EP1066109A1 - Dispositif, procede et reacteur pressurise permettant de traiter des matieres solides avec un gaz liquide sous pression - Google Patents

Dispositif, procede et reacteur pressurise permettant de traiter des matieres solides avec un gaz liquide sous pression

Info

Publication number
EP1066109A1
EP1066109A1 EP99911760A EP99911760A EP1066109A1 EP 1066109 A1 EP1066109 A1 EP 1066109A1 EP 99911760 A EP99911760 A EP 99911760A EP 99911760 A EP99911760 A EP 99911760A EP 1066109 A1 EP1066109 A1 EP 1066109A1
Authority
EP
European Patent Office
Prior art keywords
solid
pressure
reactor
pressure reactor
chamber
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Withdrawn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
EP99911760A
Other languages
German (de)
English (en)
Inventor
Ties Karstens
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.)
Cerdia Produktions GmbH
Original Assignee
Rhodia Acetow GmbH
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 Rhodia Acetow GmbH filed Critical Rhodia Acetow GmbH
Publication of EP1066109A1 publication Critical patent/EP1066109A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • B01J19/20—Stationary reactors having moving elements inside in the form of helices, e.g. screw reactors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/008—Processes carried out under supercritical conditions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/02—Feed or outlet devices therefor
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B1/00—Preparatory treatment of cellulose for making derivatives thereof, e.g. pre-treatment, pre-soaking, activation
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C3/00—Pulping cellulose-containing materials
    • D21C3/02—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes
    • D21C3/024—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes with NH3 or H2O
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C7/00—Digesters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/18—Details relating to the spatial orientation of the reactor
    • B01J2219/185—Details relating to the spatial orientation of the reactor vertical
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/19—Details relating to the geometry of the reactor
    • B01J2219/194—Details relating to the geometry of the reactor round
    • B01J2219/1941—Details relating to the geometry of the reactor round circular or disk-shaped
    • B01J2219/1943—Details relating to the geometry of the reactor round circular or disk-shaped cylindrical

Definitions

  • the invention relates to a method, a device and a pressure reactor for treating solids with liquefied gases, in particular with liquefied ammonia, under pressure.
  • a generic method emerges, for example, from WO 96/3 04 11.
  • polysaccharides are brought into contact with liquid ammonia under pressure.
  • the volume available to the polysaccharide / liquid ammonia system is explosively increased by lowering the pressure by at least 5 bar. In this way, an increased accessibility and reactivity of the treated polysaccharides can be achieved.
  • a method for introducing fibrous lignose cellulose raw material into a pressurized container is known.
  • the raw material is pre-compressed to a density of at least 0.72 gram / cm3 before entering the pressure vessel and then introduced into the vessel by a screw conveyor.
  • the pre-compressed raw material thus acts as a plug which seals the inlet opening of the pressure vessel so that the pressure in the vessel can be maintained. This makes it possible to continuously supply cellulose to the container.
  • the known method requires a dwell time (approx. 4 minutes) of the cellulose in the pressure vessel, which is unnecessarily long, in particular for the treatment with liquid ammonia under pressure, especially under high pressure, since it is known that liquid ammonia within one Diffuses from a few seconds to a minute into solids and is evenly distributed.
  • a reliable and adequate sealing of the device is also problematic when operating with liquid ammonia under pressures of up to 40 bar, in particular at the location of the drive shaft for the pressure vessel and for the screw conveyor in the outlet part under the pressure vessel. Sealing the
  • the smallest possible size of the device for carrying out the known method is at a throughput of about 400 tons per year, which is much too large for certain areas of application.
  • a method is known from US Pat. No. 5,171,592 in which the biomass to be treated is pressed against a large valve by means of a solids pump in order to compress the material and to press out the air contained therein before the valve is opened in order to open the biomass bring in the reactor.
  • the reactor is equipped with finger-like teeth on the inside of the reactor and on a rotating tool. Show your teeth -3-
  • the reactor outlet is provided with a valve, through which the biomass treated with ammonia can escape explosively into a collecting container.
  • the device for carrying out the method is therefore relatively complex and is not suitable for processes which are carried out under high pressure, since rotating machine parts are in the area of the high pressure, which causes the known device to be more susceptible to wear and malfunction.
  • the object of the present invention to provide a method with which the disadvantages of the prior art described are avoided, while at the same time the treated solid is to be obtained almost continuously.
  • the invention is also based on the object of providing a device or an associated pressure reactor which is suitable for carrying out the method and is distinguished by high availability and low maintenance expenditure.
  • the solid to be treated is introduced into a pressure reactor at ambient pressure, then the liquid gas is fed under pressure to the pressure reactor and the resulting mixture of liquid gas / solid is explosively expanded into an expansion tank after a predetermined dwell time, at least two Reactors are operated temporally killed.
  • the solid to be treated can be at the beginning of the process according to the invention, in particular after a previous preparation in the sense of a fragmentation or comminution, up to a desired bulk density or up to a certain one
  • the method according to the invention can be used for the treatment of cellulose, starch, gelatin, guar or wood chips and very generally of substances containing polysaccharides, but also for the treatment of minerals such as silicates and zeolites and of thermoplastic polymers. Because of its particularly good diffusion properties, ammonia has proven itself extremely well for use as a liquefied petroleum gas.
  • a quasi-continuous treatment of the solid can be achieved by the timed operation of at least two pressure reactors, so that starting material is provided for further processing almost without interruption.
  • the gas released in the explosion-like expansion is preferably recovered.
