1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS EN ISO 10082:2000 The
2、European Standard EN ISO 10082:1999 has the status of a British Standard ICS 83.080.10 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Plastics Phenolic resins Classification and test methodsThis British Standard, having been prepared under the direction of the Sector Committe
3、e for Materials and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 August 2000 BSI 08-2000 ISBN 0 580 34098 8 BS EN ISO 10082:2000 Amendments issued since publication Amd. No. Date Comments National foreword This British Standard is the English la
4、nguage version of EN ISO 10082:1999. It is identical with ISO 10082:1999. It supersedes BS EN ISO 10082:1996 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee PRI/42, Fibre reinforced thermosetting plastics and prepregs, which has the responsibility to:
5、 aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. A list of organi
6、zations represented on this committee can be obtained on request to its secretary. Cross-references Attention is drawn to the fact that CEN and CENELEC Standards normally include an annex which lists normative references to international publications with their corresponding European publications. T
7、he British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A
8、 British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a
9、 front cover, an inside front cover, the EN ISO title page, the EN ISO foreword page, the ISO title page, pages ii to iv, pages 1 to 11 and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued.EN ISO 10082:1999Referencenumber ISO10082:1999(E)
10、INTERNATIONAL STANDARD ISO 10082 Secondedition 1999-12-15 PlasticsPhenolicresinsClassification andtestmethods Plastiques Rsines phnoliques Classification et mthodes dessai EN ISO 10082:1999ii EN ISO 10082:1999 iii Contents Page Foreword.iv 1 Scope1 2 Normativereference1 3 Basisofclassificationofphen
11、olicresins.1 3.1 General1 3.2 Rawmaterials.2 3.3 Typesofphenolicresin.2 3.4 Formsofcommercialproduct3 3.5 Degreeofcondensation3 3.6 Catalystsandhardeners.3 4 Testmethods4 4.1 Numericallist.4 4.2 Alphabeticallist.5 4.3 Descriptionoftestmethods.6 EN ISO 10082:1999iv Foreword ISO(theInternationalOrgani
12、zationforStandardization)isaworldwidefederationofnationalstandardsbodies(ISO memberbodies).TheworkofpreparingInternationalStandardsisnormallycarriedoutthroughISOtechnical committees.Eachmemberbodyinterestedinasubjectforwhichatechnicalcommitteehasbeenestablishedhas therighttoberepresentedonthatcommit
13、tee.Internationalorganizations,governmentalandnon-governmental,in liaisonwithISO,alsotakepartinthework.ISOcollaboratescloselywiththeInternationalElectrotechnical Commission(IEC)onallmattersofelectrotechnicalstandardization. InternationalStandardsaredraftedinaccordancewiththerulesgivenintheISO/IECDir
14、ectives,Part3. DraftInternationalStandardsadoptedbythetechnicalcommitteesarecirculatedtothememberbodiesforvoting. PublicationasanInternationalStandardrequiresapprovalbyatleast75%ofthememberbodiescastingavote. AttentionisdrawntothepossibilitythatsomeoftheelementsofthisInternationalStandardmaybethesub
15、jectof patentrights.ISOshallnotbeheldresponsibleforidentifyinganyorallsuchpatentrights. InternationalStandardISO10082waspreparedbyTechnicalCommitteeISO/TC61, Plastics, Subcommittee SC12, Thermosetting materials. Thissecondeditioncancelsandreplacesthefirstedition(ISO10082:1991)andISO/TR8244:1988,whic
