Classifications

• • 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
  • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
  • C08J9/0014—Use of organic additives
  • C08J9/0028—Use of organic additives containing nitrogen
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L25/00—Compositions of, homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Compositions of derivatives of such polymers
  • C08L25/02—Homopolymers or copolymers of hydrocarbons
  • C08L25/04—Homopolymers or copolymers of styrene
  • C08L25/06—Polystyrene
• • 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
  • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
  • C08J9/0066—Use of inorganic compounding ingredients
• • 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
  • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
  • C08J9/16—Making expandable particles
• • 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
  • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
  • C08J9/22—After-treatment of expandable particles; Forming foamed products
  • C08J9/228—Forming foamed products
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
  • C08K5/00—Use of organic ingredients
  • C08K5/16—Nitrogen-containing compounds
  • C08K5/34—Heterocyclic compounds having nitrogen in the ring
  • C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
  • C08K5/3477—Six-membered rings
  • C08K5/3492—Triazines
• • 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
  • C08J2201/00—Foams characterised by the foaming process
  • C08J2201/02—Foams characterised by the foaming process characterised by mechanical pre- or post-treatments
  • C08J2201/03—Extrusion of the foamable blend
• • 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
  • C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
  • C08J2325/02—Homopolymers or copolymers of hydrocarbons
  • C08J2325/04—Homopolymers or copolymers of styrene
  • C08J2325/06—Polystyrene

Definitions

• the present invention relates to an expandable styrene polymer containing 0.2 to 30.0 wt .-% of at least one triazine derivative, based on the expandable styrene polymer, in homogeneous distribution, a process for preparing this expandable styrene polymer by co-extruding the expandable Styrolpo- lymerisats and the at least one triazine derivative, as well as the use of at least one triazine derivative for reducing the thermal conductivity of expandable styrene polymers.
• Expandable styrene polymers containing melamine are already known from the prior art.
• WO 95/05414 discloses polymer beads containing a vinyl aromatic compound, a blowing agent and at least 0.2% by weight, for example 0.2 to 10% by weight, based on the uncoated bead, of a triazine derivative as a coating. The expert thus learns from WO 95/05414 that high amounts of triazine derivative of up to 10 wt .-% can be applied as a coating on polystyrene beads. That very high amounts of triazine derivatives can be homogeneously distributed in the polymer beads is not disclosed in WO 95/05414.
• EP 3799 and EP 69364 disclose polymer beads comprising at least one styrene homopolymer, a blowing agent, a halogen-containing flame retardant and from 0.0001 to 0.1% by weight, based on the weight of the polymer, of a triazine derivative.
• expandable styrene polymers which contain athermanous particles for lowering the thermal conductivity are known from the state of the art.
• EP 1 448 681 B1 discloses a bright, expandable vinyl aromatic polymer and a process for the preparation thereof.
• IR reflectors titanium dioxide or barium sulfate are used in the vinyl-aromatic polymer.
• expandable styrene polymers are to be provided, which are characterized by a particularly uniform, ie homogeneous distribution of the triazine derivative in the polymer.
• Another object of the present invention is to provide a process for producing the expandable styrene polymers of the present invention.
• Another object is to use triazine derivatives for reducing the thermal conductivity of expandable styrene polymers.
• the expandable styrene polymer of the invention containing from 0.2 to 30.0% by weight of at least one triazine derivative, based on the expandable styrene polymer, in homogeneous distribution.
• These objects are also achieved by a process for the preparation of the styrene polymer according to the invention by coextruding the expandable styrene polymer and at least one triazine derivative, and by the use of at least one triazine derivative for reducing the thermal conductivity of expandable styrene polymers.
• the styrenic polymer is a styrene homopolymer or a styrene copolymer having up to 40% by weight, based on the weight of the polymer, of at least one further ethylenically unsaturated monomer, in particular alkylstyrenes, for example divinylbenzene, para-methyl- ⁇ -methylstyrene, ⁇ -Methylstyrene or acrylonitrile, butadiene, acrylic acid esters or methacrylic acid esters.
• Blends of polystyrene with other polymers, in particular with rubber, polyphenylene ethers and polyolefins such as polyethylene and polypropylene are possible.
• the expandable styrene polymer according to the invention is selected from the group consisting of styrene polymers, impact polystyrene, anionically polymerized impact polystyrene, styrene-acrylonitrile polymers (SAN), acrylonitrile-butadiene-styrene polymers (ABS), acrylonitrile-styrene polymers.
