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    Organomercaptomethyl silicon compounds and production thereof
    1.
    发明授权
    Organomercaptomethyl silicon compounds and production thereof 失效
    有机巯基甲基硅化合物及其制备

    公开(公告)号：US3350437A

    公开(公告)日：1967-10-31

    申请号：US32987563

    申请日：1963-12-11

    Applicant: BAYER AG

    Inventor： WALTER SIMMLER ,  HANS NIEDERPRUM ,  HEINZ JONAS

    IPC: C07F7/08 ,  C08G18/61 ,  C08G77/00 ,  C08G77/392

    CPC classification number: C08G77/00 ,  C07F7/0856 ,  C07F7/0889 ,  C08G18/61 ,  C08G77/392 ,  C10M2227/04 ,  C10M2229/053 ,  C10N2220/02

    Abstract: Organo-mercaptomethylsiloxanes are prepared by reacting a chloromethyl- or bromethyl siloxane comprising Cl- or units, any remaining units being , wherein n is 1-3, R is an inertly substituted or unsubstituted alkyl or aryl radical, and m is 1 or 2, with an alkylmercaptan, a mono- or poly-hydroxylated alkylmercaptan, a mercaptocarboxylic acid or a thiophenol in the presence of an alkanol having 1-4 carbon atoms, as solvent, and at least a stoichiometric amount of an alkali metal hydroxide or tertiary amine. Typical examples describe the preparation of (2) a polysiloxane of formula wherein a + b + c = 21, from the corresponding tris(bromomethyl)- siloxane and thiophenol; and (8) 1,3 - di - (b - hydroxy - ethyl - mercaptomethyl) - 1,1,3,3 - tetramethyl disiloxane. Many other examples are given.

    Organosiloxy methyl alkanes
    4.
    发明授权
    Organosiloxy methyl alkanes 失效
    有机甲硅烷氧基甲烷

    公开(公告)号：US3040080A

    公开(公告)日：1962-06-19

    申请号：US7511360

    申请日：1960-12-12

    Applicant: BAYER AG

    Inventor： HORST KOPNICK ,  DETLEF DELFS ,  WALTER SIMMLER

    IPC: A61K8/894 ,  A61Q19/00 ,  C07F7/08 ,  C08G77/00 ,  C08G77/14 ,  C08G77/42 ,  C08G77/46

    CPC classification number: C08G77/46 ,  A61K8/894 ,  A61Q19/00 ,  C07F7/0834 ,  C07F7/0852 ,  C07F7/0859 ,  C07F7/0885 ,  C07F7/0889 ,  C08G77/00

    Abstract: Organosilicon compounds of the general formula: wherein R is an alkyl radical of 1 to 4 C atoms, each R1 and R11 are H atoms or alkyl radicals of 1 to 4 C atoms, n is 3 or 4, x is an integer greater than 3 and y is an integer greater than 2, may be made by heating to between 50 DEG and 300 DEG C. a polyalkylene glycol monoalkyl ether of the formula R-(-O.CH2.CHR1)x-OH, a dialkoxy dimethylpolysiloxane of the formula: R111O-(-Si(CH3)2-O-)y-R111, wherein R111 is a lower alkyl radical, and a polyol of one of the formulae: wherein z is zero or an integer, in the presence of an acid catalyst in amount of at least 0.05% by weight of the reactants, driving off the alcohol R111OH formed during the reaction, and recovering the reaction product after neutralising the catalyst. The process can be effected in one step, or advantageously in two steps by first reacting the siloxane with the alkoxylated polyol or the glycol ether, in the presence of a catalyst (preferably a fluorinated fatty acid), then further transesterifying the product by refluxing with the glycol ether or the polyol (respectively) in the presence of an acid catalyst. In a typical example (1), a mixture of toluene, 1,2-bis-(b -hydroxypropoxy)-ethane, a , o -diethoxy-dime-thylpolysiloxane, mono-n-butyl ether of polypropylene glycol and trifluoroacetic acid, was refluxed until homogeneous, whilst the ethanol formed and some toluene were distilled off; the mixture was then neutralised with b -hydroxyethylamine, freed of solvent and filtered to yield an oily product of 1, 2-bis-[b -(n-butoxy-poly-propoxy-dimethylpolysiloxy)-propoxy] ethane. The compounds, similar to those of the parent Specification, are hydrophilic and of use in cosmetic preparations and as emulsifying agents.

