CN104781491A - Method for producing profiled elements - Google Patents

Method for producing profiled elements Download PDF

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Publication number
CN104781491A
CN104781491A CN201380057656.0A CN201380057656A CN104781491A CN 104781491 A CN104781491 A CN 104781491A CN 201380057656 A CN201380057656 A CN 201380057656A CN 104781491 A CN104781491 A CN 104781491A
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China
Prior art keywords
section bar
porous material
organic porous
organic
composite component
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CN201380057656.0A
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Chinese (zh)
Inventor
M·弗力可
M·埃尔宾
N·蒙梅耶
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BASF SE
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BASF SE
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Priority to CN201811413109.2A priority Critical patent/CN109488160A/en
Publication of CN104781491A publication Critical patent/CN104781491A/en
Pending legal-status Critical Current

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Classifications

    • E—FIXED CONSTRUCTIONS
    • E06—DOORS, WINDOWS, SHUTTERS, OR ROLLER BLINDS IN GENERAL; LADDERS
    • E06B—FIXED OR MOVABLE CLOSURES FOR OPENINGS IN BUILDINGS, VEHICLES, FENCES OR LIKE ENCLOSURES IN GENERAL, e.g. DOORS, WINDOWS, BLINDS, GATES
    • E06B3/00—Window sashes, door leaves, or like elements for closing wall or like openings; Layout of fixed or moving closures, e.g. windows in wall or like openings; Features of rigidly-mounted outer frames relating to the mounting of wing frames
    • E06B3/04—Wing frames not characterised by the manner of movement
    • E06B3/06—Single frames
    • E06B3/08—Constructions depending on the use of specified materials
    • E06B3/20—Constructions depending on the use of specified materials of plastics
    • E06B3/205—Constructions depending on the use of specified materials of plastics moulded or extruded around a core
    • E—FIXED CONSTRUCTIONS
    • E06—DOORS, WINDOWS, SHUTTERS, OR ROLLER BLINDS IN GENERAL; LADDERS
    • E06B—FIXED OR MOVABLE CLOSURES FOR OPENINGS IN BUILDINGS, VEHICLES, FENCES OR LIKE ENCLOSURES IN GENERAL, e.g. DOORS, WINDOWS, BLINDS, GATES
    • E06B3/00—Window sashes, door leaves, or like elements for closing wall or like openings; Layout of fixed or moving closures, e.g. windows in wall or like openings; Features of rigidly-mounted outer frames relating to the mounting of wing frames
    • E06B3/04—Wing frames not characterised by the manner of movement
    • E06B3/06—Single frames
    • E06B3/08—Constructions depending on the use of specified materials
    • E06B3/20—Constructions depending on the use of specified materials of plastics
    • E06B3/22—Hollow frames
    • E06B3/221—Hollow frames with the frame member having local reinforcements in some parts of its cross-section or with a filled cavity
    • E06B3/222—Hollow frames with the frame member having local reinforcements in some parts of its cross-section or with a filled cavity with internal prefabricated reinforcing section members inserted after manufacturing of the hollow frame
    • E06B3/223—Hollow frames with the frame member having local reinforcements in some parts of its cross-section or with a filled cavity with internal prefabricated reinforcing section members inserted after manufacturing of the hollow frame the hollow frame members comprising several U-shaped parts assembled around a reinforcing core member

Abstract

The present invention relates to composite elements comprising a profile and an insulating core at least partially enclosed by the profile, wherein the insulating core consists of an organic porous material which has a thermal conductivity ranging from 13 to 30 mW/m*K, determined in accordance with DIN 12667, and a compressive strength of greater than 0.20 N/mm2, determined in accordance with DIN 53421, to methods for producing such composite elements and to the use of such a composite element for producing windows, doors, refrigerating and/or freezing units and cabinets or facade-structure elements.

Description

Be prepared into the method for shaped piece
The present invention relates to the composite component of adiabatic core comprising section bar and surrounded by section bar at least to a certain extent, wherein adiabatic core is made up of organic porous material, and described organic porous material is from 13 to 30mW/m*K according to the thermal conductivity scope that DIN 12667 measures and is greater than 0.20N/mm according to the compressive strength that DIN 53421 measures 2, relate to the preparation method of this type of composite component and this type of composite component for the preparation of window, door, refrigerator and chest freezer or the purposes of component being used as vertical-face building.
Prior art provides the measure of the multiple heat transfer property for optimizing composite material, mainly comprises the integration to hollow cavity or foam-filled hollow cavity.Therefore, the technology of preparing of this type of thermal insulation member is normally complicated, because in time using foam, there is a problem, difficult technique namely must be used to be inserted by foam in hollow cavity or in thermal insulation member, an only part for whole free space can be used to foam-filled technique.Due to the active demand of the growing heat-insulating property aspect to section bar, independent chamber has become less and chamber wall becomes thinner, therefore along with the final difficulty relevant to mould (tooling) and extruding technology and cost.In order to meet particularly relevant to the insulation aspect of building construction requirement (also becoming more and more stricter), the processing of thermal insulation material and composite component is subject to more strict requirement.
Such as, DE 28 44 006 A1 discloses a kind of method for extrusion plastic section bar, described plastic material has the core be made up of foamed plastic, the outer cover that every one side of this core is all made of plastics surrounded, operation separately is wherein used to introduce in extruder die (extuder die) by the material being used for outer cover, core material is introduced in the chamber of molding outer cover simultaneously, wherein by extruder die, the gas introduced in the chamber of outer cover is dispersed during the foaming of core material.
WO 99/16996 A1 discloses a kind of method of the frame section bar for the preparation of window or door, wherein first prepare outside section bar by a kind of thermoplastic, then the expandable mixtures based on polyurethane is introduced in section bar, and, along with completing of mixture foaming, generate between outside section bar and foam and firmly combine (secure bond).Described file also discloses a kind of method, and wherein outside section bar is first shaping, and subsequently, prefabricated instant foaming (ready-foamed) core is inserted into wherein.
DE 199 61 306 A1 also discloses a kind of by extruding the method preparing section bar.This section bar comprises the inner core of shell and foaming.In this method, first outside section bar shell is extruded, then with filling by expanded material.
DE 1 959 464 also discloses a kind of for continuing to extrude the outer cover that has and be made up of thermoplastic and having the method for the continuous section bar of foam core, wherein first prepare outer cover by thermoplastic by extruding, then the foamable material of this outer cover is filled.
EP 2 072 743 A2 discloses a kind of foam to fill the method for hollow window frame or hollow doorframe.For this reason, the plastic material by extruding preparation is capable of being combined produces finished product window frame or finished product doorframe, then by introducing foamable material with foam-filled.
Prior art also discloses the method for the section bar for the preparation of this type of with foaming core, and the plug-in unit of wherein instant foaming is inserted in prepared section bar by extruding, such as, in DE202009003392 U1 or WO 02/090703 A2 described in.
DE 10 2,009 037 851 A1 discloses for window member, door component and for the heat insulation thermal insulation member in the section bar of facade element, a kind of for window member, door component and the section bar and preparation method thereof for facade element.
EP 2 062 717 A1 also disclose a kind of in coextrusion method preparation there is the method for plastic material of foaming core, wherein can expanded material-especially solid-state can expanded material-be coextruded foam wherein in the chamber entering hollow plastic material.
But, along with becoming more strict to the demand of adiabatic aspect, use other thermal insulation materials with larger insulation effect to be also necessary.Such as, for window, there is no the further space that section bar thickness can increase, and thermal conductivity must be reduced when not causing any varied in thickness to improve thermal insulation.
Therefore other thermal insulation materials used except polyurethane foam in prior art are organic aerogel and xerogel, and it has the good performance profile as thermal insulation material.Such as, WO2012/059388 A1 discloses aeroge and xerogel, and aeroge and xerogel are as thermal insulation material and the purposes in vacuum heat-insulating plate.Manual also discloses a kind of method of the porous material for the preparation of aeroge and xerogel form, wherein makes the polyfunctional isocyanates of at least one react with the amine component of the aromatic amine comprising the multifunctional replacement of at least one.
Disclosed in this file, material has good heat-insulating property.But preparation method has prepared the material of sheet-form, method well known in the prior art therefore can not be used to include in the hollow cavity of section bar to make it.
Therefore, from prior art, an object of the present invention is to provide component, in particular for the component of window, it has good heat-insulating property and can by using the preparation of simple technology.
The present invention is by comprising section bar and the composite component of adiabatic core that surrounded by section bar at least to a certain extent realizes described object, wherein said adiabatic core is made up of organic porous material, described organic porous material is from 13 to 30mW/m*K according to the thermal conductivity scope that DIN 12667 measures, and is greater than 0.20N/mm according to the compressive strength that DIN 53421 measures 2.
Composite component of the present invention comprises section bar and at least to a certain extent by adiabatic core that section bar surrounds.For object of the present invention, section bar is herein solid structure, and it has the perforate (cutouts) or hollow cavity that extend along section bar.In the present invention, adiabatic core is positioned at these perforates or the hollow cavity of composite component.Therefore, section bar surrounds adiabatic core at least to a certain extent, and preferably surrounds completely.Therefore, adiabatic core extends along section bar.
