CS217440B1 - Method of preparing pentaerythritol - Google Patents

Method of preparing pentaerythritol Download PDF

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Publication number
CS217440B1
CS217440B1 CS840779A CS840779A CS217440B1 CS 217440 B1 CS217440 B1 CS 217440B1 CS 840779 A CS840779 A CS 840779A CS 840779 A CS840779 A CS 840779A CS 217440 B1 CS217440 B1 CS 217440B1
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CS
Czechoslovakia
Prior art keywords
reaction mass
pentaerythritol
npn
mhhyt
carbonate
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CS840779A
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English (en)
Inventor
Valerij M Druzkov
Konstantin Orlov
Alexandr E Obrazcov
Simeon S Sopov
Stojan G Cankov
Michail P Zaprjanov
Christo T Stojmenov
Original Assignee
Valerij M Druzkov
Konstantin Orlov
Alexandr E Obrazcov
Simeon S Sopov
Stojan G Cankov
Michail P Zaprjanov
Christo T Stojmenov
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Application filed by Valerij M Druzkov, Konstantin Orlov, Alexandr E Obrazcov, Simeon S Sopov, Stojan G Cankov, Michail P Zaprjanov, Christo T Stojmenov filed Critical Valerij M Druzkov
Publication of CS217440B1 publication Critical patent/CS217440B1/cs

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  • Silicates, Zeolites, And Molecular Sieves (AREA)
  • Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Heat Treatment Of Steel (AREA)

