WO2006029841A1 - Procede de production de carboxylates metalliques - Google Patents

Procede de production de carboxylates metalliques Download PDF

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Publication number
WO2006029841A1
WO2006029841A1 PCT/EP2005/009883 EP2005009883W WO2006029841A1 WO 2006029841 A1 WO2006029841 A1 WO 2006029841A1 EP 2005009883 W EP2005009883 W EP 2005009883W WO 2006029841 A1 WO2006029841 A1 WO 2006029841A1
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Prior art keywords
reaction mixture
ultrasound
microwaves
metal
generating
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PCT/EP2005/009883
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German (de)
English (en)
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WO2006029841B1 (fr
Inventor
Jürgen HAUK
Valentin Ausserbauer
Hans Sommer
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Baerlocher Gmbh
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Publication of WO2006029841A1 publication Critical patent/WO2006029841A1/fr
Publication of WO2006029841B1 publication Critical patent/WO2006029841B1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/10—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
    • B01J19/122—Incoherent waves
    • B01J19/126—Microwaves
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/41—Preparation of salts of carboxylic acids
    • C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00548—Flow
    • B01J2208/00557—Flow controlling the residence time inside the reactor vessel
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0873—Materials to be treated
    • B01J2219/0875—Gas
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0873—Materials to be treated
    • B01J2219/0877—Liquid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0873—Materials to be treated
    • B01J2219/0881—Two or more materials
    • B01J2219/0884—Gas-liquid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0873—Materials to be treated
    • B01J2219/0892—Materials to be treated involving catalytically active material

Definitions

  • the present invention relates to a method and an apparatus for the production of metal carboxylates from a reaction mixture, wherein in at least one process step, the reaction mixture is treated with micelles.
  • metal carboxylates from carboxylic acids or carboxylic acid esters, for example from fats or fatty acids and metal oxides, metal hydroxides or other metal soaps has a long tradition.
  • fats or fatty acids are mixed with a corresponding metal compound in the context of such a method and brought by the supply of thermal energy, often also using a catalyst for reaction.
  • metal carboxylates in particular in the form of metal soaps, in addition to their function as acid scavengers as release agents and lubricants, increasingly play an important role in the solution of theological problems.
  • the finished articles In addition to a production-optimizing effect of the metal soaps, the finished articles often also get smoother surfaces with less sliding friction.
  • the metal soaps used consist to a large extent of natural raw materials and often tend to decompose under the influence or temperatures. This manifests itself in the context of using such metal soaps as stabilizers for polymeric products often in a discoloration of the product itself, which is often not tolerated by the customer.
  • metal soaps Due to their excellent lubricating and separating action and their ability to thicken or form gels, metal soaps are used in the pharmaceutical and cosmetics industry.
  • the lubricating and separating action is used in the tableting and coating, reduce the hydrophobic properties or verhin ⁇ in powdered pharmaceuticals and cosmetics the Wasseraumahme and thus often also the agglomeration of corresponding powders.
  • metal soaps are often used in cosmetic products or personal care products in small quantities, but the total amount of these products leads to a great demand for corresponding metal soaps.
  • metal soaps are used, for example, in detergents and cleaners to reduce their moisture absorption.
  • metal soaps frequently form mold release agents, in the textile auxiliaries industry they are used for dry impregnation and as an antistatic additive.
  • metal soaps are used as swelling and suspension agents as well as lubricants and release agents for pastel pencils and as matting agents for gravure printing inks. Because of their excellent oil-binding capacity they are added to kitten and putties.
  • wax production and processing of liquid wax components they often serve as suspending agents and for increasing the water-repellent properties. The production of metal soaps is carried out in awake ⁇ most diverse manner according to the prior art.
  • a fatty acid is heated, for example, in a large excess of water to a temperature above its melting point and first mixed with a suitable base, so that a water-soluble metal soap is formed.
  • the desired water-insoluble metal soap is formed by adding a solution of a corresponding metal salt.