In the present invention, adiabatic core is made up of organic porous material, and described organic porous material is from 13 to 30mW/m*K according to the thermal conductivity scope that DIN 12667 measures, and is greater than 0.20N/mm according to the compressive strength that DIN53421 measures 2.
Suitable material is known in principle.Such as, organic aerogel and xerogel have these character.
Therefore, a preferred embodiment of the present invention provides the above-mentioned composite component of adiabatic core comprising section bar and surrounded by section bar at least to a certain extent, and wherein organic porous material is a kind of material being selected from organic xerogel and organic aerogel and two or more combination thereof.
Composite component of the present invention has unexpected good heat-insulating property.Owing to using the organic porous material of low heat conductivity, although the low thickness specified due to the construction technology of thermal insulation material, also can realize meeting the ever-increasing superperformance to the active demand of heat insulation aspect herein.
Composite component of the present invention is particularly suitable for the building unit that preparation requires low u value (thermal transmittance), and example is window and door.
In addition, composite component of the present invention can easily be prepared with low cost.
Present invention also offers a kind of for the preparation of the continuation method of the composite component of adiabatic core comprising section bar and surrounded by described section bar at least to a certain extent, wherein said adiabatic core is made up of organic porous material, described organic porous material is from 13 to 30mW/m*K according to the thermal conductivity scope that DIN 12667 measures, and is greater than 0.20N/mm according to the compressive strength that DIN 53421 measures 2, wherein said section bar is around adiabatic core construct.
The organic porous material that the present invention uses is from 13 to 30mW/m*K according to the thermal conductivity scope that DIN 12667 measures, particularly 13.5 to 25mW/m*K, more preferably 14 to 22mW/m*K, particularly preferably 14.5 to 20mW/m*K.
The present invention particularly preferably is and uses organic aerogel as organic porous material, and the thermal conductivity scope of described organic aerogel is from 14 to 22mW/m*K, particularly preferably 14.5 to 20mW/m*K.
The organic porous material used in the present invention also have according to DIN 53421 measure compressive strength for being greater than 0.20N/mm 2, be particularly greater than 0.25N/mm 2, more preferably greater than 0.30N/mm 2and be especially preferably greater than 0.35N/mm 2.
The high compressive strength of described material is that rigidity a kind of weighs and allow production and the storage of material, and this facilitates composite component processing during preparation.In addition, described material also has structural meaning.
The thermal conductivity scope that the standard rigid foam being generally used for thermal insulation such as has is that compressive strength is only about 0.15N/mm from 20 to 25mW/m*K 2.Although the compressive strength of such material improves by increasing thickness, simultaneously also can improve thermal conductivity and heat-insulating property by therefore and become poorer.
For object of the present invention, xerogel is a kind of porous material, its porosity is at least 70 volume % and volume-average pore size is 50 microns at the most, and it is by sol-gel process (sol-gel process) preparation, wherein liquid phase by gel lower than liquid phase critical-temperature and lower than the critical pressure (" undercritical conditions ") of liquid phase under removed by dry.
Therefore, for object of the present invention, aeroge is a kind of porous material, its porosity is at least 70 volume % and volume-average pore size is 50 microns at the most, and it is prepared by sol-gel process, wherein liquid phase is removed by dry under the critical-temperature higher than described liquid phase and the critical pressure higher than described liquid phase (" super critical condition ") by gel.
Average pore size to be measured by mercury injection method according to DIN 66133 and is volume averaging in principle for the object of the invention.
Preferably, the volume-average pore size of porous material is 20 microns at the most.Particularly preferably, the volume-average pore size of porous material is 10 microns at the most, and is very particularly preferably 5 microns at the most, and particularly at the most 3 microns.
Although from the angle of lower thermal conductivity, the minimum-value aperture with high porosity is desirable, and preparation method defines an actual lower limit to volume-average pore size.Volume-average aperture is generally at least 50nm, preferably at least 100nm.In many cases, volume-average aperture is at least 200nm, particularly at least 300nm.
Therefore, a preferred embodiment of the present invention provides a kind of composite component of adiabatic core comprising section bar and surrounded by described section bar at least to a certain extent, wherein said adiabatic core is made up of organic porous material, described organic porous material is from 13 to 30mW/m*K according to the thermal conductivity scope that DIN 12667 measures, and is greater than 0.20N/mm according to the compressive strength that DIN 53421 measures 2, and it is a kind of material being selected from organic xerogel and organic aerogel and two or more combinations thereof.
Be preferred for the organic xerogel of object of the present invention and aeroge is described below.
Preferred organic aerogel or xerogel are based on isocyanates and optionally have reactive component based on other to isocyanates.Such as, organic aerogel or xerogel can based on isocyanates and based on OH-official can and/or NH-official can compound.
Such as, the present invention is preferably based on organic xerogel of polyurethane, polyisocyanurate or polyureas or the organic aerogel based on polyurethane, polyisocyanurate or polyureas.
Therefore, a preferred embodiment of the present invention provides a kind of composite component of adiabatic core comprising section bar and surrounded by described section bar at least to a certain extent, as mentioned above, wherein said organic porous material is be selected from following a kind of material: based on organic xerogel of polyurethane, polyisocyanurate or polyureas; Based on the organic aerogel of polyurethane, polyisocyanurate or polyureas; And two or more combinations.
Particularly preferably be organic aerogel or xerogel has reactive component based on isocyanates and based on to isocyanates, wherein use the polyfunctional aromatic amine of at least one to have reactive component as to isocyanates.Preferably organic xerogel or aeroge are based on polyureas and/or poly-isocyanurate.
" based on polyureas " to mean in organic xerogel or aeroge at least 50mol%, preferably at least 70mol%, particularly at least connection of the monomeric unit of the 90mol% form of taking urethane to connect." based on polyureas " to mean in organic xerogel or aeroge at least 50mol%, preferably at least 70mol%, particularly at least connection of the monomeric unit of the 90mol% form of taking urea to connect." based on polyisocyanurate " to mean in organic xerogel or aeroge at least 50mol%, preferably at least 70mol%, particularly at least connection of the monomeric unit of the 90mol% form of taking isocyanuric acid ester to connect." based on polyureas and/or polyisocyanurate " to mean in organic xerogel or aeroge at least 50mol%, preferably at least 70mol%, and particularly at least the form that urea connects and/or isocyanuric acid ester connects is taked in the connection of the monomeric unit of 90mol%.
Also the combination of various aeroge and xerogel can be comprised at this composite component of the present invention.For object of the present invention, composite component also can comprise multiple adiabatic core.For object of the present invention, composite component can also comprise another kind of thermal insulation material except organic porous material, such as polyurethane.
The term organic porous material hereinafter used refers to the organic aerogel or xerogel that use in the present invention.
Preferably, the organic porous material of use obtains in the method comprising following step:
A () makes the polyfunctional isocyanates of at least one (a1) and the polyfunctional aromatic amine of at least one (a2) optionally react in solvent under the existence of at least one catalyzer (a4) under the existence of water as component (a3) and optionally;
B () removes solvent to obtain aeroge or xerogel.
The component (a1) being preferred for step (a) object is explained as follows to (a4) and quantitative proportion.
The term component (a1) used hereinafter is all polyfunctional isocyanates (a1).Correspondingly, the term component (a2) used hereinafter is all polyfunctional aromatic amines (a2).It is evident that the monomer component mentioned exists with the form of reaction in organic porous material for those of ordinary skills.
For object of the present invention, the degree of functionality of compound means the number of active group in each molecule.When monomer component (a1), degree of functionality is the number of isocyanates in each molecule.When the amino group of monomer component (a2), degree of functionality is the number of active amine groups in each molecule.2 are at least in the degree of functionality of this polyfunctional compound.
If the mixture with the compound of different degree of functionality is used as component (a1) or (a2), the degree of functionality of so described component can be obtained by the number-average of each compound in each case.Polyfunctional compound comprises at least two aforementioned functional groups at each molecule.
Component (a1)
The polyfunctional isocyanates of preferred use at least one is as component (a1).
For the object of method of the present invention, the use amount of component (a1) is preferably at least 20 % by weight, particularly at least 30 % by weight, especially preferably at least 40 % by weight, very particularly preferably at least 55 % by weight, particularly at least 68 % by weight, in each case based on component (a1), (a2) and if---being correlated with---total weight of (a3), gross weight is in 100 % by weight.For the object of method of the present invention, the use amount of component (a1) is also preferably at the most 99.8 % by weight, particularly at the most 99.3 % by weight, particularly preferably at the most 97.5 % by weight, separately based on component (a1), (a2) and if---being correlated with---total weight of (a3), gross weight is in 100 % by weight.
Spendable polyfunctional isocyanates is aromatics, aliphatic series, alicyclic and/or araliphatic isocyanates.This type of polyfunctional isocyanates itself is known or prepares by known method itself.Specifically, polyfunctional isocyanates also uses as a mixture, and component (a1) also comprises various polyfunctional isocyanates in the case.The polyfunctional isocyanates that can be used as monomeric unit (a1) has plural isocyanate groups (wherein term vulcabond hereafter for the former) in the molecule of each monomer component.
