EP2091639A1 - Verfahren zur kontinuierlichen herstellung von dispersionen in einem wirbelkammerreaktor - Google Patents
Verfahren zur kontinuierlichen herstellung von dispersionen in einem wirbelkammerreaktorInfo
- Publication number
- EP2091639A1 EP2091639A1 EP07818529A EP07818529A EP2091639A1 EP 2091639 A1 EP2091639 A1 EP 2091639A1 EP 07818529 A EP07818529 A EP 07818529A EP 07818529 A EP07818529 A EP 07818529A EP 2091639 A1 EP2091639 A1 EP 2091639A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- temperature
- wax
- vortex chamber
- reactor
- bar
- 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.)
- Withdrawn
Links
Classifications
-
- 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
- B01F23/50—Mixing liquids with solids
- B01F23/56—Mixing liquids with solids by introducing solids in liquids, e.g. dispersing or dissolving
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/10—Mixing by creating a vortex flow, e.g. by tangential introduction of flow components
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/20—Jet mixers, i.e. mixers using high-speed fluid streams
- B01F25/25—Mixing by jets impinging against collision plates
Definitions
- the present invention relates to a one-step process for the continuous preparation of siabiie ⁇ dispersions, in particular of wax dispersions having defined particle sizes and narrow particle size distribution in a vortex chamber reactor.
- Dispersions are found in everyday life and in industry in many areas such as the preparation of e.g. of cosmetics, pharmaceuticals, but also in chemical engineering a widespread application. Dispersions are advantageous to the user in comparison to powdery substances. They are pumpable, not dust explosive and not inhalation toxic, less hygroscopic and can be easily incorporated homogeneously in formulations.
- Dispersions are prepared discontinuously (conventionally in a vessel), quasi-continuously or continuously.
- (conventional) static mixers with fixed internals which effect the mixing of fluid streams using the flow energy are used.
- the integrated mixing structures must always be adapted to the dispersing conditions.
- dynamic mixers the homogenization is carried out by turbulent flows, which are generated mechanically by stirrers in a stirred tank.
- the preparation of dispersions, in particular of emulsions, is carried out batchwise, for example, in stirred-cell kettles. It is disclosed in DE-A-29 26 197 that the production of a wax emulsion is achieved by mixing the wax to be emulsified, in particular an acid wax or ester wax based on montan wax, melts, mixed with a saponifying agent, the emulsifier is added and the mixture emulsified by mixing with water with stirring with a stirrer and homogenized.
- suspensions of montan wax are prepared by subjecting the previously comminuted montan wax to an intensive
- the preparation of dispersions may also be carried out using a rotor-stator system, such as, e.g. an Ultra-Turrax or in a high pressure system such as e.g. in high-pressure homogenizers, in a membrane system such as e.g. with a porous membrane contactor or in an ultrasound system, e.g. Ultrasonic homogenizers are performed.
- a rotor-stator system such as, e.g. an Ultra-Turrax or in a high pressure system such as e.g. in high-pressure homogenizers, in a membrane system such as e.g. with a porous membrane contactor or in an ultrasound system, e.g. Ultrasonic homogenizers are performed.
- microstructured apparatus relies on multilamination, in which the fluid streams are each generated in a plurality of microliter-sized fluid laminations, juxtaposed and assembled (US 2006/0 057 485 A1).
- a major disadvantage of these diffusion-controlled mixing processes is the relatively low flow velocity of laminar flows.
- parabolic profiles of velocity are established in the microchannels which no longer have a uniform residence time profile and lead to greatly differing particle sizes.
- EP 1 171 227 B1 describes a combination of multilamination and application of mechanical vibrations for emulsion production. Here, an attempt is made to influence the process of fragmentation and the position of the maximum of the distribution targeted and thus to achieve a narrower distribution of the particle sizes.
- a relatively new process for the preparation of emulsions is the emulsification with porous membranes or perforated inserts, which are integrated in a microstructured apparatus (US 2006/0120213 A1).
