EP0472991B1 - Fluides électrovisceuses à base de dispersions de polymères avec une phase dispersée contenant des électrolytes - Google Patents

Fluides électrovisceuses à base de dispersions de polymères avec une phase dispersée contenant des électrolytes Download PDF

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Publication number
EP0472991B1
EP0472991B1 EP91113465A EP91113465A EP0472991B1 EP 0472991 B1 EP0472991 B1 EP 0472991B1 EP 91113465 A EP91113465 A EP 91113465A EP 91113465 A EP91113465 A EP 91113465A EP 0472991 B1 EP0472991 B1 EP 0472991B1
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Prior art keywords
electroviscous
component
liquid
liquids
evf
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Expired - Lifetime
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EP91113465A
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German (de)
English (en)
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EP0472991A1 (fr
Inventor
Robert Dr. Bloodworth
Günther Dr. Penners
Günter Dr. Oppermann
Roland Dr. Flindt
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Momentive Performance Materials GmbH
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Bayer AG
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • 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
    • C10M171/001—Electrorheological fluids; smart fluids

Definitions

  • the invention relates to an electroviscous liquid, the viscosity of which is increased when a voltage is applied.
  • Electroviscous liquids are dispersions of finely divided solids in hydrophobic and electrically non-conductive oils, the viscosity of which changes very quickly and reversibly from the liquid to the plastic or solid state under the influence of a sufficiently strong electric field.
  • the viscosity reacts to both DC electrical fields and AC fields, whereby the current flow through the EVF should be very low.
  • EVF can be used wherever the transmission of large forces with the help of low electrical power is required, e.g. in couplings, hydraulic valves, shock absorbers, vibrators or devices for positioning and fixing workpieces.
  • the abrasiveness and settling stability of the disperse phase play an important role in practical use.
  • the disperse phase should not sediment as far as possible, but in any case it should be easy to redisperse and should not cause any abrasion even under extreme mechanical stress.
  • the increase in viscosity in an EVF when an electric field is applied can be explained qualitatively as follows:
  • the colloidally chemically stable disperse particles polarize in the electric field and agglomerate through dipole interaction in the field direction, which leads to an increase in viscosity.
  • the agglomeration is reversible: if the electric field is switched off, the particles redisperse and the viscosity is reduced to the original value.
  • the polarizability of the disperse phase is therefore an important prerequisite for the development of the electroviscous effect. For this reason, ionically or electronically conductive materials are often used as the disperse phase.
  • the disperse phase consists of organic solids, such as Saccharides (DE 2 530 694), starch (EP 284 268 A2, US 3 970 573), polymers (EP 150994, A1, DE 3 310 959 A1, GB 1 570 234, US 4 129 513, ion exchange resins (JP 92 278 / 975, JP 31 221/1985, US 3 047 507) or silicone resins (DE 3 912 888 A1), but inorganic materials such as Li hydrazine sulfate (US 4 772 407 A), zeolites (EP 265 252 A2 ), Silica gel (DE 3 517 281 A1, DE 3 427 499 A1) and aluminum silicates (DE 3 536 934 A1).
  • Saccharides DE 2 530 694
  • starch EP 284 268 A2, US 3 970 573
  • polymers EP 150994, A1, DE 3 310 959 A1, GB 1 570 234, US 4 129 513
  • the electroviscous effect of the substances mentioned is due to the loading of the solids with water. Small amounts of water increase the ionic conductivity, and thus the polarizability of the disperse particles, which is essential for the formation of the effect. However, hydrated systems have poor chemical stability. In addition, the temperature range in which these liquids can be used is limited.
  • the optimal properties of the disperse phase can be easily adjusted by varying the water content or by modifying the solid matrix.
  • patent specification DE 2 802 494 C2 describes an improvement in the electroviscous effect by introducing free or neutralized acid groups into a water-containing polymer phase.
  • the high conductivity of the feedstocks often requires post-treatment of the dispersion particles.