The compound of particularly suitable is diphenyl methane 2,4 '-, 2,2 '-and/or 4,4 '-vulcabond (MDI), naphthyl 1,5-vulcabond (NDI), toluene 2,4-and/or 2,6-vulcabond (TDI), 3,3 '-dimethyl diphenyl vulcabond, 1,2-diphenylethane vulcabond and/or to phenylene vulcabond (PPDI), three, four, five, six, seven and/or eight methylene diisocyanates, 2-methyl pentamethylene 1,5-vulcabond, 2-ethylbutylene Isosorbide-5-Nitrae-vulcabond, pentamethylene 1,5-vulcabond, butylidene Isosorbide-5-Nitrae-vulcabond, 1-isocyanato--3,3,5-trimethyl-5-isocyanato methylcyclohexane (IPDI, IPDI), Isosorbide-5-Nitrae-and/or 1,3-bis-(isocyanatomethyl) cyclohexane (HXDI), cyclohexane Isosorbide-5-Nitrae-vulcabond, 1-hexahydrotoluene-2,4-and/or-2,6-vulcabond and dicyclohexyl methyl hydride 4,4 '-, 2,4 '-and/or 2,2 '-vulcabond.
Preferred aromatic isocyanate is as polyfunctional isocyanates (a1).When this is particularly useful for water as component (a3).
Be the particularly preferred embodiment of the polyfunctional isocyanates of component (a1) below:
I) polyfunctional isocyanates, based on toluene di-isocyanate(TDI) (TDI), particularly 2,4-TDI or the mixture of 2,6-TDI or 2,4-and 2,6-TDI;
Ii) polyfunctional isocyanates, based on methyl diphenylene diisocyanate (MDI), particularly 2,2 '-MDI or 2,4 '-MDI or 4,4 '-MDI or oligomeric MDI (it is also referred to as polyphenyl polymethylene isocyanates), or two or three mixture of aforementioned methyl diphenylene diisocyanate, or thick MDI (it generates in the process of preparation MDI), or the mixture of the oligomer of at least one MDI and the aforesaid low-molecular-weight MDI derivative of at least one;
Iii) embodiment i) at least one aromatic isocyanate and embodiment ii) the mixture of at least one aromatic isocyanate.
Oligomeric methylene diphenyl vulcabond is particularly preferably as polyfunctional isocyanates.Oligomeric methylene diphenyl vulcabond (hereinafter referred to as oligomeric MDI) comprises the mixture of multiple oligomeric condensate and the therefore derivative of methyl diphenylene diisocyanate (MDI).Polyfunctional isocyanates also can preferably be made up of the mixture singly gathering aromatic diisocyanates and oligomeric MDI.
The degree of functionality that oligomeric MDI comprises more than one is greater than the multinuclear condensation product of the MDI of 2 (particularly 3 or 4 or 5).Oligomeric MDI is known and is often referred to as the MDI of polyphenyl polymethylene isocyanates or polymerization.Oligomeric MDI is made up of the isocyanates of the MDI class with different degree of functionality usually.Oligomeric MDI is usually to use with the mixture of monomer M DI.
(on average) degree of functionality comprising the isocyanates of oligomeric MDI can change, especially from 2.4 to 3.5, particularly from 2.5 to 3 in the scope from about 2.2 to about 5.This type of mixture with the polyfunctional isocyanates of MDI class of different degree of functionality is specially thick MDI, and it produces during MDI preparation, usually by hydrochloric acid catalysis, is the form of intermediate product prepared by thick MDI.
The mixture of polyfunctional isocyanates and the multiple polyfunctional isocyanates based on MDI is known and is such as sold by BASF Polyurethanes GmbH, and commodity are called
Preferably, the degree of functionality of component (a1) is at least 2, is particularly at least 2.2, and is particularly preferably at least 2.4.The degree of functionality of component (a1) is preferably from 2.2 to 4 and particularly preferably from 2.4 to 3.
The content of the isocyanate groups of component (a1) is preferably from 5 to 10mmol/g, particularly from 6 to 9mmol/g, particularly preferably from 7 to 8.5mmol/g.The content (in mmol/g) that those skilled in the art recognize isocyanate groups be called equivalent (with gram/wait gauge) characteristic there is reciprocal relation.Obtained by the content in % by weight according to ASTM D5155-96 A in the content of the isocyanate groups of mmol/g.
In a preferred embodiment, component (a1) is selected from diphenyl methane 4 by least one, 4 '-vulcabond, diphenyl methane 2,4 '-vulcabond, diphenyl methane 2, the polyfunctional isocyanates of 2 '-vulcabond and oligomeric methylene diphenyl vulcabond.For the object of this preferred embodiment, component (a1) particularly preferably comprises oligomeric methylene diphenyl vulcabond and has the degree of functionality of at least 2.4.
The viscosity of the component (a1) used can change in wide region.Preferably the viscosity of component (a1) is from 100 to 3000mPa.s, particularly from 200 to 2500mPa.s.
Component (a2)
The present invention use the polyfunctional OH-official of at least one can or NH-official can compound as component (a2).
For the object of the preferred method of the present invention, component (a2) is the polyfunctional aromatic amine of at least one.
Component (a2) to a certain extent can original position preparation.In the embodiment of this type, the reaction for step (a) object is carried out under the existence of water (a3).Water and isocyanate groups react and generate amino group and along with the release of carbon dioxide.Therefore, polyfunctional amine is prepared as intermediate product original position to a certain extent.In the process of reaction, they and isocyanate groups react to form urea connecting key.
In this preferred embodiment, described reaction is under water (a3) and polyfunctional aromatic amine are as the existence of component (a2) and optionally carry out under the existence of catalyzer (a4).
In another embodiment, also preferably, component (a1) and polyfunctional aromatic amine optionally carry out as the reaction of component (a2) under the existence of catalyzer (a4).There is not water (a3) herein.
Polyfunctional aromatic amine is originally known as those of ordinary skill in the art.Polyfunctional amine is that each molecule has at least two amine to the amino group of responding property of isocyanates.Be primary amine group and secondary amine group to the group of responding property of isocyanates, and the reactivity of primary amine group is herein significantly higher than the reactivity of secondary amine group usually herein.
Polyfunctional aromatic amine preferably have two primary amine groups double-core aromatic compounds (dual functional aromatic amine), correspondingly there is three cores more than two primary amine groups or multi-nucleus aromatic compound, or the mixture of aforesaid compound.The polyfunctional aromatic amine of particularly preferred component (a2) is isomers and the derivative of diaminodiphenyl-methane.
The dual functional double-core aromatic amine mentioned is particularly preferably those compounds of general formula I,
Wherein R 1and R 2may be the same or different and hydrogen and the straight or branched alkyl group with 1 to 6 carbon atom can be selected from independently of each other, and wherein all substituting group Q 1to Q 5and Q 1' to Q 5' all identical or different and be selected from hydrogen, primary amine groups independently of each other and there is the straight or branched alkyl group of 1 to 12 carbon atom, wherein alkyl group can have other functional group, condition is that the compound of general formula I comprises at least two kinds of primary amine groups, wherein Q 1, Q 3and Q 5at least one be primary amine group, and Q 1 ', Q 3 'and Q 5 'at least one be primary amine group.
In one embodiment, the alkyl group for the substituting group Q object of general formula I is selected from methyl, ethyl, n-pro-pyl, isopropyl, normal-butyl, sec-butyl and the tert-butyl group.This compounds is called the aromatic amine (a2-s) of replacement hereinafter.But can be all hydrogen by preferably all substituting group Q, they are not amino defined above (term of use are unsubstituted polyfunctional aromatic amine) on that point yet.
Preferably, for the R of general formula I object 1and R 2identical or different and hydrogen, primary amine group can be selected from independently of each other and there is the straight or branched alkyl group of 1 to 6 carbon atom.Preferably, R 1and R 2be selected from hydrogen and methyl.Particularly preferably be, R 1=R 2=H.
Other suitable polyfunctional aromatic amines (a2) are specially isomers and the derivative of toluenediamine.The isomers of the particularly preferred toluenediamine for component (a2) object and derivative are toluene 2,4-diamines and/or toluene 2,6-diamines, and diethyl toluene diamine, particularly 3,5-diethyltoluene-2,4-diamines and/or 3,5-diethyltoluene-2,6-diamines.
Very particularly preferably be, component (a2) comprises at least one and is selected from 4,4 '-diaminodiphenyl-methane, 2,4 '-diaminodiphenyl-methane, 2, the polyfunctional aromatic amine of 2 '-diaminodiphenyl-methane and oligomeric diamino diphenyl methane.
Oligomeric diamino diphenyl methane comprises more than one aniline and the multinuclear methylene-bridge joint condensation product of formaldehyde.Oligomeric MDA comprises at least one, but usual multiple degree of functionality is greater than 2, particularly the oligomer of MDA of 3 or 4 or 5.Oligomeric MDA is known or prepares by known method itself.Oligomeric MDA uses with the form of the mixture with monomer M DA usually.
(on average) degree of functionality of the polyfunctional amine (comprising oligomeric MDA) of component (a2) can change, especially from 2.3 to 3.5, and particularly from 2.3 to 3 in the scope from about 2.3 to about 5.This mixture with the MDA class polyfunctional amine of different degree of functionality is a thick MDA specifically, its specifically prepare as thick MDI during aniline and formaldehyde condensation in intermediate products and prepare, it is usually by hydrochloric acid catalysis.
