EP1527329A2 - Rheometre capillaire - Google Patents

Rheometre capillaire

Info

Publication number
EP1527329A2
EP1527329A2 EP03787722A EP03787722A EP1527329A2 EP 1527329 A2 EP1527329 A2 EP 1527329A2 EP 03787722 A EP03787722 A EP 03787722A EP 03787722 A EP03787722 A EP 03787722A EP 1527329 A2 EP1527329 A2 EP 1527329A2
Authority
EP
European Patent Office
Prior art keywords
capillary rheometer
rheometer according
channel
brush
sample
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Withdrawn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
EP03787722A
Other languages
German (de)
English (en)
Inventor
Axel Goettfert
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.)
Goettfert Werkstoff-Pruefmaschinen GmbH
Original Assignee
Goettfert Werkstoff-Pruefmaschinen 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
Priority claimed from DE10239530A external-priority patent/DE10239530B4/de
Application filed by Goettfert Werkstoff-Pruefmaschinen GmbH filed Critical Goettfert Werkstoff-Pruefmaschinen GmbH
Publication of EP1527329A2 publication Critical patent/EP1527329A2/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
    • G01N11/02—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material
    • G01N11/04—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material through a restricted passage, e.g. tube, aperture
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/44—Resins; Plastics; Rubber; Leather
    • G01N33/442—Resins; Plastics
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
    • G01N2011/0006—Calibrating, controlling or cleaning viscometers

