30 | The Regents Of The University Of California | Method of low pressure and/or evaporative drying of aerogel |
| DE4316540A1 (en) | 1993-05-18 | 1994-11-24 | Hoechst Ag | Process for subcritical drying of aerogels |
| US5508341A (en) | 1993-07-08 | 1996-04-16 | Regents Of The University Of California | Organic aerogel microspheres and fabrication method therefor |
| DE69424941T2 (en) | 1993-07-22 | 2000-11-02 | Huntsman Ici Chem Llc | ORGANIC AEROGELS |
| US5484818A (en) | 1993-07-22 | 1996-01-16 | Imperial Chemical Industries Plc | Organic aerogels |
| CN1042822C (en) | 1993-08-31 | 1999-04-07 | Basf公司 | Hydrophobic silicic aerogels |
| JP2725573B2 (en) | 1993-11-12 | 1998-03-11 | 松下電工株式会社 | Manufacturing method of hydrophobic airgel |
| US5795556A (en) | 1993-12-14 | 1998-08-18 | Hoechst Ag | Xerogels and process for their preparation |
| DE4342548A1 (en) | 1993-12-14 | 1995-06-22 | Hoechst Ag | Xerogels, processes for their manufacture and their use |
| DE4404701A1 (en) | 1994-02-15 | 1995-08-17 | Hoechst Ag | Composite foams, processes for their production and their use |
| US5494858A (en) | 1994-06-07 | 1996-02-27 | Texas Instruments Incorporated | Method for forming porous composites as a low dielectric constant layer with varying porosity distribution electronics applications |
| DE4430669A1 (en) | 1994-08-29 | 1996-03-07 | Hoechst Ag | Process for the production of fiber-reinforced xerogels and their use |
| US5476878A (en) | 1994-09-16 | 1995-12-19 | Regents Of The University Of California | Organic aerogels from the sol-gel polymerization of phenolic-furfural mixtures |
| DE4437424A1 (en) | 1994-10-20 | 1996-04-25 | Hoechst Ag | Airgel-containing composition, process for its preparation and its use |
| DE4439217A1 (en) | 1994-11-03 | 1996-05-09 | Hoechst Ag | Process for the production of aerogels |
| DE4441567A1 (en) * | 1994-11-23 | 1996-05-30 | Hoechst Ag | Airgel-containing composite material, process for its production and its use |
| CN1063246C (en) | 1994-12-21 | 2001-03-14 | 卡伯特公司 | Nonwoven fabric-aerogel composite material containing two component fibers, method of producing said material and use thereof |
| DE19502453C1 (en) | 1995-01-27 | 1996-09-05 | Hoechst Ag | Process for the production of modified Si0¶2¶ aerogels and their use |
| DE19506141A1 (en) | 1995-02-22 | 1996-08-29 | Hoechst Ag | Use of aerogels in pharmacy, cosmetics and crop protection |
| DE19533564A1 (en) * | 1995-09-11 | 1997-03-13 | Hoechst Ag | Fibrous airgel composite material |
| DE19534198A1 (en) | 1995-09-15 | 1997-03-20 | Hoechst Ag | Process for the production of organofunctionalized aerogels |
| DE19537821A1 (en) | 1995-10-11 | 1997-04-17 | Hoechst Ag | Coated film used for thermal insulation, electronic applications, noise absorption or membranes |
| US5595593A (en) | 1995-10-12 | 1997-01-21 | Dow Corning Corporation | Treatment of fillers with oxa-silacycloalkanes |
| DE19541279A1 (en) | 1995-11-06 | 1997-05-07 | Hoechst Ag | Process for the production of organically modified aerogels using alcohols |
| DE19541715A1 (en) | 1995-11-09 | 1997-05-15 | Hoechst Ag | Process for the production of organically modified aerogels, in which the salts formed are precipitated |
| DE19541992A1 (en) | 1995-11-10 | 1997-05-15 | Hoechst Ag | Process for the production of organically modified aerogels using alcohols, in which the salts formed are precipitated |
| DE19648798C2 (en) | 1996-11-26 | 1998-11-19 | Hoechst Ag | Process for the production of organically modified aerogels by surface modification of the aqueous gel (without prior solvent exchange) and subsequent drying |
| US5708069A (en) | 1997-02-24 | 1998-01-13 | Dow Corning Corporation | Method for making hydrophobic silica gels under neutral conditions |
| US5750610A (en) | 1997-02-24 | 1998-05-12 | Dow Corning Corporation | Hydrophobic organosilicate-modified silica gels |
-
1997
- 1997-05-02 DE DE19718740A patent/DE19718740A1/en not_active Ceased
-
1998
- 1998-04-29 JP JP54769598A patent/JP2001523162A/en not_active Ceased
- 1998-04-29 CA CA002287849A patent/CA2287849A1/en not_active Abandoned
- 1998-04-29 CN CN98805627A patent/CN1126592C/en not_active Expired - Fee Related
- 1998-04-29 KR KR19997010098A patent/KR20010012153A/en not_active Application Discontinuation
- 1998-04-29 WO PCT/EP1998/002519 patent/WO1998050144A1/en not_active Application Discontinuation
- 1998-04-29 EP EP98925496A patent/EP0979141A1/en not_active Ceased
-
1999
- 1999-11-01 US US09/433,931 patent/US6481649B1/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| CN1258230A (en) | 2000-06-28 |
| DE19718740A1 (en) | 1998-11-05 |
| CN1126592C (en) | 2003-11-05 |
| KR20010012153A (en) | 2001-02-15 |
| US6481649B1 (en) | 2002-11-19 |
| EP0979141A1 (en) | 2000-02-16 |
| JP2001523162A (en) | 2001-11-20 |
| WO1998050144A1 (en) | 1998-11-12 |
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