WO2015016730A2 - Procédé de production de panneau flexibles d'aérogel hydrophobe renforcé de feutres de fibres - Google Patents

Procédé de production de panneau flexibles d'aérogel hydrophobe renforcé de feutres de fibres Download PDF

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Publication number
WO2015016730A2
WO2015016730A2 PCT/PT2014/000053 PT2014000053W WO2015016730A2 WO 2015016730 A2 WO2015016730 A2 WO 2015016730A2 PT 2014000053 W PT2014000053 W PT 2014000053W WO 2015016730 A2 WO2015016730 A2 WO 2015016730A2
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Prior art keywords
panels
aerogel
fibres
aerogels
felts
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PCT/PT2014/000053
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English (en)
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WO2015016730A3 (fr
Inventor
Marta Leonor BATISTA OCHOA
Luisa Maria ROCHA DURÃES
Marisa La-Sálete NUNES PERDIGOTO
António Alberto TORRES GARCIA PORTUGAL
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Active Aerogels, Unipessoal, Lda.
Universidade De Coimbra
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Application filed by Active Aerogels, Unipessoal, Lda., Universidade De Coimbra filed Critical Active Aerogels, Unipessoal, Lda.
Publication of WO2015016730A2 publication Critical patent/WO2015016730A2/fr
Publication of WO2015016730A3 publication Critical patent/WO2015016730A3/fr

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B30/00—Compositions for artificial stone, not containing binders
    • C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00612—Uses not provided for elsewhere in C04B2111/00 as one or more layers of a layered structure

