Inertization of partially filled extruder inlets

Abstract

The present invention relates to a method for operating an extruder, in particular for variably adjusting the oxygen content in the supply region of the extruder, wherein the extruder has a filling shaft for supplying a material to be extruded, which filling shaft has an inlet opening at one end and opens into the extruder housing at the opposite end, and in which filling shaft at least one inert gas feed device is provided for supplying an inert gas flow into the filling shaft, wherein the inert gas volume flow of the inert gas flow is adjusted such that the Reynolds number of the inert gas flow in the filling shaft (Re) is at least 180. The invention further relates to a control device for variably adjusting the oxygen content in the supply region of an extruder during operation thereof, in particular in a method according to the invention, and to an extruder having an associated control device of this type.

Description

[0001] Inerting of partially filled extruder inlets

[0002] The present invention relates to a method for operating an extruder, in particular for variably adjusting the oxygen content in the feed area of ​​the extruder, wherein the extruder has a feed chute for supplying a material to be extruded, which has an inlet opening at one end, opens into the extruder housing at the opposite end, and in which at least one inert gas supply device is provided for supplying an inert gas stream into the feed chute. The invention further relates to a control device for variably adjusting the oxygen content in the feed area of ​​an extruder during its operation, in particular in a method according to the invention, and to an extruder with an associated control device of the aforementioned type.

[0003] State of the art

[0004] Extruders with partially filled feeds, widely used for processing or compounding thermoplastics and elastomers, present a significant challenge in assessing explosion hazards. Frequently, changing components containing potentially hazardous amounts of combustible dust (and possibly granule abrasion) are used. The typical gravimetric dosing of bulk materials with high accuracy requirements necessitates an open atmosphere with sufficient oxygen, and the exposed extruder shafts can generate friction and impact sparks, as well as locally hot surfaces due to friction.Due to the complex mechanical loads and high rotational speeds of modern extruders, especially the frequently used twin-screw extruders (TSE = Twin Screw Extruder), manufacturers generally cannot declare suitability for explosion zones (ATEX) inside the machine of zones 20 and 21 under such conditions; even suitability for zone 22 is only declared by the manufacturers under very restrictive boundary conditions for intended use.

[0005] In extruders where the screw shafts continuously cause a positive axial conveyance of the bulk material in the process direction, the introduced solids are quickly compacted into a pile and then melted, so that the occurrence of explosive mixtures inside the filled extruder is no longer to be expected.

[0006] During the introduction of bulk material, gas / air is introduced into the critical zone under atmospheric conditions along with the solid and conveyed with the solid in the process direction. The compression of the bulk material until melting and the coalescence of the particles into the melt force the insoluble fraction of this gas (the vast majority) backwards against the process direction, where it rises in the inlet opposite to the introduced bulk material. Immediately above the inlet opening, a dynamic gas equilibrium of falling and rising air exists, the relative composition of which is representative for the entire critical zone.

[0007] To reliably prevent the formation of explosive mixtures inside the extruder in the aforementioned explosion-hazardous areas, it is known to inertize this area using nitrogen. This must be done in such a way that the oxygen content inside the partially filled section of the extruder is reduced to a level that reliably falls below the oxygen limit of the dusts used.

[0008] The limiting oxygen concentration for dusts is a safety-related parameter determined according to the standard procedure DIN EN 14034-4 (2011-04). For organic dusts, it is in the range of 10 vol% under atmospheric conditions. It is subject to pressure and temperature influences. The maximum operating temperature in the gas phase of a partially filled extruder can be conservatively estimated at approximately 150 °C.

[0009] According to the research report for the BG RCI (German Social Accident Insurance Institution for the Raw Materials and Chemical Industry) "Safety-Related Parameters of Dusts under Non-Atmospheric Conditions" by Dr. Ute Hesener, DEKRA EXAM GmbH, Bochum, 2015, there are only a limited number of studies investigating the influence of elevated temperature on the limiting oxygen concentration of dusts. However, a reduced limiting oxygen concentration is to be expected. Based on the available studies, a reduction in the limiting oxygen concentration of 1.9 vol% per 100 K temperature increase can be assumed. Therefore, for the presented inerting concept, a limiting oxygen concentration of 7.4 vol% under process conditions is assumed.

[0010] To maintain a sufficient margin from critical values, a maximum oxygen content of 10 vol.%, or preferably 6 vol.%, is targeted for normal operation in the extruder. Since bulk materials are typically stored and conveyed in air, the oxygen content in the critical range must be reduced below the critical concentration by locally superimposing an inert gas at the extruder inlet. According to current technology, counterflow and crossflow dosing are the most effective methods for this. Such methods are known, for example, from EP1318903B1, JP2012162048A, CN114248415A, EP3913015A1, and JP3216321A.

