WO2008069041A1 - 高分子成形物への機能付与方法およびその装置 - Google Patents
高分子成形物への機能付与方法およびその装置 Download PDFInfo
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- WO2008069041A1 WO2008069041A1 PCT/JP2007/072800 JP2007072800W WO2008069041A1 WO 2008069041 A1 WO2008069041 A1 WO 2008069041A1 JP 2007072800 W JP2007072800 W JP 2007072800W WO 2008069041 A1 WO2008069041 A1 WO 2008069041A1
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- 0 C*(C)C1CCCC1 Chemical compound C*(C)C1CCCC1 0.000 description 1
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- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
- D06M23/10—Processes in which the treating agent is dissolved or dispersed in organic solvents; Processes for the recovery of organic solvents thereof
- D06M23/105—Processes in which the solvent is in a supercritical state
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- 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
- C08J7/04—Coating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/02—Processes for applying liquids or other fluent materials performed by spraying
- B05D1/025—Processes for applying liquids or other fluent materials performed by spraying using gas close to its critical state
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0218—Pretreatment, e.g. heating the substrate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0218—Pretreatment, e.g. heating the substrate
- B05D3/0227—Pretreatment, e.g. heating the substrate with IR heaters
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- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/06—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/02—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber
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- 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
- C08J7/12—Chemical modification
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/08—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with halogenated hydrocarbons
- D06M13/085—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with halogenated hydrocarbons cycloaliphatic
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/35—Heterocyclic compounds
- D06M13/352—Heterocyclic compounds having five-membered heterocyclic rings
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/53—Polyethers
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
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- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/94—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using dyes dissolved in solvents which are in the supercritical state
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2256/00—Wires or fibres
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/16—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using dispersed, e.g. acetate, dyestuffs
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Definitions
- the present invention relates to a method for imparting a function to a polymer molded product such as a fiber structure and an apparatus therefor, and more specifically, a function imparting agent is added to a polymer molded product using a supercritical fluid.
- the present invention relates to a deposition method and an apparatus therefor.
- Patent Document 1 Japanese Patent Application Laid-Open No. 4 245981 discloses a method for reducing waste liquid treatment costs in dyeing processing by using supercritical fluid for dyeing fiber structures, thereby reducing waste liquid to zero.
- a method is disclosed in which dyes that have not been exhausted by fibers (undyed dyes) can be recovered without using dyeing assistants that have been used in large amounts.
- Patent Document 2 Japanese Patent Laid-Open No. 2002-212884 proposes a method for providing a method for imparting a high durability function to a fiber structure that can be recovered and reused as necessary. According to Patent Document 2, when a function-imparting agent is adhered to a polymer molding in a supercritical fluid, the function-imparting agent is adhered while circulating the supercritical fluid. However, this method also has a problem in that it is a fiber structure treatment in a pressure vessel and is not as efficient as the batch type.
- Patent Document 1 Japanese Patent Application Laid-Open No. 4 245981
- Patent Document 2 Japanese Patent Laid-Open No. 2002-212884
- An object of the present invention is to be able to efficiently apply various function-imparting agents to a polymer molded product, to reduce processing waste liquid as much as possible, and to recover waste liquid and function-imparting agent. In addition, it can be reused as necessary, and the function-imparting agent can be applied to the polymer molding in a continuous manner rather than a batch method. And providing an apparatus thereof.
- the present invention relates to a method for imparting a function to a polymer molded product, which comprises jetting a supercritical fluid to the polymer molded product and fixing a function-imparting agent to the polymer molded product.
- a function-imparting agent with a supercritical fluid in advance and to perform mixing with a mixing coil.
- This mixed fluid injection uses a reactor having a substantially inverted ⁇ -shaped gap in cross-sectional view, and polymer molding is performed in one of the roughly inverted ⁇ -shaped gaps of this reactor from one to the other.
- a method is preferred in which a mixed fluid is jetted toward a polymer molded product from another gap existing between the upper end and the lower end of the central portion while the object is running.
- the mixed fluid is further mixed by another mixing coinor provided near the upper part of the reactor and heated by a heater provided near the other mixing coil.
- the method is preferred.
- a method of heating the reactor by providing a heater near the bottom of the reactor is also preferable.
- a method of heating the reactor by providing an infrared lamp near the bottom of the reactor is also preferable.
- a single-nozzle jet nozzle is used, and a supercritical fluid and a function-imparting agent are mixed in advance and supplied to the supply port of the jet nozzle. Tip force This mixed fluid may be sprayed onto the polymer molding.
- the polymer molded product may be laser-heated, and then the mixed fluid may be sprayed from the single nozzle jet nozzle to the heating site.