Particularly preferably be, the polyfunctional aromatic amine of at least one comprises the derivative of diaminodiphenyl-methane or diaminodiphenyl-methane.Particularly preferably be, the polyfunctional aromatic amine of at least one comprises oligomeric diamino diphenyl methane.Particularly preferably be, component (a2) comprises oligomeric diamino diphenyl methane as compound (a2), and its total degree of functionality is at least 2.1.Specifically, component (a2) comprises oligomeric diamino diphenyl methane and its degree of functionality is at least 2.4.
For object of the present invention, can by the reactivity using the polyfunctional aromatic amine for the replacement of component (a2) object to control primary amine group.That mention and hereafter set forth, the polyfunctional aromatic amine of the replacement that is hereafter called (a2-s) can be used alone or so that (Q all in its Chinese style I is all hydrogen, and they are not NH on that point with aforementioned (unsubstituted) diaminodiphenyl-methane 2) mixture form use.
In this embodiment, for the Q of above-mentioned formula I object 2, Q 4, Q 2' and Q 4' (comprising subsidiary definition) be preferably chosen as the compound of general formula I is had on the alpha-position relative at least one primary amine group be bonded on aromatic ring straight or branched alkyl that at least one has 1 to 12 carbon atom, wherein said alkyl can with other functional group.Preferably, Q in this embodiment 2, Q 4, Q 2' and Q 4' may be selected to be and make the aromatic amine of replacement (a2-s) comprise at least two primary amine groups, it has at alpha-position the straight or branched alkyl group that one or two has 1 to 12 carbon atom respectively, and wherein these alkyl can have other functional groups.In this sense, Q 2, Q 4, Q 2' and Q 4' in one or more may be selected to be make them be the straight or branched alkyl with 1 to 12 carbon atom, wherein these alkyl have other functional group, then preferably amino group and/or oh group and/or halogen atom as these functional groups.
Preferably, these amines (a2-s) are selected from 3,3 ', 5,5 '-tetraalkyl-4,4 '-diaminodiphenyl-methane, 3,3 ', 5,5 '-tetraalkyl-2,2 '-diaminodiphenyl-methane and 3,3 ', 5,5 '-tetraalkyl-2,4 '-diaminodiphenyl-methane, wherein may be the same or different at the alkyl of 3,3 ', 5 and 5 ' position and be selected from the straight or branched alkyl with 1 to 12 carbon atom independently of each other, wherein these groups can have other functional groups.Preferred aforesaid alkyl group: methyl, ethyl, n-pro-pyl, isopropyl, normal-butyl, sec-butyl or the tert-butyl group (not being substituted in each case).
In one embodiment, one in the more than one alkyl of substituting group Q, multiple or all hydrogen atoms can replace by halogen atom, particularly replaced by chlorine.As an alternative, one in the more than one alkyl of substituting group Q, multiple or all hydrogen atoms can by NH 2or OH replaces.But preferably, the alkyl for general formula I object is made up of carbon and hydrogen.
In an especially preferred embodiment, component (a2-s) comprises 3,3 ', 5,5 '-tetraalkyl-4,4 '-diaminodiphenyl-methane, wherein alkyl may be the same or different and independently selected from the straight or branched alkyl with 1 to 12 carbon atom, wherein these alkyl optionally can with functional group.Aforesaid alkyl is preferably selected from unsubstituted alkyl, particularly methyl, ethyl, n-pro-pyl, isopropyl, normal-butyl, sec-butyl or the tert-butyl group, is particularly preferably selected from methyl and ethyl.Very particularly preferably 3,3 ', 5,5 '-tetraethyl-4,4 '-diaminodiphenyl-methane, and/or 3,3 ', 5,5 '-tetramethyl-4,4 '-diaminodiphenyl-methane.
The polyfunctional amine of aforesaid component (a2) itself is known for those of ordinary skill in the art or prepares by known method.A kind of known method be aniline or---respectively, the derivative of aniline---with formaldehyde reaction under an acid catalysis.
As above-mentioned explanation, water can replace polyfunctional aromatic amine to a certain extent as component (a3), and wherein itself and the multifunctional aromatic isocyanate reaction in-situ of the extra component (a1) of the amount calculated in advance are to generate corresponding polyfunctional aromatic amine.
Term organogel precursor (A) below in for component (a1) to (a3).
Catalyzer (a4)
In a preferred embodiment, method of the present invention is preferably carried out under the existence of at least one catalyzer as component (a4).
The trimerization reaction of the known acceleration isocyanates of the art those of ordinary skill (these are known as trimerization catalyzer) can be used in principle and/or accelerate the reaction of isocyanates and amino (these are known as gel catalyst) and/or---accelerate in the case of using water---any catalyzer of the reaction (these are known as kicker) of isocyanates and water.
Corresponding catalyzer itself is known, and can use in aforementioned three kinds of reactions in a different manner.Therefore they can be assigned to one or more of aforementioned type according to performance.In addition, the art those of ordinary skill recognizes the reaction that also can occur except above-mentioned reaction.
Corresponding catalyzer can especially with based on their gel and the ratio of foaming for feature, be for example known in polyurethane [Polyurethanes], the 3rd edition, G.Oertel, Hanser Verlag, Munich, 1993,104 pages to 110 pages.
When not using component (a3) (namely not using water), preferred catalyzer has remarkable activity to trimerization reaction method.This has favourable effect for cancellated uniformity, thus creates particularly advantageous mechanical performance.
When using water as component (a3), preferred catalyzer (a4) has the gel of balance and the ratio of foaming, component (a1) can not excessively be accelerated with the reaction of water, net structure is had a negative impact, and obtain short gel time, therefore demould time advantageously reduces simultaneously.Preferred catalyzer has significant activity to trimerization reaction simultaneously.This has favorable influence for cancellated uniformity, thus produces particularly advantageous engineering properties.
Described catalyzer can be monomeric unit (combinative catalyzer) or can be not combinative.
The component (a4) using least effective dose (LED) is favourable.The use amount of preferred ingredient (a4) is 0.01 to 5 weight portion, particularly 0.1 to 3 weight portion, particularly preferably 0.2 to 2.5 weight portion, based on component (a1), (a2) and (a3) meter of total 100 weight portion.
The catalyzer being preferred for component (a4) object is selected from primary amine, secondary amine and tertiary amine, pyrrolotriazine derivatives, organo-metallic compound, metallo-chelate, quaternary ammonium salt, ammonium hydroxide, and the hydroxide of alkali and alkaline earth metal ions, alcoholates and carboxylate.
Suitable catalyzer is specially highly basic, such as quaternary ammonium hydroxide, such as, have tetra-alkyl ammonium hydroxide and the benzyltrimethylammonium hydroxide of 1 to 4 carbon atom at moieties; Alkali metal hydroxide, such as potassium hydroxide or NaOH; And alkali alcoholate, such as sodium methoxide, potassium ethoxide and caustic alcohol, and potassium isopropoxide.
Other suitable catalyzer are specially the alkali metal salt of carboxylic acid, such as potassium formate, sodium acetate, potassium acetate, 2 ethyl hexanoic acid potassium, Potassium Adipate and Sodium Benzoate, and there are 8 to 20 (particularly 10 to 20) carbon atoms and optionally there is the alkali metal salt of LCFA of OH side base.
Other suitable catalyzer are specially N-hydroxy alkyl quaternary ammonium carboxylate, such as trihydroxy methyl propylformic acid ammonium.
Suitable organic phosphorus compound---specifically, phospholene (phospholene) oxide---example be 1-methylphospholene oxide, 3-methyl isophthalic acid-phenyl phospholene oxides, 1-phenyl phospholene oxides, 3-methyl isophthalic acid-benzyl phospholene oxides.
Organo-metallic compound is especially known for those of ordinary skills as gel catalyst itself and is also suitable as catalyzer (a4).Such as the organo-tin compound of 2 ethyl hexanoic acid tin and dibutyl tin laurate and so on is preferred for the object of component (a4).Also preferred acetyl acetone salt, particularly zinc acetylacetonate.
Quaternary ammonium is known as gel catalyst and trimerization reaction catalyzer itself to those skilled in the art.Quaternary ammonium is particularly preferably by as catalyzer (a4).Preferred quaternary ammonium is specially N, N-dimethyl benzyl amine; N, N '-dimethyl piperazine; N, N-dimethyl cyclohexyl amine; N, N ', N "-three (dialkyl aminoalkyl)-s-hexahydrotriazine, such as N, N ', N " and-three (dimethylaminopropyl)-s-hexahydrotriazine; Three (dimethyl aminomethyl) phenol; Two (2-dimethylaminoethyl) ether; N, N, N, N, N-five methyl diethylentriamine; Methylimidazole; Methylimidazole; Aminopropylimidazol; Dimethyl benzyl amine; 1,6-diazabicylo [5.4.0]-ten one-7-alkene; Triethylamine; Triethylenediamine (IUPAC:1,4-diazabicylo [2,2,2] octane); Dimethylaminoethanol amine; Dimethylaminopropylamine; N, N-dimethylaminoethoxyethanol; N, N, N-trimethylaminoethylethanolamine; Triethanolamine; Diethanol amine; Triisopropanolamine; And diisopropanolamine (DIPA); Methyl diethanolamine; Butyl diethanolamine; And ethoxylaniline.
