US20040113300A1 - Method and device for producing spherical particles from a polymer melt - Google Patents

Method and device for producing spherical particles from a polymer melt Download PDF

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Publication number
US20040113300A1
US20040113300A1 US10/356,330 US35633003A US2004113300A1 US 20040113300 A1 US20040113300 A1 US 20040113300A1 US 35633003 A US35633003 A US 35633003A US 2004113300 A1 US2004113300 A1 US 2004113300A1
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Prior art keywords
air
loop
fall tower
supplied
droplets
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Abandoned
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US10/356,330
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English (en)
Inventor
Theodor Jurgens
Rudolf Geier
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Buehler AG
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Buehler AG
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Assigned to TESSAG INDUSTRIE-ANLAGEN GMBH reassignment TESSAG INDUSTRIE-ANLAGEN GMBH ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: JURGENS, THEODOR
Publication of US20040113300A1 publication Critical patent/US20040113300A1/en
Assigned to BUHLER AG reassignment BUHLER AG CORRECTIVE ASSIGNMENT TO CORRECT RECEIVING PARTY RECORDED OCTOBER 17, 2003 AT REEL 014611, FRAME 0831. Assignors: JURGENS, THEODOR
Priority to US11/085,929 priority Critical patent/US7208107B2/en
Abandoned legal-status Critical Current

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    • 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
    • B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
    • B01J2/04—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a gaseous medium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00—Making granules
    • B29B9/10—Making granules by moulding the material, i.e. treating it in the molten state
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00—Making granules
    • B29B9/16—Auxiliary treatment of granules
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00—Making granules
    • B29B9/16—Auxiliary treatment of granules
    • B29B2009/165—Crystallizing granules
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00—Making granules
    • B29B9/16—Auxiliary treatment of granules
    • B29B2009/166—Deforming granules to give a special form, e.g. spheroidizing, rounding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2791/00—Shaping characteristics in general
    • B29C2791/004—Shaping under special conditions
    • B29C2791/008—Using vibrations during moulding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2067/00—Use of polyesters or derivatives thereof, as moulding material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2067/00—Use of polyesters or derivatives thereof, as moulding material
    • B29K2067/006—PBT, i.e. polybutylene terephthalate

