CS248252B1 - Method of azo-dye stuffs production - Google Patents

Method of azo-dye stuffs production Download PDF

Info

Publication number
CS248252B1
CS248252B1 CS791666A CS166679A CS248252B1 CS 248252 B1 CS248252 B1 CS 248252B1 CS 791666 A CS791666 A CS 791666A CS 166679 A CS166679 A CS 166679A CS 248252 B1 CS248252 B1 CS 248252B1
Authority
CS
Czechoslovakia
Prior art keywords
hjih
polyorganosiloxanes
hydrolysis
process according
azo
Prior art date
Application number
CS791666A
Other languages
English (en)
Inventor
Gunter Horn
Bodo Hirsch
Hellmut Reuther
Original Assignee
Gunter Horn
Bodo Hirsch
Reuther Hellmuth
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 Gunter Horn, Bodo Hirsch, Reuther Hellmuth filed Critical Gunter Horn
Publication of CS248252B1 publication Critical patent/CS248252B1/cs

Links

Classifications

    • 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
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/38—Polysiloxanes modified by chemical after-treatment
    • C08G77/382—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon
    • C08G77/388—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
    • C07F7/02—Silicon compounds
    • C07F7/08—Compounds having one or more C—Si linkages
    • C07F7/0834—Compounds having one or more O-Si linkage
    • C07F7/0838—Compounds with one or more Si-O-Si sequences
    • 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
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
    • C08G77/26—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen nitrogen-containing groups
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B69/00—Dyes not provided for by a single group of this subclass
    • C09B69/008—Dyes containing a substituent, which contains a silicium atom

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • General Chemical & Material Sciences (AREA)
  • Silicon Polymers (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Description