• Acrylic ester polymers (ASA), methyl acrylate-butadiene-styrene polymers (MBS), methyl methacrylate-acrylonitrile-butadiene-styrene polymers (MABS), alpha-methylstyrene-acrylonitrile polymers (AMSAN), para-methyl-alpha-methylstyrene-acrylonitrile polymers (MAMSAN) and mixtures thereof.
• polystyrene is used.
• the polymers used generally have a weight average
• Molecular weight of 50,000 to 500,000 g / mol, preferably 70,000 to 400,000 g / mol, on. This weight-average molecular weight can be determined by methods known to those skilled in the art, for example by gel permeation chromatography (GPC) and comparison with corresponding reference samples.
• GPC gel permeation chromatography
• the expandable styrene polymer according to the invention generally contains from 60 to 99.7% by weight, preferably from 70 to 92% by weight, particularly preferably from 70 to 90% by weight, of at least one of the stated styrene polymers.
• the expandable styrene polymer according to the invention are from 0.2 to 30.0 wt .-% of at least one triazine derivative, based on the expandable styrene polymer, in a homogeneous distribution.
• triazine derivatives known to those skilled in the art are suitable.
• triazine derivatives of the general formula (I) are suitable.
• R 1 , R 2 , R 3 independently of one another are hydrogen, alkyl radical having 1 to 20 C atoms, cycloalkyl radical having 5 to 18 C atoms, heterocycloalkyl radical having 5 to 12 C atoms and at least one heteroatom, aryl radical having 5 to 12 C atoms Atoms, heteroaryl radical having 5 to 12 C atoms and at least one heteroatom, where the cyclic radicals can be attached via C chains having 1 to 6 carbon atoms and optionally at least one heteroatom, and / or with alkyl and / or heteroalkyl radicals having 1 to 12 C atoms and optionally at least one heteroatom may be substituted, or functional groups selected from optionally substituted amino, imino, amido, imido, hydroxy or ether group,
• heteroatoms can be selected from the group consisting of N, O, P and S.
• R 1 , R 2 and R 3 independently of one another are hydrogen, alkyl, cycloalkyl, aryl, heteroaryl having 1 to 18 C atoms or amino group (-NH 2 ). More preferably, at least one group of R 1 , R 2 and R 3 is an amino group (-NH 2 ), very particularly preferably at least two groups of R 1 , R 2 and R 3 are amino groups (-NH 2 ).
• Particularly suitable further radicals R 1 , R 2 and R 3 which are preferably present in addition to at least one, more preferably at least two, amino group (s) (-NH 2 ), are for example methyl, ethyl, n-propyl, iso-propyl, nonyl , Heptadecyl, cyclopentyl, cyclohexyl, cyclohexylmethyl, phenyl, 3-pyridyl, N-phenyl, N-dodecyl, N-octadecyl, N, N'-diphenyl, N, N'N "-triphenyl or N-cyclohexyl.
• the present invention also relates to a styrene polymer according to the invention, wherein the triazine derivative is melamine.
• melamine, melene and melon condensation products derived from melamine are preferably used, see, for example, Melamine and Guanamines, Ullmann's Encyclopedia of Industrial Chemistry, Release 2008, 7 th Edition, pages 1 to 18, John Wiley and Sons, Inc.
• Triazine derivatives which can be used according to the invention are graphitic forms of carbonitride (gC 3 N 4 ), which are obtainable, for example, by further heating of the melamine condensation products.
• Other suitable triazine derivatives are resins which are obtainable, for example, by reaction of melamine with aldehydes, such as formaldehyde. Those skilled in such resins are known.
• the said preferred melamine derivatives or melamine are commercially available or can be prepared by methods known to those skilled in the art, see, for example, Melamine and Guanamines, Ullmann's Encyclopedia of Industrial Chemistry, Release 2008, 7 th Edition, pages 1 to 18, John Wiley and Sons, Inc.
• the at least one triazine derivative, more preferably melamine is present in an amount of from 0.2 to 30.0 wt .-%, preferably 0.5 to 25.0 wt .-%, particularly preferably 1 to 25 wt .-%, most preferably 1 1 to 25 wt .-%, each based on the total expandable styrene polymer , in front.