Definitions

  • the present invention relates to a method of producing spherical particles from a prepolymer and/or polymer melt, particularly made of polyfunctional carboxylic acids and alcohols, such as PET or PBT particles, the polymer melt being dripped into droplets using a drip nozzle, the droplets having a gas applied to them in counterflow in a fall tower for at least partial crystallization, and the droplets then preferably being transported to a polycondensation stage.
  • the present invention relates to a device for producing spherical particles from a prepolymer and/or polymer, particularly made of polyfunctional carboxylic acids and alcohols, such as PET or PBT particles, including at least one nozzle device which drips molten prepolymer and/or polymer, a fall tower downstream thereto, which is positioned in a gas loop via at least one gas intake opening at the floor and at least one gas outlet opening at the nozzle device, a transport device positioned in the fall tower for particles which are at least precrystallized in the fall tower, and a crystallization stage downstream from the transport device.
  • a device for producing spherical particles from a prepolymer and/or polymer particularly made of polyfunctional carboxylic acids and alcohols, such as PET or PBT particles
  • at least one nozzle device which drips molten prepolymer and/or polymer
  • a fall tower downstream thereto which is positioned in a gas loop via at least one gas intake opening at the floor and at least one gas
  • the present invention is based on the problem of refining a method and the device of the type initially cited in such a way that spheres, made of polymers, having a desired size and uniform geometry may be produced at a large scale. Simultaneously, the production of the particles is to be energetically more favorable and have a simpler facility and therefore be more cost-effective. Furthermore, more rapid melting of the spheres is to be possible.
  • the problem is solved by a method of the type initially cited essentially in that the prepolymer and/or polymer melt is dripped, by a nozzle plate excited into vibration and/or by exciting vibrations of the prepolymer and/or polymer melt itself, into droplets, which have air applied to them as the gas in counterflow, the air being supplied to the fall tower at a temperature such that the air is heated to at most a temperature T 1 of T 1 ⁇ 160° C. through heat transfer from the droplets.
  • the air is particularly supplied at a temperature T 2 of T 2 ⁇ 150° C., particularly T 2 ⁇ 110°.
  • the air is to be heated to at most a temperature T 1 of T 1 ⁇ 140° C.
  • air is supplied at a temperature T 2 of T 2 ⁇ 130° C., particularly T 2 ⁇ 80° C.
  • the air is preferably supplied to the fall tower at a temperature T 1 which lies above the glass transition point of the polymer to be dripped.
  • the air is introduced in the lower region of the fall tower, particularly in the floor region, in such a way that air flows against the droplets in the lower region of the fall tower at a higher speed than in the upper region.
  • the air intake temperature is to be set in such a way that oxidative damage of the dripped polymer is avoided and sufficient solidification and/or precrystallization is provided.
  • the air entering the fall tower may absorb reaction substances such as ethylene glycol and/or butane diol or water to a sufficient extent, the air is to have a low dew point upon entering the fall tower, preferably in the range between ⁇ 10° C. and ⁇ 40° C.
  • a refinement of the present invention provides that a portion—approximately 10%-30%—of the air flowing through the loop is removed and supplied to a spray loop, in which the reaction products are removed.
  • fresh and cold ethylene glycol and/or butane diol are sprayed in the purification loop, through which reaction substances such as ethylene glycol and/or butane diol, oligomers, and water, which are diffused in the dry air, condense out of the air loop and may be reused as valuable raw materials, for example, the ethylene glycol and/or butane diol for esterification for the process using TPA and/or for reesterification for a process using DMT.
  • the air purified in this way retains its low dew point and may again be supplied to the loop flowing through the fall tower.
  • acetaldehyde and/or THF tetrahydrofuran
  • a quantity of the intake air charged with acetaldehyde is mixed into a heat transfer facility such as a furnace and thus combusted.
  • the combusted quantity of air is constantly, particularly continuously, replaced by an equal quantity of air. In this way, the need for combustibles such as heating gas and/or oil is reduced.
  • a downstream precrystallization stage which is particularly important in the processing of comonomers and which is also operated using dry air, may also be included in the purification loop.
  • the prepolymer and/or polymer melt may be excited into vibration and dripped using a vibration generator, for example.
