WO2000008076A1 - Copolymers of tetrafluoroethylene and perfluoroalkylvinylic ethers used in the production of thermal-aggression resistant articles - Google Patents

Copolymers of tetrafluoroethylene and perfluoroalkylvinylic ethers used in the production of thermal-aggression resistant articles Download PDF

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WO2000008076A1
WO2000008076A1 PCT/RU1999/000132 RU9900132W WO0008076A1 WO 2000008076 A1 WO2000008076 A1 WO 2000008076A1 RU 9900132 W RU9900132 W RU 9900132W WO 0008076 A1 WO0008076 A1 WO 0008076A1
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mol
copolymers
mole
ranges
perfluoroalkylvinylic
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PCT/RU1999/000132
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WO2000008076A8 (en
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Margarita Alexeevna Volkova
Viktor Andreevich Gubanov
Vitaly Abramovich Kormer
Alexandr Lvovich Kuznetsov
Elena Andreevna Manuilova
Boris Andreevich Khristianchik
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Federalnoe Gosudarstvennoe Predpryatie Ordena Lenina I Ordena Trudovogo Krasnogo Znameni Nauchno-Issledovatelsky Institut Imeni Akademika S.V. Lebedeva (Fgp Niisk)
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Publication of WO2000008076A1 publication Critical patent/WO2000008076A1/en
Publication of WO2000008076A8 publication Critical patent/WO2000008076A8/en

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F214/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
    • C08F214/18—Monomers containing fluorine
    • C08F214/26—Tetrafluoroethene
    • C08F214/262—Tetrafluoroethene with fluorinated vinyl ethers

Abstract

The present invention relates to vulcanisation agents containing copolymers of tetrafluoroethylene and perfluoroalkylvinylic ethers which can be used as sealing materials in a high-temperature aggressive environment. The copolymers of the present invention correspond to structural formula (1) in which n ranges from 42 to 70 mole %, m ranges from 25 to 55 mole %, p ranges from 1 to 4 mole % and a ranges from 1 to 7 mole % for a molecular weight of between 100000 and 200000. These copolymer-containing vulcanisation agents exhibit good physical-mechanical indices, a high thermal resistance in a stress state as well as a high tensile stress index at an elongation of 100 %.

Description

\ΥΟ 00/08076 ΡСΤЛШ99/00132\ ΥΟ 00/08076 ΡСΤЛШ99 / 00132
Сοιιοлπмсρι.ι τеτρаφιορэιιιлсιιа и πсρφι ρалκπлншшлοиыχ эφиροн для τеρмοаιρсссιшοсτοπκиχ издслий.Compliance with the rules and regulations for the broadcasting of articles.
Пρедποлагаемοе изοбρсτение οτнοсиτся κ οбласτи ποлучения πеρφτορиροванпыχ сοποлимеροв, сοдеρжашнχ φушαшοπальныс гρуππы οбιцси φορмулы: (-СГ2-СΡ2)„ - (СΡ2-СΡ)„, - (СΡ2-СΡ) - (СΡ2-СΡ-)а ο ο οPρedποlagaemοe izοbρsτenie οτnοsiτsya κ οblasτi ποlucheniya πeρφτορiροvanpyχ sοποlimeροv, sοdeρzhashnχ φushαshοπalnys gρuππy οbιtssi φορmuly: (-SG 2 -SΡ 2) "- (cF -SΡ 2)" - (cF -SΡ 2) - (2 -SΡ- cF) and ο ο ο
СΡз ( СΡ2 )з СΡ2 SΡz (SΡ 2 ) s SΡ 2
Ο СΡ-СΡзΟ СΡ-СΡз
СΡ-СΡз οСΡ-СΡз ο
СΝ СΡ2-СГ2-СΝ , гдс η = 42-70 мοль % т = 25-55 мοль % ρ = 1- 4 мοль % а = 1 - 7 мοль % с мοлеκуляρнοй массοй 100000-200000.СΝ СΡ 2 -СГ 2 -СΝ, ГДС η = 42-70 mol% t = 25-55 mol% ρ = 1-4 mol% a = 1 - 7 mol% with a molecular weight of 100,000-200,000.
Ρсзины иа οсиοве τаκиχ сοποлимеροв м.οгуτ быτь исποльзοваны κаκ уπлοτнсπия, πρедназначснные для эκсπлуагации в агρсссивπыχ сρсдаχ πρи высοκиχ τемπсρаτуρаχ, наπρимеρ, в χимичесκοй, авиациοинοй, неφτедοбывающей или неφτеπеρсρабаτывающей οτρасллχ προмышленнοсτи, в авτοмοбиле - и судοсτροении.Ρsziny ua οsiοve τaκiχ sοποlimeροv m.οguτ byτ isποlzοvany κaκ uπlοτnsπiya, πρednaznachsnnye for eκsπluagatsii in agρsssivπyχ sρsdaχ πρi vysοκiχ τemπsρaτuρaχ, naπρimeρ in χimichesκοy, aviatsiοinοy, neφτedοbyvayuschey or neφτeπeρsρabaτyvayuschey οτρasllχ προmyshlennοsτi in avτοmοbile - and sudοsτροenii.
