EP0687192A1 - Procede de separation par distillation de melanges de substances multiples faisant appel a une vaporisation - Google Patents

Procede de separation par distillation de melanges de substances multiples faisant appel a une vaporisation

Info

Publication number
EP0687192A1
EP0687192A1 EP94909073A EP94909073A EP0687192A1 EP 0687192 A1 EP0687192 A1 EP 0687192A1 EP 94909073 A EP94909073 A EP 94909073A EP 94909073 A EP94909073 A EP 94909073A EP 0687192 A1 EP0687192 A1 EP 0687192A1
Authority
EP
European Patent Office
Prior art keywords
water
superheated steam
steam
working
substances
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Withdrawn
Application number
EP94909073A
Other languages
German (de)
English (en)
Inventor
Wilfried Rähse
Johann Friedrich Fues
Kathleen Paatz
Hans Scheck
Jozsef Kozma
Rolf Wiedemeyer
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Henkel AG and Co KGaA
Original Assignee
Henkel AG and Co KGaA
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Henkel AG and Co KGaA filed Critical Henkel AG and Co KGaA
Publication of EP0687192A1 publication Critical patent/EP0687192A1/fr
Withdrawn legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D1/00—Evaporating
    • B01D1/16—Evaporating by spraying
    • B01D1/18—Evaporating by spraying to obtain dry solids
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00—Refining fats or fatty oils
    • C11B3/12—Refining fats or fatty oils by distillation
    • C11B3/14—Refining fats or fatty oils by distillation with the use of indifferent gases or vapours, e.g. steam
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
    • B01D3/38—Steam distillation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
    • C07B63/00—Purification; Separation; Stabilisation; Use of additives

Definitions

  • the invention describes proposals for intensifying and / or accelerating the separation by distillation of multi-component material, at least in part of organic origin, using a water vapor stream to facilitate the discharge of water vapor-volatile fractions of the feed material.
  • the teaching of the invention thus particularly affects the cleaning steps used in a wide range of technical applications, which are subordinate to the technical term "steaming".
  • steaming the applicability of the working principle according to the invention goes beyond this.
  • the area of distillative material identification of feed materials that are flowable under working conditions, in which water vapor can be used as a distillation aid is affected.
  • the cleaning of fats and oils of vegetable or animal origin comprises a multi-stage treatment, which usually provides for the damping of the pre-cleaned goods as one of the last process steps.
  • An essential technical goal of this stage is the deodorization of the pre-cleaned material.
  • Unwanted and especially odor-disturbing and often only in trace amounts accompanying substances are here driven off from the valuable substance or mixture of substances by steam distillation.
  • this level of damping can also be used as a distillation aid, for example to facilitate the removal of short-chain fatty acids from the natural fats and oils.
  • Preferred treatment pressures are in the order of 2 to 5 mbar, the temperature, depending on the type of oil, between 240 and 260 ° C.
  • a minimization of steam consumption which can be, for example, 1 to 3% of the amount of oil.
  • the vapor streams contaminated with separated organic constituents have to be worked up.
  • Such cleaning or deodorization is not only important for raw materials. Products of chemical synthesis and the chemical conversion of raw materials of natural origin also require such cleaning steps.
  • the areas of fatty acid processing, fatty alcohol cleaning or the production of, in particular, liquid esters, which can be processed in the direction of cosmetics, pharmaceuticals and foodstuffs, are mentioned here merely by way of example. Some specific representatives are listed by way of example only: Guerbet alcohol, oleic acid ester, soybean oil epoxide, isopropyl myristate, triacetin and the like.
  • reaction products Another typical field of work for the use of cleaning by steaming with industrial importance is the removal of residues based on ethylene oxide and / or propylene oxide from reaction products, which by ethoxylation and / or propoxylation of organic compounds with at least one active Hydrogen atom have been produced.
  • Compounds of this type are of great importance, for example, as nonionic surfactants or as intermediates for the preparation of anionic surfactant compounds. They are used, for example, in the field of detergents and cleaning agents, but also to a large extent in the field of cosmetics or pharmaceutical auxiliaries.
  • the reaction products primarily obtained contain traces of ethylene oxide and / or propylene oxide as well as of undesired reaction secondary products such as dioxane due to the production process.
  • US Pat. No. 4,443,634 describes a process for cleaning fatty alcohol polyglycol ethers in which the material to be cleaned is sprayed into a chamber from which the impurities are drawn off in vapor form.
  • the material to be cleaned should be sprayed in an inert atmosphere, choosing the pressure is that droplets with a particle diameter of 50 to 1000 ⁇ m are formed. These droplets are said to be exposed to the inert gas atmosphere in the second range and then to be collected. Nitrogen, helium and argon are mentioned as inert gases.