Definitions

  • the invention relates to a capillary rheometer for determining theological properties of polymer melts, in particular the viscosity, with a channel for receiving a test material, with a nozzle that closes the channel and with a die that can be positively inserted into the channel for extruding the test material through the nozzle.
  • Capillary rheometers are test devices known in practice to determine the viscosity of polymer melts in a wide range of applications, i.e. H. to be determined, in particular, at different temperatures, as occur, for example, in a melt or during extrusion.
  • ISO 11443 describes the device structure, the test procedure and the generation of the measured values in detail.
  • a test channel that can be heated and tempered is sealed at the end with a nozzle of a defined length and diameter.
  • Test material usually in the form of granules, is introduced into the test channel and melted under constant temperature conditions.
  • the polymer melt is then extruded through the die at a constant stamp feed rate using a positive test stamp.
  • the test pressure in the channel that results at different stamp speeds which corresponds in the first approximation to the pressure drop across the nozzle, is either measured directly in front of the nozzle in the channel or via a load cell located between the stamp and the drive unit.
  • the viscosity function of the polymer melt can be determined from the measured values "test pressure" and "stamp speed" and taking into account the nozzle and channel geometry.
  • the handling of the known devices is very time-consuming and labor-intensive. After each measuring process, all parts that come into contact with the melt, such as the stamp, channel and nozzle, must be cleaned manually. To do this, the nozzle that closes the duct must be removed and reinstalled. After cleaning, the sample to be examined must be introduced manually into the test channel, and only then can the actual measuring process be started.
  • the invention is based on the object of designing and developing a capillary rheometer of the type mentioned at the outset in such a way that, with a high level of operating convenience, a user is able to examine samples faster and more easily than the prior art, while maintaining the quality of the measurement results.
  • capillary rheometer of the generic type according to the invention achieves the above object by the features of claim 1.
  • a capillary rheometer is characterized by a cleaning unit with at least one brush for mechanical cleaning of the channel and / or the stamp and / or the nozzle face facing the channel.
  • the nozzle closing the channel could be integrated in a mold plate, the distance between the mold plate and the channel underside being advantageously changeable.
  • the change in the distance between the mold plate and the underside of the channel could be carried out by controlling the mold plate by means of hydraulic lifting cylinders. Under test conditions, the mold plate could then be moved into an upper end position in which it presses against the underside of the duct.
  • the maximum possible hydraulic back pressure could be 65 kN.
  • the mold plate could be moved in the vertical direction by means of the hydraulic control. This would result in the possibility of inserting brushes between the mold plate and the underside of the duct for cleaning the underside of the duct and the nozzle face facing the duct. ever Depending on the size of the distance set between the mold plate and the underside of the channel, the brushes used could have different diameters.
  • the brush could be pivoted horizontally and vertically. By swiveling the brush in the horizontal direction, the underside of the duct and the face of the nozzle could then be cleaned. The brush could then be aligned vertically and inserted into the test channel for cleaning.
  • a vertical brush system could be provided, to which one or more brushes could be assigned.
  • a drive for example an electric motor, could be provided with a drive shaft which sets the brush system in rotation via a force-transmitting means. Due to the rotation of the brush system, polymer residues located on the outer surface of the stamp are gripped and stripped by the brushes.
  • the housing can be moved vertically along the axis of the capillary rheometer, wherein a linear motor could be used as the drive.
  • a linear motor could be used as the drive.
  • the brushes grasp the stamp over its entire length, whereby a thorough cleaning of the entire surface of the stamp is achieved.
  • the brush system could of course remain unchanged in its position while the stamp is moved relative to the brush system.
  • the brushes for cleaning the outer surface of the stamp could be arranged on the inner side wall of a cylindrical housing, the diameter of which is advantageously matched to the stamp diameter such that the brushes are in constant contact with the outer surface of the stamp when the brush system rotates.
  • the brushes within the housing it would be conceivable, for example, to provide a total of three brushes, each of which is at an angular distance of 120 ° to one another.
  • one or more brushes could also be arranged on the base plate of the housing. The housing could be moved into an upper end position by means of the linear motor, so that the brushes arranged on the base plate of the housing come into contact with the end face of the stamp.
  • the brushes for cleaning the outer surface of the stamp preferably have a round shape
  • the brush for cleaning the end face of the stamp could be elongated in a particularly advantageous manner.
  • the length of the brush could correspond to the diameter of the housing, so that when the housing rotates, the entire face of the stamp is covered and cleaned by the brush.
  • the base plate of the housing could be provided with cutouts. This constructive design ensures easier disposal of the polymer residues stuck in the brushes.
  • a brush could also be arranged below the base plate of the housing, which brush could be rigidly connected to the housing.
  • the brush could advantageously be positioned on the housing axis and have a diameter such that when the housing rotates, it strips and cleans the entire inner surface of the channel. Connected to the linear drive - as already mentioned - the end face of the stamp is cleaned in the upper end position. The test channel is cleaned in the downward movement until a lower end position is reached.
  • a further brush could be provided for cleaning the end face of the nozzle integrated in the mold plate and the underside of the channel, which could be designed to be pivotable horizontally, ie perpendicular to the vertical axis of the capillary rheometer.
  • a particularly thorough cleaning effect could be achieved by rotating the brush about its own axis in addition to the horizontal pivoting movement.
  • the choice of the distance between the mold plate and the underside of the channel during the cleaning process and the dimensioning of the horizontal brush could be coordinated so that both end faces - that of the mold plate and the underside of the channel - are simultaneously gripped by the rotating brush.
  • the brushes arranged within the housing can also be designed such that they can also rotate about their own axis in addition to the movements already described above.
  • the vertical brush system and the horizontally guided brushes could be coupled on the drive side.
  • a single drive is sufficient for the rotational movement of the brushes used for stamp or channel cleaning and for the rotational movements of the horizontally guided brush for cleaning the nozzle plate with the underside of the channel.
  • the coupling could be implemented, for example, via two intermeshing bevel gears.
  • the entire cleaning unit could be pivoted so that the cleaning unit can be easily removed and the actual measuring process started after the cleaning process has been completed.
  • a horizontal swivel range of 90 - 160 ° should be sufficient to ensure the introduction of test material into the channel and an unimpeded vertical movement of the test stamp and the mold plate.
  • the horizontal and the vertical brush system could be pivotable independently of one another.
  • the cleaning unit can be controlled manually. A user could then decide on a case-by-case basis as part of a measurement process comprising several samples, depending on the degree of current contamination, whether cleaning should be carried out.
  • the possibility of actuating individual brushes for the selective cleaning of only certain areas of the capillary rheometer is also conceivable.