The catalyzer being particularly preferred for component (a4) object is selected from N, N-dimethyl cyclohexyl amine, two (2-dimethylamino ethyl) ether, N, N, N, N, N-five methyl diethylentriamine, methylimidazole, methylimidazole, aminocarbonyl propyl imidazoles, dimethyl benzylamine, 1, 6-diazabicylo [5.4.0]-ten one-7-alkene, three dimethylamino-propyl Hexahydrotriazines, triethylamine, three (dimethylamino methyl) phenol, triethylenediamine (diazabicylo [2, 2, 2] octane), dimethylamino-ethanol amine, dimethylaminopropylamine, N, TMSDMA N dimethylamine base oxethyl ethanol, N, N, N-trimethylamine groups ehtylethanolamine, triethanolamine, diethanol amine, triisopropanolamine, diisopropanolamine (DIPA), methyl diethanolamine, butyl diethanolamine, hydroxyethyl aniline, acetyl acetone salt, the ethyl hexyl hydrochlorate of thylhexoic acid ammonium and metal ion.
The use being preferred for the catalyzer (a4) of the object of the invention creates the mechanical performance with the improvement porous material of---compressive strength specifically improved---.In addition, the use of catalyzer (a4) decreases gel time, such as, accelerate gel reaction, and do not have detrimental effect to other character.
Solvent
The organic aerogel used in the present invention or xerogel are prepared in the presence of the solvent.
For object of the present invention, term solvent comprises liquid diluent, no matter that is, be sense stricto solvent or decentralized medium.Described mixture is specially true solution, colloidal solution or the dispersion as emulsion or suspension and so on.Mixture is preferably true solution.Described solvent is the compound for liquid under step (a) condition, preferred organic solvent.
The solvent used includes the mixture of organic compounds or multiple compounds in principle, and wherein said solvent is liquid providing under the temperature condition of described mixture and pressure condition (being called for short: solution condition).The composition of solvent is chosen as and described solvent is dissolved or disperses (preferred dissolution) organogel precursor.For the object of the above-mentioned method for optimizing for the preparation of organic aerogel or xerogel, preferred solvent is the solvent for organogel precursor (A), namely dissolves the solvent of organic gel precursors (A) at reaction conditions completely.
The initial reaction product of described reaction under the existence of described solvent is gel, namely by a kind of viscoplasticity chemical network thing of solvent swell.The solvent being good sweller (swelling agent) for the net formed produces the net with pore and little average pore size usually, otherwise usually produces the gross porosity net with large average pore size for the solvent that gained gel is difference sweller.
Therefore the selection of solvent affects required pore-size distribution and required porosity.The selection of solvent is also carried out usually by this way, greatly to avoid in step (a) period of the inventive method or the precipitation caused due to the formation of precipitation reaction product afterwards or flocculation.
When selecting suitable solvent, the ratio of precipitation reaction product is less than 1 % by weight usually, based on the total weight of described mixture.The amount that precipitated product is formed in specific solvent can measure to gravimetric analysis, by described reactant mixture was passed through a kind of suitable metre filter before gel point.
Spendable solvent is those solvents for isocyanates base polymer known in the state of the art.Herein preferred solvent be those for component (a1), (a2) and if---being correlated with---solvent of (a3), namely at reaction conditions substantially complete dissolved constituent (a1), (a2) and if those solvents of the composition of---being correlated with---(a3).Can described solvent be preferably inertia for component (a1), namely reactivity be there is no to it.
The example of spendable solvent is ketone; Aldehyde; Chain acid alkyl ester (alkyl alkanoates); Acid amides, such as formamide and 1-METHYLPYRROLIDONE; Sulfoxide, such as dimethyl sulfoxide (DMSO); Aliphatic and alicyclic halogenated hydrocarbons; Halogenated aromatic compound; And fluorine-containing ether.Also the mixture be made up of two or more above-claimed cpds can be used.
Also acetal can be used as solvent, be specially diethoxymethane, dimethoxymethane and DOX.
Dialkyl ether and cyclic ethers are also suitable as solvent.Preferred dialkyl ether is specially the ether that those have 2 to 6 carbon atoms, is specially methyl ethyl ether, diethyl ether, methyl-propyl ether, methyl isopropyl ether, ethyl ether, ethyl isopropyl ether, dipropyl ether, propyl isopropyl ether, Di Iso Propyl Ether, methyl butyl ether, methyl-isobutyl ether, methyl tertiary butyl ether(MTBE), ethyl-n-butyl ether, ethyl isobutyl ether and ethyl tert-butyl ether (ETBE).Particularly preferred cyclic ethers is oxolane, dioxane and oxinane.
Other preferred solvents are chain acid alkyl ester, particularly methyl formate, methyl acetate, Ethyl formate, butyl acetate and ethyl acetate.Preferred halogenated solvent is recorded in WO 00/24799, and the 4th page the 12nd is walked to the 5th page of the 4th row.
Aldehyde and/or ketone are preferred solvent.The aldehydes or ketones being suitable as solvent is specially those and corresponds to general formula R 2-(CO)-R 1solvent, wherein R 1and R 2for hydrogen or the alkyl with 1,2,3 or 4 carbon atom.Suitable aldehydes or ketones is specially acetaldehyde, propionic aldehyde, hutanal, isobutylaldehyde, 2-ethyl butyraldehyde, valeral, isopentyl aldehyde (isopentaldehyde), 2 methyl pentanal, 2-ethyl hexanal, methacrylaldehyde, MAL, crotonaldehyde, furfural, acrolein dimer, MAL dimer, 1, 2, 3, 6-tetrahydrochysene benzaldehyde, 6-methyl-3-hexamethylene olefine aldehydr, cyanaldehyde (cyanacetaldehyde), glyoxylic acid ethyl ester, benzaldehyde, acetone, metacetone, methyl ethyl ketone, methyl iso-butyl ketone (MIBK), methyl n-butyl ketone, ethyl isopropyl ketone, 2-acetyl furan, 2-methoxyl group-4-methyl-2 pentanone, cyclohexanone and acetophenone.Also above-mentioned aldehyde and the ketone of form of mixtures can be used.Particularly preferably each substituting group has ketone containing the alkyl being up to 3 carbon atoms and aldehyde as solvent.Very particularly preferably general formula is R 1(CO) R 2ketone, wherein R 1and R 2be selected from the alkyl with 1 to 3 carbon atom independently of each other.In one first preferred embodiment, ketone is acetone.In another preferred embodiment, two substituent R 1and/or R 2at least one comprise the alkyl with at least 2 carbon atoms, particularly methyl ethyl ketone.The use of aforementioned particularly preferred ketone produces the porous material with average pore size little especially in conjunction with method of the present invention.Without any the intention of restriction, now think due to the relatively high compatibility of above-mentioned particularly preferred ketone and make the pore structure of the gel obtained thin especially.
In many cases, specially suitable solvent two or more is selected from above-mentioned solvent and the mixture of the compound of complete miscibility obtains each other by using.
Preferably component (a1), (a2) and if---relevant---(a3) and if---being correlated with---(a4), and described solvent provided in an appropriate form before the reaction of the step (a) of method of the present invention.
Can preferably on the one hand component (a1) and on the other hand (a2) and if---be correlated with---(a3) and if---being correlated with---(a4) provides separately when respective in the solvent of appropriate components.There is provided separately and make before mixed processes or period carries out desirable monitoring or control to gelling reaction.
When using water as component (a3), particularly preferably provide the component (a3) independent of component (a1).Which avoid water and component (a1) when there is not component (a2) react and form network.In addition, the premix of water and component (a1) result in comparatively disadvantageous character in the uniformity of pore structure and the thermal conductivity of resulting materials.
The mixture (s) provided before step (a) is implemented also comprises conven-tional adjuvants known in the art as other components.May mention such as surface reactive material, nucleator, oxidation stabilizers, sliding agent and demolding aids, dyestuff and filler, such as about hydrolysis, light, heat or the stabilizing agent that fades, organic and/or inorganic filler, reinforcing agent and pesticide.
Other details about above-mentioned auxiliary agent and additive can see technical literature, such as, and PlasticsAdditives Handbook, the 5th edition, H.Zweifel, ed.Hanser Publishers, Munich, the 2001,1st page and 41-43 page.
In order to implement the reaction in the step (a) of described method, before the reaction of step (a), first must produce the homogeneous mixture of provided component.
Reactive component for step (a) object can provide with usual manner.In order to obtain good mixing fast, preferably make agitator or other mixing apparatus for this object.In order to avoid the defect in mixed process, the time period of preparing homogeneous mixture needs should be less than the time period that gel reaction causes gel-forming at least partially.Other mixing conditions are normally non-key, and such as mixed process can be carried out under 0.1 to 10bar (absolute pressure) at 0 to 100 DEG C, especially carries out under such as room temperature and atmospheric pressure.Once after mixture obtains uniformly, preferably close mixing apparatus immediately.
Gelling reaction comprises the sudden reaction of a sudden reaction, particularly isocyanate groups and amine or oh group.
For object of the present invention, described gel be a kind of cross-linking system based on polymer and liquid comes into contact (term of use is lyogel (solvogel or lyogel), if or use water as liquid: hydrogel (aquagel or hydrogel)).Polymer herein defines a kind of continuous print three-dimensional network mutually.
