CS249767B1 - Method of dicyclopenadiene's concentrate production - Google Patents

Method of dicyclopenadiene's concentrate production Download PDF

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Publication number
CS249767B1
CS249767B1 CS826313A CS631382A CS249767B1 CS 249767 B1 CS249767 B1 CS 249767B1 CS 826313 A CS826313 A CS 826313A CS 631382 A CS631382 A CS 631382A CS 249767 B1 CS249767 B1 CS 249767B1
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CS
Czechoslovakia
Prior art keywords
mace
hydrocarbons
fluiifl
hjih
concentrate
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CS826313A
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English (en)
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CS631382A1 (en
Inventor
Joachim Koetter
Franz-Joerg Becker
Irene Schmerwitz
Gerhard Toerpel
Fred Schlimper
Original Assignee
Joachim Koetter
Becker Franz Joerg
Irene Schmerwitz
Gerhard Toerpel
Fred Schlimper
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Application filed by Joachim Koetter, Becker Franz Joerg, Irene Schmerwitz, Gerhard Toerpel, Fred Schlimper filed Critical Joachim Koetter
Publication of CS631382A1 publication Critical patent/CS631382A1/cs
Publication of CS249767B1 publication Critical patent/CS249767B1/cs

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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G7/00Distillation of hydrocarbon oils
    • C10G7/08Azeotropic or extractive distillation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00Purification; Separation; Use of additives
    • C07C7/148Purification; Separation; Use of additives by treatment giving rise to a chemical modification of at least one compound
    • C07C7/177Purification; Separation; Use of additives by treatment giving rise to a chemical modification of at least one compound by selective oligomerisation or polymerisation of at least one compound of the mixture

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Description

. Cnoco6 nojiytieHHH KomjeHTpaTa flHUHKJioneHTaflHeHa 06jIaCTb ΠρΗΜβΗΘΗΗΗ Η3θ6ρεΤ8ΗΗΗ Η3ο6ρετεΗκε othochtch κ cnocočy nojiyncHHH κοΗρεΗτρετε flHUHKJioneHTaflueHaH3 φρβκΐίΗΗ Cg - , nojiynaeMyio κ3κ jKHflKyio φρβκμΗΐο b npouecce nnponn3a yr- jieBOflopo,qoB, c uBJíhio ero flanbHCHuicro Hcnonb3OBaHHH.
XapaKTepHCTHKa H3B8CTHbix tcxhhhbckhx pemeHHň ‘ Uejibio ocymecTBJíaeMoro H3bccthmm o6pa3OM npopecca nHpoJiH3a 3ch,hkhx hjih raao-o6pa3Hbix yrneBOflopoROB hbjihbtch npep;nonTHTejibHoe noJiyneHne ηη3Ιπηχ οηεφΗΗΟΒΠρΗ 3tom nonyqaaTCH pan nnpo.riH3Hbix nponyKTOB, ηηηηηηη c βοαηηογο napa floBblCOKOKHnínUHX yFJICBOflOpOflOB, HanpříMGp nHpOJlH3HOe MaCJIO. 06pa3OBaBmH8CHnpoflyKTbi nnpojiH3a pa3flenHiOTCH b 33βηοημοοτη ot hx φρεκμκοΗΗοΓο cocTaBa ny-. τεΜ φρεκηΗΟΗΗροΒεΗΗοϋ KOHfl8Hcauroi η περετοΗΚΗ Ha pa3p;8JiHT8nbHoň ycTaHOBKe.B πρΗΗρΗπε πρπ 3tom noJiynaroTcn πηροπη3ηη8 npoflyKTbi, εοβερχεπριε cneayrainHe?ΚΗ,π;κΗε φρβκηΗΗ:
ππροπΗ3Ηοε Macno,. BbiKHnaromaa Βωιπε 200°C
THJKanbM nHpoJiH3Hbiň 6εΗ3ΗΗ 130-200°C
KOHflHHCaTbl ot κοΜπρεεεοροΒ 80-160 C
Φρθκιχηη C5- Cg pa3flan8HHH ra3OB 3O-9O°C
OpaKUHH, ΒΗΚΗπειοπριε b npBgojiax MBTKHy 30° h 200°C , BooSmje o6o3HanaK>TCfl no-ηητηβμ ΠΗροπΗ3Ηο.Γο 6aH3HHa h noaTOMy hx Ha3biBaioT Tax η b flajibHcňniěM τεκετε flHT(HKJIOn8HTaflH8H (flUIIfl) npCflnoHTHT8HbHO HOJiyHa8TCH H3 φρΗΚρΗΗ Cg“ Cg ΠΗ-poJiH3Horo 68H3HHa, ΒΗΚΗΠβιοιηεΓο b npenejiax 30°C - 90°C. B stoh φρεκμηκ co·nepxHTCH npaoÓJia/xaromaH nacTb oSpasoBaBinHXCH b προηεεεε nnpoJiH3a yrnBBORO-pOflOB - Cg HapHfly C OTHOCHTCJlbHO Θοηβιπημ K0JIHH8CTB0M 68H30Jia. ΤηπηηημηcocTaB noKa3aH b cnenyroqeij τβδπκηε: 249767 -2-
Ta6jmua 1 ‘l
H3onpeH UHKnoneHTaflueH (HlTfl)
BeH3OJi
ZlHixHKnoneHTaflHeH (flUIIfl) hKo#HMepbi
KojiHqecTBO TeMnepaTypa ΚΗΠβΗΗΗ, 11-13% (Mace.) 34 10-12% (Mace.) 40,8 19-23% (nace.) 80 πρη6η.10% (Mace.) 170-182 B pe3yjibTaTe TepMHwecKoň Harpy3KH φρβκιΐΗΗ C;·- Cg bo BpeMH npouecca pa3fle-jieHHH neperoHKoň, nacTb UHKJioneHTaflueHa (mm) 3Toň φρβκιρηι noflBepraeTCHflHMepn3aynn b flHiiHKJioneHTaflHeH (flUIIfl).
