SCIENTIFIC ABSTRACT MYSHLYAYEVA, L. V. - MYSKA, L.

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CIA-RDP86-00513R001135820016-4
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December 31, 1967
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SCIENTIFIC ABSTRACT
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S/02 63/148/004/020/025 B144YB101 AUTHORS: Kreshkov, A. P., Myshlyayeva, L. V., Soboleva, D. A. TITLE: Synthesis of tris-(triphenyl-ailoxy) aluminum and tetra- (triphenyl-siloxy) sodium polyalumoxane PERIODICAL: Akademiya nauk SSSR. Doklady, v. 148, no. 4, 1963, 843-645 TEXT: Monomeric trio-(triphenyl-ailoxy) aluminum (I) was economically synthesized for the first time from 0.02 M triphenyl-ethoxy silane (II) and 11 g sodium aluminate solution (III): (C 6H5 3 Sioc2H5 + H20 ---90 (C 6H5)3Sioff + C2K OR; 3(C 6H )3SiOH + NaA 102 --4v (C6H 5)3Si0j 3A1 + NaOH 5 5 0 + H20. A mixture of II obtained by distillation in vacuo at 196-201 C and reprecipitation with petrol ether, along with III containing 19.2% Al2 03 and ~0-3% Na 20, was stirred for 40 min without heating and then for 4.5 hre at 50-6000. 1 forming at the surface of the mixture as a white solid substafice was separated. The yield was 35% (related to II) Card 1/3 I S'/020J/63//14,9/004,!n~"1!,_)2 2 Synthesis of tris-(triphenyl-ailoxy) B140101 and I - 2 (related to the molar Si:Al ratio). I is a nonmelting powder, soluble in diethyl ether and benzene and resiatant to alkalies and heat. The product recovered in the filter after extraction of I contained 12-59~~ S1021 17-96% Al 0"7.68'1','~ Na 0, 46-34% C and 5.20% 11. This yielde(i the (C ff ) formula 1 6 5 33'0~ 2A1 0 (A1-0 J5 A 11( C6H5)3 Si 01 2 '18H20 for Uria tetra-(triphenyl-ailoxy) sodium polyalumoxane (IV), a white powder insoluble in organic solvents and stable to alkalies; yield 55 - 60',A. The new substances were subjected to thermal, spectral and x-ray aniilyses. The thermogram of I revealed 3 exothermic effects corresponding to a 7subsequent.splitting-off of the triphenyl-ailoxy groups at 500, ()00, and 7000C. This is confirmed by the thermogram of IV which shows two exothormic effects due to the 2 triphenyl-ailoxy groups bound to Al and .1 endothermic effect produced by_dehydration. The IR spectra indicatel an absorption maximum at 1065 cm I characteristic of the SiOA1 .-roup an-] further maitima at 700, 740, 997, 1123, 1432, and 1596 cm-1which are indicative of phenylated silanes and siloxanes. X-ray analysis showed that I and IV have crystal-line structure. There are 2 fi.gures. -.'-trd 2/3 S/020/63/148/004/020/025 Synthesis of tris-(triphenyl-ailoxy) ... B144/B101 ASSOCIATION- Moskovskiy khimiko-tekhnologicheakiy institut im. D.I. Mendeleyeva (Moscow Institute of Chemical Technology imeni D.I. Mendeleyev) PRESENTED: July 2, 1962, by A.N. Nesmeyanov, Academician SUBMITTED: June 10, 1962 Card 3/3 400238209 no AP4009839 8/019VA/000/001/0065/0067 AUTHORSs Xreshkovo APo; My*shlyayeva, L,V,; Krasnoshchekov, V.,Ve TITZEs Kethods of silicon 6ie'rmination in silico-organic com- pounds and a comparative evaluation of these methods SOURCE: Plasticheskiye massy*, no. I., 3.964p 65-67 TOPIC TAGS: substituted silanes, polyltiloxanes, silicone rubber, oxysilanes, silicon determination, analytical chemistrv LBSTWT; Because the recommended method of silicon determination VY fusion in a bomb is not always expedient,, the authors investigated and proposed other methods of Si determination in silico-organic compounds (BOO): most precise, but time consuming, is wet oxydation by a mixture of oleum and fuming nitric acid In quartz flasks with subsequent Si-determination by gravimetric and volumetric methods* SOO wddation in a platinw, oricible with the same acids is less precise than in a quartz flask but the volumetric tests Is faster, Card 1/2 :ACOZSSIOX NR: AP4009839 A fast method Is based on the oxidation of 500 by a mixture of sul- furic and chromic acid in a stream of oxygen but it cannot be used with volatile substanceso Si-determination by fusing In bomb with sodium peroxide corrodes the bomb and contaminates the substances Some improvements, which give greater analytical accuracy, consist in oxidizing In open crucibles cooled In