  • the fall tower has a cross-section, particularly a diameter, which is significantly larger than the nozzle plate in regard to an area, essentially the circular area on which the outlet openings for dripping the prepolymer and/or polymer melt are positioned.
  • the inner wall of the fall tower is to be made of a material and/or be coated with a material which prevents and/or hinders adhesion of droplets. Teflon® is an example of a suitable material.
  • baffles in the fall tower In order to additionally increase the dwell time of the droplets, which are formed in a spherical shape, an increase of the air speed is caused by baffles in the fall tower.
  • the baffles lead to a change in cross-section of the fall tower and therefore to a corresponding change of the air speed.
  • the particles are guided via a surface, which has openings, to a separating device such as an oversize separator, in which possible agglomerates are sorted out and supplied to the starting melt and/or its pre-products. Since the corresponding agglomerated particles still have a slight viscosity, rapid and good dissolving in a precondensation stage is possible.
  • a separating device such as an oversize separator
  • the surface leading to the oversize separator which may be implemented as a sieve or a perforated metal sheet or as a wind sifter, among other things, that hot air flows through it, the air speed being selected in such a way that the particles float and oscillate over the surface and/or its openings. This prevents the particles from being able to agglutinate. In addition, the dwell time, during which the particles have air applied to them, is increased.
  • the particles may be supplied to a crystallizer, which is also operated using dry air guided in a loop. Reaction substances enriched in the air may then be separated in a spray loop in the way previously described and/or non-separable substances may be supplied to a heat transfer device.
  • a facility for producing spherical particles from a polymer melt, particularly made of polyfunctional carboxylic acids and alcohols, such as PET or PBT particles, of the type initially described is distinguished in that the nozzle device has a nozzle plate set into vibration and/or a nozzle plate having a vibration generator acting directly on the melt, with nozzles which are distributed on a circular area having a diameter D d , and the fall tower is positioned in the loop which guides the air and has a diameter D f which is at least twice as large as the diameter D d .
  • the ratio of the diameter of the active area of the nozzle plate to the fall tower is particularly 1:2 to 1:10, particularly approximately 1:5.5.
  • the fall tower is lined on the inside using an anti-adhesive material or has such a material. The material is particularly Teflon®.
  • the fall tower has baffles which change the cross-section of the fall tower in the region of the air intake opening.
  • baffles may be, for example, conical or pyramidal stumps, which are coated on the outside with Teflon® or another suitable material which prevents adhesion.
  • the air outlet opening itself is positioned at a distance to the nozzle plate such that the particles dripped from the nozzle plate are subjected to an essentially laminar air flow directly after they exit the nozzle plate.
  • a slanted surface such as a sieve or perforated plate, which has openings, is provided, which has dry air flowing through it in such a way that the particles may be moved floating and/or oscillating along the surface, at least in the region of the openings.
  • the surface having the openings itself leads to an oversize separator, to which a crystallization stage operated using dry air is connected downstream.
  • Particle agglomerates separated in the oversize separator may be resupplied to the process via a line leading to the precondensation stage upstream from the nozzle plate.
  • the device includes a purification stage having a spray loop, which is connected to the first air loop, which includes the fall tower, and/or a second air loop, which includes the crystallization stage. Furthermore, connections originate from the purification stage to one of the esterification and/or reesterification stages before the precondensation stage and to a combustion device.
  • the polyester condensate has a product temperature between 210° C. and 240° C. and an intrinsic viscosity from 0.3 to 0.6.
  • the nozzle plate 18 may be set into vibration and particularly has outlet openings arranged in concentric circles, which have an area having a diameter D d of, for example, 300 mm.
  • the nozzle plate 18 having the openings and/or nozzles may be inserted elastically in a holder, the nozzle plate itself being connected to a vibration exciter.
  • the vibration exciter which is to be an electromagnetic vibration exciter, is based on a load-bearing structure, in order to be able to vibrate the nozzle plate.
  • Frequencies at which the nozzle plate may be set into vibration may lie in the range between 200 and 2000 Hz.
  • the diameter of the openings and/or nozzles is to lie in the range between 0.2 and 0.8 mm.
  • the polyester precondensate is to be supplied to the nozzle plate 18 at an overpressure of, for temple, 0.2 to 1.0 bar.
