ITTO20110201A1 - METHOD FOR THE PREPARATION OF STABLE DISPERSIONS IN THE AQUEOUS PHASE OF POWDERED COMPOUNDS - Google Patents

METHOD FOR THE PREPARATION OF STABLE DISPERSIONS IN THE AQUEOUS PHASE OF POWDERED COMPOUNDS Download PDF

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Publication number
ITTO20110201A1
ITTO20110201A1 IT000201A ITTO20110201A ITTO20110201A1 IT TO20110201 A1 ITTO20110201 A1 IT TO20110201A1 IT 000201 A IT000201 A IT 000201A IT TO20110201 A ITTO20110201 A IT TO20110201A IT TO20110201 A1 ITTO20110201 A1 IT TO20110201A1
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aqueous phase
dispersions
dispersion
preparation
colloidal system
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IT000201A
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Italian (it)
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Salvatore Cotugno
Paolo Fiorenza
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Bridgestone Corp
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Priority to IT000201A priority Critical patent/ITTO20110201A1/en
Priority to PCT/IB2012/051070 priority patent/WO2012120461A1/en
Publication of ITTO20110201A1 publication Critical patent/ITTO20110201A1/en

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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/02Emulsion paints including aerosols
    • C09D5/024Emulsion paints including aerosols characterised by the additives
    • C09D5/027Dispersing agents
    • 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
    • C04B40/00Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039Premixtures of ingredients
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D1/00Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/02Emulsion paints including aerosols
    • C09D5/024Emulsion paints including aerosols characterised by the additives
    • C09D5/028Pigments; Filters
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/45Anti-settling agents
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/70Additives characterised by shape, e.g. fibres, flakes or microspheres

Description

DESCRIZIONE DESCRIPTION

del brevetto per invenzione industriale dal titolo: of the patent for industrial invention entitled:

"METODO PER LA PREPARAZIONE DI DISPERSIONI STABILI IN FASE ACQUOSA DI COMPOSTI IN POLVERE" "METHOD FOR THE PREPARATION OF STABLE WATER-PHASE DISPERSIONS OF POWDER COMPOUNDS"

La presente invenzione è relativa ad un metodo per la preparazione di dispersioni stabili in fase acquosa di composti in polvere. The present invention relates to a method for the preparation of stable dispersions in aqueous phase of powdered compounds.

Generalmente, le dispersioni per poter soddisfare le necessità per le quali sono state realizzate, devono risultare particolarmente stabili e presentare una corretta dispersione degli ingredienti che le compongono. Generally, in order to satisfy the needs for which they were made, the dispersions must be particularly stable and present a correct dispersion of the ingredients that compose them.

Recentemente, a causa delle regolamentazioni normative sull'uso dei solventi organici (vedi ad esempio la direttiva europea 1999/13/CE) le dispersioni in fase acquosa hanno suscitato un sempre maggiore interesse in campo industriale. Infatti, l'utilizzo delle dispersioni in fase acquosa garantisce una omogenea dispersione degli ingredienti senza per questo dover coinvolgere l'impiego di solventi organici. Recently, due to the regulatory regulations on the use of organic solvents (see for example the European directive 1999/13 / EC), dispersions in the aqueous phase have aroused increasing interest in the industrial field. In fact, the use of the aqueous phase dispersions guarantees a homogeneous dispersion of the ingredients without having to involve the use of organic solvents.

Alcuni ingredienti quando aggiunti ad una dispersione acquosa possono essere soggetti a fenomeni di agglomerazione e/o precipitazione compromettendo, così, la loro omogenea dispersione. Esempi di questi ingredienti si possono trovare nella classe dei silicati come l'argilla, la mica e il caolino. Some ingredients when added to an aqueous dispersion may be subject to agglomeration and / or precipitation phenomena thus compromising their homogeneous dispersion. Examples of these ingredients can be found in the class of silicates such as clay, mica and kaolin.

