EP0979142A1 - Procede de compactage d'aerogels - Google Patents
Procede de compactage d'aerogelsInfo
- Publication number
- EP0979142A1 EP0979142A1 EP98925497A EP98925497A EP0979142A1 EP 0979142 A1 EP0979142 A1 EP 0979142A1 EP 98925497 A EP98925497 A EP 98925497A EP 98925497 A EP98925497 A EP 98925497A EP 0979142 A1 EP0979142 A1 EP 0979142A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- starting material
- pressed
- aerogels
- granules
- airgel particles
- 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.)
- Ceased
Links
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000004964 aerogel Substances 0.000 title abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 23
- 238000003825 pressing Methods 0.000 claims abstract description 10
- 239000007858 starting material Substances 0.000 claims description 22
- 239000008187 granular material Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 4
- 239000000654 additive Substances 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 claims description 2
- 239000000945 filler Substances 0.000 claims description 2
- 235000011837 pasties Nutrition 0.000 claims description 2
- 239000000499 gel Substances 0.000 description 19
- 238000004519 manufacturing process Methods 0.000 description 12
- 229910004298 SiO 2 Inorganic materials 0.000 description 9
- 238000001035 drying Methods 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 239000003960 organic solvent Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000000352 supercritical drying Methods 0.000 description 4
- 235000019353 potassium silicate Nutrition 0.000 description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 3
- -1 DE 3025437 Chemical compound 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000005903 acid hydrolysis reaction Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000007872 degassing Methods 0.000 description 2
- 239000002612 dispersion medium Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- 229910002012 Aerosil® Inorganic materials 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 230000001427 coherent effect Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000000495 cryogel Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 239000007863 gel particle Substances 0.000 description 1
- 239000000017 hydrogel Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 238000010327 methods by industry Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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
- B01J2/20—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by expressing the material, e.g. through sieves and fragmenting the extruded length
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/12—Making granules characterised by structure or composition
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/08—Making granules by agglomerating smaller particles
Definitions
- the present invention relates to a method for compacting aerogels.
- Aerogels in particular those with porosities above 60% and densities below 0.6 g / cm 3 , have an extremely low thermal conductivity and are therefore used as heat insulation material, as described in EP-A-0 1 71 722, as catalysts or Catalyst carrier, as well as an adsorbent material.
- the use for Cerenkov detectors is known due to their very low refractive index for solids.
- the literature describes a possible use as an impedance matching, for example in the ultrasound range, due to its special acoustic impedance.
- Aerogels in the broader sense ie in the sense of "gel with air as the dispersion medium" are produced by drying a suitable gel.
- airgel in this sense includes aerogels in the narrower sense, xerogels and cryogels.
- a dried gel is referred to as an airgel in the narrower sense if the liquid of the gel is largely removed at temperatures above the critical temperature and starting from pressures above the critical pressure. If, on the other hand, the liquid of the gel becomes subcritical, for example with the formation of a liquid-vapor boundary phase removed, the resulting gel is often referred to as xerogel.
- aerogels in the broad sense, i.e. in the sense of "gel with air as a dispersion medium”.
- the term does not include xerogels known from the older literature, which e.g. obtained by precipitation of silica (e.g. DE 3025437, DD 296 898), or as pyrogenic silica, e.g. Aerosil TM. In these cases, a homogeneous three-dimensional gel network is not formed over large distances during production.
- Inorganic aerogels have been known since 1 931 (SS Kistler, Nature 1 931, 1 27.741). Since then, aerogels have been made from a wide variety of starting materials.
- z. B. SiO 2 -, Al 2 O 3 -, TiO 2 -, ZrO 2 -, SnO 2 -, Li 2 O-, CeO 2 -, V 2 O 5 -Aerogels and mixtures of these can be prepared (H .D. Gesser, PCGoswami, Chem. Rev. 1 989, 89.765ff).
- organic aerogels made from a wide variety of starting materials, e.g. from Meiamine formaldehyde, known (R.W. Pekala, J. Mater. Sci. 1 989, 24, 3221).
- Inorganic aerogels can be produced in different ways.
