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WO2004056545A1 - A method for manufacturing products made of rigid and plasticised pvc, in particular tubes, section bars, cables and calendered elements - Google Patents

A method for manufacturing products made of rigid and plasticised pvc, in particular tubes, section bars, cables and calendered elements

Info

Publication number
WO2004056545A1
WO2004056545A1 PCT/EP2003/013957 EP0313957W WO2004056545A1 WO 2004056545 A1 WO2004056545 A1 WO 2004056545A1 EP 0313957 W EP0313957 W EP 0313957W WO 2004056545 A1 WO2004056545 A1 WO 2004056545A1
Authority
WO
Grant status
Application
Patent type
Prior art keywords
continuous
pvc
mixer
method
blend
Prior art date
Application number
PCT/EP2003/013957
Other languages
French (fr)
Other versions
WO2004056545B1 (en )
WO2004056545A8 (en )
Inventor
Franco Lico
Original Assignee
Lico S.P.A.
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

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE, IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00Mixing; Kneading
    • B29B7/002Methods
    • B29B7/007Methods for continuous mixing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE, IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00Mixing; Kneading
    • B29B7/30Mixing; Kneading continuous, with mechanical mixing or kneading devices
    • B29B7/58Component parts, details or accessories; Auxiliary operations
    • B29B7/60Component parts, details or accessories; Auxiliary operations for feeding, e.g. end guides for the incoming material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE, IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C47/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C47/08Component parts, details or accessories; Auxiliary operations
    • B29C47/10Feeding the material to the extruder
    • B29C47/1018Raw material pre-treatment while feeding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE, IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C47/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C47/08Component parts, details or accessories; Auxiliary operations
    • B29C47/10Feeding the material to the extruder
    • B29C47/1063Feeding the material to the extruder in liquid form
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE, IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C47/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C47/08Component parts, details or accessories; Auxiliary operations
    • B29C47/36Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C47/365Multi stage plasticisers, homogenisers or feeders
    • B29C47/366Multi stage plasticisers, homogenisers or feeders using a first screw extruder and a second screw extruder
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE, IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C31/00Handling, e.g. feeding of the material to be shaped, storage of plastics material before moulding; Automation, i.e. automated handling lines in plastics processing plants, e.g. using manipulators or robots
    • B29C31/02Dispensing from vessels, e.g. hoppers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE, IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C47/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C47/0009Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the articles
    • B29C47/0019Flat rigid articles, e.g. panels, plates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE, IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C47/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C47/0009Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the articles
    • B29C47/0021Flat flexible articles, e.g. sheets, foils or films
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE, IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C47/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C47/0009Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the articles
    • B29C47/0023Hollow rigid articles having only one tubular passage
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE, IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C47/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C47/0009Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the articles
    • B29C47/0026Hollow flexible articles, e.g. blown foils or films
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE, IN GENERAL
    • B29KINDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS
    • B29K2027/00Use of polyvinylhalogenides or derivatives thereof as moulding material
    • B29K2027/06PVC, i.e. polyvinylchloride
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE, IN GENERAL
    • B29KINDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS
    • B29K2105/00Condition, form or state of moulded material or of the material to be shaped
    • B29K2105/0005Condition, form or state of moulded material or of the material to be shaped containing compounding ingredients
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE, IN GENERAL
    • B29KINDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS
    • B29K2105/00Condition, form or state of moulded material or of the material to be shaped
    • B29K2105/0005Condition, form or state of moulded material or of the material to be shaped containing compounding ingredients
    • B29K2105/0038Plasticisers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE, IN GENERAL
    • B29KINDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS
    • B29K2105/00Condition, form or state of moulded material or of the material to be shaped
    • B29K2105/0005Condition, form or state of moulded material or of the material to be shaped containing compounding ingredients
    • B29K2105/0044Stabilisers, e.g. against oxydation, light, heat
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE, IN GENERAL
    • B29LINDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
    • B29L2023/00Tubular articles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE, IN GENERAL
    • B29LINDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
    • B29L2031/00Other particular articles
    • B29L2031/707Cables, i.e. two or more filaments combined together, e.g. ropes, cords, strings, yarns

Abstract

The invention refers to a method for manufacturing products made of rigid and plasticised PVC, in particular tubes, section bars, cables and hot rolled elements, where the method is articulated in a single passage, completely continuous with two possible outcomes depending on whether it is applied to extrusion or calendering processes.