  • the contaminants to be separated off by this spray treatment are, in particular, ethylene oxide, propylene oxide, dioxane, water and alcohol.
  • the spraying of the liquid phase into the space filled with inert gas can also be repeated several times in successive process steps.
  • the invention relates in a first embodiment to a method for intensifying and / or accelerating the separation by distillation of at least partially organic multicomponent mixtures using a water vapor stream to facilitate the discharge of water vapor-volatile fractions of the feed material - hereinafter also referred to as "steaming" -
  • This method is characterized in that a flowable feed under the treatment conditions is damped in finely divided form.
  • This steaming in the sense of the teaching according to the invention is carried out with steam superheated at working pressure.
  • the liquid phase to be cleaned is sprayed with the aid of a propellant gas, it being particularly advantageous to use multi-substance spray nozzles.
  • at least partially superheated steam is used as the propellant.
  • the invention relates to the use of this method in a wide variety of technological sub-areas.
  • One of the areas of importance according to the invention relates to cleaning, in particular the deodorization of fats and / or oils for their use, for example as food, in the field of cosmetics and / or for use as pharmaceutical auxiliaries.
  • Another area of application relates to the production of flavoring substances and flavoring concentrates.
  • Another important application is the use of the method to improve the degree of purity of valuable substances and mixtures of valuable substances of vegetable and / or synthetic origin from the field of wetting agents, detergents and / or cleaning agents, in particular for their use in the fields of textile treatment, for example in Textile detergents, cosmetics and / or pharmaceutical auxiliaries.
  • the invention relates here in particular to the use of the process described for the purification of alkoxylated valuable substances and valuable substances, in particular for the removal of impurities such as unreacted residues of EO, PO or their secondary products, such as 1,4-dioxane.
  • teaching according to the invention also relates very generally to the use of the working principles described below as a distillation aid in the separation of at least partially difficult-to-volatile mixtures of substances.
  • An essential core of the action according to the invention lies in the following exchange:
  • the conventional deodorization of, for example, fats and oils in a batch process presents the liquid to be deodorized in a closed phase
  • the water vapor used for steaming is passed through, for example Star-shaped or ring-shaped or in any other way designed injection systems in a plurality of outlet openings for the water vapor finely dispersed into the closed liquid phase to be cleaned and passed through it.
  • the teaching of the invention reverses this working principle.
  • the feed which is flowable under the treatment conditions is brought into phase contact with the water vapor in finely divided form.
  • the water vapor usually forms the closed phase.
  • the liquid material to be deodorized can be sprayed in a manner known per se.
  • the wide range of relevant technology for single-substance and / or multi-substance nozzles and the associated process technologies and process parameters are available. It is not necessary to maintain long residence times of the material to be deodorized in the sprayed state, in particular if the further sub-principles of the invention described below are also used.
  • the transfer of the material to be cleaned into the finely sprayed state and the interaction with the closed water vapor phase can, if desired, be repeated several times. You can work with the steam already used and / or with live steam in the individual spray stages.
  • the multiple spraying can take place in only one work unit or in a plurality of separate and successive work units.
  • the choice of the respective working pressure determines the boiling temperature of the water under working conditions.
  • the invention provides that the steaming is carried out with superheated steam at the respective working pressure. Accordingly, when working at normal pressure, it is preferred to keep the water vapor phase at temperatures above 100 ° C. In this context, the operating temperatures of the water vapor can be of particular importance.
  • the specific operating temperature of the superheated steam to be selected is in turn influenced or determined by a number of parameters. Significant influencing variables are, for example, the volatility of water vapor and the amount of the material components to be converted into the vapor phase from the multicomponent mixture to be treated. However, the temperature sensitivity of the material to be treated in its entirety must also be taken into account.
  • Temperature profiles in the individually sprayed droplets of this type can be desired in special cases and set specifically. As a rule, however, it will be preferred to spray the feed to be steamed into the vapor phase with a minimum temperature which corresponds at least approximately to the boiling temperature of the water under working pressure.
  • the operating temperatures of the superheated steam are preferably at least 10 to 30 ° C. and in particular at least 50 ° C. above the boiling point of the water at the selected working pressure of the cleaning stage. Unless there are any fundamental concerns - for example, from a temperature sensitivity of the material to be steamed that is to be taken into account - significantly higher operating temperatures of the water vapor are selected. It may be expedient that this operating temperature of the water vapor is at least 100 ° C. and in particular at least 150 to 200 ° C. above the boiling point of the water at the working pressure of the cleaning stage.