  • automatic cleaning could advantageously also be carried out after each individual sample examination.
  • the capillary rheometer according to the invention achieves the object mentioned at the outset by the features of patent claim 19. According to this, such a capillary rheometer is characterized by a sample loading with a sample magazine for receiving the samples and with a movable gripper arm for transporting the samples from the sample magazine into the channel.
  • the sample magazine has a total of 64 sample positions. These could, for example, be formed as recesses in a cylindrical container. This could be rotatably mounted, the sample places could be arranged in a radial manner in four concentric rings. Each beam could have a radius of curvature corresponding to the length of the gripper arm.
  • the sample transport could then proceed as follows:
  • the sample magazine is fed in such a way that the swiveling gripping arm swings over the four sample positions of a first selected beam and can therefore remove the four test materials stored there.
  • the sample magazine rotates one position so that the four samples of the next beam can be reached by the gripper arm and so on.
  • the gripper arm could, for example, be designed as a vacuum suction device.
  • the gripper arm does not bring the selected sample directly into the test channel, but first to a sample temperature control unit, in which the sample is checked to a precisely adjustable test temperature before the rheological examination is heated.
  • the sample tempering unit could have a controllable heating plate which comprises cylindrical recesses for receiving the samples.
  • the heating plate could in particular comprise four recesses which - similar to the sample locations of a beam in the sample magazine - could be at the same distance from the pivot point of the gripping arm for easy access.
  • the heating plate could advantageously cover a control range of 50 - 90 ° C. Since good temperature stabilization is essential for obtaining high-quality measured values, the heating plate could be provided with a form-fitting cover for thermal insulation.
  • Fig. 1 shows the essential parts of a schematic side view
  • FIG. 2 is a schematic side view of an embodiment of a capillary rheometer according to the invention with a cleaning unit, e
  • FIG. 3 shows a schematic top view of the cleaning unit from FIG. 2,
  • Fig. 4 in a schematic plan view of the housing of the vertical
  • FIG. 2, 5 shows a schematic top view of a sample loading of an embodiment of a capillary rheometer according to the invention.
  • FIG. 1 shows a schematic side view of an exemplary embodiment of a capillary rheometer according to the invention in the measurement state.
  • a nozzle 1 for extruding the test material is integrated in a mold plate 2, which can be moved in the vertical direction by means of hydraulic lifting cylinders 3.
  • the molding plate 2 In the measuring position shown in FIG. 1, the molding plate 2 is in an upper end position, in which it closes with a bottom surface 4 of a test channel 5 in a surface-pressing manner.
  • the material sample is introduced into the test channel 5 and extruded through the nozzle 1 through the test plunger 6, which can be moved hydraulically in the vertical direction, at a constant plunger feed rate.
  • FIG. 2 shows a schematic side view of the capillary rheometer according to the invention from FIG. 1 with a cleaning unit 7, which comprises a brush system 8, 9 guided vertically and horizontally.
  • the vertically guided brush system 8 has a cylindrical housing 10 in which a plurality of brushes 11, 12 are arranged for cleaning the stamp 6.
  • the brushes 11 for cleaning the lateral surface 14 of the stamp 6 are located on the inner side wall 13 of the housing, while the brush 12 is arranged on a base plate 16 of the housing 10 for cleaning the stamp end face 15.
  • a further brush 18 is attached to the housing axis 17 and is used to clean the test channel 5.
  • the vertical brush system 8 can be rotated around the housing axis 17 as well as moved along the housing axis 17 in the vertical direction.
  • the brushes 11 cover a larger and larger part of the lateral surface 14 of the test stamp 6 until the brush 12 finally comes into contact with the end face 15 of the stamp when the upper end position is reached.
  • the brush system 8 is moved downward, the brush 12 penetrates into the test channel 5 and removes polymer residues of the sample material which are stuck in the channel 5 by rotating the brush 12.
  • a lower end position of the brush system 8 is reached when the underside of the brush 12 has reached the underside 4 of the channel facing the nozzle 1.
  • An optimization of the cleaning process can be achieved in that the stamp - after the vertically guided brush system 8 has been brought into the position shown in FIG. 2 - is moved downwards, so that the brush 12 is also in the upper end position of the brush system 8 is still partially engaged with the test channel 5. In this way, a simultaneous cleaning of the stamp 6 and the channel 5 can be carried out on the one hand and the required stroke of the brush system 8 can be minimized on the other hand.
  • the horizontally guided brush system 8 comprises a circular rotating brush 27 which cleans both the underside 4 of the channel and the end face 19 of the nozzle.
  • the diameter of the brush 27, which is horizontally displaceable in the direction indicated by the arrows, is so matched to the distance between the underside 4 of the channel and the mold plate 2 that the underside 4 and the end face 19 of the nozzle are simultaneously gripped and cleaned by the brush.
  • FIG. 3 shows a schematic top view of the cleaning unit from FIG. 2 in a position outside the capillary rheometer. In this position, test channel 5 is freely accessible and a measuring process can be carried out without any problems.
  • FIG. 3 shows the cylindrical housing 10, in which three brushes 11 are arranged on the lateral inner wall 13 for cleaning the lateral surface 14 of the test stamp 6. The angular distance between the individual brushes 11 is 120 °. Furthermore, on the bottom plate 16 of the housing 10 there is arranged the brush 12 which is elongated for cleaning the stamp face 15 and which covers the entire diameter of the housing 10.
  • the horizontal and vertical cleaning units 8, 9 are pivotably articulated and can - independently of one another - be pivoted horizontally along the dashed circular path about a common axis of rotation 20.
  • an automatic control brings the housing 10 and the brush 27 into a position exactly above or below the test channel 5.
  • the brush 27 can also perform a cleaning-increasing movement in the horizontal direction during the cleaning process in addition to the rotational movement.
  • the entire cleaning unit is pivoted into the position shown in FIG. 3 outside the capillary rheometer, so that a next measurement can be started.
  • Fig. 4 shows a schematic plan view of the cylindrical housing 10 of the vertical brush system 8 with the three brushes 11 arranged on the inner side wall 13 and the brush 12 arranged on the base plate 16 of the housing for cleaning the stamp end face 15.
  • Base plate 16 formed recesses, which are used for easy disposal of polymer residues stuck in the brushes 11, 12.
  • FIG. 5 shows, in a schematic plan view, next to the test channel 5 and the mechanical cleaning unit 7, a sample feeder 20.
  • This comprises a sample magazine 21 formed in a cylindrical container 23 with a total of 64 sample places 22. These are in four concentric circles in a radial shape in the rotatably mounted container 23 arranged, each beam having a radius of curvature matched to the length of a gripper arm 24.
  • the gripping arm 24, which is designed as a vacuum suction device, is designed to be pivotable and, because of the special positioning of the sample locations 22, can move the four sample locations 22 of a beam with a pivoting movement along the dashed circular path shown in FIG. Another beam can be delivered to the gripping arm 24 by rotating the container 23.
  • the temperature control unit 25 which essentially comprises a controllable heating plate and a plurality of cylindrical cutouts 26 for receiving the samples, is designed and positioned in such a way that all the cutouts 26 lie on the circular path defined by the pivoting movement of the gripping arm 24.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Medicinal Chemistry (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

