Production of suspensions of hydrophobic oxide particles
Abstract
Disclosed are a process for producing a suspension of hydrophobic oxidic particles which has a defined, adjustable viscosity, which comprises suspending low structured hydrophobic oxidic particles in at least one organic suspension agent and then adding from 0.05% to 15% by weight based on the suspension medium of high structured hydrophobic oxidic particles, a suspension of hydrophobic oxidic particles which has a defined, adjustable viscosity and the use thereof for producing soil and water repellent coatings on articles.
Term
Term ended
Expired 26 September 2023, 3 years ago.
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17 claims: 10 independent, 7 dependent
- 1Verfahren zur Herstellung einer Suspension von hydrophoben Oxidpartikeln mit definierter, einstellbarer Viskosität, dadurch gekennzeichnet, dass niedrigstrukturierte hydrophobe Oxidpartikel in zumindest einem organischen Suspensionsmittel suspendiert werden und anschließend von 0,05 bis 15 Gew.-% bezogen auf das Suspensionsmedium an hochstrukturierten hydrophoben Oxidpartikeln zugegeben werden, wobei unter niedrigstrukturierten hydrophoben Oxidpartikeln hydrophobe Oxidpartikel verstanden werden, die gegenüber den entsprechenden hochstrukturierten hydrophoben Oxidpartikeln eine um mindestens 30 % verringerte Dibutylphthalat-Absorption und eine um mindestens 50 % erhöhte Stampfdichte aufweisen.
- 2Verfahren gemäß Anspruch 1, dadurch gekennzeichnet, dass als hydrophobe Oxidpartikel hydrophobe pyrogene Oxidpartikel oder hydrophobe gefällte Oxidpartikel eingesetzt werden.
- 3Verfahren gemäß Anspruch 1 oder 2, dadurch gekennzeichnet, dass hydrophobe pyrogene Oxidpartikel bestehend aus einem Material, ausgewählt aus Siliziumoxid, Aluminiumoxid, Zirkoniumoxid, Titanoxid oder eine Mischung dieser Materialien, eingesetzt werden.
- 4Verfahren gemäß zumindest einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass als hydrophobe pyrogene Oxidpartikel hydrophobe pyrogene Kieselsäuren eingesetzt werden.
- 5Verfahren gemäß zumindest einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, dass 0,05 bis 2,5 Gew.-% an niedrigstrukturierten hydrophoben Oxidpartikeln bezogen auf das Suspensionsmedium eingesetzt werden.
- 6Verfahren gemäß zumindest einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, dass ein organisches Suspensionsmittel, ausgewählt aus Alkoholen, Ketonen, Ether, Ester, aliphatischen oder aromatischen Kohlenwasserstoffen, Amide oder Sulfoxide, eingesetzt wird.
- 7Verfahren gemäß zumindest einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, dass als Suspensionsmedium ein Suspensionsmedium eingesetzt wird, das neben dem organischen Suspensionsmittel Wasser enthält.
- 8Suspension von hydrophoben Oxidpartikeln mit definierter, einstellbarer Viskosität, dadurch gekennzeichnet, dass niedrigstrukturierte hydrophobe Oxidpartikel und 0,05 bis 15 Gew.-% bezogen auf das Suspensionsmedium an hochstrukturierten hydrophoben Oxidpartikel in zumindest einem organischen Suspensionsmittel suspendiert vorliegen, wobei unter niedrigstrukturierten hydrophoben Oxidpartikeln hydrophobe Oxidpartikel verstanden werden, die gegenüber den entsprechenden hochstrukturierten hydrophoben Oxidpartikeln eine um mindestens 30 % verringerte Dibutylphthalat-Absorption und eine um mindestens 50 % erhöhte Stampfdichte aufweisen.
- 9Suspension gemäß Anspruch 8 hergestellt nach einem Verfahren gemäß zumindest einem der Ansprüche 1 bis 7.
- 10Suspension gemäß Anspruch 8 oder 9, dadurch gekennzeichnet, dass die Suspension 0,05 bis 2,5 Gew.-% an hydrophoben niedrigstrukturierten Oxidpartikel bezogen auf das Suspensionsmedium aufweist.
- 11Suspension gemäß zumindest einem der Ansprüche 8 bis 10, dadurch gekennzeichnet, dass die Suspension eine dynamische Viskosität von 1,0 bis 1000 mPa s bei einer Scherrate von größer 20 s -1 ausweist.
- 12Suspension gemäß zumindest einem der Ansprüche 8 bis 11, dadurch gekennzeichnet, dass das Suspensionsmedium neben dem organischen Suspensionsmittel Wasser aufweist.
- 13Verwendung der Suspension gemäß zumindest einem der Ansprüche 8 bis 12 zur Herstellung von schmutz- und wasserabweisenden Beschichtungen auf Gegenständen.
