EP2452071B1 - Procédé de transport de liquides - Google Patents

Procédé de transport de liquides Download PDF

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Publication number
EP2452071B1
EP2452071B1 EP20100728254 EP10728254A EP2452071B1 EP 2452071 B1 EP2452071 B1 EP 2452071B1 EP 20100728254 EP20100728254 EP 20100728254 EP 10728254 A EP10728254 A EP 10728254A EP 2452071 B1 EP2452071 B1 EP 2452071B1
Authority
EP
European Patent Office
Prior art keywords
liquid
pump
auxiliary liquid
auxiliary
conveyed
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.)
Not-in-force
Application number
EP20100728254
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German (de)
English (en)
Other versions
EP2452071A1 (fr
Inventor
Joachim Pfeffinger
Willi Gilcher
Jürgen MORELL
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.)
BASF SE
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BASF SE
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Filing date
Publication date
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Priority to EP20100728254 priority Critical patent/EP2452071B1/fr
Publication of EP2452071A1 publication Critical patent/EP2452071A1/fr
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Publication of EP2452071B1 publication Critical patent/EP2452071B1/fr
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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04B—POSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
    • F04B53/00—Component parts, details or accessories not provided for in, or of interest apart from, groups F04B1/00 - F04B23/00 or F04B39/00 - F04B47/00
    • F04B53/14—Pistons, piston-rods or piston-rod connections
    • F04B53/141—Intermediate liquid piston between the driving piston and the pumped liquid
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04B—POSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
    • F04B15/00—Pumps adapted to handle specific fluids, e.g. by selection of specific materials for pumps or pump parts
    • F04B15/04—Pumps adapted to handle specific fluids, e.g. by selection of specific materials for pumps or pump parts the fluids being hot or corrosive
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04B—POSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
    • F04B39/00—Component parts, details, or accessories, of pumps or pumping systems specially adapted for elastic fluids, not otherwise provided for in, or of interest apart from, groups F04B25/00 - F04B37/00
    • F04B39/0005—Component parts, details, or accessories, of pumps or pumping systems specially adapted for elastic fluids, not otherwise provided for in, or of interest apart from, groups F04B25/00 - F04B37/00 adaptations of pistons
    • F04B39/0011—Component parts, details, or accessories, of pumps or pumping systems specially adapted for elastic fluids, not otherwise provided for in, or of interest apart from, groups F04B25/00 - F04B37/00 adaptations of pistons liquid pistons
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04B—POSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
    • F04B43/00—Machines, pumps, or pumping installations having flexible working members
    • F04B43/02—Machines, pumps, or pumping installations having flexible working members having plate-like flexible members, e.g. diaphragms
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04F—PUMPING OF FLUID BY DIRECT CONTACT OF ANOTHER FLUID OR BY USING INERTIA OF FLUID TO BE PUMPED; SIPHONS
    • F04F1/00—Pumps using positively or negatively pressurised fluid medium acting directly on the liquid to be pumped
    • F04F1/02—Pumps using positively or negatively pressurised fluid medium acting directly on the liquid to be pumped using both positively and negatively pressurised fluid medium, e.g. alternating
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04F—PUMPING OF FLUID BY DIRECT CONTACT OF ANOTHER FLUID OR BY USING INERTIA OF FLUID TO BE PUMPED; SIPHONS
    • F04F1/00—Pumps using positively or negatively pressurised fluid medium acting directly on the liquid to be pumped
    • F04F1/06—Pumps using positively or negatively pressurised fluid medium acting directly on the liquid to be pumped the fluid medium acting on the surface of the liquid to be pumped
    • F04F1/14—Pumps using positively or negatively pressurised fluid medium acting directly on the liquid to be pumped the fluid medium acting on the surface of the liquid to be pumped adapted to pump specific liquids, e.g. corrosive or hot liquids
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04F—PUMPING OF FLUID BY DIRECT CONTACT OF ANOTHER FLUID OR BY USING INERTIA OF FLUID TO BE PUMPED; SIPHONS
    • F04F1/00—Pumps using positively or negatively pressurised fluid medium acting directly on the liquid to be pumped
    • F04F1/18—Pumps using positively or negatively pressurised fluid medium acting directly on the liquid to be pumped the fluid medium being mixed with, or generated from the liquid to be pumped
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T137/00—Fluid handling
    • Y10T137/0318—Processes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T436/00—Chemistry: analytical and immunological testing
    • Y10T436/25—Chemistry: analytical and immunological testing including sample preparation
    • Y10T436/2575—Volumetric liquid transfer