  • the recovered gas can then be returned to the process in liquid form. This enables a particularly economical procedure, since overall only a small part of the gas used, for example -5-
  • the solid can be introduced into the pressure reactor using dosing screws.
  • the method according to the invention can be carried out particularly reliably by using this known, technically sophisticated conveying means.
  • the solid can also be introduced into the pressure reactor by means of a pneumatically operating conveying device.
  • a pneumatically operating conveying device With this measure, a particularly rapid and targeted supply of the solid to be treated can be achieved.
  • the solid to be treated is preferably actively mixed with the liquefied gas in the pressure reactor. This has the advantage that the liquefied gas penetrates deeper into the solid and is distributed more homogeneously in it. In addition, this additional measure allows the residence time of the liquid gas / solid mixture in the pressure reactor.
  • the opening and closing of the reactors and / or the supply of the solid and / or the liquefied gas is controlled automatically.
  • a solid or liquid additive dissolved or dispersed therein can be introduced into the reactor together with the liquefied gas under pressure.
  • the solid can be simultaneously with the Treatment with the liquefied gas continues to add substances, for example to further increase its activation.
  • ammonia is suitably used as the liquid gas, since numerous additives can be easily dissolved in it.
  • the liquefied gas is preferably mixed with the solid or liquid additive before entering the reactor. This enables a homogeneous solution or dispersion to be prepared from the additive and the liquefied gas.
  • the device according to the invention for the treatment of solids with liquefied gases under pressure has at least two pressure reactors arranged in parallel for alternating absorption of a solid and a liquefied gas, the inlet or outlet openings for the solid each provided with shut-off elements and at least one inlet opening for the liquefied gas have, at least one expansion tank, which is connected to the respective pressure reactors, and conveying means for supplying the solid and the liquefied gas.
  • the device according to the invention enables quasi-continuous operation in the treatment of a solid with liquid gas under pressure.
  • the interior of the reactor can be sealed off from the environment in a simple manner by the shut-off elements, so that no complex construction or process engineering is required
  • Precautions are required to maintain pressure while performing the procedure.
  • shut-off devices of the pressure reactors are preferably designed as ball valves. These have the advantage of being technically mature and tried and tested. You can have many
  • the pressure reactors are designed as vertical tubular cylinders.
  • the filling with crushed and free-flowing solids is facilitated, since gravity supports the introduction of the solid here.
  • These tubular cylinders are particularly easy to manufacture and their number can be selected depending on the optimal residence time for the solids to be treated.
  • the cycle frequency, and thus the number of tube cylinders to be used, is based on the filling time of each tube cylinder. With an intended filling time of about one minute, e.g. with eight cylinders, each with a capacity of 8 kg, a throughput of 2.4
  • Tons / hour can be reached.
  • the inlet of the reactor can be widened in a funnel shape.
  • means can be used to automatically control the process sequences, in particular the introduction of the solid and / or the liquefied
  • Gas and / or the clocked actuation of the shut-off elements of the pressure reactor can be provided.
  • the pressure reactors are equipped with an external heater. This can be used in conjunction with a suitable
  • the reactors preferably each have a plurality of openings for the supply of the liquid gas.
  • the liquid gas can be distributed particularly finely over the entire interior of the reactor and thus over the solid surface.
  • the reactors can also be designed as mixers. In this case, however, technically complex measures must be taken to ensure that the reactors are sealed securely.
  • shut-off element at the inlet of each pressure reactor can be designed as a lock system.
  • the tightness of the reactor can be additionally increased or secured.
  • the device according to the invention preferably has a compressor device which compresses the solid, in particular cellulose, in the pressure reactor.
  • a compressor device which compresses the solid, in particular cellulose, in the pressure reactor.
  • the degree of filling is advantageously maintained within relatively narrow limits. A complex and expensive gravimetric dosing system can therefore be dispensed with.
  • the compressor device preferably has a compressor piston which can be moved in a cylindrical reactor chamber (34, 50; 81) or metering chamber and which compresses the solid.
  • the piston is used to compress the amount of solids in a manner that is gentle on the material.
  • the compressor piston preferably has one or more channels which extend fluid-continuously from an underside to an upper side of the compressor piston.
  • Perforation of the piston can escape disruptive propellant gas from the reactor chamber during compression and an exactly reproducible degree of filling of the solid is achieved.
  • the compression piston preferably moves the compressed amount of solids from a compression chamber into a reaction chamber of the pressure reactor. This saves extra funds for feeding the reaction chamber.
  • the compressor piston can preferably be locked or at least stopped in one position of its possible piston stroke, which saves additional shut-off means for separating the compression and the reaction process.
  • different fill levels and fill volumes of the solid can be realized in the reactor chamber.
  • a processing device for the solid is preferably provided, which processes the solid before it is fed to the pressure reactor or the pressure reactors, thereby reducing the reaction time in the pressure reactor.
  • a heating device that heats the solid is preferably used as the processing device.
  • a heat transfer fluid is preferably supplied to the solid, which heats the heating device, thereby ensuring homogeneous heating of the solid during processing.
  • Liquid or gaseous ammonia is preferably used as the heat transfer fluid, whereby the absorption of liquid ammonia in the pressure reactor is further improved and even shorter reaction times are achieved.
  • the heating device preferably heats the ammonia to a temperature of approximately 100 ° C., as a result of which favorable conditions for the ammonia uptake are generated in the pressure reactor.
