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    2.
    发明专利
    未知

    公开(公告)号：DE1545491B1

    公开(公告)日：1969-09-18

    申请号：DE1545491

    申请日：1960-04-21

    Applicant: ETHYL CORP

    Inventor： ELDON COOK SHIRL ,  OLLOISE SISTRUNK THOMAS

    IPC: C07F7/24 ,  C10L1/14 ,  C10L1/16 ,  C10L1/20 ,  C10L1/30

    Abstract: An anti-knock concentrate comprises tetramethyllead and a hydrocarbon liquid having a boiling point at atmospheric pressure in the range of from 90 DEG to 150 DEG C. and selected from alkanes and mononuclear aromatics containing only aromatic unsaturation, especially toluene.ALSO:Tetramethyllead may be prepared by reacting a sodium-lead alloy and methyl chloride in the presence of a catalyst and a hydrocarbon liquid inert to the reactants under the reaction conditions. The catalysts specified include aluminium chloride, bromide and iodide, an alkyl compound of a Group II or III metal for example, dimethyl beryllium, diethyl zinc, triethyl gallium, triethyl aluminium, trimethyl aluminium, methyl aluminium sesquichloride or dimethyl aluminium chloride, a complex alumino hydride, an alkyl boron compound or phosphorus or arsenic. The hydrocarbon liquid has a boiling point between 90 DEG and 150 DEG C., and is preferably toluene. It is used in amount not greater than 25 parts by weight per 100 parts of lead in the alloy charged, and less than 50% by volume of the methyl chloride used. The methyl chloride is used in at least 5% excess, and there should also be sufficient methyl chloride present in addition to fill the reaction system with vapour. The amount of lead is 20-60 lbs. of lead per cubic foot of reaction zone space. The process may be carried out batchwise or continuously.

    8.
    发明专利
    未知

    公开(公告)号：DE1518759A1

    公开(公告)日：1969-03-20

    申请号：DE1518759

    申请日：1965-05-11

    Applicant: ETHYL CORP

    Inventor： ARTHUR HIRSCHLER DANIEL ,  OLLOISE SISTRUNK THOMAS

    IPC: C07F7/24 ,  C10L1/30 ,  C25B3/13

    Abstract: An antiknock composition comprises a mixture of tetrahydrocarbon leads of the following formulae : PbR4, PbR3R1, PbR12 R2, PbRR13 and PbR14 wherein R is an alkyl group, preferably of 1 to 4 carbon atoms and R1 is an alkenyl group preferably of 2 to 10 carbon atoms. The relative amount of each compound in the mixture is according to a statistical distribution of the hydrocarbon groups among the tetrahydrocarbon leads or within 7% thereof. There are preferably two to four different groups R and R1. R1 may constitute 25 to 75% of the groups R and R1. The antiknock composition can be mixed with petroleum for use as a motor car fuel, the petroleum can have a Research Octane Number of at least 87 and a sensitivity of at least 8.5. The composition can contain 0.5-7.0 g. Pb per U.S. gal. of fuel. The preferred mixture of tetrahydrocarbon leads consists of 2-7 mol per cent tetramethyl lead, 20-35 mol per cent trimethylvinyl lead, 35-45 mol per cent dimethyldivinyl lead, 20-35 mol per cent trivinylmethyl lead and 2-7 mol per cent tetravinyl lead. 0.2-2.5 theories of an organic halide scavenger, or mixture thereof, can be present. A solution of dyes and stabilizers can be present in the fuel, e.g. naphthalene and alkylated phenols, e.g. 2,6-di-tert-butyl phenol, 2,6-di-tert-butyl-4-metyl phenol and 4,41-methylene-bis-2,6, di-tert-butyl phenol in tolucene, tricresyl and trimethyl-phosphate. The fuel can contain other antiknocks, e.g. methylcyclopentadienyl manganese tricarbonyl, cyclopentadienyl manganese tricarbonyl, cyclopentadienyl nickel nitrosyl, tetraethyl lead, tetramethyl lead, tetravinyl lead, manganese pentacarbonyl, iron carbonyl, dicyclopentadienyl iron, dimethylcyclopentadienyl iron, aniline and N-methylaniline. Specified anti-oxidants, metal deactivators, phosphorous additives, synergists, dyes, boron additives, corrosion inhibitors, detergents and anti-icing additives may also be present. ALSO: An anti-knock composition comprises a mixture of tetrahydrocarbon leads of the following formulae: PbR4, PbR3R1, PbR12R2, PbRR13 and PbR14 wherein R is an alkyl group, preferably of 1 to 4 carbon atoms and R1 is an alkenyl group preferably of 2 to 10 carbon atoms. The relative amount of each compound in the mixture is according to a statistical distribution of the hydrocarbon groups among the tetrahydrocarbon leads or within 7% thereof. There are preferably two to four different groups R and R1. R1 may constitute 25 to 75% of the groups R and R1. The composition may be prepared by contacting a compound of the formula PbRnR1(4- n), n=1,2 or 3, or a mixture of at least two compounds of the formula PbRxR1(4- x), x=0, 1, 2, 3 or 4 with a catalyst the compounds being such that both R and R1 are in the mixture. The catalyst may be used in the amount 0.1 to 5% wt. of the total weight of reactants and may be an activated aluminosilicate, e.g. zeolite, or active Al2O3, AlCl3, (Et)2Zn, ZnF2, (Me)2AlCl, ZrCl4, PCl3, FeCl3 or Me3Al2Cl3. The reaction may be carried out from below 0 DEG C. up to the decomposition temperature of the tetrahydrocarbon lead, e.g. at 20 DEG to 70 DEG C. The composition may also be prepared by reacting a Pb salt, Pb oxide or sulphide under anhydrous conditions with a mixture of at least two Grignard reagents, the mixture containing both R and R1. This reaction temperature may be 20 DEG to 120 DEG C., the pressure may be 0.2 atm. to 2000 p.s.i. The composition is recovered by washing, filtering and distilling the filtrate. A desensitizing agent, e.g. toluene, naphthalene and alkylated phenols, may be added before recovery. The Grignard reagents may be methyl or ethyl magnesium chloride and vinyl magnesium chloride.

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