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WO2009000275A2 - Procédé de traitement d'article polymère - Google Patents

Procédé de traitement d'article polymère Download PDF

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Publication number
WO2009000275A2
WO2009000275A2 PCT/DK2008/050151 DK2008050151W WO2009000275A2 WO 2009000275 A2 WO2009000275 A2 WO 2009000275A2 DK 2008050151 W DK2008050151 W DK 2008050151W WO 2009000275 A2 WO2009000275 A2 WO 2009000275A2
Authority
WO
WIPO (PCT)
Prior art keywords
polymer
item
container
wall section
porous wall
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.)
Ceased
Application number
PCT/DK2008/050151
Other languages
English (en)
Other versions
WO2009000275A3 (fr
Inventor
Jan Damgaard
Mikkel Petersen
Anne Marie Jensen
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.)
NANON AS
Original Assignee
NANON AS
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
Application filed by NANON AS filed Critical NANON AS
Publication of WO2009000275A2 publication Critical patent/WO2009000275A2/fr
Publication of WO2009000275A3 publication Critical patent/WO2009000275A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • 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
    • B29C71/00—After-treatment of articles without altering their shape; Apparatus therefor
    • B29C71/0009—After-treatment of articles without altering their shape; Apparatus therefor using liquids, e.g. solvents, swelling agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/06—Cleaning involving contact with liquid using perforated drums in which the article or material is placed
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
    • B08B7/0021—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by liquid gases or supercritical fluids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/02—Chemical treatment or coating of shaped articles made of macromolecular substances with solvents, e.g. swelling agents
    • 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
    • B29C71/00—After-treatment of articles without altering their shape; Apparatus therefor
    • B29C71/0009—After-treatment of articles without altering their shape; Apparatus therefor using liquids, e.g. solvents, swelling agents
    • B29C2071/0027—Removing undesirable residual components, e.g. solvents, unreacted monomers

