EP0201827A2 - Fluides électrovisqueux - Google Patents

Fluides électrovisqueux Download PDF

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Publication number
EP0201827A2
EP0201827A2 EP86106109A EP86106109A EP0201827A2 EP 0201827 A2 EP0201827 A2 EP 0201827A2 EP 86106109 A EP86106109 A EP 86106109A EP 86106109 A EP86106109 A EP 86106109A EP 0201827 A2 EP0201827 A2 EP 0201827A2
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Prior art keywords
weight
evf
polymers
silica gel
dispersant
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.)
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EP86106109A
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German (de)
English (en)
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EP0201827A3 (en
EP0201827B1 (fr
Inventor
John Goossens
Günter Dr. Oppermann
Wolfgang Dr. Podszun
Volker Dr. Härtel
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Bayer AG
Metzeler GmbH
Original Assignee
Metzeler Kautschuk GmbH
Bayer AG
Metzeler GmbH
Metzeler Kautschuk AG
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Publication of EP0201827A2 publication Critical patent/EP0201827A2/fr
Publication of EP0201827A3 publication Critical patent/EP0201827A3/de
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Publication of EP0201827B1 publication Critical patent/EP0201827B1/fr
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    • C10M171/00—Lubricating compositions characterised by purely physical criteria, e.g. containing as base-material, thickener or additive, ingredients which are characterised exclusively by their numerically specified physical properties, i.e. containing ingredients which are physically well-defined but for which the chemical nature is either unspecified or only very vaguely indicated
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Definitions