IlyTeM flanbHeňiueH TepMHHecKoň o6pa6oTKH πρκ TeMnepaTypax Meawy 90 h 130° CocymecTBJíHeTCH rjiy6oKoe npeoBpaaoBaHne Ullfl b flHMepHyio <})opMy. PeaKUHH αημθ-pnaaipiH mm h flUim Hcnonb3yeTCH μηογημη cnocoSaMH c uejibio nojiyneHHH hhcto-ro flHUHKJioneHTaflueHa. B o6meM πρκ stom πρημθηηιοτ cjieflywmHe paSonne 3Tanbi: 1. flHMepH3a,u;nH Uim b flUnfl b HcxoflHoň φρβκιχΗκ; 2. OTflejieHwe neperoHKOíi ηθγκηχ yrjieBOflopoflOB ot o6pa3OBaBmerocH flUnfl» 3. MoHOMepH3au;Hfl ZUUm b UREJ; 4. IIoBTopHaH flHMepH3apHH nojiyHeHHoro b pe3yjibTaTe pacmeiuieHHH imn b HHCTMň flmw. / npHMBHeHneM flpyrnx cnoco6oB H3 φρθκιρίΗ Cg- Cg noJiynawT mm πρη ΠΟΜΟΠρί npo-UeCCOB H3BJieneHHH HJIH 3KCTpaKB;HOHHOň neperoHKoň. npHMeHHeMbie flJIH 3ΤΟΓΟpacTBOpHTejiH, yKa3aHHbie b 6ojibniHHCTBe b JiHTepaType cneflyromne: apeTOHHTpHJI, φypφypOJI, H-MeTHJIHMHflO3OJI, H_MeTHJHIHppOJIHflOH, ΑΗΜΘΤΗΒφορ-MaMHfl, aHHJIJIHH Η Τ.Π. 3to nepeqHCjreHHe yace yxa3biBaeT Ha to, hto ejih nojiyneHHH mm 6e3 npeneapH-TeJIbHOH nHMepH3aiíHH B Ztmm, HeOČXOflHMbl 3HaHHTejlbHbie 3aTpaTbl. B flaJibHeňmeM cjiejjyeT paccMOTpeTb τοηβκο OTflejieHHe neperoHkoň jierxnx yrjie-BOfíopofíOB ot o6pa3OBaBinerocH b nponecce p,BMepB3avfiii flHiiHKJioneHTaflHeHa,.t.k. H3o6peTeHne othochtch jihuib k npopeccy pa3fl&amp;rceHHH neperoHKoň. yKaaaHHan CTyneHb npoyecca ormcaHa b naTeHTHoň JiHTepaType HeflocTaTOHHo,t.k. 3p;ecb penb ηηθτ o npoyecce neperoHKH, KOTopbtíi oTBenaeT o6biHHOMy coc-TOHHHK) TeXHHKH.