- 14Verwendung gemäß Anspruch 13, dadurch gekennzeichnet, dass die Suspension auf zumindest einer Oberfläche eines Gegenstandes aufgebracht und das Suspensionsmedium anschließend entfernt wird.
- 15Verwendung gemäß Anspruch 13 oder 14, dadurch gekennzeichnet, dass die Suspension mittels eines Rakels aufgetragen wird.
- 16Verwendung gemäß zumindest einem der Ansprüche 13 bis 15 zur Herstellung von schmutz- und wasserabweisenden Beschichtungen auf Textilien.
- 17Verwendung gemäß Anspruch 16 zur Herstellung von Bekleidung, technischen Textilien und Geweben des textilen Bauens.
Independent claims17
56 paragraphs, as filed
The invention relates to a process for the preparation of a suspension of hydrophobic oxide particles with a defined, adjustable viscosity, as well as a suspension of hydrophobic oxide particles with a defined, adjustable viscosity and their use for the production of dirt- and water-repellent coatings on articles.
Suspensions of hydrophobic, nanostructured particles are used in the production of dirt- and water-repellent coatings on articles and textile fabrics. In the preparation of these coatings, hydrophobic particles are applied to the surface of an article, thus creating a surface structure with elevations on the surface of the article having dirt and water repellency.
The principle of self-cleaning coatings is generally known. In order to achieve good self-cleaning of a surface, the surface must have a certain roughness in addition to a very hydrophobic surface. A suitable combination of structure and hydrophobicity makes it possible for already small amounts of moving water to carry dirt particles adhering to the surface, thus cleaning the surface (<patcit id="pcit0001" dnum="WO9604123A"><text>WO 96/04123</text></patcit>; <patcit id="pcit0002" dnum="US3354022A"><text>US 3,354,022</text></patcit>).
Out <patcit id="pcit0003" dnum="EP0933388A"><text>EP 0 933 388</text></patcit> A process for the production of structured surfaces with hydrophobic properties is known, in which a negative form is first produced by photolithography, a plastic film is embossed with this negative form, and then the plastic film is hydrophobized with fluoroalkylsilanes.
The <patcit id="pcit0004" dnum="EP0909747A"><text>EP-A 0 909 747</text></patcit> Describes a process for producing a self-cleaning property on ceramic bodies, such as, for example, roof tiles, in which a dispersion of clay particles in an organic silicone resin solution is applied to the ceramic body and the coating subsequently cures.
From the <patcit id="pcit0005" dnum="JP7328532A"><text>JP 7328532-A</text></patcit> A coating process is known in which finely divided particles with a hydrophobic surface are applied to a moist lacquer and hardened. Water repellent surfaces are obtained.
In <patcit id="pcit0006" dnum="DE10022246A1"><text>DE 100 22 246 A1</text></patcit> Describes a process in which hydrophobic nanostructured particles are used together with an adhesive or a glue-like component in spray form. By means of this method, structured surfaces are produced which, however, are not permanently stable.
The methods described in the prior art for producing surfaces which are difficult to wet are either very complex or lead to unsatisfactory results. The production of a structured surface by embossing processes is complex and can only be used economically on planar surfaces. Surfaces in which structuring is achieved by subsequent application of hydrophobic particles can often be poorly reproduced or have only a low mechanical load-bearing capacity. This process is also very complex. Furthermore, fluorine-organic compounds or fluorine-containing polymers are often required, which are not only very expensive, but also ecologically very serious.
In the German patent application <patcit id="pcit0007" dnum="DE10135157"><text>DE 101 35 157</text></patcit> A method for applying a self-cleaning coating to textiles is described. In this process, hydrophobic nanostructured fumed silicas are admixed with the chemical cleaning agents, such as, for example, perchlorethylene, tetrachlorethylene or heavy benzine, and a self-cleaning, water-repellent effect on the garments is generated following the chemical cleaning. Ecologically safe halogen-containing solvents are also used in this process.
One possibility for producing self - cleaning textile surface structures with water - repellent surfaces is described <patcit id="pcit0008" dnum="DE10118346"><text>German patent application DE 101 18 346</text></patcit>. The suspensions of hydrophobic structured particles described in this application have the disadvantage that these suspensions can only be applied to the corresponding textiles by means of immersion processes or transfer processes and the particles are firmly anchored in the polymer fiber surface by dissolving the polymer fiber.