  • the invention is based on electroviscous suspensions which contain more than 25% by weight of silica gel with a water content of 1 to 15% by weight as the disperse phase and liquid hydrocarbons as the liquid phase and a dispersant.
  • Electroviscous liquids are dispersions of finely divided hydrophilic solids in hydrophobic, electrically non-conductive oils, the viscosity of which can be increased very quickly and reversibly from the liquid to the plastic or solid state under the influence of a sufficiently strong electric field. Both electrical DC fields and AC fields can be used to change the viscosity.
  • the currents flowing through the EVF are extremely low. Therefore EVF can be used wherever the transmission of large forces should be controlled with the help of low electrical power, e.g. in couplings, hydraulic valves, shock absorbers, vibrators or devices for positioning and holding workpieces.
  • General requirements made in practice are that the EVF has a temperature range of approx. -50 . C to 150 .
  • C is liquid and chemically stable and at least in a temperature range of -30 .
  • C to 110 ° C shows a sufficient electroviscous effect. It is also important that the EVF remains stable over a long period of time, ie there is no phase separation and in particular no sediment that is difficult to redisperse is formed.
  • EVF based on silica gel dispersions in non-conductive oils are described in detail in British Patent No. 1,076,754.
  • water-containing silica gel particles are dispersed in a non-conductive oil.
  • the water content of the silica gel particles and the way in which this water is bound is said to be critical with regard to the electrical activity of the EVF.
  • Nonionic surfactants and / or surfactants which contain a basic N atom are used to disperse the particles.
  • these EVF tend to settle heavily and to form a sediment that is difficult to redisperse.
  • the examples of the aforementioned patent therefore also relate to strongly thixotropic liquids and pastes.
  • both limit the application possibilities of the EVF This applies in particular to the use of a thixotropic EVF as clutch fluid or the use of a paste as hydraulic fluid.
  • the object of the present invention is to provide EVF which are liquid, not or little thixotropic dispersions at room temperature, preferably no phase separation when standing for a long time show or are at least easily redispersible in a phase separation. Furthermore, it should have strong electroviscous effects over a larger temperature range and react quickly and reversibly to changes in the electric field.
  • this object is achieved according to the invention by adding dispersants which are polymers which are soluble in the liquid hydrocarbon phase, these polymers 0.1 to 10% by weight N and / or OH and 25 to 83 wt .-% C 4 - to C 24 alkyl groups and have a molecular weight in the range of 5 ⁇ 10 3 to 106.
  • the polymeric dispersants are added at a concentration of 1 to 30% by weight, preferably up to 20% by weight, based on the silica particles. Surprisingly, it was also found that significantly stronger electroviscous effects can be achieved with the aid of the aforementioned polymeric dispersants than with the known dispersants.
  • Polymers which contain amine, amide, imide, nitrile groups or nitrogen-containing 5- or 6-membered heterocyclic rings are primarily suitable as N-containing polymers.
  • the polymer contains 25 to 83% by weight, preferably 45 to 78% by weight, of C 4 to C 24 -alkyl radicals.
  • Alkyl radicals are understood to mean both linear and branched alkyl radicals. Alkyl radicals having 8 to 18 carbon atoms are particularly preferred. These alkyl radicals can be part of the functional monomers described above, for example when using 2-vinyl-5-stearylpyridine. In general, however, the alkyl groups are introduced into the polymer by copolymerization. Suitable comonomers are, for example, stearyl methacrylate, dodecyl methacrylate, decyl methacrylate, 2-ethylhexyl methacrylate and the corresponding acrylate compounds.
  • the favorable properties of the polymer are retained if to a lesser extent, for example up to a maximum of 35% by weight, other known vinyl and vinylidene compounds, such as C 1 to C 3 alkyl acrylate, C 1 to C 3 alkyl methacrylate, vinyl acetate, vinyl propionate, styrene, methyl styrene, butadiene, vinyl chloride or vinylidene chloride can be copolymerized with.
  • other known vinyl and vinylidene compounds such as C 1 to C 3 alkyl acrylate, C 1 to C 3 alkyl methacrylate, vinyl acetate, vinyl propionate, styrene, methyl styrene, butadiene, vinyl chloride or vinylidene chloride can be copolymerized with.
  • the figure shows the dependence of the shear stress measured in the EVF as a function of the electric field strength at constant shear rate, Tables I and II the characteristic data of the EVF according to the invention in comparison with the prior art.
  • the process engineering measures for the production of the EVF, the chemical production route for the dispersants, the measurement technology required to control the desired physical properties and typical exemplary embodiments for the EVF according to the invention are given.
  • silica gels can be used to manufacture EVF. If necessary, the moisture content of the silica gel can be increased or decreased.
  • the dispersion medium and part or all of the amount of dispersant are introduced and the silica gel is stirred into the dispersion medium with constant stirring.
