Classifications

• • 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
  • C10M173/00—Lubricating compositions containing more than 10% water
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
  • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
  • B01F23/40—Mixing liquids with liquids; Emulsifying
  • B01F23/41—Emulsifying
  • B01F23/4105—Methods of emulsifying
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
  • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
  • B01F23/40—Mixing liquids with liquids; Emulsifying
  • B01F23/41—Emulsifying
  • B01F23/411—Emulsifying using electrical or magnetic fields, heat or vibrations
  • B01F23/4111—Emulsifying using electrical or magnetic fields, heat or vibrations using vibrations
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B28—WORKING CEMENT, CLAY, OR STONE
  • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
  • B28B7/00—Moulds; Cores; Mandrels
  • B28B7/38—Treating surfaces of moulds, cores, or mandrels to prevent sticking
  • B28B7/384—Treating agents
• • 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
  • C10M173/00—Lubricating compositions containing more than 10% water
  • C10M173/02—Lubricating compositions containing more than 10% water not containing mineral or fatty oils
• • 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
  • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
  • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
• • 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
  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/04—Ethers; Acetals; Ortho-esters; Ortho-carbonates
• • 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
  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/28—Esters
  • C10M2207/281—Esters of (cyclo)aliphatic monocarboxylic acids
• • 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
  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/28—Esters
  • C10M2207/283—Esters of polyhydroxy compounds
• • 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
  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/40—Fatty vegetable or animal oils
• • C—CHEMISTRY; METALLURGY
  • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
  • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
  • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
  • C10N2020/01—Physico-chemical properties
  • C10N2020/02—Viscosity; Viscosity index
• • C—CHEMISTRY; METALLURGY
  • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
  • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
  • C10N2040/00—Specified use or application for which the lubricating composition is intended
  • C10N2040/08—Hydraulic fluids, e.g. brake-fluids
• • C—CHEMISTRY; METALLURGY
  • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
  • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
  • C10N2040/00—Specified use or application for which the lubricating composition is intended
  • C10N2040/20—Metal working
  • C10N2040/24—Metal working without essential removal of material, e.g. forming, gorging, drawing, pressing, stamping, rolling or extruding; Punching metal
• • C—CHEMISTRY; METALLURGY
  • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
  • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
  • C10N2040/00—Specified use or application for which the lubricating composition is intended
  • C10N2040/36—Release agents or mold release agents
• • C—CHEMISTRY; METALLURGY
  • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
  • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
  • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
  • C10N2050/01—Emulsions, colloids, or micelles
  • C10N2050/011—Oil-in-water