OflHaKO, yHHTbIBaH ΟΠεηΗφΗΗεΟΚΗΘ CBOňCTBa npoflyKTOB Heo6xOflHMO ΠΡΗ-'ΒΤΟΜ co- 6raoflaTb Ηβκοτορωθ oco66hhocth. Tax, HanpHMep HeofixoflHMo paGoTaTb nofl ea-
KyyMOM H3-3a HannHaiomeň yace πρκ TeMn§paType 140°C MOHoMepH3aijHH BbiKHnaio- mero npn 170°C HHijHKJioneHTaflHeHa b HHKJioneHTanHeH. /Via toto, hto6h CHH3HTb .TeMnepaTypy κκπεΗΜ ho 120°C HyacHo flasJíeHHe b 20 Kila. OflkaKo, npH thkom 249767 -3 5Ke p;aBJieHHH xoHfleHcau,HH oxnaacflaiomeň βο^οη οτγοηηρ.μβιχ nerxHX yrjieBOftopoflOBy®e HeBO3MO5KHa. nponecc xoH^eHcaiiHH oxJiaawaranteH BOfloň nerxHX yrneBORopoflOBb τεχΗΜκε oSbWHo TpeByeT TeMnepaTypbi KOHfleHcauHH CBbiiue 45° C. A npn yxa3aH~hom flaBJíeHHH 20 Kila OTflenbHbie κομποηθητμ (JjpaKynH Cs- Cg KOHfleHcupyjOT npncneflywinHx TeMnepaTypax:
yrjieBofíopoflbí - C5 -30°C fló -5°C
yrjieBOflopoflbí - Cg 0°C no +25°C
6eH3OJi 35°C IIoaTOMy b τθχηηκθ paSoTaioT Ha χοποβΗΠΒΗωχ ycTaHOBKax, ητοΒω KOHneHcnpoBaTbnerxHe yrneBOflopoflbí, oTroHaeMbie H3 nnííHKnoneHTanHena non BaxyyMOM. nonywaeMbiň b npopecce neperoHKH flnu,nKJioneHTap;HeH nocjie BbnueynoMHHyTbix flanb-HeňuiHx CTyneHeň nponecca nopBepraeTCH οηκοτκε nyTeM MOHOMepH3au,HH η ποβ-τορκοΗ p;HMepH3aij(HH. BbinycKaeMbiň τθκημ o6pa3OM flUUfl hhctotoh Bbnue 95% cny-JMT CbipbeM flJIH npOH3BO,n;CTBa HCKyCCTBeHHblX CMOJI Ha OCHOBe HUUH.
Uejib H3o6peTeHHH
Uejib Η3θ6ρετβΗΗΗ 3axJnonaeTCH b nojiyneHHH H3 φρεκρΗΗ Cg- Cg πηροηη3Ηογο6eH3Hna KOHijeHTpaTa HHnHKJioneHTanHeHa, πρηγοαηογο ajih npoH3Bo#CTBa HCKyc-CTBeHHbrx cmoji Ha OCHOBe flUIlfl nyTeM πρημθηθηηη npocToft TexHOJiorHH 6e3 Ba-KyyMa h xonoflHJibHbix ycTaHOBox, a TaKKe 6e3 nonojiHHTejibHoň CTyneHH ohhctkh.
H3JioaceHHe cynjecTBa H3o6peTeHHH
-3anana, pa3pemaeMaH H3o6peTeHneM 3aflaHa H3o6peTeHHH coctoht b pa3pa6oTKe cnoco6a, c ποΜοπξΒίο κοτοροΓΟ mojkhoocymecTBHTb πρκ ηορμηιιβηομ fíaBJíeHHH βηαθπθηηθ neperoHKoň H3 φρηκιρίΗ C5-Cg ΠΗΡΟΗΗ3ΗΟΓΟ 6eH3HHa HH3KOKHnHmHX ΚΟΜΠΟΗΘΗΤΟΒ, B HaCTHOCTH yrJieBOflOpOftOBCs- Cé, c nojiyneHneM KOHneHTpaTa 6e3 μοηομθρη33ιι,ηη ero, a Taxace npH-.
MeHeHne KOHneHTpaTa flUIIfl 6e3 nanbHeňmeH oBpačoTXH ero hjih npoH3BoncTBaHCKyccTBeHHbix cmoji Ha OCHOBe flHUHKJioneHTapHeHa.
“ΠρΗ3Η3ΚΗ H3o6peTeHHH B cootbstctbhh c H3o6peTeHHeM naHiian nanana peinaeTCH nocpencTBOM τογο, htonojiyneiiHe πηπη neperoHKoň H3 $paxn;HH C5-Cg πηροηη3ηογο 6eH3HHa ocymecTBJíHeTCHoBbinHbíM nponeccoM p,HMepH3au;HH HHKJioneHTaflHeHa b HHUHKnoneHTanňeH b npHcyT"ctbhh TOJiyona h/hjih apoMaTHnecxHX yrnesonoponoB Cg. Ilonana Tonyona h/hjih • apoMaTHnecKHX yrneBonoponoB C0 cornacHo Η3οδρετεΗΗΚ) ocymecTBJíHeTCH jih6oHenocpep;cTBeHHo bó φρεκηπιο C5- Cg nepen BCTynneHneM ee b neperoHHyio kojioh-Hy, jih6o xax oTnenbHbiň ποτοκ npop,yi<Ta b neperoHHyio KonoHHy.