• the expandable styrene polymers according to the invention may further comprise the customary auxiliaries and additives known to the person skilled in the art, for example athermanous particles, nucleating agents, UV stabilizers, chain transfer agents, blowing agents, plasticizers, coating compositions, water repellents, flame retardants and / or antioxidants.
• auxiliaries and additives known to the person skilled in the art, for example athermanous particles, nucleating agents, UV stabilizers, chain transfer agents, blowing agents, plasticizers, coating compositions, water repellents, flame retardants and / or antioxidants.
• the present invention therefore also relates to an expandable styrene polymer according to the invention, additionally containing athermanous particles.
• Suitable athermanous particles are, for example, selected from the group consisting of non-metal oxides, for example SiC> 2 , carbon, for example carbon black, graphite, diamond and organic dyes or dye pigments and mixtures thereof.
• Suitable organic dyes are, in particular, those which show an absorbing and / or reflective behavior in the infrared range.
• the abovementioned materials can be used either alone or in combination, ie in the form of a mixture of a plurality of materials.
• the athermanous particles are graphite and / or carbon black.
• Carbon black which can be used according to the invention preferably has a primary particle size of from 1 to 1000 nm, more preferably from 5 to 500 nm.
• the D BP absorption of the preferably used carbon blacks measured according to ASTM D2414, is 10 to 300 ml / 100 g, more preferably 20 to 200 ml / 100 g.
• the surface of the preferably used carbon blacks is preferably 2 to 400 m 2 / g, more preferably 5 to 200 m 2 / g, each measured according to ASTM D6556.
• Graphite which can be used according to the invention preferably has an average particle size of from 0.1 to 50 ⁇ m, in particular from 1 to 12 ⁇ m, a bulk density of from 100 to 800 g / l and a specific surface area of from 1 to 20 m 2 / g. It can be used natural graphite, synthetic graphite or expanded graphite.
• the preferably used graphite has an ash, determined according to DIN 51903 of generally 0 to 15 wt .-%, preferably 0.005 to 10 wt .-%, particularly preferably 0.01 to 8 wt .-%, on.
• the athermanous particles are present in the expandable styrene polymer according to the invention in an amount of from 0.05 to 30 wt .-%, particularly preferably 0.1 to 20 wt -.%, In each case based on the expandable styrene polymer, before.
• the optionally present athermanous particles may be regularly and / or irregularly shaped.
• the athermanous particles can be prepared by all methods known to those skilled in the art and / or are commercially available.
• the expandable styrene polymer according to the invention preferably contains at least one flame retardant. Therefore, the present invention also relates to a styrene polymer according to the invention, additionally containing at least one flame retardant.
• the at least one flame retardant is selected from halogen- or phosphorus-containing compounds or substances.
• organic bromine compounds are particularly preferably used.
• the organic bromine compounds should have a bromine content of ⁇ 40 wt .-%.
• Particularly suitable are aliphatic, cycloaliphatic and aromatic bromine compounds, such as hexabromocyclododecane (HBCD), Pentabrommonochlorcyclohexan, Pentabromphenyl Lallylether, 2,2 ', 6,6'-tetrabromobisphenol A-bisallyl ether, N-2,3-dibromopropyl-4,5-dibromohexahydrophthalimid and mixtures thereof.
• HBCD hexabromocyclododecane
• Pentabrommonochlorcyclohexan Pentabromphenyl Lallylether
• Suitable phosphorus-containing compounds or substances are, for example, phosphates such as trimethyl phosphate, triethyl phosphate, tributyl phosphate, tributoxyethyl phosphate, triphenyl phosphate, tricresyl phosphate, tris (chloroethyl) phosphate, tri (dichloropropyl) phosphate, tris (chloropropyl) phosphate or tris (2,3-dibromo-propyl ) phosphate, or red phosphorus.
• phosphates such as trimethyl phosphate, triethyl phosphate, tributyl phosphate, tributoxyethyl phosphate, triphenyl phosphate, tricresyl phosphate, tris (chloroethyl) phosphate, tri (dichloropropyl) phosphate, tris (chloropropyl) phosphate or tris (2,
• the at least one flame retardant is hexabromocyclododecane (HBCD).
• bromine-containing flame retardants is significantly improved by the addition of C-C or O-O-labile organic compounds.
• flame retardant synergists are dicumyl and dicumyl peroxide.
