EP3253712A1 - Procédé de fabrication d'aérogel et matériau composite à base d'aérogel - Google Patents

Procédé de fabrication d'aérogel et matériau composite à base d'aérogel

Info

Publication number
EP3253712A1
EP3253712A1 EP16705420.4A EP16705420A EP3253712A1 EP 3253712 A1 EP3253712 A1 EP 3253712A1 EP 16705420 A EP16705420 A EP 16705420A EP 3253712 A1 EP3253712 A1 EP 3253712A1
Authority
EP
European Patent Office
Prior art keywords
gel
sol
acid
airgel
fibers
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.)
Pending
Application number
EP16705420.4A
Other languages
German (de)
English (en)
Inventor
Lukas Huber
Ivo Kym-Mijuskovic
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.)
Rockwool AS
Original Assignee
Flumroc AG
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 Flumroc AG filed Critical Flumroc AG
Publication of EP3253712A1 publication Critical patent/EP3253712A1/fr
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/157After-treatment of gels
    • C01B33/158Purification; Drying; Dehydrating
    • C01B33/1585Dehydration into aerogels
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/145Preparation of hydroorganosols, organosols or dispersions in an organic medium
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/155Preparation of hydroorganogels or organogels
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/157After-treatment of gels
    • C01B33/158Purification; Drying; Dehydrating
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/157After-treatment of gels
    • C01B33/159Coating or hydrophobisation
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10Coating
    • C03C25/42Coatings containing inorganic materials
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/24Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/0045Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by a process involving the formation of a sol or a gel, e.g. sol-gel or precipitation processes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28Compounds of silicon
    • C09C1/30Silicic acid
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28Compounds of silicon
    • C09C1/30Silicic acid
    • C09C1/3081Treatment with organo-silicon compounds
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/10Solid density
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/32Thermal properties
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20Resistance against chemical, physical or biological attack
    • C04B2111/28Fire resistance, i.e. materials resistant to accidental fires or high temperatures
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/30Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
    • C04B2201/32Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors

Definitions

  • the present invention relates to a process for producing an airgel according to the preamble of claim 1 and to a process obtainable by the process
  • Aerogels have a low density, large porosity with open pores in the range ⁇ 50nm and a large inner surface. This results in a low thermal conductivity.
  • aerogels are also suitable as thermal insulation materials.
  • the high porosity also leads to a low mechanical stability of the airgel.
  • the method described has the disadvantage that the gel must be dried under supercritical conditions, for which an autoclave required usually at least one solvent change is made. This is a very time-consuming and time-consuming process.
  • the drying requires special equipment (pressure reactor for the critical point drying, eg drying CO 2 at> 74 bar /> 30 ° C). Accordingly, the supercritical drying of aerogels is only suitable for small batches and on a laboratory scale.
  • glass wool based aerogels which on the one hand are sufficiently stable in acidic pH, but on the other hand have only insufficient temperature resistance in case of fire,
  • WO 94/25149 describes a process for producing a highly porous xerogel in which the surface of the gel is hydrophobed with surface-modifying compounds in order to reduce the capillary pressure in the pores of the gel before drying, so that the gel does not collapse in the final drying step.
  • the process consists of a sequence of aging, washing and drying steps.
  • the process described is very complicated because before and after the hydrophobing with trimethylchlorosilane, the gel must be washed with aprotic solvents.
  • Another disadvantage is the hydrochloric acid liberated during the hydrophobic treatment, which would attack, for example, rock wool fibers.
  • DE-OS-1 648 798 describes a process for the preparation of organically modified aerogels by surface modification of the aqueous gel (without previous
  • the silylating agent used is preferably hexamethyldisiloxane (H DSO).
  • a base or acid may also be present as a catalyst for the hydrophobization reaction.
  • Preferred acids are hydrochloric, sulfuric, phosphoric, hydrofluoric, oxalic, acetic or formic, but hydrochloric acid is preferred.
  • the gel formed is preferably dried undercritically. Since according to the teaching of DE-OS 196 48 798 is completely dispensed with the use of organic solvents, all for the used
  • WO 2013/053951 discloses a method for producing a xerogel with a
  • a sol is poured into a reactor in which a fibrous reinforcing material was previously arranged.
  • the sol is then gelled, aged and rendered hydrophobic.
  • the hydrophobized alcogel is then first predried at temperatures up to 80 ° C and then dried under subcritical conditions and temperatures> 100 ° C and preferably between 120 ° C and 140 ° C until the residual alcohol content is ⁇ 3% to the last-mentioned process step, be carried out in the same reactor. It is important that the inner walls have a distance of 70 mm or less from each other. Become bigger
  • the produced fiber-reinforced xerogels have a thermal conductivity> 25 mW / Km.
  • the alcogel formed in the second process step has an alcohol content between 15% by weight and 90% by weight relative to the weight of the original sol.
  • the hydrophobing with preferably HMDSO (hexamethyldisiloxane) is carried out in the presence of hydrochloric acid at a pH of between 1 and 3.
  • hydrochloric acid formic acid is vorgesehlagen,
  • US patent r. 5,746,992 relates to the production of a silicon airgel.
  • the alcohol is removed from the alkogel under subcritical conditions.
  • the hydrolysis of tetraethoxysilane takes place in two stages: in a first stage, the tetraethoxysilane, methanol, some water and nitric acid are mixed together in a glass container, the glass container sealed and during 24 hours at 60 ° C.
  • the tetraethoxysilane partially hydrolyzes under acidic conditions, after which the mixture is passed through Added basic aqueous solution and kept again at 60 ° C for 24 hours to achieve a secondary hydrolysis under basic conditions. Under these conditions, a clear silica gel was obtained, which after drying in an oven had an internal particle porosity of 74 percent. According to US 5,746,992 no hydrophobization of the gel is provided.
  • WO 2015/014813 discloses a process for producing an airgel material which is similar to that of WO 2013/053951.
  • an alcoholic medium is first prepared in an alcoholic medium, which can be reacted with an acid-catalytically activatable hydrophobing agent, in this case HMDSO.
  • HMDSO acid-catalytically activatable hydrophobing agent
  • I hydrophobicizing HMDSO is added to the silica sol in the first step.
  • the volume fraction of the hydrophobizing agent in the sol is 3 to 80%. This is only after formation of the gel, which may optionally also be aged, by release or addition of at least one with the hydrophobing agent
  • WO 2015/014813 describes an exemplary embodiment for producing a granulate, which is characterized in that the gel formed and aged is mechanically comminuted, then transferred to a closed pressure vessel and rendered hydrophobic by means of HCl in the presence of HMDSO, and subsequently on a conveyor belt at 50 ° C first pre-dried and then dried at 150 ° C ready.
  • an airgel insulation board is made by adding an alcoholic solution containing a 22% SiO 2 content of polyethoxydisiloxane sol and a slow release agent doped with 10% HCl to HMDSO. After adding an ammonia solution, the mixed sol is placed in a fit previously laid out with a polyester non-woven fiber mat. After a 5-hour aging, the
  • Gel plate is lifted out of the mold and stored in a closed vessel for 24 h at 65 ° C. and rendered hydrophobic, at which temperature HCl exits the microencapsulation and activates the HMDSO present
  • the vessel is then opened and the gel plate first at 50 ° C. and then dried at 130 ° C.
  • the airgel material (without fiber matrix) should have a porosity of> 80%, preferably> 90% and particularly preferably> 92%, and a density ⁇ 0.2 g / ml and preferably 0.15 g / ml and particularly preferably ⁇ 0.12 g / ml. Yet another goal is that it is possible to dispense with supercritical drying of the airgel material during production. Another goal is an airgel composite
  • the aim is to use a fiber-airgel composite material with a
  • Silylating agent in the presence of an acid as a catalyst, and then drying the gel preferably by subcritical drying.