KojiHnecTBo Tonyojia h/hjih yrneBonoponoa Cg cnenyeT ycTaHOBHTb Tax, πτοΒω bflHpHKJioneHTaflHeHe, nonynaeMOM b ημηθη nacTH neperoHHoň xojiohhh, čoflepaca-Jiocb 6bi ot 5 no 20% (Mace.) TOJiyona h/hjih apoMaTHnecxHX yrneBonoponoB C0.Bjiaroftapn iipepjioHceHHOMy cnocoBy nonyneHHH neperoHKoň H3 φρηκρΗΗ C5- Cg nHpojiH3Horo 6eH3HHa b npHcyTCTBHH TOJiyona h/hjih apoMaTHnecxHx yrjieBOflopo- ρ,ΟΒ Cg oxa3biBaeTCB βο3μο3κημμ rjiyBoxoe BbifleneHHe ηη3κοκηπηικηχ yrneBonoponoB, 249767 -4- B. H3CTHOCTH 6eH3OJia B T3KHX TeXHOJlOrHneCKHX yCnOBHHX, ΠΟ3ΒθηίΙ!011ξΗΧ H36eraTbh pa3/io»eHHH flUIIfl h npuMeHeHHH BaxyyMa η xonoflHnbHbix ycTaHoB.OK.
BbifleaeHHe neperoHKoií conepjKauiHxca bo φρβκυ,ΗΗ C$- CŘ ηη3κοκηπηβιηχ npoflyKTOB,b nacTHocTH 6eH3OJia b HopManbHbix ycnoBHáx flaBJíeHHH tojibko pep,Ko ynaeTcn.Xtaate npn TeMnepaTypax 150°C b ηροκηθη nacTH kojiohhh coflepacaHne 6eH3ona bflUIIfl eme cocTaBJífleT 3,5% (Mace.). flo chx nop hh b κοβΜ cnynae ηθ yflanocb noeranb HacbímeHHH flUIIfl b nponyKTeH3 HujKHeň uacTH KojioHHbí cBbmie 65% (Mace.). ΠρΗ TeMnepaTypax Bbnue 130°C koh-yeHTpauiHH flUIIfl ^aace cHHacaeTca b pe3ynbTaTe ycnneHKo npoTeKarameň MOHOMepn-3annH. '
OflHaKO, b cnynae npoBeneHHH neperoHKH b cooTBeTCTBHH c H3o6peTeHneM b npn-cyTCTBun Tonyona 3φφεκτΗΒΗοοτΒ pa3n,eneHHH kojiohhm 33μθτηο ynynniaeTcn.. Koh-neHTpanna flUIIfl, pacnHTaHHan Ha OTcyTCTBne apoMaTHnecKHX yrneBOflopoaoB, tfloCTnraeT βθληηηη, jieacamnx πρηδη. Ha 10% (Mace.) Bbnne no cpaBHeHHio c peatH-mom paOoTbi 6e3 nonann Tojiyona. C uenbio flocTiDKeHHH 3τογο 3φφεκτ8 ,ηοετβτοη-Hw coflepMcaHHH Tonyona b nponyKTe H3 HnacHeň nacTH kojiohhm 8-12% (Mace) . Πο-BbiineHne conepscaHHH Tonyona He πρηβοαητ κ 3HannTejibHOMy ynynnieHHio. IloBMme-HHe KOHneHTpannH flUIIfl b nponyKTe H3 HH3a kojiohhm 3a cneT neperoHKH b npH-cyTCTBun Tonyona coxpaHjieTCH η b τηκηχ TeMnepaTypHbix ycnoBHHX, npn koto-pbix óe3 noflann Tonyona yace npoTeKaeT cnnbHaji MOHOMepn3annH flIUlfl. Tlasce npnTeMnepaTypax b HnacHeň nacTH κοποηημ 140°C eme flocTHraioTCH KOHijeHTpaipiHflUHH fló 75% (Mace.), b το BpeMH KaK npoyecc 6e3 nonann Tonyona npn 3Toňace TeMnepaType naeT KOHneHTpapnio ímilfl-πρηδη.57% (Mace.).
Enaronápn nonane Tonyona nocTnraioTCH h ynyniueHne οφφβκτηΒΗοοτΗ pa3fleneHnnh 3aMenneHne MOHOMepn3annn flUIIfl. 3aMenneHne MoHoMepH3anHH flUIIfl Ha6monaeTcn h b tom cnynae, eenn npopecc ne-peroHKH ocymecTBnaeTcn c nonaneň apoMaTHnecKHX yraeBOflopoflOB Cfl.