Definitions

  • Aerogels offer unique physical properties for thermal and acoustic insulation due to their very low thermal conductivity and high porosity. Aerogels are generally used to minimize heat transfer by conduction and convection. Other properties, namely hydrophobicity, help extending the applications of those materials.
  • aerogels can be used in numerous applications involving heating and cooling, particularly in buildings, industrial equipment, satellites, launchers and pipelines.
  • characteristics such as size and flexibility and production costs have limited utilization of aerogels, making the preparation of monoliths a considerable technical challenge for large-scale production. Numerous attempts have been made to improve the performance and maturity of the manufacturing process.
  • This invention relates to a process for the production of silica-based composite aerogels that also contain fibres in the form of felt panels.
  • This invention discloses a method for producing aerogel flexible panels that can be used for thermal insulation in the building, oil and gas, cryogenics, thermoelectric, aeronautical, and space sectors.
  • Other applications of this type of composite aerogel panels include aerosols controlled adsorption, separation of hydrophobic and hydrophilic species, as well as selection of specific chemical functionalities.
  • the high specific surface area of aerogel is attractive for catalysis applications, removal of pollutants from water, controlled release of active species, as well as filtration and percolation of liquids in porous media.
  • State of the art state of the art
  • Aerogel is a porous lightweight synthetic material derived from a gel in which the liquid component of the gel is replaced by a gas, resulting in a solid with extremely low density and thermal conductivity.
  • the first aerogels were synthesized from silica gels and offered unique properties of thermal and acoustic insulation. Initially, aerogels were produced in a granular form and their development was slow because of the time and labour required to complete the process, in addition to other technical difficulties. The technologies for aerogel production have been strengthened in recent decades, being reflected in the growing number of patents and the importance and diversity of applications.
  • Silica aerogel a substance derived from a silica gel, is the most common type of aerogel and the one most studied and applied in a systematic way.
  • Aerogels are sol-gel materials dried carefully to avoid collapse of the pores, creating a solid porous nanostructure with porosity higher than 90%. High porosity leads to some unusual physical properties.
  • silica aerogels can be made with low thermal conductivity ( ⁇ 20 mW m "1 K “1 ) , high surface area ( ⁇ 1000 m 2 g “1 ) and low density ( ⁇ 50 kg m “3 ) .
  • Some aerogel properties particularly chemical (composition, reactivity, hydropho- bicity) , thermal (conductivity, heat capacity, flammabi- lity) , structural (Young's modulus, tensile strength, elastic strain limit) , optical (luminescence, transparency) , acoustic (speed of sound, absorption) and electrical (conductivity, polarization, magnetic susceptibility) , are often unique in the field of synthetic. materials.
  • Silica aerogels can be prepared by various processes, typically comprising four stages: (i) gelation, (ii) aging, (iii) washing, (iv) drying.
  • the first stage involves gelation, i.e. the condensation of one or more silicon precursors to form a matrix based on silica by sol- gel chemistry. The pores of the matrix are filled with reaction by-products and solvent. Gelation is defined as the process corresponding to the transformation of a polymeric or colloidal suspension in a solid permeated by a liquid through continuous formation of a porous three- dimensional solid network, which is uniform throughout the whole solvent and without formation of any precipitate.
  • the second phase we proceed to the aging of the multiphase structure of the gel.
  • Aging is the process in which the material is maintained for a predefined time under controlled environmental conditions, while slowly varying the characteristics of the material.
  • aging is a curing period in which the structure is immersed in a liquid mixture, to obtain a strong solid structure.
  • the third stage includes washing the gel that is an optional step. This step can be used to remove salts or other components from the structure used in the reaction and, in many cases, to replace the solvent in the interior of the solid network by another network that facilitates the subsequent step.
  • the last phase, drying involves solvent extraction without causing the collapse of the structure, leaving the silica nanostructure intact. Drying may be achieved by freezing, at ambient pressure (evaporative drying), or using supercritical fluids.
  • the invention essentially describes a sol-gel process, starting from the precursor methyltrimethoxysilane (MTMS) or methyl- triethoxysilane (MTES) for synthesizing a silica gel and preparing flexible aerogel large monoliths with superior thermal insulation characteristics.
  • MTMS methyltrimethoxysilane
  • MTES methyl- triethoxysilane
  • the reinforced aerogel structure is produced through the incorporation of a felt of fibres. Aerogels have been used for multiple applications, from space to terrestrial applications, to preserve heat or cold, remove moisture, and make cosmetics. Hundreds of patents and utility models about methods, processes, and applications of aerogels are known. Solutions involving aerogel have been used for fire protection and as flame retardant (e.g.
  • JPH11314940 and JP2000182420 have been added to improve the mechanical properties and developing specific technologies (e.g. CN202597930 and KR20100083543) . Aerogels were also used in filament coatings, namely for elastomers (GB1159063 and GB1345944), and proposed for encapsulation applications (e.g. processors), casting (e.g. motors), and multilayer insulation (GB821822, GB980109, and WO2011119745 ) . However, thermal and acoustic insulation are the most common applications of these materials (e.g.
  • Aerogels have been used in the field of electronic and electromechanical parts, including engines (GB1247673 and GB1433478) and engines coating (EP0041203) .
  • Electromechanical applications e.g. for power supplies