1
ÍJ22S2SS£_S22É2£ZSSHS
CnocoS nony^eHHH a3OKpacHTejieň
06j}acTb_ngHMeHeHH2_H3o6geTeHHH Η3θ6ρβτβΗΗβ KacaeTca cnocoSa nojijnieHHH a3OKpacHTejieň Ha ocHOBe opraHOcn-jiOKcaHOB hjih nojiHOpraHOCHJioKcaHOB. Ohh MoryT HcnojibsoBaThCH κ3κ KayqyK,MacJtO HJIH CMOJia oGblHHblM CnOCOfíOM, a ΤβΚΧβ CIIOCOGHbl CMeWHBaTbCH C OGbRHblMHjjoGaBKaMH, OTBepxg^aTbcH h cnoiBaTbCH. Ohh MoryT τβκ«β c flpyrHMH HeoKpameH-HblMH HJIH OKpameHHMMH CHJIHKOHaMH HJIH C flpyrHMH ΠΟΗΗΜβρβΜΗ Ηβ TOJIbKO ϋΜβΠΒϊ-BaTbCH, HO H nOHHMepH3OBaTbCH HJIH COnOJlHMepH3OBaTbCH. OHH ΠρΗΓΟ^ΗΜ 3ΘΤβΜTSKXe BO Bcex flpyrHX H3BeCTHblX flJIH CHJIHKOHOB oGjiaCTHX ΓψΗΜβΗβΗΗΗ TaKHX,xax o6pa6oTxa hjih ποκρκτΗβ noBepxHOCTeň, HanpHMep, KepaMHHecKOň, cHJiHKaT-Hoň hjih MeTanjiHHecKoft πρκροβΜ, a Taxxe fljia oČpafioTKH TeKCTHJift,XapaxTepHCTHKa H3BecTHbix TexHHwecKHX pemeHHň
HaBecTHO OKpaniHBaHHe nojmopraHocHJiOKcaHOB flofiaBKOň noflxoflHnmx Heoprammec-khx hjih opraHHHecKHX πηγμθητοβ hjih KpacHTejieň,
Tax fíbuio npefljioaceHO πρημθηητβ flJia OKpanwBaHHH ÓTBepxflaeMbix nojmopraHOCHJioK-CHHOB KpacHTejm, KOTOpwe COgepXaT TpHC-(TpHMeTHJIČHJIOKCH-)CHJIHJiajIKHJiaMHHOByiOrpynny. B onHcaHHSX Η3θ6ρβτβΗΗή κ naŤeHTaM CD1A 3 888 891, 3 963 744 h3 981 859 penb HfleT b ochobhom o xhhohobmx, ηηαηγοβμχ, τηοηη^ηγοββιχ, ifcTajio-Hhhhhhobmx η aaoKpacHTejiHX. y«e πρκ nojryqeHHH tphc-(TpHMeTHJiCHJioKCH“)cHJiHjiajiKHJiaMHHa TpeCyeTCH cjioxHaa,flopórajt TexHojiorHH, πρκΗβΜ aMHH ofípaayeTCH jmmb b HeaHaHHTejibHbix KOjranecT-Bax. KpoMe Toro, KpacHTejm Ha 3τοή ocHOBe πρΗΜβΗΗΜΜ jmmb b orpaHHueHHOM .OČbeMe H3-3a ΗββΚΤΗΒΗΜΧ flJIJI nOJIHMepH3aHHH TpHC-(TpHMeTHJICHJIOKCH-)cHJlHJIbHb!XpaflHKajioB. B onHcaHHHX H3o6peTeHHň κ naTeHTaM C1IIA 2 925 3Í3, 2 927 839, 2 931 693 h2 957 744 onncbroaioTCJi xpacHTejiH Ha ocHOBe apHJiaMHHoajiKHjicHJiaHOB, Ohh τοματ-CH flJIH OKpaiUHBaHHH CTeKJIOBOJIOKOH, HaTypajIbHblX BOJIOKOH TaKHX, T3K mepCTb,xjionqaTOňyMajKHoe bojiokho, mejíK, a τβκκβ opraHHHecKHX CHHTeTHnecKHX bojiokoh; 248252 2 tskhx, K3K nojmaMHflHoe, nojmaqeTaTHoe, nojiH34>HpHoe bojiokho η t.a. ΠρΗΜβΗε-ηηθ τβΚΗΧ KpacHTejieň ftjifl nojiHopraHOCHJiOKcaHOB hejihctch o/jHaico aaTpynHeHHbíMH3-3a ckjiohhocth srn KpacHTejieft κ cHHepesHca (onHcaHHe Η3ο6ρετε- hhh k naTeHTy CU1A 3 888 891).
HecoflepJKamne κρεΜΗΗΗ opraHHnecKue KpacHTejm MoryT Taxxe npHMeHHTbcn ajihOKpaniHBaHHH CHJIHKOHOBMX ΠΟΠΗΜβρΟΒ. OflHaKO H3“3a ΤβΜΠβρβΤγρΗΗΧ BO3fleňCTBHÍÍ,KOTOpbIM nOgBepraiOTCH nOjmOpraHOCHJIOKCaHbl npH HX ΜΗΟΓΟΗΗΟΠεΗΗΜΧ ΠρΗΜεΗεΗΗΗΧ,KpacHTextH pa3pymawTCfl: hjih BbmejiHioTeH H3 cujihkohoboio nojiHMepa.
HeopraHHyecKue ΠΗΓΜεΗτω hbjihwtch τεκχε no πρηηΗΗε bmcokhx TpeSoBaHHň κ τερ-MoycToňnnBOCTH jihpjb orpaHHneHHonpHMeHHMMMH. Tax, HanpHMep, caxca πρπ B03-fleňCTBHH Bbl(?OKHX TeMnapaTyp MOW8T OKHCJIHTbCH flO flByOKHCH yrjiepOfla H CJiyJKHTΠΟ3ΤΟΜΥ B fiojIblDHHCTBe CJiynaeB TOjibKO fljlH flOCTHXeHHH npOBOflHMOCTH' CHJIHKOHO-Bbix ποπΗΜεροΒ (onHcaHHe Η3ο6ρετεΗΗΗ κ naTeHTy BejiHKo6pHTaHHH 884 208). Πρ«-MeneHne HeopraHnnecKHX ΠΗΓΜεΗτΟΒ HBjíneTCH, κροΜε τογο, TexHOjiornnecKHoneHb floporo η ΗΜεετ τοτ κεβοοτετοκ, ητο H3-3a BBefleHHH sthx nyxcepoflHbix noOTHomeHHio κ cujiHKOHy ΠΗΓΜβΗΤΟΒ yxyffraawTCH onpefleneHHbie cBoňcTBa nanojmen-Hbix nojiHopranocHJioKcaHOB.
