CN1086626A - Epoxy impregnated tape backing - Google Patents

Epoxy impregnated tape backing Download PDF

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Publication number
CN1086626A
CN1086626A CN93118640A CN93118640A CN1086626A CN 1086626 A CN1086626 A CN 1086626A CN 93118640 A CN93118640 A CN 93118640A CN 93118640 A CN93118640 A CN 93118640A CN 1086626 A CN1086626 A CN 1086626A
Authority
CN
China
Prior art keywords
backing
flexible belt
adhesive
belt backing
family
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN93118640A
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Chinese (zh)
Inventor
K·施里哈
J·N·凯伦
R·W·普里劳
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
3M Co
Original Assignee
Minnesota Mining and Manufacturing Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Minnesota Mining and Manufacturing Co filed Critical Minnesota Mining and Manufacturing Co
Publication of CN1086626A publication Critical patent/CN1086626A/en
Pending legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/14—Polycondensates modified by chemical after-treatment
    • C08G59/1433—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds
    • C08G59/1438—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds containing oxygen
    • C08G59/145—Compounds containing one epoxy group
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
    • C08G59/22—Di-epoxy compounds
    • C08G59/226—Mixtures of di-epoxy compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
    • C08G59/22—Di-epoxy compounds
    • C08G59/24—Di-epoxy compounds carbocyclic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
    • C08G59/32—Epoxy compounds containing three or more epoxy groups
    • C08G59/38—Epoxy compounds containing three or more epoxy groups together with di-epoxy compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/68—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/20—Adhesives in the form of films or foils characterised by their carriers
    • C09J7/205—Adhesives in the form of films or foils characterised by their carriers characterised by the backing impregnating composition
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/20—Adhesives in the form of films or foils characterised by their carriers
    • C09J7/21—Paper; Textile fabrics
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/20—Adhesives in the form of films or foils characterised by their carriers
    • C09J7/29—Laminated material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/002—Inhomogeneous material in general
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
    • H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
    • H01B3/40—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes epoxy resins
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00—Additional features of adhesives in the form of films or foils
    • C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
    • C09J2301/16—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the structure of the carrier layer
    • C09J2301/162—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the structure of the carrier layer the carrier being a laminate constituted by plastic layers only

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Emergency Medicine (AREA)
  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Adhesive Tapes (AREA)
  • Laminated Bodies (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The present invention relates to a kind of flexible belt backing, wherein contain a kind of matrix that has been coated with a kind of photopolymerization epoxy composite thereon, described composition contains multiple epoxides, comprise at least a this group and at least a aliphatic epoxide of forming by bisphenol A epoxide and cycloaliphatic epoxide that be selected from; Contain 0.1～2% at least a can be at the cationic initator of the organic metal of 200～600 nano wave length initiated polymerizations; Also contain at least a promoter, wherein said backing need not heating steps with regard to full solidification in irradiation after 1～15 second.

Description

Epoxy impregnated tape backing
The present invention relates to backing, wherein comprise or be coated with or flooded the flexible matrix of polymerisable sun from sensing composition.Polymerization realizes as light trigger with the ionic organo-metallic compound.
(chemistry) species formation polymerization crosslinking structure with the cation sensitivity is well-known.The whole bag of tricks that is used to make these species polymerizations is disclosed in the prior art, comprising the polymerization of epoxy material.The report the earliest of epoxy material polymerization relies on the hot curing of using such as polyfunctional amine or acid anhydride.See also Polymers such as Industrial, Ulrich, Hanser Publishing Co., Copyright 1982, pp.91-94.
Recently, the more convenient method that at room temperature makes curable epoxide is disclosed, i.e. photopolymerization.These class methods rely on the active species that produce the energy initiated polymerization and need not heat.This is by using the active light trigger of the light of specific wavelength to be realized the most frequently.The light trigger that can be used for the cation sensitive species has three major types, i.e. aryl diazonium salts; Sulfonium salt, salt compounded of iodine and allied compound, general designation " " salt, and organo-metallic compound; See also the photo-crosslinking of Photocrosslinking of Epoxy Resins(epoxy resin), Advances in Polymer Science(polymer science progress) 78, F.Lohse ﹠amp; H.Zweifel, Springer-Verlag Publ., 1986, pp.61-81.
Epoxy resin is used to be with backing, also is known in present technique.
Epoxy resin is used to be with backing, also is known in present technique.
JAP61197869 discloses the composition that uses the epoxy monomer admixture that contains porous porous fabric or matrix.This impregnate fabric can be cured to rigid state by being exposed to the ultraviolet energy.