[0011] The problem here is that the oxygen content in the critical area of ​​the extruder is difficult to determine continuously with reasonable effort and sufficient accuracy. This is partly due to the fact that the available oxygen sensors do not function reliably in a dusty medium and are not robust enough to withstand the necessary mechanical and, if applicable, aqueous cleaning processes in this area.

[0012] To address this problem pragmatically, a significantly larger quantity of nitrogen is often used for safety reasons than would actually be necessary. This increases the extruder's operating costs and the risk of transporting fine particles of the formulation out of the feed chute.

[0013] Therefore, there is a need for a solution to reduce nitrogen dosing to the actual technical level as much as possible and thereby increase the economic efficiency of the extrusion process.

[0014] Object of the invention

[0015] The object of the present invention was therefore to provide a method by which the nitrogen dosage for reducing the oxygen content in the critical area of ​​the extruder, namely in the feed area, can be continuously reduced to the technically required level while simultaneously ensuring safe operation of the extruder.

[0016] Solution to the problem: The problem was solved by a method for operating an extruder, in particular for variably adjusting the oxygen content in the feed area of ​​the extruder, wherein the extruder has a feed chute for feeding a material to be extruded, which has an inlet opening at one end, opens into the extruder housing at the opposite end and in which at least one inert gas supply device is provided for feeding an inert gas stream into the feed chute, wherein the method is characterized in that the inert gas volume flow rate of the inert gas stream is adjusted in such a way that the Reynolds number of the inert gas stream in the feed chute is at least 180.

[0017] During the development work that led to the present invention, it was surprisingly discovered that, by maintaining this Reynolds number of the inert gas flow in the feed chute, the oxygen concentration at the inlet of the feed chute into the extruder housing can be set and maintained at a maximum of 10 vol.% under normal pressure, preferably at a maximum of 6 vol.%, as determined according to DIN EN 14789, without the need for an actual measurement of the oxygen concentration.

[0018] Equally surprisingly, it was found that the relationship between the amount of nitrogen and the achieved oxygen concentration can be represented dimensionlessly, and that predictions of a safe operating range are possible without elaborate measurement series for, for example, co-rotating, closely meshing twin-screw extruders with shaft diameters of 32 mm - 130 mm (corresponding throughputs between approx. 200 kg / h and > 8000 kg / h).

[0019] Furthermore, it is surprising that the commonly used counter-current flow of the inert gas stream to the oxygen-laden inlet stream is not optimal. Instead, a targeted cross-flow with high local gas velocities at the inert gas inlet achieves more favorable results overall.

[0020] Detailed description of the invention

[0021] In an advantageous further development of the method according to the invention, the Reynolds number of the inert gas flowing out of the drop shaft is 180 to 2000, in particular 300 to 2000, preferably 400 to 2000, and particularly preferably 500 to 2000. In this way, the oxygen concentration at the inlet of the filling shaft can be adjusted to the desired level, for example, when concentrations lower than 10 vol.% below normal flow are desired.

[0022] Within the scope of the invention, the Reynolds number of the inert gas stream is preferably defined as with l = characteristic length of the filling shaft, where I is defined in the case of a rectangular filling shaft as l = characteristic length of a rectangular shape = with a and b as side lengths of the

[0023] Rectangle, and in the case of a round or elliptical filling chute as l = 2 * a with a as the radius of the circle or in the case of an ellipse as the long radius,

[0024] N2 = volume flow rate of inert gas in standard liters, g = kinematic viscosity of inert gas under normal conditions, vmittei = — as average velocity in the drop shaft

[0025] ■^s

[0026] As = Cross-sectional area of ​​the filling shaft at the point that is 2 to 6 times

[0027] The distance of the screw diameter above the screw comb corresponds to this.

[0028] Normal conditions within the scope of the present inventions are a temperature of 18

[0029] °C and a pressure of 1 bar.

[0030] Furthermore, the Reynolds number of the inert gas stream Re is preferred, defined as with transverse = proportion of cross flow of the inert gas addition to the total flow of inert gas

[0031] O2 = target oxygen concentration in vol.%, A = 2.2 to 2.8;

[0032] B = 21 to 22;

[0033] C = -0.003 to -0.0035 and

[0034] D = - (A-0.3) to - (A+1).