  • the silica gel can be quickly metered in at the beginning, while the silica gel is slowly added towards the end as the viscosity increases. If only a part of the dispersant is initially introduced, the remaining amount of dispersant is added simultaneously while the silica gel is being added.
  • the type of mixing is also not critical for the end properties of the EVF. For example, simple stirring devices, ball mills or ultrasound can be used for dispersion. With intensive mixing, however, the dispersions can generally be produced more quickly and also become somewhat finer.
  • the amount of dispersant required depends very much on the specific surface of the silica gel used. Approx. 1 to 4 mglm 2 are required as a guideline. However, the absolute amount required still depends on the type of silica gel used and the dispersant.
  • silica gels are, for example, Ultrasil, Durosil, Extrusil from Degussa or Vulkasil, Silicasil and Baysikal types from Bayer.
  • the silica gels used do not need to be pure Si0 2 and can easily contain up to 20 wt .-% A1 2 0 3 , Na 2 0 and Ca0. Furthermore, a few percent by weight of SO 3 , Cl and Fe 2 O 3 can often be present.
  • the loss on ignition is the weight loss at 1000 . C, generally ranges between 10 and 15% by weight. An average of approx. 6% by weight of this is moisture, which is equivalent to the weight loss which is determined by drying at 105 ° C.
  • the specific surface measured by the BET method, is generally between 20 and 200 m 2 / g. However, it is not critical and can be a bit smaller or larger. Too high a specific surface area can, however, lead to an excessive dispersant requirement, which can easily lead to an inadmissibly high intrinsic viscosity of the dispersion, particularly in the case of dispersants with higher molecular weights.
  • Liquid hydrocarbons suitable as the dispersion medium can be paraffins, olefins and aromatic hydrocarbons. Since the EVF has the lowest possible basic viscosity and should also be used at higher temperatures, hydrocarbons with a boiling range between 150 and 220 ° C are preferred. Substances which also have a high flash point, such as e.g. Isododecane.
  • ionic and preferably radical polymerization methods can be used to prepare the polymers, it being possible for the reaction to be carried out as a bulk, solution, precipitation, suspension or emulsion polymerization.
  • a radical solution polymerization in non-polar solvents for example in toluene or isododecane, is particularly advantageous.
  • the polymerization is initiated using conventional radical formers, such as peroxides and azo compounds.
  • the electrode area of the inner rotating cylinder with a diameter of 50 mm is approximately 78 cm 2 , the gap between the electrodes is 0.58 mm.
  • the shear load can be set up to a maximum of 2330 s -1 .
  • the measuring range of the viscometer for the shear stress is a maximum of 750 Pa. Static and dynamic measurements are possible.
  • the EVF can be excited with both DC voltage and AC voltage.
  • a constant shear rate of 0 ⁇ D ⁇ 2330 s is set and the dependence of the shear stress T on the electrical field strength E is measured.
  • Alternating fields can be measured with the test equipment up to a maximum effective field strength of 2370 kV / m at a maximum effective current of 4 mA and a frequency between 50 to 550 Hz. However, measurement is preferably carried out at 50 Hz, because then the total current is the lowest and the electrical power required is the lowest. Flow curves corresponding to the figure are obtained. It can be seen that the shear stress T initially increases parabolically with small field strengths and linearly with larger field strengths.
  • the measurements can be repeated with different shear rates D.
  • the values determined for E o and S generally range from about +5 % to + 20% around the mean.
  • the thixotropy and the redispersibility of the samples were checked after 2 and after 6 weeks by assessing the flow behavior of the samples and the shaking time which is necessary to make the samples thin again.
  • the shaking was done either by hand or, in the case of difficult redispersibility, with a shaking machine.
  • recipes 1 and 2 correspond to the prior art.
  • Examples 3 to 10 are the EVF according to the invention.
  • the comparative examples were based on recipes according to Example III of British Patent 1,076,754, which show the best properties both with regard to strong electroviscous properties in a DC field and in an AC field.
  • Table I lists the electroviscous properties and Table II lists the stability behavior of the samples.
  • Silica gel approx. 80% by weight SiO 2 approx. 6% by weight CaO approx. 3% by weight Na 2 O ⁇ 0.4% by weight Al 2 O 3
  • Dispersion medium isododecane
  • the polymers can be isolated by precipitation with methanol. In general, however, the polymer solutions obtained are used directly for the production of EV liquids.
  • Decyl methacrylate, NN-dimethylaminoethyl methacrylate and 1 g azoisobutyronitrile are dissolved in 500 g isododecane and heated to 60 ° C for 18 h.
  • Decyl methacrylate, acrylonitrile and 1 g azoisobutyronitrile are dissolved in 500 g isododecane and kept at 60 ° C for 18 h.
  • Dispersant CPY 1005 475 g of dodecyl methacrylate and 25 g of freshly distilled vinyl pyridine are dissolved in 500 g of isododecane and 1 g of azoisobutyronitrile is added. The solution is kept at 60 ° C. with stirring for 18 h.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Lubricants (AREA)
  • Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
  • Colloid Chemistry (AREA)
EP86106109A 1985-05-14 1986-05-05 Fluides électrovisqueux Expired EP0201827B1 (fr)