  • Aero- resp. Xerogels can be used essentially the same methods and parameters as described in WO 2013/053951 or WO 2015/014813.
  • aerogels are to be understood to mean highly porous solids, in particular those based on silicates, irrespective of the drying method.
  • airgel as used herein means a highly porous material with air as a dispersant.
  • the object is achieved by a method according to the preamble of claim 1, by using hexamethyldisiloxane as hydrophobizing agent and as acid
  • Nitric acid HN03
  • HN03 Nitric acid
  • the silicate sol is obtained by hydrolysis of alkoxysilanes or hydroxyalkoxysilanes, preferably of tetraethylene thoxy silane (TEOS) or Tr ine I! or si 1, manufactured.
  • TEOS tetraethylene thoxy silane
  • Tr ine I! or si 1, manufactured tetraethylene thoxy silane
  • the use of TEOS has the advantage that it is soluble in alcohol, eg EtOH.
  • the preparation of the sol in alcohol, an alcoholic or an alcoholic solvent can be carried out emisch, which is advantageous for the process, since less water is present in the pores of the later formed gel.
  • An alcoholic solvent mixture is to be understood as meaning a mixture in which alcohol is the main constituent and preferably has a volume fraction of> 90% by volume and particularly preferably> 95% by volume.
  • Alcohol-containing solvent mixture can be understood as one in which the percentage volume fraction of the alcohol or alcohols ⁇ 50% by volume and preferably ⁇ 40% by volume.
  • the preparation of the sol is preferably carried out in an acidic medium by hydrolysis of tetraethoxysilane (TEOS), which is initially charged in a solvent, preferably EtOH.
  • TEOS tetraethoxysilane
  • Hydrochloric acid or formic acid is preferably used for the hydrolysis.
  • Prehydrolysed sols are stable and storable, and are
  • Pre-hydrolyzed sols are preferably used which are present in an amount between 5% and 30% (m / m) S1O2 and preferably between 10% and 25% (m / m) SiO 2 alcohol, preferably EtOH.
  • the pH of the hydrophobization is advantageously set to a value between 1 and 7, preferably between 2 and 5. In the acidic range at about pH 2, HMDSO reacts rapidly with the still free Si-OH groups.
  • the pH of the hydrophobization is advantageously set to a value between 0.2 and 5, preferably between 0.5 and 3, and particularly preferably between 0.8 and 2. The pH is measured in the aqueous phase. Surprisingly, such pH is compatible with rockwool fibers when nitric acid is used
  • Hydrophobleiterskatalystor is used.
  • the gelation takes place in a temperature range between 30 ° C and 80 ° C, preferably between 50 ° C and 75 ° C, and more preferably between 60 n C and 70 ° C.
  • a base for example ammonia
  • ammonia is added to the mixture, which is present as aqueous ammonia solution.
  • Substantially alcoholic solvent preferably EtOH, carried out, wherein suitably the proportion of water is less than 20 vol.%, Preferably less than 10 vol.% And particularly preferably less than 5 vol.% Is. It has been found that a small amount of water has a positive influence on the quality of the airgel produced.
  • fibers can be added before and / or during gel production.
  • the fibers are added prior to actual gelation (condensation), i. the fibers and the sol are preferably mixed together between steps a) and b).
  • Rockwool fibers are used particularly advantageously as mineral fibers. These have the great advantage that they are virtually non-flammable.
  • the subject matter of the present invention is also an airgel, in particular xerogel,
  • hexamethyldisiloxane is used as the hydrophobizing agent and nitric acid (HNO 3) as the acid.
  • a further subject of the present invention is an airgel-fiber composite material obtainable by mixing the sol prepared according to the process described with mineral fibers, in particular rockwool fibers.
  • the airgel-fiber composite material has a porosity of> 90% and a thermal conductivity ⁇ 18 mW / m.
  • the mineral fibers are not noticeably dissolved during production.
  • the hydrophobicization would be acidic
  • the subject matter of the present invention is furthermore a composite material in the form of an insulating board consisting of the airgel according to the invention and mineral fibers.
  • Silylating agent is circulated (about 15 h at about 60 ° C). As soon as the
  • Hydrophobing is completed, the solvent / water repellent mixture is drained, worked up and later reused in a next manufacturing process. Hydrophobization of a lyogel with trimethysilyl chloride:
  • hydrophobing catalysts various organic and inorganic acids, e.g. Sulfuric acid (H2S04), hydrochloric acid (HCl), phosphoric acid (H3P04),
  • the thermal conductivity was determined according to standard EN 12667 (Standard hot plate method) at 20 oC and normal pressure.
  • the aging of the gel takes place between 24 and 120 hours, preferably between 48 and 96 hours and more preferably for about 72 hours the gel in the same container by adding an excess of HMDSO (in this case from about 270 L of a 20 to 98% (m / m) HMDSO - solution) and about 5 L of a substantially alcoholic HNO 3 solution (about 4 to 7 % m / m) for 24 h at 75 oC dynamic, ie hydrophobic by circulation of the liquid phase.
  • HMDSO in this case from about 270 L of a 20 to 98% (m / m) HMDSO - solution
  • a substantially alcoholic HNO 3 solution about 4 to 7 % m / m
  • the mixer / setter water is added to the partly used hydrophobizing solution (about 10% of the volume of the hydrophobizing solution present) and the mixture is stirred vigorously for 10 to 30 minutes. Thereafter, the mixture is allowed to stand overnight with an aqueous phase settling to the bottom. The aqueous phase is separated and discarded.
  • the alcoholic hydrophobizing solution can then be added to the partly used hydrophobizing solution (about 10% of the volume of the hydrophobizing solution present) and the mixture is stirred vigorously for 10 to 30 minutes. Thereafter, the mixture is allowed to stand overnight with an aqueous phase settling to the bottom. The aqueous phase is separated and discarded.
  • the alcoholic hydrophobizing solution can then
  • the present invention relates to a process for airgel production and to a composite material made from an aerogei and mineral fibers produced by means of this process.
  • a silicate-based airgel material with a thermal conductivity coefficient of ⁇ 18 mW / mK is obtainable by hydrophobicizing with HMDSO in the presence of nitric acid.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Silicon Compounds (AREA)

