CS260015B1 - Method of phthalimide production - Google Patents

Abstract

The solution relates to the production method phthalimide used in the synthesis of retarders vulcanization of rubbers. Production of phthalimide is performed by interaction phthalic anhydride with urea to be used in a molar ratio of 1: 0.5 to 0.7, at temperature of 95 to 115 ° C and pressure of 2 to 80kPa. The reaction mass was then heated to 150 to 170 ° C to yield the target product in quantity 99 to 100% having a melting point 234 to 237 ° C and contains no more than 0.5% acid additives and at most 50% ammonium salts.

Description

-1- A. OIIHCAHHE H3OBPETEHHH TO ABTOPCKOMY CBHflETEJIBCTBy 3aHBJieHo: 29.06.813aflBKaj Ν »3328304 / 23-04 MKH1: C 07 D 209/48

Abtopm: A.A.Obmhhhhkob, Β.Π.Αυαηη, B.B.Kohob, M.M.PanonopT, Β.Η.ΧπμΟοβ, B.B.flaBHTyjiHaHH, B.H.rópCyHOB, E.C.MaKaposa 3aHBHTeni>: HayuHo-HccnenoBaTeJii »CKHft ηηοτητυτ χημηκθτοβ ππη ποπΗΜβρΜΜχ Μβτβ-pnajiOB (HHHXHMnOJIHMEP)

HaaBaHHe Η3θ6ρβτβΗΗπ: CIIOCOB ΠΟΠΥΗΕΗΗΒ ΦΤΑΠΗΜΗΑΑ Η3θ6ρβΤβΗΗδ OTHOCHTCB Κ yCOBepmeHCTBOBaHHOMy cnocoey nonyneHHH φΤβΗΗΜΗΑβ, mHpoKo HcnojiBsyeMoro b XHMunecKoft npoMbimneHHocTH b xanecTBe npoMesyroBHoronpoflyKTa Rip cHHTe3e saMenroiTejieft noAByjiKaHHaamní xaynyKOB H B-φβρΜβηβΒΤΗ qecKoň npóMbnnneHHocTH np "CHHTese aaahhh.

KsBecTeH cnocoG nonyaeHHa φτβηκΜΗΑβ BsauMOAeftcTBHeM 1 hojíš φτβπβΒοΑ khcť · JIOA hjih ee 3ηγηαρηαβ c 0.5-2 mojihmh (c πρβΑηοΗτκτεπΒΗΟ 0.75-1 money) xapGa-; IMFF NPH TewnepaType 130-230 DEG C. b cpefle apoMaTHaecxoro pacTBopHTeaa, ογρΒηη-aeHHo pacTBOpawmero IrByByw xacnoTy h eHhflpufl, ho He pacTBOparomero xap-> 6aMH «. UeaeBoft nponyKT BbweaajoT hs eyeneHSHH ιχβΗτρΗφνΓκροΒβΗΗβΜ, ocaaox προ-'MUBaioT ot pacTBopHTejia boao # h cymaT. Buxoai φτβπΗΜΗΒβ cocTaBJíaeT 90-96X otTeopHH, TeMnepaTypa naaBneHHa panna 232-235’C (1).

AND

HeptocTaTKOM yxa3aHHoro cnocoCa aBaaeTča ΗΟπαπΜΟΒβΗΗβ tokchbhmx h noaca-pOOnaCHUX paCTBOpHTeaeA, HeoGxOAHMOCTb φΗΠΙ> ΤΡ0ΒβΗΗΗ eyeneHSHH, npOMWBKH HcymxH ocaflKa, pereHepaimn pacTBOpHTena, ηηπηηηθ 3HaHHTenbHoro xonnaecTBactokhmx boa, 3arpH3HeHHhix pacTBOpHTeaeM.