  • EP0814520, EP0875950, US5948464, and US6148503 have also been developed. Indeed, applications can be very diverse and these materials were even developed for special niches, including metamaterials (CN102531519) , shape memory alloys (US20100144962 and WO2008057297 ) , and endoscopes ( JP2000107121) .
  • Patents that to some extent relate to the present invention are: CN101698584, CN1749214, JPH0834678, KR100831877, KR20100053350, KR20100083543, KR20100092683, KR20110082379, US5973015, and US6087407.
  • Patent KR20100053350 discloses a method for manufacturing aerogel blankets. The purpose of the invention is the manufacture of aerogel blankets that provide better insulation. The process utilizes tetraethylorthosilicate (TEOS) as precur- sor and fibres to improve elasticity at a large scale.
  • Patent KR20100083543 discusses a method of manufacturing insulating silica aerogel blankets at high temperature, including fibreglass fillers.
  • Patent KR100831877 discloses a method for the preparation of monolithic silica aerogels, which is obtained by drying at normal pressure from the hydrolysis mixture of a precursor of organically modified silicon methanol and oxalic acid.
  • the mixture can contain one or more silanes and preferably comprises MTMS (C 4 Hi 2 0 3 Si) .
  • This method for the preparation of silica aerogel monoliths also results without adding any fibres.
  • Patent KR20100092683 discusses a method of manufacturing a flexible silica aerogel. The material is produced through a drying process with carbon dioxide in a supercritical state. The mixture of solutions containing MTES or TEOS is used to produce small plates of flexible aerogel. Fibres are not included and the material is brittle.
  • Patent KR20110082379 discloses a method for preparation of materials with a high degree of thermal insulation based on fibres impregnated with aerogels. Mixtures of silica gel containing alkoxysilane and isopropyl alcohol are hydrolysed by adding acidic aqueous solutions.
  • the polymerization reaction of the TEOS solution is favoured by addition of small amounts of a basic solution.
  • the silica sol is impregnated into the fibres to produce flexible aerogels.
  • the invention provides a translucent aerogel JPH0834678.
  • the silica skeleton is reinforced with fibres.
  • a well-structured and multilayer fabric is used to make translucent properties.
  • the rigidity of the material obtained is significant.
  • Patents US6087407 and US5973015 discuss a process for manufacturing flexible aerogel composites with improved mechanical stability.
  • the invention relates to a process for the production of aerogels based on organic, flexible, mechanically stable, polymeric condensates of formaldehyde and containing composites that are mixed with glass, carbon, aramid or plastic fibres.
  • Patent CN1749214 discloses a method for preparing composite aerogels for thermal insulation. The process involves the mixture of silicon oxides and titanium fibres, and supercritical drying. The invention requires the use of TEOS, ethanol, deionized water and ammonia with well-defined molar fractions, as well as a vacuum impregnation process.
  • Patent CN101698584 describes a method for preparing a silicon oxide aerogel structure that uses a felt for the purpose of mechanical reinforcement. The method comprises winding of felt, preparation of the silica solution, impregnating the felt, aging, surface treatment, and drying under supercritical conditions.
  • the continuous fibre reinforcement can be selected from the following fibres: glass, aluminium silicate, carbon and basalt; organic felts can also be chosen.
  • the preferred silicon alkoxide used in the process is TEOS.
  • the recommended solvent is ethanol or a mixture of ethanol and isopropanol. According to this method, large composite rolls can be made (e.g. 1x10 m) .
  • the surface treatment consists of trimethylchlorosilane (TMCS) in a solution of 50% ethanol for 32 h after aging at room temperature for 24 h.
  • TMCS trimethylchlorosilane
  • Patent with reference US2012/046469 and the associated document WO2013/009984A2 discuss a method for producing porous gels from a silane and a catalyst solution. A non-supercritical drying of the gel delivers a porous material without elastic recovery. The method is applied to alkyl-linked silanes; it is specifically claimed utilization of MTMS .
  • Filler fibre e.g.
  • Figure 1 illustrates the process of producing composite aerogels, where the sol solution (1) is poured from a container (2) in to a tray (3) containing a felt matrix (4) .
  • Figure 2 shows an image obtained by scanning electron microscopy with the aerogel impregnated in the fibre felt.
  • Figure 3 shows a plot of thermogravimetric analysis where the weight loss is plotted as a function of temperature.
  • Figure 4 presents the stress vs. strain curves of the aerogel composite before and after immersion in liquid nitrogen.
  • Table 1 shows physical properties of aerogel composites described in the document.
  • Silica-based aerogels possess remarkable properties for various applications. However, the applicability of these materials has been limited by the difficulty of making them in larger dimensions. This problem is mainly due to the fragility of the materials; a process suitable to improve the mechanical strength of aerogels is addition of fibres.
  • a felt based on silica-fibres to improve the mechanical properties of aerogels prepared from MTMS and MTES.
  • This felt which is flexible and low density, has fibres arranged uniformly, allowing a homogeneous distribution of the fibres in the final composite material. Additionally, the felt has high thermal and mechanical resistance.
  • the aerogels prepared with MTMS and MTES precursors show very interesting properties, namely high flexibility, very low density and thermal conductivity, and are also hydrophobic.
  • this invention uses a felted fibre of silica and a solution ('sol') prepared from the hydrolysis and condensation reactions of the above precursor solutions.
  • the synthesis process of the final composite material is fairly simple.
  • the solution is prepared using a silica precursor, aqueous solutions of acid and basic catalysts, and an organic solvent. Subsequently, this 'sol' is added in a tray containing the felt, which fits the internal dimensions of the tray. After a few hours a gel is obtained. This gel is kept for a day or more in the same conditions of pressure and temperature to strengthen its solid structure, and the gel is finally dried in an oven at ambient pressure, and subjected to various temperatures between 60 and 200°C.