Abstract

La présente invention concerne un procédé de fabrication d'aérogel et un matériau composite à base d'un aérogel et de fibres minérales, obtenu au moyen dudit procédé. Un matériau aérogel préparé à base de silicate, ayant un coefficient de conductivité thermique <18 mW/mK peut être obtenu, par imperméabilisation dudit matériau aérogel avec HMDSO en présence d'acide nitrique.
EP16705420.4A 2015-02-04 2016-02-04 Procédé de fabrication d'aérogel et matériau composite à base d'aérogel Pending EP3253712A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CH00147/15A CH710694B1 (de) 2015-02-04 2015-02-04 Verfahren zur Herstellung eines Aerogels resp. eines Aerogel-Verbundwerkstoffs, sowie Aerogel resp. Aerogel-Verbundwerkstoff erhältlich nach dem Verfahren.
PCT/CH2016/000024 WO2016123724A1 (fr) 2015-02-04 2016-02-04 Procédé de fabrication d'aérogel et matériau composite à base d'aérogel

Publications (1)

Publication Number Publication Date
EP3253712A1 true EP3253712A1 (fr) 2017-12-13

Family

ID=53723958

Family Applications (1)

Application Number Title Priority Date Filing Date
EP16705420.4A Pending EP3253712A1 (fr) 2015-02-04 2016-02-04 Procédé de fabrication d'aérogel et matériau composite à base d'aérogel

Country Status (7)

Country Link
US (1) US20180016152A1 (fr)
EP (1) EP3253712A1 (fr)
CN (1) CN107531494B (fr)
CA (1) CA2975409A1 (fr)
CH (1) CH710694B1 (fr)
RU (1) RU2721110C2 (fr)
WO (1) WO2016123724A1 (fr)