Rhéomètre capillaire permettant de déterminer les propriétés rhéologiques de masses fondues polymères, en particulier la viscosité, qui comporte un canal (5) destiné à recevoir une matière à tester, une buse (1) fermant le canal (5) et une matrice (6) pouvant être introduite par liaison de forme dans le canal (5), pour l'extrusion de la matière à tester par la buse (1). En vue d'une étude rapide et simple d'échantillons, ledit rhéomètre est équipé d'une unité de nettoyage (7) pourvue d'au moins une brosse (11, 12, 18, 27) destinée au nettoyage mécanique du canal (5) et / ou de la matrice (6) et / ou de la face (19) de la buse orientée vers le canal (5). La présente invention concerne en outre un rhéomètre capillaire pourvu d'un système de transfert (20) d'échantillons possédant un magasin (21) destiné à recevoir les échantillons et un bras de saisie (24) mobile destiné au transport des échantillons du magasin (21) dans le canal (5).
EP03787722A 2002-08-01 2003-07-23 Rheometre capillaire Withdrawn EP1527329A2 (fr)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
DE10235335 2002-08-01
DE10235335 2002-08-01
DE10239530 2002-08-23
DE10239530A DE10239530B4 (de) 2002-08-01 2002-08-23 Kapillarrheometer
PCT/DE2003/002475 WO2004017049A2 (fr) 2002-08-01 2003-07-23 Rheometre capillaire