Nell'arte nota il problema relativo all'agglomerazione e alla precipitazione di alcuni ingredienti sono stati superati mediante l'utilizzo di tensioattivi in qualità di agenti disperdenti. Spesso l'utilizzo dei tensioattivi nella dispersione in fase acquosa può comprometterne l'efficacia nell'applicazione finale. In the known art, the problem relating to the agglomeration and precipitation of some ingredients has been overcome by using surfactants as dispersing agents. Often the use of surfactants in the aqueous phase dispersion can compromise its effectiveness in the final application.

Era quindi sentita l'esigenza di disporre di un metodo alternativo che garantisse la preparazione delle dispersioni in fase acquosa senza il verificarsi dei fenomeni di agglomerazione e precipitazione. The need was therefore felt to have an alternative method that would guarantee the preparation of the dispersions in the aqueous phase without the occurrence of agglomeration and precipitation phenomena.

Oggetto della presente invenzione è un metodo per la preparazione di dispersioni in fase acquosa di un composto in polvere caratterizzato dal fatto che detta fase acquosa comprende un sistema colloidale di particelle nanometriche atte a realizzare una dispersione del detto composto in polvere. The object of the present invention is a method for the preparation of dispersions in aqueous phase of a powdered compound characterized in that said aqueous phase comprises a colloidal system of nanometric particles suitable for producing a dispersion of said compound in powder form.

Preferibilmente, il sistema colloidale è realizzato con particelle nanometriche di ossido inorganico. Preferably, the colloidal system is made with nanometric particles of inorganic oxide.

Preferibilmente, le particelle nanometriche di ossido inorganico comprendono silice ad elevata area superficiale. Preferibilmente, il sistema colloidale comprende da 1 al 50 % p/v, più preferibilmente da 20 al 40 % p/v, di detta silice ad elevata area superficiale. Preferably, the nano-sized particles of inorganic oxide comprise silica with a high surface area. Preferably, the colloidal system comprises from 1 to 50% w / v, more preferably from 20 to 40% w / v, of said silica with a high surface area.

Preferibilmente, il composto in polvere è compreso nel gruppo composto da caolino, feldspar, mica, silice, allumina, betonite, argilla. Preferably, the powdered compound is included in the group consisting of kaolin, feldspar, mica, silica, alumina, betonite, clay.

Come alternativa a quanto sopra indicato, preferibilmente il sistema colloidale è realizzato con particelle nanometriche di materiale organico. As an alternative to the above, the colloidal system is preferably made with nanometric particles of organic material.

Preferibilmente, le particelle nanometriche di materiale organico comprendono nanotubi di carbonio. Preferably, the nanometric particles of organic material comprise carbon nanotubes.

Preferibilmente, il composto in polvere è Nero di Carbonio. Preferably, the powdered compound is Carbon Black.

Un ulteriore oggetto della presente invenzione è una dispersione realizzata con il metodo sopra definito. A further object of the present invention is a dispersion carried out with the method defined above.

Ancora un ulteriore oggetto della presente invenzione è un materiale solido ottenuto dalla dispersione realizzata con il metodo sopra definito. Still a further object of the present invention is a solid material obtained from the dispersion carried out with the method defined above.

Per una migliore comprensione dell'invenzione, di seguito sono riportati degli esempi di realizzazione a scopo illustrativo e non limitativo con l'ausilio delle figure annesse, (Figg. la e lb) le quali sono due immagini relative ad una analisi SEM dei materiali seccati provenienti da due differenti dispersioni. For a better understanding of the invention, examples of embodiment are reported below for illustrative and non-limiting purposes with the aid of the attached figures, (Figs. La and lb) which are two images relating to a SEM analysis of the dried materials coming from two different dispersions.