Definitions

  • the invention relates to a process for the continuous production of a liquid which is used as feedstock in a chemical process.
  • the invention further relates to a process for the hydrogenation of aromatic compounds, in particular aromatic amines, and a process for the preparation of esters, wherein the starting materials are fed to the reactor by means of the inventive method for the continuous conveying of liquids.
  • Another object of the present invention is the use of a product resulting from hydrogenation of an aromatic compound as an auxiliary liquid for conveying an aromatic compound and the use of an alcohol or an ester of alcohol and carboxylic acid as an auxiliary liquid for conveying carboxylic acids or carboxylic acid derivatives.
  • a disadvantage of this type of pump is that to drive the gears an outwardly guided and sealed drive shaft must be used and it can thus come to contamination of the fluid with sealants and lubricants or leakage of the fluid to the outside.
  • this disadvantage is remedied, since the drive is effected by means of a hermetically sealed membrane and thus there can be neither contamination with sealants and lubricants nor leakage of the pumped medium to the outside.
  • diaphragm pumps can not be used to convey hot liquids or melts. For this purpose, then either metallic membranes with completely heatable pump heads or so-called "pendulum pumping systems" must be used.
  • Pendulum pumping systems are used, for example, in the DE-A-1453576 . DE-A-1528547 . EP-A1-048535 . DE-A1-3021851 . DE-T5-19782185 . DE-A-2553794 . WO-A-80/01706 . DE-A-4124 290 or EP-B1-36945 disclosed.
  • DE-A-1453576 describes a device for pumping a corrosive liquid, such as ammonium carbamate solution, by means of a pendulum pump unit, which is divided into two elements.
  • the first element (“main pump”) causes a non-corrosive auxiliary liquid, such as water, in a lifting movement and thus drives the second pump element with two non-return flaps for conveying the corrosive liquid via a connecting line ("transfer line").
  • the auxiliary liquid is constantly fed via a small auxiliary pump to the connecting line.
  • DE-A-1528547 describes a nearly identical pump concept with continuous metering of neutral auxiliary fluid to the suspension line.
  • EP-A1-048535 describes a pendulum pump system for conveying a hot coal slurry, wherein an oil mixable with the coal slurry is used as the auxiliary liquid.
  • auxiliary liquid is preferably not miscible with the liquid to be delivered and in which the pendulum line is arranged spatially very compact.
  • DE-T5-19782185 is a pendulum pump system for pumping hot media as well as solid / liquid mixtures ("slurries") with a similar pump as in DE-A-1453576 described, wherein the pendulum line is cooled in the horizontal part to prevent overheating of the main pump. On the addition of an auxiliary liquid is omitted here.
  • WO-A-80/01706 also describes a pendulum pump system for pumping hot liquids, wherein the connecting line consists of a horizontal and a vertical part and is also cooled. A similar system will be in DE-A-4124 290 described.
  • DE-A-2553794 discloses a pendulum pump system with vertically mounted shuttle, wherein a temperature gradient between the hot liquid and the main pump is maintained by cooling.
  • EP-B1-36945 describes a similar pumping device, in which case a movable piston between the conveying fluid and auxiliary fluid to prevent their mixing.
  • the maximum permissible temperature of the pumped medium is generally limited by the resistance of the membrane material, for example when using plastic membranes, such as PE or PTFE membranes.
  • plastic membranes such as PE or PTFE membranes.
  • the use of metal membranes would lead to very large and therefore expensive pump heads due to their very low flexibility.
  • the pump heads of diaphragm pumps, especially on the membrane drive and on the membrane itself, are not completely heatable, so that it can lead to solidification (crystallization) during the pumping of melts and thus to the mechanical destruction of the membrane.
  • a lubricating oil or similar fluid is usually required to lubricate the piston. This can mix with the liquid to be pumped and contaminate it.
  • the heating of piston pumps is generally not completely possible, so that deposits can also form here at unheated areas of the pump.
  • High-pressure diaphragm pumps with a transfer line to a spatially separate pump body with suction and delivery valve are in principle suitable for conveying hot melts.
  • the use of an auxiliary liquid for transmitting the pumping movement from the diaphragm pump to the melt to be conveyed is necessary for such a pump arrangement.
  • a part of the auxiliary liquid can mix with the melt to be conveyed. This leads to contamination of the liquid to be delivered with the auxiliary liquid.
  • a cooling of the pendulum line usually leads after a short time to parts of the melt diffuse through the pendulum line in the direction of the main pump, there solidify and lead to blocking of the pump.
  • the use of auxiliary piston in the pendulum line would lead to rapid blockage of the piston by solidifying melt.
  • the object was to reduce the formation of deposits and residues in the pump system in the transport of liquids that tend to form deposits.
  • Liquids that can form deposits and residues are, for example, liquids that solidify themselves or their ingredients when falling below a minimum temperature, crystallize or fail.