  • the temperature of the superheated steam used being used approximately corresponding to the temperature of the liquid material to be damped, but if desired also below this can, however, as a rule be chosen with an inlet temperature which is again above the operating temperature of the liquid material.
  • the method according to the invention provides for the flowable material, which is present and in particular to be cleaned as a liquid phase at working temperature, to be sprayed into a stream of the preferably superheated steam and subsequently to separate the liquid phase from the vapor phase. Details on the practical design of these work stages are given below with the discussion of the attached FIGS. 1 to 3. First of all, let us consider the special feature already mentioned, which relates to particularly preferred embodiments of the teaching according to the invention.
  • the flowable phase to be cleaned is sprayed with the aid of a propellant gas.
  • the relevant technology knows the most diverse configurations of such spray devices, in particular spray nozzles. Reference is made to the relevant specialist literature, see for example H. Brauer “Fundamentals of the Phase and multi-phase flows "in BASICS OF CHEMICAL TECHNOLOGY, process engineering in chemical and related industries, Verlag Sauerators, Aarau and Frankfurt am Main (1971), pp. 308-323, AH Lefebvre” Ato ization and Sprays "Hemisphere Publishing Corp. New York (1989), pp. 10-20, Chemical Engineering, Vol. 2, Unit Operations (2nd Edition - 1968) Pergamon Press, Oxford, New York, pp.
  • multi-substance spray nozzles and co-use of propellant gas are used, the most important embodiment of the invention using at least partially overheated water vapor as the propellant gas.
  • the most important embodiment is the use of superheated steam as the sole propellant for spraying the flowable multicomponent mixture and its transfer into the finely dispersed liquid phase.
  • the teaching of the invention enables the use of practically all of the water vapor used as a propellant. tel during the atomization process of the liquid phase to be cleaned.
  • a predetermined flow direction of the gas phase in the spray chamber is set and maintained by a partial flow of, in particular, superheated steam.
  • an important modification of the method according to the invention provides for working without using the propellant gas based on superheated steam in such a way that the flowable, at least predominantly organic feedstock to be cleaned is sprayed into the stream of superheated steam in finely divided form.
  • the decoupling of the superheated water vapor as a working medium in the spraying process - in this embodiment it is possible to work with single-component nozzles in a manner known per se - in particular allows the amount of superheated water vapor used to be reduced, based in each case on a basic unit of the organic liquid material to be cleaned .
  • the operating parameters of the respectively selected and used work stages in the sense of the action according to the invention are based on the corresponding information from the prior art.
  • the working pressures can be selected in the range from about 1 to 50 mbar, in particular in the range from about 3 to 30 mbar, provided that the cleaning of difficultly volatile feedstocks - for example fats and / or oils of natural origin - is to be carried out.
  • important embodiments of the teaching according to the invention provide for cleaning in the spray zone in the range of normal pressure or in the range of only moderately reduced pressures.
  • the required quantities of superheated water vapor are determined by the parameters to be taken into account, in particular by the choice of the feed material and the extent of its load, as well as by the specifically selected process technology.
  • the amounts of steam used are usually in the range from approximately 1 to 30% by weight of the items to be cleaned, preferably in the range from approximately 5 to 20% by weight for the embodiment of working with the superheated steam Propellant.
  • quantities of steam in the range from about 2 to 10% by weight, based on the feed material to be steamed can be particularly preferred.
  • Particularly suitable feedstocks for this work without propellant gas are at least largely water-free. Organic substances with a water content of ⁇ 10% by weight, expediently ⁇ 5% by weight and in particular ⁇ 1-3% by weight are preferred.
  • the mean droplet sizes of the sprayed product are in the technically accessible range of, for example, 20 to 500 ⁇ m and in particular in the range of approximately 50 to 200 ⁇ m.
  • the duration of treatment in the respective working stage is in the range of seconds and, as already mentioned, can be increased by a multi-stage working method, but is then still extremely short in comparison to the methods of steaming customary today, even in its highly developed embodiments.
  • 1 and 2 show in a schematic representation the batch deodorization of a feed material which is liquid and sprayable at the working temperature.
  • work can be carried out both at normal pressure and at any desired negative pressure.
  • Fig. 1 shows a batch deodorization in the boiler 1, the wall of which is thermally insulated and / or equipped with the possibility of heating 2.
  • a de-mister device 3 for example a corresponding vapor-permeable packing, is provided in the head part of the boiler, below which one or more spray nozzles 4 are arranged.
  • the water vapor is partly supplied to the multi-component nozzle 4 via line 5 and the superheater 6; if desired, a portion of the steam can also be supplied to a distributor element 7 provided in the bottom part of the boiler 1.
  • the liquid material 8 to be cleaned is drawn off by means of the pump 9 via line 10 at the bottom of the boiler 1.