HanConee Ďjihskhm to npeAnoxeHHOMy cnocoCy no TexHHaecxoň cynpiocTH h aocth-raeMOMy peayjibTaTy asaaeTca cnocoG nonyaeHna Φτβπημηαβ BsaHMOAeňcTBHeM φτβ-nesoro aHrHApHAa c xapfíaMHAoM πρη "μοπβηομ οοοτηοπιθηηη 1: 0.8 πρκ TeMnepaType150-170 ° C (2). .....__ 260015 . 2- 06pa3OBaBUieecH b pe3ynbTaTe peaKflnn TBepfloe BemecTBO cycneHflnpyioT b κηπη-Men BOfle (J) * HjibTpyroT npoMbreaioT BOfloň η οτ3κημ3ιοτ, Bbixofl cocTaBJíneT 91.5% bnepecneTe Ha 3arpyxeHHbiň φτβηεΒΜή aHrnflpnfl. TeMnepaTypa nnaBneHHH fleneBoronpoflyKTa 232-237 ^ 0. K HeflocraTKaM oriHcaHHoro cnoco6a othochtch HeynpaBnneMocTb TexHonornnec-Koro npoflecca,, ero noBbnneHHan onacHocTb BcneflcTBne BcneHHBaHHH η βο3μομηογοBbiGpoca HarpeToň «170 ° C peaKflnoHHoň Maccbi H3 peaKTopa, nonyneHne npOMewy-TOHHoro npoflyKTa b BHfle TBepfloň πθηη η ηθο6χοαημοοτβ pa3pynieHHH yKasaHHoňneHbl BOfloň (npn 3TOM BO3MO» eH BblĎpoC KHnHmeň BOflbl H pea KflHOHHbIX Γ33ΟΒ H3annapaTa), Hannnne cTaflnn Φηλβτροβηηηη h otmmbkh fleneBoro npoflyKTa ot conen, HeflocTaTOMHO Bbicoxnn Bbixofl. flpyrnM HeflocTaTKOM HBnneTCH arnoMepnpoBaHne fle-neBoro npoflyKTa BcneflcTBne cneKaHnn peaKflnoHHoM Maccbi n HenonHoro ee pa3py-raeHHH npn κηπηηθηηη c βοαοη. KpoMe Tóro, fleneBoň npóflyKT coflepwnT 4-7% boaw.