  • the object of the present invention was to develop a process for the promotion of organic melts and concentrated solutions of organic compounds, especially organic melts, which should be dispensed with costly designs for complete heating of all product wetted components, in particular the membrane of a diaphragm pump to keep investment and operating costs as low as possible.
  • the object underlying the invention has been achieved by a method for continuously conveying a liquid which is used as a starting material in a chemical reaction by means of positive displacement pump with spatially separated delivery valves and a liquid-filled transfer line between the positive displacement pump and delivery valves, characterized in that in the pendulum line a Auxiliary liquid is, which is a product or a reactant of the chemical reaction and has a melting point, which is below the melting point or below the saturation temperature of the liquid to be conveyed dissolved.
  • a pump system which valves a positive displacement pump (“main pump”) with spatially separated delivery and comprises a transfer line between positive displacement pump and delivery valves.
  • the delivery valves are generally housed in a housing.
  • the housing together with the delivery valves therein is referred to hereinafter as "valve body".
  • the valve body generally has an inlet on the suction side and an outlet on the pressure side in each case.
  • the inlet or the outlet are usually connected to a feed line on the suction side or a discharge on the pressure side, through which the liquid to be conveyed is conveyed.
  • the delivery valves are usually mounted at the inlet and outlet in the valve body so that the fluid to be delivered is passed through the valves.
  • the valves are generally designed so that the fluid to be pumped can pass the valves only from the suction side in the direction of the pressure side. The flow in the opposite direction (from the pressure side to the suction side) is generally blocked.
  • the valves can be designed as check valves, preferably ball check valves. Between the valves is usually located in Ventilgroper a cavity through which the liquid to be conveyed flows. This space is usually designed as a pipe with preferably cylindrical geometry, wherein the geometry may also differ from the cylindrical geometry and, for example, may be configured spherical.
  • valve body is arranged vertically or vertically, i. the axis, which can be placed through the delivery valves and the space between the delivery valves, is vertical.
  • the delivery valves are spatially separated from the positive displacement pump by a transfer line.
  • the pendulum line preferably has an "L" -shaped geometry, ie the pendulum line has in this geometry an area which extends horizontally and a part which extends vertically. Deviations from this geometry are possible, for example, to allow a connection between positive displacement pump and valve body, if the arrangement of positive displacement pump and valve body due to structural conditions does not allow a strictly 'L''- shaped geometry. If the valve body is arranged vertically, then usually the horizontal part of the shuttle leads into the valve housing into the cavity between the two delivery valves.
  • the adjoining the horizontal part of the pendulum line vertical region of the pendulum line is usually connected directly or via another area of the pendulum line, which does not necessarily have to be arranged vertically, with the pump chamber of the positive displacement pump. If the valve body is arranged horizontally, usually the vertical part of the shuttle leads into the cavity of the valve body between the two delivery valves.
  • the adjoining the vertical part of the pendulum line horizontal region of the pendulum line is usually connected directly or via another area of the pendulum line, which does not necessarily have to be arranged horizontally, with the pump chamber of the positive displacement pump.
  • the part of the pendulum line, which is connected to the valve body, and the valve body itself are heated to a temperature above the melting temperature or above the saturation temperature of the liquid to be delivered.
  • the heating of the heated part of the pendulum line and the valve housing can usually be done with steam or heat transfer oil.
  • the heated part of the pendulum line is preferably so large that, together with the cavity in the valve body between the two delivery valves at least one volume is included, which is about 3 to 20 times, preferably 5 to 15 times and more preferably 7 to 12 times the displacement of the positive displacement pump corresponds. Thus, it is generally ensured that the fluid to be delivered comes into contact only with the heated part of the shuttle.
  • the shuttle line is connected to the pressure side of a positive displacement pump ("main pump").
  • the positive displacement pump (“main pump”) is a piston pump or a diaphragm pump, with a diaphragm pump being particularly preferred since it has no Sealing and lubricants needed that could contaminate the liquid to be pumped.
  • Suitable membrane materials are elastomeric materials such as ethylene-propylene-diene rubber (EPDM), silicone rubber (MVO, VMO), fluoro-silicone rubber (MFO, FVMO), fluoro rubber (FPM, FKM), perfluoro rubber (FFKM, FFPM), polychloroprene rubber (CR), nitrile butadiene rubber (NBR), polyester urethane rubber (AU, EU), butyl rubber (IIR) and natural rubber (NR).
  • EPDM ethylene-propylene-diene rubber
  • MVO silicone rubber
  • MFO fluoro-silicone rubber
  • FPM fluoro rubber