liquid air and in the use of sodium fluoride Instead of ammonium fluoride In acidimet'ric titration. The use of nickel or Or-NI bombs instead of steel is recommended to avoid contaminations About 40 mono- and polymer SOO were analyzed by the authors using the most appropriate of the above methods and the resul-I '6s are consolidated in tables,. The methods are explained and described In details Origo art& has no figurest 3 foz%mlas, 4 tables. ASSOCIATION: None SUBMUTTED: 00 DATE AGQ: 1OPeb64 MM: 00 SUB CODE: OH NO REP SOV: 010 OTMMt OOT Card 2/2 KRESHKOV, A.P.; WSHLYAYEV .,L,Yl GENSHAFT, Yu.S.; KRASNOS'HCHEKOV, V.V. - Interaction of silicohydrofluoric acid with benzidine. Zhur.neorg.khijr,. 9 nc.1-183-186 Ja 164. (MIRA 17:2) MYSHLYAYEVA L.V.- MIKHArLENKO, Yu.Ta.; KRASNOSHCHEKOV, V.V.; KUCHKAREV, Ye.A. -::,---,-,-"~-~.r~llz.r.-~----.,,~~-, 9 Rapid method of determining chlorine in alkvl(aryl)chlorosilanes. Trudy MKHTI no.44il39-IV 164. (MIRA 1811) M,YSHLYAYFIA, L.V., KRA-SNO-SHCHEKOV.. V.V.-, SHATUNOVA, T,G,-, SEDCVA, I.V, Determination of tron. '-n farrio-,ene anti I-tq cr;~anos:licon derivatives. Zuv. lab. 30 no.S.-944 164. (FIRA !P:3')' 1. Moskov5k-'y khlm!ko-tekhnol.cgicheskiy institut iment Mendelpyeva. L 38118-66 &1T(m)/EWP(J)/FNP(t)/F.T1 IJP(c) JD/RM ACC NR' ha AP6014141 (A) SOURCE CODE: UR/0075/65/020/012/1325/1329 Kreshkov. A. P.; Myeblyayeva, L. V.; Kuchkarev, Ye, A.; To Go ORG: Moacow Chomico-technological Institute im, Do I* MendeleMv (Moscovski'y kbimiko-tekhnologiabaskiy insti-t-u-t-T- TITLE: Quantitative determination of titan'tum~7n titanium-orgarilc and titanium-silicon-organic compounds : Zhurnal analiticheskoy khimii,, v. 20,, no. 12,, 19659 1325-1329 TOPIC TAGS: quantitative analysis,, titanium, titanium compound, silicon compound ABSTRACT: The article describes two methods for the determination of titanium, a titration (complexometric) and a spectroscopic method. In the titration method, a weighed portion of the compound to be analyzedg containing 10-15 Mg of titanium, is introduced Into 5-7 M1 of concentrated sulfuric acid, The mixture Is heated for 10-15 minutes up to the evolution of H2301L vapors. The solution Is cooled to 90-1000 and complete mineralization i5f the weighed portion is carried out with ammonium persulfate. The solution is cooled and 30 ml of water are UDC: 543.7C-:q43-80 - ')01.18-66 ACC NRI AP6014141 carefully added and the solution is boiled for 5-10 min to decompose the ammonium persulfate. The silicle acid is filtered off and the silicon is determined by weighing in the form Of S102. Final titration of the titanium in the filtrate is done with a 0,05 M solution of ZnS%. The relative error of the method does not exceed 2.5%. In the spec rosco Ic method, the titanium is determined in the form of tetrabutoaxti-anillT- and silicon In the form of tetraoi silan I In this methods the standard relative error in the determination is 2.2% for titanium and V1. for silicon. Comparative results by the two methods are shown in tabular form. According to the article, the spectroscopic method 13 to be !preferred in practice, since no preliminary mineralization 1.8 required, !Or'-'g. art, has: 2 figures and 2 tables, !SUB CODE: 07/ SUBM DATE: 28Nov64/ ORIG REFt OJO/ OTH REF-. 002 qH - 2- f I ormu MISHLYAYE;VA, L.V.; SOBOLEVA, D.A. Synthesis of poly (triplienylsiloxyalumoxydiphenylsUoxane). Zhvr. prikl. khim. 38 no.5:1170-1171 My 165. (MIRA 18: 11) ~AP601~9449 ~~~ SO~URCE~CODE-~URIO~303/661000/003/0060/0062 AUTHOR: Kreshkov, A. P.; Shatunova, T. G.; Myshlyffeva, L. V.; Kuchkarev, Ye. A. ORG: none TITLE: Accelerated methods for determining aluminum and silicon in organic compounds containing aluminum and silicon SOURCE: Lakokrasochnyye materialy i ikh primeneniye, no. 3, 1966, 60-62 TOPIC TAGS: 4A_.iiW7W_C';W C0M,'*V1 461 ewe'"'eZ 'n r Rr rc t, V b$ spoitt 0,6141-red&# ABSTRACT: Current methods for determining Al and Si in Al- and Si-containing organic compounds (ASOC) require complete mineralization of such compounds and are time-consuming. The authors have developed two accelerated methods for determining these elements in ASOC. The first method is the determination of altminum by titra- tion involving complex ion formation. The -'-'--Si-0