    Trialkylsiloxanes and their production
    5.
    发明授权
    Trialkylsiloxanes and their production 失效
    三烷基硅氧烷及其生产

    公开(公告)号：US3012052A

    公开(公告)日：1961-12-05

    申请号：US75412758

    申请日：1958-08-11

    Applicant: BAYER AG

    Inventor： WALTER SIMMLER

    IPC: A61K8/58 ,  A61K8/891 ,  A61K47/24 ,  C07F7/08 ,  C08G77/00 ,  C08G77/06 ,  C08K5/00 ,  C09K5/02 ,  C09K5/08 ,  G01K5/12

    CPC classification number: G01K5/12 ,  A61K47/24 ,  C07F7/0849 ,  C07F7/0874 ,  C08G77/00 ,  C08G77/06 ,  C08K5/0008 ,  C09K5/02 ,  C09K5/08 ,  C08L83/04

    Abstract: 884,807. Siloxane compositions. FARBENFABRIKEN BAYER A.G. July 17, 1959 [July 26, 1958], No. 24707/59. Class 2(7) A composition comprises a siloxane of the formula wherein R is a hydrocarbon radical of at least 2 C atoms and n is an integer from 1 to 10, and a liquid, pasty or waxy, organic compound, e.g. alcohols with a low water content such as methanol, ethanol, isopropanol, butanol, 2-ethylhexanol and amyl, cetyl, lauryl and stearyl alcohols; benzine, benzene, toluene, beeswax, mineral oil, ceresine, paraffin and petroleum; oleic and stearic acids; butyl-acetate, -oleate and -stearate, glycerol monostearate, isopropyllaurate, -myristate, -palmitate and -stearate, lanoline, methyl phthalate, sesame oil and olive oil; diethyl and diisopropyl ethers; chloroform, carbon tetrachloride and trichloroethylene. The siloxanes are obtained by cohydrolyzing a mixture of more than 1 mol. but not more than 3 mols. of (CH 3 )SiCl and I mol. of RSiCl 3 with half the molar amount of water as there are gram atoms of chlorine in the silane mixture, and subsequently heating the reaction mixture to 100‹ C. until it is free from HC1. If desired the reaction product may be fractionated. Siloxanes in which R is phenyl, n-butyl and ethyl are disclosed and their miscibility with organic compounds is compared with that of other siloxanes. Uses: mould release agents; cosmetic preparations. Specification 848,719 is referred to.

    Process for the production of siliconcontaining trioxane copolymers
    8.
    发明授权
    Process for the production of siliconcontaining trioxane copolymers 失效
    制备含硅三氧杂环己烷共聚物的方法