[0035] Solving for the target oxygen concentration in vol% O2, the equation is as follows:

[0036] 02 = A + B * e c * Re + D * across

[0037] Within the scope of the present invention, it is particularly preferred that the target oxygen concentration in the equation is set at least 2 vol% lower than the actual permissible temporary maximum O2 concentration, more preferably at least 3 vol% lower, or even at least 3.5 vol% lower. This is preferred to ensure a larger safety margin during operation, for example, to compensate for sudden fluctuations in the feed of the material to be extruded. Thus, for example, instead of the targeted permissible temporary maximum O2 concentration of 6 vol% in the above formula, the target oxygen concentration can be conservatively entered as 2.5 vol%.

[0038] In the method according to the invention, the extruder typically has at least one screw shaft, in particular at least two screw shafts, which are preferably driven in the same direction.

[0039] In the extruder used, the feed chute is preferably located above the extruder housing and is oriented almost vertically. This means, for example, an angle of 90° + / - 10° between the extruder housing and the feed chute, and in particular 90° + / - 5°.

[0040] In the process according to the invention, preferably at least one of the inert gas supply devices is aligned at an angle of 90 ± 45° relative to the feed direction of the material to be extruded, preferably at an angle of 90 ± 15°, and more preferably at an angle of 90 ± 5°. By orienting the inert gas substantially transversely to the feed direction, particularly efficient utilization of the inert gas and better mixing with the air contained in the feed chute can be ensured, thus largely preventing locally higher oxygen concentrations than the desired concentration.

[0041] According to a further preferred embodiment of the method according to the invention, at least one of the inert gas injection devices is arranged at a distance of at most three times the outer diameter of the extruder screw above the upper edge of the screw shaft. This is advantageous because it allows the desired oxygen concentration to be reliably controlled, especially in the critical area above the extruder screws.

[0042] It is further preferred that the cross-sectional area of ​​the feed chute in the feed direction of the material to be extruded is largely constant below the inert gas supply device, wherein, when several inert gas supply devices are used, the cross-sectional area of ​​the feed chute in the feed direction of the material to be extruded is largely constant below the inert gas supply device located closest to the extruder housing.

[0043] In a preferred embodiment of the inventive method, the cross-sectional area of ​​the feed chute at its end opening into the extruder housing is largely constant over a length of at least twice the characteristic length l.

[0044] When carrying out the process according to the invention, the feed capacity of the extruder should be greater than the metered flow rate of the material to be extruded. This ensures that the extruder is operated partially filled and that there is no build-up of material to be extruded in the feed area.

[0045] In principle, all materials processable by extrusion can be used within the framework of the process according to the invention. Preferably, the material is selected from organic materials, in particular from thermoplastic or elastomeric polymer materials. The material to be extruded is preferably selected from polycarbonate, polyamide, polyester, in particular polybutylene terephthalate and polyethylene terephthalate, polylactide, polyether, thermoplastic polyurethane, polyacetal, fluoropolymer, in particular polyvinylidene fluoride, polyethersulfones, polyolefins, in particular polyethylene and polypropylene, polyimide, polyacrylate, in particular poly(methyl) methacrylate, polyphenylene oxide, polyphenylene sulfide, polyetherketone, polyaryletherketone, styrene polymers, in particular polystyrene, styrene copolymers, in particular styrene acrylonitrile copolymer, acrylonitrile butadiene styrene block copolymers, polyvinyl chloride, or a blend of at least two of the aforementioned materials.

[0046] The material to be extruded may further comprise additives, which are in particular selected from flame retardants, thermostabilizers, antioxidants, UV stabilizers, demolding agents, pigments, mineral fillers and mixtures thereof, wherein the mineral fillers are in particular selected from talc, wollastonite, kaolin, calcium carbonate, quartz glass, graphite or mixtures thereof.

[0047] According to a particularly preferred embodiment of the method according to the invention, the oxygen concentration at the inlet of the feed chute into the extruder housing is less than 10 ol% under normal pressure, determined according to DIN EN 14789 - 2017- 05, in particular at most 8 vol%, preferably at most 7 vol%, more preferably at most 6 vol%.

[0048] In principle, any gas that does not react with the material to be extruded under the given conditions can be used as an inert gas. In practice, the inert gas is typically selected from nitrogen, noble gases, especially argon, carbon dioxide, or mixtures thereof.