Definitions

  • the present invention relates to a method of treating an item of a polymer comprising undesired residuals which are dissolvable in CO2, such as a silicone rubber item, such as a medical item or other polymer items where high quality is desired.
  • Silicone rubber has been used in a variety of fields as medical instruments, building materials, electric and electronic parts, automotive parts, and business machine parts because of its superior properties including physiological inertness (non-toxicity), weather resistance, durability, release properties, and heat resistance.
  • Silicone rubber items may today be produced in many ways using various starting materials and tempering systems.
  • US 5519082 discloses a silicone rubber composition that cures through hydrosilylation. This reaction type is known as the addition tempering type.
  • US 5973030 discloses production of liquid silicone rubber compositions.
  • EP 384 609 and US 6020449 disclose single-component silicone rubber mixtures (RTV1 ) which readily cure simply by heating, leading to a very high production yield. Two component silicon rubbers are also very popular.
  • WO 03/068846 and WO 06/045320 owned by applicant describe methods for treating silicone items by subjecting them to CO2 in liquid and or supercritical form. As described therein the treatment may beneficially be performed in a rotating drum.
  • WO 06/045320 describes a method where a plurality of substrates war treated in a nylon bag for simply handling. After the treatment the treated substrates are packed in a packing material for avoiding re-contamination.
  • the CO2 treatment is in general a relatively clean process and as described in WO 06/045320, it has further been found that the CO2 treatment may have a sterilizing effect on the treated items.
  • CO2 is primarily used for cleaning processes at high pressure about 73 bars and above where the CO2 is in its supercritical state or near supercritical state (when the temperature is below the supercritical temperature about 32 0 C.
  • CO2 in its supercritical state or near supercritical state is generally known as an effective cleaning solvent in particular when pulsed or when energized e.g. by a simultaneously treatment e.g. as described in US 5,344,493.
  • a simultaneously treatment e.g. as described in US 5,344,493.
  • the properties of CO2 is highly dependant on its state and that CO2 in liquid state both in physical and in chemical aspects is incomparable to CO2 in its supercritical state or near supercritical state.
  • the inventors of the present invention have accordingly found new improvements which result in a liquid CO 2 treatment process which results in even more clean items.
  • the object of the invention is thus to provide a method which results in an improved liquid CO2 treatment of polymer items.
  • the method of the invention for treating at least one polymer item comprises treating the at least one item by liquid CO2 at a pressure of up to about 50 bars in a vessel, wherein the at least one polymer item is packed in a closed container during the treatment, where the container comprises a wall wherein at least 10 % of the area of said wall is a porous wall section which is permeable to liquid CO2, said porous wall section having a pore size up to about 500 ⁇ m.
  • the treatment is performed below the critical temperature of CO2.
  • the treatment is kept below about 30 0 C.
  • All pore sizes mentioned herein may preferably be measured using by Bubble Point and Mean Flow Pore Test e.g. according to ASMT Method F316, for example F316-03 Standard "Test Methods for Pore Size Characteristics of Membrane Filters by Bubble Point and Mean Flow Pore Test", e.g. Test Method A and/or Test Method B.
  • the vessel has a volume which is much larger than the size of the polymer item, and naturally for cost reasons it is desired to treat several items, such as 5 or more, such as 10 or more, such as 100 or more polymer items simultaneously in the same vessel.
  • the method may thus comprise treating such several items simultaneously.
  • the several polymer items treated simultaneously may have the same shape and/or size or they may differ in size and shape from each other.
  • the several polymer items may be packed in individual containers or several items may be applied in one container.
  • the part of the wall which constitutes the porous wall section may in principle be the whole wall or any smaller parts thereof.
  • the porous wall section may be provided in one segment of the wall or in two or more segments. For practical reasons it will often be desired that the porous wall section is in one continuous section.
  • the porous wall section constitutes at least 10 % by wall area of the total wall of the container.
  • at least 20 % such as at least 30 %, such as at least 40 %, such as at least 50 %, such as at least 60 %, such as at least 70 %, such as at least 80 %, such as at least 90 %, such as at least 95 %, such as essentially all of said wall is a porous wall section.
  • the container is made from one material sheet which is folded and fastened to form the container.
  • the material sheet may for example comprise 1 , 2, 3 or more layers to provide the desired porosity.
  • the porous wall section has a pore size of up to about 400 ⁇ m, such as of up to about 300 ⁇ m, such as of up to about 200 ⁇ m, such as of up to about 150 ⁇ m, such as of up to about 100 ⁇ m, such as of up to about 50 ⁇ m, such as of up to about 10 ⁇ m, such as of up to about 1 ⁇ m.
  • the pore size(s) should preferably be sufficiently small to protect the polymer items within the container from being contaminated by undesired dirt.
  • the pore size(s) of the porous wall section is sufficiently small to protect the polymer items within the container from being contaminated by dust generated by the treatment external to the container.
  • the pore size(s) of the porous wall section is sufficiently small to protect the polymer items within the container from being contaminated by dirt and grease from hands, during the handling of the container.
  • the pore size(s) of the porous wall section is even sufficiently small to protect the polymer items within the container from being contaminated by microorganism.
  • the said porous wall section has a pore size of at least about 0.01 ⁇ m, such as at least about 0.1 ⁇ m, such as at least about 1 ⁇ m, such as at least about 5 ⁇ m, such as at least about 10 ⁇ m, such as at least about 50 ⁇ m.
  • the container may have pores of essentially the same size or the size of the pores may vary e.g. in a desired pattern.
  • the pores may be evenly distributed in the porous wall section or the distribution may vary.
  • the polymer item(s) may be packed in the container and treated according to the invention without risk of undesired contamination under loading and unloading of the vessel, even when the loading/unloading is performed manually.
  • the container may have any shape. Often it may be desired to shape the container such that it is adapted to the polymer items which should be treated according to the invention.
  • the size of the container may also be as desired, but preferably adapted to the polymer items to be treated.
  • the container has a volume which is at least 1.1 times the total volume of the polymer item (s) (the total volume of all the polymer items treated therein), such as preferably at least 1.2 times, such as at least 1.5 times, such as 2 to 25 times the total volume of the polymer item (s).
  • the volume of the container may be adapted to contain 1 , 2, 3, or more polymer items such as up to 10000 polymer items, which polymer items may be identical or may differ in composition and/or in shape and/or in size.
  • the container is or comprises a cage, preferably having relatively stiff walls.
  • Such cage with relative stiff walls may be simple to handle and simple to stack.
  • the cage may be provided for specific polymer items to thereby make it simple to load and unload.
  • the container comprises a cage covered by said wall e.g. in the form of a flexible layer coated onto the cage, e.g. a relatively stiff cage.
  • the container may in one embodiment be a bag preferably having essentially flexible walls. In principle any type and any size of bag having a porous wall section as described above may be used.