  • the water-soluble salt formed in the course of the reaction is removed from the metal soap by washing. In this case, light, fine powders with a large surface are usually obtained.
  • soaps are generally used everywhere where sliding and separating properties based on a large surface are desired.
  • the ratio of fatty acid / water often influences the size of the particles formed and thus the surface area and the bulk density. With increasing dilution, a decreasing particle size and thus a larger surface are obtained.
  • the reaction takes place between carboxylic acids and metal oxides, metal hydroxides or another suitable metal salt at elevated temperature in a large excess of water.
  • the metal carboxylates formed in this process are likewise obtained as fine powders of usually high purity, which are substantially free of water-soluble salts.
  • the reaction is often carried out under pressure.
  • the metal oxides or Metallhydroxi ⁇ de or other suitable metal salts with fatty acids are heated with stirring to a temperature above the melting point of the metal soaps.
  • the resulting water in the reaction escapes, since the melting point of the soaps formed is usually above 100 ° C.
  • the soaps produced in this way often no longer have to be dried.
  • the soaps can be obtained, for example, in the form of pastes, flakes or as powders from the melt.
  • metal oxides, metal hydroxides or suitable metal salts can be heated to temperatures approximately equal to the melting point of the soaps.
  • the water formed during the reaction and the water added before the reaction are removed under reduced pressure after the reactor has been expanded.
  • the metal soaps obtainable in this way can also be prepared as granules or powders.
  • metal carboxylates by way of example by the melt process by reaction of the molten fatty acid with metal oxides, hydroxides and / or suitable metal salts or by the precipitation process by double reaction of their sodium soaps with water-soluble salts of the corresponding metals can perform.
  • the precipitation process generally produces clean and bulky products that can be processed at temperatures below 100 ° C.
  • it is often much more expensive than a melt-through process by filtration and drying costs.
  • the stabilizers prepared by the melt process are sufficient.
  • Suitable stabilizers for example, the lead, barium and cadmium compounds have proven in practice. However, these substances are highly toxic, especially if they are in powder form. For the manufacturer of pulverulent stabilizers, in particular the formation of dust during processing poses a particular hazard since the pulverulent metal soaps are absorbed by the respiratory organs and can develop their toxic effect there.
  • WO 91/19691 relates to a process for the preparation of solid, neutral or basic metal soaps by a controlled solid-liquid reaction of liquid fatty acids with solid metal oxides and / or metal hydroxides in an external premixing zone under reduced pressure and the use of the metal salts as a stabilizer and / or lubricant mixture in the processing of plastics.
  • DE 3403621 relates to a process for the preparation of water-insoluble metal soaps of aliphatic monocarboxylic acids, the metal soaps having a significantly improved filterability.
  • a small amount of a polymeric fatty acid, an aliphatic dicarboxylic acid, a by-product acid obtained from the ozonization of oleic acid or an aliphatic, cycloaliphatic or aromatic polycarboxylic acid or anhydride thereof is added to the aliphatic monocarboxylic acid.
  • No. 5,164,523 describes a process for the preparation of granular metal soaps.
  • a mixture of metal oxide, fatty acid and a catalyst is reacted in the course of a continuous process in a heated reactor and forms a metal soap.
  • This metal soap is introduced through a spray nozzle in a cooling tower, forming a granulate.
  • the reaction itself takes place in a spiral helix surrounded by a heating fluid.
  • the reaction is at a temperature of about 150 to about 170 ° C.
  • Dicarboxylic acids are used in particular as catalysts.
  • melt processes known from the prior art frequently have the disadvantage that the melt products obtained according to the process described have a high turbidity.
  • the present invention is therefore based on the object to provide a process for the preparation of metal carboxylates, which leads in a simple and economically competitive manner to metal carboxylates.
  • the object of the present invention was to provide a process for the preparation of metal carboxylates which with the lowest possible energy input.
  • the object of the present invention was to provide a process for the preparation of metal carboxylates which can be used in a simple manner continuously for the preparation of metal carboxylates.
  • the present invention was based on the object of providing a process for the preparation of metal carboxylates which has the shortest possible reaction times.