For the object of the step (a) of described method, described gel, usually by leaving standstill preparation, namely leaves standstill simply by making to comprise the container of mixture, reactor or reactor (being hereafter called gel equipment).Can preferably described in gelatinization (gel-forming) mixture no longer experience and further stir or mixing, because this may suppress the formation of gel.Now prove to cover described mixture in gelatinization or sealing gel equipment is favourable.
Described gel method itself is known for one skilled in the art and the 21st page 19 of being recorded in such as WO 2009/027310 walks to 23 page of 13 row.
For the object of described method, in step (b) (drying), remove solvent.Generally speaking, dry run can be carried out in the supercritical state, preferably with CO 2or other solvents being applicable to supercritical drying object replace this solvent after carry out.This kind of drying means itself is known to those of ordinary skill in the art.The statement of super critical condition means to require the temperature and pressure when liquid phase removed exists with supercriticality.Therefore the contraction of jel product during removal of solvents can be reduced.The material obtained from supercritical drying process is called aeroge.
But, consider the simple application of the method, preferably by being the dry gained gel of gaseous state by the liquid conversion contained in gel under the temperature and pressure lower than the critical-temperature and critical pressure that comprise the liquid contained in gel.The material obtained from precritical drying means is called xerogel.
Preferably, gained gel is by being gaseous state by described solvent conversion under lower than the critical-temperature of described solvent and the temperature and pressure of critical pressure and dry.Therefore, preferably, described dry run is not undertaken by the solvent that other solvents are replaced in advance by removing during reaction existence.Suitable method is known for those of ordinary skill in the art equally and is recorded in the 26th page the 22nd of WO-2009/027310 and walks to the 28th page of the 36th row.
Said method obtains the organic porous material with superperformance and is used as thermal insulation material.
Preferably, the density range being used as the organic porous material of adiabatic core in composite component of the present invention is from 70 to 300kg/m 3, particularly scope is from 75 to 250kg/m 3, more preferably scope is from 85 to 220kg/m 3, particularly preferably scope is from 90 to 200kg/m 3.
Therefore, a preferred embodiment of the present invention provides a kind of composite component of adiabatic core comprising section bar and surrounded by this section bar at least to a certain extent, and as mentioned above, wherein the density range of organic porous material is from 70 to 300kg/m 3.
Preferred organic porous material also has heat resistance, and it allows section bar around adiabatic core continuous structure, is such as namely stable in the extrusion of section bar.Therefore the heat resistance of preferred organic porous material is greater than 160 DEG C.
Therefore, a preferred embodiment of the present invention provides a kind of composite component of adiabatic core comprising section bar and surrounded by section bar at least to a certain extent, and as mentioned above, wherein the heat resistance of organic porous material is greater than 160 DEG C.
First the performance profile that the organic aerogel preferably used in the present invention and xerogel have ensure that the heat-insulating property that described composite component provides good, secondly, by means of stability, composite component is easily prepared.
Therefore, in the present invention especially it is possible that preparation has the adiabatic core of required size and shape, then around section bar described in adiabatic core construct.Avoiding problems and need to prepare the complex steps that then described thermal insulation material inserts hollow profile.
Adiabatic core usually can have seem for those of ordinary skills to be applicable to needed for the shape of any needs used.The cross section of described adiabatic core can be circle and/or polygonal.The shape of this core also can be uniform or heterogeneous, and such as it can have perforate, groove, ridge etc., and these shear actions can be parallel or perpendicular to preparation direction carry out.
The size of adiabatic core is generally 5 to 250mm, and preferably 10 to 150mm, particularly preferably 15 to 100mm, be specially 20 to 80mm, and when erose core, these sizes describe ultimate range in any direction.
In a preferred embodiment, the composite component that prepared by the present invention comprises a kind of adiabatic core be made up of organic porous material definitely.In the present invention, composite component also can have two, three or four cores be made up of organic porous material.When there is two, three or four cores in composite component prepared by the present invention, these cores can have identical or different shape.In the present invention, composite component also can have adiabatic core that at least one is made up of organic porous material and other adiabatic cores that at least one is made up of other materials (such as polyurethane foam).
Composite component of the present invention comprises a kind of section bar, and wherein this section bar is made up of any possible suitable material in principle, is particularly made up of thermoplastic workability material, or is made up of aluminium.
Described section bar to a certain extent or completely (preferably complete) surrounds described adiabatic core.In a preferred embodiment, described section bar also comprises the filler rod be attached on core.
Section bar itself or section bar and any thickness belonging to the filler rod of section bar are generally 1 to 20mm, preferably 2 to 15mm, particularly preferably 3 to 10mm, and section bar herein and filler rod can have identical or different thickness.In a preferred embodiment, the outer cover at section bar different loci place or filler rod have different thickness; But these thickness are identical alterable in the horizontal in the vertical.Such as this depends on the shape of this section bar, and it depends on follow-up use conversely.
The section bar of composite component prepared by the present invention preferably includes at least one thermoplastic material.This is known and such as being selected from those of following material as those of ordinary skill in the art for suitable thermoplastic material: polyolefin, such as acrylonitrile-butadiene-styrene (ABS) polymer (ABS), poly methyl methacrylate (PMMA), polyethylene (PE), polypropylene (PP), polystyrene (PS) or polyvinyl chloride (PVC); Condensation polymer, such as polyamide (PA) is as PA6 or PA6,6, poly-lactic acid ester (polylactate, PLA), Merlon (PC), polyester such as PETG (PET); Polyether-ether-ketone (PEEK); Polyadduct, such as thermoplastic polyurethane, wooden plastic composite and composition thereof.In an especially preferred embodiment, the outer cover of this section bar that prepared by the present invention comprises polyvinyl chloride (PVC).Polyvinyl chloride (PVC) and be known for those of ordinary skill in the art by the preparation of the polymerization of vinyl chloride itself.
Therefore, a preferred embodiment of the present invention provides a kind of composite component, and described composite component comprises section bar as mentioned above and at least to a certain extent by the core that section bar surrounds, wherein this section bar is made up of polyvinyl chloride or aluminium.
A particularly preferred embodiment of the present invention provides a kind of composite component of adiabatic core comprising section bar and surrounded by this section bar at least to a certain extent, and as mentioned above, wherein said section bar is made up of polyvinyl chloride.
In a preferred embodiment, described section bar comprises a kind of fusing point lower than the thermoplastic material of 220 DEG C.
For object of the present invention, composite component of the present invention can be prepared in various manners, such as continuous production or in batches prepare, the preferred continuous production of the present invention.
For object of the present invention, many methods can in order to prepare composite component of the present invention in principle, as long as they ensure that adiabatic core can accurately be introduced in section bar.
Herein preferably section bar around adiabatic core construct.This simplify the preparation method of composite component of the present invention, because this facilitate the shaping of hollow-core construction in section bar, because adiabatic core defines the shape of hollow-core construction.
Therefore, present invention also offers a kind of for the preparation of a kind of continuation method of the composite component of adiabatic core comprising section bar and surrounded by section bar at least to a certain extent, wherein said adiabatic core is made up of organic porous material, the scope of the thermal conductivity that described organic porous material measures according to DIN 12667 is from 13 to 30mW/m*K, according to DIN 53421 measure compressive strength for being greater than 0.20N/mm 2, wherein said section bar is around adiabatic core construct.
Therefore, adiabatic core can be prepared into required form and store in the present invention, and processes subsequently again.
Section bar herein can construct, such as, by extruder, particularly preferably by ring extruder by various different mode.
Therefore, a preferred embodiment of the present invention provides a kind of method of the composite component of adiabatic core comprising section bar and surrounded by section bar at least to a certain extent of preparation, as mentioned above, wherein this section bar by ring extruder around adiabatic core continuous structure.
Other embodiment of the present invention one also provides a kind of for the preparation of a kind of method of the composite component of adiabatic core comprising section bar and surrounded by section bar at least to a certain extent, as mentioned above, wherein this section bar around adiabatic core by multiple piece construction.
Such as, in the present invention, section bar described herein can be constructed around adiabatic core by multiple preformed member, but to parts preformed, can insert adiabatic core equally, then such as by making section bar close.
If described section bar is constructed by multiple preform part around adiabatic core, then all parts of this section bar can differently be connected to each other, such as, by bonding or by weld or by pushing-being connected (push-fit connections) (" cutting ").
Therefore, described section bar can construct from thermoplasticity machinable material, such as polyvinyl chloride.
Therefore, the present invention's preferred embodiment provides a kind of method of the composite component of adiabatic core comprising section bar and surrounded by section bar at least to a certain extent of preparation, and as mentioned above, wherein this section bar is made up of polyvinyl chloride.
In the present invention, composite component is preferably prepared by ring extruder.The method comprises and to be introduced into by adiabatic core in the subsidiary extruder for the preparation of the extrusion die of annular section bar herein, thus is loaded by adiabatic core in the section bar be made up of at least one thermoplastic material and also therefore obtain composite component.
Adiabatic core is introduced in an extruder with the punch die of reproducible profile shapes herein.Then the thermoplastic being intended to be formed outer cover is applied to the form of melting on the core in extruder.The embodiment of this extruder used in the present invention is in the art known by those of ordinary skill and is such as recorded in WO 2009/098068.