- a double nozzle type jet nozzle is used, and both of them without mixing the supercritical fluid and the function-imparting agent in advance are separately supplied to the jet nozzle. They may be supplied to the mouth, mixed at the tip of the nozzle, and this mixed fluid injected into the polymer molding.
- the supercritical fluid and the function-imparting agent are separately heated in the vicinity of the supply port on the upstream side of the double nozzle type jet nozzle.
- the polymer molded product may be laser-heated, and then the mixed fluid may be sprayed from the double nozzle type jet nozzle to the heated portion.
- the present invention relates to a fluid storage container for storing a supercritical fluid, a fluid pump for compressing and transporting the fluid, a function-imparting agent pump for transporting the function-imparting agent, And the function-imparting agent storage container are sequentially connected through the connection pipe, the mixing pipe is branched from the connection pipe between the fluid pump and the function-imparting agent pump, and is opposed to the leading end of the mixing pipe.
- a reactor having a substantially inverted ⁇ -shaped gap when viewed in cross-section, wherein one gap for running a polymer molding that penetrates from one side of the substantially inverted T-shape of the reactor to the other, and a substantially central portion
- a reactor having another gap for function-imparting agent injection existing between the upper end portion and the lower end portion of the mixing pipe, and further the tip of the mixing pipe
- the present invention relates to a function-imparting device for a polymer molded article in which a nozzle provided in a section is connected to an upper end of another gap in the reactor, and a mixing coil is connected to a path of the mixing pipe.
- another mixing coil is connected between the mixing pipes between the mixing coil and the reactor, and a heater is provided near the other mixing coil.
- a preferred embodiment is a preferred embodiment.
- an apparatus in which a heater is provided near the bottom of the reactor is also mentioned as a preferred embodiment.
- an apparatus in which an infrared lamp is provided near the bottom of the reactor is also mentioned as a preferred embodiment.
- various function-imparting agents can be efficiently applied to a polymer molded product, and processing waste liquid can be reduced as much as possible, and the waste liquid and function-imparting agent can be recovered. In addition, it can be reused as necessary, and the function-imparting agent can be applied to the polymer molding in a continuous manner rather than a batch method. , And apparatus thereof.
- FIG. 1 is a schematic diagram showing an example of a function providing device of the present invention.
- FIG. 2 is a schematic view showing another example of the function providing device of the present invention.
- FIG. 3 is a schematic view showing another example of the function providing apparatus of the present invention.
- FIG. 4 is a cross-sectional configuration diagram of a single nozzle type jet nozzle used in the present invention.
- FIG. 5 is a cross-sectional configuration diagram of a double nozzle type jet nozzle used in the present invention.
- FIG. 6 is a configuration diagram of the laser heating assist cluster jet method of the present invention.
- FIG. 7 is a perspective view of FIG.
- the supercritical fluid used in the present invention is a fluid under a temperature and pressure exceeding the critical temperature and critical pressure, and is defined as a non-condensable dense fluid. This state cannot be said to belong to either the gas phase or the liquid phase, and has a diffusion performance similar to that of a gas even though the density is similar to that of a liquid.
- the supercritical fluid causes a large density change with a slight pressure change, and also has a low viscosity and a high diffusivity, so that various function-imparting agents can be dissolved. Since the function-imparting agent is well dissolved, it can be said that these function-imparting agents can penetrate into the details of the polymer molded product and are suitable for function-imparting processing.
- the supercritical fluid includes a gas or liquid fluid (subcritical fluid) that is sufficiently higher than the pressure of an apparatus used in normal fiber processing, for example, in a high pressure state higher than IMpa.
- the fluid in such a high pressure state can dissolve various function-imparting agents as in the supercritical fluid, and easily penetrates into the details of the polymer molded product. Presents.
- the supercritical fluid includes carbon dioxide, N20 (Japanese name: nitrous oxide), water, and ethano.
- carbon dioxide it is most preferable to use carbon dioxide in consideration of the ease of conditions for making it a supercritical fluid, safety, heat resistance, pressure resistance, and corrosion resistance of the equipment! /.
- Carbon dioxide has a critical temperature of 31.1 ° C and a critical pressure of 7.2 MPa.
- the supercritical carbon dioxide fluid will be described more specifically. Carbon dioxide fluid under supercritical conditions of carbon dioxide critical temperature of 31. 1 ° C or higher and critical pressure of 7. 48MPa or higher. It is also a preferred embodiment in the present invention to use a subcritical carbon dioxide fluid that is a carbon dioxide fluid under subcritical conditions, that is, near the critical point.
- the subcritical carbon dioxide fluid refers to a carbon dioxide fluid that is at a pressure of 7. OMPa or higher and a temperature of 25 ° C or higher and is not in a supercritical state.
