CS217410B1 - Method of preparing organic tin mercapto compounds - Google Patents

Abstract

Organo-tin mercapto cpds. are made by reaction of (A) organo-tin chlorides of formula (YCH2CH2)nSnCl4-n, (in which Y is CN, CONH2 of COOH; n is 1 or 2), and (B) chloro cpds. of formula YCH2CH2Cl. (B) is obtd. by reaction of metallic tin and/or tin chlorides with excess acrylonitrile and HCl. The prod. before or after reaction with alkali sulphides, is subjected to hydrolysis and esterification in presence of alcohols of formula ROH and/or R'(OH)m, (in which R is opt. substd. 1-18C alkyl, Aralkyl or cycloalkyl; R' is 2-6C alkylene; m is 2-6) and acids. The cpds. are stabilisers for chlorine-contg. polymers, e.g. PVC. Higher yields are obtd. by a more economic process which reduces formation of by-products, gives stabilisers of higher efficiency, and avoids use of inert organic solvents.

Description

- 1 - 217 410 HA3BAHHE H30EPETEHM3

Cnocoó nOJiyneHIÍH OJIOBOOpraHHHeCKHX ΜβρΚΗΠΤΟΟΟβ «ΜΗβΗΗΐ1

OKJIACTL ΠΡΚΜΕΗΕΗΜΗ M30EPETEHHH Μ3Ο0ρβΤΘΗΗβ OTHOCHTCH K CnOCOÓy nOJiyHeHHH OJIOBOOpraHHHeCKHXMepKanTocoeflHHeHHft peaxmiefi opraHHHecKHX xjioph «ob OJiOBa cCyJILQ) H« AMH meJIOHHUX MeTajUIOB H OpraHHHeCKHMH ΟΟβ «ΗΗβΗΗΗΜΗxjiopa. Προ «γκτΗ peaKipiH npe« CTaBJimoT coóoíi npeawe Bcero bhcoko-φφθΚΤΗΒΗΗβ CTad «JIH3aT0pH« JIH XJIOpOCO «ep) KaiItHX nOJIHMepOB»

TaKiix, KaK ΠΒΧ. XAPAKTRPHCTHKA H3BRCTHUX TEXřWÍECKMX PHUEHMfl nojiyneHne ojiOBOopraHHHecKHX, MepKanTOcoe «HHeHHft rivet peawmopraHHHecKHX xjioph« ob OJiOBa c cy "B $ K« aMituieaoHHHX hjih njejiOHHO-36MejILHHX MSTaJIJIOB H OpraHHHeCKHMH ΟΟΘ «ΗΗβΗΗΗΜΗ XJIOpa yne« aB-HO H3BeCTHO.