JP58002372 discloses the interpolation fire retardant and has come to provide this ideal characterisitics to consolidated structures.
United States Patent (USP) 4,704,322 disclose a kind of three layers of electrical insulation tape of epoxy impregnation.A mica sheet internal layer is clipped between the two-layer Si Kelinbu (scrim).This composite construction is coated with a kind of low viscosity, fluid, polymerisable epoxy composite.This composition comprises three kinds of key components: a kind of epoxy resin, a kind of phenol promoter and a kind of organic titanate.Coating is with realization by this fluid is brushed.This band has absorbed fluid, thereby has flooded this epoxy composite.Heating makes this band be transformed into B-level (B-staged) state.In this state, this structure is stable under normal storage condition.When wishing, can be transformed into this electrical insulation tape a kind of full solid state of rigidity by heating.
United States Patent (USP) 5,089,536 disclose and use the organic metal light trigger to carry out the cationic polymerization of far-ranging polymerizable species.Yet it does not relate to when the relative curing rate relatively time the with the cationic polymerization initator of other type such as diazonium catalyst or other " " catalyst.It does not discuss for example flexible control of porous fabric material of article yet, and these article can flood epoxy composite, solidify under suitable influence of actinic radiation subsequently.This piece list of references is also mentioned the epoxy composite that needs solvent to provide to have expection viscosity, and this is undesirable.
In addition, majority contains the prior art backing rather unstable of epoxy monomer, and must use in the short time of adding curing agent.They must further be processed after polymerization, normally heat, and just can represent any bin stability.This is time taking, also is high the expense.
The present inventor has now found that, by using the epoxy admixture that makes up with some organic metal light trigger, can simplify technology, improves the backing speed of production, can also obtain having predetermined flexible backing.Use the organic metal light trigger can more effectively promote the cationic polymerization reaction as " " salt than previously disclosed cationic polymerization initator.
Even it also is stable that better composition of the present invention has light trigger to exist, till being exposed to suitable actinic radiation.Therefore, the present invention is by eliminating the demand of solvent and a kind of faster, manufacture method of saving more money being provided, and promptly removes curing schedule behind the time taking high temperature from, overcome with former backing and made relevant problem.
Also further find,, might control the flexible of the backing that forms by changing coating or dip composition.
The invention provides to various adhesives useful, have controlled flexible, the electrical insulation tape backing that has both required electrical property and handling property.
Band backing of the present invention comprises a kind of matrix that is coated with or floods the epoxy material admixture, at least a organic metal light trigger and at least a promoter.
Specifically, the invention provides a kind of band backing, wherein comprise a kind of matrix that is coated with the photopolymerization epoxy composite thereon, described composition comprises
A) multiple epoxides comprises at least a this group and at least a aliphatic epoxide of being made up of cycloaliphatic epoxide and bisphenol A epoxide that be selected from,
B) 0.1～2% at least a can the organic metal cationic initiator of 200～600 nano wave length initiated polymerizations and
C) at least a promoter, wherein said backing with regard to full solidification, need not heating steps after shining 1～15 second.
Better backing of the present invention comprises a kind of porous matrix, is therefore flooded by the epoxy composite of photopolymerization.
In a better embodiment of the present invention, use a kind of polyester matrix, thereby provide the electrical insulation tape that contains a kind of adhesive and a kind of flexible backing, described backing to comprise a kind of matrix that is coated with following ingredients thereon,
A) a kind of photopolymerisable polymer wherein contains multiple epoxides, comprises at least a this group and at least a aliphatic epoxide of being made up of cycloaliphatic epoxide and bisphenol A epoxide that be selected from,
B) at least a organic light trigger, wherein comprise the cationic ionic salt of a kind of organometallic complex at least one catalytically effective amount, that be enough to cause polymerization, described metal be selected from periodic table IV B family, V B family, VI B family, VII B family and VIII B family element and
C) at least a promoter,
The dielectric strength of wherein said band is at least 3.5 kilovolts～10 kilovolts (KV), and insulation resistance is at least 1 * 10 6Megaohm.
Employed these terms of this paper have following implication:
1. " photopolymerization " this term means that a kind of compound or composition can polymerizations when by scope being ultraviolet emission (light) irradiation of about 180 nanometers～about 420 nanometers.
2. " dipping " this term means that a kind of matrix contains the porosity that is filled into saturation point by photopolymerisable compositions.