- the supercritical carbon dioxide fluid (including subcritical carbon dioxide fluid) used in the present invention is inexpensive next to water whose critical temperature and critical pressure are both low, nontoxic, flame retardant, and non-corrosive.
- the load on the environment is small. Since the specific gravity can be changed by appropriately changing the pressure and temperature, the density difference from the mixed solution of water, organic solvent, and function-imparting agent can be easily ensured.
- supercritical carbon dioxide fluid is generated by acid-base interaction between the supercritical carbon dioxide fluid (subcritical carbon dioxide fluid) and the function-imparting agent.
- Subcritical carbon dioxide fluid is an extractant suitable for extracting a predetermined function-imparting agent from an aqueous solution or an organic solvent solution.
- the polymer molded product used in the present invention is a polyester-based polymer, polypropylene-based polymer, acetate-based polymer, polysulphated bull-based polymer, or aramid to which a function-imparting agent can be attached.
- a fiber structure such as a yarn, a woven fabric, a knitted fabric or a non-woven fabric mainly composed of a polymer or the like, or a molded body such as a film or a resin plate, or a mixture thereof.
- those mainly composed of polyester fibers are preferably exemplified.
- polyester fiber 95 moles of ethylene terephthalate repeating 90 mole 0/0 or gestures et preferred those forces beams ethylene terephthalate main repeating component and be shall have preferred instrument repeating units units 0/0 above is what is preferably an ethylene terephthalate.
- the polyester may be a specific copolymer in which a small amount of a copolymer component may be copolymerized.
- a copolymer component examples include aromatic dicarboxylic acids such as isophthalic acid, 5-sodium sulfoisophthalic acid, and naphthalenedicarboxylic acid, aliphatic dicarboxylic acids such as adipic acid and sebacic acid, and aliphatic diols such as tetramethylendalol and hexamethylene glycol.
- the polyester fiber may be added with a stabilizer, an antioxidant, an antistatic agent, a fluorescent whitening agent, a catalyst, a colorant, and the like within the range not impairing the purpose of this range.
- a supercritical fluid is sprayed onto the polymer molded product, and the function-imparting agent is fixed to the polymer molded product.
- a function-imparting agent is mixed with the supercritical fluid in advance, and this mixed fluid is sprayed onto the polymer molding to fix the function-imparting agent to the polymer molding, thereby improving the durability of the function.
- a function-imparting agent a low-polarity! / Or non-polarity // function-imparting agent can be used, and the function-imparting agent is a compound that is soluble in a supercritical fluid. It is preferable that Specifically, the following function-imparting agents can be mentioned as preferred examples. In addition, in order to improve processability, function expression and reproducibility, the function-imparting agent is preferable because it has a high solid content concentration (purity)!
- Examples of the function-imparting agent for imparting high durability and water repellency include fluorine compounds, silicone resins, and paraffin (wax) resins.
- Examples of the function-imparting agent for imparting high antifouling property and / or high hygroscopicity include polyalkylene glycol, and as the polyalkylene glycol, polyethylene glycol having a molecular weight of 20,000 or less is used. It can be mentioned as a preferred example.
- Examples of the function-imparting agent for imparting a high water repellency and / or high oil repellency and / or a texture with an enhanced slime feel include dimethylpolysiloxane (silicone). Silicone) preferably has a molecular weight of 10,000 or less
- Preferable examples of the function-imparting agent for imparting high flame retardancy include condensed halogenated phosphoric acid esters, condensed phosphoric acid esters, halogenated phosphoric acid esters, phosphoric acid esters, and hexachlorosilane decane. it can.
- the molecular weight is 1,000 to 3,0.
- a polycondensation product of 00 polyalkylene glycol and terephthalic acid, the polycondensation product having a polycondensation degree of 3 to 10 can be mentioned as a preferred example.
- the function-imparting agent for imparting high light resistance improvement examples include an ultraviolet absorber, and in particular, the ultraviolet absorber is preferably a benzotriazole derivative or a benzophenone derivative! .
- Disperse dyes are preferred as dyes for dyeing polymer moldings. Such disperse dyes are used for dyeing hydrophobic fibers from systems that are sparingly soluble in water and dispersed in water. Dyes that can be used, and are usually used for dyeing polyester fibers and acetate fibers, such as benzeneazo (monoazo, disazo, etc.), heterocyclic azo (tazonoreazo, benzothiazonorezo) , Quinoline azo, pyridine azo, imidazonole azo, phenazo phenazo, etc.), anthraquinone, and condensation systems (quinophthalene, styrin, coumarin) can be used arbitrarily. Further, it is preferable that the solid content concentration of the dye in the dye is higher because it is more easily dyed.