TaK onncaHiHiHKHxHkHQaT B3anMO «eficTBHe ojioBoopraHHHecKHx τηοηβτρηθβηχ coe« H-h6hhíí otímít <$ opMyjm rr Sn (s; 7a) 2, KOTopne nojiyneHU peaKimeň; 1 MOJI RR * SnO H 2 MOJIíí Iía2S B BO «HOM paCTBOpe B npHCyTCT“ bhh HeóojiBUMX kojihrqctb ciuipTa h nocjiejiyiomefí HeiiTpajin3aiíHeft 2 MOJIHMH KHCJIOTH, C ΟρΓΗΗΗΗΘΟΚΗΜΗ ΟΟΘ «ΗΗθΗΗΗΜΗ XJIOpa. B COOT-; BeŤCTBywix npHMepax b c cbh3h sthm oimcaHH β3ηημο «θΑοτβηηOJIOBO« HÓyTHJI- OHC (THOHaTpHH) C ÓyTHJIXJlOpH «OM 3THJieH« HÓp0MH «0M," O "eiJHJIÓpOMH« OM STHJIÓpOMaijeTaTOM, óeH30HJIXJI0pH «0M Η 0βΗ3Ο-XJIOpH« OM , lime 3TOM, Ο «ΗΗΚΟ, OTCyTCTByiOT ΒΟΗΚΗβ« Ó OÓ yCJIO- bhhx peaKipin, β, ηηοτοτθ h cBoficTBax προ ^ γκτοΒ peaKiinS. β AHaJIOrUHHUfi cnocoó nOJiyneHHH OIIHCaH ΟΠΗΟΒΗΗΗ Η300ρβΤθΗΗΗ KnaTeHTy BejiHKoópHTaHHH I 175 466. PeaKipiefi opraHHHecKHX Raji-Remi «on 0B« both hjih cyjiL $ H "OB OJiOBa cyjn c> n $« mejioHHHX hjdí AMN - 2 - The 217,410 meJIOHHO3eMeJILHHX ΜβΤβΛΠΟΒ, ΠρβΛΠΟΉΤϋΤβΛΒΗββ Β ΟΜβΙΠΒΗΗΗΧ pACT-ΒΟρΜΤθΛΗΧ (BOfla, ΤβΤρΒΓΗΛΡΟ ^ ρβΗ, Η30Πρ0ΠβΗ0Λ Η) IlOJiy-HAWT MeTajuíMHecKue cojih ojiOBOopraHircecKHX τηοοτβηηβτοβ, κό-tops HaXOflHTCH B paBHOBeCHH OJIOBOAHOpraHHHeCKHM CyJIB C $ HflOM.ΠγτθΜ Budopa pacTBopHTejiefl her ποβηγηθηκη KOJureecTBa 3arpyxaeMorocy.HB $ Mfla mejioHHoro HJM mejionHO3eMejiBHoro MeTaoa paBHOBecneCMemaeTCH b CTopoHy τηοοτβηηβτβ. SBTS 3τοτ τηοοτβηηβτ OT-BejmeTCfl m xe DE3 otjicjighjíh NOx AETC peaicmiB IIa-c coejpiHG HHHMH XJIOpa B TOM ΉΗΟΛβ C θφΗρΒΜΗ XJIOpKapdOHOBOfi KHCJIOTH.Cocjbíhchhc xjiopa pa3daBJiHeTca pacTBopHTejieM b KanecTBe co-Topór npejwoHHTaeTCH TetP-rnjípo $ ypaH. 3HaBeHHe pacTBopuTejieftOÓBHCHfleTCH ΤβΜ, HTO, B 3aBHCHM0CTH OT 3ΛθΚΤρθφΗΛΒΗΟΓΟΧαρ3Κ-Tepa opraHHHecKoro οοθεηηθηηη xjiopa, HMeromnecH cyjiB $ nflHne hohhpearapyioT HescejiaTejiBHHM odpa3OM h cnocodCTByioT odpa30BaHjnoHOdOHHHX npOjayKTOB. Β 3TOM ΟΤΗΟΠΙΘΗΗΗ KaK ΤΗΠΗΉΗΗβ ynOMHHaiOTCH3 $ HpH XJIOpKaptíOHOBOii KHCJIOTH, ΚΟΤΟρΗβ C Hpyroft CTOPOHH, cpejmnepeHHCJieHHux b npHMepax opraHMHecKHX coejiHHeHHíi xjiopa OCO-amino deHHO oTHoiuemiio κ deH30oxjiopiwyt hbjddotch Handojiee npn TOflHHMH HCXOJCHHMH ΒΘΙΙΙΘΟΤΒΒΜΗ «SOUTH ΠΟΤψΗΘΗΗΗ ΒΗΟΟΚΟδφφθΚΤΗΒΗΗΧcTaÓHjiH3aTopoB jcjih ΠΒΧ Ha ocHOBe ojioBoopraHHHecKHX coeAHHeHHft.B 3T0ÍÍ CBH3JÍ Π ΟΛΗΟΜ ΠρΗΜθρβ H3 ΗΟΓΟΑΗΟΓΟ paCTBOpa Na2S H JCH-óyTMJiojioBoxjiopHAa nojiyneH cyjiBtpiijc jmdyrajioJioBa, H3 κοτοροΓΟBojtoft BHMtiBaioT xjiophjih. IIocJie 3Toro cyjiB $ nfl jcndyrajioJioBa pea-rapyeT β J OJ c n n n n OC OC OC OC ο OC OC OC OC OC OC OC OC OC OC OC IlocJie peaKiíHH θτοϋ cycneH3HH C H3O-OKTHJixjiopaiíeTaTOMojioBa, $ h OBTpaiíHH yjcajieHna Tojiyojia h HenpopearapoBaBniero co ejlHHeHHH Xjiopa nonyneH JCHdyTHJI0JI0B0-dHC (H300KTHJITHOrJIHK0JIHT) C BHX0JC0M 88 5 B .npyroM npuMepe K3 MOHodyTHJipjioBOTpHXJiopHjia b H3onponaHOJieβ ΒΟΛΗΟΜ pacTBope Ka2s nojiyaeH TKOCTaHHaT, κοτορώί de3npejíEapHTejiBHoro βηχθλθηηη B3aHM0jceKcTByeT c H3O-OKTHJixjiopaije-TaTOM. Ilocjie sKCTpaKUHH peaKHHOHHóň cMecn χΛοροφορΜΟΜ h jiodaB-jiemM TeTparzj] after $ ypaHa jyia ο0λθγηθηηβ cyuiKH de3B0jCHHM Na2Sh nocjie yjtajieHHH neperoHKoíi H3 peaKiíHOHHoS cmcch Scex jierno- 217410 JI These HHX COO &amp; BHHX ΗΒΟΤβΚ ΠΟΛγΗββΤΟΗ Μ0Η00γΤΜΛ0Λ0Β0 "ΤρΐΙ0 (Η30-ΟΚΤΜΛΤΗΟΓΛϋΚΟΛΗΤ) C ΒΗΧΟβΟΜ 94 , 4

BuiueHa3BaHnue cnocodu nojiyHeHHH ojioBoopraHHHecKHX Μβρκβπτο-coejwHeHHÍt cBH3aHH oAHaKO c uejiHM ρηλομ HeaocTaTKOB, κοτορΗθBtipaJKaJOTCH JDldO B UeJIOM B BHCOKHX MaTepHaJIBHO-ΤβΧΗΗΗβΟΚΗΧΗ ΘΚΟΗΟΜΗΗβΟΚΗΧ 3βΤρΒΤβΧ, CBH3aHHHX C ΗβγΛΟΒΛβΤΒΟρΗΤβΛΒΗΗΜΟΒβΜΟΜ npOflyKUHH C eAHHHUH OtífcěMa B eAHHimy ΒρβΜβΗΗ, JDldO, escape XE AonoJiHJiTejiBHO b dojiee ujdi MeHee HeyAOBJíeTBopHTejn »- HHX, KaK C TOHKH 3ρ ΗΗΗ CTaÓHJDI3HpyK) IUerO fleftCTBHH, TBK HC TOHKH 3ρβΗΗΗ OdJiaCTH ΠρΗΜβΗβΗΗΗ, IIOKa3aTeJIHX no ποτρβ-dHTeJIBCKHM CBOnCTBaM.