ЗΑΜΕΗЯЮЩИЙ ЛИСΤ (ПΡΑБИЛΟ 26) \νθ 00/08076 ΡСΤ/ΚШ9/00132SIGNIFICANT FOX (BEAT 26) \ νθ 00/08076 ΡСΤ / ΚШ9 / 00132
Ичнесτπы сοποлимеρы τеτρаφ гορэτилена (ΤΦЭ) и ιιсρφτυρллκπлιшιшлυныχ эφиροн (Ι1ΙΛИ'3) υυιцеи φυρмулы: (-СΡ2 - С1-2)η - (СΙ-2 -The sources of the theory of thermophysics (ΤΦЭ) and ιιсρφτυρлκπлшшшлυных эфиροн (Ι1ΙΛИ'3) υυιцеи φυρмлы: (-СΡ 2 - С1- 2- η -
Figure imgf000004_0001
η = 30-70 мοль % ιη • 25 - мυль % ρ = 0,5 - 5,0 мοль'ο а = 2-ϊ2
Figure imgf000004_0001
η = 30-70 mol% ιη • 25 - mυl% ρ = 0.5 - 5.0 mol'ο а = 2-ϊ2
Сοπυлимеρы ποлучаюτ вοдοэмульсиοшιым меτοдοм в ιιρικуιч. нιιн χллдυπл -113 πρи τсмπсρлτуρе οτ 40 дο 60 "С н лаϊ-леπии 8, 4 κг/ем2 , κοτοροс ποддеρжинасτся πуτсм ποдачπ смеси мυнοмеροн -7ЭΦ н πеρφτορмеτιιлниιιπлοвοгο эφиρа (ПΦΜΙП). Жιιдκιιм мοιιυмсρ с СΝ-гρуπποм ιшοдмτся с πυмυщыυ шш ιυнυιυ ишκсκιυρа Паг.СШΛ /*.• ЗΜθϊЬ'Ο с πρиυρ. οτ 30.09.68. κл.260-80-73). Зулκлпизаτы ιιа οсποис τаκиχ сοποлимеροн нмсκгг πеудοнлеτнορиτелыιые ποκазаτели πο τеπлοсτοйκοсτи в πлπρяжеππυм сοсгυяπππ πρπ иысοκиχ τсмπсρаτуρаχ (ΟДС). Τаκ, πο даππым οητοροη иасτοяιцсГι заяшси, ΟДС за 24 маса πρπ 11>ϋ "С υсышιясι -11% , ц пρп 273 "С - пρυπсл.υднг р-υρушсιшс οбρазца. Κροме τοгο, τаκοй сοποлимеρ являеτся дοвοльнο жеешιм, ι.κ. еυдеρжш υκυлυ 12% κρие аллπчссκυй φачι.ι, чτυ зиачиτслыю οслοжияе егο πсρеρабοτκу.We have been working on an emulsion method in Moscow. nιιn χlldυπl -113 πρi τsmπsρlτuρe οτ 40 dο 60 "C, n-laϊ leπii 8, 4 κg / cm 2, κοτοροs ποddeρzhinasτsya πuτsm ποdachπ mixture mυnοmeροn -7EΦ n πeρφτορmeτιιlniιιπlοvοgο eφiρa (PΦΜΙP). Zhιιdκιιm mοιιυmsρ with SΝ-gρuπποm ιshοdmτsya with πυmυschyυ shsh ιυnυιυ ishκsκιυρa Pag.SShΛ /*.• ZΜθϊ'Ο with πρiυρ. οτ 30.09.68. κl.260-80-73). Zulκlpizaτy ιιa οsποis τaκiχ sοποlimeροn nmsκgg πeudοnleτnορiτelyιye ποκazaτeli πο τeπlοsτοyκοsτi in πlπρyazheππυm sοsgυyaπππ πρπ iysοκiχ τsmπsρaτuρaχ (ΟDS). Τaκ, π да да и и и и и зая ш ш ш ш ш ш ш ш ш за за за за за за за за за за за за 11 11 11 11 11 11 11 11 11 11 11 11 11 - - - - - - - - - It’s a good condition, but it’s also a very good condition, v.k.
ЗΑΜΕΗЯЮЩИЙ ЛИСΤ (ПΡΑΒИЛΟ 26) \νθ 00/08076 ΡСΤ/ΙШ99/00132SIGNIFICANT FOX (DR. 26) \ νθ 00/08076 ΡСΤ / ΙШ99 / 00132
33
Изнесτπы сυποлимсρы τеτρаφτορэτπлеπа πеρφ гυρллκнлнιшπлυными эφπρамπ οбшсιϊ φορмулы: ( -С 2 - С1 2- )„ - (Wear and tear of the impairment of impairment of impairment of the formula: (-C 2 - C1 2-) „- (
Figure imgf000005_0001
а =53 -79,8 мοль % н = 20 -45,0 мυль % с = 0,2 - 2,0 мοль % , χ = 1 , 2 π = 1- 4 Сοποлπмсρы πυлучаιυ г нοдοэмульснοπпοπ сοποлимсρнзацмси с иеποльзοπлιшсм υκπслπτслыю-нοссτанοииτслыюн снсτсмы πρπ τемπсρа гу|)е υ г 65 дυ 85 °С и πысοκοм даилсπин (3-8 Μπа). (Паτ. СНΙΛ ' 281092 с πρиορ. 22.10.79. юι. СΟ8Г8/00, 214/26).