Definitions

• the present invention relates to a method for producing dispersant-free medium and low viscosity oil-in-water dispersions, with one Process-available oil-in-water dispersions and their use.
• Oil-in-water dispersions are found in many industrial Areas of application, e.g. as a release agent in the construction industry e.g. to the Stripping of cast concrete, in the metal industry in the die casting process, in forging or the pharmaceutical industry in manufacturing of tablets and dragees, as cooling lubricants in metal cutting, i.e. when drilling, turning, milling or the like, or as a crop protection agent.
• release agents and cooling lubricants predominantly in Formulated as oil-in-water emulsions are plant protection products depending on the active ingredients mainly as solid-liquid dispersions or emulsions applied.
• dispersants are added to the dispersions, which reduce the interfacial tension between the individual phases in order to avoid segregation of the phases over a longer period of time and such a microscopic fine distribution of the dispersed phase (s) in the continuous Maintain phase over a longer period of time.
• the proportion of dispersant depends on the specific application and is in conventional crop protection products up to 20% by weight.
• Commercial concrete release agents and cooling lubricants contain up to 30% by weight of emulsifiers.
• the dispersants or emulsifiers previously considered necessary have application-related disadvantages, which even by adding more suitable Auxiliaries can often only be partially compensated for.
• concrete release agents for example, can emulsifiers because of them high interfacial affinity and interfacial activity an at least partial Emulsification of the separating agent / concrete body interface, causing a Part of the release agent penetrates into the concrete surface and closes after hardening leads to a correspondingly reduced surface quality of the concrete body.
• To at least partially compensate for these technical disadvantages is a considerable development effort for the selection and testing more suitable Auxiliaries necessary.
• Another disadvantage of the dispersants or emulsifiers is that this reliable and sufficiently long stabilization only within one ensure a very narrow concentration and temperature range.
• Exceeding or falling below the critical concentration limit values for example Evaporation or by absorption of foreign substances as a result of improper use Storage, such as dilution of the dispersion with condensate or rainwater, leads as well as corresponding temperature jumps, especially those below freezing (freeze-thaw change), to an irreversible instability the dispersion or emulsion. Unless the instability is recognized and the dispersion is used in this form, inevitably leads to Loss of the processed products.
• dispersants or emulsifiers are due to the high proportion in the dispersions and not least because for the only selected applications, often especially for the application Synthetic dispersants or emulsifiers can be used, one represents a significant cost factor.
• a mold release agent for concrete which, as an oil component, possibly alongside other substances, preferably a water-immiscible and at temperatures between 5 and 15 ° C liquid, monofunctional C 6 -C 30 alcohol component contains an unsaturated C 12 -C 22 fatty alcohol, C 16 -C 28 guebert alcohol, C 8 -C 15 oxo alcohol or a saturated C 6 -C 10 alcohol.
• the emulsifiers used are preferably fatty acid monoglycerol esters or ethoxylates of fatty alcohols, of alkylphenols or of fatty acids, and particularly preferably sodium or potassium soaps of saturated and unsaturated C 12 -C 22 fatty acids. Due to the strongly emulsifying effect of these alcohols, stable emulsions should be obtained by adding comparatively small amounts of emulsifier. However, because of the use of emulsifiers, these concrete release agents also have the disadvantages described above.
• DE 19911777 A1 describes a method for producing highly viscous cosmetic or pharmaceutical formulations, in which two or several liquid components immediately before using the formulation are mixed together from separate pantries by they are passed through a micromixer.
• Micromixers aim to achieve a homogeneous distribution of all ingredients at extreme highly viscous formulations with a viscosity of 67,000 mPa.s without additives can be achieved by emulsifiers.
• compositions with a viscosity of less than 50,000 add 2 to 50% by weight of emulsifiers, depending on the viscosity, being, in accordance with the physical principle, according to which the segregation immiscible phases with decreasing viscosity faster goes, more emulsifier are added with decreasing viscosity got to.
• the object of the present invention is to provide a method, with the oil-in-water dispersions of medium to low viscosity, in particular Release agents, coolants and / or crop protection agents, without Addition of dispersant can be prepared, which, compared with the known dispersions of the same type, at least comparable, preferably have better application properties.
• Oil-in-water dispersions can be obtained, which themselves with - apart from the dispersant - the same composition as the previous one for the individual applications known dispersions for each Use sufficient homogeneity and also sufficient stability exhibit.
