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
  • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
  • B01J2/22—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by pressing in moulds or between rollers
• • G—PHYSICS
  • G01—MEASURING; TESTING
  • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
  • G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
  • G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
• • 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
  • G01N33/0091—Powders

Definitions

• the invention relates to a method for determining the compression factor of powders for processing with roller presses with roller diameters of 100 to 400 mm.
• Roller presses are used to compress powders to form sliver belts, which are then comminuted into granules (EP-A-0 525 135). This process is called dry granulation.
• Powder takes place between 2 counter-rotating rollers, whereby depending on the manufacturer both rollers are fixed, i.e. have a fixed roller gap, or one of the two rollers is designed to be movable, is acted upon by hydraulic force and has a variable roller gap.
• All roller presses have at least 2 press rollers and are offered with different roller dimensions depending on the manufacturer.
• the rollers are fed with powder either by gravity or by the support of a stuffing screw.
• the dry granulation process is of particular economic importance in the pharmaceutical industry for the production of granules instead of the known wet granulation processes.
• Tablets or capsules can be produced from granules produced using known methods.
• the object of the invention is to provide a method for examining a powder for its suitability for the production of granules according to the dry granulate method using roller presses on an industrial scale.
• Another object is to provide an apparatus for performing the method.
• the object is achieved according to the invention in that a rotating press roll, a die and a piston are used to measure the compression factor.
• the method according to the invention has the advantage that a predetermination for dry granulation on roller presses of all kinds is possible for the first time with a single press roller in combination with a die for very small amounts of powder. It allows the important data for a To achieve a reliable prediction of the dry granulation process with roller presses with minimal material expenditure and to keep the amount of powder required for a test as low as possible.
• the required amount was basically halved.
• a narrow press roller could be selected.
• the device according to the invention has various measuring systems.
• the resulting press force is measured with a pre-defined nip.
• the resulting nip is measured with a pre-defined pressing force.
• the rotating press roll is a groove in a displaceable die and a piston over one
• the typical feed angle is active in roller presses due to the paired arrangement of the press rollers on the left and right rollers, but is only required once for the assessment.
• the unit of measurement for the highest pressing force currently exerted on the powder is: kN / cm linear roller width. This force is applied on a theoretical line across the roller at the point where the two rollers are closest. In order to use as little powder as possible, this process uses rolls with a width of 1 cm. Wider rolls can also be used for comparative measurements, e.g. used for scale up validation.
• the counter bearing can be mounted in different positions so that press roller diameters of 100 to 400 mm from different manufacturers can be simulated.
• Fig. 1 shows the device according to the invention in cross section
• Fig. 2 shows a variant of the device according to the invention for measuring with a defined pressing force and resulting roll nip.
• a bearing block is designated by the reference numeral 1.
• a counter bearing 3 which can be mounted in different positions, is also mounted on the bearing block 1 as a fixed support for a sliding surface 10 of variable thickness.
• a die 4 is provided with a groove 5 which is wider than the press roll 2. The depth of the groove 5 is greater than an angular tangent of 20 degrees on the press roll measured from the horizontal central axis.
• a cross slide 6 running tangentially to the roll surface seals the die 4 downwards and prevents the undesired outflow of the powder before the measurement.
• the groove 5 is covered with a longitudinal slide 7.
• a stop 8 is positioned on the clamping piece 9 in its height.
• a piston 11 seals the groove 5 upwards.
• a guide part 12 prevents the piston 11 from tilting in the groove 5.
• a guide part 12 and a piston 11 are mounted on the guide rod 13.
• a tared weight 14 with a fixed pointer 15 is mounted on the upper end of the guide rod 13.
• a holder 16 stabilizes the guide rod 13 in its vertical position.
• a scale 17 makes it possible to read the respective position of the piston before and after the process and to evaluate it for the calculation. The distance measurement can also be done electronically or optically.
• a load cell 18 is mounted between the back of the counter bearing 3 and a holder 19.
• Fig. 2 the process of roller presses, which are provided with a firmly defined pressing force and a variable roller gap, is simulated.
• the displacement of the thrust bearing 3 relative to the press roll is additionally displayed and read via a pointer 20 on a scale 21.
• the distance measurement can also be done electronically or optically.
• the device can be arranged at an angle between 0 and 90 degrees from the horizontal axis so that all common roller types can be simulated.
• Loose powder i.e. The basis is the bulk volume of a powder or a powder mixture on top of that
• the matrix with the loose powder or powder is the matrix with the loose powder or powder
• Powder mixture on a calibrated ramming volumimeter with 1250 strokes according to a recognized method for determining the
• the die 4 is placed horizontally on a clean, suitable surface.
• the groove 5 opened upwards is filled with powder.