  • the passivation of carbon black-filled bead polymers by the subsequent coating of the polymer particles with polyvinylidene fluoride was described in the patent specification JP 016 093. Such post-treatments, however, greatly increase the manufacturing effort.
  • EVF corresponding to the prior art are generally obtained by dispersing a solid in a dispersion medium, such as e.g. halogen-free or halogenated hydrocarbons, aromatics or silicone oil.
  • a dispersion medium such as e.g. halogen-free or halogenated hydrocarbons, aromatics or silicone oil.
  • the viscosity of the resulting suspension depends on the shape and size, or the size distribution of the dispersed particles, and on the solids concentration and the dispersing action of any dispersing agents used. High volume-related solids contents with low viscosity are difficult to achieve when using non-spherical particles.
  • the object of the invention was to provide a water-free, non-abrasive, sedimentation-stable EVF with good electroviscous properties, which despite a high volume fraction of disperse phase is characterized by a low basic viscosity.
  • electroviscous liquids can be produced on the basis of anhydrous polymers which contain the dissolved electrolyte.
  • the electroviscous properties of these liquids can be adjusted over a wide range by the type and concentration of the electrolyte.
  • the electroviscous dispersions according to the invention are anhydrous and have a high dielectric strength.
  • the EVFs described are settling-stable and not abrasive and have low basic viscosities despite high volume fractions of the disperse phase.
  • the dispersion polymerization of electrolyte-containing monomers is particularly suitable as a process for producing the EVF according to the invention.
  • the polymerization should preferably be carried out in the dispersion medium which also represents the continuous phase of the EVF, since this eliminates the need for subsequent redispersion.
  • the water-free EVF according to the invention essentially contains the following substances (I) in the disperse phase: a liquid polymer or polymer mixture: (II) an electrolyte dissolved in (I) and optionally (III): one with the solution of (I) and (II ) miscible additive.
  • the mixture of substances and their starting products are also referred to as templates.
  • the template that is dispersed into the non-conductive liquid during the EVF manufacturing process should preferably be in liquid form. If necessary, the template can be chemically modified by adding suitable reagents (IV) before, during or after the dispersing step. This modification influences the consistency of the disperse phase in the finished EVF through the partial or complete implementation of the functional groups in the template.
  • a suitable dispersant (V) is used for the dispersion.
  • the size of the dispersed particles in the EVF according to the invention is between 0.1 and 200 ⁇ m.
  • the viscosity of the EVF is between 3 and 5000 cp at room temperature, depending on the composition of the liquid and the basic viscosity of the dispersion medium.
  • linear or cross-linked polyethers or their copolymers polyethylene adipate, polyethylene succinate and polyphosphazene.
  • polyethers or polymers which can be prepared by crosslinking di- or trifunctional polyether oligomers are particularly preferred.
  • linear polyether oligomers are polyethylene glycols, polypropylene glycols, statistical ethylene glycol-propylene glycol copolymers or else ethylene glycol-propylene glycol block copolymers, such as those e.g. are sold by GAF under the trade name "Pluronic".
  • Branched polyether oligomers are, for example, tris (polypropylene oxide) ⁇ -ol) glycidyl ether or other substances which are obtained by ethoxylation or propoxylation of higher-functionality hydroxy compounds, e.g. Pentaerythritol or 1,1,1-trimethylolpropane can be obtained.
  • the molecular weight of the glycols is between 62 and 1,000,000, but preferably between 100 and 10,000.
  • the oligomers can optionally contain functional end groups. Amines, allyl or vinyl groups, or also carboxyl groups are examples of such functional end groups.
  • Polyethylene or polypropylene mono- or diamines can be purchased under the trade name "Jeffamin" from TEXACO. Examples of products containing vinyl groups are the esters of glycols with corresponding acids, e.g. Acrylic acid.
  • Other preferred polymers are e.g. the polyesters among others by the company BAYER AG under the trade name "De
  • electrolytes (II) are substances which are soluble in the polymer (I) in molecular or ionic form.
  • electrolytes are, for example, free acids or their salts with alkali or alkaline earth metals or organic cations.