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DE19853517281 DE3517281A1 (de) 1985-05-14 1985-05-14 Elektroviskose fluessigkeiten
DE3517281 1985-05-14

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EP0201827A2 true EP0201827A2 (fr) 1986-11-20
EP0201827A3 EP0201827A3 (en) 1987-10-07
EP0201827B1 EP0201827B1 (fr) 1989-11-08

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EP0350167A1 (fr) * 1988-06-13 1990-01-10 Castrol Limited Fluides fonctionnels
EP0636683A1 (fr) * 1993-07-30 1995-02-01 Nippon Shokubai Co., Ltd. Fluide électrorhéologique
EP0699743A3 (fr) * 1994-08-19 1996-09-11 Lubrizol Corp Fluides électrorhéologiques contenant des solides polaires et des semi-conducteurs organiques
EP0699744A3 (fr) * 1994-08-19 1996-09-11 Lubrizol Corp Fluides électrohéologiques contenant des particules d'un matériau solide et polaire et des particules d'un matériau polymérique inactif

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US4986689A (en) * 1988-01-11 1991-01-22 Trw Inc. Ball joint
JPH01266195A (ja) * 1988-04-19 1989-10-24 Bridgestone Corp 電気粘性液体
US5266229A (en) * 1988-05-12 1993-11-30 Tonen Corporation Stable electro-rheological fluid having a high viscosity-increasing effect
JPH02164438A (ja) * 1988-12-17 1990-06-25 Bridgestone Corp 電気粘性液体
US4992190A (en) * 1989-09-22 1991-02-12 Trw Inc. Fluid responsive to a magnetic field
US5032308A (en) * 1989-11-07 1991-07-16 The Dow Chemical Company Layered mixed metal hydroxides in electrorheological fluids
US5071581A (en) * 1990-03-01 1991-12-10 The Dow Chemical Company Electrorheological fluids based on crown ethers and quaternary amines
JPH07108989B2 (ja) * 1990-08-02 1995-11-22 株式会社コロイドリサーチ 電気レオロジー流体
DE4119670A1 (de) * 1991-06-14 1992-12-17 Bayer Ag Elektroviskose fluessigkeit auf basis von polyetheracrylaten als disperse phase
DE4131142A1 (de) * 1991-09-19 1993-03-25 Bayer Ag Elektroviskose fluessigkeit
CA2096130A1 (fr) * 1991-10-10 1993-04-11 Joseph W. Pialet Fluides electrorheologiques contenant des polyanilines
US5595680A (en) * 1991-10-10 1997-01-21 The Lubrizol Corporation Electrorheological fluids containing polyanilines
DE4142634C1 (fr) * 1991-12-21 1993-03-25 Heraeus Instruments Gmbh, 6450 Hanau, De
US5336423A (en) * 1992-05-05 1994-08-09 The Lubrizol Corporation Polymeric salts as dispersed particles in electrorheological fluids
AU666607B2 (en) * 1993-03-12 1996-02-15 Camp, Inc. Electrorheological fluids with hydrocarbyl aromatic hydroxy compounds
US5412006A (en) * 1994-03-14 1995-05-02 Dow Corning Corporation Electrorheological cels and a method for the preparation thereof
US5552076A (en) * 1994-06-08 1996-09-03 The Regents Of The University Of Michigan Anhydrous amorphous ceramics as the particulate phase in electrorheological fluids
US5607996A (en) * 1994-10-05 1997-03-04 Ford Motor Company Electrorheological elastomers useful as variable stiffness articles
DE19717693A1 (de) 1997-04-26 1998-10-29 Schenck Ag Carl Stell- und Dämpfervorrichtung
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DE102012004586A1 (de) 2012-03-09 2013-09-12 Fludicon Gmbh Elektrorheologische Zusammensetzung
WO2015057583A1 (fr) 2013-10-14 2015-04-23 The United States Of America, As Represented By The Secretary Traitement de la néphropathie chronique avec des sahp
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US10960070B2 (en) 2016-10-25 2021-03-30 The United States Of America, As Represented By The Secretary, Department Of Health And Human Services Prefusion coronavirus spike proteins and their use
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0350167A1 (fr) * 1988-06-13 1990-01-10 Castrol Limited Fluides fonctionnels
AU622910B2 (en) * 1988-06-13 1992-04-30 Castrol Limited Functional fluids
EP0636683A1 (fr) * 1993-07-30 1995-02-01 Nippon Shokubai Co., Ltd. Fluide électrorhéologique
EP0699743A3 (fr) * 1994-08-19 1996-09-11 Lubrizol Corp Fluides électrorhéologiques contenant des solides polaires et des semi-conducteurs organiques
EP0699744A3 (fr) * 1994-08-19 1996-09-11 Lubrizol Corp Fluides électrohéologiques contenant des particules d'un matériau solide et polaire et des particules d'un matériau polymérique inactif

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US4668417A (en) 1987-05-26
JPH0710993B2 (ja) 1995-02-08
JPS61259752A (ja) 1986-11-18
EP0201827A3 (en) 1987-10-07
BR8602157A (pt) 1987-01-13
DE3666835D1 (en) 1989-12-14
DE3517281A1 (de) 1986-11-20
EP0201827B1 (fr) 1989-11-08

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