  • a further object of the present invention was to provide a process for the preparation of metal carboxylates, with which products with the lowest possible contamination can be obtained in a gentle manner.
  • a further object of the present invention was to provide a process for the preparation of metal carboxylates, with which products can be obtained in a gentle manner, which have the lowest possible turbidity.
  • the present invention therefore provides a process for the production of metal soaps in which a reaction mixture comprising at least one fatty acid or a fatty acid is converted to a product in one or two or more process steps with at least one metal compound suitable for forming a metal soap to form a metal soap is, wherein the reaction mixture is irradiated in at least one process step with microwaves. It has been found in the context of the present invention to be advantageous if the production of metal carboxylates takes place using microwaves. The reaction mixture is therefore irradiated in the context of the inventive method in at least one process step with microwaves.
  • An inventive method accordingly comprises at least one procedural step.
  • the treatment of the reaction mixture with microwaves within the scope of the process according to the invention can be carried out, for example, within one process step.
  • a device for generating microwaves can be used, in which the influence of the reaction mixture by means of microwaves and ultrasound is continuous or pulsed.
  • the microwave generator is configured to influence the reaction mixture by microwaves either permanently continuously or permanently pulsating or optionally continuously or pulsating or alternately continuously and pulsating.
  • a corresponding device for generating microwaves can also be selected such that a continuous irradiation or a pulsating irradiation takes place depending on the operating state of the system, for example as a function of the temperature of the reaction mixture.
  • a process step is understood to mean a specific point in the reaction sequence in which the reaction mixture is subjected to a change in state, wherein such a state change may be, for example, a chemical or physical state change.
  • a corresponding change in state can be, for example, a change in the temperature, a change in the pressure, the speed, the number of reaction components, the action of electromagnetic radiation or the action of sound.
  • a method step in the context of the present invention may include, for example, only a change of state.
  • a single method step in the sense according to the invention comprises a change of two or more states in the sense of the above.
  • a change in temperature and pressure can take place or a reaction mixture can be exposed to energy-rich radiation within the scope of a single method step and subjected to an increase in pressure.
  • metal soaps are understood as meaning, in principle, the metal salts of carboxylic acids having at least about 6 carbon atoms, which may be metals having a valence of 1, but may also be metals with a carbon atom Valence of 2, 3 or more act.
  • the process according to the invention is suitable, for example, for the preparation of water-soluble or water-insoluble metal soaps of aliphatic monocarboxylic acids having 6 to 44 carbon atoms, including the saturated and unsaturated fatty acids, branched and straight-chain fatty acids and hydroxy-substituted fatty acids.
  • aliphatic monocarboxylic acids having 6 to 44 carbon atoms, including the saturated and unsaturated fatty acids, branched and straight-chain fatty acids and hydroxy-substituted fatty acids.
  • Mixed fatty acids derived from natural fats and oils are also well suited.
  • the process according to the invention is suitable for the production of magnesium, calcium, zinc and aluminum soaps, but it can also be used for the production of strontium, barium, iron, cobalt, nickel, copper, Cadmium, manganese, chromium, sodium, lithium, potassium or lead soaps and for the production of metal carboxylates of metals from the group of lanthanides.
  • metallic soaps are neutral or basic metal soaps of the general formula
  • n is a number from 1 to about 20, for example 1, 2, 3 or 4, and the radicals R independently of one another represent a linear or branched, saturated or unsaturated, substituted or unsubstituted hydrocarbon radical having 6 to 44 carbon atoms.
  • Suitable carboxylic acids include caprylic, pelargonic, capric, lauric, myristic, palmitic, stearic, arachidic, behenic, lignoceric and the like, or mixtures of two or more thereof.
  • unsaturated monocarboxylic acids such as, for example, oleic acid, linoleic acid. acid and the like according to the method of the invention are also used in vor ⁇ geous way and überbigt in suitable metal soaps.