  • the superheated steam laden with the impurities which have passed into the vapor phase is drawn off via line 12 by means of the pump 13.
  • Controlled cooling of the superheated steam can take place by means of the heat exchangers 14 and 15, so that condensed portions of the material taken off can be removed via 16, 17 and 18.
  • the batch of material can be removed and a new batch of the material to be cleaned can be introduced into the device via line 19.
  • a packing element 20 is provided between the spray nozzle 4 and the liquid phase 8 in the bottom part of the boiler 1 as additional help for phase separation, as is known and used, for example, in today's separation column technology for distillation and absorption.
  • Corresponding packing elements made of metal and / or plastic are working elements which are customary, in particular, for separating substances by distillation, absorption and desorption in separation columns, cf. for example the commercial brochure "Separation columns for distillation and absorption" from the company Gebrü ⁇ der Sulzer AG, product area Chemtech separation columns, Winterthur, CH (22.13.06.20-V.91-100).
  • a multi-stage damping in the sense of the invention is the subject of FIG. 3, which is based on a continuous procedure.
  • a heatable column 21, if desired, is divided into three sections by sufficiently vapor-permeable separating elements 22 and 23.
  • the vapor-permeable separating elements 22 and 23 can be designed, for example, in the form of suitable sieve trays, but also as bell bottoms or in a known manner.
  • the crude product supplied via the feed line 24 by means of the pump 25 is heated in the heat exchanger 29 and placed in the top of the column 21.
  • the working steam emerging from the column 21 via line 30 at the top and contaminated with the contaminants to be removed is first again intensively exchanged with the freshly introduced liquid product in the upper top part of the column. 3 the bell bottoms 31 are provided for this.
  • This separating element can serve, in particular, to ensure the reliable separation between the gas phase and the liquid phase in the ascending, loaded steam flow.
  • the liquid material is drawn off via line 32 by means of the pump 26 and fed directly to the spray nozzle 28.
  • the liquid phase is sprayed in finely divided form as a propellant gas by means of the superheated live steam supplied via lines 33 and 34.
  • the sprayed material strikes the separating element 35, shown again in FIG. 3 as a bubble cap, which serves for a first separation of the gas and liquid phases.
  • the gas phase rises up through the sieve tray 22 and is withdrawn from the separation column by means of the pump 36 via line 30 and the heat exchanger 37.
  • the liquid phase leaves the separating element 35 downwards and is collected by the sieve plate 23.
  • the closed, collected liquid phase is fed via line 38 and pump 39 to the next spray zone with the spray nozzle 40.
  • the renewed treatment takes place in the sense of the method according to the invention using the gas supplied via lines 33 and 41. performed live steam instead.
  • the sprayed material from this treatment stage strikes the pack 42.
  • the information relating to FIG. 2 and the pack 20 provided there at the appropriate place apply analogously here.
  • Purified liquid product is discharged at the bottom of the column via 45 by means of the pump 46, cooled in the heat exchanger 29 with the raw product supplied and removed via 47.
  • working pressures can be freely selected in the interior of the separating devices and set in a predetermined manner.
  • Pumps 13 and 36 are particularly suitable for pressure regulation in the area of normal pressure or vacuum. If, for reasons of high volatility of individual product parts, working at overpressures is desired, the pumps for moving the liquid product streams - the pumps 9 in FIGS. 1 and 2 and the pumps 25, 26, 39 and 46 in FIG. 3 - into consideration.
  • the teaching according to the invention comprises both the treatment of essentially anhydrous and the treatment of feed materials containing water.
  • a corresponding prerequisite for carrying out the method according to the invention is the technical possibility of being able to spray the multicomponent mixture to be processed in finely divided form under working conditions, the superheated steam in particular being used as the propellant gas.
  • the embodiments of the action according to the invention are dealt with in more detail, which deal with the use of corresponding water-containing feedstocks and their treatment in the process according to the invention.
  • a feed material containing water under working conditions can be subjected to the treatment according to the invention, which should be dried under process conditions and preferably freed from accompanying substances which are more volatile in steam.
  • the removal of the water from a water-containing material or material mixture is to be understood as a separation by distillation in the sense of the action according to the invention, so that here the simple acceleration of drying by using the superheated steam as propellant for fine-particle spraying of the feedstock is to be understood - preferably by means of suitable multi-component nozzles - can mean realizing the teaching according to the invention.
  • the peculiarities of the action according to the invention make such pure drying a special case that hardly ever occurs in practice.
  • Recyclable materials and mixtures of recyclable materials used in large-scale industrial practice are often at least loaded with traces of impurities which are discharged in the course of the process according to the invention during steaming and simultaneous drying via the vapor phase.