Description

Method for manufacturing products made of rigid and plastic PVC, in particular tubes, section bars, cables and calendered elements

The preparation of PVC mixtures with continuous process has for decades been a pressing problem for those who deal with this polymer. Different solutions have been proposed in the past, but none of them has been able to find widespread industrial use.

More than any other thermoplastic polymer, PVC resin requires a very accurate statistical distribution of the individual components such as plasticiser, stabiliser, lubricator, modifier and pigment in their polymeric matrix, before starting the thermal process of gelling. The good pre-dispersion of these components, therefore, is the primary condition to obtain a good final compound or extruded product.

To date, this step in PVC transformation is achieved solely by discontinuous processes, based on hot/cold rapid mixers or on slow heated mixers.

State of the art (Fig. 1 )

Depending on the final outcome of the production process, tubes, section bars, cables, calendered elements, the traditional method comprises different steps within a discontinuous process.

A. Dry-blend preparation

The raw materials, solid (resins, stabilising charges, additives) and liquid (plasticisers, stabilisers etc.), stored separately (1 ), are proportioned "in charges" (2): volumetrically, on one or more batch scales; individually in gravimetric fashion inside the mixer. The slow-speed or high-speed mixer (3) is always heated to a variable temperature and it serves the purpose of mixing all agents to the PVC resin. It will work the material loaded by the proportioning devices for a given residence and process period, to be subsequently emptied of the mixture and re-start the cycle receiving the raw material from weighing. The mixture, called dry-blend, moves to a cooler (4) which brings it to the correct temperature for the following process.

B. Intermediate granulation

The dry-blend moves from the cooler to a volumetric or gravimetric proportioning device (5) which will feed the compounder for granulation (6). The PVC granule is then transferred to the intermediate storage sites or to be sacked.

C. Cable extrusion

The PVC granule is transported from storage to a pre-heater (8), wherefrom the extruder of the cable (9) is fed by gravity, to increase its productivity.

D. Tube or section bar extrusion

This extrusion process can take place using PVC compounded in granules (see process C) or stored dry-blend (10) at the output of the cooler. From storage, the dry-blend is transported onto the extrusion line, proportioned in volumetric or gravimetric fashion (11) inside the continuous extruder (12) to produce a tube or section bar.

E. Calendering:

The dry-blend is proportioned in volumetric or gravimetric fashion (13) inside a continuous mixer (14) which directly feeds the calender (15) without granulating the PVC.

The task of the invention is to obtain a continuous method for manufacturing products made of rigid or plasticised PVC, in particular tubes, pipes, section bars, cables.

The method described herein comprises a single passage, completely continuous, but with two possible outcomes depending on whether it is applied to extrusion processes (tubes, section bars, cables) or calendering processes (wires, plates, etc.). it starts from the separate storage of the raw materials (1 ), which can be proportioned (2) according to two different methods:

- continuous volumetric or gravimetric proportioning of a pre-blend of solids (powders, granules, ground, compacted material and all kinds of grain size) and a pre-blend of liquids, distinctly fed inside the Continuous Turbo Mixer (Figure 2),

- continuous, volumetric or gravimetric but separate proportioning (Figure 3) of each individual solid or liquid material (however, compatible liquids can be pre-mixed).

Solids and liquids feed in two separate and distinct flows the Continuous Turbo Mixer (3) which disperses and diffuses all solid and liquid agents on the PVC resin and mixes them with the charges. Inside the mixer there is a constant and homogeneous flow of raw materials which, in their path towards the discharge point, are accurately mixed. What distinguishes and elevates the Continuous Turbo Mixer to the ideal machine for blends that are sensitive to shear and temperature, such as the dry blends of rigid or plasticised PVC, is the possibility of working the materials without transferring energy by mechanical friction and hence without inducing an uncontrolled rise in temperature. The absence of friction on the material to be blended will also prevent the formation of agglomerates (from additives, stabilisers and low-melting point products) in the dry blend, which comprise the quality of the final product.

The Continuous Turbo Mixer may be heated or cooled depending on the formulation.