- the disperse phase eg oil
- the continuous phase eg water
- the droplets separate from the pores or are torn away from the flow and transported away with the continuous phase.
- Another way to reduce the droplet size of the disperse phase has been described with the incorporation of a so-called shearing turbine blade, a rotating cutting device.
- emulsions with small droplets and narrow drop size distribution can be made in microchannels in this emulsification process.
- high flow rates of the continuous phase are required, which require the use of strong pump units. which are sensitive to shearing, this method is not suitable.
- sintered materials and perforated inserts tend to contamination and blocking.
- the production of these microstructured apparatus is complicated and expensive, usually still in a prototype stage, and only suitable for preparations on a laboratory scale. In practice, however, fluids with different viscosity values are difficult or impossible to coat one another to form fluid lamellae.
- the present invention seeks to provide a technically reliable and cost-effective process for the preparation of dispersions, in particular wax dispersions, with defined particle sizes and narrow particle size distribution, which can be operated continuously and directly linked to the production process, so that a re-melting of the components to be dispersed is saved and ensures good space / time yields.
- the dispersing apparatus used must allow larger throughputs, so that a large-scale implementation is made possible.
- the dispersions should be stable on storage with particle sizes ds 0 of at most 1 .mu.m and narrow particle size distribution (relative span less than 1.0). By relative range we mean the ratio (d 90 - d-io) / dso.
- the present invention is a process for the continuous production of stable dispersions containing dispersed particles of a particle size d 50 of at most 1 micrometer and in a concentration of 1 to 70 wt .-%, preferably 5 to 50 wt .-%, in particular 10 to 40 wt .-%, based on the total weight of the dispersion, characterized in that a) a component to be dispersed (disperse phase) in liquid form by a Nozzle with 1 to 2000 bar, preferably 10 to 200 bar, by means of control valve, extruder and / or pump, for example gear pump or
- Pressure generator via a first input into a vortex chamber reactor with a vVirbeizigvoiumen of 0.1 to iöö mi, preferably i to 10 ml, at a temperature of 10 to 350 0 C, preferably 25 to 300 0 C, in particular 50 to 200 ° C, is metered in continuously, b) a dispersant (continuous phase), for example water or an organic solvent, for example a liquid alkane, such as hexane, or an alcohol, via a second input into the vortex chamber reactor at a pressure of 1 to 2000 bar, preferably 10 is continuously metered to 200 bar, and a temperature of 10 to 350 0 C, preferably 25 to 300 0 C, in particular 50 to 200 ° C, c) wherein one or more dispersants either added to the disperse phase and mixed, and / or the continuous phase were added and mixed, and / or via a third input into the fluidized-bed reactor with a pressure of 1 to 2000 bar, preferably 10 to 200 bar, and
- 300 0 C, in particular 50 to 200 ° C are metered continuously, d) the mixture resulting from a) to c) 0.001 seconds to 10 minutes, preferably 0.01 seconds to 1 minute, in the fluidized-bed reactor and optionally in a residence module which allows the temperature present in the mixture formed according to a) to c) to remain constant, eg a temperature-controllable pipeline or a flow tube, and e) initiates the dispersion formed in d) into one or more heat exchangers and within 0.001 seconds to 10 minutes, preferably 0.01 seconds to 1 minute, to a temperature of 10 to 250 0 C cools.
- Dwell modules in d) and heat exchangers in e) may be, for example, tube, tube bundle, plate heat exchangers and / or microstructured heat exchangers or combinations thereof.
- the process according to the invention leads to an extremely homogeneous distribution of the disperse phase in the liquid carrier medium, ie in the continuous phase.
- the relative range is not ai (d 90 - d 10 / d 50 ).
- the dispersion prepared by the process according to the invention is very finely divided and storage-stable.
- the substances to be dispersed are, in principle, all organic and inorganic dyes, pigments and their preparations, additives such as fragrance or perfume oils, soap, biocidal silicone oil, motor oil and melting of solids, for example for the additive of biodiesel or as antifreeze of diesel fuels in the winter.