  • fatty acids derived from animal fats or oils or vegetable oils are conventionally used for the production of metal soaps. These commercial fatty acids are obtained by cleavage and fractionation of natural fats and oils and are usually mixtures of aliphatic monocarboxylic acids with the predominant acids containing about 12 to 18 carbon atoms. The acids may include both saturated and unsaturated acids.
  • Suitable commercially available fatty acid products of this type are derived from tallow, lard, fish oil, sperm oil, coconut oil, palm oil, palm kernel fat, peanut oil, rapeseed oil, cottonseed oil, sunflower oil, soybean oil, linseed oil and the like. Also suitable are hydrogenated species thereof, for example hydrogenated tallow fatty acids and the like.
  • the present invention therefore further provides a process for the production of metal soaps, in which a reaction mixture containing at least one fatty acid or a fat in one or two or more Aids ⁇ steps with at least one suitable for forming a metal soap Metall ⁇ compound to form a metal soap a product is reacted, wherein the reaction mixture is irradiated in at least one process step with microwaves and the reaction mixture is treated in at least one procedural step with ultrasound.
  • the reaction mixture is irradiated with microwaves in at least one process step and is ultrasonically treated in at least one process step.
  • the treatment of the reaction mixture with microwaves and ultrasound within the scope of a further embodiment of the method according to the invention can be carried out, for example, within one process step.
  • combined devices for generating microwaves and ultrasound can be used, in which the influence of the reaction mixture by means of microwaves and ultrasound takes place substantially simultaneously.
  • the method according to the invention with a device in which the microwave generator and the ultrasound generator are combined, for example, in such a way that simultaneously with the influence of microwaves on the reaction mixture, the reaction mixture is also influenced by ultrasound.
  • This can be achieved for example by a corresponding construction of the device suitable for generating microwaves or for generating ultrasound.
  • any desired geometric shapes are possible, in particular, for example, a cylindrical design can be selected in which the ultrasound generating device essentially surrounds the microwave-generating device.
  • the microwave generator and the ultrasound generator are arranged in such a way that according to the method a successive influence of the reaction mixture by microwave and ultrasound or by ultrasound and microwave, essentially in any desired Order, done.
  • a corresponding reaction mixture is treated with ultrasound in a first method step and subjected to a treatment with microwaves in the course of a subsequent method step.
  • the former method variant has proven to be advantageous in many cases.
  • the treatment of the reaction mixture with ultrasound in the context of the process according to the invention can be carried out, for example, within a single process Process step take place.
  • a device for generating ultrasound can be used, in which the influence of the reaction mixture by means of ultrasound is continuous or pulsating.
  • the ultrasound generator is configured such that the ultrasonication of the reaction mixture is either permanently continuous or permanently pulsating or optionally continuous or pulsating or alternately continuous and pulsating.
  • a corresponding apparatus for generating ultrasound can also be selected such that a continuous irradiation or a pulsed irradiation occurs as a function of the operating state of the system, for example as a function of the temperature of the reaction mixture.
  • a reaction mixture in the course of a process step or in the course of two process steps with microwaves and with ultrasound.
  • the number of treatments with microwaves and the number of treatments with ultrasound need not necessarily be identical in each case. It is also possible and envisaged that, for example, a reaction mixture is more frequently treated with microwaves than with ultrasound or that a reaction mixture is treated more frequently with ultrasound than with microwaves.
  • the number of differences in The frequency of the treatments with microwaves or with ultrasound can be, for example, 1, 2, 3, 4 or more, for example 5, 6, 7 or 8.
  • a reaction mixture in the context of the present invention is repeatedly brought into contact with microwave radiation or with ultrasound or both, this can in principle be carried out, for example, either in the context of successive devices for introducing microwaves or for introducing ultrasound into the reaction mixture ,
  • a reaction mixture according to the invention passes through a multiple treatment with microwaves or with ultrasound in the context of a loop, so that successive treatment steps with microwaves or with ultrasound each at the same location of a device suitable for a corresponding treatment, in particular in the context of a Schleifen ⁇ reactor done.