  • the final aerogel composite has the internal volume of the tray where it is prepared and can have different dimensions, depending only on the size of the tray and the oven where drying occurs. The thickness of the aerogel composite can vary between 1 and 4 cm.
  • the thickness of the fibres felt is between 5 and 15 mm; to increase the thickness of the final composite material, multiple layers of felt are superimposed on each other. In this case, several layers of felt are sewn to prevent felt layers from separating from the aerogel composite. For sewing several layers of felt, a line with high thermal resistance is used.
  • the process presented in this invention allows for production of large flexible panels of aerogel with low density and thermal conductivity, hydrophobic, and an operating temperature range from cryogenic temperatures up to at least 350°C.
  • cryogenic temperatures up to at least 350°C.
  • aerogels such as low density, low thermal conductivity and good performance under extreme temperatures make them appropriate for numerous applications, e.g. building insulation, aerospace devices, cryogenics, etc.
  • their applicability has been limited by the difficulty of preparing these materials in large dimensions, without degrading the structural properties.
  • the present invention overcomes some limitations of these materials, since it describes a way to prepare large pieces of aerogel, maintaining the relevant physical characteristics.
  • the present aerogel synthesis process uses the precursor MTMS, which yields superior properties such as flexibility and hydrophobicity, and is also suitable over a wide range of temperature, from cryogenic temperatures up to at least 350°C.
  • a felt of silica fibres is added (Figure 1) .
  • the felt has very low bulk density ( ⁇ 20 kg nf 3 ) and the fibres are laid homogeneously at a macroscopic scale.
  • the homogeneous distribution of fibres in the felt also ensures fibres uniformity in the final product. Since the felt possesses high mechanical and thermal resistance along with low density, the addition of this felt maintains low density, flexibility and hydrophobicity, but improves the mechanical strength of aerogels prepared from trialkoxysilanes . Furthermore, addition of this felt allows for the preparation of highly flexible aerogels with large dimensions.
  • step (A) preparation of a gel by hydrolysis and condensation reactions of a precursor, (B) aging, while condensation processes are still ongoing, and finally (C) drying.
  • a precursor, a solvent, and an aqueous acid and basic catalyst solution Precursors such as MTMS and MTES can be used.
  • Aqueous solutions of oxalic acid and ammonium hydroxide are used as acid and basic catalysts, respect- tively.
  • the concentration of acid catalyst can vary from 0.001 to 0.1 M and the concentration of the base catalyst should be higher than 5 M.
  • the solvent one or more organic solvents can be used, namely methanol and ethanol .
  • the molar ratio solvent / precursor varies between 15 and 40. Up to 10% of a tetraalkyl orthosilicate (either TMOS or TEOS) can also be added as co-precursor.
  • a tetraalkyl orthosilicate either TMOS or TEOS
  • the solution obtained by adding the precursor, the catalyst, and the solvent is poured to a vessel containing the felt.
  • the felt is trimmed according to the shape of the composite material to be obtained in the end.
  • the thickness of the felt varies between 5 and 15 mm and several layers of felt can be added to increase the final thickness. If several layers of felt are necessary, the felt should be sewn with kevlar, fibreglass, or other line of high thermal and mechanical resistance. Needling prevents the various layers to separate from each other in the final material.
  • the gel takes the shape of the container where the sol was added.
  • samples with specific dimensions can be prepared, e.g. from 250x250 mm with a thickness from 1 to 4 cm.
  • the mass of the felt with respect to the mass of the final aerogel composite is always less than 15%.
  • the size of the final material is only limited by the size of the container used in the production process.
  • the solution is maintained in a controlled environment between 25 and 30°C.
  • the gel obtained is kept between 1 and 4 days under the same conditions of temperature in order to strengthen the solid network (step (B) ) .
  • the gels are placed in an oven for drying at ambient pressure, being subjected to multiple temperature cycles between 60 and 200°C " that may last up to 2-9 days, depending on the thickness of the gel to be dried (step (C) ) .
  • the total drying time is significantly shorter than the time required for drying an aerogel 40 mm thick.
  • Table 1 shows some aerogel properties resulting from the present invention.
  • the density of the resulting material ⁇ 85 kg m ⁇ 3 , is considerably low for a material obtained by drying at ambient pressure.
  • the thermal conductivity measured at room temperature and pressure is 32 mW m "1 K “1 according to the EN12667 and ISO8302 standards.
  • Both components used in this invention, the aerogel and the felt are based in silica, which ensures structural integrity of the final aerogel composite.
  • the integrity of the final material which can be confirmed by the SEM micrograph of Figure 2, leads to small particle shedding, contrary to what happens with aerogels available in the market. Additionally, due to the inorganic character of both felt and aerogel, the material obtained in this invention can be used up to at least 350°C.
  • thermogravimetric analysis Figure 3
  • Figure 4 shows the curves of stress vs. deformation of the aerogel composite before and after immersion in liquid nitrogen.
  • the flexural modulus before and after immersion in liquid nitrogen is 58.5 ⁇ 3.3 and 40.1 ⁇ 4.1 kPa, respectively.
  • the material flexibility is maintained when the aerogel panel is wound and unwound on itself, with a radius of up to 2-3 times the thickness of the panel.
  • the flexible aerogels resulting from this invention have a contact angle of ⁇ 140 degrees, hence confirming their high hydrophobic character .
  • the dimensions of the panel are limited by the length and width of the tray. Increasing in thickness does not significantly reduce flexibility of the material, but increases the drying time.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Silicon Compounds (AREA)
  • Inorganic Fibers (AREA)
  • Nonwoven Fabrics (AREA)