- a vortex chamber reactor suitable for the process according to the invention is described in WO 2004/037 929 A1. It is characterized in that two or more nozzles, each with associated pump and supply line for injecting each of a liquid medium are provided in a swirl chamber enclosed by a housing, that the nozzles are not aligned coaxially to each other, and that an outlet opening for discharging the resulting dispersions is provided from the vortex chamber.
- a temperature measuring device is brought to the vortex chamber.
- the entry angle of the axis of the nozzles can be between 90 ° (orthogonal injection) and 0 ° (tangential injection). It is also advantageous if the axes of the nozzles at an angle between 0 ° and 90 °, relative to the cross-sectional area of the vortex chamber against the Ausiassö réelle, which is conveniently located at the head of the vortex chamber, are employed.
- the geometry of the vortex chamber can be arbitrary, but are advantageous
- the volume of the vortex chamber is limited to such an extent that a turbulent flow state is maintained.
- Suitably are 0.1 to
- the vortex chamber itself can be thermostated by a umschi manendes housing.
- the vortex chamber reactor can also be connected to a Verweiler in order to obtain the mixing state generated in the vortex chamber reactor after exiting the dispersion from the vortex chamber for a long time and exclude back-mixing.
- the liquids are conveniently pressed by pumping through the nozzles.
- the dispersant preferably water
- the vortex chamber is injected into the vortex chamber at a flow rate of between 1 and 20,000 l / h, preferably between 5 and 5,000 l / h and particularly preferably between 10 and 1000 l / h. and at the same time the component to be dispersed having a volume flow between 1 and 5,000 l / h, preferably between 5 and 1,000 l / h and particularly preferably between 10 and 500 l / h, injected into the vortex chamber.
- the very different volume flows are advantageously achieved by appropriately sized nozzle cross sections, for example 1, 0 to 5.0 mm for the nozzle (s) of the dispersant and 0.05 to 1, 0 mm for the nozzle (s) of the component to be dispersed in the form a liquid, such as a solution or melt.
- the ratio of the volume flows Dispergens to dispersed phase between 100 to 1 and 1 to 1, in particular between 50 to 1 and 1 to 1, more preferably between 30 to 1 and 1 to 1.
- the energy input can by Using smaller nozzles (ie smaller nozzle for the liquid carrier medium, For example, water and / or smaller nozzle for the melt) can be increased in the vortex chamber reactor.
- a particularly preferred subject of the invention is a process for the continuous preparation of stable wax dispersions containing dispersed wax particles having a particle size d 5 o of at most 1 micrometer and ⁇ n concentrations in the range of 1 to 70 wt .-%, preferably 5 to 50 wt. -%, In particular 10 to 40 wt .-%, based on the total weight of the wax dispersion, characterized in that a) a wax melt or a wax solution through a nozzle with 1 to
- Temperature in the range of 10 to 350 0 C, preferably 25 to 250 0 C 1, in particular 40 to 200 0 C 1 are metered continuously, d) the mixture resulting from a) to c) 0.001 seconds to 10 minutes, preferably 0.01 Seconds to 1 minute, in the fluidized-bed reactor and optionally in a residence module that keeps constant the temperature present in the resulting mixture according to a) to c), eg a temperature-controlled pipe or a flow tube, and, e) the dispersion formed in d) is introduced into one or more heat exchangers and cooled to a temperature below the dropping point of the wax in the range from 10 to 25O 0 C within 0.001 seconds to 10 minutes, preferably 0.01 seconds to 1 minute.
- the inventive method allows the production of wax dispersions in continuous operation with very good space-time yield.
- the wax melt can be metered directly from the production reactor of the wax into the vortex chamber reactor.
- the inventive method can be used in particular for waxes of any kind.
- Wax is a technological collective term for a number of natural and synthetically derived substances, which have the following properties:
- the waxes are divided into groups of natural waxes, chemically modified waxes and synthetic waxes.