  • the electrolytes thus include salts such as KCl, LiNO3, CH3COONa, LiClO4, Mg (ClO4) 2, KSCN, LiBr, LiI, LiBF4, LiPF6, NaB (C6H5) 4, LiCF3SO3, N (C2H4) 4Cl etc.
  • Additives (III) in the sense of the invention are those compounds which, when mixed with (I) and (II), give a homogeneous, solid or liquid solution.
  • capped low molecular weight polyethers e.g. bismethylated trimethylolpropane or the esters of phthalic acid, suitable as an additive.
  • an additive (IV) for example crosslinking agent
  • a crosslinking agent for example crosslinking agent
  • a crosslinking agent for example crosslinking agent
  • viscous or solid particles are formed, the spherical geometry of which is retained during and after the reaction.
  • di- or multifunctional isocyanates are preferably used as crosslinking agents (IV).
  • Isocyanates of different structures are sold under the trade name "Desmodur” by the company BAYER AG.
  • the use of tolylene diisocyanate as crosslinking agent is particularly suitable.
  • the acetate, amine, benzamide, oxime and alkoxy crosslinkers customary in silicone chemistry can also be used for crosslinking. Radical crosslinking systems are suitable for the conversion of allyl or vinyl (acrylic or methacrylic) group-modified polymer templates.
  • the EVF according to the invention contains the disperse phase (the product from the initial charge and (IV)) in an amount of 10-95% by weight, but preferably in an amount of 40-70% by weight.
  • Dispersants (V) for the disperse phase which can be used are surfactants which are soluble in the dispersion medium and are derived, for example, from amines, imidazolines, oxazolines, alcohols, glycol or sorbitol. Polymers soluble in the dispersion medium can also be used. Suitable are, for example, polymers which contain 0.1 to 10% by weight of N and / or OH, and 25 to 83% by weight Contain C4-C24 alkyl groups and have a molecular weight in the range of 5000 to 1,000,000.
  • the N and OH-containing compounds in these polymers can be, for example, amine, amide, imide, nitrile, 5- to 6-membered N-containing heterocyclic rings or an alcohol, and the C4-C24-alkyl groups are esters of acrylic or methacrylic acid.
  • Examples of the N- and OH-containing compounds mentioned are N, N-dimethylaminoethyl methacrylate, tert-butyl acrylamide, maleimide, acrylonitrile, N-vinyl pyrrolidone, vinyl pyridine and 2-hydroxyethyl methacrylate.
  • the abovementioned polymeric dispersants generally have the advantage over the low molecular weight surfactants that the dispersions prepared with them are more stable with regard to the settling behavior.
  • polysiloxane-polyether copolymers are preferably used, as are available, for example, under the trade name "Tegopren” from GOLDSCHMIDT AG in Essen (FRG).
  • An example of a particularly preferred dispenser for the production of an EVF are polysiloxane polyethers with an ethylene oxide / propylene oxide weight ratio of 49:51, which are sold by GOLDSCHMIDT under the name "Tegopren 5830".
  • the reaction products of hydroxy-functional polysiloxanes with a wide variety of silanes are dispersants for the preparation of the EVF according to the invention.
  • Particularly preferred dispersants from this class of substances are the reaction products of a hydroxyl-functional polysiloxane with aminosilanes.
  • silicone oils such as polydimethylsiloxanes and liquid methylphenylsiloxanes are preferably used as the dispersion medium (VI) for the disperse phase. These can be used alone or in combination of two or more types.
  • the solidification point of the dispersion media is preferably set below -30 ° C, the boiling point above 150 ° C.
  • the viscosity of the oils is between 3 and 300 mm2 / s at room temperature.
  • the low-viscosity oils with a viscosity of 3 to 20 mm2 / s are preferred because they achieve a lower basic viscosity of the EVF.
  • the oil should also have a density that approximately corresponds to the density of the disperse phase.
  • fluorine-containing siloxanes which are used as pure substance or as a mixture with other silicone oils, to produce EVFs according to the invention which, despite their low basic viscosity, have no sedimentation for weeks.
  • the initial charge is mixed with the reactive additive or the crosslinking agent (IV).
  • the mixture is dispersed in a liquid phase containing the dispersant.
  • the dispersion should be carried out so that the particle size does not exceed 200 microns. If appropriate, after the dispersion has taken place, the product is allowed to react for a relatively long time at a suitable temperature, which is typically in a range of 15-150 ° C., depending on the reactivity of the crosslinking agent.