Description

- 1 - 217 440 0ΠΗ0ΑΗΜΕ H30EPETEHMH K ABTOPCKOMY CBMflETEJIBCTBy3aHBjieHo: 06.12.783aHBKa: 27I4I16/23-04MHK2 C07C3I/24 Αβτορει: ,ξρρκκοΒ B.H., OpjioB K.K., 0ópa3L(OB A.E.,HHocTpaHUři IUonoB Οημθοη CaK,n;eE ,tíaHKOB CtOHH ΓβΟρΓΗΘΒ, 3anpflHOBItaawji Πθτκοβ, Οτομμθηοβ Χρηοτο To^opoB (HPB) 3aHBHTejib: I. HoBOCKÓnpcKHn čtojixaji KeMepoBCKoro HayxiHO-HCCjieflOBaTejihCKoro HHCTHTyTa χημηχιθοκοηnpOMHUUieHHOCTH ΚθΜβρΟΒΟΚΟΓΟ HayqHo-npoH3-ΒΟ,Π,ΟΤΒΘΗΗΟΓΟ OÓEeftHHeHMíI "KapÓOJIWT” 2. MHOCTpaHHOe Πρθ,Π,ΠρΗΗΤΗΘ CTonaHCKKíí XKMMnecKuíí KOMÓHHaT (HPB)
Ha3BaHne κβοόρβτβΗΗπ: CIIOCOB ΠΟΠΥΗΞΗΗΗ ΠΕΗΤΑ3ΡΜΤΡΗΤΑ I43OÓpOT6HH3 OTHOCHTCfl K OÓJiaCTH ΟΟΗΟΒΗΟΓΟ OpraHH-χιθοκογο cnHTe3a, a ημθηηο k yeoBepnieHCTBOBaHHOMy cnoco-óy nojiytieHHH neHTaspHTpHTa. Μ3Βθοτθη cnocoó nojiyxíeHHH neHTaopHTpKTa nyTeM koh-(HSHcaííHH $opMajib1n1eraID;a c aqeTajibfleraflOM npn TeMnepaTypeI5-45°C b npHcyTCTBMH ΓΜβροοκΗΟΗ KajibííHH b KaqecTBeKaTajineaTopa, HeftTpajnt3aiíHH peaK-ψϊθΗΗθΜ Maccti cepHOfókhcjiotoh ao pH 5-5,5, oÓpaÓOTKH nojiyxieHHOft Maccbi cyjib-cbaTOM HaTpHH βο ποληογο ocajmeHHfí ranča, Φμιιβτροβθηηηranča c nocjie,n,yioineíi KpncTajuin3ai;Kefó neHTaspHTpHTa m ne-peKpHCTajiJiK3aijHefi ero H3 ropOTeíi bo^h. Bhxoa ' neHTaepHT-paia 90,7%. [i] .
HeflocTaTKOM cnocoóa nBjíHeTcn ηθβο3ΜΟ3κηοοτβ Bb^ejie-HHfl miCToro qejieBoro npo,nyKTa HenocpeflCTBeHHO H3 peaKu;H-OHHOH MaCChl.
HanóoJiee 6jih3khm no τθχηη^θοκομ cynpocTH κ npejyio-aeHHOMy HBJIH6TCH cnocoó noJiyneHiiH neHTaepnTpHTa nyTeMKOHfleHcaqim (^opMajibňera.n.a c aqeTajib^eraflOM npn TeMnepa-Type I5-50°C b npucyTCTBHH ra,npooKHCH KajibU(Hfl b KaqecT-Be KaTOHeaTopa, oópaÓoTKH peaKnpíOHHOfí Maccu KapóoHaTOM 217 440 - 2 - ΗΗτρκίϊ, $HJibTpaijKH BhinaBiiiero KapóoHaTa k&jibijhh c noc»jieflyw# · oópaÓOTKOM (^osTpaTa 28% Bee. boahhm pacTBo-poM aMMuana h BtmejieHneM qejieBoro npojxyKTa KpncTajuiM3a-
Bhxoa neHTa3piíTpnTa 83%Ha n>opearapoBaBinnií aueTajib-.nerMfl. HncTOTa - 93% β] .
HeflOCTaTKOM cnocoóa πΒΛπβτοπ ηοηοη xaicTOTa qejieBO-ro npo^yím (93%).
Upjibio HsoópeTeHWH áBjííieTcn noBuiuei-ine xíhctotu nejie-βογο npoflyKTa.
IlocTaBJíeHHafi nexb AOCTMraeTCH τθμ, *ιτο b KaqecTBeKapóoHaTa B npoijecce oópaóoTKK peaKipíOHHGM Macchi ncnojib-3yioT óMKapčoHaT βμμοημη h npoaecc BejjyT πρκ CHweHMH τβΜ-nepaTypu peaKiíHOHHOM Mačeta c 45~50°C ao 38-40°C.
Mcriojib30BaHne 3aflBJieHHóro cnocoóa noeBOJifíeT nojty-qHTb neHTaapuTpliT hhctotoíí 99,5%, xíto HjutroeTpnpyeTCHcjieflyromiíMH npHMepaMH. ÍIpHMep I.
Coothoih6hh6 hcxoahmx peareHTOB: aijeTajibAernA: φορ-MajibfternA: γηαροοκηοβ κοβι^ιη: BO^a = 1:5:0,6:80. 3arpy3Ka hcxoahhx peareHTOB: aneTajibAeraA 17% - 260 rĎopMajibAerHA 37% - 406 rH3BecTKOBoe mojioko 10% - 445 rBOfta 100% - 577 rÓHKapóoHaT ημμοηηη 100% - 95 r.PeoM npon,ecca. B peaKTop c μθιποκομ θμκοοτβιο 2,5 ji 3arpy5KajoT(SopMajiMH, H3BecTK0B0e mojioko h BOAy b KOJiímecTBax, yxa-3aHHKX Bifflie. TeMnepaTypa cmsch nocjie sarpy3KH I8°C. 3a-tsm no KaiuiHM, b τβ^θΗζθ 80 MHHyT, npn nepeMenMBaniiHpaBHOMepHo AOóasjííBOT pacueTHoe KOJinxiecTBO pacTBOpa aneT-ajiBAerTO ·