BaJKHOii ΠρΜΗΗΗΟϋ BHU16Ha3BaHHlIX npHHIIHIIHaJIBHHX ΗβΑΟΟΤβΤΚΟΒΗβοοΜΗβΗΗο HBJíHeTCH HexejiaTejiBHaH peaKima cyjiB $ H £ HHX hohoba, HaxoAHiunxcH b paBHOBecHH ÉOHaMH THocTaHHaTa c, c-oópasoBa ΗΗβΜ Memaioiímx ΠΟ0ΟΉΗΗΧ npOíyKTOB, KOTOpaH HBHO 3aBHCHT OT3JieKTp0 $ HJIBH0r0 XapaKTepa ΠρΗΜβΗΗβΜΟΓΟ OpraHHHeCKOrO COeOT-ηθηιιη xjiopa. linden BHÓope doJiee 3JieKTpo $ HJiBHoro οοβΑΗΗβΗΗΧxjiopa, TAKORA, κβκ HanpHMep, xjiopncToro deH30HJia, pa3MepnodOHHHX peaKimit C SKOHOMHHeCKOĚ TOHKH 3peHHH HBJíHeTCH eměnpHeMJieMHM, XOTH nOJiyMeHHHÍi NPH 3TOM C.TadHJDI3aTOp ΒΡΗΛ JDIy ^ oBJíeTBopneT TpedoBaHHHM riepepadoTHHKOB. Ecjm XE πρηηη-MaeTCH peuiemie b nojn »3y yAoÉJieTBopHTejiBHoro KanecTBa npoH3-BOAHMHX 3 $ npOB XJIOpKapdOHOBOft KHCJIOTH, TO CKJIOHHOCTB to drive off 30BaHHK) nodOHHHX npOAyKTOB TaK BhipaxeHa, ΗΤΟ ΟΟΟΤΒβΤΟΤΒβΗΗΗβnpHHHwaeMHe προτκΒ 3Toro map, KaK πρΗΜβΗβΗΗβ cMeiuaHHoropaCTB0pHT6JIH, H3dHTOK CyJIB $ HAOB meJIOHHHX H meJIOHHO3eMeJIBHNXMeTajuiOB HHHXH BHCOKHyBCTBHTejiB — HHX K B03, nyxy H CJIOXHHX B ΠρΗΜβΗβΗΗΗ MeTajIJIHHeCKHX cojiefiOJIOBOOpraHKHeCKHX THOCTaHHaTOB, CTaBHT H3B6CTHHe cnocodHC 3KOHOMHHeCKOft ΤΟΗΚΗ 3ρβΗΗΗ ΠΟΑ ΒΟΠρΟΟ.

OcodeHHO πρΗΜβΗθΗΗβ opraHHHecKHX ΗΗβρτΗΗΧ pacTBopTHejieli ϊnpeAnoHTjrrejiBHO TeTparnApo $ ypaHa b cbh3h c θτημ 0Ka3HBaeTcýinecTBeHHoe BjniHHHe Ha 3kohomhhhoctb cnocoda nojiyneHUH, nocKOJiBKy H3 3Toro BHTeKaeT He tojibko cjioxHan, AoporocToamaHh sHeproěMKaa TexHOjioran c KpyroodopoŤaMH pacTBOpHTejiH · - 4-217 410 ycTaHOBKaMH &amp; TIH ero οτλθλθηιιη h peKynepano , βκλκηηη 3aTpaTH, CBH3aHHH6 C TpcdOBaHHHMH ΠΟ ΤβΧΗΗΚθ όθ30Πβ0Η00ΤΗ, HO Η npOO-jieMH, cBH3aHnue c oxpanoft Tpyna η 3Λοροββη, bcigtcbhc ηλο-bhtocth thiojiBUMHCTBa pacTBopHTejieii.

Kpowe Toro oiuícaHHHe cnocodH οηθηβ ογρβηηηθηη c tohkh 3peHHHHX ΠρίΤΜΘΗβΗΗΗ, nOCKOJIBKy ΚΟΜΠΟΗβΗΤ ΟρΓΒΗΗΉβΟΚΟΓΟ OJIOBa, CΟΛΗΟϋ CTOPOHH, OrpaHHHeH TOJIBKO npHHHTHMH B TOprOBJíe M6TMJI-, tíyTHJI- H OKTHJI- ΟΟβ, φΙΗβΗΚΗΜΗ OJIOBa H, C "Pyro CTOpOHH, Ηβ-B03M0JKH0 nOJiyHHTB Πρ0Η3Β0ΛΗΗβ OT flHOJIOB HJIH IIOJIHOJIOB ΠρΗ Ha3-BaHHHX yCJIOBHHX peaKIJHH H3-3a HX HyBCTBHTeJILHOCTH ΠΟ OTHO-ΙΙΙβΗΗΚ) K rHJipOJIH3y.

um M30EPETEHMH

UejiLio H30ÓpeTeriHH ηβληθίόη ycTpaHeHHe hjih xe 3HaHHTejiBHoeyM6HBIlieHH6 BHTeKaiOIilHX H3 ypOBHH pa3BHTHH ΤΘΧΗΗΚΗ Ηβ, ΚΟΟΤΗΤΚΟΒ, κοτορκθ B03HHKaioT npeame Bcero cbh3h b c odpa3OBaHHeM no-dOHHHX ΠρΟίΟΓΚί / οΒ HJIH JS.Q ΟΟΟΤΒβΤΟΤΒΘΗΗΟ C ^ ΓΜβΗΒΙΙΙΘΗΗβΜ ΠΟ HX-CpeJICTBOM OTAeJIBHOrO npOH3BOJICTBa ΚΟΜΠΟΗβΗΤΟΒ peaKimH B CBfl- 3H C HeodXOflHMHM H3dHTKOM ΗβΟρΓΗΗΗΉβΟΚΗΧ cyjIB $ HflOB H OCOdeH-HO B CBH3H C ΠρΗΜβΗβΗΗβΜ ΟΜβΙΠΒΗΗΗΧ paCTBOpHTeJieíi. B CBH3H C3THM JIOJDKHa dHTB npHHUHIIHajIBHO HCKJHOHOHa B03M0JKH0CTB 0dpa30-BaHHH MeuiaioiHHX nodoHHHX npojiyKTOB, Tax, HTodu cjioman, noporo-CToamaH h 3HeproěMKaa TexHOJiorna ajih λοοτηχθηηη yAOBJíeTBopHTejiB-ΗΟΓΟ CBEMA npOJiyKUHH C β, ΠΗΗΗΠΗ OdBěMa B eSHHHIiy ΒρβΜβΗΗ ΗβnoTpedoBajiacB, DH.