Bo bcrx cjiynaax πρκ H3BecTHbix Meroflax OKpanwBaHHH pěni HfleT o φΗ3ΗΗεεκοΜ33ΜεΠΙΗΒΗΗΗΗ KpaCHTejIH. BcjieflCTBHe 3ΤΟΓΟ OflHOpOfliHOCTb OKpaCKH nOCTOHHHOnofleepraeTCH onacHOCTH h menna cnHepe3nca n MHrpaimn MoryT bo μηογηχcjiynaax οτρκηετειίΒΗΟ ποβληβτβ Ha csoňcTBa chjjhkohobwx npoflyxTOB.
Uejib Η3θ6ρετεΗΗΗ
Uejib Η3θ6ρετεΗΗΗ 3aKjuonaeTCH b tom, hto6m, hcxo/jh H3 jierKOflocTynHbix hcxo/i,-Hbix BemecTB, ΗβΗΤΗ TexHojiorHHHbiň η προετοή cnoco6 nojiyneHHH KpacHTejieň, cnOMOmbK) KOTOpbIX BO3MOWHO ĎblJIO 6bl KpacOHHO OÓjOpMJIHTb OCOĎOHHO CHJIHKOHbl HJIHMaccbi Ha 6a3e chjihkohob η κοτορΜε no MeHbnieň Mepe oTBenaioT bmcokhm tcxho-JlOrHHeCKHM ,ΤρεβθΒ3ΗΗΗΜ K CHJIHKOHaM. flÓJBKHa ΠΟ BO3MOJKHOCTH COXpafíHTbCH H3“BecTHaa τθχηο,πογηλ nojiyqeHHJí H περερβόοτκη chjihkohob xak, HanpHMep, ot-BepwfleHHe, cniHBKa, b flaHHOM cjiynae c ΠρΗΜεΗεΗκεΜ oĎmhho Hcnojib3yeMbix fločarrbok . ΠρΗ 3 tom KpacamHň κομποηβητ flojixeH 6biTb BCTpoeH b nojiHMepHyK) MOjiexyjiyc noMombio roMeonojiapHoň cb«3h h xpacHTajm He flojcKHbí noKa3HBaTb pa3pbiBOBCMeiDHBaeMOCTH C CHJTHKOHaMH H CJiyXHTb npHHHHOft HBJíeHHH CHHepe3HCa HJIH MHrpa-Uhh πρκ flajibHeňmeft nepepaÓOTKe. H3jioaceHHe cymHocTH Η3θ6ρετεΗΗΗ B cooTBeTCTBHH c Η3θ6ρετεΗΗβΜ u,ejib Η3Ό6ρετεΗΗΗ fločTHraeTCH tcm, hto a3OKpa-cHTejiH nojiynawT Ha ochobo opraHocHJioKcaHOB hjih nojmopraHocHjioKcaHOB, koto-pbie nocTpoaHbí H3 MOHOMepHbtx eflHHHH o6meií φopMyJΠ>ϊ R3S^°1/2, R2S*-0 h/hjih RSiOg^ rp,e R o3HaqaoT oflHHaKOBbie hjih pasjíHHHMe opraHHnecKHe paflHKajibi, 3tom BOflopo-pia hjih coflepxanmií a3orpynny opraHHnecKHň pa^HKaji.
HooJKHflaHHbíM oSpaaoM ĎbUio oĎHapyxeHO, hto b KanécTBe HBeTOOĎpaayiomero κομπο-ΗβΗΤβ flJIH flHa3OTHpOBaHHbfX apOMaTHHeCKHX aMHHOB MOryT HCnojIb3OBaTbCH CHJ1OKCH“saMemeHHbie apoMaTHnecKHe coeflHHeHHH noflOĎHbie apoMaTHnecKHM φεκοπΒΜ, εκο.πΗ3Η-pyeMblM COeflHHCHHHM HJIH apOMaTHHeCKHM aMHHaM, CHJIOKCH3aMemaHHbIB apOMaTHHeC-κηθ coeflHHBHHH He Hy«flaioTCH hh b khkhx flpyrnx 3aMecTHTenax KpOMe CHjioKcano-
BblX, HTOĎbl ĎbITb cnOCOSHblMH CJiyWHTb B KaneCTBe HBeTOO6pa3y»MerO ΚΟΜΠΟΗβΗΤβ 248252 3 fljiH cojieň flHaaoHHH. TaK κεκ cHJioKCH3aMemeHHbie apoMaTHnecKHe coeflHHeHHH mo-ryT 6biTb HcnoabaoBaHM b KanecTBe HBeTOo6pa3yiomero κομποηθητη npaKTHHecKHflJifl scex flna3orapoBaHHbix apoMaTHnecKHX 3μηηοβ, oKa3biBaeŤcn bo3mojkhmm c no-Mombio peaxnHH, corjiacHO Η3θ6ρβτβΗΗΐο, nonyueHHe pa3jiHHHbix a3OKpacHTejieH, ko-Topue no3BojiHT nonyqaTb oKpaiueHHbie opranocHJioKcaHbí hjih nojiHOpraHocHJioKcaHbi. CHaoKCH3aMemeHHbie apoMaTnaecKue coeflHHeHHH MoryT 6biTb Hcnojit30BaHH b KaaecT-Be UBeTOo6pa3yioDíero KOMnoHeHTa fljiH, HanpHMep, cjieflyroiUHX apoMaTHnecKHX 3mh—BOB B flHa3OTHpOBaHHOň φΟρΜβ! 3HHJIHH, 1-3MHHO-2,4“flHHHTpo6eH3OJI, l-aMHHO-2“-xjiop-6en3oji, l-aMHHo-4-xjiop6eH3Oji, l-aMHHo-2,5-flHXjiop6eH3oji, n-aMHHo-aneT-aHHJiHfl, MeTaHHJiOBan KHCJiOTa, cyjib<i>aHHJiOBaH KHCJlOTa, o-TOjiyHflHH, M-TojiynflHH,Π—TOJiyHflHH, 3HH3HflHH, φβΗΘΤΗΑΗΗ, KCHJIHflHH, n-aMHHOa306eH30Jl, 3ΜΗΗΟΗ3φτθΤΙ,ΗΜΜΗΟΙίΒφτΟΟνΠΒφΟΗΟΒΒΗ KHCJlOTa, 1-aMHHO-2-rHflpOKCH-4-HHTpo6eH3OJl H T.fl.
Cnoco6, corjiacHO Η3θ6ρβτβΗΗΚ>, OTjiHnaeTCH HeoxHaaHHO npocToň βηποπηημοοτβιο.'TexHOjiornnecKan óaaa, coflepacaman peaKUHio οοηθτ3ηηη, ΜΟίκετ 6biTb oSbeflHHeHaC flpyrHMH OfíbWHblMH flJIH nepepa6OTKH KpeMHHHOpraHHHeCKHX COeflHHeHHň TeXHOJlO-ΓΗΗΘΟΚΗΜΗ $a3aMH. CoqgTaHHe C flna3OTHpOBaHHblMH apOMaTHMeCKHMH aMHHaMH npo-BOflHTCH B KHCJIOM paCTBOpe, flJIH ΗΘΓΟ MOXteT 6bITb npHMO HCnOJlb3OBaH KHCJIblíípacTBop rHflpojiH3a opraHOxjiopcHJiaHOB. B cjiynae Hcnojib3OBaHHH ajih rHflpojiH3ab KauecTBe pacTBopHTejia apoMaTHnecKHX coeflHHeHHň, ocymecTBjíHeTCH nocjieflyio-utaH aa coaeTaHHeM aacTKa KpacHTejiH, corjiacHO H3o6peTeHHio, npocTbiM OTflejie-ΗΗβΜ BOflHOÍÍ φβ3Η.