Uejibio Η3θ6ρετβΗΗΗ HBJíHeTCH ynpomeHn npoflecca, noBbnnnBbixofla n Kane-cTBa fleneBoro npoflyKTa. IIocTaBneHHaH flenb flocTHraeTCH onncbiBaeMbiM cnocoSoM nonyneHHH φτ3ηηΜΗΑ3, KOTopbiřt 3aKJHonaeTCH b that HTO «JrrajiHMHfl noflBepraioT B3anMoneňcTBHK) c-Kap6a MHflOM NPN nx MonbHOM cooTHomeHHH 1: 0.5-0.7 NPN TeMnepaType 95 to 115 ° C n-PO3 ρΗΜβΗΗΗ 0.02 -0.8 aTM c nocneflywmnM HarpeBOM nonyqeHHoň peaKflnoHHoň Maccwflo 150-170 ° C. HHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHHH. c nocneflyromnM HarpeBOM peaKflnoHHonMaccu flo 15O-17O ° C. Πο cnocoOy b CMecnTenb C AET-o6pa3HbiMH jionacTHMH 3arpy «araT φτβηβΒΜή H-mflpnfl n KapBaMHfl b MonbHOM coothoiuehhh 1: 0.5-0.7, npeflnoHTHTejibHo 1: 0.6, repMeTH3HpymT CMecnTenb, οοθαηηηιοτ ero NEP npHMoň xonoflnnbHHK πρηθμηηκpeaKflnoHHoň eoflbí η c BACKGROUND OF THE INVENTION 0.02-0.8 aTM nHarpeeaioT coflepacnMoNnPnEnEnEnEnEnHEnEnCoCoCoBeCoMeCoBeCoBeCoMeTeNToNToRoCoMeTyoNoNToNo. Κθ9φφΗΑΗβΗΤ 3arpy3Kn CMecnTenn πρηηημβιοτ ραβημμ 0,6-0,7. Πρη aocth-χβΗΗΗ B peaKflnoHHo Mac Macce TeMnepaTypbi 95 ° HannHaeTCH nnaBneHne peaKflnoHHoonMaccu, κοτοροβ aaKaHMHBaeTcn npn TeMnepaType 110-115 ° C. Πρη flanbHeňmeM Ha-rpeBe ot 110–115 ** C flo 125-130 ° C nonyneHHbiň nnae pa3naraeTCH c Bbifle-neHneMyrneKncnoro ra3a n o6pa3OBaHneM npoMeacyTOHHMx αμμοηηηημχ coneň φτβηεΒοηKHcnoTbi. B yKa3aHHOM HHTepBane TeMnepa Type npoflecc HfleT 6e3 BbifleneHHH Tennan conpoBoxtflaeTCH Φ33οημμ nepexoflOM: nnae npeepamaeTCH b TBepflbi KpynHOKpnc-TannHHecKHn npóflyKT. Πρη flocTmceHnn TeMnepaTypbi 125-130 HannHaeTCH npoflěcco6pa3OBaHHH ^ TanHMHfla, conpoBoacflaiomHňcH BUfleneHneM Tenjia n peaKflnoHHoň BOflbl.TeMnepaTypa peaKflnoHHoň MACC npn caMonpon3BonbHo BO3pacTaeT flo one hundred meters from 150 to 160 ° C, Sate SucTpo cHnacaeTCH Ha 5-1O ° C. PeaKflnoHHaH Macca b stot μομθητnpeflCTaBJiHeT cyxo Μβηκοκρηετβηηηηεοκηή Φτηηημηα c BKJnofleHneM oTflenbHbixKpynHbix KpncTannoB andMMOHnnHbix conen. Macy noflorpeBaioT flo 150-170 ° 0, bh-flepjKHBaioT npn yKa3aNoM TeMnepaType 10-60 MHHyT flo ποπηογο pa3jio »eHHH 3mmo — HnnHbix conen, oxnastflaioT flo κομηατηοΑ TeMnepaTypu n BurpyxaioT. C bhxoaom 99-100% nonynawT nopoinKoo6pa3Hbn MnkKpncTannnnecKHn o6e3BoaceHHbn npóflyKT, MMetontn TeMnepa nnaBneHHH 234-237 ° C, coRepacamn He 6onee 0.5% khcjimxnpHMeceftj He 6onee 0.5% aMMOHnnHbix conen. ΠρηΜβρ 1. B CMecnTenb Tnna1 ΒερΗβρ-Πφηβήηερβρ eMKoeTbio 1.5 n 3arpyxaioT 444.36. r (3 μοπλ) φτβηβΒΟΓΟ and HrnflpHfla n 90,09 r (1,5 moah) KapGaMHfla (Monbnoe coothohne κομποηθητοβ 1: 0,5). CMecnTenb cHf166H3eT-o6pa3HbiMn nonacTHMH; Ilocne 3arp3KH peareHTOB CMecHTenb repMe-THSHpyioT, ycTaHaBJWBaioT b hcm paspasenne b 0,02-0,1 aTM h npn nepeMeuiHBa-hhh HarpeBaioT CMecb co ckopoctbio 1-3 ° C b MHHyTy. Lime flocrrateHUH TeMnepaTypw95 ° C CMecb naunHaeT nnaBHTbCH, njiaBJieHHe aaKaHHHBaeTCH πρκ TeMnepaType 11Ο-Ι 15 ° C. nonyyeHHbiNjiaB HarpeBaioT no TeMnepaTypw 150 ° C h BbiflepjKHBawT πρκ yKa-saHHoon TeMnepaType. 