3. " epoxides " this term is used for representing a kind of material that contains at least one epoxy radicals." epoxy " this term is used interchangeably, and also is used for representing a kind of resin that contains the epoxides admixture.
The epoxy admixture that can be used for band backing of the present invention can be aliphatic, cyclic aliphatic, aromatics or heterocycle, and its epoxide equivalent typically is 1～6.Specifically, available have aliphatic series, cyclic aliphatic with glycidol ether type 1,2-epoxides, propylene oxide for example, chloropropylene oxide, styrene oxide, vinyl cyclohexene dioxide, glycidol, oxidation butadiene, glycidyl methacrylate etc.
Representational epoxides comprises the glycidol ether of bisphenol-A, vinyl cyclohexene dioxide, 3,4-7-oxa-bicyclo[4.1.0 carboxylic acid 3,4-epoxycyclohexyl methyl ester, 3,4-epoxy-6-methylcyclohexanecarboxylic acid 3,4-epoxy-6-methylcyclohexyl methyl ester, adipic acid two (3,4-epoxy-6-methylcyclohexyl methyl ester), with the aliphatic epoxy of polypropylene glycol modified, titanium dioxide dipentene, epoxidised polybutadiene, silicone epoxy, 1,4-butanediol diglycidyl ether, many Synthesis of Oligo Ethylene Glycol of novolaks, the resorcinol diglycidyl ether, the polyethylene glycol diepoxide, polyacrylate epoxides, polyurethane modified epoxy thing, multifunctional flexible loop oxide and their mixture.
Epoxides comprises 3 preferably, 4-7-oxa-bicyclo[4.1.0 carboxylic acid 3,4-epoxycyclohexyl methyl ester, adipic acid two (3,4-epoxy cyclohexyl), many Synthesis of Oligo Ethylene Glycol of the many alcohol of aliphatic series, many Synthesis of Oligo Ethylene Glycol of castor oil, polyethylene glycol diepoxide, tetrabromobisphenol A glycidol ether.
The epoxides of bisphenol A-type will form the structure of relative stiffness when aggregating into resin form, just as cycloaliphatic epoxide.This can come modification by adding multifunctional aliphatic epoxide, but the latter itself can provide the cured resin structure of flexure usually.When this epoxides of two types is combined into photo curable composition, just might produce cured resin system with the performance between two kinds of pure resin system performances.
By changing the ratio of cycloaliphatic epoxide and bisphenol A epoxide and aliphatic epoxide, might provide flexible to a series of resins that are easy to deflection from showing slightly rigidity.The flexible matrix that can make or be coated with Photocurable composition equally or flood this based composition has these rigidity or flexibility.
Though it is flexible to need at least two kinds of epoxides to control, and can also add other.Other epoxides can provide other attribute except that deflection control.Such attribute comprises such as water proofing property, anti-flammability etc.Brominated oxide based on bisphenol-A shows fire resistance.Brominated bisphenol A is when with other combination of epoxides and when depositing, and its certain anti-flammability just passes to said composition.
Band backing of the present invention also comprises the cationic ionic salt of a kind of organometallic complex at least one catalytically effective amount, that be enough to cause polymerization, and described metal is selected from the element of periodic table of elements IV B family, V B family, VI B family, VII B family and VIII B family.
Specifically, the general formula of this class ionic salt is:
[（L 1a）（L 2a）（L 3a）M a] g[（L 1b）（L 2b）（L 3b）M b] h[（L 1c）（L 2c）（L 3c）M c] j[（L 1d）（L 2d）（L 3d）M d] k（L 4）（L 5）（L 6） +eX f
M in the formula a, M b, M cAnd M dRepresent metallic atom, can be identical or different, and be selected from the element of periodic table of elements IV B～VIII B family.This light trigger can be monokaryon, double-core, three nuclear or the four caryogamy combination compounds that contain metallic atom and subsidiary ligand (L).
Ligand is to have one can to utilize unsaturated group be that the compound of vinyl, acetenyl or aryl provides by any, no matter the total molecular weight of this compound how, as long as pi-electron is arranged.Such compound must dissolve in a kind of reaction medium, so that these electronics can utilize, sees also United States Patent (USP) 5,089,536.
Available compound includes but not limited to hexafluoro-antimonic acid cyclopentadiene iron (II), hexafluoro phosphonic acid cyclic pentadiene iron (II), hexafluoro arsenic acid cyclopentadiene iron (II) etc.