ESEMPI EXAMPLES

Sono state realizzate cinque dispersioni (A - E), la prima delle quali (A) è una dispersione di confronto in cui non è stato utilizzato il sistema colloidale, mentre le altre (B - E) si riferiscono a dispersioni secondo la presente invenzione in cui è stato variato il contenuto di arqilla. Five dispersions (A - E) were made, the first of which (A) is a comparison dispersion in which the colloidal system was not used, while the others (B - E) refer to dispersions according to the present invention in which the arqilla content has been varied.

Le dispersioni sono state preparate pesando nel beaker di preparazione la quantità di arqilla in polvere ed aqqiunqendovi 50 mi di acqua per la dispersione di confronto (A) o 50 mi del sistema colloidale acqua e silice al 30 % p/V per le dispersioni dell'invenzione (B - E). Le soluzioni, così realizzate venqono sottoposte ad una azione di miscelazione mediante un aqitatore maqnetico in rotazione (10 minuti) e, successivamente, mediante l'azione di ultrasuoni (15 minuti). The dispersions were prepared by weighing the quantity of powdered clay in the preparation beaker and adding 50 ml of water for the comparison dispersion (A) or 50 ml of the colloidal system of water and silica at 30% w / V for the dispersions of the invention (B - E). The solutions thus obtained are subjected to a mixing action by means of a mechanical stirrer in rotation (10 minutes) and, subsequently, by the action of ultrasounds (15 minutes).

In Tabella I sono riportate le composizioni delle dispersioni. Sempre in Tabella I, per oqnuna delle dispersioni preparate sono riportati una verifica visiva relativa alla presenza di precipitato dopo 24h dalla formazione della dispersione, ed il rispettivo indice di separazione. L'indice di separazione rappresenta la separazione dopo 24h dalla formazione della dispersione tra una prima fase composta solamente dal sistema colloidale ed una seconda fase composta invece dal sistema colloidale e argilla. In particolare, l'indice di separazione è calcolato da hs/htotxl00, dove hsè l'altezza del sistema colloidale con argilla e htotè l'altezza complessiva (prima e seconda fase) nel beaker di preparazione. Come può sembrare ovvio, l'indice di separazione non può riguardare la dispersione (A) di confronto in quanto questa non comprende il sistema colloidale. In Table I the compositions of the dispersions are reported. Also in Table I, for each of the prepared dispersions a visual check of the presence of precipitate after 24h from the formation of the dispersion, and the respective separation index are reported. The separation index represents the separation after 24h from the formation of the dispersion between a first phase composed only of the colloidal system and a second phase composed instead of the colloidal system and clay. In particular, the separation index is calculated from hs / htotxl00, where hs is the height of the colloidal system with clay and htot is the overall height (first and second phase) in the preparation beaker. As it may seem obvious, the separation index cannot relate to the comparison dispersion (A) as this does not include the colloidal system.