60 MHHyT. Πο οκοηηηηηη BwnepxKH nonyneHHbi nponyKT npnnepeMemnBaHHH oxjiaxnatoT flo KOMHaTHoň TeMnepaTypw. IIonynaJOT 439.1 r MejiKOKpHCTajijnwecKoro nopomKa, HMeromero TeMnepaTypynnaBneHHH 234-235 ° C. Bbixofl cocTaBnaeT 99.5% ot TeopHH, conepmaHHe BobecTBa - 97%, Kncjibix npHMecene - 0.33%, andMMOHHNHMX conen - 0.41%. ΠρΗΜβρ 2. B CMecHTeJib, HarpeTbien no 60-90 ° C, aarpyacaroT 444,36 r (3 mojih) $ TaneBoroaHrHflpnna h 108,1 r (1,8 mojih) KapGaMHna (MOJibHoe cooTHomeHHe 4> TaneBbi aH-rnfi! Kap6aMna paBHo 1 : 0.6). 95–115 ° C CMecb pacnnaBnneTCH, npnyneHHbiň nnaB HarpeBaioT no160 ° C h BbmepxHBaioT npn s ro TeMnepaType 20-30 MHHyT. Πο οκοηηβηηη BbmepmKHpeaKUHoHHyio Maccy oxnamnaioT npn nepeMeniHBaHHH ro κομηθτηοΗ TeMnepaTypbi h bw-nepxHBawT H3 cMecHTenn. nonywawT 440.4 r MenKOKpHCTaJinHcNoCoNcOn, HMeromero TeMnepaTypynnaBneHHH 236-237 ° C. Bbixon cocTaBJinT 99.8% οτ τθορηη, conepsaHne ochobhotoBemecTBa 97.4%, andMMOHHnHMX conen - 0.15, KHCJiwe. npHMecn OTcyTCTByroT. Π CMΗΜρρ B B B B Bbiň ro B B B B B B B B B B B B C Barpy B,1,1,1,1,1,3,1,1,1 3 moj,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 , repMeTHanpyioT CMecHTejib ,. coanaioT B HeM paspameHne 0.02-0.1 aTM nsMeHBHHHHH HarpeBaioT CMecb co ckopoctbio 1-3 ° C b MHHyTy, npH 95-115 CCMecb pacnjiasnHeTCH, nonyneHHbn nnaB HarpeBaioT no 170 ° C h BbinepxHBaroT npn '3Ton TeMnepaType 10-15 MHHyT . Πο oKoímaHHn Bbinep K KH peaKpHOHHyro Maccy ox-naJsnaioT πρκ nepeMeinHBaHHH ro κομηητηοΗ TeMnepaTypw h BwrpyacaroT. m.p. 439.1 m of MenKOKpHCTannimecrOcOn, HMeromero TeMnepaTypynnaBneHHH 235-236 ° C. Bbixon cocTaBnneT 99.5% στ TeopHH, coftepmaHHe ochobhotro BemecTBa - 97.3%, con ο eň 0.21%, KHCJiwé npHMecn OTcyTCTByroT. ΠρΗΜβρ fourth _____ _ B CMeCHTejIb eMKOCTbIO 50 JI CHaSweHHblň ΠρΗΜΜΜ XOJIOflHJIbHHKOM, NPH -eMHHKOM peaKUHOHHoň Boflbí h coenHHeHHbift Cz BaKyyMHoň cncTeMoň, sarpymaroT22 κγ (0.1485 mojih) ifcTaneBoro aHrHflpHna κγ 5.35 h (0.089 μοπη) KapCaMHfla (μοπϊ BH θ BH BH BH BH BH BH BH BH BH BH BH BH BH BH BH BH BH 0,1 0,1 0,1 0,1 0,1 0,1 0,1 0,1 0,1 0,1 0,1 pe pe pe pe pe pe pe cy cy T T T T ° C. M η asa ň M M M M M M M M M M M -30 -30 -30 -30 -30 -30 -30 -30 -30 -30 -30 pe pe pe pe pe pe pe pe pe pe pe pe -20 -20 -20 -20 -20 -20 -20 -20 -20 -20 -20 -20 -20 -20. TeMnepaTypbi 110-130 ° C npopecc conpoBompaeTCH BwpeneHHeM yrne-KHCJioro rasa. Πρη flocTHmeHHH b peaKHHOHHoň MACC TeMnepaTypw 125-130 CnpexpamaioT nopany TennoHocHTenn b pySaraxy CMecHTenn, TeMnepaTypa peaKijH-ohhoh Maccbi πρκ 3ToM 3a MHHyT noBbímaeTCH ro 15-20% to 155-156 CNET Bwňena-romerocH peaKpHOHHoro Tenna Πρκ TéMnepaType 135-14O C HanHHaeTCH BbifleneHHeBOflbl Η36ΗΤΟΗΗΟΓΟ ΠρΟΤΗΒ ΟΤβΧΗΟΜβΤρΗΗββΚΟΡΟ KOJIHHeCTBa 3ΜΜΗΒΚ3. ΠρΗ flOCTH-ικβΗΗΗ yKaaaHHoft TeMnepaTypw b GHcTeMe ycTaHaBHHBaroT pa3pexeHHe b 0.7-0.8 aTM.BbinenfeomHecn NAPW boaw KOHfleHCHpyroT xonoflHnbHHKe b h b coOHparoT πρπβΜΗΗκ, ra3.oo6pa3Hbie npoflyKTw peaxflHH ynasnHBaioT b BOflHHoň notfymKe. , Πρκ flocTHmeHHHb peáKflHOHHoň TeMnepaTypw 155-156 ° C, b pyCanuty CMecHTena noflaioT τεπηο- 260015