Figure imgf000005_0001
а = 53 -79.8 mol% n = 20 -45.0 mυl% s = 0.2 - 2.0 mol%, χ = 1, 2 π = 1-4 systsmy πρπ темпсρа гу |) е υ г 65 дυ 85 ° С and ыс ο ο κ м да с с (((3-8 -8πа). (Pat. СНΙΛ '281092 with πρиορ. 10.22.79. Ju. СΟ8Г8 / 00, 214/26).
Οдπаκο вулκапπзаτы на οснοве τаκοгο сοποлπмеρа οбладаιυ г ιιслοсκι гοчπο χοροшπм ΟДС. Τаκ, πρи 204 °С ΟДС за 70 часοπ сοсτаиляе г уже 20-35 %, а πρи 275°С ( иο даππым аιггυροв πасτοящей заявκи) - 60 %. Κροме τοгο, κаκ и в πρедыдуιцем случле сυποлимеρ являеτся жесτκим, сοдеρжиτ οτ 6 дό 12 % κρисτаллπчеαсοй φазы, чτο πρиυοдиτ κ πουышсπποй жссτκοсτπ ρсзин (дο 90) и οслοжπяеτ сгο πсρсρабοτκу.Good volcanic facilities on the basis of such a compassionate blessing in good condition of the United States. For example, at 204 ° С, the UDS for 70 hours has already grown by 20-35%, and at 275 ° С (and the second augmented request) - 60%. Otherwise, both in the case of a former case and if it is a hard one, it is 6% 12% quick, which means that there is a 90% slower speed
Наиϋοлее блιπκπм апалοгοм πο дοсτигаемοму ρезульτаτу κ πρеднυлагаемυму изοбρе геπиιο янляеτся сοπυлπмсρThe most blatantly aplicable result is that we are able to find out that there is a good reason for
ЗΑΜΕΗЯЮЩИЙ ЛИСΤ (ПΡΑΒИЛΟ 26) \νθ 00/08076 ΡСΤ/ΚШ9/00132SIGNIFICANT FOX (DR. 26) \ νθ 00/08076 ΡСΤ / ΚШ9 / 00132
4 τеτρаφτορэ гилеπа с ηеρφτορалκилвинилοвыми эφиρамπ οбщей φορмулы: (-СГ2 - СГ2 -)η - (-СГ2 - СΡ- т - (-СΡ2 СΡ-)Ρ ο ο4 τeτρaφτορe gileπa with ηeρφτορalκilvinilοvymi eφiρamπ οbschey φορmuly (-SG 2 - Cl 2 -) η - (-SG 2 - SΡ- m - (2 -SΡ SΡ-) Ρ ο ο
Figure imgf000006_0001
η = 44 - 52,5 мοль % ш = 44 - 53,5 мοль % ρ = 2,5 - 3,5 мο;п> %
Figure imgf000006_0001
η = 44 - 52.5 mol% w = 44 - 53.5 mol% ρ = 2.5 - 3.5 mo; n>%
Сοποлимеρы πυлучлюτ сοπυлπмеρизацисй πρπ τсмπеρаτуρс 60°С и давлсπии 1 1 κг/см2 [ΕΡ 0708 139Α 1 с πρиορ. οτ 21.10.94. СΟ8Г/00; 214/26]. Βулκанизаτы на οснοве τаκиχ сοποлимсροв οблалаюτ χοροшим ΟДС. Τаκ, πρи 275°С за 70 часοн ΟДС сοсτавлясτ 15%. Οднаκο, вулκанизаτы на οснοвс τаκοгο сοποлимеρа имеюτ нсвысοκοе наπρяжение πρи 100% удлинении (7,6 Μπа). Κροме τοгο, наличие κρисτалличесκοй φазы в сοποлимеρе сοсτавляеτ οτ 6 дο 10 % вследсτвии чегο сοποлπмеρ являеτся жесτκим, чτο услοжняеτ егο πеρеρабοτκу.Complications πυ will improve with an increase in πρπ τcmpeperaturas with 60 ° С and pressures of 1 1 kg / cm 2 [ΕΡ 0708 139Α 1 with πρиορ. οτ 10.21.94. СΟ8Г / 00; 214/26]. The culprits on the basis of such complications will blame the bad UDS. For example, at 275 ° С for 70 hours, the UDS is 15%. However, volcanics on the basis of such a compo- lem have a high voltage and 100% elongation (7.6 psi). In addition, the presence of a crystalline phase in the compo- sition is 6 to 10% due to the fact that it is difficult to complicate it.
Целыο πρедποлагаемοгο изοбρеτения являеτся сοздание χοροшοπеρсρабаτывасмοгο τеρмοагρессивοсτοйκοгο сοποлимеρа, υулκаπизаτы иа οсπουе κοτοροгο οбладаюτ наρяду с χοροшсϊι τеπлοсτοйκοсτыο ιι наπρяжсπнοм сοсτοянπи, высοκим ποκазаτелем наπρяжения πρи 100 % удлинении.Tselyο πρedποlagaemοgο izοbρeτeniya yavlyaeτsya sοzdanie χοροshοπeρsρabaτyvasmοgο τeρmοagρessivοsτοyκοgο sοποlimeρa, υulκaπizaτy ua οsπουe κοτοροgο οbladayuτ naρyadu with χοροshsϊι τeπlοsτοyκοsτyο ιι naπρyazhsπnοm sοsτοyanπi, vysοκim ποκazaτelem naπρyazheniya πρi 100% elongation.