Publications (1)

Publication Number Publication Date
EP1527329A2 true EP1527329A2 (fr) 2005-05-04

Family

ID=31889091

Family Applications (1)

Application Number Title Priority Date Filing Date
EP03787722A Withdrawn EP1527329A2 (fr) 2002-08-01 2003-07-23 Rheometre capillaire

Country Status (3)

Country Link
EP (1) EP1527329A2 (fr)
AU (1) AU2003264236A1 (fr)
WO (1) WO2004017049A2 (fr)

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CZ304382B6 (cs) * 2008-11-07 2014-04-09 Univerzita Tomáše Bati ve Zlíně Vytlačovací hlava s inertní kapilárou s nulovou délkou
CN103257092B (zh) * 2011-12-27 2015-02-25 常州大学 竖直型双向挤出毛细管流变仪
CN103115848B (zh) * 2011-12-27 2015-02-25 常州大学 双向挤出毛细管流变仪
CN103149127B (zh) * 2011-12-27 2015-01-14 常州大学 一种双向挤出毛细管流变仪
CN102519839B (zh) * 2011-12-27 2013-09-25 常州大学 双向挤出毛细管流变仪及并联式双向挤出毛细管流变仪
CN103207132B (zh) * 2011-12-27 2015-02-25 常州大学 水平型双向挤出毛细管流变仪
CN103115847B (zh) * 2011-12-27 2015-04-15 常州大学 双向挤出毛细管流变仪
CN103257093B (zh) * 2011-12-27 2015-01-14 常州大学 双向挤出毛细管流变仪
CN102539804B (zh) * 2012-02-03 2013-12-11 上海诺甲仪器仪表有限公司 用于无转子流变仪试样的自动化加载和卸载装置
DE102019129117A1 (de) * 2019-10-29 2021-04-29 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Vorrichtung zum Analysieren eines Fluids sowie Verfahren zum Analysieren eines Fluids

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0278683B1 (fr) * 1987-02-10 1992-07-08 Sumitomo Chemical Company, Limited Dispositif automatique de nettoyage pour un plastomètre à extrusion pour matériaux thermoplastiques
US4882930A (en) * 1988-06-17 1989-11-28 Automatik Machinery Corporation Melt indexer system with robot operation
DE3922835A1 (de) * 1989-07-11 1991-01-24 Hench Automatik App Masch Verfahren zur messung der fliesseigenschaften von fliessfaehigen medien
EP0488646B1 (fr) * 1990-11-27 1997-07-23 Sumitomo Chemical Company Limited Dispositif pour tester l'écoulement de thermoplastiques, et méthode de découpage des fils
GB9408341D0 (en) * 1994-04-27 1994-06-15 Rosand Precision Ltd Improvements in and relating to rheology

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO2004017049A3 *

Also Published As

Publication number Publication date
AU2003264236A1 (en) 2004-03-03
WO2004017049A2 (fr) 2004-02-26
AU2003264236A8 (en) 2004-03-03
WO2004017049A3 (fr) 2004-09-30

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