Depending on the final product, the output of the Continuous Turbo Mixer may directly feed a continuous extruder (4) for the production of tubes, section bars or cables, or a calender (5) for the production of films, sheets, plates etc.

The advantages of the method according to the invention overcome the defects of the discontinuous processes of the prior art and are essentially qualitative and economic quantitative in nature.

The Continuous Turbo Mixer assures an excellent quality of the dry blend, free from agglomerates and polluting impurities, which are the inevitable residue of any blend obtained in batches. This is due to the absence of stagnation and pollution points, and to the fact that a short residence time and the absence of friction do not allow the components to become degraded (by friction and compaction, heat).

For the manufacturing of plasticised PVC, the proportioning-blending system according to the invention allows to homogenise different concentrations of plasticiser on resin. Equally accurate and efficient is the homogeneous diffusion of liquid agents in minimum quantity, such as stabilisers and, for example, colour pastes.

The method of the invention allows 2 different reasons for energy saving in the production of the dry-biend of rigid or plasticised PVC.

1. The Continuous Turbo Mixer allows to mix constant flows of raw materials, enormously reducing the volume of the mixing chamber and organs relative to a traditional slow or fast batch mixer. The result is a corresponding reduction in installed power.

2. In the case of cable production, the cable extruder may be fed directly with dry-blend at the desired temperature, thereby eliminating the need to pre- heat the PVC granules.

Given the short time of permanence of the products in the mixer, it may be decided at any time to stop the plant without wasting even a minimum quantity of raw material. The mixer has no areas of stagnation of the material: all that it is fed is transported to the output in the motion created by the rotating shaft. If the chamber of the mixer retains a very thin layer of residual product, it can easily be removed by feeding it only neutral resin for a far shorter time than required by a traditional mixer.

The efficient distribution capability in the blend translates into a reduction in the quantity of extremely costly additives and stabilisers which in the discontinuous process, due to the difficulty in their dispersion in the blend, are fed in excess quantities.

A traditional automated discontinuous installation can develop according to two widely employed designs: 1. vertically, for a height of over twenty meters and through several floors, allowing to manage the flow of raw materials and the passage of the PVC blend solely by gravity along the various discontinuous transformation stages, 2. otherwise, the vertical development of the building may be moderated, but the material will have to be boosted or brought back to a certain elevation passing from a transformation phase to another (storage, proportioning, mixing/cooling, compounding).

The method of the invention needs installations with moderate vertical development, variable between eight and ten meters and a single floors, whereby the raw materials and the semi-finished product are moved by gravity until the extrusion, granulation or calendering step.

Claims

Patent claims
1. A method for manufacturing products made of rigid and plasticised PVC in particular tubes, section bars, cables and calendered elements, characterised in that the method comprises a single passage, completely continuous with two possible outcomes depending on whether it is applied to extrusion or calendering processes.
2. The method as claimed in claim 1 , characterised in that raw materials (1 ) are stored separately and are proportioned (2) according to two different processes.
3. The method as claimed in claims 1 and 2, characterised by a continuous volumetric or gravimetric proportioning of a pre-mixture of solids and a pre-mixture of liquids, fed distinctly into a continuous turbo mixer (3 in
Fig. 2).
4. The method as claimed in claims 1 and 2, characterised by a continuous, volumetric or gravimetric proportioning, but separate proportioning of solids and liquids (Fig. 3).
5. The method as claimed in any of claims 1 to 4, characterised in that inside a turbo mixer (3) runs a constant and homogeneous flow of raw materials which, in their path towards discharge point, are accurately mixed.
6. The method as claimed in claim 5, characterised in that depending on the final product, the output of the turbo mixer (3) directly feeds a continuous extruder (4) for the production of tubes, section bars or cables, or a calender (5) for the production of films, sheets or plates.
7. Product manufactured according to the method as claimed in any of the claims 1 to 6.
PCT/EP2003/013957 2002-12-20 2003-12-09 A method for manufacturing products made of rigid and plasticised pvc, in particular tubes, section bars, cables and calendered elements WO2004056545B1 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
ITMI2002A002696 2002-12-20
ITMI20022696 2002-12-20

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP20030789185 EP1656241A1 (en) 2002-12-20 2003-12-09 A method for manufacturing products made of rigid and plasticised pvc, in particular tubes, section bars, cables and calendered elements