HocHTenb, HarpeBatoT Maccy no 160-165 ° C h Bbinep »HBaioT npn yKa3aHHoBoMeepa-Type 30 MHHyT, Πο OKOHxaHHH BbinepxKH peaKUHOHHyro Maccy oxjiaxnaroT no κομηητ — Them TeMfiepaTypbi h BbirpyxaioT. riojiynaioT 21.9 κγ MenKOKpHCTajuiHnecKoro noponixa, HMeOqero TeMnepaTypynjiaBjieHHH 235.5-237 ° C, conepxamero 97.5 µm and BemecTBa, 0.1% KHCJibixnpuMeceň h 0.42% aMOHOHHbix conen. Bbixon cocTaBJiaeT 99.5% οτ TeopHH. ΠρΗΜβρ 5. * B CMecHTejih eMKocTbio 1.5 ji, HarpeTbien no 60-90 ° C, 3arpyxaioT 444.36 r (3 Mojin) flwajieBoro aHrHnpuna h 108.1 r (.1.8 mojih) KapSaMuna (MOJibHoe coot-HonieHHe $ HbHnpHn: Kap6aMHn paBHo 1: 0.6), repMeTH3npyioT cMecHTenb, yaTaBaIHBaioTb ηθμ pa3pexeHHe 0.8 aTM η npn nepeMeuiHBaHHH HarpeBaroT coCKopqcTbK) 1-3 ° C b MHHyTy. 95-115 ° C CMecb pacnjiaBJiaeTCH. nojiyneHHbnnjiaB HarpeBaroT no 160 ° C h BbinepxHBaroT npn stack TeMnepaType 20 MHHyT. Πο okoh-naHHH BbmepacKH peaKnHOHHyro Maccy oxjiaxnaioT no KOMHaTHoň TeMnepaTypbi h bm-rpyxaroT. HaloHH 2 236-237 ° C, conepxamero 98.1% by weight of BemecTBa, 0.05% khcjimxnpn-Mecen, IIpHMecb andMMOHHnOncTyTCTByeT, Bbixon cocTasnaeT 98.8% rt,