TeMnepaTypa peaKAnoHHofó CMeen b KOHye noAa*ín aijeT-ajibAerufta 38°C. PeaKTop norpyacaioT b BOAHHyio óaHio, b τβ-qeHHe 5 MHHyT aoboa^t TeMnepaTypy b ηθμ a° 45°C h Btmep-«hbsuot npn 3τοϋ TeMnepaType 15 MHHyT. Ilocjie BHAepjKKH 217 440 - 3 - πρπ TeMnepaType 45°0 b peaKTop 3arpy?KaioT 95 r ÓHKapóo-naTa aMMOHHH B cyxoM BHfte. B npoijecce pacTBopeHHn ómcapóoHaTa aMMOHMH h ocajmeHHfí Mejia TeMnepaTypy b peaKTopenoHK?KaioT fto 38°C. nocjie pacTBOpeHHfi ÓHKapÓOHaTa ημμοηηηóepyT npoóy jna nojiHOTy oca^neHHH hohob Kajibn;HH. Corjiac-ho aHajiH3y, ocTaTOUHoe coflepjxaHHe hohob Kajibn,HH 0,15%.Mejl B ΤΘΗΘΗΗΘ 4 MHHyT OT$HJIbTpOBbIBaiOT Ha ΒΟρΟΗΚΘ ΒίΟΧΗβ-pa m nojiynaioT npo3panHbiw ÓeciíBeTHUíí KOH.n.OHcaijjHOHHbiH pa-CTBop. PacTBop ynapHBaioT npn TeMnepaType 55°C ,no idiot-hocth 1,24 γ/cm . ynapeHHyío Maccy KpHCTajijiH3yio.T b Tene-ηηθ 8 nacoB c θοτθοτβθηηκμ oxjiajKfleHHeM ,π,ο 25°C. riojiynenHyio cycneH3Hio (^HJibTpyioT Ha BopoHKe BioxHepa, οο^π,οκ HaφΗΛΒτρβ npoMbiBaioT AByMíi πορμΗΗΜΗ βο,π,βι c TeMnepaTypoříI0°C no 50 mji h OflHOM nopqHeíí 5%-ηογο pacTBopa MypaBbH-Hofó khcjioth-50 mji. riocjie cyuiKH nojiynaioT 115 r neHTa-apHTpHTa c TeMnepaTypon πήββλθηηη 2I0-2I5°C h 30JibH0-CTbio 0,12%. Bbixop, neHTaspHTpHTa B pacneTe Ha aijeTajib-ΛβΓΗ,π, 85%, nncTOTa iipo^yícTa 99,5%. IIpHMep 2.
CooTHomeHne peareHTOB: aqeTajibflerKp,: (JopMajibflerufl:Γκ,π,ροοκΗΟΒ KajibqHH: BOjja = 1:5:0,6:70. 3arpy3Ka ηοχο,π,ηβιχ peareHTOB: aiieTajibflerHfl 18% - 245 r $opMajibflerafl 37% - 406 r H3BecTKOBoe mojioko 10% - 445 r BO,n,a 100% - 412 r ÓHKapóoHaT βμμοηηη 100% - 95 r.
PeMM npoi^ecca. B peaKTop, οπηοθηηηη b npKMep I, 3arpyjKaioT $opMa-jihh, Η3ΒθοτκοΒοβ mojioko h Bopy. TeMnepaTypa cMecn noc-jie 3arpy3KH I5°C. 3aTeM no KanjinM,B Texienne 60 MHHyT,floóaBjínioT pacTB.op an;eTajib,n,erHfla. TeMnepaTypa peaKi^HOH-·hoíí CMecH b κοΗηβ noflatiH aiíeTajibflerHfla 40°C. PeaKTopnorpyjKaioT b BOflnHyio óslhio h b TeneHne 5 MHHyT ,π,οβο,π,ητTeMnepaTypy b ηθμ ,π,ο 50°C. PeaKtjHOHHyio CMecb BUftepo- 217 440 - 4 - bčwt πρκ θτομ TeMnepaType 15 MHHyT η 3aTeM 3orpy3KaioT95 r ÓHKapóoHaTa θμμοημη. Hocjie pacTBopeHUH ÓHKapÓOHa-Ta aMMOHHH h ocas,neHMH Měna TeMnepaTypy b peaKTope no-HHjKaioT βο 40°C. OcTaTonnoe co^epscaHiie hohob Kajiti^HH0,14%. Ποοηθ ΒΗ,π,βπβΗΗΗ neHTaopHTpHTa πρκβΜβΜΗ, ormcaH-HbiMH b npHMepe I, nojiynaioT 117 r npoflyKTa' c TeMnepaTy-pofi ΐυΐΒΒΛΘΗΗΗ 215-220°C M 30JIbH0CTbK) 0,15%. Bhxo# ΠΘΗ-TaopHTpHTa b pacneTe Ha arjeTajibflerHjj, 86%, xjMCTOTa npo-flyKTa 99,5%. 217 440 - 5 -
OWiA H30EPETEW
Cnocoó nojiyqeHHH neHTaapuTpuTa πγτθΜ KOH^eHcatíMMφορΜβΛΒ^θΓΗ^ c at(eTajibAern1noM npn TeMnepaType I5-50°CB npHCyTCTBHH ΓΜ,ςρΟΟΚΚΟΗ KHJIblJKJI B KaneCTBe KaTajIH3a-Topa c nocjaeAyiomeři oÓpaóOTKofó peaKijKOHHoří Maccu Kapóo-HaTaMM, OTJiwqaioiHHMCfí τθμ, *ito, c ijejibiQποΒΜΠβΗΗΗ wctoth i^ejieBoro npoAyKTa, b KauecTBe KapÓO-HaTa Hcnojib3yK)T ÓHKapóoHaT aMMOHHa n npoijecc BejiyT npnCHKjKeHHH TewnepaTypbi peaKijHOHHOÍí Maccti c 45-50°C pfi38-40°C.
McTOUHMKM HH$OpMaqHH, ΠρΗΗΛΤΗΘ BO BHMMaHWe ΠρΗ3KcnepTH3e: 1. ΑΒτοροκοθ CBMfleTejibCTBO CCCP JT° 585149,kji.C07C 31/24, saflBJí.'11.03.74. 2. IlaTeHT Ηποηηη # 16013, mi.I6B 424, onyÓJiHK.1962 (προτοτΜπ). - 6 - 217 440
AHHOTAHO Μ300ρβΤΘΗΗΘ 0TH0CHTCH K OÓJiaCTIÍ ΟΟΗΟΒΗΟΓΟ opraHH-xiecKoro CHHTesa, a ημθηηο k ycoBepineHCTBOBaHKio cnocoóanojiyuěHMH neHTaapMTpMTa. líejlb Η300ρθΤΘΗΜίϊ - yBSJIHXÍOHHS ΟΤΘΠΘΗΗ Βί^ΘΛθΗΗΗHeJiesoro npopjyKTa h yjiymueHne ero KaqecTBa.
Cnocoó BKJiiOTiaeT KOH^éHcaííHio aijeTajibflerafla e φορ-ΜΒΉΒ,ΓΙ,ΘΓΜ,Π,ΟΜ B npHCyTCTBHK KaTajIK3aT0pa - ΓΜΛΡΟΟΚΜΟΗKajIbqHH, ΒΒξΣξθΛΘΗΜΘ HOHa KajIbU^ÍH B ΒΚβθ OCaflKa, φHJIbTpa-φίΐο ocaflKa ot KQHfleHcaqiíOHHoro pacTBopa κ βεαθλθηηθneHTaspuTpHTa μ3Βθοτηημμ np^eMaMH. Hobhm b cnocoóe hb-jineTCfl BbmejieHne nona Kajihutun oópaóoTKOfó KOH.n.eHcaqHOH-Η0Γ0 pacTBopa ÓHKapÓOHaTOM aMMOHHH.. OópaóoTKy npoH3BO,nHT npn pH, paBHOM 6,5-7, u npnnoHWKeHHH TeMiiepaTypu KOH^eHcaLíHOHHoro pacTBopa c45-50°C ao 38-40°C.