[0049] A further object of the present invention relates to a control device for variably adjusting the oxygen content in the feed area of ​​an extruder during its operation, in particular in a method according to the invention, wherein the extruder has a feed chute for feeding a material to be extruded, which has an inlet opening at one end and opens into the extruder housing at the opposite end and in which at least one inert gas supply device is provided for supplying an inert gas stream into the feed chute, wherein the control device is designed such that the inert gas volume flow rate of the inert gas stream can be adjusted in such a way that the Reynolds number Re of the inert gas stream in the feed chute is at least 180.

[0050] Preferably, the control device is designed in such a way that the Reynolds number of the inert gas flow at the injection point can be adjusted to at least 3,000, in particular to 3,000 to 80,000.

[0051] The invention further relates to an extruder with an associated control device according to the invention for variably adjusting the oxygen content. The invention relates in particular to the following embodiments:

[0052] According to a first embodiment, the invention relates to a

[0053] 1. A method for operating an extruder, in particular for variably adjusting the oxygen content in the feed area of ​​the extruder, wherein the extruder has a feed chute for feeding a material to be extruded, which has an inlet opening at one end, opens into the extruder housing at the opposite end, and in which at least one inert gas supply device is provided for supplying an inert gas stream into the feed chute, wherein the method is characterized in that the inert gas volume flow rate is adjusted such that the Reynolds number of the inert gas stream in the feed chute is at least 180. A method according to embodiment 1, characterized in that the Reynolds number of the inert gas stream is 180 to 2000, in particular 300 to 2000, preferably 400 to 2000, and particularly preferably 500 to 2000.

[0054] 3. Method according to embodiment 1 or 2, characterized in that the Reynolds number of the inert gas stream is defined as with l = characteristic length of the filling shaft, where I is defined in the case of a rectangular filling shaft as l = characteristic length of a rectangular shape = with a and b as side lengths Rectangle, in the case of a round or elliptical filling shaft as l = 2 * a with a as the radius of the circle or in the case of an ellipse as the long radius,

[0055] N2 = Volume flow rate of inert gas in standard liters, g = kinematic viscosity of inert gas at standard conditions - 18°C, 1 bar. vmittei = — as average velocity in the drop shaft,

[0056] ■^s

[0057] As = cross-sectional area of ​​the filling shaft, where A s is determined at a height of 2 to 6 times the screw diameter above the screw crest, with

[0058] O2 = Target oxygen concentration in vol.%,

[0059] 4. Method according to embodiment 3, characterized in that the target oxygen concentration O2 is defined in vol.% as

[0060] O2 = A + B * e c * Re + D * across transverse = proportion of the cross flow of the inert gas addition to the total flow of inert gas

[0061] A = 2.2 to 2.8;

[0062] B = 21 to 22;

[0063] C = -0.003 to -0.0035;

[0064] D = - (A-0.3) to - (A+1). with Reinjekt as the Reynolds number of the inert gas flow at the injection point.

[0065] 5. Method according to one of the preceding embodiments, characterized in that the Reynolds number of the inert gas stream at the point of injection into the filling shaft is at least 3,000, in particular 3,000 to 80,000, wherein reinjection is defined as p = kinematic viscosity of an inert gas under normal conditions: 18°C, 1 bar,