- SiO 2 aerogels can be produced, for example, by acid hydrolysis and condensation of tetraethyl orthosilicate in ethanol. This creates a gel that is obtained by supercritical drying while maintaining the structure can be dried. Manufacturing processes based on this drying technique are known, for example, from EP-A-0 396 076, WO 92/03378 or WO 95/0661 7.
- An alternative to supercritical drying is a method for subcritical drying of SiO 2 gels.
- the SiO 2 gel can be obtained, for example, by acid hydrolysis of tetraalkoxysilanes in a suitable organic solvent using water. After replacing the solvent with a suitable organic solvent, the gel obtained is reacted with a silylating agent in a further step. The resulting SiO 2 gel can then be dried in air from an organic solvent. This enables aerogels with densities below 0.4 g / cm 3 and porosities above 60% to be achieved. The manufacturing process based on this drying technique is described in detail in WO 94/25149.
- the gels described above can also be mixed with tetraalkoxysilanes and aged in the alcohol-aqueous solution before drying in order to increase the gel network strength, as disclosed in WO 92/20623.
- the tetraalkoxysilanes used as starting materials in the processes described above also represent an extremely high cost factor.
- a not inconsiderable cost reduction can be achieved by using water glass as the starting material for the production of the SiO 2 gels.
- a silica can be produced from an aqueous water glass solution with the aid of an ion exchange resin, and this polycondenses into an SiO 2 gel by adding a base. After replacing the aqueous medium with a suitable organic solvent, the gel obtained is then reacted with a chlorine-containing silylating agent in a further step. The resulting, on the surface z. B. modified with methylsilyl groups SiO 2 gel can also be dried in air from an organic solvent. The manufacturing method based on this technique is known from DE-A-43 42 548.
- DE-A-1 95 02 453 also describes the use of chlorine-free silylating agents in the production of subcritically dried aerogels.
- DE-A-1 95 34 1 98 also describes organofunctionalization using organofunctionalized silylating agents in the production of subcritically dried aerogels.
- airgel particles are, however, for the sake of Process engineering and the manufacturing costs on an industrial scale limited to particle sizes smaller than 5 mm, preferably smaller than 2 mm.
- the object of the present invention is therefore to provide a method by means of which small airgel particles below 2 mm can be formed into larger airgel particles.
- This object is achieved by a method in which the airgel particles are placed in a pressing device and pressed. In this way, it is particularly easy to form small airgel particles into larger airgel particles.
- these additives, fillers and / or binders are advantageously added, which may be in particulate and / or fibrous form, optionally also liquid or pasty.
- the starting material is degassed before pressing. This is particularly advantageous if the starting material is a loose bed, since then a certain proportion of the gas located between the airgel particles must be removed before compacting.
- the starting material for degassing is expediently subjected to a negative pressure, and in another embodiment the degassing can also take place during the pressing.
- the airgel particles or the starting material can be pressed into granules, after which they are then advantageously separated according to their size. This can be done, for example, by sieving the desired particle size range in order to obtain the desired target fraction. Granules lying below the desired grain size range are advantageously returned to the pressing device, while granules lying above are expediently comminuted so that they lie in the desired grain size range. After crushing, they can also be fed directly back to the pressing device in order to be compacted again.
- the granulate is then dried before further processing in order to remove undesirable residual moisture or harmful residual moisture for the further course of the process.
- the starting material can also be pressed into a slug, which is then also dried in accordance with a further embodiment before a further process step.
- the airgel particles or the airgel particles with possible additives can be pressed using customary suitable pressing devices.
- Another embodiment provides that the starting material is pressed into a die by a punch.
- the resulting compacts can then optionally be cut to the desired size with a knife, a scraper or the like.
- the starting material is pressed between a die and a roller sliding or rolling over it.
- the die can be perforated, in which case the resulting compacts are advantageously cut off in the desired size on the exit side with a knife, a scraper or the like.
- the starting material is pressed between two rollers, at least one of which rotates, but advantageously both.
- the starting material is then expediently pressed into the roll gap by a stuffing screw.
- At least one of the rolls is designed as a perforated hollow roll.
- the compacts formed here during the pressing are advantageously cut to the desired size on the outlet side using a suitable device, for example a knife or scraper.