Tax, HanpHMep, MoryT 6ητβ rHflpojiH3OBaHbi ο6μηηβιμ cnocoBoM xjiopcHJiaHbí, coflep-xcaniHe φeHHJIbHy^o rpynny, b tbkom apoMaTHflecKOM coeflHHeHHH, xax TOJiyoji. Bkhcjimh oxjiaxaeHHbiň rHflpojiH3Hbiň pacTBop npHKanbroáwT πρκ nepeMeniHBaHHH npefl-BapHTejibHO αη33οτηροβ3ηηβιη pacTBop apoMaranecKOFO aMHHa, Moxho Tarae flo-SapnHTb KHCJlblH rHflpOJIH3HblH paCTBOp ΚρβΜΗΗΗΟρΓΒΗΗΗβΟΚΟΓΟ CoeflHHeHHH K pacT~BOpy cojih flHa30HHH. 3aTeM fljia aaBepmeHHfl coaeTaHHH flonojiHHTejibHO nepeMenm-eaioT h no οκοηη3ηηη OTflejiHWT BopHyio φa3y. OpraHHnecKyio nacTB HarpeBaioT flonpH6jiH3HTe,nbHO 160°G npH nerKOM BaxyyMe (10-200 τορρ) πρκ 9tom οτγοηηιοτοηocTaTonHaa a3eoTponHaH CMecb BOfla - xjiopHCTbiň BOflopofl - pacTBopHTejib h jie-Tynne κομποηθητη, TaKHM cnocoGoM nojiynaiOT b cootbgtctbhh c Hcnojib3OBaHHbiMflH33OTHpOB3HHbIM ΚΟΜΠΟΗβΗΤΟΜ COOTBeTCTBylOmHe KpaCHTejIH Ha OCHOBe OpraHOCHJI“oKcaHos hjih nojmopraHCHnoKcaHOB, npeRHa3HaneHHbie oco6eHHo ajih chjihkohobHJIH M3CC Ha OCHOBe CHJIHKOHOB. OcoSblM npeHMymeCTBOM penieHHH, corjiacHO H3O6-ρβτβΗΗΐο, HBjíHeTCH το, Ητο flocTaTOHHO ywe óflHoro CHJiOKcaHOBoro aaMecTHTejiab apoMaranecKOM coeflHHeHHH, hto6m cflejiaTb sto coeflHHeHHe npHroflHbíM b xa-necTBe flBeTOoČpaayiomero KOMnoHeHTa ajih αη33οτηροβ3ηηογο apoMaraHecKoro 3mh—Ha h tíTOÓM nojiyxiHTb aaoKpacHTejih. 3to 03HanaeT, hto npaKTHnecKH Bce opraHo-CHfloKcaHbí, nojmopraHocHJioKcaHbí hjih opraHocHJioKcaHOBbie coeflHHeHHH MoryT 6μτβHCnOJlb3OBaHbl Β Κ3ΗβΟΤΒβ flBeTOO6pa3ywmerO KQMnOHBHTa fljiH flHa3OTHpOB3HHbIX __apoMaTHaecKHx βμηηοβ,nocKOJibKyohh ημθιοτοαηη eflHHCTBeHHbiňHe3aMemeHHbiii apoMa-THnecKHň paflHKaji y aTOMa κρθμηηη, b npocTeňmeM cjiyaae φβΗΗΐη,Ηωύ paflHKaji.
Tax KaK b npoflecce peaxflHH coHeTaHHH coxpaHHioTCH Bce ΦνΗΚΑΗΟΗΗτίΒΗΗβ rpyn-nbi, HMeiomHecH β αΑηηομ cjiynae y aTOMa κρβΜΗΗΗ hjih b opraHOCHjioKcaHOBoň mo-Jiexyjie, το hhhto He MemaeT flajihHeňraeň nepepa6oTKe sthx KpacHTejieň, OhhMOryT 6bITb HCnOJlb3OBaHbI B ΤΗΠΗΗΗΜΧ φΟρΜβΧ ΠρΗΜΘΗΘΗΗΗ CHJIHKOHOB, HanpHMep,
B BHfle oKpameHHoro MeTHJ^eHHJi- hjih Φθηηιιοηιιηκοηοβογο Mácjia, Kax oKpameH-1 Hblň CHJIHKOHOBblň KayHVK HJIH KaK ΟΚρ3ΠΙβΗΗ3Η CHJIHKOHOB 33 CMOJia. OHH MOryT 6biTb nojiyueHbí KaK b HeHanojiHeHHOM ‘coctohhhh b BHfle OKpaineHHbrx np03panHbixnpoflyKTOB hjih B BHfle, HanpHMep, HanójiHeHfibix OKpameHHbix cnjiHKOHOBbix Kayay- 248252 4 ΚΟΒ, Tax Η ΠρΗΜβΗΘΗΜ Β BHfle ΟΤΤβΗΟΜΗΗΧ naCT flna flpyrHX nOjiHMepOB, ecjmOHH C ΗΗΜΗ ΒΜβΟΤβ CfflHBaiOTCH HJTH COnOJIHMepHByiOTCH. 06pa6OTKH HJ1H ΠΟΚρΗΤΗΗnoBepXHOCTeň c uejibio, HanpHMep προτΗΒΟχορροΒΗΟΗΗοϋ samu to MoryT c hx no-Μοπρ,ιο Taxxe npoBOflHTbcH, xax h c flpyrHMH cHJWKOHaMH, rax xax sth npopyxTH,COrnaCHO Η3θ6ρβΤβΗΗΚ>, HBJIHIOTCH X3X XpaCHTejIHMH, ΤβΚ H CHJIHXOHaMH,
ΠρΗΜβρΜ OCymeCTBJieHHH H3O6peTeHHH ΠρΗΜβρ 1