Better electrical insulation tape backing of the present invention also comprises a kind of promoter such as peroxide.Available peroxide comprises such as cumene hydroperoxide, hydroperoxidation tributyl, methyl ethyl ketone peroxide, peroxidating tributyl cumene and hydroperoxidation trityl.
Available promoter provides a kind of doing to touch thereby can coherent cured resin when being transformed into web form with hand.Unless the existence of this promoter is arranged, otherwise usually be necessary to promote the full solidification of epoxy composite of the present invention, this often will be undertaken by heating.
Better electrical insulation tape backing of the present invention also comprises at least a fire retardant.This can be a bisphenol-A bromination ether as discussed above, also can be a kind of inorganic fire-retarded additive such as various metal oxide and oxide hydrate, and the compound of nitrogenous or phosphorus.Fire retardant includes but not limited to the combination of the oxide and the brominated bisphenol A epoxides of antimony preferably.
Composition of the present invention also can comprise optional adjuvants, for example helps curing agent, curing agent, filler, plasticizer, pigment, antioxidant, surface modifier etc., and its consumption will make them not disturb the photopolymerization of epoxides.
Available matrix of the present invention comprises porous matrix such as glass cloth; Paper is as flat backing paper and crimped paper; Supatex fabric is as polyester and cellulose triacetate.Though poorly but also usefully do not have pore matrix, comprise film forming polymer such as polyester, acetic acid esters, polyphenylene sulfide, polyimides etc.
Band backing of the present invention is by following making; Epoxides is mixed with light trigger, then this photopolymerizable mixture is applied on the desirable matrix, and photopolymerization is to dried state.
For compound of the present invention, photopolymerization or curing reaction will be to carry out than the composition faster speed that lacks the organic metal light trigger.When wishing, make this compound full solidification subsequently, be that the ultraviolet light of about 180 nanometers～about 420 nanometers shines promptly by being exposed to a kind of transmitting boundary.
Material of the present invention can be used as adhesive tape, electrical insulation tape or rigid insulation composite construction.
And different, the expert of this gate technique can easily select a kind of adhesive and band backing of the present invention to be used by desirable purposes.Available adhesive includes but not limited to the rubber resin adhesive, synthetic segmented copolymer such as s-B-S, polybutadiene, polyisoprene, the styrene-isoprene copolymer, acrylic ester adhesive such as RE24, those disclosed in 905, and the admixture of above adhesive, all these can comprise tackifier and other habitual additive.But but but these adhesives can be hot melt polymerisation in solution suspension polymerisation or better be the ultra-violet radiation polymerization, for example United States Patent (USP) 4,181, those disclosed in 752.
When hope obtained a kind of electrical insulation tape, the dielectric strength of this band should be at least 3.5 kilovolts～10 kilovolts, and insulation impedance should be at least 1 * 10 6Megaohm.Adhesive also can contain a kind of flame-retardant additive, for example sees also above-mentioned can be used for in the backing those.
The useful band of the present invention is by following making: with habitual coating process such as scraper type coating, gravure printing coating, the coating of wheat rod etc., a kind of adhesive material is applied on the band backing, makes this adhesive curing with proper method then.
Method of testing
The bonding force test
Paste the band (25.4 centimetres of 2.54 cm x) of fitting, make the cleaning and the polished surface of adhesive one 302 shaped steel plate of contact (0.16 centimetre of 5 cm x, 12.2 cm x).Steel rider with one 2 kilopond coat with rubber slowly rolls twice with the speed of 5 cels on steel plate, apply constant pressure to article tape.Nearly 12.2 centimetres adhesive tape stretches out an end of steel plate.This adhesive tape constant temperature and humidity was placed 20 minutes.Bonding force is measured when requiring the steel plate location its length is vertically disposed.The band extension hangs over the steel plate lower edge.The band extension is got up from a steel plate end folding farthest, adhesive is contacted with adhesive, form about 2.54 centimeter length, tab.Catch this little protuberance and upwards lifting, can form a U-loop, make the outside of adhesive at this U-loop.Further reinforcing can produce tension force in this band, and this adhesive tape is separated with steel plate or strips down from steel plate.When adhesive tape was peeled off about 1.27 centimetres, it was INSTRON that centre, steel plate lower end is clipped in tensile machine TMIn the lower clamp of Model TM.2.54 centimetres of little protuberances are clipped in the last anchor clamps of this testing machine.Lower clamp remains on a fixed position, and last anchor clamps then promote with the speed of 30.5 cm per minute.
The mean force of record provides measuring the steel plate bonding force during adhesive tape and steel plate disengaging.