TaK, npn npopecce neperoHKH c nonaneň b HcxoflHHň nponyxT 6% apoMaTHnecKHxyrneBOflopoflOB Cg npn TeMnepaTypax b ηημθη nacTH kojiohhm 140°C - 150°C no-nynaioTCH KOHu;eHTpau;HH flUIIfl πρηδη. 70% (Mace.), b to BpeMH KaK npn nepe-roHKe 6e3 nonann apoMaTHnecKHX yrneBonoponoB Cg conepacaHHe flUIIfl b ηηκηθηnacTH κοηοΗΗΜ cocTaBnaeT τοηπκο πρηδη. 57% (Mace.). OflHaKO, ynynnieHHe nonacTH BbifleneHHH 6eH3ona He nocTHraeTcn H3-3a bmcokhx TeMnepaTyp κηπθηηηapoMaTHnecKHx yrneBonoponoB Cg. H3BneneHHe 6eH3ona mojkho npoH3BoflHTb b tom cnynae, ecnn b neperoHHyro ko-unoHHy flononHHTenbHo noflaeTcn BOflHHoň nap 3-20% (Mace.) Ha HcxoflHMH npopyKT.TaKHM oSpaaoM, HanpHMep b npHcyTCTBHH apoMaTHnecKHX yrneBonoponoB C0 yacenpn TeMnepaTypax b Hromen nacTH kojiohhm ot 105 flo 1306C nonynaiOT conepaca-HHe 6eH30Jia, cocTaBnniomee <1% (Mace.). IIonyneHHbiH nponyxT - flUIIfl - cornacHo H3o6peTeHHto H3 φρΗκιχηκ C5- Cg noflBep- ranen ηοιιμτηηηιο πρηγοαηοοτη k npoH3Bop;cTBy HCKyccTBeHHbix CMon Ha ocHOBe JUTOU Πρη 3tom ycTaHOBneHo, hto b cnynae πρημθηθηηη ero He na6nionanocb yxynuieHne cbohctb b npoH3BoncTBe HCKyccTBeHHbix cmohhhmx naKOB no cpaBHeHHio 249767 5 c JlIUm uhctotoh >95% (Mace,). CoRepHcaHHe apoMaTHHecKHX yrneBonopoflOB C8b KOHpeHŤpaTe /UUIfl, Bbipa6aTbiBaeMOM comacHo Η3θ6ρετεΗΗΐο, b o6meM He. Mema-ετ npOH3BOflCTBy HCKyCCTBeHHbIX CMOJI Ha OCHOBe ÍUtflfl, T.K. B yCJIOBHHX ΠρΗΜβ-HHfiMbix peaKUjiň noJiHMepn3aqnn h nojiHKOHfleHcaííHH HaxoflHT npHMeneHHe kchjiojib KanecTBe TpaHcnopTHpyioinero cpeflCTBa «jih yflaJieHHH Βορ,ω. KpoMe τογο, TOJiy-oji h/hjih apoMaTHnecKHe yrjieBOflopoflbí Cfl nacTo cnyacaT pacTBopHTejieM HcxyccT-BeHHbIX CMOJI H3 OCHOBe flUIIfl. ΠρΗΜβρω OCymeCTBJíeHHH Η3θ6ρεΤΘΗΗΗ
UpefljioaceHHbiÉ cnoco6 6onee noflpoSno noacHaeTcn c noMombio HHKecjieflyiomHX npH-MepoB ocymecTBJíeHHH. - npHMep 0
Ha JiaĎopaTopHoň neperoHHoH ycTaHOBKe noflBepraJiH neperoHKe (ppaKHHio Cg- CgnHpoJiH3Horo 6eH3HHa nocjte npeflmecTByromeň flHMepH3aijHH LUIfl b flUIIfl h Bbiflejie-hhh BbiKHnaiomHx Hrnce 6eH3OJia yrneBOflopoflOB. KonoHHa HMena 17 τβρβηοκ. Προ-nyKT noflaBajiCH Ha 7-yio Tapenxy. KojioHHa BKcnnyaTHpOBanacb npH cnenyiomHX na·paMeTpax:
TeMnepaTypa b ηημηθη nacTH κοποηημ 100-150°C
TeMnepaTypa Ha Bxop;e 80° C flaBjíeHHe b κόηοΗΗβ ετΜΟοφβρΗοε '
KpaTHoeTb opomeHHH 0,5 B KonoHHy noflaBajiH φρΗκυ,Ηΐο b KoranecTBe 96,7 r/nac co cnenyioinHM cocraBOM: yrjteBOHopogbi ,,Cj- Cfe
BeH3oň
TonyoJi
YrjieBOflopoflbí C?- CgflWW
KoflHMepbi (BKJHonaH M-flHIIfl) 3,1% (Mace.)33,7% (Mace.) 1,6% (Mace.)8,2% (Mace.) 38,4% (Mace.)15,0% (Mace.)