Пοсτавлсиная цель дοсτигаеτся синτезοм сοποлимеρа οбщей ψορмулы I.The goal is achieved by the synthesis of a common formula I.
ЗΑΜΕΗЯЮЩИЙ ЛИСΤ (ПΡΑΒИЛΟ 26) \УΟ 00/08076 ΡСΤ/ΙШ99/00132SIGNIFICANT FOX (DR. 26) \ УΟ 00/08076 ΡСΤ / ΙШ99 / 00132
55
Уκазаπные сυποлимсρы ποлучаюτ ιюдοэмульсποииοн сοιιυлπмсρизацисй ΤΦЭ, ПΦΜЮ π алκιυшππнлοныχ эψиρυв СГ? = СГΟ (СГ2)з ΟСГ СΝ [ ПΦΛΒЭ(Ι) ] иAre there significant alternatives to emulsifying Τ Э,,,,,,,,,,,,,,,,,,,,,,,,, ? = СГΟ (СГ 2 ) с ΟСГ СΝ [ПΦΛΒЭ (Ι)] and
. Ι'з. Ι'z
СΙ-2-- СΙ;Ο :Ρ_СΡΟ(СГ.)-'СΝ [ПΦΛΒЭ(2)] ιιρи мοлыιοмСΙ- 2 - СΙ ; Ο: Ρ_СΡΟ (SG.) - 'СΝ [ПΦΛΒЭ (2)] ιιρи млыιοм
СΡз сοοτиυшеππи сυмυποмсρυи 37,5 - 68} 26,8 - 58,0; 1,0 - 4,2; 1,0 -СΡз сοοτиυшеππи сυмυποМСρυи 37.5 - 68} 26.8 - 58.0; 1.0-4.2; 1.0 -
7,3 сοοτπеτс πеιπю. Пροцссс προнοдяτ πρи τсмπеρаτуρе 60 ± 2°С н даπлснιш 6 κг/см2. Β κачссτие эмульгаτορа исποльзуюτ смесь аммοшιшыχ сοлеπ πеρφгυρгеπгаποвοП π πеρφιορнυπлιιοиοГι κπслυι. Η κачесιπе шшππлгυρл π аκτииагυρл - аммυπии илπ κалπϋ πадссρнοκιιслыϋ и наτρиπ сеρπисτοκнс.ι.ыГι сοοгиегсгнеιιιю.7.3 compares. The process is carried out at a temperature of 60 ± 2 ° C and a temperature of 6 kg / cm 2 . Ач The quality of the emulsifier uses a mixture of ammonium sulfate and alkaline oxide. Η аче аче аче ш ш ш ш - - - - - - - - - - - - - - - υ υ υ - - Amm м и л на ϋ ϋ ϋ ϋ ϋ ϋ ϋ ϋ ϋ ϋ ϋ ϋ на ϋ на на на на на на ϋ ο ο ο ο ο ο ο ο ο ο ο ο ο.
Буψеρ - κалий ψοсψυρиοκислый двузамещенный.Buψеρ - potassium ψοсψυρ and acid double-substituted.
Пρυцесс сυποлимеρπзашιи προвοдяτ в τечеπие 30 часοв. Из ллιсκса сοποлимеρ πыдсляюτ κοагуляцπеП ΜβСЬ, πρυмынлιυг ιορмчсπ υυдυϋ с эιπлουым сππρгυм π сушаг πρπ τемπеρлτуρе 60°С. Исποльзуемые в κачесτне сοмοнοмеροв ΤΦЭ и ΙΙΦΜΒЭ, а гаκже все иιιгρсдиенτы эмульснοπποи сοποлимеρизации янляюτся дοсτуπными.The process with the deadline and the deadline is 30 hours. From lllxx, we are complying with the regulation of СβСЬ, πρυмынлιυг ιορмчсπ υυдυϋ with this πππпгυм π sagag πρπ темпеρлтуρе 60 °. The most commonly used components of ЭФЭ and ΙΙФΜΒЭ, as well as all the other emulsion components and their optimization are rendered inaccessible.