JlajiBHeiíiijafl nejiB nsodpeTemía coctoht b tom, HTodn nojiyHHTBI nponyKTH peaKiw TaKoro KanecTBa, HTodH ohh mobjih npn- ΜβΗβΗΗβ AJIH CTadHJIH3anHH ΒΗΟΟΚΟΚΗΉβΟΤΒβΗΗΗΧφορΜΟΒΗΗΗΗΧ Ma-TepnajiOB H3 ΠΒΧ. BudopoM πρΗΜβΗΗβΜΗΧ κομποηθητοβ peaKUHH cno- 1 cod ^ frosted odecneHHTB BapBnpyeMoe nojiyneHne coeflHHeHHfi coΟΠΘΙίΗφΗΉβΟΚΗΜΗ nOTpedHT6JIBCKHMH nOKa3aTeJLHMH.

K3JI0KEHHE CWOCTH M30BPETEHMH

B COOTBeTCTBHH C NOCTaBJíeHHOfi: the best B OCHOB H3OdpeTeHHH 217 410

JieJKHT 3a ^ ana rivet H3MeHeHHH HCXOAHUX ΚΟΜΠΟΗβΗΤΟΒ H ΧΜΜΗΗβΟΚΟ - TexHOJionnecKoro npouecca b HanpaBJíeHHH ynpomeHHH ycjiOBH®peaKUHM, HaaěJKHHM h npocTUM rivet nojiymiTB ojioBOopraHHHecKHeMcpKanTocoejmHeHJiH c bhcokhm cbSmom npoíyKUHH c ejwHHUH ODT Ema B eflHHHHy ΒρβΜΘΗΗ H ΠρΗ ΒΗΓΟΑΗΗΧ MHTepHaJIBHO-BKOHOMHHeC · "khx her snepreTKHecKHX ycJiOBHHX.

Jfeuiee ctoht 3anana, πρπ πρΗΜβΗβΗΗΗ προοτο npoH3BoaiiMHX HC-XOflHHX ΚΟΜΠΟΗβΗΤΟΒ, paCIUHpHTB OdJiaCTB ΠρΗΜβΗβΗΗΗ 9Τ0Γ0 0Π0 coda-h odecnemiTB BapBupyeMoe nojiynemie CTadmiH3aTopoB HBX, κοτορκβ yAOBJíeTBopHJM du BCCM TpedoBamiHM £ ajiBHe®iueit NEP-padoTKH.

CorjiacHo H3otípeTemno, ojiOBOopraHHnecKHe ΜβρκπβτοοοβΠΗΗβΗΗΗnojiynaioT τβκπΜ odpa3OM, HTO ojioBooprammecKne xjiopmm odme®ftopMyJEH (YCH2CH2) nSnCl4_n, ΓΛθ ΠρββΟΤΗΒΛΗβΤ rpyímu Y-ON, -0 (0) NH2 H / hjth -COOH H opraHHHecKHe coejtHHeHHHxjiopa odlije® $ oprzyjm ych2ch2C1, rjje Y ημθθτ BimieHa3BaHHoe3HaneHiie, no ^ BepraioT, di di j j ea ea ea $ $ $ $ ID ID ID ID ID ID ID ID ID ID ID ID ID ID ID T T T

OjioBooprammecKHe xjiopujm h oprararcecKue coejDiHeHHH xjiopanojiynaioT uejiecoodpa3Hmz rivet B3aHMOj (e®cTBHeM MeTajunraecKoroOJIOBa h / hJIH XJIOpHJJOB OJIOBa aKpHJfflHTpHJIOM C-H XJIOpHCTHM ΒΟΛΟ POJJOM B KOJDIHeCTBaX BfcClie ΟΤΘΧΗΟΜθΤρΗΗβΟΚΗΧ, ΠρΗΉβΜ Ha-3KBH BajieHT metered KOJinnecTBa OJIOBa jjaioT ot 2 jo 5 npejuioHTHTejiBHee4, SKBHBajieHTa aKpmiHHTpHJia h ot 2 jj 8, npefljioHTHTejiBHeeOT 4 AO 5, 3KBHBajieHT0B XJ10pHCTOrO BOf10pOfla, B naCTHOCTH COJI-HHO® KHCJIOTH.

CorjiacHo H30ópeTemno, πριίΜβκΗΐοτ npejmouTHTejiBHO ojioBooprami- .necKHe xjioph.hu odme® ftopMyjiu (IICCH2CH2) SnCl4 n OTjjejiBHOhjih ΒΜβοτβ c jjpyrnMH ojioBoopramrqecKHMH XJiopHjjaMH odlije® φορ-wyjiu (Ycn2CH2) nSnCi4_n, R &amp; e ^ Y NPE cTaBJífleT rpyímu -C (O) nh2η / HJIH -COOH, C n = I Π Π = 2 B ΒβΟΟΒΗΧ OTHOUieHHHX I: 99ΛΟ99: I, hb KanecTBe opranz ^ ecKoro eoejjHHeHHH xnopa npejj-noHTHTejieH xjiopnpomioHHTpHJi. B $ xanecTBe cyjiB exmples ujejioHHHx MeTajuioB npHMemnoT cyjiB $ HRH ηβτρηη - 6-217 410 npejmowTMTejiBHo b bojíhom pacTBope, npuneM xaiOT Ha θκβοβλθητojioBOopraHHHecKoro xnopHaa λο rpm 0.8 1.8 η ηη 3Κβηββλ6ητ opraHHHecKoro coeAWHeHHH xjiopa rpm 0.3 0.8 λο , npexnonraTejiLHee0,5, 3KBHBaJieHT0B ογΛΒφΗΛβ mejioHHoro MeTajuia. B icawecTBe cnnpTOB 0Ka3ajracL uejiecoo <5pa3HHMH ojmoaTOMHiie cimpth oómefl $ opwyjní ROH, R 'e R npejiCTaBJíHeT 3aMemeHHHii bTiaHHOM cJiynae 0η-018-η- ujdi -H30-ajiKHJiHHft, apajnouinHíi ujdimíKJioajnuiJiHHift ocTaTOK h / hjih nojmojM oómelt <opMyjM £ r (οπ) ώΓΛβ R npejíCTaBJIHeT JDTHeiÍHHft UJDI pa3B6TBJieHHHÍi aJIKHJieHOBilitocTaTOK wt -hhcjio rt ro 2 6 πρηήθμ Ha sKBHBajieHT ojiobo-opraHHHecKoro xjiopnxa hjih opramrcecKoro οοθακηθηκη xjiopa npn μθηηθτοη no KpaíiHeíi Mepe no I 3KBHBajieHTy cimpTa ROH h / hjihVm R (OH) m, it npejDioHTHTejiBHee h3Óhtok, κοτορπβ nocjie peaK-iDm b cooTBeTCTByiomeM cjiynae Jierao μοηθτ óhtb yjiajieH. M3óhtokcnnpTa mojkho η οοτββητβ b peaKunoHHofí CMecn, nocKOJu »Ky OH bφορΜθ jíJfflHHOnenHHX ajiKaHOJioB ujdi noJMOJiOB oTnacra OKa3HpaeTfla ^ e noJiojKHTejiLHoe B03fleficTBne KHK cTaÓHJDi3aTop ηη ποτρθ-ÓHTejiLCKHe cBoňcTBa.