Method of the present invention is preferably carried out at the temperature of the molten thermoplastic material of section bar, such as, from 100 to 220 DEG C, particularly preferably from 130 to 190 DEG C.
The solidification temperature preference of the thermoplastic in the downstream of extruder as from 25 to 180 DEG C, preferably from 50 to 150 DEG C.
Extruding of thermoplastic material itself is known for those skilled in the art and is recorded in such as " Einf ü hrung in die Kunststoffverarbeitung " [explanation (Introduction to plastics processing) of plastic processing], 5th edition, in September, 2006; 87-180 page; Walter Michaeli; Hanser Fachbuchverlag.
If be introduced in section bar by reinforcement in the present invention, when being introduced into extruder, this reinforcement can have its last shape, such as banded.In this second embodiment, this reinforcement is extruded with the outer cover of section bar in an extruder simultaneously.For this reason, the material of this reinforcement is preferably introduced with molten condition by extruder.
In a preferred embodiment, the size of reinforcement depends on the size of section bar and the stability of this stiffening profile of maximizing.Such design reinforcement is such as, in order to reduce or at least not increase the Heat transmission in section bar, in window frame or doorframe.
In the present invention, section bar also can construct around adiabatic core discontinuously, such as, constructed by multiple preform part; The all parts of this section bar can differently be connected to each other, such as, by bonding or by weld or by pushing-being connected (" cutting ").
For object of the present invention, in an alternative, also can first prepare complete section bar, then adiabatic core is inserted in preformed hollow cavity.In this embodiment, section bar is not around adiabatic core construct.
In this kind of alternative method, any conventional method can be used to be introduced in section bar by adiabatic core, such as, use suction to insert or pressure inserts, preferably use pressure to insert.
Therefore an alternate embodiment of the present invention also provides and a kind ofly prepares the method for the composite component of adiabatic core comprising section bar and surrounded by section bar at least to a certain extent, wherein adiabatic core is made up of organic porous material, this organic porous material is from 13 to 30mW/m*K according to the thermal conductivity scope that DIN 12667 measures, and is greater than 0.20N/mm according to the compressive strength that DIN 53421 measures 2; Pressure is wherein used to be inserted in section bar by adiabatic core.
Composite component of the present invention has low thermal conductivity for identical adiabatic thickness, and thus this makes them be suitable for building unit, such as, for window or door.
Therefore the independent building component (wall, window) of building envelope can meet U value limit (U value=hot transfer ratio, unit W/m 2* K), wherein these parts provide good thermal insulation.
Therefore, present invention also offers organic porous material as the purposes of thermal insulation material in section bar, described organic porous material is from 13 to 30mW/m*K according to the thermal conductivity scope that DIN 12667 measures, and is greater than 0.20N/mm according to the compressive strength that DIN 53421 measures 2.
Therefore, a preferred embodiment of the present invention provides organic porous material as the purposes of thermal insulation material in section bar, and as mentioned above, wherein this section bar is used to prepare window, door, refrigerator and chest freezer or the component as vertical-face building
Another embodiment of the present invention also provide composite component of the present invention or the composite component that obtained by method of the present invention for the preparation of window, door, refrigerator and chest freezer or the purposes of component being used as vertical-face building.
Composite component of the present invention is suitable for the construction of various building unit, such as window.
Therefore, specifically, another embodiment of the invention also provides a kind of window comprising a kind of composite component, described composite component comprises section bar and at least to a certain extent by adiabatic core that section bar surrounds, wherein adiabatic core is made up of organic porous material, this organic porous material is from 13 to 30mW/m*K according to the thermal conductivity scope that DIN 12667 measures, and is greater than 0.20N/mm according to the compressive strength that DIN53421 measures 2.
Following is a list the example of embodiment of the present invention, but do not limit the present invention.Specifically, the present invention also comprises and to obtain from following subordinate item and to form the embodiment of combination thus.
1. the composite component of adiabatic core comprising section bar and surrounded by section bar at least to a certain extent, wherein adiabatic core is made up of organic porous material, described organic porous material is from 13 to 30mW/m*K according to the thermal conductivity scope that DIN12667 measures, and is greater than 0.20N/mm according to the compressive strength that DIN 53421 measures 2.
2. the composite component according to embodiment 1, wherein organic porous material is a kind of and two or more combination be selected from organic xerogel and organic aerogel.
3. the composite component according to embodiment 1 or 2, wherein organic porous material is the one being selected from following material: based on organic xerogel of polyurethane, poly-isocyanurate or polyureas; Based on the organic aerogel of polyurethane, poly-isocyanurate or polyureas; And two or more combinations.
4. the composite component according to any one of embodiment 1 to 3, wherein the density range of organic porous material is from 70 to 300kg/m 3.
5. the composite component according to any one of embodiment 1 to 4, wherein the heat resistance of organic porous material is greater than 160 DEG C.
6. the composite component according to any one of embodiment 1 to 5, its medium section is made up of polyvinyl chloride or aluminium.
7. prepare the continuation method of composite component for one kind, described composite component comprises section bar and at least to a certain extent by adiabatic core that section bar surrounds, wherein adiabatic core is made up of organic porous material, this organic porous material is from 13 to 30mW/m*K according to the thermal conductivity scope that DIN 12667 measures, and is greater than 0.20N/mm according to the compressive strength that DIN 53421 measures 2, wherein said section bar is around adiabatic core construct.
8. the method according to embodiment 7, wherein said section bar constructs around adiabatic core continuously by ring extruder.
9. the method according to embodiment 7, wherein said section bar is by multiple piece construction around adiabatic core.
10. the method according to any one of embodiment 7 to 9, wherein said section bar is made up of polyvinyl chloride.
11. organic porous materials are as the purposes of thermal insulation material in section bar, and described organic porous material is from 13 to 30mW/m*K according to the thermal conductivity scope that DIN 12667 measures, and are greater than 0.20N/mm according to the compressive strength that DIN 53421 measures 2.
12. according to the purposes of embodiment 11, and wherein said section bar is used to prepare window, door, refrigerator and chest freezer, or is used as the component of vertical-face building.
13. composite components according to any one of embodiment 1 to 6 or the composite component that obtained by the method according to any one of embodiment 7 to 10 are for the preparation of window, door, refrigerator and chest freezer or the purposes of component being used as vertical-face building.
14. 1 kinds of composite components of adiabatic core comprising section bar and surrounded by section bar at least to a certain extent, wherein adiabatic core is made up of organic porous material, this organic porous material is from 13 to 30mW/m*K according to the thermal conductivity scope that DIN12667 measures, and is greater than 0.20N/mm according to the compressive strength that DIN 53421 measures 2, and this organic porous material is a kind of material being selected from organic xerogel, organic aerogel and two or more combination thereof.
15. 1 kinds of composite components of adiabatic core comprising section bar and surrounded by section bar at least to a certain extent, wherein adiabatic core is made up of organic porous material, this organic porous material is from 13 to 30mW/m*K according to the thermal conductivity scope that DIN12667 measures, and is greater than 0.20N/mm according to the compressive strength that DIN 53421 measures 2, and this organic porous material is the one being selected from following material: based on organic xerogel of polyurethane, poly-isocyanurate or polyureas; Based on the organic aerogel of polyurethane, poly-isocyanurate or polyureas; And two or more combinations.
16. 1 kinds of composite components of adiabatic core comprising section bar and surrounded by section bar at least to a certain extent, wherein adiabatic core is made up of organic porous material, this organic porous material is from 13 to 30mW/m*K according to the thermal conductivity scope that DIN12667 measures, and is greater than 0.20N/mm according to the compressive strength that DIN 53421 measures 2, and this organic porous material is the one being selected from following material: based on organic xerogel of polyurethane, poly-isocyanurate or polyureas; Based on the organic aerogel of polyurethane, poly-isocyanurate or polyureas; And two or more combinations.Wherein the density range of this organic porous material is 70 to 300kg/m 3.
17. 1 kinds of composite components of adiabatic core comprising section bar and surrounded by section bar at least to a certain extent, wherein adiabatic core is made up of organic porous material, this organic porous material is from 13 to 30mW/m*K according to the thermal conductivity scope that DIN12667 measures, and is greater than 0.20N/mm according to the compressive strength that DIN 53421 measures 2, and this organic porous material is the one being selected from following material: based on organic xerogel of polyurethane, poly-isocyanurate or polyureas; Based on the organic aerogel of polyurethane, poly-isocyanurate or polyureas; And two or more combinations, wherein the heat resistance of this organic porous material is greater than 160 DEG C.
18. composite components according to embodiment 17, wherein this section bar is made up of polyvinyl chloride or aluminium.
19. 1 kinds of composite components of adiabatic core comprising section bar and surrounded by section bar at least to a certain extent, wherein adiabatic core is made up of organic porous material, this organic porous material is from 13 to 30mW/m*K according to the thermal conductivity scope that DIN12667 measures, and is greater than 0.20N/mm according to the compressive strength that DIN 53421 measures 2, and this organic porous material is the one being selected from following material: based on organic xerogel of polyurethane, poly-isocyanurate or polyureas; Based on the organic aerogel of polyurethane, poly-isocyanurate or polyureas; And two or more combinations, and wherein this section bar is made up of polyvinyl chloride or aluminium.