Publications (3)

Publication Number Publication Date
WO2004056545A1 true true WO2004056545A1 (en) 2004-07-08
WO2004056545A8 true WO2004056545A8 (en) 2006-04-06
WO2004056545B1 true WO2004056545B1 (en) 2006-05-11

Family

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PCT/EP2003/013957 WO2004056545B1 (en) 2002-12-20 2003-12-09 A method for manufacturing products made of rigid and plasticised pvc, in particular tubes, section bars, cables and calendered elements

Country Status (2)

Country Link
EP (1) EP1656241A1 (en)
WO (1) WO2004056545B1 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009114761A3 (en) * 2008-03-14 2011-04-21 Dow Global Technologies Inc. Improved process for shaping polymeric articles
US8529821B2 (en) 2009-01-30 2013-09-10 Dow Global Technologies Llc Polymeric compositions and filled TPO articles having improved aesthetics

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB817981A (en) * 1956-03-19 1959-08-12 Dow Chemical Co Formed articles comprising expanded thermoplastic resinous materials and method for their formation
GB1134167A (en) * 1966-03-16 1968-11-20 Baerlocher Chem Method for the continuous processing of polyvinyl halide compositions
US4698378A (en) * 1982-12-20 1987-10-06 Buss Ag Procedure for the continuous production of free flowing and homogenous mixtures of plastic materials with admixtures
US4889673A (en) * 1988-01-22 1989-12-26 Toyoda Gosei Co., Ltd. Process for preparing polyvinyl chloride material used for extrusion molding
EP0611250A1 (en) * 1993-02-05 1994-08-17 ICMA SAN GIORGIO S.p.A. Extrusion method and plant
EP0709172A1 (en) * 1994-10-27 1996-05-01 POMINI S.p.A. Apparatus for continuously feeding extrusion and/or rolling machines with viscous material such as rubber and the like coming from discontinuous-cycle machines
EP0775718A2 (en) * 1995-11-22 1997-05-28 UNION CARBIDE CHEMICALS & PLASTICS TECHNOLOGY CORPORATION Process for preparing elastomeric compounds from granular elastomers and polymers

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB817981A (en) * 1956-03-19 1959-08-12 Dow Chemical Co Formed articles comprising expanded thermoplastic resinous materials and method for their formation
GB1134167A (en) * 1966-03-16 1968-11-20 Baerlocher Chem Method for the continuous processing of polyvinyl halide compositions
US4698378A (en) * 1982-12-20 1987-10-06 Buss Ag Procedure for the continuous production of free flowing and homogenous mixtures of plastic materials with admixtures
US4889673A (en) * 1988-01-22 1989-12-26 Toyoda Gosei Co., Ltd. Process for preparing polyvinyl chloride material used for extrusion molding
EP0611250A1 (en) * 1993-02-05 1994-08-17 ICMA SAN GIORGIO S.p.A. Extrusion method and plant
EP0709172A1 (en) * 1994-10-27 1996-05-01 POMINI S.p.A. Apparatus for continuously feeding extrusion and/or rolling machines with viscous material such as rubber and the like coming from discontinuous-cycle machines
EP0775718A2 (en) * 1995-11-22 1997-05-28 UNION CARBIDE CHEMICALS & PLASTICS TECHNOLOGY CORPORATION Process for preparing elastomeric compounds from granular elastomers and polymers

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
[Online] 2001, , XP002276812 Retrieved from the Internet: URL:http://www.polymer-age.co.uk/k1/k1comp ound.htm#Continuous%20mixer%20now%20has%20 melt%20pump%20discharge> [retrieved on 2003-04-05] page 3 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009114761A3 (en) * 2008-03-14 2011-04-21 Dow Global Technologies Inc. Improved process for shaping polymeric articles
US8709316B2 (en) 2008-03-14 2014-04-29 Dow Global Technologies Llc Process for shaping polymeric articles
US8529821B2 (en) 2009-01-30 2013-09-10 Dow Global Technologies Llc Polymeric compositions and filled TPO articles having improved aesthetics

Also Published As

Publication number Publication date Type
WO2004056545B1 (en) 2006-05-11 application
WO2004056545A8 (en) 2006-04-06 application
EP1656241A1 (en) 2006-05-17 application

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