TABELLA I TABLE I

A B C D E ACQUA (mi) 50 A B C D E WATER (mi) 50

SISTEMA COLLOIDALE (mi) 50 50 50 50 ARGILLA (g) 12,5 8,32 12,5 16 20 Precipitazione SI NO NO NO NO Indice di separazione * 72 31 17 0 Il sistema colloidale utilizzato è commercializzato con il nome commerciale LUDOX SM-30 fornito dalla società Grace Davision e comprende un 30% p/V di una silice in acqua con una area superficiale pari a 330 m<2>/g ed una granulometria pari a 7 nm. ;Dalla Tabella I si evince come solo nelle dispersioni in cui la fase acquosa è costituita dal sistema colloidale non si verifica la precipitazione dell'argilla. ;Le figure la e lb sono relative ad immagini dell'analisi SEM di materiali solidi ottenuti dalla evaporazione dell'acqua rispettivamente della dispersione A e della dispersione E. ;Da un confronto delle immagini di cui sopra è possibile constatare che mentre lo strato di materiale ottenuto dalla dispersione A (figura la) presenta una evidente formazione di agglomerati, lo strato di materiale ottenuto dalla dispersione E (figura lb) presenta invece un elevato grado di impaccamento a densità omogenea. Tali evidenze dimostrano in maniera incontrovertibile la differente omogeneizzazione del composto in polvere nelle due rispettive dispersioni. ;Dai dati ottenuti si evince come la presenza di uno stato colloidale compreso nella fase acquosa, garantisca la stabilità nel tempo della dispersione di un composto in polvere. Inoltre, con il metodo oggetto della presente invenzione è possibile ottenere un materiale con un elevato grado di impaccamento a densità omogenea con gli ovvi vantaggi applicativi che questo comporta. *COLLOIDAL SYSTEM (mi) 50 50 50 50 CLAY (g) 12.5 8.32 12.5 16 20 Precipitation YES NO NO NO NO Separation index * 72 31 17 0 The colloidal system used is marketed under the trade name LUDOX SM -30 supplied by Grace Davision and includes 30% w / V of a silica in water with a surface area of 330 m <2> / g and a grain size of 7 nm. From Table I it can be seen that clay precipitation does not occur only in the dispersions in which the aqueous phase is constituted by the colloidal system. ; Figures la and lb relate to images of the SEM analysis of solid materials obtained from the evaporation of water respectively of dispersion A and dispersion E. obtained from dispersion A (figure la) shows an evident formation of agglomerates, the layer of material obtained from dispersion E (figure 1b) on the other hand has a high degree of packing at homogeneous density. These evidences indisputably demonstrate the different homogenization of the powder compound in the two respective dispersions. From the data obtained it can be seen that the presence of a colloidal state included in the aqueous phase guarantees the stability over time of the dispersion of a powdered compound. Furthermore, with the method object of the present invention it is possible to obtain a material with a high degree of packing at homogeneous density with the obvious application advantages that this entails. *

Claims (11)