To the adhesive layer bonding force
Article one, 12.7 centimetres of 2.54 cm x, the two coating adhesive test bands on isolation liner vertically are placed on the centre of a clean steel (0.13 centimetre of 5.1 cm x, 12.7 cm x).Be attached on the steel plate with unshielded adhesive coating.Steel plate is placed on the flat surface, makes and to see test tape at the steel plate upper surface.Roller with one 2 kilopond coat with rubber rolls several times along isolation liner, applies constant pressure to adhesive tape.
Prepare a kind of single coating belt transect (12.7 centimetres of 2.54 cm x) it is carried out performance measurement, and for attachment on this test tape.The reverse side of backing is wiped examination with a kind of degreasing solvent, takes off isolation liner from test tape then.Belt transect adheres to along its length, makes the new adhesive surface that exposes of degreasing face and test tape contact.All put 7.62 centimetres single face dry adhesive tape at the Width at steel plate and belt transect two ends, so that its location.Place another 30.5 centimeter length * 1.27 centimetre wide adhesive tape at length direction, adhesive is contacted with adhesive, thereby have about 15 centimetres of dry adhesive bands to stretch out an end of steel plate.Because belt transect specific adhesion bandwidth is so any side of the latter all has the adhesive area of exposure to stretch out.These adhesive area are subjected to the protection of dry adhesive tape (12.7 centimeter length * 1.27 centimetre wide) adhesive to the adhesive effect.Formed stratiform band structure is with roll extrusion on direction of 2 kilograms of roller meanings in office some times.
Place steel plate, its longitudinal axis is vertically oriented, and makes dry adhesive band extension be suspended on its lower end.Adhesive tape is turned back from a steel plate end farthest, adhesive is contacted with adhesive, form terminal little protuberance about 1.27 centimeter length, that supply suspension usefulness.Catch this little protuberance and lifting straight up, form a U-loop, make adhesive in the U-loop outside.Further afterburning, in this band, produced tension force, and made the dry adhesive band can impel adhesive 100% to break away from this belt transect.The effect that keeps this power separates about 2.54 centimetres distance until these bands.At this moment, the steel plate lower edge being clipped in tensile machine is INSTRON TMIn the lower clamp of Model TM, the little protuberance of band is clipped in the last anchor clamps of this testing machine.
When the lower clamp of this testing machine stretches with respect to fixing last anchor clamps, just measured and make belt transect and dry adhesive band separate 5 centimetres of required power again.
Tension force and elongation test
Breaking tension-make a linear specimen fails and fragment into tensile force two obvious separating parts, per unit width.
Elongation-be subjected to institute at sample adds the tensile force effect and the moment of rupturing, the tensile sample comparison that length increases for tensile sample not.
One 17.8 centimeter length * 2.54 a centimetre wide backing sample is placed on an Instron TMBetween two anchor clamps of TM tensile machine, its longitudinal axis is vertically oriented, thereby an end of sample can be clipped in the last anchor clamps of tensile machine, and the other end of sample is clipped in the lower clamp of testing machine.
Test is to separate with the speed of 30.5 cm per minute by two anchor clamps that make testing machine to carry out.Along with sample stretches, added power increases to the degree that is damaged and ruptures in the sample centre.By measuring the maximum, force of per unit width before damage just, obtain the measured value of tension force.Elongation then is to measure with the percentage that sample length under the peak load before damaging increases.
Coiled material unclamps test
One volume width is that 2.54 centimetres adhesive tape of the present invention is wound on the 7.62 centimeter inner diameter mandrels, and its length is limited, and makes this coil diameter be no more than 16.5 centimetres.Use an improved tensile machine, i.e. Thwing-Albert, Intelect 500 TA make this band of a volume unclamp required power by following mensuration.
At the beginning, unclamping 5 circle adhesive tapes from this bonding volume earlier abandons.Then, this volume adhesive tape is enclosed within one unclamps on the mandrel, the size of this mandrel can cooperate with 7.62 centimetres of mandrels, and is positioned at the tensile machine front portion.Unclamp one section adhesive tape and it is adhered on the driven roller.The longitudinal axis that unclamps mandrel and driven roller is parallel, and they are positioned at roughly on the sustained height.Unclamping between mandrel and the driven roller, the adhesive tape coiled is inverted U-shaped, and its summit is supported on the free rotary drum surface, but does not contact with this surface is bonding.This cylinder is connected on the load sensor of tensile machine, and its diameter is similar to the diameter of the bonding roll coil of strip.Free rotary drum is positioned at top centre position, and with unclamp mandrel and driven roller on same perpendicular.Along with the motion of driven roller, adhesive tape just pulls down from the bonding roll coil of strip.Power that take place during unclamping, between adhesive and the backing passes to free rotary drum, passes to the load sensor of this power of impression then.In a previously selected cycle time, during the even running of driven roller (1.27 meters/minute), measure and pass to the power of load sensor, and will be converted into the numerical value that adhesive tape unclamps.