In <patcit id="pcit0009" dnum="EP1249468A2"><text>EP 1 249 468 A2</text></patcit> Self-cleaning polymer surfaces are disclosed by hydrophobic structures which are solubilized by a solvent and particles which are not dissolved are deposited on these polymer surfaces. After the solvent has been removed, the polymer surfaces harden again and fix the particles, which are partially stuck in the surfaces. Also in this application, the particles suspended in a solvent have the disadvantage that they are firmly anchored therein only by dissolving the polymer surface in the same. It was therefore the object of the present invention to provide a process for the preparation of a suspension of hydrophobic oxide particles with a defined, adjustable viscosity so as to provide further application methods for suspensions of hydrophobic oxide particles, for example the doctoring process, in addition to the known processes, for example dipping or spraying To use.
Surprisingly, it has been found that suspensions of hydrophobic oxide particles with a defined, adjustable viscosity can be prepared by suspending low-structured hydrophobic oxide particles in at least one organic suspending agent and subsequently adding from 0.05 to 15% by weight, based on the suspension medium, to highly structured hydrophobic oxide particles . According to the method according to the invention, suspensions which, by virtue of their adjustable viscosity, permit application processes which represent a lower investment and a lower environmental impact due to evaporating suspending agents. The circumstance proves to be particularly advantageous,
The present invention provides a process for the preparation of a suspension of hydrophobic oxide particles with a defined, adjustable viscosity wherein low-structured hydrophobic oxide particles are suspended in at least one organic suspending agent and subsequently 0.05 to 15% by weight, based on the suspension medium, of highly structured hydrophobic oxide particles Hydrophobic oxide particles are understood to mean hydrophobic oxide particles which have a dibutyl phthalate absorption which is at least 30% lower than the corresponding highly-structured hydrophobic oxide particles and a tamping density which is at least 50% higher.
The present invention also provides suspensions of hydrophobic oxide particles with a defined, adjustable viscosity and their use for the production of dirt-repellent and water-repellent coatings on articles.
The process according to the invention makes suspensions of hydrophobic oxide particles with a defined, adjustable viscosity accessible. Thus, suspensions of hydrophobic oxide particles with a higher viscosity than in the prior art and also pastes of hydrophobic oxide particles can now be produced. The suspensions prepared with the aid of the process according to the invention therefore make it possible to use other application methods, such as, for example, the doctoring process. According to the prior art, the suspensions of hydrophobic oxide particles are sprayed on or the object to be coated is immersed in the suspension of the hydrophobic oxide particles. This results in higher investment costs for the application of the hydrophobic oxide particles and also a higher environmental impact due to the higher proportion of organic suspensions. The suspensions according to the invention are particularly suitable for the self-cleaning and water-repellent coating of textiles since a doctoring process is already used here for the coatings according to the prior art, for example with polyurethane coating compositions.
The process for the preparation of a suspension with a defined, adjustable viscosity of hydrophobic oxide particles is distinguished by the fact that low-structured hydrophobic oxide particles are suspended in at least one organic suspending agent and then preferably from 0.05 to 15% by weight, preferably from 1 to 12% by weight, By weight, particularly preferably from 2 to 10% by weight, based on the suspension medium, of highly structured hydrophobic oxide particles.
In the process according to the invention, hydrophobic pyrogenic oxide particles, consisting of a material selected from silicon oxide, aluminum oxide, zirconium oxide, titanium oxide or a mixture of these materials, or hydrophobic precipitated oxide particles selected from silicon oxide, aluminum oxide, Zirconium oxide, titanium oxide or a mixture of these materials, preferably hydrophobic precipitated silicic acids. Particular preference is given to using hydrophobic pyrogenic silicas in the process according to the invention. In a particular embodiment of the process according to the invention, a mixture of low-structured hydrophobic oxide particles is used. However, a mixture of highly structured hydrophobic oxide particles can also be used.
The hydrophobicity of the oxide particles may be inherent or the oxide particles may have been rendered hydrophobic in a manner known to the person skilled in the art (series of pigments, number 18, Degussa AG). This is preferably effected by a treatment with at least one compound selected from the group of alkylsilanes, alkyldisilazanes, for example with hexamethyldisilazane, or perfluoroalkylsilanes.
In a first process step of the process according to the invention, preferably from 0.05 to 2.5% by weight, preferably from 0.1 to 2.0% by weight, particularly preferably from 0.5 to 1.2% by weight, Based on the suspension medium, to low-structure hydrophobic oxide particles in at least one organic suspending agent.
Alcohols, ketones, ethers, esters, aliphatic or aromatic hydrocarbons, amides or sulfoxides can be used as suspending agents in the process according to the invention. In a particular embodiment of the process according to the invention, it is also possible to use mixtures of the abovementioned suspension media, preferably a suspension medium which, in addition to the organic suspension medium or the organic suspension medium mixture, contains water.
The dibutyl phthalate absorption (DBP absorption) is measured according to DIN 53 601. The tamp density is measured according to DIN 53 194. For example, the Aerosil R 812 S has a tamped density of 50 g / l as a highly-structured hydrophobic fumed silica, whereas the Aerosil VP LE 8241 has a tamped density of 140 g / l as low-structured hydrophobic pyrogenic silica.