- examples of the function-imparting agent for applying chemical plating to the polymer molded product include metal complexes.
- the metal in the metal complex examples include copper, silver, nickel, and gold.
- the metal complex has a high solubility in a subcritical fluid or a supercritical fluid and is inexpensive and can be reduced at a low temperature of 20 to 100 ° C, which has little influence on the polymer molding.
- the power S is preferable.
- MnXm (COD) w Mn (COD) m (COT) w
- Mn (COD) m (OSiPh) w Mn (COT) m (OSiPh) w
- Mn (R) m (OSiPh) It is preferable to use a metal complex represented by w, Mn (RX) m (OS iPh) w, M (OR) n, M (OCOR) n, M (RCOCH COR) n.
- These metal complexes are easily reduced to metals by a reducing agent.
- X is F, CI, Br, I, CN, NO or CIO
- R is a hydrocarbon group, a halogenated carbon group such as fluorine, or a hydrocarbon group containing phosphorus.
- COD is cyclooctagene
- COT is cyclootatriene
- OSiPh is a silanol group.
- M is a metal fitting (Cu, Ag, N or Au, etc.)
- n, m and w are integers, which are determined by the valence of the metal. If M is divalent or higher, X and R exist in multiple forms in the metal-containing compound. Each state may be the same or different.
- one or more selected from the group consisting of a siloxo group, an alkyl group, and a silanol group is used as a ligand including COT or COD as a ligand, and these ligands are used. It is desirable to use a metal complex in which is bonded to a metal at the same time because metal particles can be obtained by hydrogenolysis with hydrogen at low temperature or room temperature, which has little influence on the polymer molded product.
- the reducing agent for reducing the metal complex supported on the surface of the polymer molded article is hydrogen, carbon monoxide, hydrazine, boron compound, phosphite, sulfite, Rossiel salt, jetylamine borane, formalin, hydroquinone, One or more selected from the group consisting of saccharides and organic acids are preferred.
- the reduction reaction of the metal complex supported on the surface of the polymer molding by the reducing agent may be performed in a subcritical fluid or supercritical fluid after degreasing and etching of the polymer molding, or the gas phase after decompression. You may go inside.
- the surface of the polymer molding is degreased by injecting the subcritical fluid or supercritical fluid, which is made of a metal complex containing the same metal as the plating metal, into contact with the polymer molding. After etching, the metal complex is supported on the surface of the polymer molded product. Next, the metal complex supported on the surface of the polymer molded product is reduced using a reducing agent, so that the metal in the metal complex is deposited on the surface of the substrate to form a metal nucleus. That is, the metal complex supported on the surface of the polymer molded product is reduced by a reducing agent such as hydrogen, and the ligand in the metal complex is easily released from the metal, and the metal is deposited on the surface of the base material. A genus nucleus is formed.
- the electroless plating method further includes a step of immersing a polymer molding having a metal nucleus formed on the surface in a plating solution containing the plating metal.
- a plating solution containing the plating metal.
- the metal in the plating solution the same metal as that in the metal complex is used.
- the reduction reaction of the metal complex supported on the surface of the polymer molded product by the reducing agent is performed by reducing the polymer molded product in a subcritical fluid or supercritical fluid after etching and in a gas phase after decompression. Go in the plating solution with the added agent.
- the deposited metal can be continuously reacted as an autocatalyst. Proceed to form a plating layer. That is, the metal in the plating solution is deposited on the metal core by the self-catalyzing action to form an adhesion layer. As a result, the adhesion between the metal core and the plating layer can be improved, so that the plating layer can be made difficult to peel off from the surface of the polymer molded product.
- Such solvents include methanol, ethanol, propanol, isopropyl alcohol, butanol, benzyl alcohol, acetone, acetophenone, N-methyl-2-pyridone, methyl ethyl ketone, dimethyl sulfoxide, dimethylformamide, ethylene glycol,
- polar solvents such as acetonitrile
- aromatic solvents such as toluene, benzene, and xylene.
- the concentration of the function-imparting agent in the reaction solution is usually 1 to 60% by weight, preferably about 5 to 40% by weight.
- concentration of the function-imparting agent in the supercritical fluid may be appropriately adjusted according to the properties of the function-imparting agent used.
- the adhesion amount of the function-imparting agent to the polymer molded product varies depending on the type of the function-imparting agent, but is usually 1 to 50% by weight in terms of solid content. If the adhesion amount is less than 1% by weight, the function may not be fully manifested! /.
- a supercritical fluid is jetted onto the above polymer molded product, and a function-imparting agent is fixed to the polymer molded product to give a specific function to the polymer molded product. It is.