[0066] N2 = Volume flow of inert gas in standard liters and d = diameter of the feed opening for N2. A method according to one of the preceding embodiments, characterized in that the extruder has at least one screw shaft, in particular at least two screw shafts, which are preferably driven in parallel. A method according to one of the preceding embodiments, characterized in that the feed chute is arranged above the extruder housing and is oriented largely vertically. A method according to one of the preceding embodiments, characterized in that at least one of the inert gas feed devices is oriented at an angle of 90 ± 45° with respect to the feed direction of the material to be extruded, preferably at an angle of 90 ± 15°, more preferably at an angle of 90 ± 5°.A method according to one of embodiments 6 to 8, characterized in that at least one of the inert gas injection devices is arranged at a distance of at most three times the screw outer diameter of the extruder above the upper edge of the screw shaft. A method according to embodiment 9, characterized in that the cross-sectional area of ​​the feed chute in the feed direction of the material to be extruded is largely constant below the inert gas injection device, wherein, when several inert gas injection devices are used, the cross-sectional area of ​​the feed chute in the feed direction of the material to be extruded is largely constant below the inert gas injection device located closest to the extruder housing.A method according to one of embodiments 3 to 10, characterized in that the cross-sectional area of ​​the feed chute at its end opening into the extruder housing is largely constant over a length of at least twice the characteristic length l. A method according to one of the preceding embodiments, characterized in that the feed capacity of the extruder is greater than the metered flow rate of the material to be extruded. A method according to one of the preceding embodiments, characterized in that the material to be extruded is selected from organic materials, in particular from thermoplastic or elastomeric polymer materials.Method according to embodiment 13, characterized in that the material to be extruded is selected from polycarbonate, polyamide, polyester, in particular polybutylene terephthalate and polyethylene terephthalate, polylactide, polyether, thermoplastic polyurethane, polyacetal, fluoropolymer, in particular polyvinylidene fluoride, polyethersulfones, polyolefins, in particular polyethylene and polypropylene, polyimide, polyacrylate, in particular poly(methyl) methacrylate, polyphenylene oxide, polyphenylene sulfide, polyetherketone, polyaryletherketone, styrene polymers, in particular polystyrene, styrene copolymers, in particular styrene acrylonitrile copolymer, acrylonitrile butadiene styrene block copolymers, polyvinyl chloride or a blend of at least two of the aforementioned materials.A method according to embodiment 13 or 14, characterized in that the material to be extruded further comprises additives, which are in particular selected from flame retardants, thermal stabilizers, antioxidants, UV stabilizers, demolding agents, pigments, mineral fillers, and mixtures thereof, wherein the mineral fillers are in particular selected from talc, wollastonite, kaolin, calcium carbonate, quartz glass, graphite, or mixtures thereof. A method according to one of the preceding embodiments, characterized in that the oxygen concentration at the inlet of the feed chute into the extruder housing is less than 10 vol.% under normal pressure, in particular at most 8 vol.%, preferably at most 7 vol.%, more preferably at most 6 vol.%, determined according to DIN EN 14789-2017-05.A method according to one of the preceding embodiments, characterized in that the inert gas is selected from nitrogen, noble gases, in particular argon, carbon dioxide, or mixtures thereof. A control device for variably adjusting the oxygen content in the feed area of ​​an extruder during its operation, in particular in a method according to one of embodiments 1 to 17, wherein the extruder has a feed chute for feeding a material to be extruded, which has an inlet opening at one end and opens into the extruder housing at the opposite end, and in which at least one inert gas supply device is provided for feeding an inert gas stream into the feed chute, wherein the control device is designed such that the inert gas volume flow rate can be adjusted so that the Reynolds number Re of the inert gas stream in the feed chute is at least 180.Control device according to embodiment 18, characterized in that the control device is designed such that the Reynolds number of the inert gas flow at the injection point can be adjusted to at least 3,000, in particular to 3,000 to 80,000. Extruder with an associated control device for variable adjustment of the oxygen content according to embodiment 18 or 19.

[0067] Examples

[0068] Example 1

[0069] A CPM Extricom CXE32 twin-screw extruder with a 32 mm screw outer diameter and an L / D ratio of 44 was used. The feed consisted of BPA-PC in granular form (strand granules 3 mm long and average particle weight 22 mg), as well as a proportion of BPA-PC regrind with an average diameter d50 of 600 pm – the total proportion of which in the feed stream was varied from 9% to 75% in the test series, with the regrind being the primary component. The total mass flow rate was varied from 100 kg / h to 200 kg / h.

[0070] The extruder inlet was rectangular, with an inlet length of 1 = 0.075 m and an inlet width of d = 0.05 m. Nitrogen was injected 90 mm above the upper screw crest at a 90° angle to the mass feed via a 3 mm inner diameter supply line. To measure the oxygen concentration, gas was continuously extracted from a point centrally located above the screw clevis, 45 mm from the upper screw crest, and continuously fed into a Horiba PG-250 paramagnetic oxygen detector. The measurement was performed according to DIN EN 14789, with a measuring range of 0–100 vol. % O₂ and an error rate of ±1 vol. % O₂. The measurement was calibrated with N₂ on the day of the measurement.

[0071] The target concentration of residual oxygen in the model was conservatively set at 2.5 vol% O2 to ensure that the maximum target of 6 vol% O2 measured was not exceeded. Based on this, the model derives a target Reynolds number of 755 for the inert gas, corresponding to 2.0 N / m³.3 / h (= 2.04 standard liters / h) nitrogen.

[0072] Re * A s * 7] 755 * 0.00375m 2 * 0.000015 m 2 / sl 0.075m

[0073] 0.0005663m 3

[0074] = 2.04m 3 / / is

[0075] Kinematic viscosity of nitrogen: At 18°C ​​and 1 bar ambient pressure (i.e., standard conditions), 0.000015 m 2 / s.