Dielectric breakdown is measured
Take off a 15.25 centimeter length * 2.54 centimetres of wide samples from a volume adhesive tape, one end inserts a dielectric tester as between two electrodes of an energy with the dielectric tester of 0.5 kilovolt/second even speed raising voltage, makes adhesive surface contact top electrode.Then voltage control (continuously adjustable autotransformer) is returned to zero, and reset circuit breaker.Start tester then, make the energy of position of striding this sample constantly increase, circuit breaker is disconnected until electric current.Voltage when writing down the dielectric breakdown generation then.Repeat this step at the sample other end and centre.Write down the mean value of these three puncture voltages then.
Insulation impedance is measured
This test needs 12 polishing stainless steel electrodes that 2.54 centimetres at round bone edge, 0.64 cm x, 0.64 cm x arranged, and 2.54 centimetres of each intervals are installed on the methyl methacrylate test board of cleaning with solvent.(the further information about this test board sees also ASTM D-1000).One volume adhesive tape discards the some circles of its outermost, takes off one section 23 centimetres of sample.This sample care should be used to is disposed, and does not touch the part of its inboard 2/3.Sample binder side court is placed down in above the electrode of 6 cleanings, and the second cover electrode and geometrical clamp is placed on it, forms a sandwich structure.Remove any unnecessary sample then, again test board is placed on an energy in 23 ℃ of test cabinets that keep 96% relative humidity, making adhesive is 1.336～1.34 glycerite towards a kind of refractive index.Make sample damping (leaving standstill) 18 hours 23 ℃ and 50% relative humidity.A megohmmeter is received on the test board, and be set in 120 volts.Measure the insulation impedance (totally 5 readings) between every pair of electrode terminal.Write down average insulation impedance with megaohm.
Flammable
Flammability test is included in twines a film tape on the one metal wire, make it overlap each other 50%, and repeat this step with another film tape in the opposite direction.The wire that winds is exposed to 30 seconds of naked light.Remove flame, the burning time of MEASUREMENTS OF THIN.Do not take fire or through 4 seconds of less than promptly from the material of horizontal blanking, can demonstrate desirable anti-flammability.
Following example is intended to explanation and unrestricted the present invention's intention.The personnel that are familiar with this gate technique will easily comprehend the various variations in the defined scope of the invention of claim.
Example
Example 1
How pure 60.0 grams of packing in the three neck round-bottomed flasks that blender and thermometer be housed be a kind of aliphatic series many Synthesis of Oligo Ethylene Glycol of " Heloxy84 " available from Union Carbide Inc., trade names available from Rhone Poulenc company, trade names for the caproic acid two (3,4-epoxy cyclohexyl) of " ERL 4299 " and 40 grams.This mixture is heated to 75 ℃ while stirring, remains on this temperature then.In flask, add light trigger, i.e. 1.0 gram hexafluoro-antimonic acid cyclopentadiene iron (II).This content continues to stir 1 hour, and temperature is controlled at 75 ℃.Filter this hot fluid composition, and make it be cooled to room temperature, face the preceding cumene hydroperoxides that add 1.5 grams available from Atochem company of coating.The viscosity of this coating composition＜1000 centipoises.It is applied to a kind of trade mark on the glass cloth matrix of " Burlington glass Fabric-Style I8026 ".This fluid composition is absorbed by glass cloth, makes total all flood the epoxy fluid.Use a kind of small-sized transmission cure system of American UV Company that variable modulation luminous intensity and speed control are arranged, make the time of the glass cloth of this dipping ultraviolet exposure＜10 seconds of 180～420 nanometer range.Formed backing is tested, to measure its tensile strength, percentage elongation and electrical insulation characteristics.These numerical value are listed in table 1.
Table 1
Insulation impedance (ohm) tensile strength, kg/cm 2Percentage elongation, %
3×10 1413.26 5.4
On this glass cloth backing, further be coated with a kind of rubber-based adhesive.This adhesive tape can be used for carrying out with band the purposes of electric insulation.This band is listed in the table 2 measured value that the bonding force and the coiled material of steel unclamps power.