HeoóxojDiMaH JWH OMHjiHDmeii 3Tepn $ nKawra KHCJioTa npexcTaBjmeTcoóofí MUHepajiBHyio kucjioty, npejuionTHTejiBHee cojiHHyw, cepHyioHJDI $ OC $ OpHyiO KHCJIOTy, KOTOpyiO ΠρΗΜΘΗΗΙΟΤ B KOJIHHeČTBS OT0,5 λο 2.5 3KBHBajieHT0B to 3KBHBajieHT ojioBOopraHHnecKoroXJiopnjia η rt ro 0.5 1.5 npejuioHTHTejiLHee I sKBHBajieHT Ha3KBHBajieHT opraHuneoKoro οοθακηθηκη xjiopa.

PeaKinOnOneCoWe3HoPrBeBHHTepBajie TeMnepaToO0 0 0 I00 ° C. B CBH3H C 3THM 0Ka3aJI0CL n0JIG3HHM HPOBOXHTB BceCTyneHH peaKiw go nacTL nx b bohhoh cpene.

IIPBCT OGyiHECTBJIEHHH K30EPETEHKH I. 247.5 JDL Γ (lDiaH03THJl) 0JI0BOJDIXJI0pHJia, 44.0 M0H0IÍHaH03THJI Γ-ojioBOTpuxjiopiifla 353 h r xjiopnponnoHHTpiiJia, κοτορκθ nojiy-ηθηη NPN peaKinni 118.7 r noponiKooópa3Horo ojiOBa raKpmiHiiTpHJia C 212 H 480 R κοΗηθΗτρηροΒΒΗΗοΜ cojihhoS khcjioth, pacTBopmoT b 450 r óyTaHOJia h npn nepeMeuiHBaHHH ποοτεπθΗΗοnpjíóaBjDDOT 272 r cepHofi khcjioth npn KOMHarao # TeMnepaType. - 7 - 217 410 Ποοαθ θτογο, peaKmioHHyio ομθοβ b τθηθηηθ 2 nacoBnoAorpeBa-wt £ 0 TCMnepaTypu 90 - 100 ° C. Ποοαθ οχλβλαθηηη οτφΗΑΒτρο-BUBaeTCH oópa3OBaBiiuíitcH cyjiB $ aT βμμοηηη. Φηαβτρθτ oxjiax-Αθίοτ and 5 ° C nocą Nero πρκ AaaBHeítiiieM οχλθχαθηηη ποοτθπθη-ho npnóaBJíHJOT pacTBop 156 R $ cyjiL Hjia ΗθτρΗΗ b IOOOma boah.Ποοαθ 3Toro TeMnepaTypy ποαηημθιοτ and κομηβτηοΚ h cHOBa2 NACA nepeMemiiBaiOT, nocą Nero peaKinno b τθήθηηθ I nacanpn 50C aoboaht o KOHija. Ποοαθ οκοηηθηηη nponecca nepe-MeuiHBamíH AaioT peaKUHOHHofl ομθοη ρθθαθαητβοη ria ophHhec-Kyw κ BOAHy »φθ3Η. BoAHyw $ a3y oTÓpacHBaioT, and opraHmecKyionpoMHBaioT 500 μα boah. ΠοοΑβ ποβτορηογο ρθ3Α6αθηηη caogbH3 opraHHHecKolt φθ3Η yAajiflDT neperoHKož ποα BaKyyMOM H3ÓH-TOHHLíft óyTaHOA. TIojiynaioT 665 r $ $ ατογο, ορθβηητθλβηο ηη3Κοβη3Κογο Maca, htocooTBeTCTByeT BHxoAy 94.5% ot τθορθτηηοοοοο (b pacneTeHa noTpeÓAHeMoe oaobo).

OaoBoopraHHHQCKoe μθρ ^ πτοοοθαηηθηηθ οοΑβροτ: 16,4 $ Sn (no 16,9 $) 9,5 # S (no 9.8% ").