Families Citing this family (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20170104914A (ko) 2016-03-08 2017-09-18 주식회사 엘지화학 에어로겔 블랑켓의 제조방법 및 이로부터 제조된 에어로겔 블랑켓
KR102113324B1 (ko) * 2016-09-23 2020-05-20 주식회사 엘지화학 초고온용 실리카 에어로겔 블랭킷, 이의 제조방법 및 이의 시공방법
WO2020061344A1 (fr) * 2018-09-20 2020-03-26 Blueshift Materials, Inc. Composites remplis ayant une conductivité thermique, une constante diélectrique et un poids réduits
DE102018128410A1 (de) * 2018-11-13 2020-05-14 Fraunhofer Gesellschaft zur Förderung der angewandten Forschung e.V. Verfahren zur Herstellung von Aerogelen und mit diesem erhältliche Aerogele
CN109748284A (zh) * 2019-03-27 2019-05-14 海南大学 一种无机气凝胶的制备方法
CN111285623A (zh) * 2020-04-14 2020-06-16 河南爱彼爱和新材料有限公司 一种不掉粉的复合气凝胶纤维及其制备工艺
JP2023523283A (ja) * 2020-04-30 2023-06-02 エボニック オペレーションズ ゲーエムベーハー アルカリ安定性の上昇したシリカエアロゲル
CN114539979B (zh) * 2020-11-26 2023-04-25 中国科学院大连化学物理研究所 氮化硼气凝胶基的复合定型相变材料及制备和应用
CN113060966B (zh) * 2021-03-30 2022-08-09 山东坚盾建材科技有限公司 一种纳米粉末混凝土防水剂
CN113603452B (zh) * 2021-09-09 2023-04-04 中国科学技术大学先进技术研究院 一种二氧化硅气凝胶复合材料的制备方法
CN113683389B (zh) * 2021-09-26 2022-12-06 巩义市泛锐熠辉复合材料有限公司 一种重复利用超临界废液生产二氧化硅气凝胶毡的方法
CN114181671B (zh) * 2021-12-31 2023-09-26 中国科学技术大学先进技术研究院 二氧化硅气凝胶相变复合材料的制备方法
CN117511219B (zh) * 2024-01-05 2024-04-09 中铁建设集团有限公司 一种柔性纤维增强纳米微孔气凝胶及其制备方法

Family Cites Families (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5306555A (en) * 1991-09-18 1994-04-26 Battelle Memorial Institute Aerogel matrix composites
US5565142A (en) 1992-04-01 1996-10-15 Deshpande; Ravindra Preparation of high porosity xerogels by chemical surface modification.
WO1995017347A1 (fr) * 1993-12-23 1995-06-29 Ppg Industries, Inc. Aerogel de silice produit dans des conditions sous-critiques
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
DE19648797A1 (de) * 1996-11-26 1998-05-28 Hoechst Ag Verfahren zur Herstellung von organisch modifizierten, dauerhaft hydrophoben Aerogelen
US6696258B1 (en) * 1998-01-20 2004-02-24 Drexel University Mesoporous materials and methods of making the same
US7078359B2 (en) * 2000-12-22 2006-07-18 Aspen Aerogels, Inc. Aerogel composite with fibrous batting
KR100868989B1 (ko) * 2007-05-23 2008-11-17 엠파워(주) 초소수성 실리카 에어로겔 분말의 제조방법
US9215667B2 (en) 2010-10-21 2015-12-15 Telefonaktiebolaget L M Ericsson (Publ) Device and method for transmit power control
FR2981341B1 (fr) * 2011-10-14 2018-02-16 Enersens Procede de fabrication de xerogels
KR20130051304A (ko) * 2011-11-09 2013-05-20 엠파워(주) 초소수성 실리카 에어로겔 분말
EP2644566A1 (fr) * 2012-03-30 2013-10-02 Construction Research & Technology GmbH Procédé de fabrication d'aérogels
EP2832690A1 (fr) 2013-08-02 2015-02-04 EMPA Eidgenössische Materialprüfungs- und Forschungsanstalt Procédé de fabrication d'un matériau aérogel
DE102014101709A1 (de) * 2013-12-20 2015-07-16 Interbran Systems Ag Verfahren zur Herstellung von Aerogelen