20. 1 kinds of continuation methods preparing composite component, described composite component comprises section bar and at least to a certain extent by adiabatic core that section bar surrounds, wherein adiabatic core is made up of organic porous material, this organic porous material is from 13 to 30mW/m*K according to the thermal conductivity scope that DIN 12667 measures, and is greater than 0.20N/mm according to the compressive strength that DIN 53421 measures 2, wherein said section bar constructs around adiabatic core continuously by ring extruder.
21. 1 kinds of continuation methods preparing composite component, described composite component comprises section bar and at least to a certain extent by adiabatic core that section bar surrounds, wherein adiabatic core is made up of organic porous material, this organic porous material is from 13 to 30mW/m*K according to the thermal conductivity scope that DIN 12667 measures, and is greater than 0.20N/mm according to the compressive strength that DIN 53421 measures 2, wherein said adiabatic core is inserted in section bar under stress.
22. 1 kinds of windows comprising composite component, described composite component comprises section bar and at least to a certain extent by adiabatic core that section bar surrounds, wherein adiabatic core is made up of organic porous material, this organic porous material is from 13 to 30mW/m*K according to the thermal conductivity scope that DIN 12667 measures, and is greater than 0.20N/mm according to the compressive strength that DIN 53421 measures 2.
23. according to claim 14 to the composite component described in 19 any one or the composite component that obtained by the method according to any one of embodiment 20 to 22 for the preparation of window, door, refrigerator and chest freezer or the purposes of component being used as vertical-face building.
Following embodiment contributes to illustrating the present invention, but to theme of the present invention definitely without any restrictive effect.
Embodiment
Preparation embodiment: aeroge
1. raw material
Following compound is used to prepare gel:
Component a1: oligomeric MDl ( m200), described MDI is 30.9g/100g according to the NCO content of ASTMD5155-96A, and degree of functionality is about 3, is 2100mPa.s (being hereinafter " compound M200 ") according to the viscosity of DIN53018 at 25 DEG C.
Component a2:3,3', 5,5'-tetraethyl-4,4'-diaminodiphenyl-methane (being hereinafter " MDEA ")
Catalyzer: butyl diethanolamine, methyl diethanolamine
2. prepare embodiment 1
At 20 DEG C, in glass beaker, under agitation 80g compound M200 is dissolved in the 2-butanone of 220g.In second glass beaker, by 8g compound MDEA and 8g butyl glycol amine and 1g water-soluble in the 2-butanone of 220g.By the two kinds of solution mixing obtained in step (a).This results in low viscous clarified mixture.This mixture is at room temperature left standstill 24 hours to harden.Then gel taken out from glass beaker and pass through to use supercritical CO in autoclave 2carry out solvent extraction and dry.
Gel monolith is taken out from glass beaker and is transferred in the autoclave of 25 liters.The acetone of >99% to be loaded in autoclave to make acetone cover gel monolith completely, then autoclave is sealed.The method can stop at gel monolith and supercritical CO 2the contraction that before contact, gel monolith causes due to the volatilization of organic solvent.By gel monolith at CO 2drying 24 hours under steam.Pressure (in drying system) is 115 to 120bar; Temperature is 40 DEG C.Finally, at the temperature of 40 DEG C, in about 45 minutes, in a controlled manner intrasystem Pressure Drop is low to moderate atmospheric pressure.Open autoclave, and take out dried gel monolith.
The porous material obtained has the density of 150g/L.
According to DIN EN 12667 by using the protective heat plate measuring apparatus thermal conductivity λ purchased from Hesto (Lambda Control A50).Thermal conductivity at 10 DEG C is 20.0mW/m*K.
Tensile strength according to DIN 53292 mensuration is 0.87N/mm 2.
Modulus of elasticity according to DIN 53292 mensuration is 15.3N/mm 2.
3. prepare embodiment 2
At 20 DEG C, in glass beaker, under agitation 80g compound M200 is dissolved in the 2-butanone of 220g.In second glass beaker, by 8g compound MDEA and 8g butyl glycol amine and 2g water-soluble in the 2-butanone of 220g.By the two kinds of solution mixing obtained in step (a).This results in low viscous clarified mixture.This mixture is at room temperature left standstill 24 hours to harden.Then gel taken out from glass beaker and pass through to use supercritical CO in autoclave 2carry out solvent extraction and dry.
Gel monolith is taken out from glass beaker and is transferred in the autoclave of 25 liters.The acetone of >99% to be loaded in autoclave to make acetone cover gel monolith completely, then autoclave is sealed.The method can stop at gel monolith and supercritical CO 2the contraction that before contact, gel monolith causes due to the volatilization of organic solvent.By gel monolith at CO 2drying 24 hours under steam.Pressure (in drying system) is 115 to 120bar; Temperature is 40 DEG C.Finally, at the temperature of 40 DEG C, in about 45 minutes, in a controlled manner intrasystem Pressure Drop is low to moderate atmospheric pressure.Open autoclave, and take out dried gel monolith.
The porous material obtained has the density of 153g/L.
According to DIN EN 12667 by using the protective heat plate measuring apparatus thermal conductivity λ purchased from Hesto (Lambda Control A50).Thermal conductivity at 10 DEG C is 21.0mW/m*K.
Be 0.64N/mm according to the compressive strength that DIN 53421 measures when compression 5.3% 2.
Modulus of elasticity is 31N/mm 2.
4. prepare embodiment 3
At 20 DEG C, in glass beaker, under agitation 80g compound M200 is dissolved in the ethyl acetate of 250g.In second glass beaker, 8g compound MDEA and 8g methyl diethanolamine are dissolved in the ethyl acetate of 250g.By the two kinds of solution mixing obtained in step (a).This results in low viscous clarified mixture.This mixture is at room temperature left standstill 24 hours to harden.Then gel taken out from glass beaker and pass through to use supercritical CO in autoclave 2carry out solvent extraction and dry.
Gel monolith is taken out from glass beaker and is transferred in the autoclave of 25 liters.The acetone of >99% to be loaded in autoclave to make acetone cover gel monolith completely, then autoclave is sealed.The method can stop at gel monolith and supercritical CO 2the contraction that before contact, gel monolith causes due to the volatilization of organic solvent.By gel monolith at CO 2drying 24 hours under steam.Pressure (in drying system) is 115 to 120bar; Temperature is 40 DEG C.Finally, at the temperature of 40 DEG C, in about 45 minutes, in a controlled manner intrasystem Pressure Drop is low to moderate atmospheric pressure.Open autoclave, and take out dried gel monolith.
The porous material obtained has the density of 110g/L.
According to DIN EN 12667 by using the protective heat plate measuring apparatus thermal conductivity λ purchased from Hesto (Lambda Control A50).Thermal conductivity at 10 DEG C is 20.0mW/m*K.
Compressive strength is 0.52N/mm when compression 10% 2.

Claims (13)

1. the composite component of adiabatic core comprising section bar and surrounded by section bar at least to a certain extent, wherein adiabatic core is made up of organic porous material, described organic porous material is from 13 to 30mW/m*K according to the thermal conductivity scope that DIN12667 measures, and is greater than 0.20N/mm according to the compressive strength that DIN 53421 measures 2.
2. composite component according to claim 1, wherein organic porous material is a kind of and two or more combination be selected from organic xerogel and organic aerogel.
3. composite component according to claim 1 and 2, wherein organic porous material is the one being selected from following material: based on organic xerogel of polyurethane, poly-isocyanurate or polyureas; Based on the organic aerogel of polyurethane, poly-isocyanurate or polyureas; And two or more combinations.
4. the composite component according to any one of claims 1 to 3, wherein the density range of organic porous material is from 70 to 300kg/m 3.
5. the composite component according to any one of Claims 1-4, wherein the heat resistance of organic porous material is greater than 160 DEG C.
6. the composite component according to any one of claim 1 to 5, its medium section is made up of polyvinyl chloride or aluminium.
7. prepare the continuation method of composite component for one kind, described composite component comprises section bar and at least to a certain extent by adiabatic core that section bar surrounds, wherein adiabatic core is made up of organic porous material, described organic porous material is from 13 to 30mW/m*K according to the thermal conductivity scope that DIN 12667 measures, and is greater than 0.20N/mm according to the compressive strength that DIN 53421 measures 2, wherein said section bar is around adiabatic core construct.
8. method according to claim 7, wherein said section bar constructs around adiabatic core continuously by ring extruder.
9. method according to claim 7, wherein said section bar is by multiple piece construction around adiabatic core.
10. the method according to any one of claim 7 to 9, wherein said section bar is made up of polyvinyl chloride.
11. organic porous materials are as the purposes of thermal insulation material in section bar, and wherein said organic porous material is from 13 to 30mW/m*K according to the thermal conductivity scope that DIN 12667 measures, and are greater than 0.20N/mm according to the compressive strength that DIN 53421 measures 2.
12. purposes according to claim 11, wherein said section bar is used to prepare window, door, refrigerator and chest freezer, or is used as the component of vertical-face building.
13. composite components according to any one of claim 1 to 6 or the composite component that obtained by the method according to any one of claim 7 to 10 are for the preparation of window, door, refrigerator and chest freezer or the purposes of component being used as vertical-face building.
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