  • the container may e.g. be a bag of the type which today is used in autoclaves, e.g. STERIKING Sterilisation Pouches marketed by WIPAK MEDICAL.
  • STERIKING Sterilisation Pouches marketed by WIPAK MEDICAL.
  • other useful steriaisation bags the following can be mentioned: Breather Bags marketed by General Econopak, Inc, USA and LUKASTERIK sterilization bags marketed by OLSANSKE PAPIRNY a. s, Czech Republic
  • the container e.g. in the form of a bag is applied in a net or a cage, e.g. a net or a cage which may be used to fix the container in a rotary basket within the vessel as described in applicants co-pending application with the same priority date.
  • the net may preferably be fixed to the rotary basket at 2 or more locations, preferably 3 or more locations, such as 4 or more locations to thereby provide a sufficient fixing of the container.
  • the container should be a closed container which means that the container should preferably not have any openings into the container during the treatment which are larger than the pores described above. Preferably the only openings into the container during the treatment are the pores of the porous wall section.
  • the container may be closed by any desired means such as by adhesive, by welding, by heat sealing, by Velcro, by stitching, by zipper(s), by tying or by any combinations thereof.
  • porous wall section may comprise 1 , 2, 3 or more layers to provide the desired porosity.
  • the porous wall section has a single material layer.
  • the porous wall section comprises two or more layers.
  • the two or more layers may be of the same or of different material.
  • the two or more layers may for example be laminated to each other or they may be un-bonded.
  • the total layer of the wall should preferably be sufficiently large to provide the container with the desired strength for handling e.g. manually and/or by machines.
  • the porous wall section has a thickness of from 1 ⁇ m to 2 mm, such as from 10 ⁇ m to 1 mm, such as from 20-200 ⁇ m.
  • the one or more layer of the porous wall section may preferably comprise at least one layer of a material selected from the group consisting of paper, polymer and textile, such as linen.
  • the porous wall section comprises at least one layer of a polymer, preferably selected from the group consisting of olefin, such as poly ethylene (PE); polyamide (PA); aramid such as Kevlar®; Polyimide (Pl), polyester (PE), polyacrylate (PMMA), Poly phenylene-sulphide (PPS), Thermoplastic polyether (PET/PBT).
  • a polymer preferably selected from the group consisting of olefin, such as poly ethylene (PE); polyamide (PA); aramid such as Kevlar®; Polyimide (Pl), polyester (PE), polyacrylate (PMMA), Poly phenylene-sulphide (PPS), Thermoplastic polyether (PET/PBT).
  • the porous wall section comprises at least one woven layer. In one embodiment the porous wall section comprises at least one non-woven layer.
  • the porous wall section comprises at least one woven layer and at least one non-woven layer.
  • the vessel used for the treatment may in principle be any type of vessel which can be used for liquid CO2 treatment. Any of the methods and the vessels (reactors) described in WO 03/068846 and WO 06/045320 may be used in combination with the present invention which adds the additional features that the polymer item(s) are packed in a bag as defined in the claims during the treatment.
  • the method of the invention comprises treating said at least one item by liquid CO2 in a vessel comprising a rotary basket.
  • the method of the present invention may in one embodiment be combined with the method described in applicants co-pending patent application filed simultaneously with this application, which method comprises fixing the container non-concentrically in the vessel, the method preferably comprising fixing said container to an annular wall of the rotary basket.
  • the polymer items may be any kind of polymer items.
  • the method is in particular beneficial for treating polymer items of polymer comprising liquid residuals or solid residuals dissolvable in liquid CO2, such as polymer item(s) of a polymer selected from silicone rubber, such as functionalized silicone rubber, such as RTV- 1 silicone rubbers, RTV-2 silicone rubbers and HTV silicone rubbers.
  • the method may, however, also be highly beneficial for removing dust polymer item(s), for impregnating polymer item(s) and/or for sterilization or semi sterilization of polymer item(s).
  • the method is highly beneficial for treating polymer silicon rubber item(s) made from a precursor silicon mixture comprising one or more silicone components, preferably said precursor silicon mixture comprises one or more of the silicone components selected from the group consisting of dialkylsilicone elastomers wherein alkyl means hydrocarbon side groups of 1-12 carbon atoms such as methyl, ethyl, hexyl, and octyl; vinyl silicone elastomers; phenyl silicone elastomers; nitrile silicone elastomers; fluorosilicone elastomers, room temperature vulcanising (RTV) silicone elastomers; liquid silicone elastomers (LSR); borosilicone elastomers; the precursor silicon mixture preferably comprises dimethyl silicone elastomers.
  • the polymer item(s) may be shaped by any means such as by moulding, such as compression moulding, transfer moulding or injection moulding; extrusion, blowing or combinations thereof.
  • the silicone rubber is cross-linked, preferably by a method from the group of condensation reaction, addition reaction, peroxide assisted reaction and mixtures thereof.
  • the polymer item can be packed in the container during the whole CO2 treatment so that the polymer item(s) are packed in the container(s) while they are loaded into the vessel and while they are un-loaded from the vessel.
  • the polymer item(s) may be packed in the container(s) immediately after shaping or any time thereafter until immediately prior to loading into the vessel.
  • the item(s) are packed in said container within 24 hours after shaping, preferably within 12 hours, such as within 8 hours, such as within 4 hours, such as within 2 hours such as within 1 hour after shaping.
  • the item(s) are produced at a production site and packed in said container at said production site where they were shaped.
  • This embodiment provides a highly beneficial method because very often the step of CO2 treating polymer items is provided by an external supplier.
  • the factory producing the polymer item(s) can then assure that the polymer items are returned after the CO2 treatment in the same closed container(s).
  • the packed polymer item(s) may then be transported to the CO2 treatment supplier, who treats the packed polymer item(s) and returns them still in packed condition.
  • the polymer item(s) are transferred from the production site to a remote location where the container(s) are applied in the vessel and the polymer item(s) are treated with liquid CO2.
  • the container(s) may there after preferably be withdrawn from the vessel and transferred to a remote location in said sealed container(s).
  • the method of treating the polymer item(s) may for example be as described in WO 03/068846 and WO 06/045320 with the provision that the polymer item(s) are packed in a container as described herein. Other methods of CO2 treatment may also be used.
  • the treatment of said polymer item(s) comprises subjecting the polymer item(s) to an extraction treatment using carbon dioxide comprising a solvent at a pressure between 10 and 50 bars, wherein the item has an initial temperature below 60 °C in the extraction treatment, and in at least a part of the extraction time the item has a temperature below 25 °C and a pressure so that the carbon dioxide is in its liquid state.
  • the treatment of the polymer item(s) exclude any simultaneously microwave treatment.
  • the treatment of the polymer item(s) exclude any simultaneously electromagnetic energy treatment.
  • Group A (10 items) put in a commercial sterilisable bag (name: steriking).
  • Group B (10 items) used as first reference items.
  • Group C (10 items) used as second reference items.
  • Groups A and B were applied in a rotary basket of a vessel and treated by CO2 Treatment parameters:
  • Group C - not treated average: 1.14% std. dev. 0.03%
  • Group B - not in sterilisable bag Average: 0.22% std. dev 0.01 %
  • Group A - inside sterilisable bag average: 0.23% std. dev. 0.01 %