  • FFKM perfluoro rubber
  • CR polychloroprene rubber
  • NBR n
  • polymer membranes made of polytetrafluoroethylene (PTFE), polyethylene (PE) and polypropylene (PP) or other plastic membranes which are chemically resistant to the auxiliary liquid used.
  • coated membranes such as PTFE-coated elastomeric membranes or multi-layer membranes made of different materials.
  • Preferred membrane materials are polytetrafluoroethylene (PTFE) and polyethylene (PE), wherein the use of PTFE and PTFE-coated elastomer membranes as membrane material for promoting aromatic compounds and carboxylic acids or carboxylic acid derivatives are particularly preferred.
  • the main pump is connected on the suction side with a pipe ("connecting line") through which auxiliary liquid can be supplied.
  • the supply of the auxiliary liquid through the connecting line is preferably carried out by a further positive displacement pump ("auxiliary pump").
  • the auxiliary pump is a positive displacement pump, which is preferably designed as a piston or diaphragm pump, particularly preferably as a diaphragm pump.
  • Suitable membrane materials are the aforementioned materials, such as PTFE and PTFE-coated membranes, which are resistant to the respective auxiliary liquid.
  • a check valve is preferably attached, which prevents liquid from the main pump can flow in the direction of the auxiliary pump.
  • a valve for venting the pump chamber of the main pump is usually mounted at the highest point of the pump system to allow complete venting.
  • delivery valves are attached to the suction and delivery side directly on the pump head of the auxiliary pump. The delivery valves are generally designed so that the fluid to be delivered can pass the valves only from the suction side in the direction of the pressure side. The flow in the opposite direction (from the pressure side to the suction side) is generally blocked.
  • the valves can be designed as check valves, preferably ball check valves.
  • auxiliary pump At the highest point between the delivery valve on the pressure side and the check valve in the connecting line usually another valve is attached, which serves to vent this part of the pipeline.
  • the suction side of the auxiliary pump is connected to a reservoir, for example a container or a tank in which the auxiliary liquid is located.
  • the auxiliary liquid can be heated prior to introduction into the pump space of the auxiliary pump, for example by a heat exchanger or by heating the receiver tank, wherein the temperature should not be so high that neither the main nor the auxiliary pump, in particular the membrane material of a diaphragm pump, is damaged.
  • the pendulum line is usually filled with liquid.
  • the pendulum line and the space within the valve body, which is located between the delivery valves, before the start of the process according to the invention for the delivery of liquids - ie before the start of the pumping operation - completely or almost completely filled with auxiliary fluid are advantageous if at least the non-heated part of the pendulum line is filled with auxiliary liquid, since the auxiliary liquid has a lower melting point than the liquid to be conveyed and does not or does not need to be heated so much to remain liquid. Thus, the formation of deposits of solids in the pump system can be further reduced.
  • the auxiliary liquid in the main pump and the valve body is initially pumped out by a lifting movement of the main pump (delivery) from the pump system.
  • the delivery valve in the valve body on the suction side prevents backflow in the direction of the reservoir tank of the liquid to be conveyed and the check valve in the connecting line prevents auxiliary fluid pumped out of the main pump from flowing back to the auxiliary pump.
  • the liquid to be conveyed is conveyed through the supply line on the suction side into the valve body and partly into the transfer line.
  • the liquid to be conveyed usually does not reach the entire part of the transfer line, since the auxiliary liquid usually forms approximately a liquid barrier, which hinders the propagation of the liquid to be conveyed in the pendulum line.
  • the displacement pump in particular also the diaphragm of a diaphragm pump, does not come into contact with the fluid to be delivered, but is generally surrounded by the auxiliary fluid.
  • the auxiliary liquid does not form an ideal liquid barrier, so that part of the liquid to be conveyed mixes with the auxiliary liquid and diffuses in the direction of the main pump, for example when a high temperature gradient occurs between the heated valve body and the pump head of the main pump. Due to the diffusion of the liquid to be conveyed, deposits may occur in the region of the main pump and the unheated part of the transfer line.
  • auxiliary liquid is introduced into the commutation line.
  • the introduction of the auxiliary liquid causes a flow towards the valve body of the main pump, which generally counteracts the propagation of the liquid to be conveyed by convection or diffusion.
  • the introduction is preferably carried out continuously.
  • the auxiliary liquid is introduced by means of a positive displacement pump ("auxiliary pump") through the connecting line into the pump chamber of the main pump.
  • a check valve in the connection line generally causes the liquid to flow only in the direction of the main pump.
  • the volume flow of the auxiliary liquid to the volume flow of the liquid to be conveyed is preferably in the range of 1: 100 to 1:10, more preferably in the range of 1:80 to 2:10, particularly preferably 1:50 to 5:10.