Table 2
To the bonding force of steel, newton/decimetre coiled material unclamps power, gram per centimeter
Glass cloth backing 16.6 248.4
Example 2～3
The epoxy fluid of example 1 is coated on respectively available from Mosinee Paper Corporation(state of Wisconsin Moses Buddhist nun), the trade mark is on the crimped paper of " M-2251 " and available from Lydell, Inc.(New York Te Luoyi) " #525 " flat backing paper on.By the insulation impedance of testing these materials as mentioned above, tensile strength and percentage elongation, the results are shown in Table 3.
Table 3
Insulation impedance (ohm) tensile strength, kg/cm 2Percentage elongation, %
Crimped paper 5 * 10 1316.65 7.9
Flat backing paper 8 * 10 102.3 13.9
These backings also have been coated with rubber-based adhesive, and test its bonding force and coiled material unclamps power.The results are shown in table 4.
Table 4
To the bonding force of steel, newton/decimetre coiled material unclamps power, gram per centimeter
Crimped paper 23.9 173
Flat backing paper 28.3 215
Example 4
By in coating composition, comprising a kind of flame-retardant polymer and a kind of fire-retardant pigment, prepared a kind of fire-retardant backing of the present invention.
Composition contains 40.0 grams " ERL 4299 ", 30.0 gram " Heloxy 84 ", 30.0 gram is the tetrabromobisphenol A diglycidyl ether of Epirez 5163 available from Rhone Poulenc company, trade names, 4.0 gram is available from the ultra-fine level antimony trioxide of Laurel Industries company, 1.0 gram light triggers and 1.4 restrain cumene hydroperoxides.This composition is applied on a kind of non-woven polyester matrix, and is exposed to 180～420 nm radiations of ultraviolet source.
Formed backing UL TM(Underwriters Laboratory) carries out 510 flame assays.Be 14 seconds the average time of fray-out of flame.
Example 5 and 5C
Method by example 1 prepares following coating composition, but changes light trigger.
Example 5 example 5C
ERL 4,299 40.0 grams 40.0 grams
Heloxy 84 30.0 grams 30.0 grams
Epirez 5,163 30.0 grams 30.0 grams
Antimony trioxide 4.0 grams 4.0 grams
Light trigger 1.0 grams 3.0 grams 2
Cumene hydroperoxide 1.0 grams 0.0 gram
1. hexafluoro-antimonic acid cyclopentadiene iron (II) dimethylbenzene
2.FX 512-hexafluoro-antimonic acid sulfonium.
Use continuous coating, exposure and Wiring apparatus, example 5 and 5C are applied to respectively on the non-woven polyester host material sample.This fabric that has been coated with epoxy is carried by a ultraviolet light station with the speed of 180 cm per minute, and this station is with the radiation of 200 watts/inch intensity emission 180～420 nanometer range.Example 5 is a kind of compositions of the present invention, provides a kind of and does to the full curing backing that can touch.Otherwise example 5C is a kind of composition beyond the scope of the invention, does not have full solidification and toughness still.
Then, the fabric transporting velocity is reduced to half of former speed, i.e. 90 cm per minute, the light condition is constant.Example 5C can not full solidification; 5 full solidification of example.This confirm composition of the present invention than in the past the report, make the composition of " " type catalyst solidify sooner.These backings wore out 10 minutes at 100 ℃, so that example 5C full solidification is coated with rubber adhesive then described in example 1, and tested for tensile strength and percentage elongation.The results are shown in Table 5.
Table 5
Tensile strength, newton/decimetre percentage elongation, %
Example 5 578 26.00
Example 5C 394 35.50
These examples are all made according to example 1, and different is epoxy ratio such change as shown in table 6.
These backings have been coated with a kind of caoutchouc adhesive that is clamminess and a kind of Isooctyl acrylate monomer/acrylic acid/methyl acrylate adhesive (7 and 8), and carry out bonding force, tensile strength and percentage elongation and flammable test.The results are shown in Table 6.