  • the crosslinking agent is only mixed into the dispersion after the dispersion process.
  • the disperse phase can be separated from the original dispersant after the reaction and transferred to a new dispersion medium.
  • the template is sprayed with or without surfactant or additive (IV) into a fine powder, and the resulting powder is subsequently dispersed into the liquid phase.
  • the electrode area of the inner rotating cylinder with a diameter of 0.50 mm is approx. 78 cm2, the gap between the electrodes is 0.50 mm.
  • the shear load can be set to a maximum of 2640 s ⁇ 1.
  • the measuring range of the shear stress of the viscometer is a maximum of 750 Pa. With this device, both static and dynamic measurements are possible.
  • the EVF can be excited with both DC voltage and AC voltage.
  • a constant shear rate 0 ⁇ D ⁇ 2640s ⁇ 1 is set and the dependence of the shear stress ⁇ on the electric field strength E is measured.
  • alternating fields up to a maximum effective field strength of 2370 kV / m at a maximum effective Current of 4 mA and a frequency between 50 and 550 Hz can be generated.
  • 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 Fig. 1 are obtained. It can be seen that the shear stress ⁇ initially increases parabolically with small field strengths and linearly with larger field strengths.
  • the relative increase in viscosity determines the switching behavior of an EVF in practice and is therefore, in addition to the absolute effect S, an important parameter.
  • comparative approaches 1 to 5 correspond to the prior art.
  • the EVF described in Comparative Examples 1 to 3 contain water-containing polymers as the disperse phase bound to it covalently, free or neutralized acid groups. They are based on Examples 1, 2 and 7 of patent specification DE 2 820 494 C2.
  • the liquids described in these examples, which are representative of the patent, show good electroviscous effects, but have a high plastic viscosity, which means that the relative effect is significantly smaller.
  • the EVF described in Comparative Examples 4 and 5 contain anhydrous, differently coated aluminum particles as the disperse phase. They are taken from Japanese Laid-Open Specification 64-6093 (Examples 1 and 4 there). The EVF described have poor sedimentation properties due to the density and size of the disperse particles (> 20 ⁇ m).
  • Examples 1 to 10 are EVFs according to the invention.
  • the mean particle diameter is approximately 2 ⁇ m.
  • the maximum particle diameter is 6 ⁇ m.
  • the samples were measured at a temperature of 60 ° C.
  • Table I lists the electroviscous properties of the EVF according to the invention and their viscosity. Particularly noteworthy is the low basic viscosity of the liquids and the resulting high relative electroviscous effect.
  • Fig. 3 shows the course of the electroviscous effect S, and the viscosity of an EVF, produced according to Example 9, at a shear rate of 1000 s ⁇ 1 depending on the weight concentration of the disperse phase. It can be seen that the liquid according to the invention is characterized by low viscosities despite high solids concentrations.
  • Example 1 of DE 2 820 494 C2 30 vol% dispersion of a polyacrylic acid crosslinked with divinylbenzene in a polychlorinated diphenyl fraction.
  • the electroviscous effect at 30 ° C was between 975-1070 Pa ⁇ mm / kV.
  • Example 2 of DE 2 830 494 C2 30 vol% dispersion of a methacrylic acid crosslinked with divinylbenzene in a polychlorinated diphenyl fraction.
  • the electroviscous effect at 30 ° C. was 690 Pa ⁇ mm / kV.
  • Example 1 of Japanese Patent Application 64-6093 20% by volume dispersion of an aluminum oxide coated aluminum powder in TRIMEX T-08.
  • the electroviscous effect at an alternating voltage of 60 Hz was 327 Pa ⁇ mm / kV.
  • Example 4 of Japanese Laid-Open Publication 64-6093 20 vol.% Dispersion of an aluminum oxide coated aluminum powder in TRIMEX T-08.
  • the electroviscous effect at an alternating voltage of 60 Hz was 371 Pa ⁇ mm / kV.
  • 0.6 g of the dispersant is dissolved in 20 g of the dispersion medium in a beaker with a nominal volume of 100 ml.
  • 17.5 g of the glycol are mixed with 6.79 g of the crosslinker.
  • this amount of crosslinker leads to the stoichiometric conversion of the hydroxyl groups in the glycol and thus corresponds to an OH conversion of 100 mol%.
  • the reactive mixture of glycol and crosslinker is emulsified into the dispersant solution immediately after homogenization using a rotor-stator shear homogenizer (Ultra-Turrax T25 from IKA Labortechnik). The emulsification time at a rotational speed of the rotor of 10,000 rpm is 2 min. The samples were subsequently reacted at 90 ° C. for 15 hours.