- the surface of the polymer molding is treated with the above-mentioned various function-imparting agents such as dyes, metal complexes, and flame retardants, and a supercritical fluid is sprayed onto the treated polymer molding. Then, the function-imparting agent may be fixed to the polymer molded product.
- the fixing means in the present invention functions in the polymer molded product by mixing the function-imparting agent in the supercritical fluid in advance and then injecting the mixed fluid onto the polymer molded product such as a fiber structure. A specific function is imparted by fixing the imparting agent.
- a fluid storage container 11 for storing a supercritical fluid
- a fluid pump Pl for compressing and transporting the fluid
- a function-imparting agent for converting CO cylinder to a supercritical fluid
- the function-imparting agent pump P2 and the reaction liquid container 12 are sequentially connected through the connecting pipes LI and L2. Then, the mixing pipe L3 is branched at point A from the connecting pipe between the fluid pump P1 and the function-imparting agent pump P2. Between the pump P1 and the branch point A, a filter for removing dirt in the carbon dioxide, a cylinder bottle and other contaminants, and a high-pressure vessel cooler for storing the carbon dioxide are sequentially installed. It may be.
- the reaction liquid container 12 may be a simple solvent container. In this case, a means for injecting a donating agent such as a syringe is separately provided between the pump P2 and the point A.
- the reactor R1 has a substantially inverted T-shaped gap in a cross-sectional view, facing the tip of the mixing pipe L3, and has high fibers such as fibers penetrating from one D to the other E of this reactor.
- An annular reactor R1 having one gap hi for traveling the molecular molded article and another gap h2 for jetting the function-imparting agent existing between the upper end B and the lower end C of the central part is arranged.
- the nozzle L3p at the tip of the mixing pipe L3 is connected to the upper end B of the other gap of the reactor.
- a mixing coil 13 is connected to the route of the mixing pipe L3.
- the connection between the nozzle L3p and the upper end B of the reactor includes the case where the nozzle L3p is inserted into the upper end B and the case where the both are connected together. .
- the carbon dioxide supplied from the carbon dioxide cylinder 11 is boosted and heated to the supercritical state (or subcritical state) by the pump P1 via the pipe L1, and the branch point A To the mixing pipe L3.
- the reaction liquid (function-imparting agent solution) in the reaction liquid container 12 passes through the pipe L2, passes through the pump P2, reaches the mixing pipe L3 at the branch point A, and is mixed with carbon dioxide in the supercritical state.
- the superfluid carbon dioxide and the reaction liquid are uniformly mixed by the mixing coil 13 connected on the mixing pipe L3.
- the mixing coil 13 extracts the function-imparting agent from the mixed supercritical fluid by flowing the fluid through the coiled flow path. It is further promoted by putting things in and baffle plates.
- the nozzle L3p of the mixing pipe is placed in the gap h2 in the direction B ⁇ C.
- a mixing coil 14 is separately provided in the passage, and a heater 15 is installed in the vicinity of the mixing coil 14 so that the supercritical or subcritical state is held in the mixing pipe L3 path! /,
- the reactor R1 has a reverse T-shaped gap in cross-sectional view, and is composed of a hollow aluminum pipe, stainless steel pipe or the like, and its dimensions are not particularly limited.
- the pipes and equipment in each of the above locations are designed to maintain a smooth flow by polishing the interior and reducing the resistance of the fluid.
- the nozzle diameter of the nozzle L3p is, for example, about 1 to 500, ⁇ , preferably about 10 to 200 ⁇ 111.
- the function imparting device 20 in FIG. 2 uses a flat disk reactor as the reactor R2, and a heater 16 is provided near the bottom of the reactor instead of the mixing coil 14 and the heater 15 in FIG. Except for this, the configuration is the same as in Fig. 1.
- the heater 16 provided at the bottom of the reactor R2 The polymer molding itself such as the traveling fiber is heated to reduce the effect of applying the function-imparting agent.
- the reactor R2 has a reverse-shaped air gap in cross-sectional view and a substantially disk-shaped force made of a pipe made of aluminum, stainless steel or the like in front view. It ’s not limited.
- FIG. 3 uses a transparent reaction cell R3 as the reactor R3, and an infrared laser is provided near the bottom of the reactor instead of the mixing coil 14 and the heater 15 in FIG.
- the configuration is the same as that shown in Fig. 1 except that amplifier 17 is added.
- the infrared lamp 17 provided at the bottom of the reactor R3 is used.
- the supercritical state of the mixed fluid becomes a subcritical state. To be kept up.