  • the nozzle plate 18 is also uniformly heated, a temperature in the magnitude between 220 and 250°—for PBT between 190° C. and 220° C.—particularly being selected.
  • the melt may be excited to vibration using a vibration exciter for dripping.
  • the nozzle plate 18 By setting the nozzle plate 18 into vibration, it is ensured that the molten prepolymer is uniformly dripped in identically large and identically shaped particles and a fall tower 20 , which is equivalent to a Prill tower.
  • the length of the fall tower 20 may lie in the range between 10 and 30 meters, particularly in the range of 20 meters. Of course, tower heights of more than 30 meters are also technically possible.
  • the fall tower 20 is to have a diameter of 1600 mm.
  • the fall tower 20 is to be lined on the inside with an anti-adhesive agent, particularly Teflon®, and/or be made of this material, in order to ensure that droplets leaving the nozzle plate 18 are not able to adhere.
  • the droplets in the fall tower 20 fall in an essentially laminar portion of an air flow, which runs in counterflow to the falling direction of the droplets, directly after leaving the nozzle plate 18 .
  • This air counterflow is used for further solidification of the spheres and their precrystallization, the flow speed of the particles which are falling and/or floating downward being adjusted as a function of their diameter.
  • baffles 26 of conical or conical stump geometry, for example, which change the cross-section, located in the floor region of the fall tower 20 , through which the flow speed in the floor region of the fall tower 20 is increased in comparison to the head region, with the consequence that the dwell time of the droplets reaching the floor region, which are precrystallized and/or prehardened, is increased.
  • the airspeed in the floor region may be set to a speed between 3 and 7 m per second.
  • the baffles 26 themselves are to at least have an anti-adhesive material such as Teflon® on the outside or be made of such a material.
  • the air flowing in via the air intake openings 22 , 24 in the floor region, which flows against the falling particles, has a starting temperature between 80° C. and 16° C.—for PBT between 60° C. and 120° C.—the air temperature in the intake to lie above the glass transition point of the precondensate (approximately 70° C.-80° C. for PET and 35° C.-50° C. for PBT).
  • a temperature of 160° C. for PET and/or 120° C. for PBT is not, however, to be exceeded, in order to avoid oxidative damage to the particles, adequate solidification and/or precrystallization nonetheless to be ensured simultaneously.
  • the entering air is also to have a low dew point upon entering the fall tower 20 , preferably between ⁇ 10° C. and ⁇ 40° C., for absorbing ethylene glycol, water, etc.
  • a slanted surface 30 in the form of a sieve or a perforated metal sheet, for example, which has passages 28 , runs in the floor region of the fall tower 20 .
  • One of the air intake openings in the exemplary embodiment the air intake opening 24 , discharges into the space between the floor 32 of the fall tower 20 and the slanted surface 30 .
  • the speed of the dry air 24 flowing through the openings 28 is selected so that the particles reaching the floor 30 float and/or oscillate at least in the region of the openings 28 . These measures also hinder agglutination of particles. Simultaneously, the dwell time of the particles in the fall tower 20 through which the air flows is increased.
  • the particles and/or pellets reach an oversize separator 34 , through which the agglomerates are separated from the particles, in order to be resupplied to the precondensation stage 14 via a line 36 . Due to the slight viscosity which they still have, possibly occurring agglomerates may be dissolved without problems in the precondensation stage 14 and may thus be resupplied to the process.
  • the pellets are supplied to a crystallization stage 38 , which is also operated using dry air, from the oversize separator 34 and/or its funnel-shaped floor region 36 . From the crystallization stage 38 , the particles may reach a typical SSP polycondensation stage, which is particularly operated under partial vacuum.
  • the air permeating the fall tower 20 is conveyed in a—first-loop 40 , the intake openings 22 , 24 having flaps 42 , 44 connected upstream for air quantity regulation. Furthermore, there is a fan 46 before the control flaps 42 , 44 .
  • reaction products such as ethylene glycol and/or butane diol, water, oligomers, or acetaldehyde and/or tetrahydrofuran, which arise from the dripped precondensate and/or molten prepolymer.
  • reaction products such as ethylene glycol and/or butane diol, water, oligomers, or acetaldehyde and/or tetrahydrofuran, which arise from the dripped precondensate and/or molten prepolymer.
  • a portion from the loop 40 is supplied via a line 48 to a—second-loop 50 , a spray loop, which includes a spray condenser 52 , in which fresh and cold ethylene glycol and/or butane diol, which is supplied via a line 54 , is sprayed via a spray device 56 .