- the natural waxes include, for example, vegetable waxes such as candelilla wax, carnauba wax, Japan wax, Espartograswachs, cork wax, guaruma wax, rice germ oil wax, sugarcane wax, ouricury wax or montan wax, animal waxes such as beeswax, shellac wax, spermaceti, lanolin (wool wax) or raffia fat, mineral waxes such as ceresin or ozokerite (Earthwax) or petrochemical waxes such as petrolatum, paraffin waxes or microwaxes.
- the chemically modified waxes include, for example, hard waxes such as montanic acid waxes, montan ester waxes, Sassol waxes or hydrogenated jojoba waxes.
- the chemically modified waxes include functionalized polyolefin waxes, which means low molecular weight polyolefin chains having carboxylate, keto and / or alcohol groups. They can be produced by air oxidation of polyolefin waxes. Examples are Hartwadise such as Montanklarewachse and Montanesterwachse, which are obtained by extraction from the lignite (Rohmontanwachse) and downstream refining steps to acid waxes and ester waxes.
- functionalized polyolefin waxes which means low molecular weight polyolefin chains having carboxylate, keto and / or alcohol groups. They can be produced by air oxidation of polyolefin waxes. Examples are Hartwadise such as Montanklarewachse and Montanesterwachse, which are obtained by extraction from the lignite (Rohmontanwachse) and downstream refining steps to acid waxes and ester waxes.
- Synthetic waxes are generally understood as meaning polyalkylene waxes, oxidized polyalkylene waxes and polyalkylene glycol waxes. They can be e.g. by polymerization of alkylene, in particular ethylene and / or propylene by the method of Ziegler-Natta or Fischer-Tropsch and / or under
- polyalkylene waxes can then be subjected to oxidation.
- Functionalized polyalkylene waxes are also accessible by copolymerization of ethylene and / or propylene with carboxy-containing monomers, such as acrylic acid.
- amide waxes are amide waxes, copolymers of hexene, octene, norbornene, ethyl vinyl acetate and polyethylene, which may optionally be oxidized, and polytetrafluoroethylene (PTFE). Also the group of polypropylene and polyethylene waxes, as well as their
- Copolymers of hexene, octene, norbornene which have been functionalized by grafting with MSA can be used in the process according to the invention for the preparation of wax dispersions.
- wax alcohols in the context of the present invention, for example, the so-called wax alcohols are calculated.
- Wax alcohols are higher molecular weight, water-insoluble fatty alcohols having generally about 22 to 40 carbon atoms.
- the wax alcohols are used, for example, in the form of wax esters of relatively high molecular weight fatty acids (wax acids) as the main constituent many natural waxes.
- wax alcohols are lignoceryl alcohol (1-tetracosanol), cetyl alcohol, myristyl alcohol or melissyl alcohol.
- the inventive method for the production of wax dispersions also includes wax Sesterheim with a, for example, myristyl myristate, myristyl palmitate, myristyl stearate, Myristylisostearat, myristyl, Myristylbehenat, Myristylerucat, cetyl myristate, cetyl palmitate, cetyl stearate, Cetylisostearat, cetyl oleate, cetyl behenate, Cetylemcat, Stearylmyristat, Stearyipaimitat, Stearyistearat, Stearylisostearat, stearyl oleate, stearyl behenate, Stearylerucat, isostearyl, isostearyl palmitate, Isostearylstearat,
- waxes which, by virtue of their acid number in the range from 5 to 150, have carboxyl groups and optionally further polar functional groups and viscosities of 5 m-Pas to 2000 m Pas (at 170 ° C.), for example montan wax acids whose soaps are on and divalent cations, montan acid wax esters of mono- and polyhydric alcohols, partially esterified montan ester waxes, fully esterified montan ester waxes, carnauba wax, candellila wax, sugarcane wax, peat wax, hydrocarbon compounds oxidized or grafted by various processes, in particular oxidized polyalkylene waxes, such as oxidized polyethylene waxes.