Пροдуκτы выπусκаюτся πυ следующим сτандаρгам: ΙЗΦ - ΤУ 6 -02 -581 -80, ПΦΜΙЗЭ- ΤУ 301 -14-26-90, Κислοτл πсρψτυρгеπτанοвая ΤУ 301-14-36-90 Κислοг πсρψτορποπаиοвая ΤУ 301-14-35-90The products are produced πυ in the following standards: ΙЗΦ - ΤУ 6 -02 -581 -80, ПФΜΙЗЭ- ΤУ 301 -14-26-90, Дислтппрпупгпптаной УУ 301-14-36-90 Прпппψψ
ЗΑΜΕΗЯЮЩИЙ ЛИСΤ (ПΡΑΒИЛΟ 26) \ΥΟ 00/08076 ΡСΤ/Κϋ99/00132SIGNIFICANT FOX (DR. 26) \ ΥΟ 00/08076 ΡСΤ / Κϋ99 / 00132
Αммοиии надссρнοκислый ΤУ 20 478 - 75Umdis acid acid ΤУ 20 478 - 75
Κалпи πадсеριюκислыπ ГΟСΤ 4146-74Κалпі πадсеριюкислыπ ГΟСΤ 4146-74
Паτρπи ссρнисτυκислый ГΟСΤ 195-77Paτρπ and ssrnisτυκ acid ГΟСΤ 195-77
Κални ψοсψο.шοκиαιый двузамещсπный ГΟСΤ 2493-75See ψοсψο . shocked two-substitution ГСС 2493-75
Μοнοмеρы ПΦΑΒЭ (1) и ПΦΑΒЭ (2) выπусκаюτся на οπыτнοм προизвοдсτве ГП ΗИИСΚ πο СΤП 38.40 3429-82.The PFΑΒE (1) and PFΑΒE (2) technologies are available on the experimental products of the State Enterprise ΚIISΚ πο СПП 38.40 3429-82.
Сοсτав ποлученныχ сοποлимсροв οπρеделяюτ с ποмοщыο элсмеπτποгο анализл и Я Μ ΡΙ9Г - ' сπсκτροсκοππи. СπеκτρыSοsτav ποluchennyχ sοποlimsροv οπρedelyayuτ with ποmοschyο elsmeπτποgο analizl and I Μ Ρ Ι9 D - 'sπsκτροsκοππi. Theory
ЯΜΡΙ9Ρ сπимаюτ ιιа πρибορс ΑΜ-500 ψиρмы "Βгиксг" для чсгο исποльзуюτ ρасτвορы сοποлимеροв в геκсаψτορбензοле. С ποмοшыο элемснτнοι υ аиализа οπρеделяюτ сοдсρжаиие С и Ρ.YAΜΡ Ι9 Ρ sπimayuτ ιιa πρibορs ΑΜ-500 ψiρmy "Βgiksg" for chsgο isποlzuyuτ ρasτvορy sοποlimeροv in geκsaψτορbenzοle. With the simple elements of vialysis, they share the resources of C and Ρ.
Сτеπеπь κρнсτаллнчнοсτπ οπρсдсляюτ мсτοдοм меχаπичесκοи сπсκτροсκοπин в инτеρвалс τемπсρаτуρ οτ - 80 дο + 150°С.The speed of the process is quickly reduced by the mechanical speed of the temperature to 80 ° C + 150 ° C.
Пρедποлагаемοе изοбρеτение иллюсτρиρуеτся следующими πρимеρами: Пρимеρ 1.The invention is illustrated by the following examples: EXAMPLE 1.
Β οτваκуумиροванный, πρедваρиτельнο προсушенный аρгοнοм или азοτοм лπτοκлаη емκοсτыο 1 л. загρужасτся 340 г. дисτиллиροвашюй вοды, 2,55 г. πеρсульψаτа аммοния, 3,4 г. двузамещеннοгο ψοсψορнοκислοгο κалия, 5, 1 г. смеси πсρψτορгеπτанοаτа и πеρψτορποианοаτа аммοиия и 0,6 г. сеρнисτοκислοгο наτρия. Пοсле эτοгο в авτοκлав ποдаюτ смесь мοнοмеροв, сοсτοящую из 45,78 г. ΤЭΦ, 106,40 г. ПΦΜΒЭ, 4,45 г. ПΦΑΒЭ(Ι) и 13,36 г. ПΦΑΒЭ(2) в мοлыюм сοοτиο.ιιсπни 40:56: 1 :3 сοοτвеτсτвеннο. Сοποлимеρизацию προвοдяτ πρи давлсπин 6 κг/см2 π τсмπеρаτуρс 60°С. Ρсаκция προτсκаеτ в τечеιшс 30 часοн. Сοπυлимеρ из лаτеκса выделяюτ κοагуляцιϊейPre-cooked, pre-dried, dry or sapon 1 liter. 340 g of distilled water are loaded, 2.55 g of ammonium sulphate, 3.4 g of disubstituted potassium hydroxide, 5, 1 g of mixed sodium and ammonium sulphate After this, a mixture of monomers is supplied to the autoclave, which consists of 45.78 CEE, 106.40 APEE, 4.45 ADFE (Ι) and 13.36 ADFE (2) in the small community of 40.: 56: 1: 3, respectively. Composite polymerization and pressure are 6 kg / cm 2 π cm / s at 60 ° С. The site is available for 30 hours. Concomitantly secreted from the latex by coagulation
ЗΑΜΕΗЯЮЩИЙ ЛИСΤ (ПΡΑΒИЛΟ 26) \νθ 00/08076 ΡСΤЛШ99/00132SIGNIFICANT FOX (DR. 26) \ νθ 00/08076 ΡСΤЛШ99 / 00132
ΜβСЬ, προмываюτ гορячей вοдοй с эτилοвым сπиρτοм, сушаτ ιιρπ гемικ-ρл ιуρе 6()"( '. πυд илκуумυм. Βыχυд сυπυлπмсρл 1 "/„.СβСЬ, it washes hot water with ethyl alcohol, dries ιιρπ gemικ-ρл іуруе 6 () "('. Πυд илкуумυм. Βыχυд сυπυлπсрл 1" / „.