20.8 Kaptí0KCH3THA0A0B0TpHXJI0pHAa second Γ, Γ aMHHOKapdOKCH 7,8-3THA0A0B0TpHXA0pHAa 23 XJIOpnponJÍOHOBOň KHCAOTH Γ H 8,7 ΓaMHAa xaopnponnoHOBofí khcaoth, κοτορπθ noayHeHH πρκ Pean-iíhh 22.6 r SnCl2 · 2 H20 C 21.2 h 67 r aKpujiHHTpujia , 2 rΚΟΗΠΘΗΤρΗρΟΒΗΗΗΟίί COAHHOÍt KHCAOTH, B3aHMOAeÍÍCTByiOT c 20 ΓH3OAeKHAOBoro οππρτθ. 3Ty ομθοβ oxAasmaiOT and I0 ° C, nocaenero ποοτθπβΗΗΟ npHóaBAHMT pacTBop 31,2 r cyAB $ HAa τθτρκπb 200 ma boah. Π ρ 30 30 30 30 30 30 30 30. noAorpeBaeTCH and TeMnepaTypn 60 ° C. Ποοαθ οκοηήθηηηnponecca nepeMeuiHBaHHH ομθοβ ρθθαθαηθτοη Ha opraHHHecKyioη BOAHyio $ a3H. H 3 BA i H H H H H H H H H H H H H r r r r r r r r r r r r r r r r ,7 ,7 ,7 ,7 ,7 ,7 ,7 ,7 ,7 ,7 ,7 ,7 ,7 ,7 ,7 ,7 ,7 ,7 ,7 ,7 ,7 ,7 ,7 ,7 ,7 ,7 Iμθοβ β τθηθηηθ I naca noAorpeBaioT cOÓpaTHHM XOAOAHABHHKOM, ΠΟΟΑΘ 3ΤΟΓΟ ΠΟΑ BaKyyMOM ΟΤΓΟΗΗΙΟΤ ΑΘΓΚΟΑΘΤ3ΓΉΗΘ COCTaBHHe HaCTH AO TeMHepaTypH JKHAKOCTHI00 ° C. - 8 - 217 410 ΠοοΛβ φϋΛίτρΗΐξΐίπ nojiynaioT 63,8 r ^ ejiTosaTO-Kopn ^ HeBoro, ΒΗ3Κ0Γ0 MacJia, οοοτΒθτοτΒγβτ BHXojjy 89,3% οτ τβο-peTHHecKoro (p Ha Ha e Ha NoTpeÓjweMHlt Sn012).

OjroBoopraHJiHecKoe MepKanTocoejuiHeHHe cojiepjKHT: 16.7% Sn (no more than 16.6%) 13.3% s (no more than 13.4%). Third npn IIojiyHeHHaH B3aHM0ji, efícTBHH nopouiKooópa3HoroojioBa 59.4 r 106 r 240 r h aKpmiHHTpHJia KOHneHTpnpoBaHHoit cojin-Hor khcjioth peaKimoHHaH CMEC cocTOHman 100.9 H3 r-unaHO STHJIJIOJIBOXJIOpHfla, Γ aMHH0KapÓ0KCH3THJI0JI0B0XJI0pHJia 31.4, 16.3 r KapÓoKCH3THJiojiOBOXJiopHfla (98% oJioBojmopraHHHecKHXcoej (HHeHiHiHHiHi) h 30,4 rXJiopnponwoHHTpHJia, 10,5 r aivMjia xjiopnponHouqBoft khcjioth h 5.3 r xjiopnpoiiHoiiOBofi khcjioth, nojiBepraiOT peaKinm c 112,5 r

1,4-oxo-5-hydroxy-oxime is 5 ° C. Π ο n j i i i i i i i i B B j j 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 Hocjie οκοηήβηκη jioÓaBJíeHHH eiqě nepeMeuiHBaiOT I nac πρΗ κομηητηο15 TeMnepaType h 2 naca npn TeMnepaType50 ° C. PeaKijHOHHyio cmccl cHOBa oxJiaswaioT η ποοτθπβΗΗο jio-óaBJIHIOT 192 Γ KOHIjeHTpHpOBaHHOfi cojihhoíí khcjioth, nocjienero 2 naca κηπητητ c oóparaHM xojiojjhjibhhkom.

Ilocjie oKOHiaHHH nponecca nepeMeuiHBaHHH peaKimoHHaH cmccbpa3nejnieTCH Ha 2 $ a3H. ΡΪ3 ra ec ec ň ň ň a a a a ň ň ň ň ň ň ň a a a a ie ie ie ie ie ie ie ie ie ie ie Ba Ba Ba Ba (BaKyyMOM.

Ilocjie SuJiLTpaijHH nojiynaioT 292.5 r βη3κογο xejiTOBaTO-κορΗΉ-ΗΘΒΟΓΟ MaCJia, ΉΤΟ COOTBOTCTByCT BHXOJiy 93.2% οτ TeopeTH-necKoro (b pacneTe Ha noTpeójweMoe ojiobo).

OjiOBOoprarareecKoe MepKanTocoejuiHeHHe cojiepsHT: .θ.θ% Sn (no longer 18.9%) 9.8 # s (no 10.2%). - 9 - 217410 ΦΟΡΜΑ Μ30ΕΡΕΤΕΗΗΗ first Cnocoó nojiyneHHH ojiOBOopraHHnecKHX MepKanTocoeEKHeHHft, npn MeHHeMtix npejiMyiuecTBeHHO flJifl CTaÓHJM3aiDiH xjiopocoflepjicamHXnOJIHMepOB, B3aHMO ^ elÍCTBHeM OJIOBOOpraHHHeCKHX XJIOpHflOB cΟΥΛΒφΗΛΒΜΗ meJIOHHUX MGTaJUIOB H OpraHHHGCKHMH ΟΟβΕΗΗβΗΗΗΜΗXJIOpa, OTJMHaiOUPlitCH ΤθΜ, HTO OJIOBOOpraHHHeCKHe ΧΛΟΡΗΑΗOÓmeH roopMyJDJ (YCH2CH2) nSnCl4-N (Y -ON, -C (O) HH 2, -COOH, η = I go n = 2 H i 1 CM 6 CH coesHHHHHit c η = I hn = 2) h oprHHHecKHe coeDraeHHH xjiopa omemeitφορι / iyjni YCHgGHgGl (γ ΗΜθθτ BNiiieHa3BaHHoe 3HaHeHHe), nojiynaeMne npn B3aHMO #eitcTBHH MeTajunnecKoro ojiOBa H / C hjihXJIOpHJXOB OJIOBa npeBHUiaiOmHMH ΟΤθΧΟΜθΤρΗΗθΟΚΗθ ΚΟΛΗΉβΟΤ-bhmh aKpwjiHJiTpííJia h xjiopucToro Bo-curtain πρημθηηιοτοη bKanecTBe peaKUHOHHHX κομποηθητοβ, κοτορυθ HJM λο ηλη nocJiepeaKnnH c ,, ^ cyjiL HflaMH mejioHHnx MeTajuioB b πρκογτοτΒΗΗ ο κ ix-H H H H H H H H H H H H H H H H H H H H H H H H H H H H 30 30 30 30 30 30 30 30 30 30 30 30 30 30 30 30 30 30 30 r '= o2 -o &amp; - JIHHEĚHHItT HJIH pa3BeTBJI6HHHit aJIKHJieHOBhrfi οοτβτοκ; m - OT2 £ 0 6), H KHCJIOT nOffBepra »T OMHJIHKJmeft 3ΤθρΗφΗΚΒΙξΗΗ.