  • any device for the treatment of a reaction mixture with microwaves in the context of a method according to the invention, basically any device is suitable which is capable of irradiating a reaction mixture in a corresponding container either batchwise or continuously with a suitable amount of microwaves. Suitable devices are described, for example, in WO 90/03840 or in DE 199 38 501 A1 (for B atch methods and continuous methods).
  • resonators with fixed or variable geometry are suitable, which, for example, form the reaction mixture. wise in a quartz tube, passes through. Also possible is the entry of microwaves directly into the reaction mixture by means of antenna technology.
  • microwave radiation is understood to mean an electromagnetic field having a frequency of approximately 0.5 to approximately 24 GHz, for example having a frequency of approximately 1 to approximately 5 GHz or having a frequency of approximately 2 to approximately 3 GHz oscillates.
  • the frequency in particular the frequency between about
  • the microwave input is preferably selected such that energy input through the microwave is 1 to 5000 W / kg. If necessary, the amount of energy required for optimal reaction control may also be slightly outside the range mentioned. In many cases, it has been proven that the energy input by the microwave is adjusted to within a range of about 5 to about 1200 W / kg or about 10 to about 500 W / kg or about 30 to about 100 W / kg reaction mixture.
  • the temperature of the reaction mixture during or after contact with the microwaves can be used. In some cases, it has proven to be advantageous if the temperature of the reaction mixture after contact with the microwave radiation is above the melting point of the reaction mixture. or as far as above the softening point of the reaction product that flow of the reaction product in the device is possible. Suitable temperatures are, for example, about 90 to about 200 0 C, more particularly sondere about 100 to about 180 0 C.
  • the treatment of the reaction mixture to be treated according to the invention with ultrasound can, as already mentioned above, be carried out together with the treatment with microwaves in one process step.
  • Suitable devices for the treatment of a reaction mixture with ultrasound are known to the person skilled in the art.
  • devices are suitable which make it possible to treat the reaction mixture in a batch process.
  • Equally suitable are devices which make it possible to treat the reaction mixture in a continuous process.
  • the entry of ultrasound can take place, for example, via a sonotrode to the vessel containing the reaction mixture or a corresponding line. It is, however, so possible that the entry of ultrasound via an ultrasonic conductor can be made directly into the reaction mixture.
  • the reaction mixture can be treated, for example, with microwaves and ultrasound until the reaction has reached the desired degree of conversion, the product formed being subsequently the apparatus used for carrying out the reaction, for example after appropriate control of the temperature. can be taken ent.
  • reaction mixture in at least one further step after treatment with microwaves and after the treatment with ultrasound for a period of at least 5 s, for example for a period of at least about 15 s or a period of time of at least about 30 s at a temperature of at least about 130 ° C, for example at least about 150 or at least about 170 0 C.
  • a process step in which the reaction mixture treated with microwave and ultrasound is kept at an elevated temperature for a certain period of time, can lead to an improvement of the yield and to a purer product.
  • the reaction mixture in the reactor can, for example, be in wel ⁇ the irradiation or the influence of ultrasound has taken place, and kept at a certain temperature.
  • Suitable periods are for example about 5 seconds to about 120 minutes, in particular about 15 seconds to about 60 minutes or about 30 seconds to about 30 minutes, for example 1 minute to about 10 minutes or about 2 minutes to about 5 minutes.
  • Suitable temperatures are in the range of about 80 to about 200 ° C, for example about 90 to about 190 0 C, or about 140 to about 180 ° C.
  • the inventive method can be carried out in the context of the present invention, for example at ambient pressure.
  • a pressure which is between about 1 bar and about 20 bar or about 1 bar and about 6 bar.
  • an inert gas can be used in the context of the present invention to pressurize the reaction vessel.
  • an inert gas can be used in the context of the present invention to pressurize the reaction vessel.
  • Suitable inert gases are in principle all gases which are inert to the components present in the reaction mixture. Preference is given to commercially available inert gases, for example nitrogen or argon, in particular due to its availability and its price of nitrogen.