The low-structured hydrophobic oxide particles can be produced by means of a dry-milling method according to <patcit id="pcit0010" dnum="EP0637616B1"><text>EP 0 637 616 B1</text></patcit> or <patcit id="pcit0011" dnum="US5959005A"><text>US 5,959,005</text></patcit> Can be produced from highly structured hydrophobic oxide particles, which is an intensive grinding process which leads to a destructuring of the oxide particles beyond the normal reduction in the particle size. This is an irreversible process.
In a particular embodiment of the process according to the invention, aerosols are used as both low-molecular and highly-structured hydrophobic pyrogenic oxide particles<sup>®</sup> Respectively. As a low-structure hydrophobic aerosil<sup>®</sup> The aerosil is preferred<sup>®</sup> VP LE 8241 is used. The Aerosil<sup>®</sup> In this particular embodiment of the process according to the invention, R 812 S is used as a highly structured hydrophobic aerosol<sup>®</sup> Respectively.
The low-structured hydrophobic oxide particles used in the method according to the invention preferably have a surface with an irregular fine structure in the nanometer range, that is to say in the range from 1 nm to 1000 nm, preferably from 2 nm to 750 nm and very particularly preferably from 10 nm to 100 nm . A fine structure is understood to mean structures having heights, peaks, gaps, ridges, cracks, undercuts, notches and / or holes in the abovementioned distances and regions. The fine structure of the low-structured hydrophobic oxide particles can preferably have elevations with an aspect ratio of greater than 1, particularly preferably greater than 1.5. The aspect ratio, in turn, is defined as the quotient of maximum height to maximum width of the survey,
Preference is given to using low-structured hydrophobic oxide particles in the process according to the invention which have an average particle diameter of from 0.005 μm to 100 μm, preferably from 0.01 μm to 50 μm and particularly preferably from 0.01 μm to 30 μm. Thus, it is also possible to use low-structured hydrophobic oxide particles which accumulate in the suspension medium from primary particles to form agglomerates or aggregates with a size of 0.02 μm to 100 μm.
For the destruction of possibly existing agglomerates, it is advantageous to carry out the suspension of the hydrophobic oxide particles with high shear energy inputs, for example by means of a dissolver disk. The use of turbulence-increasing internals such as flow breakers or other obstacles which serve to prevent the formation of water rollers can also be advantageous. The Reynolds number is preferably above 2320. The Richardson number sets the strength of the thermal stratification in a ratio to the magnitude of the shear of a flow. It is thus a measure of the ratio of the magnitudes which are responsible for the propagation or decay of the turbulence. The Richardson number refers to a local gradient at a point of the flow, for the method according to the invention the Richardson number lies at a maximum of 0.25.
Depending on the amount of highly structured hydrophobic oxide particles added, suspensions with dynamic viscosities at a shear rate of> 20 s can be used<sup>-1</sup> Preferably from 1.0 to 1000 mPa s, preferably from 1 to 500 mPa s, more preferably from 1 to 400 mPa s. For an amount of highly structured hydrophobic oxide particles such as the Aerosil<sup>®</sup> R 812 S, of ≥ 5% by weight, based on the suspension medium, even suspension with a structure-viscous flow behavior can be produced by means of the process according to the invention.
The suspension according to the invention of hydrophobic oxide particles with a defined, adjustable viscosity is characterized in that low-structured hydrophobic oxide particles and from 0.05 to 15% by weight, based on the suspension medium, are suspended in highly structured hydrophobic oxide particles suspended in at least one organic suspending agent Structurally hydrophobic oxide particles are hydrophobic oxide particles which have a dibutyl phthalate absorption which is at least 30% lower than the corresponding highly structured hydrophobic oxide particles and a tamping density which is at least 50% higher.
In the suspension according to the invention of hydrophobic oxide particles with a defined, adjustable viscosity, preference is given to suspending the suspension medium with highly structured hydrophobic oxide particles suspended in at least one organic suspending agent, preferably from 1 to 12% by weight and particularly preferably from 2 to 10% by weight.
The suspension according to the invention preferably has from 0.05 to 2.5% by weight, preferably from 0.1 to 2.0% by weight, particularly preferably from 0.5 to 1.2% by weight, based on the suspension medium Of low-structure hydrophobic oxide particles.
The suspension according to the invention is preferably prepared by the above-described process according to the invention.