- the reactor R3 is a force composed of a hollow quartz glass pipe having a reverse T-shaped gap in cross-section and a shape in which the center in the D ⁇ E direction swells. S, its dimensions are not particularly limited.
- the mixed fluid may be injected from the tip of the nozzle onto the polymer molding.
- the supercritical fluid (CO) and the function-imparting agent (sample) are used.
- the sample is dissolved in a supercritical fluid such as CO.
- the (sample) must also be hydrophobic. Also, because CO and the sample are heated at the same time
- Thermally degradable samples can not be used.
- a double nozzle type jet nozzle is used, and a supercritical fluid (CO) and a function-imparting agent (sample) are prepared in advance.
- both may be supplied to separate supply ports of the jet nozzle, mixed at the tip of the nozzle, and this mixed fluid may be injected onto the polymer molding.
- the function-imparting agent (sample) is dissolved in the supercritical fluid (CO 2).
- the function-imparting agent may be either hydrophobic or polar.
- Sex samples are also applicable.
- the pipes L1 and L2 are not merged at the branch point A, and the arrangement of the supercritical fluid (CO) and the function-imparting agent (sample) and the pipe route are not used except that the mixing condenser 13 is not used.
- FIGS. 6 to 7 is a single nozzle type jet nozzle or a double nozzle type jet nozzle, which indicates that it can also be applied to registration and deviation.
- a polymer molded product such as a film is moved in one direction at a constant moving speed V, and the film is laser-heated. Subsequently, T seconds after the laser irradiation, at a position at a distance of Lmm from the heating portion.
- the mixed fluid of the supercritical fluid and the function-imparting agent is jetted from the jet nozzle to the heating site.
- the heating width can be reduced by laser heating, and the adjustment of the heating depth is easy.
- the cooling of the heating part is performed. Diffusion is suppressed.
- the jet nozzle drives the cooling of the heating part by laser heating at the same time that the function-imparting agent (sample) is driven into the surface of the polymer molded product.
- a function-imparting agent (sample) can be injected into the heating portion in a short time after laser heating.
- the force S is used to optimize the height, depth, and width of the surface of the molded polymer after processing.
- the laser light output in the above laser heating is;! -50W, Preferably;
- the K / S value when the same polymer molded product is dyed with a normal aqueous system is measured, and the dyeability is evaluated by the ratio (percentage) of the K / S value of the polymer molded product to the value. did.
- LOI limit oxygen index
- a multi-layer of 83dtex / 24 filaments obtained by melt spinning polyethylene terephthalate with an intrinsic viscosity (measured in o-chlorophenol at 35 ° C) containing 0.05 wt% titanium oxide.
- the filament drawn yarn is scoured at 70 ° C for 20 minutes with an lg / 1 score roll # 400 (manufactured by Kao), washed with water and dried, then D to E of the capillary type T reactor in the equipment shown in Fig. 1.
- the mixed fluid was sprayed from the nozzle L3p at the tip of the mixing pipe L3 while traveling in the gap hi at 200 m / min in the direction.
- the gas from the carbon dioxide cylinder 11 is sent to the mixing pipe L3 by the pump P1 via the pipe L1, while the water repellent function additive in the reaction liquid container 12 is dimethylsiloxane having a molecular weight of 10,000 and a concentration of 10 %
- Aqueous dispersion is pumped out by pump P2 via pipe L2, merged with carbon dioxide fluid at branch point A, mixed well at mixing coil 13, and then mixed at mixing coil 14 and heater Heated at 15.
- This mixed fluid was sprayed onto the above-mentioned traveling fiber from the nozzle L3p of the mixing pipe L3 having a pore diameter of lO ⁇ m.
- the reactor R1 has a diameter hi of the gap hi in the direction D ⁇ E of 2 mm and a length of 60 mm, and a gap h2 between B and C has a diameter of 2 mm and a length of 15 mm. .
- the obtained fiber was sufficiently washed with water and dried.
- Example 1 treatment and evaluation were conducted in the same manner as in Example 1 except that the function-imparting agent was replaced with polyethylene glycol having a molecular weight of 10,000.
- Example 1 the treatment and evaluation were conducted in the same manner as in Example 1 except that the function-imparting agent was replaced with hexose oral mocyclododecane.
- Example 1 the treatment and evaluation were performed in the same manner as in Example 1 except that the function-imparting agent was replaced with a UV absorber (benzotriazole derivative).
- a UV absorber benzotriazole derivative
- Example 1 in addition to the function-imparting agent, disperse dye SM1P (Ciba 'Specialty' Chemicals: CI Disperse Blue 60) was added to the reaction solution in an amount of 6% by weight. Treated and evaluated as in Example 1.