Claims (1)

  1. 217 440 PŘEDMĚT VYNÁLEZU Způsob výroby pentaerytritu kondenzací formaldehydu sacetaldehydem při teplotě 15 až 50 °C v přítomnosti hy-droxidu vápenatého jako katalyzátoru s následujícímzpracováním reakční hmoty uhličitany, vyznačující setím, že za účelem zvýšení čistoty požadovaného produktuse jako uhličitan použije hydrogen uhličitan amonný apostup se provádí při snižování teploty reakční hmotyz 45 až 50 °C na 38 až 40 °C. Uznáno vynálezem na základě výsledků expertizy, provede·né Státním výborem pro vynálezy a objevy SSSR,Moskva,SU Vytiskly Moravské tiskařské závody,provoz 12, Leninova 21, Olomouc Cena: 2,40 Kčs
CS840779A 1978-12-06 1979-12-04 Method of preparing pentaerythritol CS217440B1 (en)

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Application Number Priority Date Filing Date Title
SU782714116A SU807608A1 (ru) 1978-12-06 1978-12-06 Способ получени пентаэритрита

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CS217440B1 true CS217440B1 (en) 1983-01-28

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CS840779A CS217440B1 (en) 1978-12-06 1979-12-04 Method of preparing pentaerythritol

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CS (1) CS217440B1 (cs)
DD (1) DD156478A3 (cs)
SU (1) SU807608A1 (cs)

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SU807608A1 (ru) 1991-09-07
DD156478A3 (de) 1982-09-01

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