  • reaction substances such as ethylene glycol, butane diol, oligomers, water, etc.
  • reaction substances such as ethylene glycol, butane diol, oligomers, water, etc.
  • a heat exchanger 60 in the loop 50 , through which the temperature of the air flowing through the loop 50 may be adjusted optimally.
  • pump 62 to convey the loop liquid itself.
  • the proportion of air transferred out of the first loop 40 is preferably between 10 % and 30 %.
  • the air which leads the spray loop 50 via a line 64 is purified and has a low dew point and may be supplied to the loop 40 flowing through the fall tower 20 via a line 66 . Due to the low temperature of the air leaving the spray loop 50 via the line 66 and its low dew point, the temperature in the loop 50 is adjusted to a desired intake temperature in the floor region of the fall tower 20 .
  • acetaldehyde and/or THF tetrahydrofuran
  • small quantities of air are supplied to the first loop 40 via a connection 68 .
  • An identical quantity of air is removed from a line 64 , which connects the spray loop 50 with the loop 40 of the fall tower 20 and/or a third loop 70 including the precrystallization stage 38 , via a connection 72 , in order to be mixed into a heat transfer facility for the purpose of combustion, through which the requirement for external energy such as heating gas and/or oil may be reduced.
  • the precrystallization stage 38 which is particularly necessary for the processing of comonomers, also includes a loop 70 , in which dry air is conveyed using a fan 74 .
  • the air flowing in the loop 70 may also be heated to the desired extent via a heating device 76 .
  • the loop 70 is connected via a line 78 to the spray loop 50 , in order to be able to condense out reaction substances with which the circulating air is enriched and resupply them to the esterification and/or reesterification process.
  • a quantity of air, having a low dew point, corresponding to the quantity of air removed via the line 78 is resupplied via the line 64 to the loop 70 .
  • reaction substances from the loop 70 is advantageous for economic reasons alone, since due to their relatively low intrinsic viscosities, a relatively large amount of ethylene glycol and/or butane diol is still in the air loop 70 , so that, as mentioned, condensing out ethylene glycol and/or butane diol and returning them to the esterification and/or reesterification stage 12 suggests itself.
  • the following is to be noted in regard to the temperatures of the particles and/or the air loops permeating the fall tower 20 .
  • the particles leave the nozzle plate at the temperature of approximately 230° for the PET process and/or 190° for the PBT process and reach a temperature of approximately 180° in the middle region of the fall tower 20 .
  • a temperature of approximately 160° C. for the PET process and/or 130° C. for the PBT process exists in the oversize separator 34 .
  • the quantity and temperature of air entering the fall tower 20 via the intake openings 22 , 24 is adjusted according to the throughput.
  • the air removed from outlet opening 27 has a temperature of approximately ⁇ 160° C. for a PET process and ⁇ 130° C. for a PBT process.
  • the air is cooled to approximately 20° and is supplied at this temperature to both the first loop 40 and the second 70 .
  • the air supplied underneath the slanted surface 30 which exercises the function of a fluidized bed, via the intake opening 24 is to be supplied at a temperature at which the crystallization speed for the pellets to be produced is optimal. This means approximately 160° C. for the production of PET spheres and ⁇ 130° C. for PBT pellets.
  • the air supplied via the opening 22 above the surface 30 is to be below the temperatures indicated previously, since it is heated through heat transfer from the falling droplets as it flows through the tower 20 .
  • a connection 67 leads from the line 64 , which comes from the spray loop 50 , to the tower, via which purified air of relatively low temperature (approximately 20-30° C.) is introduced directly into the tower 20 , through which the temperature of air flowing through the tower 20 is reduced overall. Therefore, air of a desired relatively high temperature may be supplied in the region of the fluidized bed 30 , without the optimum crystallization temperature being exceeded inside the tower 20 , since cooler air is mixed in via the line 67 , as described.
  • Spherical pellets which lie in a narrow grain spectrum may be produced.
  • Spherical pellets having a diameter of 0.8 millimeters may be obtained at a nozzle diameter of 0.5 mm, a nozzle plate frequency of 1000-2000 Hz, and a fall height of 20 meters.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Polyesters Or Polycarbonates (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
US10/356,330 2000-08-29 2003-01-31 Method and device for producing spherical particles from a polymer melt Abandoned US20040113300A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US11/085,929 US7208107B2 (en) 2000-08-29 2005-03-21 Method and device for producing spherical particles from a polymer melt