  • the heat transfer fluid circulates in a heating circuit, whereby energy and
  • the solid is preferably heated in a screw conveyor, whereby an exact time of action of the heat transfer fluid on the solid and thus a constant and precise heating of the solid can be achieved.
  • the process according to the invention preferably comprises the following pressure reactor phases, a pressure reactor being charged with solid during a filling phase, the solid being subsequently compressed in a pressure phase during a compression phase, liquefied gas then being fed to the compressed solid in the pressure reactor during a reaction phase, with a liquid gas / solid mixture is generated, and then the liquid gas / solid mixture is explosively expanded into an expansion tank.
  • a liquefied gas e.g. a mixture of ammonia and urea are added to the pulp in the pressure reactor in order to produce CeHulose carbamate using the method according to the invention, the device according to the invention or the pressure reactor according to the invention.
  • the filling phase and the subsequent compression phase of the solid can be repeated one or more times in the pressure reactor -11-
  • one compression stroke or several successive compression strokes of a compression piston of the pressure reactor can be carried out in order to achieve the desired degree of filling.
  • the pressure reactor according to the invention for treating a solid, in particular cellulose, with a gas or a liquid, in particular liquid ammonia, optionally with urea, under pressure comprises a compression device which compresses the solid which has been introduced into the pressure reactor in order to compress it, as a result of which the already Advantages explained above can be obtained.
  • the process according to the invention for treating a solid, in particular cellulose, with a gas or a liquid, in particular liquid ammonia, under pressure is carried out with the following steps: a pressure reactor is charged with solid during a filling phase, and then the solid is in the pressure reactor during a compression phase compressed, then the gas or liquid is compressed during a reaction phase
  • Solid is fed into the pressure reactor to produce a liquid / solid mixture or gas / solid mixture, and then the mixture is explosively expanded into an expansion tank.
  • Figure 2 is a schematic view of the device for performing the method of Figure 1, with a pressure reactor with dosing;
  • Figure 3 is a side view of the device of Figure 2;
  • FIG. 4 is a plan view of the device of Figure 2;
  • FIG. 5 shows a schematic view of the pressure reactor according to the invention in accordance with a first embodiment for use in the device according to the invention;
  • Figure 6 is a schematic view of the pressure reactor of Figure 5 to explain a
  • FIG. 7 shows a schematic view of the pressure reactor according to FIG. 5 to explain a compression phase of the pressure reactor
  • Figure 8 is a schematic view of the pressure reactor of Figure 5 to explain a
  • Figure 9 is a schematic view of a solids processing
  • FIG. 10 is a schematic view of an alternative solids processing
  • Solid feed device for use in the device according to the invention
  • FIG. 11 shows a schematic view of a feed device for use in the device according to the invention.
  • Figure 12 is a schematic view of a second embodiment of the inventive pressure reactor for use in the inventive
  • Figure 13 is a schematic and perspective view of a pressure reactor group with four pressure reactors according to Figure 12 for use in the invention
  • FIG. 14 shows a schematic overall view of a device according to the invention with the pressure reactor group according to FIG. 13.
  • the pressure reactors 10 (here five parallel reactors) are conveyed in succession via a conveying means 22, for example the solid
  • Liquid gas here liquid ammonia
  • An additive e.g. Urea, which is mixed with the liquid ammonia.
  • the centerpiece of the system consists of the pressure reactors 10, which have a shut-off device 11 and 12, which stand vertically at the top and bottom, and which can be designed, for example, as valves.
  • a shut-off device 11 and 12 which stand vertically at the top and bottom, and which can be designed, for example, as valves.
  • Three openings 13 are provided here for the supply of the liquefied gas, so that a uniform penetration of the solid to be treated is ensured.
  • shut-off device which has a pressure resistance of up to approximately 40 bar is suitable for use in the device according to the invention, for example ball valves, segment ball valves, flaps, rotary valves or the like.
  • So-called lock systems i.e. two ball valves arranged in tandem can be used as shut-off devices.
  • the first ball valve is in contact with the product (and may lose its pressure stability over time), whereas the second ball valve does not come into contact with the product and should therefore have a lower leak rate.
  • the pressure reactor 10 it is also possible to design the pressure reactor 10 as a mixer. In this case, the shut-off devices at the inlet and outlet must be designed so that the tightness of the reactor is not endangered by the rotation of the mixing device.
  • the pressure reactor 10 is equipped with an external heater (not shown) which enables an increased temperature in the pressure reactor 10 and moreover compensates for the temperature drop after the rapid expansion into the expansion tank 14.
  • the pressure reactor 10 is appropriately filled with the solid
  • Transport of the solid matter into a storage container e.g. be ensured by screw conveyors, the closure of this storage container from the atmosphere and a supply of compressed ammonia gas for pneumatic conveying.
  • FIGS. 1 and 2 The main elements of the device according to the invention are shown in FIGS.
  • the individual containers are suitably fastened to a supporting structure, preferably made of steel, and comprise the pressure reactors 10 (only one is visible in FIGS. 2 to 4), the expansion container 14, washer 26 and an absorber 28 -15-
  • the steel structure is expediently accessible. Additional units, e.g. Pumps, cooler compressors are located below the system. The control, regulating units and the computer are not shown here. These elements can be separated from the system, for example in an adjoining room. In this way, the operator must monitor the
  • the expansion tank 14 consists of three parts screwed together with about 900 L content here.
  • FIG. 2 shows the receptacle for the explosion ball valve and the pressure reactor 10 attached to it on the right above the expansion tank 14.