PacTBOp 21,2 BecoBOfl nacTH 4>eHHJrrpHXjiopcHJiaHa b 10 BecoBbix aacTHx TOjiyojianpHKanbiBaiOTonpH nepeMemnBaHHH b τβηβΗΗβ 10 mhh. b Tpexropjiyw xoji6y c 06-paTHblM XOJIO^HJIbHHKOM, B KOTOpOH HaXOflHJlHCb 54~BeCOBbie M3CTH flHCTHrtJIHpOBaH ·Hoň BOflbí h 32 BecoBwe mbcth MeTaHojia. Ho οκοημηηηη npHKanuBaHHH pacTBOpa(fceHHJiTpHXjiopcHJiaHa peaxnHOHHyio CMecb oxjiawflaioT flo 5°C h ΜβρυιβΗΗΟ npHxanbi-BaiOT paeTBOp COJIH ffiHa3OHHH, nOJTiyHeHHOfi 06blHHblM cnocoeoM H3 9,3 Becosoftmbcth aHHJiHHa, c Taxoň cKopocTBio, hto6m TeMnepaTypa ne npeBbímajia 10°0,Ilocae 3τογο coflepatHMoe nepeMenmBajOT etne τρκ qáca npa noHHxeHHoň TeMnepaTy-pe, mto6h nojiHOCTbw 3aBepmHTb peaKymo ccnieTaHna. Πο OKomamm οτρ,εηπητBOflHyro 4>a3y h «HcTRnnanHeň ynajjflioT opraromecKuň pacTBopHTejib. OcTaBnraňcHnpoflyKT npeflCTaBJíaeT co6oň npO3paMHy» xejiTO-xopHHHeByio CMOjiy, KpacanjHňκομποηθητ β κοτοροή xapaxTepHayeTCH MOHOMepHbíMH eflHHHpaMH cnepyromeň o6qeft4>opMy.ní>i: (CéH5-N=N-CéH4SÍO3/2 )x ngHMeg_2
CoOTBGTCTBeHHO npHMepy 1 ΓΟΤΟΒΗΤ FHflpOJIH3HbIH paCTBOp 4>eHHnTpHXJIOpCHJiaHa.06bWHbiM cnocofíoM AHaaorapyioT 18,3 BecoBoň tiaCTH 2,4-flHHHTpoaHHjiHHa, Tuňpo-jni3Hbiň paeTBOp npHxanbiBaioT npH nepeMeuiHBaraiH B oxjia«peHHbiň flo 0°C pacTBopcojth flna3OHna c Taxoň cxopocTbto, mto6h TeMnepaTypa He npeBbirnajia 5°C. ΠοoxoHwaHHH npHxanbroaHHH flanbHeňmyio o6pa6oTxy ηροΒΟ^ΗΤ Tax xe, xax onucanob npHMepe 1. ΤβΜΗΟ-κορΗΜΗβΒΗή npoflyxT coflepxHT b xanecTBe xpacantero χομπο-HeHTa MOHOMepHbie 3BeHbH, onHCbmaeMbie cjienyioineft oómseň 4>opMyjioň: I . C(O2N\ CsH3-N=N-CeH4SiO3/2Jx 10 BecoBbix aacTeťí cmojim pacTBoparoT B 90 BecoBbtx nacTflx Tonyojia h hshochttohxhm cjioeM Ha ajuoMHHHeBbie, CTajibHbie h MeflHbie nojiocKH. Taxxe nocTynajiH cocMonoťi, flaHHoň b npHMepe 1, nojiyneHHOň, o#Haxo, 6es floĎaBKH cojih flHa3OHHH.Ó6pa6oTaHHbie MeTajuiHMecxne hojiockh noMemajin b sxcHxaTOp c cojiHHoxHcjioft cpe-floň. Ilocjie 20 flHeň BbwepxKH hojiockh, xoTOpwé 6mjih ποχρωτω HeoxpameHHoft cmo-noň, noxa3broajiH yxenpH3HaxH xoppO3HH, TOrfla xax apyrne 6mjih eme 6β3 sthxnpH3HaxOB. ΠρΗΜβρ 3 CMecb h3 50 BecoBbix nácTeň φβΗΗήτρΗΧΠοροΗΠβΗΗ, 25 BecoBbix nacTeň ,π,ΗφβΗΗπ-flHXJiopcHJiaHa h 100 BecoBbix nacTeň Tojiyojia CMeioHBaioT nocTeneHHO npn nepeMe-ΠΜΒβΗΗΗ B XpyrJlOflOHHoft XOJl6e C OÓpaTHMM XOJIOffHJIbHHKOM C 200 BeCŮBblMH MaCTH“mh flHCTHJuiHpoBaHHoň BOflbi. Ποτομ nepeMeniHBaioT eme 30 mhh, η 3βτβΜ npHxanhiBa-KJT ΠΡΗ 0°C paCTBOp COJIH £H33OHHH, nojiyMeHHOň H3 56 BecóBbix Hacreň Π-ΗΗΤρθ-aHHJiHHa, c τβκοή cxopocTbio, mto6w TeMnepaTypa He npeBbímajia 5 C, fljia aaBep-meHHH peaxHHH coMeTariHH nepeMemHBajiH eme 30 mhh, Hocjie οτρεηβΗΗΗ HeopraHH- 248252 5 qecKoro pacTBopa οτγοηηιιη c πομοπιβιο BaKyyMHoň ahctujuihuhh oprammecKuňpacTBOpHTenb. lIojiyqajicH KpacHO-κορΗΗΗβΒωή pacnjiae, Π£ΗΜ£2_4 B KpyrnoflOHHoň Koji6e CMemHBaiOT npH nepeMeniHBaHHH 58,6 BecoBoň qacTH ΜετΗΠ-TpHaneTOKCHCHJiaHa c 29 BecoBbíMH qacTHMH fln<beHnjicmiaH#HOjia, Πο oJcjiajK#eHHHflo 0°C npoflyKT Hcnojib3ywT b KaqecTBe UBeT0o6pa3yromero κομποηθητβ ^jih pacT-Bopa cojih flHa30HHH, nojiyqeHHoro H3 27,6 BecoBoň qacTH n—HHTpoaHHJiHHa, noč-ně saBepme.Wia πρκ okojio 5 C peaKimu coqeTaHHH h OTflejieHHH o6pa3OBaBnierocHnojiHopraHocHJiOKcaHa nojiyqaioT 3ejieHo—KopHqHeBbiň pacnjiaB, κοτορωή xapaKTepn-3yeTca cjienymmeň o6meň <l>opMy.noň: (CH3COO)2 (CH3)Si-O-Si(RťR2) -O-Si(CH3)(CHjCOO^ R’ = -C6H5-N=N-C6H4-NO2 R< Π£ΗΜβ£_5 nonyqaiomywcH no npnMepy 1 CMecb no OTgejieHHH BOflHOň φβ3Μ oxjiaacflaiOT eme pa3flO npH6jlH3HTeJlbHO 0-5°C H CMeiDHBaiOT C paCTBOpOM COJIH ΉΗ33ΟΗΗΗ, nOJiyqeHHOňH3 