The suspension according to the invention, as a hydrophobic oxide particle, both low-molecular and highly-structured, preferably hydrophobic pyrogenic oxide particles consisting of a material selected from silicon oxide, aluminum oxide, zirconium oxide or titanium oxide, or hydrophobic precipitated oxide particles selected from silicon oxide, aluminum oxide, zirconium oxide or titanium oxide, Preferably hydrophobic precipitated silicic acids. The suspension according to the invention particularly preferably has hydrophobic pyrogenic silicas. In a particular embodiment of the suspension according to the invention, this suspension has a mixture of structurally structurally hydrophobic oxide particles. However, the suspension according to the invention can also have a mixture of highly structured hydrophobic oxide particles.
The hydrophobicity of the oxide particles may be inherent or the oxide particles may have been rendered hydrophobic in a manner known to the person skilled in the art (series of pigments, number 18, Degussa AG). This is preferably effected by a treatment with at least one compound selected from the group of alkylsilanes, alkyldisilazanes, for example with hexamethyldisilazane, or perfluoroalkylsilanes.
As suspensions, the suspension according to the invention can comprise alcohols, ketones, ethers, esters, aliphatic or aromatic hydrocarbons, amides or sulfoxides. The suspension according to the invention preferably contains a mixture of the abovementioned suspension media, but preferably a suspension medium which has water in addition to the organic suspension medium or the organic suspension medium.
The dibutyl phthalate absorption (DBP absorption) is measured according to DIN 53 601. The tamp density is measured according to DIN 53 194. For example, the Aerosil R 812 S has a tamped density of 50 g / l as a highly-structured hydrophobic fumed silica, whereas the Aerosil VP LE 8241 has a tamped density of 140 g / l as low-structured hydrophobic pyrogenic silica.
The low-structured hydrophobic oxide particles can be produced by means of a dry-milling method according to <patcit id="pcit0012" dnum="EP0637616B1"><text>EP 0 637 616 B1</text></patcit> or <patcit id="pcit0013" dnum="US5959005A"><text>US 5,959,005</text></patcit> Can be produced from highly structured hydrophobic oxide particles, which is an intensive grinding process which leads to a destructuring of metal oxides beyond the normal reduction in the particle size. This is an irreversible process.
The suspension according to the invention preferably has aerosils as both low-molecular and highly-structured hydrophobic oxide particles<sup>®</sup> on. This suspension has a low-structured hydrophobic Aerosil<sup>®</sup> Preferably the Aerosil<sup>®</sup> VP LE 8241. In this particular embodiment of the suspension according to the invention, this suspension has a highly structured hydrophobic aerosol<sup>®</sup> The Aerosil<sup>®</sup> R 812 S.
The low-structured hydrophobic oxide particles contained in the suspension according to the invention preferably have a surface with an irregular fine structure in the nanometer range, that is to say in the range from 1 nm to 1000 nm, preferably from 2 nm to 750 nm and very particularly preferably from 10 nm to 100 nm . A fine structure is understood to mean structures having heights, peaks, gaps, ridges, cracks, undercuts, notches and / or holes in the abovementioned distances and regions. The fine structure of the low-structured hydrophobic oxide particles can preferably have elevations with an aspect ratio of greater than 1, particularly preferably greater than 1.5. The aspect ratio is again defined as the quotient of maximum height to maximum width of the survey,
The suspension according to the invention preferably has low-structured hydrophobic oxide particles which have an average particle diameter of from 0.005 μm to 100 μm, preferably from 0.01 μm to 50 μm and particularly preferably from 0.01 μm to 30 μm. For example, low-structure hydrophobic oxide particles, which are composed of primary particles into agglomerates or aggregates with a size of 0.02 μm to 100 μm, can also be contained in the suspension according to the invention.
Depending on the amount of highly structured hydrophobic oxide particles present, the suspension according to the invention can have a dynamic viscosity at shear rates of greater than 20 s<sup>-1</sup> Preferably from 1.0 to 1000 mPa s, preferably from 1 to 500 mPa s, more preferably from 1 to 400 mPa s. For an amount of highly structured hydrophobic oxide particles such as the Aerosil<sup>®</sup> R 812 S, of ≥ 5% by weight, based on the suspension medium, the suspension according to the invention can have a structure-viscous flow behavior.
The suspensions according to the invention and the suspensions prepared by means of the process according to the invention can be used for the production of dirt-repellent and water-repellent coatings on objects, hydrophobic particles being applied to the surface of the objects during coating and thus creating a surface structure with elevations on the surface of the objects Which has dirt and water repellency. The coating of the objects is characterized in that a suspension according to the invention or a suspension prepared by means of the method according to the invention is applied to at least one surface of an object and the suspension medium is subsequently removed.
In a particular embodiment of the suspension according to the invention or of a suspension prepared by means of the process according to the invention for the production of soil and water-repellent coating, the suspension according to the invention or a suspension prepared by means of the process according to the invention is applied by means of a doctor blade to the surface to be coated, . The suspension according to the invention or a suspension prepared by means of the process according to the invention is preferably suitable for the production of coated textile surface structures which have water- and dirt-repellent properties, or for the production of dirt-repellent and water-repellent coatings on textiles.