  • the use of inert gases can also serve to change the rheological properties of the reaction mixture.
  • the use of inert gas can lead to foamed products being obtained.
  • the reaction mixture used in carrying out the process according to the invention may in principle contain any desired components, provided that the components contained in the reaction mixture lead to a metal carboxylate under the process conditions.
  • the components present in the reaction mixture are selected such that the amount of free fatty acids in the Product less than 2% by weight, preferably less than 1.5% by weight, for example less than 1% by weight or less than 0.8% by weight, for example less than 0.5% by weight. % is.
  • a reaction mixture which can be employed in the context of a process according to the invention preferably contains at least one carboxylic acid or a compound which under the reaction conditions is capable of releasing a carboxylic acid and at least one metal compound which under the reaction conditions with the carboxylic acid a metal carboxylate can react. It is possible in the context of the process according to the invention, in the reaction mixture only one carboxylic acid, d. h. use only one type of carboxylic acid, for example stearic acid. However, it is also possible according to the invention that a reaction mixture which can be used in the context of a process according to the invention contains a mixture of two or more different carboxylic acids.
  • Carboxylic acids which are preferably used according to the invention are, for example, stearic acid, caprylic acid and hydroxystearic acid and mixtures of two or more thereof.
  • a reaction mixture which can be used in the context of a process according to the invention may contain, for example, only one metal compound.
  • a corresponding reaction mixture contains a mixture of two or more metal compounds which can react with a carboxylic acid under the reaction conditions to form a metal carboxylate. It may be In the case of the different metal compounds, for example, different compounds of a certain metal, for example, different compounds of calcium or different compounds of zinc act.
  • a reaction mixture receives different metal compounds such that the reaction mixture contains compounds of different metals, for example compounds of calcium together with compounds of zinc.
  • a reaction mixture used in the context of a process according to the invention may also contain water contain.
  • the amount of water is, for example, in a range from about 0 to about 15% by weight, based on the amount of fatty acid or fatty acid released or related to the amount of fatty acid-releasing compounds.
  • the amount of water in the reaction mixture is about 0 to about 10 wt%, or about 1 to about 4 wt%.
  • the reaction mixture is mixed before contacting with microwaves and with ultrasound in such a way that the reaction proceeds as favorably as possible in terms of yield and product properties.
  • the carboxylic acids or the carboxylic acids are initially charged in a contacting step with microwaves and ultrasound supplying compounds are brought into the most miscible, for example, in a liquid form.
  • the production of a melt of the carboxylic acids or the carboxylic acid precursors ge is suitable.
  • the other components present in the reaction mixture are then mixed intensively with the carboxylic acid or the carboxylic acid precursor.
  • water can be added at this point and a mixing of the water with the other components present in the reaction mixture can be achieved.
  • the mixing of the components present in the reaction mixture can be effected essentially by any mechanical means. It is also possible that mixing of the components present in the reaction mixture is effected by the influence of ultrasound. However, it has in some cases led to good results if prior to treatment with ultrasound and before treatment with microwave radiation intensive mixing of the reaction mixture, for example by treatment of the reaction mixture with a colloid mill, a dissolver or similar mechanical aids.
  • a melt of the carboxylic acids or carboxylic acid precursors is first of all produced and then feeding the metal compound or mixture of two or more metal compounds together with the water to the melt.
  • the reaction mixture thus obtained is supplied to the parts of the reaction apparatus, for example, by means of a pump, which enable irradiation with microwaves or the use of ultrasound.
  • a reaction mixture which can be used in the context of a process according to the invention may comprise, in addition to a carboxylic acid or a mixture of two or more carboxylic acids or a carboxylic acid precursor or a mixture of two or more carboxylic acid precursors or a mixture of one or more carboxylic acids and one or more carboxylic acid precursors and a metal compound or a mixture of two or more Metall ⁇ compounds and optionally water further auxiliaries and additives.
  • auxiliaries and additives are, for example, catalysts or inert solvents, for example from the group of additives for polymers, for example polyolefin waxes.