- disperse dye SM1P Ciba 'Specialty' Chemicals: CI Disperse Blue 60
- Example 2 in addition to the function-imparting agent, 6% by weight of disperse dye SM1P (Ciba 'Specialty' Chemicals: CI Disperse Blue 60) was added to the reaction solution and treated at the same time as dyeing. Treatment and evaluation were conducted in the same manner as in Example 2.
- disperse dye SM1P Ciba 'Specialty' Chemicals: CI Disperse Blue 60
- Example 3 in addition to the function-imparting agent, 6% by weight of disperse dye SM1P (Ciba 'Specialty' Chemicals: CI Disperse Blue 60) was added to the reaction solution and treated at the same time as dyeing. Treatment and evaluation were carried out in the same manner as in Example 3.
- disperse dye SM1P Ciba 'Specialty' Chemicals: CI Disperse Blue 60
- Example 4 in addition to the function-imparting agent, 6% by weight of disperse dye SM1P (Ciba 'Specialty' Chemicals: CI Disperse Blue 60) was added to the reaction solution and treated at the same time as dyeing. Treatment and evaluation were conducted in the same manner as in Example 4.
- disperse dye SM1P Ciba 'Specialty' Chemicals: CI Disperse Blue 60
- the obtained fiber had a benzotriazole derivative attached! /.
- this fiber has the absorption performance in the ultraviolet region, the same fiber A K / S value of 89% was obtained when dyeing with normal water.
- Example 1 treatment and evaluation were conducted in the same manner as in Example 1 except that the function-imparting agent was not used.
- Example 1 instead of using the equipment shown in Fig. 1, using a Tecsum Giken mini-color dyeing machine, except for normal immersion exhaustion treatment (130 ° CX 60 minutes) without carbon dioxide injection Were treated and evaluated in the same manner as in Example 1.
- the resulting fiber had almost no dimethylsiloxane attached, and most of the fiber did not show water repellency.
- Example 1 an autoclave was used instead of the apparatus of FIG. 1, and the same treatment as in Example 1 was performed except that the supercritical carbon dioxide was not circulated and treated at 145 ° C. for 60 minutes. Dimethylsiloxane was locally attached to the obtained fiber, and there were hard textured parts and no water / repellent parts.
- Example 2 Experiments were performed in the same manner as in Example 1 except that the apparatus 20 in FIG. 2 was used instead of the apparatus in Example 1.
- the temperature of the heater 16 was set to 200 ° C.
- the flat disk reactor R2 has a D ⁇ E direction gap (vertical direction) hi is 2 mm, depth is 2 mm, length is 600 mm, and B ⁇ C gap (left and right)
- the h2 is 2 mm, the depth is 2 mm, and the length is 15 mm.
- Example 2 Experiments were performed in the same manner as in Example 1 except that the apparatus 30 in FIG. 3 was used instead of the apparatus in Example 1. As a result, it was confirmed by XMA that dimethylsiloxane was attached to the obtained fiber! Moreover, this fiber had water repellency.
- the reactor R3 has a diameter of D part and E part of 2 mm, a diameter of the central part in the direction of D ⁇ E is 8 mm, a length of D ⁇ E is 60 mm, and B ⁇ C.
- the gap h2 has a diameter of 2 mm and a length of 15 mm 3 ⁇ 4) ⁇ ⁇ .
- Example 2 The same procedure as in Example 1 was performed except that the function-imparting agent in Example 1 was replaced with palladium acetate (catalyst for plating). The appearance of the fiber changed from white to black, and it was confirmed that the catalyst was applied to the surface.
- the obtained fiber is activated in 0.72% HC1 aqueous solution for 303 minutes for 5 minutes, and the first electroless copper plating reagent is "OPC500A" 100 mL / L made by Okuno Pharmaceutical Co., Ltd. + Okuno Pharmaceutical Co., Ltd. “OPC500B” 100 mL / L was used, and the treatment was performed at 303 K for 30 minutes. In appearance, the fiber was formed with a glossy glossy film (thickness of the glossy layer: 10 m) without blistering.
- Example 11 Experiments were performed in the same manner as in Example 11 except that the apparatus 20 in FIG. 2 was used instead of the apparatus in Example 1.
- the temperature of the heater 16 was set to 200 ° C.
- the fiber was discolored from white to black in appearance, and it was confirmed that the catalyst was applied to the surface.
- the resulting fiber was treated in the same manner as in Example 11. As a result, a glossy gloss film (mesh layer thickness: 10 ⁇ m) without appearance of blisters was formed on the fiber.
- the flat disk reactor R2 has a D ⁇ E direction gap (vertical direction) hi is 2 mm, depth is 2 mm, length is 600 mm, and B ⁇ C gap (left and right)
- the h2 is 2 mm, the depth is 2 mm, and the length is 15 mm.