Пυ даπιιым ΙΜΡ|υΡ - сπсκτρυсκυιιππ α ρуκτуρа ποлучсπιιυгο сοποлιιмеρа сοοτисτсτηуеτ ψορмуле I, а н = 42,0 мοль % т = 54,2 мοль % ρ = 1 ,0 мοль л ~ 2,8 мυль%Да | υ Ρ с π | υ с - π с α у κ |
Μυлеκулмρиля млссл - 1 0000. Сτсπснь κρисτалличπυсτи - I % Элсмеπτиыи сυсτан сυπυлимсρа:Леυлеκρмм мл мл мл млсл мл 1сс С - 1 1. 0000 1 0000.. 1 1 1 - 1 1 1 - 1 1 1 1 1 1 1 1 1 1 1 - 1 1 1 1 - 1 1 1 1 - - 1 1 - 1 1 - - 1 1 1 - - 1 - 1 - - 1 - 1 1 - 1 - - 1 - - 1 - - 1 1 - 1 - 1 1 - - 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1Μле 1 мл мл мл мл мл мл мл мл 1 мл 1 1 1 мл 1 1 1 1 1 1 1 1 мл 1 1 1с 1 1 1 1 1 1 1 1 1 мл мл С С С С С С С С С I I I I I I I I I I
Βычисленο НайденοCalculated Found
С 22,6 22,0 ' C 22.6 22.0 '
Г 70,2 70,0D 70.2 70.0
Ν 0,4Ν 0.4
Ο 6,7Ο 6.7
Иρимеρ 2.And ρimer 2.
Β услοвияχ πρπмсρа 1 προвοдяτ сοποлимеρизацию из 42,14г. 'ГЭΦ, 108,19г. ПΦΜΒЭ, 13,1 1г. ПΦΛПЭ(Ι) π 6,56г. ПΦΑΒЭ(2).Π Conditions πρπmsρа 1 π 'GEΦ, 108.19 g. PΦΜΒE, 13.1 1g. ПΦΛПЭ (Ι) π 6.56 g. ПΦΑΒЭ (2).
Μοльнυе сοοτιюшснπе мοнοмсροв 37,5: 58,0: 3,0 : 1 ,5 % мοль (•υυ гне гс ι неππυ. Пυлучлιοτ 158, 1 г. сοποлπмсρл с πыχοдυм 93% π мυлсκуляϊ ϊιοι"ι млссυπ 120000. Сτеπеπь κρπсгалличнυсτи 1 %. Пο данπым ЯΜΡΙ9Ρ- сπеκзροсκοπии ποлучеиπый сοποлимсρ сοοτвеτсτвуеτ ψορмулс I, гдс η = 42,0 мοль %Μοlnυe sοοτιyushsnπe mοnοmsροv 37.5: 58.0: 3.0: 1, 5% mοl (• υυ gne n ι neππυ Pυluchlιοτ 158, 1 g sοποlπmsρl πyχοdυm with 93% π mυlsκulyaϊ ϊιοι "ι mlssυπ 120000. Sτeπeπ κρπsgallichnυsτi 1. %. For the sake of YaΡΙ9, the result is the best result complying with the law I, where η = 42.0 mol%
ЗΑΜΕΗЯЮЩИЙ ЛИСΤ (ПΡΑΒИЛΟ 26) \УΟ 00/08076 ΡСΤЛШ99/00132SIGNIFICANT FOX (DR. 26) \ УΟ 00/08076 ΡСΤЛШ99 / 00132
т = 55,0 мοль % ρ = 2,0 мυль % а = 1 ,0 мυль %t = 55.0 mol% ρ = 2.0 mυl% a = 1, 0 mυl%
Элϋмсιπнмπ сοсπш: ычислсиο ΗаπденοElϋmsιπnmπ sospsh: irrelevant
С 22,8 22,0 Г 70,4 70,0 Ν 0,3 - Ο 6,3 -C 22.8 22.0 G 70.4 70.0 Ν 0.3 - Ο 6.3 -
Пρимеρ 3.Example 3.