The suspensions according to the invention or the suspensions produced by means of the process according to the invention can be used for the production of clothing, in particular for the production of protective clothing, rainwear and safety clothing with signaling effects, technical textiles, in particular for the production of cover tarpaulins, tent tarpaulins, protective covers truck tarpaulins, and fabrics Of textile construction, in particular for the production of sun protection roofs, such as, for example, awnings, sun sails, sunshades.
The following examples are intended to illustrate the process according to the invention and the suspensions according to the invention in more detail without the invention being restricted to this embodiment.
Example 1:
In an Ultraturax, 1 part by weight of Aerosil<sup>®</sup> VP LE 8241 (Degussa AG) was suspended in 100 parts by weight of absolute ethanol which had been precipitated. To this suspension of Aerosil<sup>®</sup> VP LE 8241 in ethanol was purified using an Ultraturax 5 weight aerosol<sup>®</sup> R 812 S (Degussa AG) was added and mixed vigorously.
Example 2:
The suspension of Aerosil prepared in Example 1 was obtained<sup>®</sup> VP LE 8241 in denatured ethanol by means of a doctor blade with a layer thickness of 50 μm on a kraft laminating paper from the company SCA Flex Pack Papers GmbH. After evaporation of the suspension medium at room temperature, a polyurethane dispersion from Novotex Italy according to Table 1 was applied to the pretreated laminating paper by means of a film pulling blade with a layer thickness of 50 μm. A tricot fabric of a polyamide fabric (DECOTEX from IBENA Textilwerke Beckmann GmbH) was laminated into the still moist surface of the polyurethane coating. The polyurethane coating was thermally cured at a temperature of 150 ° C for 2 minutes and then the liner was removed.<tables id="tabl0001" num="0001"><table frame="all"><title><b>Table 1: Experimental parameters for Example 2</b></title><tgroup cols="4"><colspec colnum="1" colname="col1" colwidth="18mm" /><colspec colnum="2" colname="col2" colwidth="69mm" /><colspec colnum="3" colname="col3" colwidth="21mm" /><colspec colnum="4" colname="col4" colwidth="59mm" /><thead><row><entry morerows="1" align="center" valign="top"><b>attempt</b></entry><entry namest="col2" nameend="col4" align="center" valign="top"><b>Polyurethane dispersion</b></entry></row><row><entry align="center" valign="top"><b><i>designation</i></b></entry><entry align="center" valign="top"><b><i>Type</i></b></entry><entry align="center" valign="top"><b><i>Characterization of the lotus effect</i></b></entry></row></thead><tbody><row><entry align="center">2.1</entry><entry align="center">Larithane<sup>®</sup> AL 227</entry><entry align="center">Aliphatic</entry><entry align="center">+++</entry></row><row><entry align="center">2.2</entry><entry align="center">Laripur<sup>®</sup> SH1020 in methyl ethyl ketone / dimethylformamide</entry><entry align="center" /><entry align="center">++</entry></row><row><entry align="center">2.3</entry><entry align="center">Impranil<sup>®</sup> ENB-03</entry><entry align="center">Aromatic</entry><entry align="center">++</entry></row><row><entry align="center">2.4</entry><entry align="center">Larithane<sup>®</sup> MA 80</entry><entry align="center">Aromatic</entry><entry align="center">++</entry></row></tbody></tgroup></table></tables>
The characterization of the coated textile sheets was initially visual. +++, water drops are almost completely formed. The rolling angle is below 10 °. ++ means the shaping of the water drop is not ideal, the roll angle is below 20 °.