- montan wax acids whose soaps are on and divalent cations
- montan acid wax esters of mono- and polyhydric alcohols partially esterified montan ester waxes, fully esterified montan ester waxes, carnauba wax, candellila wax, sugarcane wax, peat wax
- the dispersions prepared by the process according to the invention contain one or more dispersants in the amounts by weight of 0.1 to 20 wt .-%, preferably 1 to 10 wt .-%, particularly preferably 2 to 6 wt .-%, based on the total weight of dispersion.
- Suitable dispersants are anionic or anionic, cationic or cationic and nonionic or amphoteric substances or mixtures of these agents.
- Suitable anionic substances are, for example, fatty acid taurides, fatty acid N-methyltaurides, fatty acid isethionates, alkylphenylsulfonates, for example dodecylbenzenesulfonic acid, alkylnaphthalenesulfonates, alkylphenol polyglycol ether sulfates, fatty alcohol polyglycol ether sulfates, fatty acid amide polyglycol ether sulfates, alkyl sulfosuccinamates,
- Alkyl sulfates are water-soluble salts or acids of the formula ROSO 3 M 1 where R preferably a Cio-C 24 hydrocarbon radical, more preferably an alkyl or hydroxyalkyl radical having 10 to 20 carbon atoms, and particularly preferably a Ci 2 -Ci 8 alkyl or Represents hydroxyalkyl.
- M is hydrogen or a cation, preferably an alkali metal cation (eg sodium, potassium, lithium) or ammonium or substituted ammonium, eg a methyl, dimethyl and trimethylammonium cation or a quaternary ammonium cation, such as tetramethylammonium and dimethylpiperidinium cation and quaternary ammonium cations, derived from alkylamines such as ethylamine, diethylamine, triethylamine and mixtures thereof.
- alkali metal cation eg sodium, potassium, lithium
- ammonium or substituted ammonium eg a methyl, dimethyl and trimethylammonium cation or a quaternary ammonium cation, such as tetramethylammonium and dimethylpiperidinium cation and quaternary ammonium cations, derived from alkylamines such as ethylamine, diethylamine
- alkyl glycerol sulfates are suitable.
- the alkyl ether sulfates are water soluble salts or acids of the formula RO (A) m SO 3 M wherein R preferably is an unsubstituted C 2 -C 4 alkyl or hydroxyalkyl, more preferably a C 2 -C 2 o alkyl or hydroxyalkyl group, and particularly preferably a Ci 2 -Ci 8 alkyl or hydroxyalkyl radical.
- A is an ethoxy or propoxy moiety
- m is a number greater than 0, typically between about 0.5 and about 6, more preferably between about 0.5 and about 3
- M is a hydrogen atom or a cation, preferably a metal cation (eg, sodium, potassium, lithium, calcium, magnesium), ammonium, or a substituted ammonium cation.
- substituted ammonium cations are methyl, dimethyl, trimethylammonium and quaternary ammonium cations such as tetramethylammonium and
- Dimethylpiperidiniumkationen as well as those derived from alkylamines, such as ethylamine, diethylamine, triethylamine or mixtures thereof.
- alkylamines such as ethylamine, diethylamine, triethylamine or mixtures thereof.
- Ais Examples include Ci 2 -cis-alkyl polyethoxylate (1, 0) sulfate, C 12 -C 8 alkyl polyethoxylate (2.25) sulfate, C 12 -C 18 alkyl polyethoxylate (3, 0) sulfate, Ci 2 -d 8 -alkyl-polyethoxylate- (4,0) sulfate, wherein the cation is sodium or potassium.
- alkyl sulfonates having straight-chain or branched Ce-C 22 -alkyl chains
- primary paraffin sulfonates for example primary paraffin sulfonates, secondary paraffin sulfonates, alkylarylsulfonates, for example linear alkylbenzenesulfonates having C 5 -C 20 -alkyl chains, alkylnaphthalenesulfonates, condensation products
- isethionates such as the acyl isethionates, N-acyl taurides, alkyl succinamates, sulfosuccinates, Monoester of sulfosuccinates (especially saturated and unsaturated C-
- nonionic and amphoteric substances are fatty amine carboxyglycinates, amine oxides, fatty alcohol polyglycol ethers, fatty acid polyglycol esters, betaines, such as fatty acid amide N-propyl betaines,
- Phosphoric acid esters of aliphatic and aromatic alcohols, fatty alcohols or Fettalkoholpolyglykolethem, fatty acid amide ethoxylates, fatty alcohol alkylene oxide adducts and Alkylphenolpolyglykolether into consideration.