TeMnepaTypbi b Hnacneft nacTH kojiohhm BapbHpoBanH bBbuiH nojiyneHbí cjieflyronyie noKa3aTejin: a npeflenax 110 C h TeMnepaTypa b HHJKHeňnacTH KonoHHbí °C 110 120 130 140 150 KoJinnecTBO npoflyxTa bHHJKHeň qacTH κοποηημ r/n 75,8 65,0 57,3 50,0 41,6 CoflepKaHHe 6eH3ona bnpoflyKTe, yxonumeM H3 HH3a KOJIOHHbl %(Macc.) 22,5 •16,6 9,8 . 6,3 3,5 KoHijeHTpauHH ZRUBl,b περεεηετε Ha 6es-6eH3OJlbHbIH %(Macc.) 64,4 63,5 65,3 58,3 56,7 249767 -6- . IIpuMep 1 B HcxoflHbiň nponyKT, cornacHo npHMepy 0, nočamuiHBepraiiH neperoHKe πρπ τβχ xe ycnoBHHX npHMepa 0.yKa3aHHyio φρηκηπιο b KOJiHnecTBe 101,1 r/nac. Bmjih3aTejiH: 10% (MaceB KOJioHHynojiyneHbí . )1 ToiryoJianoflaBajiH cneflyronpiě Η ΠΟΑ' Bbirae- noKa- TeMnepaTypa b HHXHeň nacTH kojiohhei °c 130 140 150 KoJiHnecTBo npoflyKTa b HMtHeft nacra kojiohhm r/n 65 50,9 49,7 ConepacaHHe 6eH3OJia Z(m4CC.) 8,3 2,6 0,13 CoflepxaHHe Tonyona %(Macc.) 14,7 19,6 17,9 KoHu;eHTpanHH flUIIfl, b nepecneTe Ha 6e3TonyoJibHbiň h 6e36eH3onbHMň %(Macc.) 71,4 72,4 69,9 ΠρΗΜερ 2 B hcxo/xhmh προΑγκτ, corjiacHo npHMepy 0, no6aBHJiH cjieflyromne KOJOTnecTBa to-Jiyona h noflBeprajiH hx neperoHKe а) npH TeMnepaType 130°C b ηηχηθη nacTH kojiohhm h б) npH .TeMnepaType l40eC b HHXHeň wacTH kojiohhm
BbUiH noJiyneHbí cjiepyromne aHaraíTunecKue noKa3aTeJiH nponyKTá hb ηηχηθη nacTHkojiohhm: flofíaBKa Tonyona % 0 i 6 10 20 ConepxaHHe 6eH- 3OJia 7. a) 12,5 10,3 8,3 4,7 6) 6,3 4,3 2,6 0,19 CoflepxaHHe Tonyona 7° a) - 10,0 14,7 29,9 6) 12,5 19,6 30,5
KoHijeHTpau,HH '/Wm,b nepecneTe Ha 6e3- TOJiyOJIBHblH H 6e3" 6eH3OJIbHblň % a) 65,3 73,0 71,4 67 6) 58,3 ' 70,5 72,4 73 IIpHMep 3 B HcxoflHbiů npo^yKT, cornačHo npHMepy 0, noSaBHJiH 6% apoMaTHnecKHX yrjieBo- flopoflOB Cg h noflBeprajiH neperoHKe npH TeMnepaTypax 14O°C h 15O°C b HHxneň nacTH kojiohhm. B KOJioHHy nonasanH BbnneyKa3aHHyto φρβκηΗΐο b KOJinnecTBe 93 r/n. Ebinn nonyneHM cnenyioinHe aHajiHTHnecKHe noKa3aTenH: 249767 -7-
TeMnepaTypa
KojiHnecTBa npoflyKTa bHHacHeň nacTH kojiohhhCo,n;epwaHHe 6eH3ojiaCoflepacaHHe yrjieBOfloponoB
KoHqeHTpaiíHH flUHq, b nepe-cneTe Ha yrjteBOflopoflbí Cgh Ha 6e36eH3onhHMň
KoHfleHTpaflHH flUJIfl, 6e3 .«o6aBKH yrneBoflopoflOB Cfl,b nepecHGTe Ha 6e36eH3OJib-HHH °c 140 150 r/nac 43,1 41,2 %(Macc.) 7,9 9,0 %(Macc.) 12,8 15,4 %(Macc.) 68,6 70,1 %(Macc.) 58,3 56,7 IIpHMep 4 B HcxoflHbiň npoflyKT, corjiacHo npHMepy 0, floČaBHJiH 10% yrjieBoflopoflOB C0 .
Bo BpeMH neperoHKH b hhjkhioio nacTb kojiohhh noflaeajiH BOflHHoň nap b kojih-necTse 10% hjih 20% Ha HCXOflHbiň npoflyxT. B KonoHHy noflaBann BbímeyKaaaHHyioΦρηκπηκ) b KOJnroeCTBe 47Q r/nac. Ehjih noJiyneHH cjieflyfomne aHajiHTHqecKHe no-Ka3aTenn npoflyKTa b HHWHeň qacTH kojiohhh:
TeMnepaTypa b HHJKHeft qacTH KOJIOHHbl íloflana βοαηηογο napa °C %(Mace.) 105 20 110 TO 120 20 130 10 10 20 KoJinnecTBa npoflyKTa b hhjk-Heň qacTH kojiohhh r/qac 242 290 199,5 266 171 237 CoflepacaHHe 6eH3OJia %(Macc.) 1,5 3,4 0,4 2,3 0,3 1,3 CoflepjKaHHe yrneBOflopoflOB CB %(Macc.) 14,7 17,1 8,1 16,1 8,8 12,0 KoHfleHTpaflHH JUOIfl, b .·* nepecneTe na yrjieBOflopo-flbl Cg H Ha 6e36eH3OJIbHblft %(Macc.) 72,6 70,8 71,9 69,5 72,2 70,4 ΠρΗΜβρ 5
BbipaĎaTbiÉaeMbiň corjiacHo Η3θ6ρβτβΗΗΐο KOHneHTpaT flUIIfl c yenbio noflTBep»fleHHHero npHroRHocTH b xanecTBe cbipbH no cpaBHeHHio c hhcthm flUIIfl, HcnojibaoBa-nu b npoflecce CHHTe3a aJiKHflHoň cmojih. B οτθκιιηηηηη cocyfl BMecTHMocTbio1,5 n c MemajiKoň, τβρΜΟΜβτροΜ, fle$JierMaTopoM h flO3aTopoM noMecTHJiH 120 rrjiHpepHHa, 44 r nsHTaspHTpHTa h 147 r MaJieHHOBoro aHraflpHfla, HarpeBajiHhx no TeMnepaTypbi 120°C h b bifle p®a jih b TeqeHHe 30 mhh. 3aTeM npnČaBHJiH198 r HHCToro OTIIfl (coflepacaHHe > 97% Mace.) κ CMOJie A hjih 248 r noJiyneHHo-ró cornacHo Η3θ6ρβτεΗΗκ> KOHfleHTpaTa JlUIIfl (no npHMepy 1) c coflepxcaHHeM 6eH-3OJia i. 1% κ CMOJie B. PearHpyiomHe cMecH nepeMeuiHBaJiH b TeneHHe 2-x nacoBnpH TeMnepaType 150°C h nocjie stoto floSaBHJiH κ hhm 214 r ca<t>JiopoBoro Macaa 249767 8 ΜρΗΟΗ KHCJioTbi h HacKoJihKo HyjKHo κ cn.no ji a b KanecTBe TpaHcnopTHpyjomero Be-mecTBa; a řípu TeMnepaType 200°C nopseprann BTepnýHKaipra po nonyneHHH khc-hothocth MeHee 20 μγ KOH/γ. Cmojm pacTBopann b KCHJione. Ebinn nonyneHbí cne
pyiomne noKa3aTenn: CMona A CMona B KnCJlOTHOCTb 16,6 μγ KOH/r 15,9 μγ KOH/r Bfl3KOCTb (60%-Han b KCHJione) 1510 m, Ila.c 1550 m.Ila.c ΗΗ,ρεκο pseTa no hoahoh niKane 5 ΜΓ I2/1OO ΜΠ-, 5 μγ I2/100 MH
CmOJIH A Η B 3aTHpaJTO AByOKHCblO ΤΗΤ3Η3 R Β COOTHOHieUHH ΠΗΓΜβΗΤβ K CBH3yromeMy, paBHOM 1:2, c počaBKOH 0,05% Co h 0,5 Pb (κβτκρβιη β φορΜβ hx oktobtob)Ha TBep^yio CMony, h 1% obbBíHoro npepoxpaHHTejiBHoro njieHKOo6pa3yromerocBcpeflCTBa b Čejiyio naKOByro KpacKy. HcnbrraHne npopyKTa b xanecTBe cymaqerocHBO3flyXOM ΠΟΚρωΤΗΗ Ha JKeCTH Η ΟΤβΚΗβ npOH3BOJliHJIOCb C TOJimHHOH ΠΗθΗΚΗ B35(Bm . BbuiH nojiyneHM cjieflyramne noKaaaTeroi:
CMOJia A CMOJia B
CyuiKa no ΤΓΒ 14 301/3 CTeneHb BbicyuiHBaHHH 1 2 n CTeneHb BbicyuiHBaHHH 4 15 ί y#apHaH BH3K0CTb ΠΟ MaflTHHKO- BOMy Konpy no TFJI 29 771 nocne 8 cyTOK 98 c
EnecK no TTJI 107-06104/1 100%
HcnbiTaHne Ha BbiTíOKKy no OpuxceHy 6 3 ino TFJI 14 302/3 1,75 η15,5 n 102 c102%
6,2 MM nonyneHHbie noKa3aTenn n pepynbTaTbi ncnbiTaHHH JiaxoB CBnpeTenbCTByioT o npn-ropHocTH BbipačaTbiBaeMoro cornacHo H3o6peTeHHio KOHpeHTpaTa flltflfl b xanecTBecbipbH fljia cHHTeaa HCKyccTBeHHbix cmoji.