  • the recyclable slurry to be processed is sprayed with nitrogen as a propellant gas via a two-component nozzle and dried in countercurrent with superheated steam.
  • the superheated steam is used directly as the propellant gas. In this way, both the cleaning result and the drying of the material mixture used can be substantially improved and accelerated.
  • the teaching of the earlier application for industrial property rights mentioned above also relates in particular to the production of recycled materials and mixed materials which have been cleaned in the dried state.
  • the teaching now given according to the invention extends to water-containing and sprayable preparations of such valuable substances or mixtures of valuable substances.
  • the work results possible in the processing of such feed materials and the work parameters to be complied with are the subject of, in particular, the applicant's earlier German patent application DE-A 4234376.
  • This older application describes how a microporous good structure can be formed and fixed in a feed material primarily obtained by steam drying and how, based on this, mixtures of valuable materials of the product area concerned here can be designed in a previously unknown manner.
  • the teaching according to the invention in the last discussed embodiment covers the combination of the cleaning of the used material or mixture of materials by steaming and the drying of the water-containing preparations used, at the same time the elements from the older German patent application DE-A 4234376 the applicant are taken into account.
  • the teaching of the invention thus describes, inter alia, a method which is characterized in that solid or recyclable materials are used in a flowable and sprayable aqueous preparation which, under the working conditions of steaming and superheated steam drying, are suitable for forming solid bodies with an open-pore internal structure whose plasticity and surface stickiness are preferably restricted such that substantial sticking of the particles to one another and / or their open-pored inner structure also occur under the conditions of the action of the superheated steam.
  • the teaching according to the invention also encompasses the processing of such valuable materials or mixtures of valuable materials which are water-containing forms of preparation of valuable materials or valuable materials mixed under normal conditions.
  • the aspects of the separation of undesirable water vapor-volatile components can advantageously be combined with partial or complete drying by superheated steam.
  • materials of this type are water-containing alkoxylation products of feed compounds with at least one reactive hydroxyl group that are flowable under normal conditions, for example corresponding water-containing preparations of nonionic components.
  • the invention enables the effective separation of these undesirable trace impurities and the simultaneous drying of the goods originally containing water to a predetermined extent. Taking into account the general specialist knowledge, it is immediately evident that the procedural measures and work equipment to be selected in the individual case are to be adapted to the conditions specified by the product properties.
  • the teaching according to the invention encompasses modes of operation in which the phase of the superheated steam loaded with discharged fractions of the feedstock is at least partially freed from the incorporated fractions of the feedstock after it has been separated from the cleaned goods.
  • valuable materials can be separated from the loaded vapor phase and recovered and / or problems from wastewater disposal can be prevented, but, if desired, the cleaned aqueous phase can also be recycled.
  • the selection and adaptation of the respective membrane separation processes according to the type and nature of the selected membranes and the particular technology used is determined by the mixture of substances to be separated.
  • the loaded aqueous phase can be worked up in one stage or in several stages.
  • the selection of suitable membrane types ranges from microfiltration to ultra and nanofiltration to reverse osmosis.
  • the technical action is determined in detail by the particularities of the mixture of substances to be separated which are to be taken into account in each case.
  • FIGS. 4 and 5 show, in a schematic representation, possibilities for such a separation of substances in aqueous condensate phases which are obtained as a liquid phase as a rule under normal conditions by taking up the portions to be separated off from the feed material and after condensation of the vapor phase.
  • FIG. 4 shows a schematic representation of the treatment of steaming according to the invention with the treatment of the loaded waste steam or waste water.
  • the steaming stage is provided in a 2-stage cascade arrangement. The following applies in particular:
  • the feed to be damped is fed via the heat exchanger 48 through line 49 to the head of the container 50 and is sprayed here in finely divided form via one or more spray nozzles 51.
  • Live steam is fed via line 53 after heating to the desired working temperature in the heat exchanger 52 to the distributor element 54 in the lower part of the container 50 and builds up the closed phase of the superheated steam in this working space. It is additionally provided as a possibility to supply this superheated water vapor at least in part as a propellant gas via line 55 to the spray nozzle (s) 51.
  • the damped liquid material is drawn off via line 57 by means of a pump 56 and is introduced via line 58 into the head of the second spray container 59 and is sprayed here in finely divided form by means of the spray nozzle (s) 60.
  • Superheated live steam is transferred to this spray zone Line 61 and the distributor element 62 supplied in the lower part of the container 59.
  • the superheated steam is supplied to the spray system 60 in part or completely as a propellant gas via line 63.
  • the dampened liquid material is drawn off by means of the pump 64 via line 65 and can be removed via 66.