Second Cnocoó no nyHKTy I oTJMHaiomHiicH τθΜ, HTO npejnioHTHTejiLHOnpHMCHJKOTCH OJIOBOOpraHHHeCKHe XJIOpHjm OÓmefl φορίφΗ (N0CH2CH2) nSnCl4_n OTfleJILHO HJDI ΒΜθΟΤβ CJ ^ pyTHMH OJIOBO-OpraKHHeCKHMH XJIOpHAai4H OÓmeĚ $ OpMyjIH (YCH2CH2) nSnCl4 Q-C n H 2 n ot b BecoBHX οτηοιιιθηηηχ I: 99 and o99:! · 3. Cnocoó no nyHKTaM I h 2, oTjmnaioiUHitcH τθΜ, hto b KanecTBeopraHHnecKoro οοθαηηθηηη xjiopa npejmoHTHTejiLHO ηρκΜθΗΗθτθΗXJIOpnponHOHHTpHJI.

Fourth Cnocoó well nyHKTaM 1-3 OTjiHHaiomHfiCH τθΜ, HTO cyjit ^ HAmejioHHoro MeTajma b ηθοτηοοτη cyjn> $ HFL ηβτρηη, npennoHTHTejn> -HQ ΠρΗΜθΗΗθΤΟΗ B B0JÍH0M paCTBOpe, ΠρΗΗθΜ Ha 3KBHBaJieHT - ΙΟ - 217410 OJioBOQprararcecKoro xJiopHRa jxaioT οτ 0.8 at 1.8 µl βκβηββ-jieHT ra HHHecKoro coeHHeHHH xjiopa 0,30.3 ro 0.8, npeR-noHTMTejiBHee 0.5, 3KBHBajieHT0B cyju ^ Ra mejoHHoro MeTaJuia. Fifth Cnocoó well nyHKTaM 1-4 OTJnnaioimiítcH τθμ, HTO-Ha θκβηββ jieHT ojioBoopraHHHecKoro XJiopHRa h opramnecKoro οοθαηηθηηηxjiopa óepeTca no μθηβιιιθΑ Mepe No I 3KBHBajieHTy crnipTa ROH JI / hJDÍ 1 / tn of R (OH) m, Πρβ ξΠΟ ^ ^ ΤΗΤβ / ΙΒΗθβ ORHaKO H3ÓHTOKcnnpTa, οτοριώ b οοοτβθτοτβτοτοιιιθμ cjiynae yRajiaeTca nocjieOKOHHaHHH peaKIBÍH.

Sixth Cnocoó well nyHKTaM 1-5 OTJMHaioRHiicH τθμ, HTO npuMeHneMaH RJIH OMNJIHXJmeft 3TepH $ HKaiIHH KHCJIOTa HBJIHeTCH MHHepaJILHOfíKHCJiOTOít, npejmoHTHTejiLHee cojihhoíí, cepHofi ra φοοφόρΗοβKHCHOTOÍÍ, ΠρΗΗΘΜ Ha SKBHBajieHT OJIOBOOpraHHHeCKOrO XJIOpa οτ # 0 0.5 2.5 Ha SKBHBajieHT opraHHHecKoro coeRHHeHHHxjiopa RaioT οτ 0.5 ro 1.5, npeRnoHTHTejiBHee I, βκβηβητιθητηKHCJIOTH. 7. Cnocoó no nyHKTaM 1-6, OTJiHHaiomHficH τθμ, hto Bce CTyneHHpeaKIíHH HJIH HaCTB HX ηρΟΤΘΚΘΙΟΤ B BORHOft cpefle. 8. Cnocoó no nyHKTaM I'- 7, oTJMHaiomHííCH τèμ, hto peaKiw npeRnoHTHTejiLHO βθτογτοη b HHTepBajie TewmepaTyp οτ 0 ro I00 ° C. 9. Cnocoó no nyHKaTM 1-3, oTJiHHaioiyHiicH τθμ, hto Ha skbh-BajieHT oómero κοηηηθοτββ ojioBa RaeTCH οτ 2 ro 5, npejyion-THTejiLHee 4, SKBHBajieHTa aKpnjiHHTpHJia η οτ 2 ro 8, npeRnon-T OT 4 RO 5 , BHaCTHOCTH COJIHHOS KHCJIOTH. 217,410-11

AHHOTAIW M30ÓpGTGHHG OTHOCHTCH K ClIOCOÓy ΠΟΛ ^ ΉβΗΗΗ OJIOBOOpraHHHGCKHXMcpKanTocoejvíHeHHÍi, πρημθηηχηχης npeuMymecTBeííHO ejih οτη0ηλη-3anHH xjiopocoaepjKamnx ποπημθροβ. IIocTaHOBKa ugjih h reaching h3oópgtghhh 3aKjnoHaeTCH b that HTO-OH ^ M3MGHGHHGM HCXO HHX ΚΟΜΠΟΗβΗΤΟΒ Η ΧΗΜΗΚΟ-ΤβΧΗΟΛΟΓΗΗβΟΚΟΓΟnpouecca ycTpaHHTB ηλη mg 3HaHHTGHi> H0 υμθηβιιιητβ npHcymneypoBHio tgxhhkh HenocTaTKH, κοτορκβ BHTeKaxJT b HacraocTH H3Meuiawíx nodoHHHX peaKiinít h retrieves H3 ηθλοοτητοπηογο KanecTBanpouyKTa.