•<t>opMyjia H3o6peTeHHH "CnocoS nonyneHHH KOHyeHTpaTa flUIH H3 (JjpaKpHH Cg πηροηη3Ηογο ČeH3HHa,nonynaeMoro b npopecce nnpojiH3a κηρκπχ hhh ra3oo6pa3Hbix yrneBopopopoBnyTeM flHMepn3au;HH pHKnoneHTaflneHa n nocnepyioinero oTpeneHHH neperoHKoň HH3-κοκηπηπιηχ yrneBopopopoB, b qacTHocra 6eH3ona, OTJiiraaiomHÍJCH τβΜ, hto oTfle-neHHe neperoHKoň ηη3κοκηπηιμ,ηχ yrnesonoponoB ocymecTBJíHeTCH npn HopManbHOMflaBJíeHHH b npncyTCTBHH Tonyona η/ηηη apoMaTHnecKHX yrneBopoponoB Cg, no/ja-BaeMbix b ncxonHbiň nponyKT. jihSo nepep pncTHnnHpHOHHOH KonoHHoň, jih6o khkOTfíejibHbiň npoflyKTOBbiň ποτοκ nenocpeflCTBeHHo B pucTHnnHHHOHHyio KonoHHy Ta-kom KOJinnecTBe, ητο6η b KOHpeHTpaTe flUIlfl ycTaHOBnnocb copepacaHne Tonyonah/hjih apoMaTHHecKHX yrneBoflopopoB Cg ot 5% po 30%, npnneM b cnynae neoSxó-flHMOCTH Β HH3KH1OK) HaCTh flHCTHJIJISIJHOHHOň KOJIOHHbl flOnOJlHHTejIbHO ITOflaeTCH BO~Β,ηηοη nap b KoímnecTse ot 3% ρ,ο 20% Ha HcxopHbiň npoflyKT n KOJinnecTBO nofla- 249767 9
BaeMbix BemecTB Β33ημηο cornacóBbiBaeTca τβκ, πτο6μ conepxaHHe 6eH3OJia bκοΗΐχβΗτρβτβ He npeBbmiano 1 . ÁHHOTaiXHfl
CnocoO nojiyneHHH KOHpeHTpaTa nnpHKnoneHTaflHeHa Η3θ6ρβτβΗΗβ othochtcm κ cnocoCy noJiyMeHHH KOHijeHTpaTa flHpHKJioneHTaflHeHaHa φρβκμΗΗ Cg- Cj , noJiywaeMyio κβκ sMflKyio φρβκιχΗΐο b npoqecce imponnaa yr-πβΒΟβοροΑΟΒ c penbw ero flajibHeňraero Hcnojib3OBaHHH.
IJeJIb Η3Ο0ρβΤβΗΗΗ COCTÓHT B TOM, MTO nyTeM ΠρΗΜβΗβΗΗΜ npOCTOň ΤβΧΗΟΛΟΓΗΗOea BaKyyMa, xonoflmibHbix ycTaHoBOK h flonoJiHHTenbHoň cTyneHH otoctkh momhoftónyuMTh AHutHKJioneHTaflHeH, npn6aBJiMH cornacno H3o6peTeHHio bo φρβκιχιηοCg— C6 onpefleneHHoe KonHqecTBo Tonyona h/hjih apoMaTHqecKHX yrneBoflopoflOB a b cjiyqae HeoOxoflHMocTH Taicxce BoflMHoň nap hjih πρημο riepefl BCTynJieHHCMb neperoHHyw KOJioHHy HJiH KaK oTflejibHbiň ποτοκ ;npo^yKTa b neperoHHyio kojioh-Hy. IIojiyqeHHbiň TaKHM oSpasoM ηΗπΗκποπβΗτβηκβΗ 6ea .flajibHeňmeň οβρββοτκη mo-Μβτ npHMeHHTbCH B KaueCTBe HCXOflHOro CbipbH B npOMblIUJieHHOCTH HCKyCCTBGHHblXCMOJI.
IlpnáHaHo Η3ο6ρβτβΗΗβΜ no peayjibTaTaM sKcnepTHSM, ocymecTBJíeHHoň Βλαομοτβομno flenaM HaoCpeTeHHň η πβτβΗτοΒ fflP. 249767

Claims (1)

  1. 249 767 P R B D M fi T VYNÁLEZU Způsob výroby koncentrátu dicyklopentadienu DCPD z frakceC^ až Cg pyrolyzního benzinu, získaného při pyrolyze kapal-ných nebo plynných uhlovodíků dimerizaci cyklopentadienua následujícím oddělením destilací nízkovroucích uhlovodí-ků, zejména benzinu, vyznačující se tím, že oddělení nízko-vroucích uhlovodíků destilací se uskutečni při normálnímtlaku v přítomnosti toluenu anebo aromatických uhlovodíkůCQ přidávaných do výchozí suroviny nebo před destilačni kolonu, jako samostatný tok suroviny.přímo do destilačni« kolony, v takovém množství, aby v koncentrátu DCPD se ustá-lil obsah toluenu a/nebo aromatických uhlovodíků Οθ od $ do5O %, přičemž se v případě potřeby do spodní části destilač-ní kolony přidává vodní pára v množství 3 až 20 % výchozísuroviny a množství přidávaných látek je vzájemně upravenotak, aby obsah benzenu v koncentrátu nepřevyšoval 1
CS826313A 1981-09-22 1982-08-31 Method of dicyclopenadiene's concentrate production CS249767B1 (en)

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DD23346381A DD207096A3 (de) 1981-09-22 1981-09-22 Verfahren zur gewinnung eines dicyclopentadienkonzentrates

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US3860497A (en) * 1973-05-02 1975-01-14 Shell Oil Co Multi-stage distillation of bicycloheptadiene

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RO85634B (ro) 1984-11-30

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