Example 3:
In an Ultraturax, 1 part by weight of Aerosil<sup>®</sup> VP LE 8241 in 100 parts by weight of an organic suspending agent. To this suspension of Aerosil<sup>®</sup> VP LE 8241 was purified using an Ultraturax Aerosil<sup>®</sup> R 812 S is added and mixed vigorously. Subsequently, the resulting suspension was applied to a polyester blend fabric (DECOTEX from IBENA Textilwerke Beckmann GmbH) by means of a doctor blade with a layer thickness of 50 μm. The suspension medium was then evaporated at room temperature or in a drying cabinet.<tables id="tabl0002" num="0002"><table frame="all"><title><b>Table 2: Experimental parameters for Example 3</b></title><tgroup cols="3"><colspec colnum="1" colname="col1" colwidth="34mm" /><colspec colnum="2" colname="col2" colwidth="30mm" /><colspec colnum="3" colname="col3" colwidth="33mm" /><thead><row><entry align="center" valign="top"><b>Organic</b></entry><entry align="center" valign="top"><b>Aerosil<sup>®</sup> R 812 S</b></entry><entry align="center" valign="top"><b>characterization</b></entry></row><row><entry align="center" valign="top"><b>Suspensions</b></entry><entry align="center" valign="top">In weight parts</entry><entry align="center" valign="top"><b>Of the Lotus effect</b></entry></row></thead><tbody><row><entry>Isopropanol</entry><entry>3</entry><entry>++</entry></row><row><entry morerows="1">Dimethyl sulfoxide</entry><entry>3</entry><entry>++</entry></row><row><entry>5</entry><entry>+++</entry></row><row><entry morerows="1">toluene</entry><entry>3</entry><entry>+++</entry></row><row><entry>5</entry><entry>+++</entry></row><row><entry morerows="1">Tetrahydrofuran</entry><entry>1</entry><entry>++</entry></row><row><entry>3</entry><entry>+++</entry></row><row><entry morerows="1">Cyclohexanone</entry><entry>1</entry><entry>++</entry></row><row><entry>3</entry><entry>++</entry></row></tbody></tgroup></table></tables>
The characterization of the coated textile sheets was initially visual. +++, water drops are almost completely formed. The rolling angle is below 10 °. ++ means the shaping of the water drop is not ideal, the roll angle is below 20 °.
Example 4:
<ol><li>A.) In an Ultraturax, 5 parts by weight of Aerosil<sup>®</sup> R 812 S in 100 parts by weight in toluene and vigorously mixed. The suspension obtained was then applied to a polyester mixture fabric (DECOTEX from IBENA Textilwerke Beckmann GmbH) by means of a doctor blade with a layer thickness of 50 μm. The suspension medium was then evaporated at room temperature or in a drying cabinet. After drying the coated fabric, there were defects. The Lotus effect could not be determined due to deficient adhesion of the oxide particles to the tissue.</li><li>B.) In an Ultraturax 1 part by weight of Aerosil<sup>®</sup> VP LE 8241 in 100 parts by weight in toluene. To this suspension of Aerosil<sup>®</sup> VP LE 8241 was purified using an Ultraturax Aerosil<sup>®</sup> R 812 S is added and mixed vigorously. The suspension obtained was then applied to a polyester mixture fabric (DECOTEX from IBENA Textilwerke Beckmann GmbH) by means of a doctor blade with a layer thickness of 50 μm. The suspension medium was then evaporated at room temperature or in a drying cabinet. The characterization of the thus-coated textile fabric was initially visual and gave a judgment of the lotus effect of +++. This means that water droplets form almost completely and the rolling angle is below 10 °.</li></ol>
Example 5:
Analogous to Example 1, suspensions of Aerosil<sup>®</sup> VP LE 8241 and Aerosil<sup>®</sup> R 812 S with various solvents and then the dynamic viscosity at a temperature of 23 ° C. and a shear ramp of γ = 0.3-50 s<sup>-1</sup> By means of a rheometer of the company Haake type RS75 by means of the plate cone measuring system HC 60/2 °. A summary of the results and the respective composition of the suspension is shown in Table 3.<tables id="tabl0003" num="0003"><table frame="all"><title><b>Table 3:</b></title><tgroup cols="6"><colspec colnum="1" colname="col1" colwidth="12mm" /><colspec colnum="2" colname="col2" colwidth="22mm" /><colspec colnum="3" colname="col3" colwidth="16mm" /><colspec colnum="4" colname="col4" colwidth="21mm" /><colspec colnum="5" colname="col5" colwidth="24mm" /><colspec colnum="6" colname="col6" colwidth="73mm" /><thead><row><entry valign="top"><b>No.