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10042476A DE10042476A1 (de) 2000-08-29 2000-08-29 Verfahren und Vorrichtung zum Herstellen kugelförmiger Partikel aus einer Polymerschmelze
DE10042476.7 2000-08-29
PCT/EP2001/000518 WO2002018113A1 (de) 2000-08-29 2001-01-18 Verfahren und vorrichtung zum herstellen kugelförmiger partikel aus einer polymerschmelze

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US11/085,929 Expired - Fee Related US7208107B2 (en) 2000-08-29 2005-03-21 Method and device for producing spherical particles from a polymer melt

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US (2) US20040113300A1 (de)
EP (1) EP1313599B1 (de)
JP (1) JP2004514571A (de)
KR (1) KR20030027102A (de)
CN (1) CN1450950A (de)
AT (1) ATE423662T1 (de)
AU (1) AU2001226782A1 (de)
BR (1) BR0113694A (de)
DE (2) DE10042476A1 (de)
EA (1) EA007520B1 (de)
MX (1) MXPA03001809A (de)
TW (1) TW200413148A (de)
WO (1) WO2002018113A1 (de)
ZA (1) ZA200300697B (de)

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US20050065315A1 (en) * 2003-09-19 2005-03-24 Bonner Richard Gill Process for heating PET pellet feed to a solid stating process by heat exchange with hot solid stated pellets
US20100289166A1 (en) * 2008-01-16 2010-11-18 Automatik Plastics Machinery Gmbh Drop pelletizing device and method for the operation thereof
US20180238664A1 (en) * 2015-11-03 2018-08-23 Jinagbo CHEN Cold firework spurting apparatus
US10852105B1 (en) * 2017-11-22 2020-12-01 Zhou Xiaowen Machine for discharging a waterfall of low temperature sparks
US10948271B1 (en) * 2017-07-18 2021-03-16 Zhou Xiaowen Cold fireworks

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DE10204954A1 (de) * 2001-12-11 2003-06-18 Buehler Ag Verfahren und Vorrichtung zum Herstellen kugelförmiger Partikel aus einer Schmelze aus Kunststoff
DE10259694A1 (de) * 2002-12-18 2004-07-01 Bühler AG Herstellung eines Polyester-Performs mit reduziertem Acetaldehydgehalt
DE10328637A1 (de) * 2003-01-23 2004-12-16 Zimmer Ag Verfahren zur Zugabe der Rohstoffe bei der Herstellung von Polyestern oder Copolyestern
DE102004010680A1 (de) 2004-03-04 2005-10-06 Zimmer Ag Verfahren zur Herstellung von hochkondensierten Polyestern in der festen Phase
DE102006012587B4 (de) 2006-03-16 2015-10-29 Lurgi Zimmer Gmbh Verfahren und Vorrichtung zur Kristallisation von Polyestermaterial
EP2046863A2 (de) * 2006-05-04 2009-04-15 Uhde Inventa-Fischer AG Verfahren zur kontinuierlichen herstellung von polyamid-granulat
US7638593B2 (en) * 2006-05-24 2009-12-29 Eastman Chemical Company Crystallizer temperature control via fluid control
US7638076B2 (en) * 2007-10-26 2009-12-29 Martin Resource Management Corporation Method and system for pelletizing sulfur
DE102007055242A1 (de) * 2007-11-16 2009-05-20 Bühler AG Verfahren zur Kristallisation von kristallisierbaren Polymeren mit hoher Klebeneigung
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DE50114730D1 (de) 2009-04-09
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ATE423662T1 (de) 2009-03-15
EP1313599A1 (de) 2003-05-28
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BR0113694A (pt) 2003-07-22
ZA200300697B (en) 2003-10-01
EA007520B1 (ru) 2006-10-27
KR20030027102A (ko) 2003-04-03
CN1450950A (zh) 2003-10-22
MXPA03001809A (es) 2003-06-04
US7208107B2 (en) 2007-04-24
AU2001226782A1 (en) 2002-03-13

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