Abstract

Cette invention concerne un procédé de production de grandes pièces d'aérogel. Un feutre de fibres est ajouté à la solution de silice, qui est préparée à partir d'un trialcoxysilane (méthyltriméthoxysilane et méthyltriéthoxysilane). Les propriétés les plus intéressantes de l'aérogel produit à partir de ces trialcoxysilanes sont la flexibilité, la faible masse volumique, la faible thermoconductivité et l'hydrophobicité; ces propriétés sont conservées depuis les températures cryogéniques jusqu'à au moins 350 °C. Les feutres sont utilisés pour améliorer la résistance mécanique des aérogels, ce qui permet la fabrication de pièces de grandes dimensions, qui constituaient une limitation majeure de l'application de ces matériaux. Les applications du matériau décrit ici comprennent l'isolation thermique dans les domaines de la construction, du pétrole et du gaz, de la cryogénie, de la thermoélectricité, de l'aéronautique et de l'espace. Toutefois, en raison de sa surface spécifique élevée, ce matériau est également important pour des applications dans les produits pharmaceutiques et le traitement des eaux usées.
PCT/PT2014/000053 2013-08-02 2014-08-01 Procédé de production de panneau flexibles d'aérogel hydrophobe renforcé de feutres de fibres WO2015016730A2 (fr)

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PT107101 2013-08-02
PT107101A PT107101A (pt) 2013-08-02 2013-08-02 Painéis flexíveis de aerogel hidrofóbico reforçado com feltro de fibras

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WO2015016730A3 WO2015016730A3 (fr) 2015-04-09

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CN105597635A (zh) * 2016-01-29 2016-05-25 卓达新材料科技集团有限公司 一种毛毡/硅铝气凝胶复合保温板的常压干燥方法
EP3208082A1 (fr) * 2016-02-18 2017-08-23 Panasonic Intellectual Property Management Co., Ltd. Matériau d'isolation thermique et son procédé de production
JP2018140554A (ja) * 2017-02-28 2018-09-13 パナソニックＩｐマネジメント株式会社 複合材料およびその製造方法
JP2019098713A (ja) * 2017-12-08 2019-06-24 パナソニックＩｐマネジメント株式会社 断熱材
CN111252775A (zh) * 2018-11-30 2020-06-09 李训谷 气凝胶粒子及其制备方法
CN112376269A (zh) * 2020-11-17 2021-02-19 国佳新材湖北环保凝胶产业园有限公司 一种气凝胶复合纤维毡结构件及其制备方法
WO2022012358A1 (fr) * 2020-07-11 2022-01-20 巩义市泛锐熠辉复合材料有限公司 Procédé de fabrication d'un mat d'aérogel renforcé par des fibres de silicate d'aluminium et cuve de réaction en immersion dans un sol
CN114620736A (zh) * 2021-12-15 2022-06-14 航天海鹰(镇江)特种材料有限公司 一种压缩可控的SiO2气凝胶复合材料制备方法
US20220289939A1 (en) * 2014-10-03 2022-09-15 Aspen Aerogels, Inc. Heat resistant aerogel materials
CN115108809A (zh) * 2022-07-11 2022-09-27 中国人民解放军国防科技大学 一种耐高温改性氧化硅气凝胶隔热复合材料的制备方法
CN115583829A (zh) * 2022-10-26 2023-01-10 中化学华陆新材料有限公司 一种低导热系数纤维复合气凝胶湿法毡及其制备方法
CN115784299A (zh) * 2022-11-29 2023-03-14 航天特种材料及工艺技术研究所 一种不掉粉柔性气凝胶复合材料及其制备方法
CN115849771A (zh) * 2023-03-01 2023-03-28 百能(天津)能源科技有限公司 一种气凝胶毡及其制备方法和应用

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CN106826337B (zh) * 2017-03-02 2019-10-11 航天特种材料及工艺技术研究所 一种耐高温隔热夹层材料构件的数控加工方法

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