</b></entry><entry valign="top"><b>Aerosil</b></entry><entry valign="top"><b>Aerosil</b></entry><entry valign="top"><b>Solvent</b></entry><entry valign="top"><b>Dynamic</b></entry><entry valign="top"><b>comment</b></entry></row><row><entry valign="top" /><entry valign="top"><b>VPLE 8241</b></entry><entry valign="top"><b>R 812 S</b></entry><entry valign="top" /><entry valign="top"><b>viscosity</b></entry><entry valign="top" /></row><row><entry valign="top" /><entry valign="top"><b>[in %]</b></entry><entry valign="top"><b>[in %]</b></entry><entry valign="top" /><entry valign="top"><b>in</b> Η <b>MPa s</b></entry><entry valign="top" /></row></thead><tbody><row><entry>5.1</entry><entry>1.0</entry><entry>1.0</entry><entry>Ethanol</entry><entry>1.6</entry><entry>Fast newtonian flow behavior</entry></row><row><entry>5.2</entry><entry>1.0</entry><entry>3.0</entry><entry>Ethanol</entry><entry>4.3</entry><entry>Fast newtonian flow behavior</entry></row><row><entry>5.3</entry><entry>1.0</entry><entry>5.0</entry><entry>Ethanol</entry><entry>17</entry><entry>Structure-viscous flow behavior</entry></row><row><entry>5.4</entry><entry>1.25</entry><entry>7.5</entry><entry>Ethanol</entry><entry>370</entry><entry>Structure-viscous flow behavior, with flow limit</entry></row><row><entry>5.5</entry><entry>1.0</entry><entry>1.0</entry><entry>DMF</entry><entry>1.6</entry><entry>Fast newtonian flow behavior</entry></row><row><entry>5.6</entry><entry>1.0</entry><entry>3.0</entry><entry>DMF</entry><entry>5.0</entry><entry>Fast newtonian flow behavior</entry></row><row><entry>5.7</entry><entry>1.0</entry><entry>5.0</entry><entry>DMF</entry><entry>52</entry><entry>Structure-viscous flow behavior</entry></row><row><entry>5.8</entry><entry>1.25</entry><entry>11.25</entry><entry>DMF</entry><entry>340</entry><entry>Structure-viscous flow behavior, with flow limit</entry></row><row><entry>5.9</entry><entry>1.0</entry><entry>1.0</entry><entry>toluene</entry><entry>1.2</entry><entry>Fast newtonian flow behavior</entry></row><row><entry>5.10</entry><entry>1.0</entry><entry>3.0</entry><entry>toluene</entry><entry>3.5</entry><entry>Fast newtonian flow behavior</entry></row><row><entry>5.11</entry><entry>1.0</entry><entry>5.0</entry><entry>toluene</entry><entry>9.5</entry><entry>Structure-viscous flow behavior</entry></row><row><entry>5.12</entry><entry>1.25</entry><entry>8.75</entry><entry>toluene</entry><entry>180</entry><entry>Structure-viscous flow behavior, with flow limit</entry></row></tbody></tgroup></table></tables>
Every citation, both ways
| Document | Relation | Office |
|---|---|---|
| EP0637616A | Cites | European Patent Office (EPO) |
| EP1249468A | Cites | European Patent Office (EPO) |
| DE10118346A | Cites | Germany |
12 members in 7 offices
Priority claims7
| Document | Office | Kind | Date |
|---|---|---|---|
| 10250328 | Germany | A | |
| 10250328 | Germany | – | |
| 0310722 | European Patent Office (EPO) | W | |
| 10250328 | – | – | – |
| DE2002150328 | – | – | – |
| EP2003010722 | – | – | – |
| WO2003EP10722 | – | – | – |
Members12
| Document | Office | Kind | |
|---|---|---|---|
| DE10250328A1 | Germany | A1 | |
| WO2004039909A1 | World Intellectual Property Organization (WIPO) | A1 | |
| AU2003267416A1 | Australia | A1 | |
| EP1597334A1 | European Patent Office (EPO) | A1 | |
| JP2006505476A | Japan | A | |
| US2006049376A1 | United States of America | A1 | |
| US7399353B2 | United States of America | B2 | |
| EP1597334B1This record | European Patent Office (EPO) | B1 | |
| AT412719T | Austria | T | |
| ATE412719T1 | Austria | T1 | |
| DE50310724D1 | Germany | D1 | |
| JP4589117B2 | Japan | B2 |
57 legal events, as 6 offices reported them to INPADOC
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|---|---|---|---|
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Numbers
- Publication
- 1597334
- Publication, DOCDB
- 1597334
- Publication, EPODOC
- EP1597334
- Application
- 3748096
- Application, DOCDB
- 03748096
- Application, EPODOC
- EP20030748096
Titles3
- German
- HERSTELLUNG VON SUSPENSION HYDROPHOBER OXIDPARTIKEL
- English
- PRODUCTION OF SUSPENSIONS OF HYDROPHOBIC OXIDE PARTICLES
- French
- PRODUCTION D'UNE SUSPENSION DE PARTICULES D'OXYDE HYDROPHOBES
Classification
- CPC, 20
- C09C3/12
- B08B17/065
- B82Y30/00
- C01P2004/54
- C01P2004/61
- C01P2004/62
- C01P2004/64
- C01P2006/11
- C01P2006/19
- C01P2006/22
- C09C1/3081
- C09D17/007
- C09K3/18
- D06M11/45
- D06M11/46
- D06M11/79
- D06M23/10
- D06M2200/12
- C09D7/61
- Y10T428/31663
- IPC, 9
- C09K3 18
- D06M11 45
- D06M11 46
- D06M11 79
- D06M23 10
- C09C1 30
- C09C3 12
- C09D7 12
- C09D17 00
Designated states1
- Contracting states, 1
- Türkiye