  • a reaction mixture which can be used in the context of a process according to the invention contains, for example, about 0.1 to about 99% by weight of a carboxylic acid, a carboxylic acid mixture of two or more carboxylic acids, a carboxylic acid precursor, a mixture of two or more carboxylic acid precursors or a mixture of two or more of the above compounds.
  • the proportion of a metal compound or a mixture of two or more Metall ⁇ compounds in the reaction mixture is about 0.1 to about 40 wt .-%.
  • Of the Percentage of water if water is provided in the reaction mixture, is about 0.1 to about 30 wt .-%.
  • the process according to the invention can be carried out with any device which is capable of treating a reaction mixture with microwaves in at least one process step and treating it with ultrasound in at least one process step, both processes optionally being carried out in the context of a single process step Vietnamese ⁇ can be performed.
  • devices that allow batchwise process control are suitable.
  • Vorsatzvor ⁇ devices that support a continuous process management.
  • the subject matter of the present invention is therefore also an apparatus for continuously carrying out a chemical reaction with simultaneous or sequential use of microwaves and ultrasound, comprising at least one mixing device for producing a reaction mixture, at least one device for generating microwave radiation and at least one device for generating ultrasound, wherein the mixing device is connected upstream of the device for generating microwave radiation or the device for generating ultrasound or both.
  • the device for generating microwaves and the device for generating ultrasound can stand essentially in any desired sequence. It is, as already indicated in the context of the present text, so possible that both devices are arranged such that the reaction mixture is simultaneously exposed to microwaves and ultrasound.
  • the entire device for carrying out the method according to the invention comprises, for example, a device for generating microwaves and a device for generating ultrasound.
  • a device according to the invention comprises two or more devices for generating microwaves or two or more devices for generating ultrasound.
  • a reaction mixture may for example be exposed to ultrasound and microwaves in different sequences. The sequence can be alternating.
  • a mixture to be subjected, for example successively, to ultrasound in the context of two or more method steps and then to microwaves during one, two or more method steps.
  • An alternating sequence of microwaves and ultrasound can take place, for example, by switching corresponding devices alternately one behind the other.
  • the reaction mixture it is also possible for the reaction mixture to be exposed to ultrasound or microwaves for an alternating sequence of ultrasound treatment and microwave treatment in the context of a reactor loop until the desired result has been achieved.
  • a device according to the invention comprises a loop for regulating the residence time of the reaction mixture in the device.
  • a corresponding loop can in principle be arranged at any point of the device according to the invention.
  • the residence time in a corresponding loop can be controlled, for example, over the length of the loop or the diameter of the pipe. It is possible and provided that there are possibilities for removal of the reaction mixture at different points of the loop, so that different residence times are made possible.
  • a device according to the invention may only comprise one loop for regulating the residence time.
  • a device according to the invention has two or more loops for regulating the residence time or for performing other actions on the reaction mixture.
  • a device according to the invention can have, for example, at least one possibility for supplying an inert gas.
  • Such a possibility for adding an inert gas is advantageously arranged, for example, at a point which makes it possible to add inert gas before the reaction mixture is treated with ultrasound and microwaves.
  • a device according to the invention can also have further devices which serve to carry out a corresponding method or at least serve to improve it.
  • pumps for promoting the reaction mixture to call are, for example, pumps for promoting the reaction mixture to call.
  • a device according to the invention may for example comprise a device for mixing the individual components of the reaction mixture, for example a colloid mill, dissolver or the like.
  • a device according to the invention comprises, for example, a corresponding batch container in which the reaction mixture can be mixed in the course of a first process step.
  • a device according to the invention may for example comprise components for removing gaseous components from the reaction mixture (vapors, distillation units and the like). Provided that this is conducive to the method carried out in the device, there are also provided locations for taking samples and for removing the product.
  • a device according to the invention may comprise a further device for the corresponding fabrication of a product produced by means of the device according to the invention.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

Procédé et dispositif de production de carboxylates métalliques à partir d'un mélange de réaction. Selon ledit procédé, le mélange de réaction est traité à l'aide de micro-ondes lors d'au moins une étape dudit procédé.