  • a frame On the left side above the expansion tank 14, a frame is attached, on which a cellulose dosing trolley 23 is attached.
  • the lower part of the expansion tank 14 is tapered towards its end.
  • a slide system with a silicone seal ensures that the
  • a removable sieve plate is provided in the upper part of the expansion container 14, so that no pulp gets into the absorber 28.
  • a pressure measuring device is installed in front of and behind the sieve bottom, by means of which the pressure difference is determined. An increase in the pressure difference signals to the operator that the strainer is blocked.
  • the absorber here has a capacity of about 680 liters and is usually provided with a fill level sight glass so that it can be determined to what extent the immersion tubes protrude into the water in the absorber.
  • the absorber 28 can have an electrical level probe and a temperature sensor. At the bottom of the absorber 28 there are several outlets, two of which are connected via a pump to a flow cooler with a flow meter in order to circulate the absorber water and to keep it at a temperature of about 20 ° C. Fresh water can be fed in manually via an overhead connection to replace used water. The used water is drained by hand through a third nozzle on the floor.
  • the absorber is connected to the scrubbers 26, which in the present case have a volume of about 40 liters each, via flange connections via the two upper rear-facing exhaust air sockets of the absorber.
  • the air guided by the absorber is prewashed in the washers 26 before it is passed into the atmosphere.
  • the exhaust air is washed in a known manner via spray nozzles which are supplied with automatic refill via a recirculating cooler.
  • the gas required for the process is stored in a storage container, e.g. an .Ammoniak bottle stored, which is arranged on a dosing and connected to a control device.
  • a storage container e.g. an .Ammoniak bottle stored, which is arranged on a dosing and connected to a control device.
  • the reactor has a volume of approximately 1.2 liters and is heated on two opposite sides in the full length by means of a heat exchanger to a desired temperature. If ammonia is used as the liquid gas, a reactor temperature of approximately 80 ° C. has proven to be particularly suitable.
  • a chemical pressure gauge can be provided in the main line for controlling the pressure of the liquid gas, a valve for venting the absorber and one or more safety valves at a suitable location. Fine metering valves are preferably used for introducing the liquefied gas into the reactor 10. -17-
  • the cellulose dosing trolley 23 stands above the expansion tank 14 and is equipped with a storage tank and a double screw. It is controlled by a PLC control and the control device already mentioned.
  • the ball valves, butterfly valves, fine metering valves and the other valves are pneumatically controlled via the PLC control, which is connected to a computer. In the usual way, they have position indicators for the PLC control.
  • the pressure on the pneumatic valves is kept constant by a compressor.
  • the control consists of two control and regulation circuits, the PLC control (e.g. Sematic Step 5) and a computer with Intouch software as the user interface. Via the input unit of the
  • the entire system is also operated on the computer.
  • suitable display devices which, among other things, display all alarms.
  • the invention provides a method and a device suitable therefor, according to which liquid gas, preferably liquid ammonia, can be fed under pressure to a solid in whatever form.
  • liquid gas preferably liquid ammonia
  • This solid is kept in contact with the liquid ammonia under pressure for a predetermined period of time without there being any pressure drop in the reactor and without the substance to be treated itself having to be used to maintain the pressure, since the reactor is filled at ambient pressure . For this reason, the morphology of the solid to be treated is not changed or impaired.
  • the rapid and uniform diffusion of the liquid ammonia under pressure ensures a homogeneous distribution of the same in the solid to be treated and, as a result, a uniform activation of the solid.
  • the method according to the invention and the device specified for carrying out the method are particularly suitable for the treatment of cellulose, starch, gelatin, guar or wood chips and very generally of substances containing polysaccharides. Furthermore -18-
  • FIG. 5 shows schematically an inventive pressure reactor according to a first embodiment for use in the device according to the invention.
  • the pressure reactor 30 comprises a compressor device, a pressure reactor vessel 31, at least one solids inlet 36 and at least one conveying agent outlet 37 for a solids conveying means and is functionally subdivided into at least one compression section 32 and one reaction section 33, the two sections using a
  • Separator e.g. a ball valve, a flap or a lock can be separated from each other.
  • the pressure reactor vessel 31 is of a substantially cylindrical shape and is arranged vertically.
  • the pressure reactor vessel 31 has the compression section in the upper region
  • the compression section 32 essentially comprises a compression chamber 34, a compression device 35, the solids inlet 36, through which the solids into the
  • Compressor chamber 34 can be fed, and a conveyor outlet 37 through which a conveyor, e.g. Gas, air or nitrogen or the like with which the solid material is fed into the compression chamber via the solids inlet 36 is removed from the compression chamber 34 again.
  • a conveyor e.g. Gas, air or nitrogen or the like with which the solid material is fed into the compression chamber via the solids inlet 36 is removed from the compression chamber 34 again.
  • the compressor device 35 comprises a compressor 38 and a compressor drive device 42 which is coupled to the compressor 38 and drives the compressor 38.
  • the compressor 38 compresses or compresses or compresses the solid, which is present, for example, as torn pulp, that is to say as a relatively coarsely broken cellulose, in the compressor chamber 34 of the pressure reactor 30. -19-
  • the compressor 38 shown in FIG. 5 comprises a compressor piston 39 and a compressor rod 40 which is connected to the compressor piston 39.
  • the compressor piston 39 matches the diameter to the cross-sectional inner diameter of the compressor chamber 34 of the reactor vessel 31 and is arranged vertically within the compressor chamber 34 and also movable up and down into a reaction chamber 50 of the reaction section 33.