Also Published As

Publication number Publication date
CN107531494B (zh) 2021-07-06
RU2721110C2 (ru) 2020-05-15
CH710694A1 (de) 2016-08-15
WO2016123724A1 (fr) 2016-08-11
RU2017130923A (ru) 2019-03-04
US20180016152A1 (en) 2018-01-18
CA2975409A1 (fr) 2016-08-11
RU2017130923A3 (fr) 2019-07-17
CH710694B1 (de) 2019-05-15
CN107531494A (zh) 2018-01-02

Similar Documents

Publication Publication Date Title
EP3253712A1 (fr) Procédé de fabrication d&#39;aérogel et matériau composite à base d&#39;aérogel
DE19648798C2 (de) Verfahren zur Herstellung von organisch modifizierten Aerogelen durch Oberflächenmodifikation des wäßrigen Gels (ohne vorherigen Lösungsmitteltausch) und anschließender Trocknung
EP0859739B1 (fr) Procede de preparation d&#39;aerogels modifies de maniere organique a l&#39;aide d&#39;alcools
EP0805781B1 (fr) Procede de production d&#39;aerogels modifies
EP0778815B1 (fr) Procede de production de xerogels renforces par des fibres et leur utilisation
EP0859740B1 (fr) Procede de preparation d&#39;aerogels modifies de maniere organique, selon lequel les sels formes sont precipites
EP0778814B1 (fr) Materiaux composites contenant un aerogel, leur procede de production et leur utilisation
WO1996026890A2 (fr) Procede de production d&#39;aerogels inorganiques hydrophiles ou partiellement hydrophiles
EP0861207B1 (fr) Procede de preparation d&#39;aerogels modifies de maniere organique a l&#39;aide d&#39;alcools, selon lequel les sels formes sont precipites
EP0789667B1 (fr) Procede de production d&#39;aerogels
DE19648797A1 (de) Verfahren zur Herstellung von organisch modifizierten, dauerhaft hydrophoben Aerogelen
CH712479A1 (de) Anlage und Verfahren zur Herstellung eines Aerogel-Verbundwerkstoffs und Aerogel-Verbundwerkstoff.
EP3762137A1 (fr) Procédé de production d&#39;un matériau aérogel
DE19752456A1 (de) Verfahren zur Herstellung von organisch modifizierten Aerogelen auf Basis von Siliciumtetrachlorid
EP0925256A1 (fr) Procede de production d&#39;aerogels modifies de maniere organique
DE19631267C1 (de) Verfahren zur Herstellung von organisch modifizierten Aerogelen
EP0837832B1 (fr) Procede de production d&#39;aerogels organiquement modifies et leur utilisation
DE19801004A1 (de) Verfahren zur Herstellung von im wesentlichen kugelförmigen Lyogelen in wasserunlöslichen Silylierungsmitteln
EP4201882A1 (fr) Corps moulé monolithique en silice et sa fabrication

Legal Events

Date Code Title Description
STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE INTERNATIONAL PUBLICATION HAS BEEN MADE

PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: REQUEST FOR EXAMINATION WAS MADE

17P Request for examination filed

Effective date: 20170831

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

AX Request for extension of the european patent

Extension state: BA ME

DAV Request for validation of the european patent (deleted)
DAX Request for extension of the european patent (deleted)
RAP1 Party data changed (applicant data changed or rights of an application transferred)

Owner name: ROCKWOOL INTERNATIONAL A/S

TPAC Observations filed by third parties

Free format text: ORIGINAL CODE: EPIDOSNTIPA

TPAC Observations filed by third parties

Free format text: ORIGINAL CODE: EPIDOSNTIPA

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: EXAMINATION IS IN PROGRESS

17Q First examination report despatched

Effective date: 20190820

TPAC Observations filed by third parties

Free format text: ORIGINAL CODE: EPIDOSNTIPA

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: EXAMINATION IS IN PROGRESS

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: EXAMINATION IS IN PROGRESS

RAP3 Party data changed (applicant data changed or rights of an application transferred)

Owner name: ROCKWOOL A/S