• a preferred combination consists of 0.1 to 5 wt .-%, based on the expandable styrene polymer, organic bromine compounds and 0.05 to 1, 0 wt .-%, based on the expandable styrene polymer, the CC or O- 0-labile organic compounds.
• the expandable styrene polymer according to the invention preferably contains at least one wax based on a polyolefin or a polyolefin copolymer, for example Luwax® AH3 from BASF SE.
• the at least one wax in an amount of 0.001 to 5.0 wt .-%, particularly preferably 0.01 to 2.0 wt .-%, each based on the total expandable styrene polymer before.
• the expandable styrene polymer according to the invention has the advantage over the melamine-containing styrene polymers known from the prior art that the at least one triazine derivative is distributed homogeneously according to the invention and is not present as a coating on the styrene polymer.
• homogeneous means that the at least one present triazine derivative is present distributed over the entire cross-section of the expandable styrene polymer or of expanded styrene polymer and foams which can be produced therefrom.
• expandable styrene polymer according to the invention and of expanded styrene polymerisable therefrom Styrene polymer and foams is that they are white or light, and not, as the polymers and foams according to the prior art, dark, colored.
• At least one blowing agent is present in the expandable styrene polymer according to the invention.
• the propellant is generally present in the usual amounts of from 1 to 10% by weight, preferably from 2 to 8% by weight, based on the total expandable styrene polymer.
• the blowing agents used are usually aliphatic and cycloaliphatic hydrocarbons having 3 to 10, preferably 4 to 6, carbon atoms, for example n-pentane, isopentane, cyclopentane or mixtures thereof.
• carbon dioxide, water, ethanol, methanol, acetone, methyl ethyl ketone and methyl formate are suitable.
• the present invention also relates to a process for the preparation of the expandable styrene polymer according to the invention by coextruding the expandable styrene polymer and the at least one triazine derivative.
• the at least one triazine derivative and, if appropriate, further components are mixed with a melt of the styrene polymer in an extruder, the melt being metered into a blowing agent at the same time. It is also possible to incorporate the at least one triazine derivative and optionally further components into a melt of propellant-containing styrene polymer, using, for example, screened edge fractions of a bead spectrum of propellant-containing polystyrene beads produced in a suspension polymerization.
• the at least one triazine derivative in the form of particles, preferably having a particle size of less than 1200 ⁇ m, particularly preferably less than 1000 ⁇ m, very particularly preferably given less than 100 microns, especially less than 50 microns.
• the particles preferably used have a particle size of at least 0.1 .mu.m, more preferably at least 1, 0 .mu.m.
• the triazine derivative particles preferably used according to the invention can be regularly and / or irregularly shaped.
• the at least one triazine derivative and optionally further components can be added directly to the polymer melt. It is also possible to add at least one triazine derivative and optionally further components in the form of a concentrate in the corresponding polystyrene of the melt. Preferably, polystyrene granules, and the at least one triazine derivative and optionally further components are added together in an extruder, the polymer is melted and mixed with the at least one triazine derivative and optionally other components.
• the polystyrene melt containing the propellant, at least one triazine derivative and optionally further components is squeezed out and comminuted to give propellant-containing granules. Since the existing at least one triazine derivative optionally nucleating, should preferably be cooled after pressing under pressure to avoid foaming. It is therefore expedient to carry out an underwater granulation under pressure. If the polymer melt is not treated under pressure, foaming of the expandable styrene polymer occurs, forming expanded styrene polymer particles or a foam.
• this direct foaming takes place by pressing out the blowing agent-containing melt through a corresponding nozzle, whereby it foams up, so that foam sheets of a desired size are formed directly from the expandable styrene polymer.
• the melt is pressed through another suitable nozzle and foams up, so that expanded particles are formed from the expandable styrene polymer.
• the present invention therefore also relates to a process for the preparation of an expanded styrene polymer according to the invention, in particular in the form of a particle, wherein an expandable styrene polymer according to the invention is foamed.
• the present invention also relates to an expanded styrene polymer, in particular in the form of a particle, containing from 0.2 to 30.0% by weight of at least one triazine
• the expandable styrene polymer according to the invention can be processed into foams having densities of preferably 5 to 200 g / l, particularly preferably 8 to 100 g / l and in particular from 10 to 80 g / l.
• the present invention therefore also relates to a foam which can be produced from the expandable styrene polymer according to the invention.