• the period of stability of the semi-stable dispersion according to the invention depends mainly on the quality and the degree of energy input the mixing and must be optimized for the respective application.
• Both for cooling lubricants during machining and for Manufacture of concrete release agents must have the appropriate energy input parameters When mixing, set so that the oil-in-water emulsion a stability of ⁇ 10 seconds, corresponding to the time required for distributing and spreading release agent in the mold.
• the dispersions are preferably prepared immediately before use. This ensures that the dispersion is the largest possible when used Has homogeneity.
• dispersant-free dispersions can be obtained by adding the previously known oil-in-water dispersions usually to compensate for the application technology disadvantageous side effects of the dispersants added excipients become.
• Another advantage of the method according to the invention is that only the organic phase has to be stored before use, since water is usually available at the place of use from water pipes stands. Furthermore, since the water and oil phases immediately before use can be brought together in defined volume ratios Exceeding or falling below the critical concentration limit values due to improper use Storage, for example by absorbing foreign substances or due to uneven evaporation of individual phases, no longer occur.
• the ratio of the oil and water phase immediately before using the special conditions on site adapt flexibly, whereas in the case of the dispersions known hitherto corresponding ratio is inevitably predetermined by the emulsion.
• the mixing of the at least two phases can be carried out on the person skilled in the art can be carried out in a known manner for this purpose, for example by injection one phase into the at least other phase, by turbulent mixing, by applying vibrations and cavitation such as ultrasound Homogenizers or other commercially available mixing devices.
• static micromixers have proven to be like them e.g. are described in DE 199 28 123 A1, which are hereby introduced as a reference and is therefore considered part of the revelation.
• these static micromixers the individual phases are defined by individual management channels Dimensions led and divided into a variety of liquid fins before the individual liquid lamellae with fragmentation of at least one of the Phases are merged. Allow these static micromixers a very high energy input during mixing, which makes it semi-stable Oil-in-water emulsions of comparatively long stability can be obtained can.
• these mixers ensure an even energy input, leading to high reproducibility with regard to homogeneity, the particle size distribution and the stability of the dispersions thus produced leads.
• the size distribution of the droplets forming the emulsified phase can be targeted to one by the flow velocity of the individual phases suitable value for the specific application.
• the droplet size of the dispersed phase as well the droplet size distribution depends in particular on the pretreatment of the Membrane and the pressure with which the phase to be dispersed through the Membrane is pressed off, even droplets with a lower Diameter than that of the membrane pores can be formed.
• According to the invention is based on the addition of emulsifiers, as previously provided was waived.
• micromixers Also particularly suitable for mixing the at least two Phases have proven to be dynamic micromixers, e.g. in the DE 199 17 148 A1 are described, which is hereby introduced as a reference and is therefore considered part of the disclosure.
• Micromixers can be the size distribution of the emulsified phase Droplets due to the flow speed of the individual phases, the frequency as well as intensity of the mechanical vibrations targeted at one for appropriate value can be set for the specific application.
• the invention Carry out procedures in the form of a circular process.
• First semi-stable oil-in-water dispersions are produced as described above and fed to use.
• the dispersions collected and for the purpose of separating the individual phases, for example in one Separating funnel incubated before the at least two phases, if necessary after separation of impurities resulting from the application and possibly after Compensation for any liquid loss by means of metering pumps again the mixing device are supplied in which the phases become semi-stable with one another Dispersions are mixed.
• Such a cycle process is particularly suitable for cooling and Lubrication in metal cutting, in which the oil-in-water emulsion only briefly comes into contact with the product to be processed and the contamination in the form of chips caused by the application can be separated particularly easily.
• Any liquid losses occurring in the individual phases can then occur the mixing can be easily compensated for by appropriate metering.
• Biocides or other preservatives only need to be aqueous Phase added as the growth of microorganisms in the organic Phase is inhibited anyway.
• the organic one Treat phase as special chemical waste, as it is weak at best organically contaminated water phase can be eliminated in conventional sewage treatment plants can. So compared to the previously used stable emulsions considerable cost savings can be achieved.
• Such a continuous process can also be used, for example, for release agents, especially in the pharmaceutical field in the manufacture of tablets and coated tablets.