28,7 BecoBoň qacTH 1 —ημηηοη3Φτηιι3μηη3 . CMecb nepeMeniHeaiOT eme 3 qac. npHnoHHHceHHoň TeMnepaType, 3βτβΜ b nejiHTejibHÓň BopoHKe OTflejiaioT BOflHyio φa3y hocTaTOK flHCTHJumpyioT b BaxyyMe tijih yflajieHHH pacTBopHTejiH, nojiyqaeTCH xpac-Hbiň pacnnaB, κοτοριπή πθγκο pacTBopneTCH b 6eH3ojie, Tojiyojie, KCHJione, rh-ΜβτηηφορΜβΜΗΑβ, 3THJiaťieTaTe, aqeTOHe h T.fl, ΠρΗΜβρ 6 B KpyrnoflOHHoň Koji6e pacTBopawT 13 BecoBbix qacTeň n-xnopaHHJiHHa, 50 BecoBbixqacTeň BOflbí h 30 BecoBbix qacTeň KOHueHTpHpOBaHHoň cojiHHQň khcjiótij h no ox-jiajKfleHHH flo 0°C flHa3OTHpy»T. B stot pacTBOp cojih αη33οηηη npHKanbiBawT πρκ0°C CMecb H3 22 BecoBbix qacTeň AeHHJiTpHXJiopcHJiaHa h 20 eecoBbix qacTeň to-jiyojia c τβκοή cKopocTbio, ητοβω TeMnepaTypa peaKiiHOHHoň cMecn He npeBbímajia+5 C. Πο OKOHqaHHH npHKanbroaHHH nepeMemHBaioT πρκ ποηη^κθηηοη TeMnepaTypeeme 3 qac. ajih 3aBepmeHHH peaKiiHH coqeTaHHH h 3aTeM nocTynaioT Tax we, khkonncaHO b npHMepe 1. nojryqaeTCH CMOjiHCTbiň npOflyKT necoqHoro flBeTa.
OopMyjia H3o6peTeHHH 1. Cnocoó nojiyqeHHH aáOKpacHTejieň Ha. ocHOBe opraHOCHJioKcaHOB h nojmopraHO-CHJIOKCaHOB, CHHTeSHpOBaHHbIX H3 MOHOMepHbIX eflHHHfl R3SiO^2 , RjSiO h/hjih RSiO3/2 rfle R o3HaqaeT oflHHaKOBbie hjih pa3jiHqHbie opraHHqecKHe paflHKajibi, 3tom BOflůpo-fla hjih κοΜποΗεκτ, coflepxaniHH a3orpynny, c πομοπιβιο rHflpojiH3a h KOHfleHcaiiHHopraHoxjiopcHjiaHOB hjih qepe3 peaKUHio opraHocHJiaHOB hjih OpraHOCHJioKcaHOB, hjihnojiHopraHocHjiOKcaHOB,OTjiHqajotnHňcH τβΜ, hto CHJioKCH3aMemeHHbie apoMaTHqecKHeCOeflHHeHHH ČoqeTaiOT c AH33OTHpOBaHHbIMH apOM3THqeCKHMH aMHHHMH· 2. Cnocofí no nyHKTy 1, OTJinqaiomHňcH τθμ, hto coqeTaHHe c flHa3OTHpoBaHHbiMHapOMHTHqeCKHMH aMHHaMH npOHCXOflHT B KHCJIOM BOflHOM paeTBOpe BO BpeMH rHfl-pojiHaa opranoxjiopcHjiaHOB. 248252 6 3. Cnocofí no nynKTy 1, OTJiHHawinHHCH τβΜ, mto coneTaHHe c αηη3οτηροβ3ηημμηapoMaTunecKHMH aMHHaMH προτβκθβτ b khcjiom bo#hom pacTBope nocjie rHflpojiH·3a opraHOxnopcnJiaHOB. 4. Cnoco6 no nyHKTy 1, OTjnrqáioDutňcH τβΜ, ητο coneTaHHe c αη33Οτηροβ3ηημμηapoMaTHMecKHMH aMHHaMH προτεκββτ nocne hjih bo BpeMa npeBpameHHH b nojiH-OpraHOCHJlOKČaHM. AHHOTAUHfl_
Η3θ6ρβτβΗΗβ KacaeTCH a3OKpacHTejieň Ha οοηοβθ OpraHOCHJioKcaHOB hjih nojinop-raHOCHJIOKCaHOB. OhH CHHTe3HpOBaHbI H3 MOHOMepHbIX eflHHHIU R5SÍOf^2 , RzŠíO m/hjih RSiO3/2 ryje R osHanaeT oflHHaKOBwe hjih pa3jiHHHbie opr&amp;HHHecKHe pa^HKanbi, btom BOflopo-fla hjih κομποηθητ, conepJKamHň a3orpynny. KpacHmHň κοΜΠΟΗβΗΤ CB«3aH c chjihko-HOBoň MojieKynoň roMeonojiupHoň cbh3I>jo h BCTpanBaeTCB b nojiHMepHyro MOjieKyjiyconeTaHHeM c αηββοτηροββηηημη apoMHTHUecKHMH aMHHaMH. Πο 3 το My npocroMy cnoco6y mojkho nojiyuaTb OKpameHHbie b mHpoKHň οπβκτρ chjihkoho-Bbie npoayKTbi Bcex bh«ob . 3thKpacHTeJiH npHMeHHMbi ksk cMonbi,MacJia hjih KayqyK,cMe~raaHHbiň b naHHOM cnynae c ο6ηηημμη flo6aBKaMH,TaK h b xanecTBe οττβΗΟΗΗωχ nacr ^jihOKpameHHbix chjihkohob.Ohh npHroflHhi TaiCKe ftJiíi Bcex flpyrnx H3BecTHbix nejieBbixΠρΗΜβΗβΗΗΗ pHJIHKOHOB ΤΗΚΗΧ, KBK cononHMepH3an;HH C ftpyFHMH nojiHMepaMH, o6-paÓoTKa hjih ποκρΜΤΗβ nosepxHOCTeň, ttanpHMep, KepaMHnecKofi, cHJiHKaTHoň hjihMeTanJiHneeKOH npHpoflbí, a τβκχβ hjih o6pa6oTKH τθκοτηπη. ΠρΗ3Η3ΗΟ Η3θ6ρβΤβΗΗβΜ ΠΟ pe3yjIhTaTaM 3KCnepTH3bI, OCyiHeCTBJíeHHOfl BeflOMCTBOMΠΟ fleJiaM Η3θ6ρεΤβΗΗ/ί Η ΠβΤβΗΤΟΒ FflP. 248252