16、hhave beentechnicallyrevised. EN ISO 10082:1999 1 PlasticsPhenolicresinsClassificationandtest methods 1 Scope ThisInternationalStandardgivesanoverviewofthedifferenttypesofphenolicresinusedinthemanufactureof thermosettingplasticsandasummaryofavailabletestmethods. Clause3definestermsrelatingtothechemi
17、calstructureofphenolicresins,theirphysicalstateandtheirdegreeof condensationorpolycondensation. Clause4givesasummaryoftestmethods.Thesemethodsapplytothedeterminationofpropertieswhichare relevanttotheproduction,processinganduseofphenolicresinsasdescribedinclause3.Theusershouldselect fromtheteststhose
18、thatareappropriateforaparticularapplication.Foragivenmethod,onlythestandard(s)listed maybeused. 2 Normativereference Thefollowingnormativedocumentcontainsprovisionswhich,throughreferenceinthistext,constituteprovisionsof thisInternationalStandard.Fordatedreferences,subsequentamendmentsto,orrevisionso
19、f,thispublicationdo notapply.However,partiestoagreementsbasedonthisInternationalStandardareencouragedtoinvestigatethe possibilityofapplyingthemostrecenteditionofthenormativedocumentindicatedbelow.Forundatedreferences, thelatesteditionofthenormativedocumentreferredtoapplies.MembersofISOandIECmaintain
20、registersof currentlyvalidInternationalStandards. ISO472:1999, Plastics Vocabulary. 3 Basisofclassificationofphenolicresins Thisclausedefinestermsrelatingtothechemicalstructureofphenolicresins,theirphysicalstateandtheirdegree ofcondensationorpolycondensationforclassificationpurposesinthemanufacturin
21、gandprocessingoftheresins. Thedefinitionsapplytoallfieldsofapplicationofphenolicresinsinplastics(seealsorelateddefinitionsin ISO472). 3.1 General 3.1.1 Theterm“phenolicresins“asusedinthisInternationalStandardrefersto a) syntheticresinsormodifiedproductsobtainedbycondensationofphenolwithaldehydes,par
22、ticularly formaldehyde; b) productsoftheadditionofphenolstounsaturatedcompounds(forexampleacetylene,terpenesandnatural resins) 1 . 1 Strictlyspeaking,theseresinsarenotwhatarenormallyregardedasresinsfortheproductionofplastics.Theyareused particularlyincertainsurfacecoatings. EN ISO 10082:19992 NOTE R
23、esinsinwhichtheoriginalpropertiesaresochangedbythemodificationthattheyresemblemorecloselythoseof themodifyingmediumarenotregardedasphenolicresins. 3.1.2 Phenolicresinsmaybeclassifiedinanumberofways,suchasby a)thetypeofrawmaterial(see3.2); b)thetypeofresinproduced(see3.3); c)thetypeofmodification(see
24、3.3.2); d)thephysicalformofthecommercialproduct(see3.4); e)thedegreeofcondensation(see3.5); f)thetypeofcatalystused(see3.6.1); g)thetypeofhardenerused(see3.6.2). 3.2 Rawmaterials 3.2.1 Phenols Besidesunsubstitutedphenol,derivativesofphenolareusedforthemanufactureofphenolicresins.Theseinclude cresols
25、,xylenolsandotheralkylphenols(forexample p-tert-butylphenol, p-tert-octylphenol and p-tert-nonylphenol), arylphenols(forexamplephenylphenolandnaphthols)anddivalentphenols(suchasresorcinolandbisphenolA). 3.2.2 Aldehydes Themostimportantaldehydecomponentisformaldehyde,whichisusedinvariousforms,includi
26、ngaqueous solutionandsolidparaformaldehyde,andalsoascompoundswhichgiverisetoformaldehyde.Otheraldehydes (forexampleacetaldehyde,acrolein,benzaldehydeandfurfural)areemployedtoamorelimitedextent,asalsoare ketones. 3.3 Typesofphenolicresin 3.3.1 Unmodifiedphenolicresins Unmodifiedphenolicresinsareprodu
27、cedbycondensationreactionsofphenolswithanaldehyde.Dependingon factorssuchasthevolumeandmolarratiooftherawmaterials,thereactionconditionsandthecatalysts employed,twodifferentclassesofproductareobtained:novolaksandresols. 3.3.1.1 Novolaks(two-step) Novolaksarenon-self-curing,soluble,fusiblephenolicres