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Treatments Of Macromolecular Shaped Articles (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)

Abstract

L'invention concerne un procédé qui permet de traiter au moins un article polymère, selon lequel on traite l'article avec du CO2 liquide à une pression inférieure ou égale à 50 bars environ dans un récipient, le ou les articles polymères étant emballés dans un contenant fermé au cours du traitement. Le contenant fermé comprend une paroi dont au moins 10 % de la surface est constituée d'une partie de paroi poreuse qui est perméable au CO2 liquide. La partie de paroi poreuse possède une taille de pores inférieure ou égale à 500 µm environ. Le procédé de l'invention permet de traiter des articles polymères avec du CO2 liquide alors que ces derniers sont emballés ou pré-emballés. L'invention permet de la sorte de protéger le ou les articles contre une recontamination.
PCT/DK2008/050151 2007-06-22 2008-06-17 Procédé de traitement d'article polymère Ceased WO2009000275A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DKPA200700906 2007-06-22
DKPA200700906 2007-06-22

Publications (2)

Publication Number Publication Date
WO2009000275A2 true WO2009000275A2 (fr) 2008-12-31
WO2009000275A3 WO2009000275A3 (fr) 2009-02-19

Family

ID=40010642

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/DK2008/050151 Ceased WO2009000275A2 (fr) 2007-06-22 2008-06-17 Procédé de traitement d'article polymère

Country Status (1)

Country Link
WO (1) WO2009000275A2 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107503121B (zh) * 2017-07-28 2020-04-28 上海工程技术大学 运动状态的芳纶纤维张力作用下的超临界co2改性方法和装置

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5213619A (en) * 1989-11-30 1993-05-25 Jackson David P Processes for cleaning, sterilizing, and implanting materials using high energy dense fluids
US6558622B1 (en) * 1999-05-04 2003-05-06 Steris Corporation Sub-critical fluid cleaning and antimicrobial decontamination system and process
JP4133209B2 (ja) * 2002-10-22 2008-08-13 株式会社神戸製鋼所 高圧処理装置
CN101048448A (zh) * 2004-10-25 2007-10-03 南农股份公司 制备硅橡胶物品的方法和通过这种方法获得的产品
US7253253B2 (en) * 2005-04-01 2007-08-07 Honeywell Federal Manufacturing & Technology, Llc Method of removing contaminants from plastic resins

Also Published As

Publication number Publication date
WO2009000275A3 (fr) 2009-02-19

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