Claims (3)

  1. 248 252 PfiiDMST VYNALEZU
    1. Způsob výroby azobarviv na základě organosiloxanů apolyorganosiloxanů syntetizovaných z monomerních jedno- tek a/nebo RSiO. Rj SÍOj/2 » Rg SJ.O' «/ UBUU HOXU^/2 »kde R znamená stejné nebo rozdílné organické radikály,atom vodíku nebo složku obsahující azoskupinu, hydrolýzoua kondenzací organochlorsilanů nebo reakcí organosilanůnebo organosiloxanů, nebo polyorganosiloxanů, vyznačujícíse tím, že aromatické sloučeniny substituované siloxysku-pinami se kopulují s diazotovanými aromatickými aminy.
  2. 2. Způsob podle bodu 1, vyznačující se tím, že kopulaces•diazotovanými aromatickými aminy probíhá v kyselém Vod-ném roztoku o hodnotě pH 1 až 3 v době hydrolýzy organo-chlorsilanů. 3· Způsob podle bodu 1, vyznačující se tím, že kopulaces diazotovanými aromatickými aminy probíhá v kyselém vodnémroztoku o hodnotě pH 1 až 3 po hydrolýze organochlorsilanů.
  3. 4. Způsob podle bodu 1, vyznačující se tím, že kopulace sdiazotovanými aromatickými aminy probíhá po přeměně nebov době přeměny na polyorganosiloxany.
CS791666A 1978-04-05 1979-03-12 Method of azo-dye stuffs production CS248252B1 (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DD20458978A DD140469B1 (de) 1978-04-05 1978-04-05 Verfahren zur herstellung von azofarbstoffen