    公开(公告)号：US3369039A

    公开(公告)日：1968-02-13

    申请号：US52484466

    申请日：1966-02-03

    Applicant: BAYER AG

    Inventor： DER EMDEN WOLFGANG VON ,  KUNO WAGNER ,  HANS NIEDERPRUM ,  WALTER SIMMLER

    IPC: C07F7/08 ,  C08G2/00

    CPC classification number: C08G2/06 ,  C07F7/0841 ,  C08G2/18

    Abstract: 1,142,646. Silicon-containing copolymers of trioxane; sila formals and esters. FARBENFABRIKEN BAYER A.G. 15 March, 1966 [15 April, 1965], No. 11337/66. Headings C3P and C3S. Silicone-containing copolymers are prepared by copolymerizing a formal or a carbonic acid ester of a bis-(hydroxyalkyl) silicon cornpound with trioxane at from 50‹ C. to 120‹ C. in the presence of a cationic initiator. Prefered copolymers are those of trioxane and a compound of the formula where X represents two hydrogen atoms or an oxygen atom, n = 1, 3 or 4, m = 0, 1, 2, 3 or 4 and o = 0 or 1, R 1 is -CH 3 , -O-Si(CH 3 ) 3 Particularly preferred copolymers contain 99À5 to 95À0 mol per cent of trioxane and 0À5 to 5 mol per cent of the formal or carbonic acid ester. A preferred copolymer is with 2,2,8,8-tetramethyl-2,8-disila-1,4,6-trioxa-cyclooctane. In Example 9 the condensation product of bis- (hydroxymethyl)-tetramethyl-disiloxane and pformaldehyde is used. Cationic initiators include strong acids e.g. sulphuric, perchloric, alkane-sulphonic and p-toluene sulphonic acids and Lewis acids e.g. boron trifluoride and its adducts and 2-methyl-1,3-dioxolenium fluoborate. The process may be carried out as an emulsion or solution polymerization in an inert organic liquid. It may be carried out as a bulk copolymerization, the catalyst being melted with the trioxane and the comonomer added simultaneously, or the trioxane being melted initially with the comonomer and then the catalyst added, possibly in an inert solvent. Further comonomers may be employed e.g. ethylene oxide, 1,3-dioxolane, 1,3-oxthiolane, bismethane - sulphonyl - imidazoline or hexamethyl - cyclotrisiloxane. The sila-formals employed in the invention may be obtained by treating bis-(hydroxy alkyl) - silicon compounds with formaldehyde or formaldehyde-yielding substances (e.g. paraformaldehyde or fomals of low-boiling alcohols) in the presence of catalyst e.g. small quantities of strong acid (e.g. p-toluenesulphonic acid or sulphuric acid) with moderate heating, the water which forms being removed by azeotropic distillation with an inert water-immiscible solvent or, in the case of re-acetalization, the volatile alcohol formed being distilled off. The corresponding carbonic acid esters are obtained in a similar manner by reaction with phosgene.

    Lubricants of organopolysiloxanes
    10.
    发明授权
    Lubricants of organopolysiloxanes 失效
    有机聚硅氧烷润滑剂

    公开(公告)号：US3122507A

    公开(公告)日：1964-02-25

    申请号：US1824560

    申请日：1960-03-29

    Applicant: BAYER AG

    Inventor： WALTER SIMMLER

    IPC: C07F7/08 ,  C08L83/04

    CPC classification number: C10M3/00 ,  C07F7/0847 ,  C08G77/04 ,  C08G77/16 ,  C08G77/24 ,  C08G77/70 ,  C08L83/04 ,  C10M2229/04 ,  C10M2229/043 ,  C10M2229/044 ,  C10M2229/051 ,  C10N2220/02 ,  C08L2666/44

    Abstract: A lubricant comprises, by weight, (a) 5 to 20% of heptamethyl-(hexachloro-dicycloheptenyl)-trisiloxane of the formula and (b) 95 to 80% of a liquid phenylmethylsiloxane composed of chains, end-blocked by (CH3)3SiO- units, of siloxane units of one of the formulae wherein each R is a methyl or phenyl radical, and within each siloxane chain the ratio of phenyl to methyl radicals is more than 1:5. Examples are given of mixtures of 10 pts. (by wt.) of the above trisiloxane with 90 pts. of different linear trimethylsiloxy-terminated phenylmethylsiloxanes, and of comparative mixtures of siloxanes.ALSO:A lubricant comprises, by weight, (a) 5 to 20% of heptamethyl-(hexachloro-dicycloheptenyl)-trisiloxane of the formula and (b) 95 to 80% of a liquid phenyl methyl siloxane composed of chains, end-blocked by (CH3)3SiO units, of siloxane units of one of the formulae wherein each R is a methyl or phenyl radical, and within each siloxane chain the ratio of phenyl to methyl radicals is more than 1:5. Examples are given of mixtures of 10 pts. (by wt.) of the above trisiloxane with 90 pts. of different linear trimethylsiloxy-terminated phenyl methyl siloxanes, and of comparative mixtures of siloxanes. By reacting hexachloropentadiene with a vinyl silane or a derivative thereof, the desired trisiloxane may be obtained as well as long chain siloxanes containing the chloroheptenyl radical and other diorganosiloxanes which may be copolymerized in known manner.

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