28、insthatremainstablewhenstored.Thephenolnucleiare linkedprimarilybymethylenebridges.Novolakscanbemadetoreactfurtherandcrosslinkbytheadditionof hardeners(see3.6.2);heatingisalsousuallynecessary. Seealso novolak in ISO 472. 3.3.1.2 Resols(one-step) Resolsaresoluble,fusiblephenolicresinswhich,incontrast
29、tonovolaks,containmethylolgroupsandmethylene- etherandsometimesalsomethylene-aminebridges.Resolsareself-curing:theycrosslinktogiveinsoluble productswhenheatedand/ormixedwithcatalysts,withoutadditionoffurtherreactioncomponents.Resolsare perishableandcanbestoredforalimitedtimeonly. Seealso resol in IS
30、O 472. EN ISO 10082:1999 3 3.3.2 Modifiedphenolicresins Phenolicresinscanbemodifiedbychemicalreactionofthemethylolorthephenolichydroxylgroupsand/orby physicaldispersioninthemodifyingagent.Suchmodifiedphenolicresinscanbeeitherself-curingornon-self- curing,dependingontheirstructure. 3.3.3 Phenolicaddi
31、tionresins Phenolicresinscanalsobeproducedwithoutcondensationwithformaldehydebyreactionofphenolwith unsaturatedhydrocarbons.Examplesofthesearephenol/acetyleneandphenol/terpeneresins,whicharenot alwaysself-curing. 3.4 Formsofcommercialproduct Phenolicresinsaremanufacturedandusedinvariousforms,suchas
32、a)liquids; b)solids,aspelletized,flake,granularorfinelypowderedproducts; c)solutionsordispersionsinwaterand/ororganicsolvents. Aso-called“aqueoussolution“(itisnotarealaqueoussolution)isonethathasawatercontentofmorethan 5%(m/m)andanorganic-solventcontentoflessthan5%(m/m)(freephenolisnotcountedasorgan
33、icsolvent). Asolvent-containingphenolicresinsolutionisonethathasmorethan5%(m/m)oforganicsolvents. 3.5 Degreeofcondensation Phenolicresinscanbecrosslinkedbytheuseofheatand/orhardenersand/orcatalysts.Theypassthroughthe followingtransitionalstagesofcondensation: A-stage:startingstate(resolornovolak);li
34、quidorfusible,andsolubleinalcoholandacetone; B-stage:intermediatestate(resitol);infusible,butstillmouldablewithheatandcapableofswellinginalcoholor acetone; C-stage;finalstate(resite);infusible,andinsolubleinalcoholoracetone. Seealso A-stage, B-stage, C-stage, resite and resitol in ISO 472. 3.6 Catal
35、ystsandhardeners 3.6.1 Catalysts Catalystsacceleratethecrosslinkingreaction.Bothacidandbasiccompoundsaresuitableforthispurpose. 3.6.2 Hardeners(crosslinkingagents) Formaldehyde,orcompoundsthatreleaseformaldehyde,forexamplehexamethylenetetramine(hexamine),canbe usedashardeners.Resolsandisocyanatescan
36、alsobeusedashardeners.Hardenersaregenerallyaddedonlyto non-self-curingphenolicresinsandcurebychemicalreaction(three-dimensionalcrosslinking). EN ISO 10082:19994 4 Testmethods 4.1 Numericallist ISO60:1977, Plastics Determination of apparent density of material that can be poured from a specified funn
37、el. ISO565:1990, Test sieves Metal wire cloth, perforated metal plate and electroformed sheet Nominal sizes of openings. ISO760:1978, Determination of water Karl Fischer method (General method). ISO2555:1989, Plastics Resins in the liquid state or as emulsions or dispersions Determination of apparen
38、t viscosity by the Brookfield Test method. ISO2811-1:1997, Paints and varnishes Determination of density Part 1: Pyknometer method. ISO3146: 2) , Plastics Determination of melting behaviour (melting temperature or melting range) of semi- crystalline polymers by capillary tube and polarizing-microsco