  • the lift linkage of the main pump and the auxiliary pump are mechanically coupled together.
  • the mechanical coupling is designed so that the auxiliary pump is exactly in the delivery stroke when the main pump is in the suction stroke and vice versa.
  • the temperature can be set lower in this area, since it is only necessary that the temperature in the pump head and in the non-heated part of the shuttle is so high that the auxiliary liquid remains in a liquid state and the formation of deposits is largely avoided.
  • the pump head of the main pump and the unheated part of the transfer line is not additionally heated and uses an auxiliary liquid having a melting point below the ambient temperature. This embodiment allows a particularly economical embodiment of the pump system.
  • the auxiliary liquid may be heated before being introduced into the pump space of the auxiliary pump as described above.
  • the geometric arrangement of the pump system is generally carried out depending on the substances to be conveyed.
  • the valve body When the density of the liquid to be delivered is higher than the density of the auxiliary liquid, in each case at the operating temperatures, the valve body is usually arranged lower than the main pump. Accordingly, the valve body is usually arranged above the main pump when the liquid to be conveyed has a lower density than the auxiliary liquid.
  • liquids which are used as starting materials in a chemical reaction can be conveyed.
  • feedstocks for reactions such as hydrogenations, oxidation, esterifications and polymerizations can be promoted in a chemical reactor.
  • the starting material can be used as a melt or as a concentrated solution of the starting material.
  • the liquid to be conveyed is particularly preferably used as a melt, particularly preferably as a melt of the commercially available pure substance.
  • the use of a melt generally has the advantage that the compound to be conveyed does not have to be dissolved in a separate process step in order to obtain a recoverable liquid.
  • the feedstock is also not diluted by a solvent, so that the reactor can usually be charged with a higher amount of starting material and a complicated separation of the solvent after completion of the reaction is generally not required.
  • the starting material can also be used as a solution of the starting material.
  • the solvent used for the starting material is generally the solvent, which is preferably used in the corresponding process or in the respective reaction.
  • This embodiment is advantageous, for example, if the starting materials tend to discolour or to give secondary reactions during melting.
  • the temperature for transferring the feedstock to the liquid state can be lowered.
  • a solution which is as concentrated as possible is generally prepared.
  • the inventive method is also suitable for the promotion of non-meltable starting materials, such as terephthalic acid, for example, to promote a slurries of the starting material terephthalic acid in ethylene glycol.
  • melts having a melting point of 20 ° C. or more can be conveyed by means of the process according to the invention.
  • solutions of a starting material may preferably be promoted, wherein the saturation temperature of the solution at a temperature of 20 ° C or more, preferably 50 ° C or more, more preferably at 75 ° C or more, and most preferably 100 ° C or more .
  • the saturation temperature is understood to be the temperature at which a solution of a starting material, with a certain concentration, reaches the saturation state and the starting material begins to precipitate out of the solution.
  • the temperature at which the liquid to be conveyed is conveyed is above its melting temperature or above its saturation temperature.
  • the conveying temperature is 1 ° C to 100 ° C, preferably 5 ° C to 80 ° C and more preferably 10 ° to 50 ° C above the melting temperature or the saturation temperature of the liquid to be conveyed.
  • the temperature of the liquid to be conveyed should not exceed 300.degree. C., preferably not more than 250.degree. C., and more preferably not more than 200.degree. Since the temperature of the auxiliary liquid in the region of the pump head is usually limited by the temperature resistance of the membrane, as described below, a high temperature gradient between valve body and pump chamber can lead to increased mixing between the liquid to be conveyed and the auxiliary liquid. As a rule, the ratio of the volume flow of the auxiliary liquid to the volume flow of the fluid to be conveyed should be higher, the higher the temperature gradient between the valve body and the pump chamber.
  • the auxiliary liquid according to the invention is a product of the chemical reaction or an educt of the chemical reaction. If a product of the chemical reaction is used as the auxiliary liquid, preferably the main product is used as the auxiliary liquid which preferably forms under the conditions of the respective chemical reaction. The fact that either an educt or a product of the chemical reaction is used as the auxiliary liquid, it is prevented that the liquid to be conveyed is contaminated by foreign matter.
  • the melting point of the auxiliary liquid according to the invention is below the melting temperature or below the saturation temperature of the liquid to be conveyed.
  • the melting point of the auxiliary liquid is below the temperature at which the membrane of a membrane pump is stable, so that the membrane is not thermally damaged.