  • the compressor piston 39 has an upper side and a lower side, the upper side pointing to the conveying means outlet 37 and the lower side pointing to an expansion tank 89. Between the top and the bottom of the compressor piston 39 there are a plurality of fluid-permeable channels which provide a fluid-permeable connection for the gaseous conveying medium from the underside to the top of the compressor piston 39 to the conveying medium outlet 37.
  • the compressor rod 40 is attached to the top of the compressor piston 39, which in turn is moved by the compressor drive device 42 and converts its movement on the compressor piston 39.
  • the compressor drive device 42 comprises a pneumatic cylinder which is connected to a corresponding pneumatic system.
  • the compressor drive device 42 can also be designed as a hydraulic system or as a mechanical system driven by an electric motor.
  • the compressor piston 39 is shown in its starting position or rest position A, which it generally assumes when the compressor chamber 34 is charged with solid via the solids inlet 36.
  • the rest position A of the compressor piston 39 generally corresponds to the topmost position seen vertically, which the compressor piston 39 can assume.
  • a sensor device 43 is arranged, which for
  • the sensor device 43 has one or more sensors which, for example, are based on -20-
  • a ß sensor with the appropriate detector can be used.
  • the solids inlet 36 is continuously connected to a solids transport system or a Festste ff conveyor, which feeds the solids to the pressure reactor 30.
  • pulp in the form of the Torn Pulp is used as the solid.
  • guar splits or another granular solid or a mixture of solids can also be used.
  • the solid matter conveying device pneumatically requires the pulp or solid matter, ie using air or nitrogen or a similar gas as the conveying means. The funding that when filling the compressor chamber 34 on the
  • Solid inlet 36 enters the compression chamber 34 together with the solid, escapes via the conveyor outlet 37 from the compression chamber 34 or the pressure reactor interior.
  • the conveyor outlet 37 is fluidly coupled to a return device 96 (cf. FIG. 14) which controls the conveyor, e.g. Air, from the inside or the reactor chamber of the pressure reactor 30 back into the pulp
  • shut-off device 53 or separation device is provided, which is in an open position
  • the shut-off device 53 is indicated schematically in FIG. 5 as a ball valve. But it can also be used as a hinged closure device or e.g. as
  • Sluice device or double sluice device or the like can be designed in any case to establish a secure separation between the compression section 32 and the reaction section 33.
  • the reaction section 33 of the pressure reactor 30 has a cylindrical reaction chamber 50, the inside diameter of which corresponds to the diameter of the compression chamber 34.
  • a plurality of ammonia inlets 51 are formed in the wall of the reaction chamber 50, through which liquid ammonia can be fed to the reaction chamber 50.
  • a number of ammonia inlets 51 are provided in order to ensure a homogeneous loading of the reaction chamber 50 when the pulp is being filled.
  • a heating device 44 is arranged in or on the wall of the reaction chamber 50.
  • the reaction chamber 50 can be shut off or accessible upwards through the ball valve and downwards, i.e. towards the expansion chamber 89, through a further shut-off device 54, e.g.
  • reaction chamber 50 is thus separated from the expansion chamber 89 when the shut-off device 54 is closed, or is connected to the expansion chamber in a fluid or solid manner when the shut-off device 54 is open.
  • FIGS. 6, 7 and 8 show different phases or cycles of the pressure reactor function in order to describe the method according to the invention.
  • a filling phase is shown in FIG. 6, in which the compressor piston 39 is in its uppermost position within the compressor chamber 34, i.e. is in a rest position A.
  • FIG. 7 shows a typical compression phase, in which the compressor piston 39 compresses or compresses the amount of solids in the compressor chamber 34.
  • FIG. 8 shows an ejection phase in which, after the filling and compression of the solid in the
  • Pressure reactor 30 of the compressor piston 39 pushes the compressed amount of solids from the compression chamber 34 through the opened shut-off device 53 into the reaction chamber 50 of the pressure reactor 30, the compressor piston 39 being in an ejection position C for the compressed amount of solids from the compression chamber 34 into the reaction chamber 50 .
  • the compression pistons 39 are in their rest position A or retracted position A, while the solids supply device via an opened feed flap 52 and the solids inlet 36 also contains the compression chamber 34 of the pressure reactor 30 Solid, in this case cellulose in the form of torn pulp, using compressed air as the conveying medium.
  • the air that has entered the compressor chamber 34 during filling escapes through the channels 41 or the perforation of the compressor piston 39 to the conveyor outlet 37 located above in the conveyor circuit.
  • the shut-off device 53 of the pressure reactor 30 is closed during the filling.
  • the sensor signals from sensor device 43 are constantly monitored by a central control device. Since the sensor signals are a measure of the bulk density of the solid or pulp in the compression chamber 34, the central control device, e.g. a programmed computer, determine when a predetermined, specific output level or density of the
  • Solid is given in the compressor chamber 34.
  • the solids feed device now continuously feeds solids or cellulose to the compression chamber 34 until the central control device detects a corresponding predetermined filling level.
  • the central control device stops the solids feed device, closes the feed flap 52 or a corresponding shut-off device and controls the compressor drive device 42 to carry out a compression stroke in which the compressor rod 40 and thus also the compressor piston 39 are moved downward or downward from position A, in order to compress or compress the solid matter in the compression chamber 34, as shown in FIG. 7, the compression piston assuming a compression position B, for example.
  • the compression phase is in turn monitored by the central control device via the evaluation of the sensor signals of the sensor device 43.