[0076] At a throughput of up to 200 kg / h and a maximum mass fraction of powdered BPA-PC feed, the following values ​​were obtained at 2.0 Nm: 3 / h N2 addition measured values ​​of 5 vol. % O2 not exceeded.

[0077] Subsequently, the nitrogen flow was intentionally reduced below the specified quantity according to the invention in order to demonstrate that this actually resulted in exceeding the specified maximum target oxygen concentration. The following example is therefore a reference example: Within the measurement series, BPA-PC powder was fed into the total feed at a flow rate of 100-150 kg / h and 23-50 wt%, along with nitrogen flows in a cross-flow of 1 to 1.5 Nm³. 3 The oxygen concentration was measured at a maximum of 7.4 vol.% O2 per hour. A plausibility check based on a 4.9 vol.% O2 concentration, corresponding to a confidence interval up to 7.4% O2, yielded a Re(N2) of 508 and a theoretical N2 flow rate of 1.37 Nm³. 3 / h.

[0078] Nitrogen was added through a circular capillary with a diameter of 3 mm. At 2.0 Nm 3 The nitrogen flow is thus characterized with a Reynolds number Reinjekt of 15,720 at 1.5 Nm. 3 / h of Reinjekt = 11,790.

[0079] Example 2

[0080] A Coperion ZSK92MC twin-screw extruder with a 92 mm screw outer diameter and an L / D ratio of 36 was used. The feed consisted of a PC / SAN / ABS blend formulation comprising 74% by mass of PC and SAN granules (strand granules 3 mm long and average particle weight 22 mg), 24% of an ABS powder with a d50 of 800 pm, and 2.0% of an additive mixture of powders based on the same ABS powder with added demolding agents and stabilizers. The throughput was 2800 kg / h. The extruder inlet was rectangular, with an inlet length of 1 = 0.165 m and an inlet width of d = 0.15 m. Nitrogen was injected 45 mm above the upper screw crest at an angle of 90° to the mass feed via a supply line with an 8 mm inner diameter.For oxygen concentration measurement, gas was continuously extracted from a point centrally located above the screw head, 45 mm from the upper screw crest, and continuously fed into a Horiba PG-250 paramagnetic oxygen detector. The measurement was performed according to DIN EN 14789, with a measuring range of 0-100 vol. % O2 and an error rate of + / -1 vol. % O2. The detector was calibrated with nitrogen on the day of measurement.

[0081] The target concentration of residual oxygen in the model was conservatively set at 2.5 vol.% O2 to avoid exceeding the maximum target of 6 vol.% O2 measured. Based on this, the model derives a target Reynolds number for the inert gas of 755, corresponding to 6.1 Nm³ / h. 3 Nitrogen per hour. At a throughput of up to 2800 kg / h of the target formulation and 6.1 Nm 3 A maximum of 6.0 vol. % O2 was measured per hour of N2 addition. The nitrogen injection in the cross-flow is characterized by a coefficient of 17.979. Kinematic viscosity of nitrogen: At 18°C ​​and 1 bar ambient pressure (i.e., standard conditions), 0.000015 m 2 / s.

[0082] A forecast calculation based on 0.8 vol. % O2 target yields Re (N2) of 1260 and a nitrogen flow of 10 Nm³. 3 / h. At 10 Nm 3 / h N2 - addition, reproducibly measured 1.3-1 , 6 vol.% O2.

[0083] Example 3

[0084] A Coperion ZSK133 twin-screw extruder with a 133 mm screw outer diameter and an L / D ratio of 36 was used. The feed consisted of a PC / PET / ABS blend formulation comprising 87.1% by mass of PC and PET granules (average particle weight 22 mg), 10% of an ABS powder with a d50 of approximately 700 pm, and 2.9% of an additive mixture of powders based on a BPA-PC milled material with a d50 of 600 pm, containing demolding agents and stabilizers. The throughput was 3,800 kg / h.

[0085] The extruder inlet was rectangular, with an inlet length of 1 = 0.26 m and an inlet width of d = 0.22 m. Nitrogen was injected 45 mm above the upper screw crest at a 90° angle to the mass feed via a supply line with an 8 mm inner diameter. For oxygen concentration measurement, gas was continuously extracted from a point centrally located above the screw clevis, 45 mm from the upper screw crest, and continuously fed into a Horiba PG-250 paramagnetic oxygen detector. The measurement was performed according to DIN EN 14789, with a measuring range of 0–100 vol. % O₂ and an error rate of ±1 vol. % O₂. The measurement was calibrated with N₂ on the day of measurement.