39、pe methods. ISO3219:1993, Plastics Polymers/resins in the liquid state or as emulsions or dispersions Determination of viscosity using a rotational viscometer with defined shear rate. ISO3451-1:1997, Plastics Determination of ash Part 1: General methods. ISO3675:1998, Crude petroleum and liquid petr
40、oleum products Laboratory determination of density Hydrometer method. ISO4610:1977, Plastics Vinyl chloride homopolymer and copolymer resins Sieve analysis using air-jet sieve apparatus. ISO8618:1995, Plastics Liquid phenolic resins Conventional determination of non-volatile matter. ISO8619:1995, Pl
41、astics Phenolic resin powder Determination of flow distance on a heated glass plate. ISO8974: 3) , Plastics Phenolic resins Determination of residual phenol content by gas chromatography. ISO8975:1989, Plastics Phenolic resins Determination of pH. ISO8987:1995, Plastics Phenolic resins Determination
42、 of reactivity on a B-transformation test plate. ISO8988:1995, Plastics Phenolic resins Determination of hexamethylenetetramine content Kjeldahl method and perchloric acid method. ISO8989:1995, Plastics Liquid phenolic resins Determination of water miscibility. ISO9020:1994, Binders for paints and v
43、arnishes Determination of free-formaldehyde content of amino resins Sodium sulfite titrimetric method. ISO9396:1997, Plastics Phenolic resins Determination of the gel time of resols under specific conditions using automatic apparatus. ISO9397:1995, Plastics Phenolic resins Determination of free-form
44、aldehyde content Hydroxylamine hydrochloride method. 2)Tobepublished.(RevisionofISO3146:1985) 3)Tobepublished.(RevisionofISO8974:1997) EN ISO 10082:1999 5 ISO9771:1995, Plastics Phenolic resins Determination of the pseudo-adiabatic temperature rise of liquid resols when cured under acid conditions.
45、ISO9944:1990, Plastics Phenolic resins Determination of electrical conductivity of resin extracts. ISO11401:1993, Plastics Phenolic resins Separation by liquid chromatography. ISO11402: 4) , Phenolic, amino and condensation resins Determination of free-formaldehyde content. ISO11409:1993, Plastics P
46、henolic resins Determination of heats and temperatures of reaction by differential scanning calorimetry. ISO12058(bothparts), Plastics Determination of viscosity using a falling-ball viscometer. 4.2 Alphabeticallist ISOstandard Subclause Acidreactivityofphenolicresols 9771 4.3.2.3 Ash,determinationo
47、f 3451-1 4.3.2.9 Conductivity,electrical,ofphenolicresinextracts,measurementof 9944 4.3.1.7 Density,apparent,determinationof 60 4.3.1.3 Densityorrelativedensity,determinationof,hydrometermethod 3675 4.3.1.4 Densityofpaintsandvarnishes,determinationof 2811 4.3.1.4 Differentialscanningcalorimetry,dete
48、rminationofheatsandtemperaturesof reaction 11409 4.3.2.2.3 Flowdistance,onaheatedglassplate,ofphenolicresins,determinationof 8619 4.3.2.1 Formaldehyde,free,contentinaminoresins,sodiumsulfitetitrimetricmethod 9020 4.3.2.6.2 Formaldehyde,free,contentincondensationresins 11402 4.3.2.6.3 Formaldehyde,fr
49、ee,contentinphenolicresins,hydroxylaminehydrochloride method 9397 4.3.2.6.1 Geltimeunderspecificconditionsbyautomaticapparatus,determinationof 9396 4.3.2.2.2 Hexamethylenetetraminecontentofphenolicresins,Kjeldahlmethodand perchloricacidmethod 8988 4.3.2.7 Liquidchromatographyofphenolicresins,separationof 11401 4.3.2.10 Meltingbehaviourofsemi-crystallinepolymers 3146 4.3.1.1 Non-volatilematterinliquidphenolicresins,determinationof 8618 4.3.2.4 pHofphenolicresins