  • the central control device determines on the basis of the sensor signals from the sensor device 43 that a target filling level or a -23-
  • the control device stops the compressor drive device 42 in order to stop the compression phase.
  • the central control device then opens the shut-off device 53 with the shut-off device 54 closed at the same time and controls the shut-off device
  • the central control device waits until the compressor piston 39 is again in its rest position A, which e.g. via motion or displacement sensors on the
  • Compressor rod 40 can be monitored. After the compressor piston 39 has reached its rest position A again, the central control device now closes the shut-off device 53 via corresponding electrical signals and actuating devices, as a result of which the reaction chamber 50 is hermetically separated from the compressor chamber 34. The central control device now leaves liquid via the ammonia inlets 51
  • Ammonia solid mixture expanded explosively from the reaction chamber 50 into the expansion chamber below.
  • Control device determines by evaluating the sensor signals from the sensor device 43, the compression piston 39 is returned to its rest position A or to its top dead center. The downward compression stroke is repeated. If, despite one or more repetitions of the compression stroke, none of the predetermined degrees of target compression are reached, a further filling phase is carried out, as was explained above with reference to FIG. 6.
  • This intermediate filling phase or additional or supplementary filling phase takes place e.g. such that only a relatively small amount of solids is fed into the compression chamber 34 from the solids supply device when the flap 52 is open. This small amount of filler can be brought about by the central control device via a brief or short-phase opening of the flap 52 when the solids supply device is active, without taking into account the sensor signals from the sensor device 43.
  • the central control device again initiates a compression phase (cf. FIG. 7) in order to obtain the degree of target compression of the filled solid.
  • a compression phase cf. FIG. 7
  • several compression strokes of the compressor piston 39 can again be carried out until the target compression degree is reached and the method can be continued with the discharge and reaction phase.
  • the central control device repeatedly performs supplementary filling and compression phases until the target compression level is reached, and the process can be continued with the discharge, reaction and expansion phases explained above. -25-
  • the solid preparation and feeding device shown in FIG. 9 essentially comprises a heating stage followed by a comminution stage, a gas or a liquid being fed to the solid or pulp in the heating stage in order to prepare the solid or pulp for further processing and to adjust the pulp for the absorption in the pressure reactor of unheated liquid ammonia more reactive.
  • the heating stage comprises a screw conveyor 63, the input side of a
  • the heating stage further comprises a heating device 73 and a pump 72, which are arranged in a heating circuit 66, in which the screw conveyor 63 is also at least for a certain section.
  • the heating circuit 66 is still appropriate
  • Feed devices such as pipes, valves etc. are fluidly connected to an ammonia reservoir 74, liquid or gaseous ammonia being able to be fed into the heating circuit 66 from the ammonia reservoir 74.
  • the pump 72 circulates the gaseous or liquid ammonia in the heating circuit 66.
  • the heating device 73 heats the ammonia to a temperature of approximately 100 ° C., which is fed to the pulp in the screw conveyor 63 in order to prepare the pulp for further processing.
  • the ammonia gas or the liquid ammonia acts in the screw conveyor 63 on the pulp along an exposure path during a predetermined exposure time.
  • the heating stage is followed by the shredding stage, which consists of a shredder 64, e.g. one
  • a shredder or crusher for wood chips and a subsequent screening device 65, in which excessively coarse solid or pulp is screened out and fed back to the shredder 64 via a solids return 71 on the input side.
  • the fine pulp passes through the screening device 65 and can then be fed via a further feed or further solid feed device, as explained below -26- is, for example, the pressure reactor 30 or distributed to a pressure reactor group consisting of a plurality of pressure reactors 30.
  • the preparation in the heating stage makes the solid or pulp more reactive for the later absorption of liquid ammonia in the pressure reactor 30, as a result of which the
  • Dwell time or cycle time during the reaction phase of pulp of ammonia in the pressure reactor can be reduced and the yield rate in the overall process can thereby be increased.
  • the further comminution of the solid or the pulp and subsequent sieving in the comminution stage make it possible for the pressure reactor 30 to be provided with pulp with improved homogeneity and an enlarged reaction surface, as a result of which the reaction phase in the pressure reactor is further shortened and the yield rate of the overall process is accordingly increased or the cycle times of the quasi-continuous manufacturing process of the invention can be shortened.
  • FIG. 10 shows a supplemented or alternative embodiment of the fixed processing and crushing device of FIG. 9 again schematically.
  • the same parts and devices of the processing stage of FIG. 10, as are also used in the embodiment of FIG. 9, are given the same reference numerals in FIG. 10 and are therefore not explained in more detail below.
  • the processing device of FIG. 10 has an additional heating stage followed by an additional comminution stage, the additional heating stage and additional comminution stage following the screening device 65 on the output side in this order.
  • the additional heating stage essentially in turn comprises a screw conveyor 67 and an ammonia feed device 70, which feeds the screw conveyor 67 preheated liquid ammonia, which in turn is in the screw conveyor 67 for an exposure time over a -27-
  • Conveying line acts on the pulp or solid, which is conveyed on by the screw conveyor 67.
  • the additional heating stage is followed by the additional comminution stage 68, which essentially consists of e.g. there is another shredder, e.g. as cold
  • Shredder 68 (available e.g. from the company Fryma, Switzerland) can be designed and the shredded pulp is fed to the solids feed device or the transport system or directly via a shut-off device, e.g. a slide or a flap 69, the pressure reactor 30 supplies.