Publications (1)

Publication Number Publication Date
CS248252B1 true CS248252B1 (en) 1987-02-12

Family

ID=5512076

Family Applications (1)

Application Number Title Priority Date Filing Date
CS791666A CS248252B1 (en) 1978-04-05 1979-03-12 Method of azo-dye stuffs production

Country Status (7)

Country Link
JP (1) JPS54148819A (cs)
CS (1) CS248252B1 (cs)
DD (1) DD140469B1 (cs)
DE (1) DE2908206A1 (cs)
FR (1) FR2421931A1 (cs)
GB (1) GB2018804B (cs)
SU (1) SU973579A1 (cs)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5070158A (en) * 1987-03-12 1991-12-03 Hewlett-Packard Company Covalently labeled siloxane polymers
EP0283206A3 (en) * 1987-03-12 1990-08-22 Hewlett-Packard Company Covalently labeled siloxane polymers
DE19710461A1 (de) 1997-03-13 1998-09-17 Wacker Chemie Gmbh Farbstoffreste aufweisende Organopolysiloxane
JP5518697B2 (ja) * 2007-05-11 2014-06-11 ビーエーエスエフ ソシエタス・ヨーロピア 高分子色素

Also Published As

Publication number Publication date
DD140469A1 (de) 1980-03-05
SU973579A1 (ru) 1982-11-15
DD140469B1 (de) 1980-12-24
JPS54148819A (en) 1979-11-21
GB2018804A (en) 1979-10-24
FR2421931A1 (fr) 1979-11-02
GB2018804B (en) 1982-12-08
DE2908206A1 (de) 1979-10-11

Similar Documents

Publication Publication Date Title
Zimmer Effects of the antibiotics netropsin and distamycin A on the structure and function of nucleic acids
CA1131629A (en) 20-0-acylmaytansinoids
US4361650A (en) Fermentation process of preparing demethyl maytansinoids
Griffiths et al. Cycloamyloses as catalysts
AU526571B2 (en) Alkyl derivatives of c-076 compounds
ES402651A1 (es) Procedimiento para la preparacion de derivados de la cefa- losperina.
KR840004712A (ko) 벤조퀴논 유도체의 제조방법
CS248252B1 (en) Method of azo-dye stuffs production
WO1999009965A3 (en) Anti-inflammatory agent
GB1428793A (en) Cephalosporins
DK0602597T3 (da) Fremgangsmåde til fremstilling af indolopyrrolocarbazolderivater
JPS56161393A (en) Beta-lactam compound
HUP9903806A2 (hu) Eljárás kolchicionid vegyületek biológiai átalakítására a megfelelő 3-glikozil-származékokká
Kugelman et al. Semisynthetic aminoglycoside antibacterials. Part III. Synthesis of analogues of gentamicin X 2 modified at the 3′-position
AU6221596A (en) Method for the preparation of taxol and its derivatives
JPS5515445A (en) Introduction of amino-protecting group by microorganism
DK484584A (da) Oestran- og androstanderivater, fremgangsmaade til deres fremstilling og praeparater indeholdende disse forbindelser
EP0004466A1 (en) Demethyl maytansinoids and methods for producing them
CA2044696A1 (en) Process for the production of organosilicon compounds
Oscarson et al. A stereoselective approach to phosphodiester-linked oligomers of the repeating unit of Escherichia coli K52 capsular polysaccharide containing β-D-fructofuranosyl moieties
Argoudelis et al. Microbial transformation of antibiotics. V. Clindamycin ribonucleotides
KR970043017A (ko) 종속영양배양(암배양)에 의한 고농도 클로렐라 배양방법
AU1200395A (en) Steroid derivative
Wu et al. Thalicsessine, a new C20-diterpenoid alkaloid from Thalictrum sessile Hayata
ES437842A1 (es) Procedimiento para la preparacion de cefalosporinas.