• the foam according to the invention has a density of 5 to 200 g / l, preferably 8 to 100 g / l, particularly preferably 10 to 80 g / l.
• the foam of the invention has a density of ⁇ 35 g / l and a thermal conductivity which is lowered so far that it meets the requirements of the heat conductivity class 040 (according to DIN 18164), Part 1. Table 4.
• the present invention also relates to a process for producing foams by preparing an expandable styrene polymer according to the invention by the process according to the invention and foaming this expandable styrene polymer.
• the production of the foams of the invention from the blowing agent-containing expandable styrene polymers is usually also carried out by methods known in the art.
• the expandable styrene polymers of the invention are prefoamed in a first step with steam in open or closed prefoams to form the corresponding expanded styrene polymer particles.
• These expanded particles generally have an average particle size of 0.3 to 12 mm, in particular from 0.5 to 8 mm.
• the prefoamed, expanded styrene polymer particles according to the invention are then welded in a second step in gas-permeable forms by means of steam to moldings or plates made of foam.
• the foam produced from this expandable styrene polymer has a reduced thermal conductivity in comparison to products according to the prior art.
• the thermal conductivity of the foam according to the invention can be measured according to DIN 52612.
• the thermal conductivity of the foam according to the invention is generally less than 38 mW / (m * K), preferably less than 37 mW / (m * K), more preferably less than 36 mW / (m * K).
• the present invention also relates to the use of the foam according to the invention for thermal insulation, for example of buildings or building parts, such. B. in the perimeter insulation.
• the foams of the invention can be applied to the outside as well as on the inside of the parts to be insulated.
• the present invention also relates to the use of the foam according to the invention for thermal insulation of machines and household appliances, such as ovens, refrigerators, freezers, water heaters or jugs.
• the present invention also relates to the use of the foam according to the invention as packaging material.
• the foam can be used particulate, so that the object to be packaged lies in a loose bed. It is also possible that a one-piece workpiece is produced from the foam according to the invention, in which the article to be packaged is embedded.
• the present invention also relates to the use of at least one triazine derivative for reducing the thermal conductivity in foams, preferably in the foams according to the invention.
• the triazine derivatives the foams, quantities and other characteristics, what has been said applies.
• Example 1 (according to the invention):
• the thermal conductivity according to DIN 52612 is 36.4 mW / (m * K) at a density of 14.4 g / l and 32.6 mW / (m * K) at a density of 24.8 g / l.
• Example 2 The procedure is as in Example 1, except that the polymer melt contains 84.0 wt .-% polystyrene 158 K (BASF SE), 0.2 wt .-% Luwax AH3 (BASF SE), 9.3 wt .-% MeI- amine powder and 6.5% by weight of pentane.
• BASF SE polystyrene 158 K
• BASF SE 0.2 wt .-% Luwax AH3
• MeI- amine powder 9.3 wt .-% MeI- amine powder and 6.5% by weight of pentane.
• the thermal conductivity according to DIN 52612 is 35.4 mW / (m * K) at a density of 14.7 g / l and 32.2 mW / (m * K) at a density of 24.9 g / l.
• Example 2 The procedure is as in Example 1, except that the polymer melt contains 74.6 wt .-% polystyrene 158 K (BASF SE), 0.2 wt .-% Luwax AH3 (BASF SE), 18.7 wt .-% MeI- amine powder and 6.5% by weight of pentane.
• BASF SE polystyrene 158 K
• BASF SE 0.2 wt .-% Luwax AH3
• MeI- amine powder 18.7 wt .-% MeI- amine powder and 6.5% by weight of pentane.
• the thermal conductivity according to DIN 52612 is 34.2 mW / (m * K) at a density of 14.6 g / l and 31.9 mW / (m * K) at a density of 24.8 g / l.
• the thermal conductivity according to DIN 52612 is 37.8 mW / (m * K) at a density of 14.5 g / l and 33.8 mW / (m * K) at a density of 25.0 g / l.

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• Inorganic Chemistry (AREA)
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• 2009
  • 2009-12-09 WO PCT/EP2009/066694 patent/WO2010066771A2/de active Application Filing
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  • 2009-12-09 EP EP09768056A patent/EP2376562A2/de not_active Withdrawn
  • 2009-12-09 CN CN200980150100XA patent/CN102245686A/zh not_active Withdrawn
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