- rollers are profiled.
- the starting material can then be pressed directly either into granules or into a coherent product band, a so-called Schülpe.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Silicon Compounds (AREA)
- Oxygen, Ozone, And Oxides In General (AREA)
- Colloid Chemistry (AREA)
Abstract
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19718741 | 1997-05-02 | ||
DE19718741A DE19718741A1 (de) | 1997-05-02 | 1997-05-02 | Verfahren zur Kompaktierung von Aerogelen |
PCT/EP1998/002520 WO1998050145A1 (fr) | 1997-05-02 | 1998-04-29 | Procede de compactage d'aerogels |
Publications (1)
Publication Number | Publication Date |
---|---|
EP0979142A1 true EP0979142A1 (fr) | 2000-02-16 |
Family
ID=7828545
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP98925497A Ceased EP0979142A1 (fr) | 1997-05-02 | 1998-04-29 | Procede de compactage d'aerogels |
Country Status (8)
Country | Link |
---|---|
US (1) | US6620355B1 (fr) |
EP (1) | EP0979142A1 (fr) |
JP (1) | JP2001525721A (fr) |
KR (1) | KR20010012152A (fr) |
CN (2) | CN1258231A (fr) |
CA (1) | CA2287832A1 (fr) |
DE (1) | DE19718741A1 (fr) |
WO (1) | WO1998050145A1 (fr) |
Families Citing this family (30)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE19648798C2 (de) * | 1996-11-26 | 1998-11-19 | Hoechst Ag | Verfahren zur Herstellung von organisch modifizierten Aerogelen durch Oberflächenmodifikation des wäßrigen Gels (ohne vorherigen Lösungsmitteltausch) und anschließender Trocknung |
US7118801B2 (en) * | 2003-11-10 | 2006-10-10 | Gore Enterprise Holdings, Inc. | Aerogel/PTFE composite insulating material |
US9469739B2 (en) | 2005-04-07 | 2016-10-18 | Aspen Aerogels, Inc. | Microporous polyolefin-based aerogels |
US8461223B2 (en) | 2005-04-07 | 2013-06-11 | Aspen Aerogels, Inc. | Microporous polycyclopentadiene-based aerogels |
US9476123B2 (en) | 2005-05-31 | 2016-10-25 | Aspen Aerogels, Inc. | Solvent management methods for gel production |
CN1317233C (zh) * | 2005-07-06 | 2007-05-23 | 北京科技大学 | 一种采用凝胶注模法成型硅石气凝胶粉体的方法 |
US20070014979A1 (en) | 2005-07-15 | 2007-01-18 | Aspen Aerogels, Inc. | Secured Aerogel Composites and Methods of Manufacture Thereof |
US9181486B2 (en) | 2006-05-25 | 2015-11-10 | Aspen Aerogels, Inc. | Aerogel compositions with enhanced performance |
WO2007146945A2 (fr) * | 2006-06-12 | 2007-12-21 | Aspen Aerogels, Inc. | Composites d'aérogel et de mousse |
KR101091860B1 (ko) * | 2006-10-10 | 2011-12-12 | 한국생산기술연구원 | 영구적 소수성을 갖는 에어로겔의 제조 방법 및 이로부터 제조된 영구적 소수성을 갖는 에어로겔 |
US7794805B2 (en) * | 2007-06-29 | 2010-09-14 | Schlumberger Technology Corporation | Thermal insulation barriers |
WO2009020615A1 (fr) * | 2007-08-07 | 2009-02-12 | Hunter Douglas Inc. | Panneau de verre isolé translucide |
US8952119B2 (en) | 2010-11-18 | 2015-02-10 | Aspen Aerogels, Inc. | Organically modified hybrid aerogels |
US8906973B2 (en) | 2010-11-30 | 2014-12-09 | Aspen Aerogels, Inc. | Modified hybrid silica aerogels |
US9133280B2 (en) | 2011-06-30 | 2015-09-15 | Aspen Aerogels, Inc. | Sulfur-containing organic-inorganic hybrid gel compositions and aerogels |
SI24001A (sl) | 2012-02-10 | 2013-08-30 | Aerogel Card D.O.O. | Kriogena naprava za transport in skladiščenje utekočinjenih plinov |