Takhte o6pa3OM, onHCbiBaeMbiň cnoco6 HMeeT PNN npenMymecTB Nepen H3BecTHbiM a) OnucbiBaeMbiň nponecc 3HawHTeJibHo nponje b ηθμ oTcyTCTByioT CTAN ^ n c? NeHnHpOBaHHH peajCIÍHOHHoň MaCCbl B Bone <!> HJIbTpOBaHHH CycneH3HH, npOMbIBKHocanKaj 6) Ilponecc jierKo ynpaBJíaeM HB npoMbinuieHHbix ycnoBHHx μοχθτ 6μτβ ocymecT -BJieH well 3anaHHoň nporpaMMe, Tax xak nponecc coctoht H3 τρεχ nocjienoBaTeiib-Hbix CTannň (nojiynefine ββτθκτηκη, pa3JioxeHHe ββτθκτηκη well aMMOHHňHoň cojih, TepMoo6pa6oTKa cojih well npeBpameHHH φτεηΗΜκη bo ee) Kaxnaa H3 κοτορωχ jihmh-THpyeTCH TOJibKo TeMnepaTypoň peaKnnoHHoň Maccw η μοχθτ 6biTb no xenaHHio 3a-MenJieHa hjih ycKopeHa, Πο HSBecTHoft TexHonorHH nponecc npaKTiwecKH HeynpaBJinM, tbk xax nocjiepacnnaBJieHHH peareHTOB ρββκηκη προτεκβετ oneHb 6ypHo h 3aKaHHHBaeTCH b τε-ΗβΗΗβ HeCKOJIbKHX MHHyT. b) B onncbiBaeMOM cnocoSe OTcyTCTByeT BcneHHBHHHe peaKUHOHHoň Maccbi, hnoBTOMy OH 3HaHHTenbHo 6e3onacHee, neM HSBecTHbiň. Πο toh xe npHHHHe naHHbiňcnoco6 nosBOJiseT yBejnwHTb κοΘφφκηΗβΗΤ 3arpy3KH peaxTopa b 4-4.5 Mr. OTCyTCTBHe ΒΟΠβΗΗΒΗΗΗΗ oSbHCHHeTCH CnOKOňHblM, nOCTanHHHbíM πρΟΤΘΚΗΗΗβΜnponecca »pacTHHyTOCTbio ra30BbinejieHHfl bo speMeHH, OTcyTCTBHeM nonojiHHTenb-Hbnt- TenjioBbineneHHH (TénnoBoro οφφεκτε peaKnHH) NPN nepexone οτ χιιηκοή Sb-K ΤβΚΤΗΚΗ TBepnoň aMMOHHňHoň COJIH. Πο H3BeCTHOŮ TeXHOJIOrHH BCe peaKnHOHHbiera3bi (yrneKHCJibi ra3, napbi Bonn, HenpopearHpoBaBmHn andMMHax) BbinejunoTCH bTeneHHe HecKonbKHX MHHyT. B TeneHHe τβχ xe MHHyT BbinejiHeTCH Bce peaKnHOHHoeTenno, and peaKnHoHHan Macca HaxonTCH h b stot μομθητ b χκηκοΜ, pacnJiaBJíeHHOMBHne. r) Cnoco6 o6ecnenHBaeT noBbnneHHe Bbixona Ha 8-9%, HecKOJibxo 6onee BbicoKyioTeMnepaTypes nnaBJíeHHH, nojiHoe OTcyŤcTBHe bobh.b nenoM nponyKTe. n) flaHHbift cnoco6, b ο η η 3 ot 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 p p p p p p p p p p p p p p p p p p H H H. MacniTaSa peaieropa. OTcyTCTBHe arnoMepaTa o6ecnenHBaeTCH c onwoňCTopoHM, ycjioBHHMH noJiyneHHH nponyKTa (oTcyTCTBHeM TBepnoň, cneKiueňCH πθημ, noJiyneHHeM φτΒΐίΗΜΗηε nepes Mr npoMexyTOHHbix. NponyKTOB) and c ^ npyroň CTopo- HBI, τθμ, ητο Hcnojib3yeMbie B KanecTBe peaKTopa cMecHTenu ηβηςποτοη χοροιπημηnncnepraTopaMH η ωκροκο πρημθηηιοτοη b npoMbnnneHHocTH ρ, ππ pa3MOJa pa3JiHHHbixMaTepHajioB. 