  • the melting temperature of the auxiliary liquid is 150 ° C or less, more preferably 100 ° C or less, even more preferably 50 ° C or less, and most preferably 25 ° C or less. At these temperatures, safe operation of diaphragm pumps is usually possible.
  • the temperature at which the auxiliary liquid is introduced into the connecting line is above its melting temperature.
  • the temperature at which the auxiliary liquid is introduced into the connecting line 1 ° C to 100 ° C, preferably 5 ° C to 80 ° C and more preferably 10 ° to 50 ° C above the melting temperature of the auxiliary liquid.
  • the temperature at which the auxiliary liquid is introduced into the connecting line is in the range of 0 ° C to 150 ° C, preferably in the range of 10 ° C to 100 ° C, more preferably in the range of 20 ° C to 80 ° C. particularly preferably in the range from 20 ° C to 50 ° C.
  • the boiling point of the auxiliary liquid should preferably be above the conveying temperature of the liquid to be conveyed, since otherwise undesired gas formation may occur at the interface of the auxiliary liquid and the liquid to be conveyed in the region of the commutation line.
  • the particularly preferred embodiment in which a product of the chemical reaction is used as auxiliary liquid, is also suitable for the promotion of carboxylic acids or carboxylic acid derivatives in the preparation of esters or polyesters.
  • the corresponding carboxylic acid derivatives of carboxylic acids can also be used as starting materials.
  • the corresponding carboxylic acid anhydrides of the abovementioned carboxylic acids in particular phthalic anhydride, maleic anhydride or succinic anhydride, are used.
  • an ester of carboxylic acid and alcohol is used as an auxiliary liquid for promoting the carboxylic acid or the carboxylic acid derivative.
  • methyl benzoate can be used as an auxiliary liquid for the promotion of benzoic acid in the preparation of benzoic acid methyl ester from benzoic acid and methanol.
  • the auxiliary liquid in the process according to the invention for conveying a liquid is an educt of the chemical reaction.
  • the corresponding carboxylic acid derivatives of carboxylic acids can also be used as starting materials.
  • the corresponding carboxylic acid anhydrides of the abovementioned carboxylic acids in particular phthalic anhydride, maleic anhydride or succinic anhydride, are used.
  • an educt of the chemical reaction is used as the auxiliary liquid.
  • the auxiliary liquid according to the invention is an alcohol with which the carboxylic acid or the carboxylic acid derivative is to be reacted.
  • the process according to the invention will preferably be used to promote aromatic compounds used in a hydrogenation.
  • the present invention relates to a process for the hydrogenation of aromatic compounds, characterized in that an aromatic compound or a solution of an aromatic compound by means of a positive displacement pump with spatially separated delivery valves and a liquid-filled transfer line between the positive displacement pump and delivery valves to the reactor, wherein in the Pendulum is an auxiliary liquid which is the product of the hydrogenation of the aromatic compound and wherein the auxiliary liquid has a melting point which is below the melting point of the aromatic compound or below the saturation temperature of the solution of the aromatic compound.
  • the hydrogenation is usually carried out at suitable pressures and temperatures.
  • the temperature is generally in the range of 50 and 300 ° C, the temperature range of 120 to 280 ° C is preferred, and the pressure is usually from 1 to 500 bar, preferably from 50 to 325 bar, particularly preferably from 150 to 250 bar.
  • the hydrogenation process can be carried out continuously or in the manner of a batch process. With continuous process control, the amount of compound or compounds for hydrogenation is preferably about 0.01 to about 3 kg per liter of catalyst per hour, more preferably about 0.05 to about 1 kg per liter of catalyst per hour.
  • the hydrogenation gases any gases containing hydrogen and having no harmful amounts of catalyst poisons such as CO may be used.
  • reformer exhaust gases can be used.
  • pure hydrogen is used as the hydrogenation gas.
  • the hydrogenation is usually carried out in the presence of a homogeneous or heterogeneous catalyst which is suitable for hydrogenations.
  • a homogeneous catalyst which is suitable for hydrogenations.
  • the hydrogenation is carried out in the presence of a heterogeneous catalyst.
  • Suitable homogeneous catalysts are liquid and / or soluble hydrogenation catalysts, for example Wilkinson catalysts, Crabtree catalysts or Lindlar catalysts.
  • heterogeneous catalysts for example, noble metals such as platinum, palladium, ruthenium, osmium, iridium and rhodium or other transition metals such Molybdenum, tungsten, chromium, but especially iron, cobalt and nickel, either singly or in admixture.
  • the catalyst metals can be used directly in the form of the metal or an inorganic metal compound or the catalyst metals are applied to an inert, inorganic support material such as alumina, SiO 2 , TiO 2 and activated carbon.
  • the hydrogenation can be carried out without solvent or in the presence of a solvent.
  • a solvent alcohols such as methanol, ethanol, propanol, isopropanol, isobutanol or t-butanol, or ethers such as diethyl ether, glycol dimethyl ether, dioxane or tetrahydrofuran can be used.