• a continuous Process not on medium-sized and lower oil-in-water dispersions Viscosity is limited, but with any kind of dispersant-free Dispersions is feasible.
• Other examples are the production of cakes, Sweets, chocolates or gummy bears.
• Another object of the present invention are dispersant-free Oil-in-water dispersions, in particular release agents, cooling lubricants and Plant protection products which can be obtained by the process according to the invention.
• the oil-in-water dispersions according to the invention can with regard to the ingredients and the proportions of Ingredients have the same composition as the previously known stable oil-in-water dispersions of the same type.
• the in many known oil-in-water dispersions to compensate for the negative application effects of the dispersants added to be dispensed with.
• biocides or preservatives only required if the aqueous phase or an equivalent Concentrate over the preparation of the semi-stable dispersion is stored for a longer period of time or if the semi-stable dispersion over a to be used several times over a longer period of time.
• the release agents according to the invention can, for example, be mineral oils, White oils, waxes, triglycerides, esters from aliphatic carboxylic acids and one or polyhydric alcohols, alcohols or ethers or a mixture of two or more substances from one or more of the aforementioned Groups included.
• the ratio of the aqueous to the organic phase is preferably between 20: 1 and 1: 1.
• the release agents according to the invention particularly preferably contain an oil phase a mixture of 90 to 98% by weight of a base oil, 0 to 10% by weight of one separating components, 0.2 to 1 wt .-% of an anti-corrosion additive and 0.2 to 5% by weight of a wetting agent.
• a base oil Hydrocarbons triglyceride mixtures, esters, very particularly preferred Esters of a carboxylic acid with more than 16 carbon atoms and an alcohol component with more than 8 carbon atoms, fatty alcohols and a mixture of two or more substances from one or more of the aforementioned groups.
• Examples of separating components are Mixtures of fat and resin acids, triglyceride mixtures, esters and polyol alcohol derivatives as well as their mixtures.
• a corrosion protection additive are merely For example, succinic acid esters, amine phosphates, sulfonate / carboxylate mixtures, Imidazole derivatives, N-oleyl sarcosine and phosphoric acid esters, which are used both alone and in combination can.
• Suitable wetting agents are fatty acid polyethylene glycol esters, sodium diisooctyl sulfosuccinate, Sorbitan trioleate, glycerol monooleate, glycerol dioleate, Alcohol derivatives, ester derivatives and silicone additives, which both alone and can also be used in combination.
• Cooling lubricants according to the present invention can e.g. as organic Phase a mixture of 5 to 80 wt .-% base oil, 5 to 20 wt .-% corrosion protection additives as well as metal inhibitors, possibly preservatives and contain other common additives.
• Suitable base oils are ester oils, paraffinic or naphthenic hydrocarbons, alcohols, ethers, polyisobutenes, Polyalkylene glycols and mixtures of two or more substances one or more of the groups listed above.
• the oil phase can also alkylsuccinimides, castoroil ethoxylates, Petroleum sulfonates, solid lubricants, toluyltriazoles, defoamers and / or Anti-fog additives included as other common additives.
• the proportion of the oil phase can in the cooling lubricant according to the invention between 2 and 25 % By weight.
• the crop protection agents according to the invention can in principle be all common agrochemical active ingredients, such as herbicides, pesticides, insecticides, acaricides, algicides Aphicides, bactericides and virucides.
• Active substances such as D, L- and L-phosphinothricin ammonium, D, L- and D-fenoxapropethyl, Diclofopmethyl, ethofumesate, phenmedipham and desmediphan called.
• the plant protection products further customary additives, such as inert substances, fillers or anti-foaming agents, be inflicted.
• the present invention Plant protection products in the form of oil-in-water emulsions or in the form of solid / liquid oil-in-water dispersions.
• an oil phase was first prepared from the following components: 90% by weight spindle oil 5% by weight rapeseed oil 3% by weight oleic acid 0.5% by weight BernsteinTexreester 0.5% by weight FettTexrepolyethylenglykolester
• an oil phase was first prepared from the following components: 98% by weight rapeseed oil 1% by weight AdditinRC 4820 (commercial product) 1% by weight Isooctylsulfosuccinat
• the oil phase was then added with water as described in Example 1 one mixed into an oil-in-water emulsion with an oil content of 13.3% by weight.
• an oil phase was first prepared from the following components: 91.2% by weight Isooctyloleat 5% by weight oleic acid 0.8% by weight AdditinRC 4220 (commercial product 9 3% by weight glycerol oleate
• the oil phase was then added with water as described in Example 1 one mixed to form an oil-in-water emulsion with an oil content of 24.4% by weight.

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Citations (8)

• 2002
  • 2002-04-16 DE DE50207291T patent/DE50207291D1/de not_active Expired - Lifetime
  • 2002-04-16 EP EP02008174A patent/EP1356857B1/fr not_active Expired - Lifetime
  • 2002-04-16 AT AT02008174T patent/ATE330697T1/de active

Patent Citations (8)

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