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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)
  • Lubricants (AREA)
  • Colloid Chemistry (AREA)
  • Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Claims (10)

  1. Liquides électrovisqueux anhydres contenant essentiellement
    A) un polymère ou un mélange de polymères liquide,
    B) un électrolyte dissous dans A,
    C) éventuellement, un additif miscible avec la solution composée de A) et de B),
    D) un agent de dispersion et
    E) un milieu de dispersion non aqueux.
  2. Liquides électrovisqueux selon la revendication 1, caractérisés en ce que A) se compose de polyéthers ou de leurs oligomonomères linéaires ou ramifiés, éventuellement fonctionnalisés ou du produit de la réaction de tels polyéthers ou de tels oligomonomères avec des composés monofonctionnels ou oligofonctionnels.
  3. Liquides électrovisqueux selon la revendication 1 ou 2, caractérisés en ce que le composant A ou les monomères ou substances de départ oligomères du composant A se présentent sous forme liquide pendant le processus de dispersion et sont éventuellement transformés sous forme très visqueuse ou solide par l'addition d'additifs réactifs avant, pendant ou après la dispersion.
  4. Liquides électrovisqueux selon une des revendications 1 à 3, caractérisés en ce qu'ils contiennent comme composant E) une huile de silicone.
  5. Liquides électrovisqueux selon une des revendications 1 à 3, caractérisés en ce qu'ils contiennent comme composant E) un siloxane fluoré.
  6. Liquides électrovisqueux selon une des revendications 1 à 3, caractérisés en ce qu'ils contiennent comme composant E) un hydrocarbure.
  7. Liquides électrovisqueux selon une des revendications 1 à 5, caractérisés en ce qu'ils contiennent comme composant D) un copolymère polysiloxane-polyéther.
  8. Liquides électrovisqueux selon une des revendications 1 à 5, caractérisés en ce qu'ils contiennent éventuellement comme composant D) un alcoxy- ou acétoxypolysiloxane contenant des radicaux amino.
  9. Liquides électrovisqueux selon une des revendications 1 à 8, caractérisés en ce que le composant I) est éventuellement un polyéthylèneglycol, un polypropylèneglycol ou un copolymère éthylène-propylène et le composant (IV) est un isocyanate difonctionnel ou multifonctionnel.
  10. Procédé de préparation des liquides électrovisqueux par dispersion de particules polymérisables électriquement dans un milieu de dispersion non aqueux en utilisant un agent de dispersion, caractérisé en ce que les particules polymérisables électriquement sont produites par dispersion d'un polymère ou d'un mélange de polymères liquide qui contient un électrolyte sous forme dissoute, un additif provoquant la réticulation du polymère ou du mélange de polymères étant éventuellement utilisé.
EP91113465A 1990-08-25 1991-08-12 Fluides électrovisceuses à base de dispersions de polymères avec une phase dispersée contenant des électrolytes Expired - Lifetime EP0472991B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT91113465T ATE99356T1 (de) 1990-08-25 1991-08-12 Elektroviskose fluessigkeiten auf der basis von polymerdispersionen mit elektrolythaltiger disperser phase.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4026881A DE4026881A1 (de) 1990-08-25 1990-08-25 Elektroviskose fluessigkeiten auf der basis von polymerdispersionen mit elektrolythaltiger disperser phase
DE4026881 1990-08-25

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EP0472991A1 EP0472991A1 (fr) 1992-03-04
EP0472991B1 true EP0472991B1 (fr) 1993-12-29

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US (1) US5268118A (fr)
EP (1) EP0472991B1 (fr)
JP (1) JP2660123B2 (fr)
AT (1) ATE99356T1 (fr)
BR (1) BR9103640A (fr)
CA (1) CA2049719A1 (fr)
DE (2) DE4026881A1 (fr)
ES (1) ES2061137T3 (fr)
RU (1) RU2109776C1 (fr)

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WO2013131659A1 (fr) 2012-03-09 2013-09-12 Fludicon Gmbh Compositions électro-rhéologiques

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US10199687B2 (en) 2016-08-30 2019-02-05 Wildcat Discovery Technologies, Inc Electrolyte formulations for electrochemical cells containing a silicon electrode
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Publication number Priority date Publication date Assignee Title
DE102011018177A1 (de) 2011-04-19 2012-10-25 Raino Petricevic Paste und deren Verwendung
WO2013131659A1 (fr) 2012-03-09 2013-09-12 Fludicon Gmbh Compositions électro-rhéologiques
DE102012004586A1 (de) 2012-03-09 2013-09-12 Fludicon Gmbh Elektrorheologische Zusammensetzung

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DE4026881A1 (de) 1992-02-27
CA2049719A1 (fr) 1992-02-26
BR9103640A (pt) 1992-05-19
ES2061137T3 (es) 1994-12-01
JPH04255795A (ja) 1992-09-10
RU2109776C1 (ru) 1998-04-27
ATE99356T1 (de) 1994-01-15
EP0472991A1 (fr) 1992-03-04
JP2660123B2 (ja) 1997-10-08
US5268118A (en) 1993-12-07
DE59100777D1 (de) 1994-02-10

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