CorjiacHO Η3θόρβτβΗΗ », ojioBOopraHHHGCKHG MepKanTocoejmHeHHHMoryT óhtb NOx yneHH τβΧΗΟΛΟΓΗΗβοκπ προοτΗΜ h ηβαθχηημ cno-COO- πρκ BHCOKOM CBGMG ΠρΟίζ / ΚφίΗ C β, φΙΗΗΠΗ oótGMa b ejniHunyΒρθΜΘΗΗ Η πρκ ΒΗΓΟβΗΝΧ MaTepHaJILHO ~ 3KOHOMHHGCKHX yCJIOBHHX, ecjiH b khhgctbg κομποηθητοβ peanymi nofflBepraeMHx hjih, π, ο, ηληnOCJie peaKLIHH C CyjU ^ HJiaMH meJIOHHHX MGTHJIJIOB B npHCyTCTBHHCnupTOB H KHCJIOT ΟΜΗΛΗΙΟΙΙΙβίί ΘΤβρΗφΗΚΗΙξΗΗ, npHMGHHIOTCH OHOBO-OpraHHHGCKHS XJIOpHEH OOUGUGIT & OpMyjIH (YCH2CH2) nSnCl4-n

(Y = -CN, -C (O): th 2, -COOH} η = X ηλη n = 2 hjih mgCMGCH COGJIJIHGHHII, B KOTOpHX η = I H n = 2) H OpraHHHGCKHGCOGJUIHGHHH XJIOpa OOIUGIt $ OpMyJIH

YCH2CH2CX (s MMGGT BHUieHa3BaHHOe 3ΗβΗ6ΗΗβ) ΠΟΛγΉβΗΗΗβ ΠρΗ Β38ΗΜ0-AefícTBHH MGTajuniHGCKoro ojiosa h / c hjih xjiopuflOB ojioBa npGBMiia-101UHMH CTGXHOMGTpHHGCKHG KOJDTCGCTBaMH aKpHJIHHTpHJia H XJIOpHCTOIOBosopojia.

Claims (9)

OBJECT OF THE INVENTION 217 4io A process for the production of organic mercapto compounds useful in particular for stabilizing chlorine-containing polymers, by reacting organic tin chlorides with alkali metal sulfides and inorganic chlorine compounds, characterized in that the organic tin compounds of the formula (YCH 2 CH 2) nSnCl 2, where Y is -CN, -C (O) NH2, -COOH, n is equal to 1 or 2, or mixtures of compounds of the general formula wherein n = lan = 2, and organic chlorine compounds of the general formula ych2ch2ci wherein Y is as defined above, ) prepared by reacting metal tin and / or chlorides with acrylonitrile in an amount higher than stoichiometric and hydrogen chloride, forming reactants which either before or after the reaction of the sulfidyalkali metals are in the presence of alcohols of the general formula ROHa / or R 1 (OH) m, wherein R represents a substituted ΟΟ^, θ-η- or anisoalkyl, aralkyl or cycloalkyl radical, R'denotes 6666ffffvenývenývený branched alkylene, m it has a value of from 2 to 6, and the acids undergo saponification esterification. 2. Process according to claim 1, characterized in that the organotin chlorides of the general formula (NCCH3C1) nSnCl4 are used separately or with other organic chlorides of the general formula (YC1CH3N2Cl2, where n = lan = 2 in weight ratio 1). : 99 to 99: 1 · 3. The process according to claim 1, wherein chloropropionitrile is used as the organic chlorine compound. 4. A process according to any one of claims 1 to 3, wherein the alkali metal sulfide, in particular sodium sulfide, is used in an aqueous solution wherein from 0.8 to 1.8 and the organic equivalent is used per equivalent of organic tin chloride. chlorine compounds of from 0.3 to 0.8, preferably 0.5 to equivalents of alkali metal sulfide. SUMMARY OF THE INVENTION No. 2 - 13 217 410 5. A process according to any one of claims 1 to 4, wherein at least 1 equivalent of an alcohol of general formula ROH and / or 1 / m R * (OH) m, preferably an excess of alcohol, is used in equivalents of the organic tin chloride and the organic chlorine compound. which is optionally removed after the reaction is complete. 6. A process as claimed in claim 1, wherein the acid used for the saponification esterification is a mineral acid, preferably hydrochloric, sulfuric or phosphoric acid, using from 0.5 to 2.5 equivalents of the organic chlorinated tin compound. per equivalent of chlorine organic compound from 0.5 to 1.5, preferably 1, equivalent of acid. 7. A process according to any one of claims 1 to 6, characterized in that all or part of the steps are carried out in an aqueous medium. 8. The process according to claim 1, wherein the reaction is carried out at temperatures from 0 to 100 ° C. 9. A process as claimed in claim 1, wherein the equivalent amount of tin is from 2 to 5, preferably 4, equivalents of acrylonitrile and from 2 to 8, preferably from 4 to 5 equivalents of hydrogen chloride, in particular acid. hydrochloric acid. Recognized by the invention on the basis of the results of an expert review by the Office of Invention and Patenting, Berlin, DD.