  • the phase of the superheated steam laden with volatiles which have been absorbed is withdrawn from the head of the first container 50 via line 67 and from the head of the second container 59 via line 68 and fed to the condenser 69 and condensed here.
  • the resulting liquid is fed to the intermediate container 70 via line 84.
  • the aqueous phase collected here and loaded with discharged organic components is drawn off by means of pumps 72 and 73 via 71 at the bottom of the intermediate container 70 and fed into the membrane separation plant 75 via line 74.
  • the permeate passes through the semi-membrane membrane 76 and can be removed via line 77 and, for example, fed to the conventional wastewater treatment.
  • the retentate that does not pass through the separation membrane is removed via line 78.
  • FIG. 4 also shows the possibility of working up the uncondensed gas phase occurring in the condenser 69. Under the influence of the blower 80, this gas phase is fed via line 81 to the tower 82 filled with an absorbent and is fixed here to the solid adsorbent. In a manner known per se, the step-by-step desorption of the absorbed good components is made possible by arranging a second absorption tower. These can, for example, be fed via line 83 to the storage container 70 and then together with the via line 84 condensate fed from the condenser 69 can be worked up in the manner described above.
  • FIG. 5 only shows a variation in the configuration of the membrane separation process for the liquefied condensate from the previous cleaning stage with superheated steam, which is no longer shown in detail here.
  • the condensate of the superheated steam phase loaded with discharged portions of the feed material is fed via line 84 to the reservoir 70 and is fed into the first membrane separation stage 75 via line 71 by means of pumps 72 and 73 via line 74.
  • the permeate passes through the semipermeable membrane 76 and is withdrawn via line 77.
  • the retentate leaves this first membrane separation stage via line 78 and can be partly circulated by means of pump 73 and line 74 and / or removed via line 79 and sent for further use and / or destruction.
  • the permeate of the first membrane separation drawn off via line 77 is fed to the storage container 85 and fed to the second membrane separation stage 90 via line 86 by means of pumps 87 and 88 via line 89.
  • the permeate passes through the semipermeable membrane 91 and is drawn off via line 92, for example as sufficiently purified waste water.
  • the retentate leaves this second membrane stage via line 93 and can at least partly be circulated here by means of pump 88 and line 89. Instead of or at the same time, the circulation of this retentate via line 94 and its return to the storage container 70 of the first membrane separation stage is shown as a work possibility.
  • the damping in particular for deodorization of fats and / or oils for their use, for example in the field of food, in the field of cosmetics and / or as pharmaceutical auxiliaries.
  • the cleaning of alkoxylated and recyclable materials especially for the removal of impurities of the type mentioned above.
  • the teaching according to the invention is also particularly suitable as a distillation aid for the separation of at least partially difficultly volatile mixtures of substances.
  • the respective working conditions in particular temperature and pressure
  • the principle of facilitating material separation by steam distillation can be used effectively.
  • the above-mentioned removal of excess free fatty alcohols from the reaction mixtures of the APG production is a typical example of this application concept of the invention.
  • An important area of application in special cases can also be simply the effective removal of otherwise difficult-to-remove residual amounts of water from a feed material and thus the effective drying of such valuable substances or valuable substances.
  • the method according to the invention by adapting its parameters, in particular pressure and temperature, enables work results which are often difficult to set in conventional separation methods and can only be set with increased effort.
  • the design according to the invention for carrying out a steam-based distillative material separation is exceptionally broad possible forms of application are technically meaningful and advantageous to use or exploit.
  • the separation of small and very small quantities of disruptive additions, which often entails considerable technical difficulties, is just as effective and technologically easy to obtain as the separation of substances by steam distillation, in which a considerable or even large amount of the feed material has to be separated from the distillation residue.
  • An example of this can be the production of aromatic substances which are discharged by means of the superheated steam phase and then separated and recovered therefrom.
  • the esterification of fatty acid with glycerol to a glycerol tri-oleate (Myritol 318 ( R ), Henkel) was carried out in a reaction vessel at 180 to 220 ° C using a catalyst.
  • the water of reaction obtained was first stripped off under normal pressure, then under vacuum.
  • the esterification reaction lasted about 15 hours.
  • the ester was then deacidified in a refining container with 10% sodium hydroxide solution, washed and dried in vacuo. After bleaching using diatomaceous earth as bleaching agent and filtration, the residual fatty acid content is removed in a deodorization step.
  • the glycerol-tri-oleate ester is sprayed into a standing deodorization container through a 2-component nozzle using superheated steam as the propellant gas.
  • the ester collects on the bottom of the container and is fed to the nozzle device again by a pump.