[0086] The target concentration of residual oxygen was conservatively set at 2.5 vol.% O2 in the model to avoid exceeding the maximum target of 6 vol.% O2 measured. Based on this, the model derives a target Reynolds number of 755 for the inert gas, corresponding to approximately 9 Nm³. 3Nitrogen per hour. At throughputs up to 3,800 kg / h of the target formulation and 10 Nm 3 A maximum of 3.7 vol. % O2 was measured per hour of N2 addition. At 16 Nm 3 With N2 addition per hour, reproducible O2 concentrations of 1.7–2.2 vol.% were achieved. A forecast calculation based on a target O2 concentration of 0.8 vol.% yields a Re(N2) value of 1260 and a nitrogen flow rate of 15 Nm³ / h. 3 / h. -In (21.006) + ln(2.5 - 2.289 + 1.971 * 1)

[0087] Re => 755

[0088] -0.003

[0089] £ Injector 7

[0090] T] 0.000015 m 2 / s

[0091] Kinematic viscosity of nitrogen: At 18°C ​​and 1 bar ambient pressure (i.e., standard conditions), 0.000015 m 2 / s.

[0092] Example 4

[0093] A Krauss Maffei Extrusion ZA130 twin-screw extruder with a screw outer diameter of 139 mm and a nominal L / D ratio of 36 was used. The feed consisted of a PC / SAN / ABS blend formulation comprising 96.3% by mass of PC, SAN, and ABS granules with an average particle weight of approximately 22 mg, and 3.7% by mass of an additive mixture of powders based on an ABS powder with a d50 of 800 pm, including demolding agents and stabilizers. The throughput was 8,500 kg / h.

[0094] The extruder inlet was rectangular, with an inlet length of 1 = 0.22 m and an inlet width of d = 0.20 m. Nitrogen was supplied counter-currently through bores in the inlet housing and via a pressure superposition of the extruder stuffing box (0.5 Nm). 3The gas was blown in at a rate of 1 / h, rising at an angle of 180° to the mass feed in the inlet housing. For oxygen concentration measurement, gas was continuously extracted from a point centrally located above the screw head, 45 mm from the upper screw crest, and continuously fed into a Horiba PG-250 paramagnetic oxygen detector. The measurement was performed according to DIN EN 14789, with a measuring range of 0-100 vol. % O2 and an error rate of + / -1 vol. % O2. The detector was calibrated with N2 on the day of measurement.

[0095] Due to the use of counterflow instead of crossflow of the inert gas in this line, the predicted required Reynolds number, and thus the nitrogen prediction, varies considerably even with small variations in the target oxygen concentration. Therefore, the target concentration of residual oxygen in the model was conservatively set at 2.3 vol.% O₂ to avoid exceeding the maximum target of 6 vol.% O₂ measured. Based on this, the model derives a target Reynolds number for the inert gas of 2518, corresponding to 27.2 Nm³ / h. 3 / h nitrogen. Since, in the case of countercurrent injection, the nitrogen exits from below through the screw gaps via the entire funnel opening, no rectangle is defined in this experimental setup.

[0096] -In (21.006) + ln(2.3 - 2.289 + 1.971 * 0)

[0097] Re * A s * T 2518 * 0.044m 2 * 0.000015 m 2 / s

[0098] N2 = l = 0.22m

[0099] 0.00755m 3

[0100] - = 27.2m 3 / / is

[0101] Kinematic viscosity of nitrogen: At 18°C ​​and 1 bar ambient pressure (i.e., standard conditions), 0.000015 m 2 / s.

[0102] At a throughput of 8,500 kg / h of the target formulation and 22.5 Nm 3 A maximum of 5.5 vol. % O2 was measured per hour of N2 addition.

[0103] A comparative calculation for nitrogen addition in cross-flow under otherwise identical boundary conditions yields target Re of the inert gas of 800 and 9 Nm. 3 / h Target of the N2 injection. In comparison to Example 3 with geometrically similar conditions, where Re numbers of 800-1200 (corresponding to N2 injections of 9-15 Nm) 3Example 4 shows that the model calculation according to the invention also provides reliable results when N2 is fed in countercurrently, and also demonstrates the advantageous effect of adding inert gas in crosscurrent instead of countercurrent flow.

Claims

Patent claims 1. A method for operating an extruder, in particular for variably adjusting the oxygen content in the feed area of ​​the extruder, wherein the extruder has a feed chute for feeding a material to be extruded, which has an inlet opening at one end, opens into the extruder housing at the opposite end and in which at least one inert gas supply device is provided for supplying an inert gas stream into the feed chute, characterized in that the inert gas volume flow rate of the inert gas stream is adjusted such that the Reynolds number of the inert gas stream in the feed chute is at least 180.