RIVENDICAZIONI 1. Metodo per la preparazione di dispersioni in fase acquosa di un composto in polvere caratterizzato dal fatto che detta fase acquosa comprende un sistema colloidale di particelle nanometriche atte a realizzare la dispersione del detto composto in polvere. CLAIMS 1. Method for preparing dispersions in aqueous phase of a powdered compound characterized in that said aqueous phase comprises a colloidal system of nanometric particles suitable for achieving the dispersion of said powdered compound. 2. Metodo per la preparazione di dispersioni in fase acquosa secondo la rivendicazione 1, caratterizzato dal fatto che detto sistema colloidale è realizzato con particelle nanometriche di ossido inorqanico. 2. Method for the preparation of dispersions in aqueous phase according to claim 1, characterized in that said colloidal system is made with nanometric particles of inorganic oxide. 3. Metodo per la preparazione di dispersioni in fase acquosa secondo la rivendicazione 2, caratterizzato dal fatto che le dette particelle nanometriche di ossido inorqanico comprendono silice ad elevata area superficiale. 3. Method for the preparation of dispersions in aqueous phase according to claim 2, characterized in that said nanometric particles of inorganic oxide comprise silica with a high surface area. 4. Metodo per la preparazione di dispersioni in fase acquosa secondo la rivendicazione 3, caratterizzato dal fatto che il sistema colloidale comprende da 1 al 50 % p/v di detta silice ad elevata area superficiale. 4. Method for preparing dispersions in aqueous phase according to claim 3, characterized in that the colloidal system comprises from 1 to 50% w / v of said silica with a high surface area. 5. Metodo per la preparazione di dispersioni in fase acquosa secondo la rivendicazione 4, caratterizzato dal fatto che il sistema colloidale comprende da 20 al 40 % p/v di detta silice ad elevata area superficiale. 5. Method for preparing dispersions in aqueous phase according to claim 4, characterized in that the colloidal system comprises from 20 to 40% w / v of said silica with a high surface area. 6. Metodo per la preparazione di dispersioni in fase acquosa secondo una delle rivendicazioni precedenti, caratterizzato dal fatto che detto composto in polvere è compreso nel gruppo composto da caolino, feldspar, mica, silice, allumina, betonite, argilla. 6. Method for preparing dispersions in aqueous phase according to one of the preceding claims, characterized in that said powder compound is included in the group consisting of kaolin, feldspar, mica, silica, alumina, betonite, clay. 7. Metodo per la preparazione di dispersioni in fase acquosa secondo la rivendicazione 1, caratterizzato dal fatto che detto sistema colloidale è realizzato con particelle nanometriche di materiale organico. 7. Method for preparing dispersions in aqueous phase according to claim 1, characterized in that said colloidal system is made with nanometric particles of organic material. 8. Metodo per la preparazione di dispersioni in fase acquosa secondo la rivendicazione 7, caratterizzato dal fatto che dette particelle nanometriche di materiale organico comprendono nanotubi di carbonio. 8. Method for preparing dispersions in aqueous phase according to claim 7, characterized in that said nanometric particles of organic material comprise carbon nanotubes. 9. Metodo per la preparazione di dispersioni in fase acquosa secondo la rivendicazione 8, caratterizzato dal fatto che detto composto in polvere è Nero di Carbonio. 9. Method for the preparation of dispersions in aqueous phase according to claim 8, characterized in that said powdered compound is Carbon Black. 10. Dispersione in fase acquosa caratterizzata dal fatto di essere stata realizzata con il metodo secondo una delle rivendicazioni precedenti. 10. Dispersion in aqueous phase characterized in that it has been carried out with the method according to one of the preceding claims. 11. Materiale solido ottenuto da una dispersione secondo la rivendicazione 10.Solid material obtained from a dispersion according to claim 10.
IT000201A 2011-03-07 2011-03-07 METHOD FOR THE PREPARATION OF STABLE DISPERSIONS IN THE AQUEOUS PHASE OF POWDERED COMPOUNDS ITTO20110201A1 (en)

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IT000201A ITTO20110201A1 (en) 2011-03-07 2011-03-07 METHOD FOR THE PREPARATION OF STABLE DISPERSIONS IN THE AQUEOUS PHASE OF POWDERED COMPOUNDS
PCT/IB2012/051070 WO2012120461A1 (en) 2011-03-07 2012-03-07 Method of producing stable liquid dispersions of powder compounds in an aqueous medium

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US20140090842A1 (en) * 2012-09-28 2014-04-03 Halliburton Energy Services, Inc. Cement Compositions Comprising Deagglomerated Inorganic Nanotubes and Associated Methods

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EP1348677A2 (en) * 2002-03-21 2003-10-01 Halliburton Energy Services, Inc. Storable water-silica suspensions for use in well cements
US20050051057A1 (en) * 2003-09-09 2005-03-10 Evans Timothy O. Thermal protective coating for ceramic surfaces
WO2006079098A1 (en) * 2005-01-24 2006-07-27 Lubrizol Advanced Materials, Inc. Aqueous dispersions of nanoparticle/polyurethane composites
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WO2009099640A1 (en) * 2008-02-08 2009-08-13 Northwestern University Highly-dispersed carbon nanotube-reinforced cement-based materials

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US20050051057A1 (en) * 2003-09-09 2005-03-10 Evans Timothy O. Thermal protective coating for ceramic surfaces
WO2006079098A1 (en) * 2005-01-24 2006-07-27 Lubrizol Advanced Materials, Inc. Aqueous dispersions of nanoparticle/polyurethane composites
WO2009099640A1 (en) * 2008-02-08 2009-08-13 Northwestern University Highly-dispersed carbon nanotube-reinforced cement-based materials
CN101328389A (en) * 2008-07-25 2008-12-24 魏大勇 Nanometer grade environment-friendly type color aqueous waterproof coating material

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