  • superheated steam is introduced into the deodorization tank via a lance system in counterflow to the liquid.
  • the steam and the entrained odorous substances are discharged via a vacuum system consisting of a steam jet compressor with a water ring pump. Table 1 below shows the dimensions of the container and nozzle as well as the operating parameters.
  • Example 1 A cetylstearyl alcohol (Lanette ⁇ ( R ), from Henkel) is deodorized by spraying through a 2-component nozzle.
  • the cetylstearyl alcohol is a mixture of higher saturated fatty alcohols, mostly cetyl and stearyl alcohol. It is a skin-friendly raw material and consistency-giving factor with emulsion-stabilizing properties for emulsions, in particular creams and acidic hair treatment preparations and pharmaceutical ointments.
  • the short-chain free fatty alcohols of chain lengths CJO to C14 obtained from the production reduce the product quality due to their unpleasant odor. These fatty alcohols are removed by 95% by weight in a 2-stage deodorization.
  • the APG was produced via direct synthesis (1-stage process), in which the glucose, which is insoluble in fatty alcohol, is reacted with fatty alcohol directly to give the alkyl polyglycoside.
  • the reaction mixture consisted of 30% by weight APG and 70% by weight fatty alcohol. The majority of the excess fatty alcohol is separated off at 10 mbar and 160 ° C. in a falling film evaporator. The fatty alcohol content was then 8% by weight. This residual fatty alcohol amount is reduced to ⁇ 1% by weight in a 3-stage deodorization system according to specifications.
  • the APG feedstock to be cleaned is sprayed with superheated steam (160 ° C.) as the propellant gas via a two-component nozzle (diameter 1 mm).
  • superheated steam 160 ° C.
  • the resulting viscous APG paste is removed from the deodorization tank by forced discharge. Diluted with water to an active substance content of 50% by weight and bleached. Due to the short dwell time in the 2nd stage of the removal of fatty alcohol at the high temperatures of approx. 160 ° C there was only a slight brown color. In this way, the bleaching of the aqueous APG paste with H2O2 can be relieved. In the aqueous form with 50% by weight of active substance, the APG product is easily flowable at about 40 ° C.
  • a soybean oil was deodorized.
  • the deodorization removes undesirable odors and flavors, which are formed mainly by oxidative and hydrolytic reactions on a chemical or enzymatic basis. Mainly, these are aliphatic, saturated and unsaturated aldehydes of C6_ ⁇ o- Re ihe, aliphatic ketones (methylheptyl, methylnonyl, methylundecyl ketone, etc.) so ⁇ as low molecular weight fatty acids.
  • the bleaching treatment step gives the oil an earthy odor. Fat hardening leads to the typical hardening smell and taste.
  • Hydrogenated soybean oil has been shown to contain up to 37 volatile compounds, predominantly higher aldehydes, ketones, lactones and alcohols.
  • the tank pressure was 5 mbar. * With a circulation ratio of 4, the final free fatty acid content was 0.04% by weight. The sensory test was positive.
  • Example 4 The procedure was as in Example 4. An olive oil was deodorized. The temperature of the oil was 220 ° C. After one Circulation ratio of 4, the required quality in terms of smell and taste is achieved.
  • Table 3 shows the oils used for deodorization, the internal container pressure (mbar) and the temperature of the oil sprayed through the two-component nozzle (superheated steam as propellant).
  • Glycerol is reacted with the ⁇ -io fatty acids in the presence of a catalyst under normal pressure at 120 to 200 ° C. to form the triester.
  • the esterification is then continued under increasing vacuum. Total reaction time about 14 hours.
  • the damping with nitrogen takes place under the same operating conditions.
  • the reaction product is cooled, bleached and filtered.
  • the deodorization is then carried out by spraying in superheated steam (2-component nozzle, diameter 0.5 mm, pressure in the deodorization tank 5 mbar, superheated steam as propellant) under the following conditions:
  • Example 12 Deodorizing is used as the starting materials to be cleaned, n-butyl stearate (example 13) and isobutyl stearate (example 14), each produced from Ci6_i8 fatty acid mixtures and n-butanol or isobutanol.
  • the respective process product was odorless after 5 runs.
  • the fatty alcohols or ethoxylated fatty alcohols identified in Table 5 below are deodorized as indicated in Examples 4 to 14 using a two-component nozzle (superheated steam as propellant) in countercurrent to the additionally introduced superheated steam.