  • a shut-off device e.g. a slide or a flap 69, the pressure reactor 30 supplies.
  • the additional size reduction serves to further homogenize the size
  • FIG. 12 schematically shows a further embodiment of a pressure reactor 80 according to the invention for use in the device according to the invention.
  • the pressure reactor 80 consists of a vertically or vertically arranged pressure reactor housing with a cylindrical cross section, which is closed at the top and at the bottom, i.e. towards the expansion chamber 89, with a shut-off device 88, e.g. a ball valve is provided which, in the open state, provides a continuous connection between a reactor chamber 81 or the interior of the pressure reactor 80 and the expansion chamber 89 and in the closed state shuts off the interior of the pressure reactor 80 with respect to the expansion chamber 89.
  • a shut-off device 88 e.g. a ball valve
  • the interior of the pressure reactor 80 is designed as a single chamber with the reactor chamber 81.
  • the pressure reactor 80 further comprises a compressor device and one
  • Separating device which separates the solid or pulp or pulp particles fed via a continuously working feed device from a conveying means, for example air or nitrogen.
  • the compressor device includes a compressor piston 84, a piston rod 85, which attaches to an upper side of the compressor piston 84, and a drive device (see, for example, 98 in FIG. 14), which is coupled to the piston rod 85, around the compressor piston 84 within the reactor chamber 81 to move up and down and carry out appropriate compressor strokes.
  • the compressor piston 84 fits circumferentially in the clear
  • the drive device of the compressor piston 84 can in turn, e.g. be designed pneumatically.
  • the solids feed device is designed pneumatically, for example, and compressed air is accordingly used as the conveying means.
  • the separating device is designed as a cyclone 83, to the input side of which the supplied solid material is fed with conveying means via a solids inlet 86 and the conveying means is removed from the outlet side via a conveying means outlet 87.
  • a section of the reactor chamber 81 serves as the vortex chamber of the cyclone 83.
  • a plurality of ammonia inlets 90 which are offset in height and radially from one another are formed.
  • the lower region of the reactor chamber 81 serves as the reaction region 82 in which the solid ammonia or cellulose is charged with the liquid ammonia in order to form the cellulose / ammonia mixture.
  • a sensor device is in turn attached to the pressure reactor 80, which detects the fill level and degree of compaction of the solid matter in the reactor chamber 81 and is connected to a control device for the pressure reactor 80, which performs all the filling, compression, reaction and closing and opening processes controls and monitors at the pressure reactor 80.
  • the compressor piston 84 is in its uppermost position, namely its rest position D, above the feed device -29- and the cyclone 83, the reactor chamber 81 of the pressure vessel 80 is filled with solid, the conveying means being discharged via the conveying means outlet 87.
  • a compression phase is initiated by the control device.
  • the compressor piston 84 driven by a pneumatic drive device via the piston rod 85, carries out a downward compression stroke or a plurality of successive compression strokes until a predetermined degree of compression of the pulp is given in the reactor chamber 81, which in turn monitors the control device by means of the sensor device and is controlled. If the target degree of compression of the pulp is reached, the compressor piston 84 remains in the deflected position, namely the end position E. of the last compression stroke.
  • the pulp in the reactor chamber 81 then has e.g. the fill level or associated volume V2, as can be seen in FIG.
  • Compression piston 84 can be adjusted, allowing different volumes, e.g. also VI, can be realized.
  • a reaction area 82 within the reactor chamber 81 is then delimited by the compression piston 84 in position E, by the cylindrical wall of the reactor housing and by the closed shut-off device 88, the volume of the reaction area 82 corresponding to the volume that was compressed
  • the central control device then initiates the reaction phase, while the liquid ammonia is fed under pressure to the solid or pulp in the reaction area 82 via the ammonia inlets 90. After the end of the reaction phase or the assigned reaction time, the control device opens the shut-off device 88 and the intended explosion-like explosion of the pulp / ammonia mixture now present in the reaction area takes place into the expansion chamber 89. -30-
  • the central control device then closes the shut-off device 88 again and the compressor piston 84 is withdrawn into its rest position D (return phase), after which a new cycle of filling phase, compression phase, reaction phase and expansion phase is carried out.
  • the compressor piston 84 itself has the function of limiting or closing the reaction area 82 without requiring an additional shut-off device.
  • FIG. 11 shows an example of a device that can be used in the device according to the invention
  • the feed device shown essentially has a screw conveyor 91, which is coupled to an associated drive 93, and a conveyor propeller 94, which is connected on the input side to the screw conveyor area and on the output side to a distribution system 95.
  • the screw conveyor has a left-hand section and a right-hand section and is connected to a solids supply 92 from which the screw conveyor 91 solids, e.g. Cellulose, promotes.
  • the conveyor propeller 94 starts to detect solid matter fed from the screw conveyor 91 and feed it to the distribution system 95, which finally feeds the accelerated solid matter to one or more pressure reactors.
  • the solid feed device shown in FIG. 11 continuously feeds solid to the pressure reactors.
  • a compressed gas line can be attached to the screw conveyor
  • Set up 91 that conveys a pressurized gas to the screw conveyor 91, e.g. compressed air, nitrogen, in order to enable the solid to be transported continuously into the distribution system from the screw conveyor 91; the pressurized gas then acts as a propellant gas and conveying agent for the solid in the distribution system 95 the pressure reactor.