- polyglycerol esters e.g. Polyglycerol polyricinoleate and polyglycerol poly-12-hydroxy stearate. Preference is given to liquid fatty acid esters which may be both ethoxylated (PEG-10 polyglyceryl-2 laurate) and non-ethoxylated (polyglyceryl-2 sesquiisostearate).
- sorbitol esters prepared by reaction of sorbitol with fatty acid methyl esters or fatty acid triglycerides.
- the fatty acid residue in the fatty acid methyl esters and fatty acid triglycerides generally contains 8 to 22 carbon atoms and may be straight-chain or branched, saturated or unsaturated. Examples of these are palmitic acid, stearic acid, lauric acid, linoleic acid, linolenic acid, isostearic acid or oleic acid.
- Suitable fatty acid triglycerides are all native animal or vegetable oils, fats and waxes, for example olive oil, rapeseed oil, palm kernel oil, sunflower oil, coconut oil, linseed oil, castor oil, soybean oil, optionally also in a refined or hydrogenated form. Since these natural fats, oils and waxes are usually mixtures of fatty acids with different chain lengths, this also applies to the fatty acid residues in the sorbitol esters used according to the invention.
- the sorbitol esters used according to the invention may also be alkoxylated, preferably ethoxylated.
- alkoxylated, preferably ethoxylated and not ethoxylated mono-, di- or tri-phosphoric acid esters with alkyl groups and / or aryl groups preferably 2,4,6-tris (sec-butyl) phenyl and 2,4,6-tris (n-butyl) -phenyl groups, 2, 4,6-tris (sec-butyl) phenylpolyethylenglykolphosphorklareester with an average of 4 ethylene oxide units per molecule, _Tristyrylphenyl deficit, in particular one or more 2,4,6-tristyrylphenyl, more preferably 2,4,6-tristyrylphenyl-polyethylene glycol phosphoric esters with an average of 6th Ethyienoxi ⁇ units per Moieküi.
- arylsulfonic acid esters and alkoxylated arylsulfonic acid esters are suitable. It is likewise possible to use cationic emulsifiers, such as mono-, di- and tri-alkyl quats and their polymeric derivatives. Also suitable are mixtures of compounds of several of these classes of substances.
- cation-active substances are, for example, quaternary ammonium salts, Fettaminoxalkylate, polyoxyalkyleneamines, alkoxylated polyamines,
- Fatty amine polyglycol ethers for example alkyl, cycloalkyl or cyclized alkylamines, in particular fatty amines, di- and polyamines derived from fatty amines or fatty alcohols and their oxalkylates, fatty acid-derived imidazolines, polyaminoamido or polyamino compounds or resins having an amine index between 100 and 800 mg KOH per g of the polyaminoamido or polyamino compound, and salts of these cationic substances, such as acetates or chlorides, into consideration.
- alkyl, cycloalkyl or cyclized alkylamines in particular fatty amines, di- and polyamines derived from fatty amines or fatty alcohols and their oxalkylates, fatty acid-derived imidazolines, polyaminoamido or polyamino compounds or resins having an amine index between 100 and 800 mg KOH per g of the polyamin
- the dispersions prepared by the process according to the invention may contain further additives in amounts by weight of preferably 0.001 to 2 wt .-%, particularly preferably 0.01 to 1 wt .-%, and in particular 0.05 to 0.8 wt .-%, based on the total weight of the dispersion.