PCT/EP2005/009883 2004-09-15 2005-09-14 Procede de production de carboxylates metalliques WO2006029841A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102004044687.3 2004-09-15
DE200410044687 DE102004044687A1 (de) 2004-09-15 2004-09-15 Verfahren zur Herstellung von Metallcarboxylaten

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WO2006029841A1 true WO2006029841A1 (fr) 2006-03-23
WO2006029841B1 WO2006029841B1 (fr) 2006-05-11

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Cited By (2)

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WO2007093883A2 (fr) * 2006-02-17 2007-08-23 Universita' Degli Studi Di Milano Procédé d'activation de processus chimiques ou chimico-physiques par utilisation simultanée de micro-ondes et d'impulsions ultrasoniques et réacteur chimique réalisant ledit procédé
ITUA20162615A1 (it) * 2016-04-14 2017-10-14 Desmet Ballestra S P A Processo di saponificazione in continuo e apparato

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DE102007055548B4 (de) 2007-11-21 2013-05-08 Baerlocher Gmbh Vorrichtung zum Eintrag von Mikrowellen in einen Reaktionsraum
SG189567A1 (en) * 2011-10-14 2013-05-31 Singapore Polytechnic System and method for providing mixed mode energies during a continuous chemical flow process

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DE2401159A1 (de) * 1973-01-16 1974-07-18 Fuji Photo Film Co Ltd Verfahren zur herstellung von silbercarboxylaten
GB2361918A (en) * 2000-05-06 2001-11-07 Interpole Ltd Transesterification and Hyrolysis Reactions activated by Microwave Radiation
RU2198136C1 (ru) * 2001-10-16 2003-02-10 Бурангулов Наиль Идрисович Способ получения растворов фуллеренов
KR20030058987A (ko) * 2003-05-14 2003-07-07 (주)프탈로스 금속 또는 무금속 프탈로시아닌의 제조방법 및 이를 위한장치
WO2004101574A1 (fr) * 2003-05-14 2004-11-25 Daehan Specialty Chemicals Co., Ltd. Procede et appareil de preparation d'un metal ou de phtalocyanine non metallique

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IT1297850B1 (it) * 1997-06-19 1999-12-20 Giuseppe Pesenti Procedimento di idrolisi di grassi a strato sottile
BR9913755A (pt) * 1998-09-16 2001-06-05 James K Jeanblanc Processo para remover enxofre de materiais carbonáceos contendo enxofre, material carbonáceo de enxofre reduzido, e, óleo bruto pesado da califórnia tratado
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GB2361918A (en) * 2000-05-06 2001-11-07 Interpole Ltd Transesterification and Hyrolysis Reactions activated by Microwave Radiation
RU2198136C1 (ru) * 2001-10-16 2003-02-10 Бурангулов Наиль Идрисович Способ получения растворов фуллеренов
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WO2004101574A1 (fr) * 2003-05-14 2004-11-25 Daehan Specialty Chemicals Co., Ltd. Procede et appareil de preparation d'un metal ou de phtalocyanine non metallique

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007093883A2 (fr) * 2006-02-17 2007-08-23 Universita' Degli Studi Di Milano Procédé d'activation de processus chimiques ou chimico-physiques par utilisation simultanée de micro-ondes et d'impulsions ultrasoniques et réacteur chimique réalisant ledit procédé
WO2007093883A3 (fr) * 2006-02-17 2007-11-08 Univ Degli Studi Milano Procédé d'activation de processus chimiques ou chimico-physiques par utilisation simultanée de micro-ondes et d'impulsions ultrasoniques et réacteur chimique réalisant ledit procédé
ITUA20162615A1 (it) * 2016-04-14 2017-10-14 Desmet Ballestra S P A Processo di saponificazione in continuo e apparato

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WO2006029841B1 (fr) 2006-05-11
DE102004044687A1 (de) 2006-03-30

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