US9302247B2 (en) | 2012-04-28 | 2016-04-05 | Aspen Aerogels, Inc. | Aerogel sorbents |
US11053369B2 (en) | 2012-08-10 | 2021-07-06 | Aspen Aerogels, Inc. | Segmented flexible gel composites and rigid panels manufactured therefrom |
US9593206B2 (en) | 2013-03-08 | 2017-03-14 | Aspen Aerogels, Inc. | Aerogel insulation panels and manufacturing thereof |
FR3007025B1 (fr) | 2013-06-14 | 2015-06-19 | Enersens | Materiaux composites isolants comprenant un aerogel inorganique et une mousse de melamine |
US9434831B2 (en) | 2013-11-04 | 2016-09-06 | Aspen Aerogels, Inc. | Benzimidazole based aerogel materials |
US11380953B2 (en) | 2014-06-23 | 2022-07-05 | Aspen Aerogels, Inc. | Thin aerogel materials |
JP6487542B2 (ja) | 2014-10-03 | 2019-03-20 | アスペン エアロゲルズ,インコーポレイティド | 改善された疎水性エアロゲル材料 |
DE102015207944A1 (de) | 2015-04-29 | 2016-11-03 | Wacker Chemie Ag | Verfahren zur Herstellung organisch modifizierter Aerogele |
DE102015207939A1 (de) | 2015-04-29 | 2016-11-03 | Wacker Chemie Ag | Verfahren zur Herstellung organisch modifizierter Aerogele |
DE102015211812A1 (de) | 2015-06-25 | 2016-12-29 | Wacker Chemie Ag | Wirtschaftliches Verfahren zur Herstellung von organisch modifizierten Lyo- oder Aerogelen |
SG11202011338TA (en) | 2018-05-31 | 2020-12-30 | Aspen Aerogels Inc | Fire-class reinforced aerogel compositions |
CN108905912B (zh) * | 2018-08-01 | 2020-10-30 | 纳诺科技有限公司 | 气凝胶复合材料的制备方法 |
EP4382498A1 (fr) | 2022-12-09 | 2024-06-12 | EMPA Eidgenössische Materialprüfungs- und Forschungsanstalt | Materiau en aerogel de silice en vrac exempt de liant, procede de production et utilisations |
WO2023148082A1 (fr) | 2022-02-03 | 2023-08-10 | Empa Eidgenössische Materialprüfungs- Und Forschungsanstalt | Matériau d'aérogel de silice en vrac exempt de liant, son procédé de production et ses utilisations |
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-
1997
- 1997-05-02 DE DE19718741A patent/DE19718741A1/de not_active Ceased
-
1998
- 1998-04-29 KR KR19997010097A patent/KR20010012152A/ko not_active Application Discontinuation
- 1998-04-29 CN CN98805628A patent/CN1258231A/zh active Pending
- 1998-04-29 EP EP98925497A patent/EP0979142A1/fr not_active Ceased
- 1998-04-29 JP JP54769698A patent/JP2001525721A/ja active Pending
- 1998-04-29 CN CNA2006100048970A patent/CN101015781A/zh active Pending
- 1998-04-29 CA CA002287832A patent/CA2287832A1/fr not_active Abandoned
- 1998-04-29 WO PCT/EP1998/002520 patent/WO1998050145A1/fr not_active Application Discontinuation
-
1999
- 1999-11-01 US US09/430,982 patent/US6620355B1/en not_active Expired - Lifetime
Non-Patent Citations (1)
Title |
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See references of WO9850145A1 * |
Also Published As
Publication number | Publication date |
---|---|
KR20010012152A (ko) | 2001-02-15 |
DE19718741A1 (de) | 1998-11-05 |
JP2001525721A (ja) | 2001-12-11 |
WO1998050145A1 (fr) | 1998-11-12 |
US6620355B1 (en) | 2003-09-16 |
CA2287832A1 (fr) | 1998-11-12 |
CN101015781A (zh) | 2007-08-15 |
CN1258231A (zh) | 2000-06-28 |
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