  • a solvent it is also possible to use the end product formed during the reaction. Suitable solvents are also mixtures of the abovementioned solvents.
  • the following aromatic compounds are preferably used in the process of the invention for the hydrogenation of aromatic compounds.
  • the process according to the invention is, as explained above, also preferably suitable for the extraction of carboxylic acids or carboxylic acid derivatives which are used in a process for the preparation of esters or polyesters, for example by esterification or transesterification.
  • the present invention relates to a process for the preparation of esters, characterized in that supplying a carboxylic acid or a carboxylic acid derivative or a solution of a carboxylic acid or a carboxylic acid derivative by means of a positive displacement pump with spatially separated delivery valves and a liquid-filled transfer line between the positive displacement pump and delivery valves to the reactor the auxiliary line is an auxiliary liquid which is the product of ester production or an alcohol used as starting material and wherein the auxiliary liquid has a melting point below the melting point of the carboxylic acid or of the carboxylic acid derivative or below the saturation temperature of the solution of the carboxylic acid or Carboxylic acid derivative is located.
  • esters such as in Ullmann's Encyclopedia of Industrial Chemistry, Polyesters (Electronic Release DOI : 10.1002 / 14356007.a21_227), the abovementioned carboxylic acids or carboxylic acid derivatives and the abovementioned alcohols catalyst-free or preferably in the presence of esterification catalysts, advantageously in an atmosphere of inert gases, such as. B. nitrogen, carbon monoxide, helium, argon and others in the melt at temperatures of 150 to 250 ° C, preferably 180 to 220 ° C optionally under reduced pressure to the desired acid number, which is advantageously less than 10, preferably less than 2, be condensed.
  • inert gases such as. B. nitrogen, carbon monoxide, helium, argon and others in the melt at temperatures of 150 to 250 ° C, preferably 180 to 220 ° C optionally under reduced pressure to the desired acid number, which is advantageously less than 10, preferably less than 2, be condensed.
  • the organic polycarboxylic acids and / or derivatives and polyhydric alcohols are advantageously used in a molar ratio of 1: 1 to 1.8, preferably 1: 1.05 to 1.2.
  • catalysts it is possible to use basic or acidic catalysts, preferably acidic catalysts, such as toluenesulfonic acids, preferably organometallic compounds, in particular those based on titanium or tin, such as titanium tetrabutoxide or tin (II) octoate.
  • the auxiliary liquid used according to the invention is the product of ester production or an alcohol which is used as starting material in the preparation of the ester.
  • the process according to the invention is particularly suitable for promoting compounds which have a high melting point or which are in the form of concentrated solutions and have a high saturation temperature.
  • Such substances can - due to the high melting point or its high saturation temperature - form deposits at insufficiently heated points of the feed pump.
  • the heating of feed pumps proves to be technically complex, since on the one hand not all conventional materials that are used for the construction of pumps are thermally stable, in particular membranes and seals.
  • the production of high temperature pumps is relatively expensive, despite sacrificing performance compared to conventional pumps that can be operated at ambient temperature.
  • high-melting compounds or highly concentrated solutions can be conveyed with conventional pumps, the tendency for the formation of deposits in the area of the pump system being reduced.
  • reaction mixture is not contaminated by non-reactive substances that would otherwise have to be separated from the desired product in complex steps.
  • Feedstock (liquid to be pumped) Melting point ° C Reaction product "auxiliary liquid” Melting point ° C 2,4-toluenediamine (TDA) 97 2,4-diamino-1-methyl-cyclohexane ⁇ 0 2,6-toluenediamine (TDA) 104 2,6-diamino-1-methyl-cyclohexane ⁇ 0
  • Example 2 Hydrogenation of optionally substituted MDA to cycloaliphatic amines
  • Feedstock (liquid to be pumped) Melting point ° C Reaction product "auxiliary liquid” Melting point ° C m-Phthalodintril 163 1,3-bis (aminomethyl) cyclohexane ⁇ 0 o-Phthalodintril 140 1,2-bis (aminomethyl) cyclohexane ⁇ 0 p-Phthalodintril 224 1,4-bis (aminomethyl) cyclohexane ⁇ 0
  • Example 5 Hydrogenation of acid anhydrides and aromatic acids to the corresponding cycloaliphatic compounds
  • Feedstock (liquid to be pumped) Melting point ° C Reaction product "auxiliary liquid” Melting point ° C phthalic anhydride 131 Cyclohexane-1,2-dicarboxylic anhydride 32 benzoic acid 121 cyclohexanecarboxylic 28
  • Example 6 Esterification of benzoic acid with various alcohols to the corresponding esters of benzoic acid
  • Feedstock (liquid to be pumped) Melting point ° C Reaction product "auxiliary liquid” Melting point ° C benzoic acid 121 benzoate -12 121 benzoate -34 121 butyl benzoate -20
  • Example 7 Esterification of dicarboxylic acids with various alcohols to the corresponding esters of adipic acid
  • Feedstock * Melting point ° C "Auxiliary liquid” diol Melting point ° C
  • a feedstock for example, a melt of the feedstock, a concentrated solution of the feedstock or suspended finely divided solids of the feedstock ("slurry driving style") can be used with one of the auxiliary liquids mentioned in the right column or a process solvent.