  • Table 5 summarizes the feed materials to be deodorized, their operating temperature and the working pressure in the deodorizing tank (mbar): The products were adequately cleaned after every 5 runs.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Microbiology (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Cosmetics (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

Un procédé permet d'intensifier et/ou d'accélérer la séparation par distillation de mélanges de substances multiples au moyen d'un courant de vapeur d'eau (5, 7) qui permet d'enlever plus facilement les composants volatils dans la vapeur d'eau des matières à séparer (vaporisation). Selon ce procédé, les matières à séparer (4, 19, 1) qui sont fluides dans les conditions de traitement sont vaporisées sous forme finement pulvérisée. De préférence, on utilise de la vapeur d'eau surchauffée à la pression de traitement; cette vapeur d'eau sert notamment au moins en partie comme gaz propulseur permettant de pulvériser les phases liquides à purifier. Les substances à traiter sont pulvérisées à l'aide de ce gaz propulseur par des tuyères de pulvérisation de substances multiples. Si l'on adapte les paramètres de traitement, notamment la température et la pression de travail, ce procédé peut se prêter à une large gamme d'applications.
EP94909073A 1993-03-06 1994-02-25 Procede de separation par distillation de melanges de substances multiples faisant appel a une vaporisation Withdrawn EP0687192A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE4307115 1993-03-06
DE4307115A DE4307115A1 (de) 1993-03-06 1993-03-06 Verbessertes Verfahren zur destillativen Trennung von Mehrstoffgemischen durch Dämpfen
PCT/EP1994/000563 WO1994020187A1 (fr) 1993-03-06 1994-02-25 Procede ameliore de separation par distillation de melanges de substances multiples faisant appel a une vaporisation

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EP0687192A1 true EP0687192A1 (fr) 1995-12-20

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EP (1) EP0687192A1 (fr)
JP (1) JPH08507464A (fr)
KR (1) KR960700785A (fr)
CN (1) CN1118995A (fr)
AU (1) AU6207194A (fr)
CA (1) CA2157660A1 (fr)
CZ (1) CZ215995A3 (fr)
DE (1) DE4307115A1 (fr)
PL (1) PL310531A1 (fr)
WO (1) WO1994020187A1 (fr)

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DE4402883A1 (de) * 1994-02-01 1995-08-03 Henkel Kgaa Optimiertes Verfahren zur Aufarbeitung von wasserdampfbasierten Brüdenströmen
DE4420730A1 (de) * 1994-06-15 1995-12-21 Henkel Kgaa Verfahren zur Desodorierung und Stabilisierung biotechnologisch gewonnener Wertstoffe und ihrer wäßrigen Zubereitungen
GB9804479D0 (en) * 1998-03-02 1998-04-29 Chemtech International Ltd Stripping of volatile substances from less volatile fluids
CN102058989B (zh) * 2010-11-30 2013-01-16 洁星环保科技投资（上海）有限公司 一种螺旋送料蒸发器的蒸发工艺
CN102553275A (zh) * 2012-03-16 2012-07-11 瑞安市四方药化机械有限公司 一种常温蒸发浓缩机
JP6001347B2 (ja) * 2012-06-22 2016-10-05 株式会社ブリヂストン 混合液体の分離方法
CN109865304A (zh) * 2017-12-01 2019-06-11 田高 一种溶液中多物质的提取工艺及提取装置
WO2021173738A1 (fr) 2020-02-28 2021-09-02 The Procter & Gamble Company Procédé d'élimination de contaminants chimiques
CN115430165B (zh) * 2022-09-14 2023-12-01 轻工业杭州机电设计研究院有限公司 磺化二噁烷脱除设备
CN116077961B (zh) * 2023-02-01 2024-02-02 江苏森禾化工科技有限公司 一种自动电脱醇方法及使用该方法的脱醇釜

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GB1269771A (en) * 1968-02-16 1972-04-06 Arjun Dev Passey Method of and apparatus for treating material
NL173768C (nl) * 1971-06-01 1984-03-01 Stork Amsterdam Werkwijze en inrichting voor het onder vacuuem behandelen van vloeistoffen met een gasvormig stripmedium.
US4171243A (en) * 1975-06-17 1979-10-16 The Chemithon Corporation Spray drying method
DE4030688A1 (de) * 1990-09-28 1992-04-02 Henkel Kgaa Verfahren zur spruehtrocknung von wertstoffen und wertstoffgemischen unter verwendung von ueberhitztem wasserdampf

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See references of WO9420187A1 *

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CN1118995A (zh) 1996-03-20
WO1994020187A1 (fr) 1994-09-15
KR960700785A (ko) 1996-02-24
DE4307115A1 (de) 1994-09-08
PL310531A1 (en) 1995-12-27
CA2157660A1 (fr) 1994-09-15
JPH08507464A (ja) 1996-08-13
CZ215995A3 (en) 1996-02-14
AU6207194A (en) 1994-09-26

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