• the cross slide 6 and the longitudinal slide 7 are pushed into their guides and the piston 11 is inserted.
• the powder chamber is closed.
• the die 4 is raised and pushed onto the press roll 2 until the cross slide 6 touches the roll surface and the die lies against the counter bearing 3 on its rear closed side.
• the cross slide 6 is now removed and the die 4 is pushed downward onto the press roll 2 until the powder rests on the roll surface.
• the stop 8 of the longitudinal slide 7 will rest on the support 9.
• the position of the pointer 15 is tared against the scale 17 and the zero point is thus set.
• the feed angle can now be read from a table.
• This recoil value is generated indicated and read the pointer 15 on the ruler 17 via the piston 11, the guide rod 13
• the recoil value is added to the path of the die for the calculation of the compression factor.
• the following formula results, for example Roller path on the circumference 100 mm
• the feed angle can now be read from a table.
• the force exerted on the load cell 18 and the torque applied to the drive shaft of the press roll 2 are recorded simultaneously.
• the press force exerted directly results in a value that can be transferred to production machines, i.e.KN/cm lin.
• the torque applied gives a value that can be directly transferred to production machines if the effective width of the press rolls in cm is multiplied by the measured value. However, it makes more sense to define this value in Nm / cm roller width.
• the pressed powder dressing removed from the matrix can now be processed into granules and pressed into one or more tablets or filled into capsules.
• the powder dressing can be drilled in a separate, standardized tablet drilling apparatus at different locations according to a defined procedure.
• the values obtained provide information about the Tensile strength of the powder dressing, which in turn is comparable to a corresponding tablet hardness.
• the counter bearing 3 is mounted on a linear guide 18.
• bearing block 1 there is the invisible, motor-driven drive shaft, on which the exchangeable press roller 2 is mounted.
• the bearing block 1 is mountable in one of various positions
• Hydraulic cylinder 19 mounted as a movable support for the counter bearing 3 and the sliding surface 10.
• the die 4 is provided with a groove 5 which is wider than the press roll 2. The depth of the groove 5 is greater than an angular tangent of 20 degrees on the press roll measured from the horizontal central axis.
• a cross slide 6 running tangential to the roll surface seals the die 4 and prevents the undesired outflow of the powder before the measurement.
• the groove 5 is covered with a longitudinal slide 7.
• a stop 8 is positioned on the clamping piece 9 in its height.
• a piston 11 seals the groove 5 upwards.
• a guide part 12 prevents the piston 11 from tilting in the groove 5.
• the guide part 12 and the piston 11 are on the
• a tared weight 14 with a fixed pointer 15 is mounted on the upper end of the guide rod 13.
• a holder 16 stabilizes the guide rod 13 in its vertical position.
• a scale 17 makes it possible to read the respective position of the piston before and after the process and to evaluate it for the calculation. The distance measurement can also be done electronically or optically.
• a defined pressure is applied to the hydraulic cylinder 19; the applied force, which acts on the counter bearing, is calculated from the sum of the pressure x area of the hydraulic cylinder. In order to compact the powder, When pulling in, the force applied by the hydraulic cylinder must be overcome and the thrust bearing 3 must be moved in the linear guides. The value by which the counter bearing 3 shifts is transferred to the scale 21 via the ruler 20 and read off as the thickness of the pressed powder.
• Measuring method 1 it can both loose powder, i.e. The basis is the bulk volume of a powder or a powder mixture to be tested for compacting behavior or, according to measurement method 2, the die with the loose powder or powder mixture is precompressed on a calibrated ramming volumimeter with 1250 strokes according to a recognized method for determining the ramming oil volume.
• the die 4 For filling, the die 4 is placed horizontally on a clean, suitable surface. The groove 5 open at the top is filled with powder. After filling the powder into the groove 5 of the die 4, the cross slide 6 and the
• the distance covered on the circumference of the forward rotating press roll 2 is equal to the distance of the moving die 4 and the piston 11. This means that the total amount of powder filled has been compressed by the factor resulting from the following equation results in:
• the feed angle can now be read from a table.
• the applied pressing force KN / cm lin. was predefined as a fixed size and can be transferred directly to production machines.
• This recoil value is displayed and read on the ruler 17 via the piston 11, the guide rod 13, the pointer 15. The The recoil value is added to the path of the die for the calculation of the compression factor.
• the feed angle can now be read from a table.
• the applied pressing force KN / cm lin. was predefined as a fixed quantity, the distance traveled by the counter bearing 3 can be read off on the scale 21 as the resulting gap width and can be transferred directly to production machines.
• the torque applied to the drive shaft of the press roll 2 is recorded at the same time.
• Production machines can be transferred directly if the effective width of the press rolls in cm is multiplied by the measured value. However, it makes more sense to define this value in Nm / cm roller width.
• the pressed powder dressing removed from the die can now be further processed into granules and pressed into one or more tablets or filled into capsules. Alternatively, the powder dressing can be drilled at different points in a separate, standardized tablet drilling apparatus using a defined method. The values obtained provide information about the tensile strength of the powder dressing from a comparison table, which in turn is comparable to a corresponding tablet hardness.