Landscapes

  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Reciprocating Pumps (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Furan Compounds (AREA)

Claims (12)

  1. Procédé de transport continu d'un liquide (1) au moyen d'une pompe volumétrique (12) comprenant des vannes de transport séparés dans l'espace (10) et (11) et une conduite pendulaire remplie de liquide (7) entre la pompe volumétrique (12) et les vannes de transport, un liquide auxiliaire (3) se trouvant dans la conduite pendulaire (7), dont le point de fusion est inférieur au point de fusion ou inférieur à la température de saturation du liquide à transporter (1), caractérisé en ce que le liquide à transporter (1) est utilisé en tant que matière première dans une réaction chimique et le liquide auxiliaire (3) est un produit ou un réactif de la réaction chimique.
  2. Procédé selon la revendication 1, caractérisé en ce que le liquide est un composé organique.
  3. Procédé selon la revendication 2, caractérisé en ce que le composé organique est un composé aromatique, la réaction chimique est une hydrogénation et le produit de l'hydrogénation du composé aromatique est utilisé en tant que liquide auxiliaire.
  4. Procédé selon la revendication 3, caractérisé en ce que le composé aromatique est une amine aromatique.
  5. Procédé selon la revendication 2, caractérisé en ce que le composé organique est un acide carboxylique ou un dérivé d'acide carboxylique, la réaction chimique est un procédé de fabrication d'esters et l'ester formé lors de la réaction ou l'alcool utilisé en tant que réactif est utilisé en tant que liquide auxiliaire.
  6. Procédé selon au moins l'une quelconque des revendications 1 à 5, caractérisé en ce que le liquide présente un point de fusion ou une température de saturation de 50 à 300 °C.
  7. Procédé selon au moins l'une quelconque des revendications 1 à 6, caractérisé en ce que le point de fusion du liquide auxiliaire est de 50 °C et moins.
  8. Procédé selon au moins l'une quelconque des revendications 1 à 7, caractérisé en ce que la pompe volumétrique est une pompe à membrane.
  9. Procédé selon au moins l'une quelconque des revendications 1 à 8, caractérisé en ce que le liquide auxiliaire est introduit en continu dans la conduite pendulaire.
  10. Procédé selon au moins l'une quelconque des revendications 1 à 9, caractérisé en ce que le débit volumétrique du liquide auxiliaire par rapport au débit volumétrique du liquide à transporter se situe dans la plage allant de 1:10 à 1:100.
  11. Procédé selon au moins l'une quelconque des revendications 1 à 10, caractérisé en ce que l'introduction du liquide auxiliaire a lieu avec une pompe à membrane.
  12. Procédé selon au moins l'une quelconque des revendications 1 à 11, caractérisé en ce que les mécanismes d'entraînement de la pompe pour le transport du liquide auxiliaire et de la pompe volumétrique sont couplés mécaniquement ou électroniquement l'un avec l'autre.
EP20100728254 2009-07-09 2010-07-06 Procédé de transport de liquides Not-in-force EP2452071B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP20100728254 EP2452071B1 (fr) 2009-07-09 2010-07-06 Procédé de transport de liquides

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP09165074 2009-07-09
EP20100728254 EP2452071B1 (fr) 2009-07-09 2010-07-06 Procédé de transport de liquides
PCT/EP2010/059627 WO2011003899A1 (fr) 2009-07-09 2010-07-06 Procédé de transport de liquides

Publications (2)

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EP2452071A1 EP2452071A1 (fr) 2012-05-16
EP2452071B1 true EP2452071B1 (fr) 2014-01-08

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Country Status (5)

Country Link
US (1) US8940250B2 (fr)
EP (1) EP2452071B1 (fr)
JP (1) JP2012533011A (fr)
CN (1) CN102549262B (fr)
WO (1) WO2011003899A1 (fr)

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WO2011003899A1 (fr) 2009-07-09 2011-01-13 Basf Se Procédé de transport de liquides
WO2014095898A1 (fr) * 2012-12-21 2014-06-26 Tetra Laval Holdings & Finance S.A. Agencement de pompe à piston pour des applications de traitement hygiénique
WO2014095896A1 (fr) * 2012-12-21 2014-06-26 Tetra Laval Holdings & Finance S.A. Système de pompe à piston destiné à des applications de traitements hygiéniques
HUE035346T2 (en) 2013-12-11 2018-05-02 Basf Se Process for hydrogenation of 4,4'-methylene dianiline
EP2883864A1 (fr) 2013-12-11 2015-06-17 Basf Se Procédé d'hydrogénisation de composés aromatiques
DE102013114320A1 (de) * 2013-12-18 2015-06-18 Mhwirth Gmbh Heißschlammpumpe
EP3844165A1 (fr) 2018-08-29 2021-07-07 Nederlandse Organisatie Voor Toegepast- Natuurwetenschappelijk Onderzoek Tno Réaction de diels-alder avec des composés furaniques pour obtenir des composés aromatiques
EP3663297A1 (fr) * 2018-12-06 2020-06-10 Nederlandse Organisatie voor toegepast- natuurwetenschappelijk onderzoek TNO Réaction de diels-alder avec des furaniques pour obtenir des composés aromatiques
CN111219885A (zh) * 2020-01-19 2020-06-02 侯中泽 一种流体活塞热源泵

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Also Published As

Publication number Publication date
US20120116099A1 (en) 2012-05-10
JP2012533011A (ja) 2012-12-20
EP2452071A1 (fr) 2012-05-16
US8940250B2 (en) 2015-01-27
CN102549262B (zh) 2014-12-24
CN102549262A (zh) 2012-07-04
WO2011003899A1 (fr) 2011-01-13

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