- the fiber is discolored from white to black in appearance, and the catalyst is applied to the surface. It was confirmed that
- the resulting fiber was treated in the same manner as in Example 11. As a result, a glossy gloss film (mesh layer thickness: 10 ⁇ m) without appearance of blisters was formed on the fiber.
- the reactor R3 has a diameter of D part and E part of 2 mm, a diameter of the central part in the direction of D ⁇ E is 8 mm, a length of D ⁇ E is 60 mm, and B ⁇ C.
- the gap h2 has a diameter of 2 mm and a length of 15 mm 3 ⁇ 4) ⁇ ⁇ .
- a function-imparting process having particularly excellent durability can be performed without using an apparatus such as an autoclave.
- Useful in applications such as fields of application, transportation and supply, and textiles.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Treatments Of Macromolecular Shaped Articles (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
Description
Claims
Priority Applications (7)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CA002663874A CA2663874A1 (en) | 2006-12-01 | 2007-11-27 | Method of imparting function to molded polymer and apparatus therefor |
EP07832525.5A EP2100913A4 (en) | 2006-12-01 | 2007-11-27 | METHOD FOR ASSIGNING A FUNCTION TO A MOLDED POLYMER AND APPARATUS THEREFOR |
BRPI0717017-3A2A BRPI0717017A2 (pt) | 2006-12-01 | 2007-11-27 | Método e aparelho para conferir uma função a um artigo formado por polímero |
CN2007800444975A CN101547962B (zh) | 2006-12-01 | 2007-11-27 | 赋予高分子成型物机能的方法及其装置 |
US12/516,133 US20100075068A1 (en) | 2006-12-01 | 2007-11-27 | Method of imparting function to molded polymer and apparatus therefor |
JP2008548225A JP5129756B2 (ja) | 2006-12-01 | 2007-11-27 | 高分子成形物への機能付与方法およびその装置 |
NO20090154A NO20090154L (no) | 2006-12-01 | 2009-01-12 | Fremgangsmate for a overfore funksjon til en formet polymer samt apparat derfor. |
Applications Claiming Priority (2)
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JP2006-325764 | 2006-12-01 | ||
JP2006325764 | 2006-12-01 |
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WO2008069041A1 true WO2008069041A1 (ja) | 2008-06-12 |
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ID=39491944
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PCT/JP2007/072800 WO2008069041A1 (ja) | 2006-12-01 | 2007-11-27 | 高分子成形物への機能付与方法およびその装置 |
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Country | Link |
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US (1) | US20100075068A1 (ja) |
EP (1) | EP2100913A4 (ja) |
JP (1) | JP5129756B2 (ja) |
KR (1) | KR20090089838A (ja) |
CN (1) | CN101547962B (ja) |
BR (1) | BRPI0717017A2 (ja) |
CA (1) | CA2663874A1 (ja) |
NO (1) | NO20090154L (ja) |
TW (1) | TW200846399A (ja) |
WO (1) | WO2008069041A1 (ja) |
Cited By (1)
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JP2010174071A (ja) * | 2009-01-27 | 2010-08-12 | Kobe Steel Ltd | 高圧処理方法および高圧処理装置 |
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CN102493135B (zh) * | 2011-11-14 | 2013-12-04 | 淄博兰雁集团有限责任公司 | 布料表面处理方法及设备 |
CN102926194A (zh) * | 2012-10-26 | 2013-02-13 | 无锡裕通织造有限公司 | 阻燃纺织品 |
US10537661B2 (en) | 2017-03-28 | 2020-01-21 | DePuy Synthes Products, Inc. | Orthopedic implant having a crystalline calcium phosphate coating and methods for making the same |
US10537658B2 (en) | 2017-03-28 | 2020-01-21 | DePuy Synthes Products, Inc. | Orthopedic implant having a crystalline gallium-containing hydroxyapatite coating and methods for making the same |
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Also Published As
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US20100075068A1 (en) | 2010-03-25 |
NO20090154L (no) | 2009-06-30 |
BRPI0717017A2 (pt) | 2013-10-08 |
KR20090089838A (ko) | 2009-08-24 |
CA2663874A1 (en) | 2008-06-12 |
CN101547962B (zh) | 2012-06-06 |
JPWO2008069041A1 (ja) | 2010-03-18 |
TW200846399A (en) | 2008-12-01 |
EP2100913A4 (en) | 2014-03-05 |
CN101547962A (zh) | 2009-09-30 |
EP2100913A1 (en) | 2009-09-16 |
JP5129756B2 (ja) | 2013-01-30 |
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