  • a pressurized gas e.g. compressed air, nitrogen
  • FIG. 13 shows an example of a pressure reactor group which comprises four identical pressure reactors 80.1, 80.2, 80.3 and 80.4 of the type shown in FIG. 12, one pneumatic cylinder 98 per pressure reactor for driving the respective compressor piston 84 via the piston rod 85.
  • Pressure reactors 80.1 to 80.4 are connected to the distribution system 95 of a solids supply device (cf. 91, 92, 95, 100 of FIG. 14), the conveying device outlets 87 of the cyclones 83 into a common conveying medium return device 96, as in the figure 14 is shown.
  • the ammonia inlets 90 of the individual pressure reactors 80.1 to 80.4 are connected to an ammonia source for liquid pressurized ammonia via a line system shown in FIG.
  • the individual pressure reactors 80.1 to 80.4 are operated either individually or in groups, e.g. in groups of two, operated and controlled offset to each other in order to obtain a quasi-continuous overall manufacturing process.
  • the filling and compression phase are carried out, while in the two rear pressure reactors 80.3 and 80.4 the reaction and
  • the operation of the pressure actuator group can, however, also take place out of phase, as will be explained below.
  • the corresponding pressure reactors are filled for the first time out of phase
  • the filling phase is then carried out in a first step, for example in the pressure reactor 80.1, while the compression phase is carried out simultaneously in the pressure reactor 80.2, the reaction phase in the pressure reactor 80.3 and the expansion phase and return phase of the compressor piston 84 in the pressure reactor 80.4.
  • the next, second step they are then simultaneously to each other, corresponding to the figure -32-
  • the expansion and return phases are then carried out simultaneously in the pressure reactor 80.1, the filling phase in the pressure reactor 80.2, the compression phase in the pressure reactor 80.3 and the reaction phase in the pressure reactor 80.4.
  • FIG. 14 shows the supply system which is designed to match FIG. 13 and comprises a supply of solid material, a conveyor circuit 96 and a heating circuit 66.1.
  • the solids supply comprises a storage container (silo) 92, to which 100 solids, for example pulp as Tora Pulp or ground pulp, are fed on the input side via a cellular wheel sluice, and the pulp prepared in the silo 92 is removed on the output side via a further cellular wheel sluice.
  • the rotary valve 100 transfers the pulp from the silo 92 to the screw conveyor 91 (see, for example, FIG. 11), at the output of which compressed air as propellant gas and funding from the conveyor circuit 96 is fed to the pulp conveyed by the screw conveyor 91, causing the pulp to enter the pulp Distribution system 95 is conveyed to the pressure reactors 80.1 to 80.4.
  • the conveyor outlets 87 of the cyclones 83 of the pressure reactors are fluidly connected to a conveyor return device 96 of the conveyor circuit, the -33-
  • Conveyor return device 96 supplies the recirculated conveying device to a compressor device 97, which compresses the compressed air again and, as said, feeds into the distribution system 95 for conveying the pulp.
  • a filter device can be used in the conveying means return device in order to filter out solid particles from the conveying means or propellant gas return flow.
  • a funding supply 98 is connected to the funding cycle.
  • the pulp or solid in the silo 92 is charged with liquid or gaseous ammonia in a heating circuit 66.1, with a pump 72 in the heating circuit 66.1 which recirculates and feeds the
  • the gaseous or liquid ammonia e.g. heated to 100 ° C.
  • the relatively large volume of the silo 92 ensures that a desired processing reaction or a desired action of the heated ammonia on the pulp in the silo 92 is ensured before the solid is removed from the silo 92.
  • Heating circuit 66.1 is also connected to an ammonia source 74, which is used to compensate for ammonia losses in the heating circuit.

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Abstract

L'invention concerne un procédé permettant de traiter des matières solides avec des gaz liquides, notamment de l'ammoniaque liquide, sous pression. Selon ce procédé, la matière solide à traiter à une pression ambiante est introduite dans un réacteur pressurisé (10). Ensuite, le gaz liquide sous pression est introduit dans le réacteur pressurisé (10). Au bout d'un temps de séjour donné, le mélange gaz liquide/matière solide ainsi obtenu est détendu par explosion dans un contenant d'expansion (14). Au moins deux réacteurs sont exploités de manière cadencée. L'invention concerne également un dispositif qui permet de traiter des matières solides avec des gaz liquides sous pression. Ce dispositif comprend au moins deux réacteurs pressurisés parallèles destinés à recevoir alternativement une matière solide et un gaz liquide. Chaque réacteur possède des orifices d'entrée et de sortie qui sont dotés d'organes de fermeture (11, 12) et destinés à la matière solide; au moins un orifice d'entrée (13) destiné au gaz liquide; au moins un contenant d'expansion (14) relié aux réacteurs pressurisés (10) concernés et un moyen de transport (18) destiné à l'alimentation en matière solide et en gaz liquide.
EP99911760A 1998-03-13 1999-03-09 Dispositif, procede et reacteur pressurise permettant de traiter des matieres solides avec un gaz liquide sous pression Withdrawn EP1066109A1 (fr)

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DE19810741 1998-03-13
DE19810741 1998-03-13
DE19832853 1998-07-21
DE19832853 1998-07-21
PCT/EP1999/001517 WO1999047250A1 (fr) 1998-03-13 1999-03-09 Dispositif, procede et reacteur pressurise permettant de traiter des matieres solides avec un gaz liquide sous pression

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AU3032899A (en) 1999-10-11
WO1999047250A1 (fr) 1999-09-23
DE19910562A1 (de) 1999-09-16
US6416621B1 (en) 2002-07-09

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