- further additives are saponification agents, such as alkali metal hydroxides, in particular NaOH or KOH, ammonium hydroxides, amines and carbonates, monoethylaminoethanol,
- Diethylaminoethanol or triethanolamine, or storage stability improvers such as multidentate organic complexing agents, for example, N (CH 2 -COOH) 3- nitrilotriacetic acid, (HOOCCH 2 ) 2N- (CH 2 ) 2 -N (CH 2 COOH) 2 Ethylenediaminetetraacetic acid, HN (CH 2 -PO 3 H) 2 amidodimethylenediphosphonic acid and (HO 3 PCH 2 ) 2 N- (CH 2 ) 2 -N (CH 2 PO 3 H) 2 ethylenediaminetetramethylenetetrosphonic acid.
- the additives can be metered into the fluidized-bed reactor together with the disperse phase and / or continuous phase and / or the dispersant (s), but preferably together with the dispersant.
- Montanic acid ester wax (dropping point 80-85 ° C) 26% fatty alcohol polyglycol ether (dropping point about 55 ° C) 4%
- Input of the vortex chamber reactor was dosed with drinking water at a temperature of about 107 0 C (35 Kg / h).
- the residence time in the vortex chamber reactor was about 0.02 seconds.
- the dispersion was then in a heat exchanger within about 1, 5 sec. cooled to about 36 ° C (cooling medium: drinking water, 25 ° C, 100 kg / h).
- the residence time in the vortex chamber reactor was about 0.02 seconds.
- the dispersion was then in a heat exchanger within about 1, 5 sec. cooled (cooling medium: drinking water, 25 ° C, 100 kg / h).
- D 50 0.105 ⁇ m
- D 90 0.170 ⁇ m
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Colloid Chemistry (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102006053497A DE102006053497A1 (de) | 2006-11-14 | 2006-11-14 | Verfahren zur kontinuierlichen Herstellung von Dispersionen in einem Wirbelkammerreaktor |
PCT/EP2007/008446 WO2008058593A1 (de) | 2006-11-14 | 2007-09-28 | Verfahren zur kontinuierlichen herstellung von dispersionen in einem wirbelkammerreaktor |
Publications (1)
Publication Number | Publication Date |
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EP2091639A1 true EP2091639A1 (de) | 2009-08-26 |
Family
ID=38799402
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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EP07818529A Withdrawn EP2091639A1 (de) | 2006-11-14 | 2007-09-28 | Verfahren zur kontinuierlichen herstellung von dispersionen in einem wirbelkammerreaktor |
Country Status (3)
Country | Link |
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EP (1) | EP2091639A1 (de) |
DE (1) | DE102006053497A1 (de) |
WO (1) | WO2008058593A1 (de) |
Families Citing this family (2)
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ES2378677B1 (es) * | 2010-04-28 | 2013-02-28 | Repsol Lubricantes Y Especialidades, S.A. | Emulsiones con acción dual de barrera antihumedad y anti-pintadas. |
CN103459008B (zh) | 2010-12-28 | 2015-08-19 | 荷兰联合利华有限公司 | 乳化的方法 |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
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US3912674A (en) * | 1973-04-30 | 1975-10-14 | Du Pont | Ethylene copolymer dispersions as water repellent coatings |
EP0965680A1 (de) * | 1998-06-18 | 1999-12-22 | Clariant International Ltd. | Wässrige Dispersionen, ihre Herstellung und Verwendung |
DE10249747A1 (de) * | 2002-10-25 | 2004-05-06 | Clariant Gmbh | Verfahren und Vorrichtung zur Durchführung chemischer und physikalischer Prozesse |
-
2006
- 2006-11-14 DE DE102006053497A patent/DE102006053497A1/de not_active Withdrawn
-
2007
- 2007-09-28 EP EP07818529A patent/EP2091639A1/de not_active Withdrawn
- 2007-09-28 WO PCT/EP2007/008446 patent/WO2008058593A1/de active Application Filing
Non-Patent Citations (1)
Title |
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See references of WO2008058593A1 * |
Also Published As
Publication number | Publication date |
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WO2008058593A1 (de) | 2008-05-22 |
DE102006053497A1 (de) | 2008-05-15 |
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