2. Method according to claim 1, characterized in that the Reynolds number of the inert gas stream is Re 180 to 2000, in particular 300 to 2000, preferably 400 to 2000, particularly preferably 500 to 2000.

3. Method according to claim 1 or 2, characterized in that the Reynolds number of the inert gas stream is defined as with l = characteristic length of the filling shaft, where I is defined in the case of a rectangular filling shaft as l = characteristic length rectangular = where a and b length and width of the rectangle, in the case of a round or elliptical filling chute as l = 2 * a with a as the radius of the circle or in the case of an ellipse as the long radius, N2= volume flow of inert gas in standard liters, q = kinematic viscosity of inert gas at standard conditions (18°C and 1 bar) v middle = — as average speed in the drop shaft and ■^s As = Cross-sectional area of ​​the filling shaft at the point that is 2 to 6 times The distance of the screw diameter above the screw comb corresponds to this.

4. Method according to one of the preceding claims, characterized in that the Reynolds number of the inert gas stream Re is defined as with O2 = oxygen target concentration in vol.-%, transverse = proportion of the cross flow of the inert gas addition to the total flow of inert gas A = 2.2 to 2.8; B = 21 to 22; C = -0.003 to -0.0035 and D = -(A-0.3) to -(A+1).

5. Method according to one of the preceding claims, characterized in that the Reynolds number of the inert gas stream at the point of injection into the filling shaft is at least 3,000, in particular 3,000 to 80,000, wherein Reynolds is defined as with 4*7V2 mittel2 rr^a p = kinematic viscosity of inert gas at standard conditions (18°C and lbar), N2 = Volume flow inert gas in standard liters and d = diameter of the feed opening for N2.

6. Method according to one of the preceding claims, characterized in that the extruder has at least one screw shaft, in particular at least two screw shafts, which are preferably driven in the same direction.

7. Method according to one of the preceding claims, characterized in that the feed chute is arranged above the extruder housing and is largely vertically oriented.

8. Method according to one of the preceding claims, characterized in that at least one of the inert gas supply devices is aligned at an angle of 90 + / - 45° relative to the feed direction of the material to be extruded, preferably at an angle of 90 + / - 15°, more preferably at an angle of 90 + / - 5°.

9. Method according to one of claims 6 to 8, characterized in that at least one of the inert gas injection devices is arranged at a distance of at most three times the screw outer diameter of the extruder above the upper edge of the screw shaft.

10. Method according to claim 9, characterized in that the cross-sectional area of ​​the feed chute in the feed direction of the material to be extruded is largely constant below the inert gas supply device, wherein, when using several inert gas supply devices, the cross-sectional area of ​​the feed chute in the feed direction of the material to be extruded is largely constant below the inert gas supply device located closest to the extruder housing.

11. Method according to one of claims 3 to 10, characterized in that the cross-sectional area of ​​the feed chute at its end opening into the extruder housing is largely constant over a length of at least twice the characteristic length l.

12. Method according to one of the preceding claims, characterized in that the feed capacity of the extruder is greater than the metered flow rate of the material to be extruded.

13. Method according to one of the preceding claims, characterized in that the oxygen concentration at the inlet of the feed chute into the extruder housing is less than 10 vol.% under normal pressure, in particular at most 8 vol.%, preferably at most 7 vol.%, further preferably at most 6 vol.%, determined according to DIN EN 14789 - 2017-05.

14. Control device for variably adjusting the oxygen content in the feed area of ​​an extruder during its operation, in particular in a method according to one of claims 1 to 13, wherein the extruder has a feed chute for feeding a material to be extruded, which has an inlet opening at one end and opens into the extruder housing at the opposite end and in which at least one inert gas supply device is provided for supplying an inert gas stream into the feed chute, wherein the control device is designed such that the inert gas volume flow rate of the inert gas stream can be adjusted in such a way that the Reynolds number Re of the inert gas stream in the feed chute is at least 180, wherein the control device is preferably designed such that the Reynolds number of the inert gas stream at the point of injection into the feed chute is at least 3.000 is adjustable, in particular to 3,000 to 80,000, where relic is defined as. with 4*7V2 mittel2 rr^ap = kinematic viscosity of an inert gas under normal conditions (18°C and lbar), N2 = Volume flow inert gas in standard liters and d = diameter of the feed opening for N2.

15. Extruder with an associated control device for variable adjustment of the oxygen content according to claim 14.

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