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• Chemical & Material Sciences (AREA)
• Health & Medical Sciences (AREA)
• Life Sciences & Earth Sciences (AREA)
• Physics & Mathematics (AREA)
• Analytical Chemistry (AREA)
• Biochemistry (AREA)
• General Health & Medical Sciences (AREA)
• General Physics & Mathematics (AREA)
• Immunology (AREA)
• Pathology (AREA)
• Organic Chemistry (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Engineering & Computer Science (AREA)
• Food Science & Technology (AREA)
• Medicinal Chemistry (AREA)
• Medical Preparation Storing Or Oral Administration Devices (AREA)
• Glanulating (AREA)
• Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
• Battery Electrode And Active Subsutance (AREA)
• Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
• Crushing And Grinding (AREA)
• Analysing Materials By The Use Of Radiation (AREA)

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Applications Claiming Priority (2)

Publications (1)

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Citations (7)

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• 1999
  • 1999-05-14 AT AT99919015T patent/ATE273510T1/de not_active IP Right Cessation
  • 1999-05-14 JP JP2000551234A patent/JP3860413B2/ja not_active Expired - Lifetime
  • 1999-05-14 WO PCT/CH1999/000204 patent/WO1999061885A1/de not_active Ceased
  • 1999-05-14 DE DE59910214T patent/DE59910214D1/de not_active Expired - Lifetime
  • 1999-05-14 US US09/701,120 patent/US6711962B1/en not_active Expired - Fee Related
  • 1999-05-14 EP EP99919015A patent/EP1082597B1/de not_active Expired - Lifetime
  • 1999-05-14 DK DK99919015T patent/DK1082597T3/da active
  • 1999-05-14 ES ES99919015T patent/ES2226380T3/es not_active Expired - Lifetime

Patent Citations (8)

Non-Patent Citations (2)

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