'Β услοπияχ πρимсρа 1 προвοдяτ сοποлимеρизаπшο из'Β condition 1 π ρ в в с с с с из из
87, 1 1 г. ΤЭΦ, 56,98Г. ПΦΜΒЭ, 20,92Г. ПΦΑΒЭ(Ι) И 4,98Г. ПΦΑΒЭ(2). Μοлыюс сοοτнοшеиие мοποмеροв 68,0 : 26,8 : 4,2 : 1 ,0 % мοль сυυгнеτсτвеπиο. Пοлучаюτ 160, 1г. сοποлимсρа с выχοдοм 94 % н мοлеκуляρнοй массοй 200000. Сτсπсиь κρисτалличποсτи 2%. Сτρуκτуρа сοποлимсρа πο данным ЯΜΡ,ι Ρ- сπсκτρυсκοιпш сοοτвс ι сτвуеτ ψορмуле I, где η = 70,0 мοль % т = 25,0 мοль % ρ = 4,0 мοль % а = 1 ,0 мοль %87, 1 1 g. ΤЭΦ, 56.98Г. PΦΜΒE, 20.92G. PΦΑΒE (Ι) AND 4.98G. ПΦΑΒЭ (2). The majority of the population is 68.0: 26.8: 4.2: 1, 0% moles are oppressed. Received 160, 1g. complications with an output of 94% on a molecular mass of 200,000. Compression rate of 2%. The structure is consistent with the data of Ya , ι Ρ- π с π π π π с с с ψ ψ,,,,,, где где где где, where η = 70.0 mol% t = 25.0 mol% ρ = 4.0 mol% a = 1, 0 mol%
ЗΑΜΕΗЯЮЩИЙ ЛИСΤ (ПΡΑΒИЛΟ 26) \ΥΟ 00/08076 ΡСΤ/ΙШ99/00132SIGNIFICANT FOX (DR. 26) \ ΥΟ 00/08076 ΡСΤ / ΙШ99 / 00132
ЭлсмеιггныГι ^οсτав:ElsmeggniGi ^ const:
Βычисленο Пандсπο с 23,4 23,0Calculated Pands from 23.4 23.0
Ρ 71 ,8 72,0Ρ 71, 8 72.0
Ν 0,5 ο 4,3Ν 0.5 ο 4.3
Пρимеρ 4Example 4
Β услυиияχ πρимеρа I πρυυοдяτ сοποлимеρπзашπο из 51 ,04г. ΤΦЭ, 82, 16г. ПΦΜ ΒЭ, 5,56г. ПΦΑΒЭ(Ι) и 31 ,23г. ПΦΑΒЭ(2). Μοлыюс сοοτποшеιше мοποмсροв 46,4:45,0: 1 ,3:7,3 мοль % сυυ гнеτсгнеιшο. Пοлучаюτ 159г. сοποлимеρа с выχοдοм 93,5 %ι и мοлсκуляρποй массοй 100000. Сτеπень κρисτаллιιчπυсτи I %. Сτρуκτуρа сοποлимеρа πυ даπным ЯΜΡ,,,Ι; - сπеκτρυсκυπии сουτвеτеτнуеτ ψορмуле 1 , где η = 50,0 мοль % т = 42,0 мοль % ρ = 1 ,0 мυль % а = 7,0 мοль % Элемеиτный сοсτав:Β condition χ πρimera I I πρυυοdyat οπο limеρπzashπο of 51.04g. ΤΦЭ, 82, 16g. ПΦΜ ΒЭ, 5.56g. ПΦΑΒЭ (Ι) and 31, 23g. ПΦΑΒЭ (2). It is better than 46.4: 45.0: 1, 3: 7.3 mole% with no anger. Received 159g. compulsory with an output of 93.5% ι and a mass of 100,000. The degree of crystallinity is I%. STRUCTURE OF SOCIETY πυ DAP Ya ,,, Ι ; - the concept is consistent with formula 1, where η = 50.0 mol% t = 42.0 mol% ρ = 1, 0 mol% a = 7.0 mol% Elemental composition:
Βычислеπο I ΙайденυΒΒисислеππ Ι I ΙΙυ υ
С 23, 1 22,9 Ρ 70,0 71 ,0 Ν 0,7 Ο 6,7C 23, 1 22.9 Ρ 70.0 71, 0 Ν 0.7 Ο 6.7
ЗΑΜΕΗЯЮЩИЙ ЛИСΤ (ПΡΑΒИЛΟ 26) \УΟ 00/08076 ΡСΤ/ΙШ99/00132SIGNIFICANT FOX (DR. 26) \ УΟ 00/08076 ΡСΤ / ΙШ99 / 00132
1010
Из сυποлπмеροв, сиπιсзиροванπыχ πο πρимсρам 1 -4, гοτοвяτ κοмποзиции, сοдеρжащие: κаучуκ - 100 масс. ч. бис 4,4 дπυκси 3,3, дπамиποдиψснилгеκсаψτορπροπаπ- 1 ,5 масс.ч. сажа П-701 - 25 масс.ч.Of the terms and conditions, the ideas are 1-4, there are the following components: rubber - 100 mass. h. bis 4.4 dπυκSI 3.3, dpiamidisnickel ψτορπροπаπ-1, 5 mass parts soot P-701 - 25 parts by weight
Κοмποзπцπи вулκанизуюτ в τечеπИе» 30 минуτ πρи 160°С с ποследующей τсρмοοбρабοτκοй в τечение 20 часοв πρи 250°С.It is vulcanized for 30 minutes at 160 ° С, followed by 20 minutes at 250 ° С.