Table 6
Instance number
Composition 6789
ERL 4299-epoxy 70 60 50 40
Epirez 5163-fire retardant 30 30 30 30
Heloxy 84-epoxy 0 10 20 30
Light trigger
Figure 931186404_IMG1
1111
Cumene hydroperoxide 1.5 1.5 1.5 1.5
Antimony trioxide 4444
Tensile strength (kg/cm 2) 2.4 2.3 2.4 2.3
Percentage elongation (%) 4 13 25 25
Two adhesive layer bonding forces (newton/decimetre) 133 133 140 111
(105 *) (106 *)
Bonding force (newton/decimetre) 43 46 43 39
(49 *) (49 *)
Dielectric strength (kilovolt) 5.1 4.9 4.7 5.0
(4.3 *) (5.7 *)
Insulation impedance (ohm) 1.2 * 10 132.9 * 10 123.3 * 10 112.0 * 10 10
Thickness (micron) 135 127.5 127.5 130
Flammable (second) 13 23 34＜20
1. hexafluoro-antimonic acid cyclopentadiene iron (II) dimethylbenzene
* the numerical value with asterisk is to obtain from the band structure that acrylic ester adhesive is arranged.

Claims (10)

1, a kind of flexible belt backing wherein comprises a kind of matrix that has been coated with a kind of photopolymerization epoxy composite thereon, and described composition contains
A) multiple epoxides comprises at least a this group and at least a aliphatic epoxide of being made up of cycloaliphatic epoxide and bisphenol A epoxide that be selected from,
B) 0.1～2% at least a can the cationic initator of the organic metal of 200～600 nano wave length initiated polymerizations and
C) at least a promoter,
Wherein said backing is full solidification after shining 1～15 second, need not heating steps.
2, according to the flexible belt backing of claim 1, described band is suitable for electric purposes, and the dielectric strength of wherein said band is at least 3.5 kilovolts～10 kilovolts, and insulation impedance is at least 1 * 10 6Megaohm.
3, according to the flexible belt backing of claim 1 or 2, wherein said epoxides comprises the glycidol ether of at least a bisphenol-A.
4, according to the flexible belt backing of claim 1 or 2, at least a in the wherein said multiple epoxides is the bromo epoxides.
5, according to the flexible belt backing of claim 1 or 2, wherein said cycloaliphatic epoxide contains at least one epoxycyclohexyl.
6, according to the flexible belt backing of claim 1 or 2, wherein said light trigger is a kind of cationic ionic salt of organometallic complex that is enough to cause polymerization, and described metal is selected from the element of periodic table of elements IV B family, V B family, VI B family, VII B family and VIII B family.
7, according to the flexible belt backing of claim 1 or 2, wherein said matrix is selected from this group of being made up of glass cloth, paper and supatex fabric and contains many apertures, enters in the described hole and described epoxy composite is impregnated.
8, according to the flexible belt backing of claim 1 or 2, wherein said matrix is a kind of non-porous film forming polymer, is selected from this group of being made up of polyester, acetic acid esters, polyphenylene sulfide and polyimides.
9, according to the flexible belt backing of claim 1 or 2, wherein said promoter is a kind of peroxide, and the amount of described promoter is 0.1～5% of an epoxy resin total amount.
10, according to the flexible belt backing of claim 1 or 2, wherein said adhesive is selected from this group of being made up of rubber adhesive, elastomeric adhesive, acrylic adhesives and isocyanate adhesive.
CN93118640A 1992-10-09 1993-10-08 Epoxy impregnated tape backing Pending CN1086626A (en)

Applications Claiming Priority (2)

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US958,930 1992-10-09

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CN110352462A (en) * 2017-03-10 2019-10-18 3M创新有限公司 Electrically insulating material

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US5667893A (en) * 1992-10-09 1997-09-16 Minnesota Mining And Manufacturing Company Substrate coated or impregnated with flexible epoxy composition
DE19960466A1 (en) * 1999-12-15 2001-09-20 Beiersdorf Ag Adhesive tape, especially for masking a KTL primer
CN1957041A (en) * 2004-05-28 2007-05-02 雅宝公司 Flame retardant polyurethanes and additives therefor
JP5150436B2 (en) * 2008-09-26 2013-02-20 株式会社寺岡製作所 Heat resistant adhesive tape
DE102009035097A1 (en) * 2009-07-29 2011-02-03 Siemens Aktiengesellschaft Flächenisolierfolie and application
NL1038884C2 (en) * 2011-06-23 2013-01-02 Holland Novochem Technical Coatings B V Protective polymer layers.
CN102982923A (en) * 2012-12-04 2013-03-20 江苏亚威变压器有限公司 Novel insulating paper applied to transformer

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US4286047A (en) * 1979-07-25 1981-08-25 Minnesota Mining And Manufacturing Company Pressure-sensitive adhesive susceptible to ultraviolet light-induced detackification

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Publication number Priority date Publication date Assignee Title
CN110352462A (en) * 2017-03-10 2019-10-18 3M创新有限公司 Electrically insulating material

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