260,015 '-5- ΦΟΡΜΥΛΑ Η3ΟΒΡΕΤΕΗΗΛ ϋποςοβ nonyqeHHH Φτ &amp; πημηαβ B3anMoneňcTBneM φτ &amp; πβΒΟΓο anrHflpHfla c KapĎaMH-Flom NPH HarpeBaHHH, oTjnrqaromtoftcH τβΜ, UTOrc uenbio ynponjeHHH nponecca, ποβμ-meHHH Bbrxofla h káMecTBa neneBoró nponyKTa, BsaHMofteftcTBHe φταπβΒΟΓο βηγημρη-Fla c KapOaMHfloM ocyjqecTBnnioT npn mojibhom cooTHomeHHH HáaBaHHWx peareHTOB1: 0.5-0.7, TeMnepaType 95-115 ° C h paapaxeHHH 0.02-0.8 htm, and oCpasyromyiocHpeaKixtfoHHyro Maccy 3βτεΜ HarpeBawT no TCMnepaTypes 150-170 ° C. HCTOUHHKH ΗΗφορΜβίρΐΗ, ΠρΗΗΛΤΜε BO BHHMaHHe NPH 3KCnepTH3e 1. US, A, Η · 3819648th second Οτπετ BHHHXC3P 1977 (MocKBa "ΟκβΒβΗΗε TexHHqecKoň noMonjH npn nycxeΗ 0CB08HHH OCHOBHNX npOH3BOflCTB (npOHSBOffCTBO φτβίΐοφοεε)"), C 70 Ρ Ε II Ε Ρ A Τ CIIOCOB ΠΟΠΥΉΕΗΜΗ ΦΤΑΙΒΜΗΒΑ ΗΒοδρετεΗκε othochtch κ cnocoOy nonyMeHHH φτβπΗΜΗηβ, HcnonbsyeMoro πρκcHHTeae aaMennHTenen noABynKaHHsanmi KayqyxOB. nonyqeHHe φτβπκΜΗηβ ετβηεΒΟΓΟ anrHflpH-6a c KapOaMHflOM, KOTopue Óepyr b MOJibHOM cooTHomeHHH 1: 0,5-0,7, πρκ TeMne-paType 95-115 ° C η paapaxeHHH 0,02-0,8 htm. O6pasy »myioca npn stem peaKUHOHHywMaccy aaTeM HarpeeaioT no 150-170 ° C c nonynetmeM neneBoro nponyKTa c BbixonoM99-100%, HMeniuero TeMnepaNnaBneHHa 234-237 ° C, conepatamero He 6onee0,5% khcjimx npHMeceň h 6e6e 50% 8μμοηηΛηνχ coneft. IIpHSHaHO Η3ο6ρετεΗΗεΜ no peaynbTaTaM 3KcnepTH9N, ocymecTBJíeHHoTocynapcT-BeHHUM ΚοΜΗΤβΤΟΜ CCCP ΠΟ nenM H3o6peTeHHfl H OTKpUTHft. 260015

Claims (1)

DESCRIPTION OF THE INVENTION A process for the preparation of phthalimide by the interaction of phthalanhydride with urea with heating, wherein the reaction of phthalimide with urea is carried out at a molar ratio of said agents of 1: 0.5 to 0.7, a temperature of 95 to 115 ° C and a pressure of 2. the reaction mass is then heated to 150-170 ° C. 260015