Ρезульτаτы исπыτаний πρиведены в τаблице:The test results are given in the table:
Τаблица Сοсτав сοποлимеρа πο ЯΜΡ19Г, % мοл. 1 2 3 4 ΤΦЭ 42,0 42,0 70,0 50,0The table of the Compositions of the Communist Party ΜΡ 19 Y,% mol. 1 2 3 4 ΤΦЭ 42.0 42.0 70.0 50.0
ПΦΜΒЭ 54,2 55,0 25,0 42,0PFΜΒE 54.2 55.0 25.0 42.0
ПΦΑΒЭ (Ι) 1,0 2,0 4,0 1 ,0ПΦΑΒЭ (Ι) 1.0 2.0 4.0 1.0
ПΦΑΒЭ (2) 2,8 1 ,0 1 ,0 7,0PΦΑΒE (2) 2.8 1, 0 1, 0 7.0
Сτсπень κρисτалличиοсτи, масс. % 1 ,0 1 ,0 2,0 1 ,0The degree of crystallinity, mass. % 1, 0 1, 0 2.0 1, 0
Услοвня вулκаиизации: 30 мин. 160° С + 20 час. 250°С Ηаπρяжсιшс πρи 100 % удлπнсниπ, ΜПа 10, 1 10,0 10,5 10,4 Пροчиοсτь πρи ρасτяжении, ΜПа 14,0 13,0 15,0 14,5Vulcanization level: 30 min. 160 ° C + 20 hours. 250 ° С for discharge and 100% elongation, ΜPa 10, 1 10.0 10.5 10.4 Precedence and tension, ΜPa 14.0 13.0 15.0 14.5
Οτнοсиτельнοе удлииение, % 140 150 130 140Substantial elongation,% 140 150 130 140
ΟДС за 24 час. πρи 275°С 12,0 12,5 13,0 15,0ΟDS in 24 hours. πρ and 275 ° С 12.0 12.5 13.0 15.0
Τаκπм οбρазοм πρедлагаемые сοποлимеρы πο сρавнению с извесτиыми аналοгами πρедсτавляюτ сοбοй πρаκτичесκи неκρисτаллизующнеся сοединсπия, вулκанизаτы на οснοве κοτορыχ οбладаюτ наρяду с χοροшими ψизиκο-меχаничесκимиΤaκπm οbρazοm πρedlagaemye sοποlimeρy πο sρavneniyu with izvesτiymi analοgami πρedsτavlyayuτ sοbοy πρaκτichesκi neκρisτallizuyuschnesya sοedinsπiya, vulκanizaτy on οsnοve κοτορy χ οbladayuτ naρyadu with χοροshimi ψiziκο-meχanichesκimi
ЗΑΜΕΗЯЮЩИЙ ЛИСΤ (ПΡΑΒИЛΟ 26) ιιυьл злιслямιι πыιυκυπ τеιυлχ гυπκυсгью И шιπρижснιιυм сυ ιυнιιиπ н сυчеιлшш с нысυκπмπ πυκазаιслямπ πлιιρяжсπпя πρπ 100 % удлиπснии. Сοποлнмеρы χοροшο леρсρлблιывлюτся πа сτандаρτποм οбορудοвании.SIGNIFICANT FOX (DR. 26) ιιυl zlιslyamιι πyιυκυπ τeιυl χ gυπκυsgyu AND shιπρizhsnιιυm sυ ιυnιιiπ n sυcheιlshsh with nysυκπmπ πυκazaιslyamπ πlιιρyazhsπpya πρπ udliπsnii 100%. Comply with standard equipment, it is not necessary to use standard equipment.
ЗΑΜΕΗЯЮЩИЙ ЛИСΤ (ПΡΑΒИЛΟ 26) SIGNIFICANT FOX (DR. 26)

Claims

\ΥΟ 00/08076 ΡСΤ/ΚП99/00132\ ΥΟ 00/08076 ΡСΤ / ΚП99 / 00132
1212
Φορмула изοбρеτения.Description of the invention.
Сοποлимеρы τеτρаψτορэτилена и πеρψτορалκилвинилοвыχ эψиροв οбщей ψορмулы:Compounds of thermo-ethylene and pyrotechnic vinyl ester in the total formula:
(-СΡ2-СΡ2-)η - (-СГг-СГ-)т - (-СГг-СГ-)ρ - (СГ2-СГ-)а (-CΡ 2 -CΡ2-) η - (-СГг-СГ-) t - (-СГг-СГ-) ρ - (СГ 2 -СГ-) а
ΟСГз Ο ΟΟСГз Ο Ο
I II I
(СΡ2)3 СΡ2 (СΡ 2 ) 3 СΡ 2
0 СΡ-СΡз0 СΡ-СΡз
СΡ-СГз οСΡ-СГз ο
СΝ СГ2 сг2 СΝ SG 2 sg 2
СΝ , где η = 42 - 70 мοль %СΝ, where η = 42 - 70 mol%
т = 25 - 55 мοль % ρ = 1 - 4 мοль %t = 25 - 55 mol% ρ = 1 - 4 mol%
а = 1 - 7 мοль %a = 1 - 7 mol%
с мοляρнοй массοй 100000 - 200000 для τеρмοагρессивοсτοйκиχ изделий.with a molar mass of 100,000 - 200,000 for thermally aggresive products.
ЗΑΜΕΗЯЮЩИЙ ЛИСΤ (ПΡΑΒИЛΟ 26) SIGNIFICANT FOX (DR. 26)
PCT/RU1999/000132 1998-08-05 1999-04-27 Copolymers of tetrafluoroethylene and perfluoroalkylvinylic ethers used in the production of thermal-aggression resistant articles WO2000008076A1 (en)

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