24.
    发明专利
    未知

    公开(公告)号:CH605497A5

    公开(公告)日:1978-09-29

    申请号:CH1610473

    申请日:1973-11-15

    Applicant: BASF AG

    Abstract: 1440669 Substituted phenylindans BASF AG 16 Nov 1973 [18 Nov 1972 1 June 1973 30 May 1973] 53220/73 Heading C2C The invention comprises 1-methyl-3-(monohalogeno)-phenyl indans of the general Formula I in which R 1 , R 2 and R 3 are identical or different and each is alkyl or hydrogen and R 4 is halogen also dihalogeno-1-methyl-3-phenylindans of the general Formula II in which R 1 and R 2 are identical or different and each is alkyl or hydrogen and R 4 is a halogen substituent in the m- or p-position of the phenyl ring and in the 4-, 5- or 6-position of the indan nucleus, provided that when both radicals R 1 are methyl and one radical R 2 is hydrogen the other radical R 2 is alkyl. The compounds of Formula I may be prepared by reacting a mixture of styrene of the general Formula III and of halogenostyrene of the general Formula IV in which R 1 to R 4 have the above meanings, in the presence of phosphoric acid of at least 75% strength by weight and optionally, additionally to the acid, in the presence of an organic compound irradiated with light of 2000 to 8000 Š and capable of absorbing the said light. The compounds of Formula II in which R 1 and R 3 are identical or different and each is alkyl or hydrogen and R 4 is halogen may be obtained by reacting one or more halogeno styrenes of the general Formula IV as sole starting material(s) in the presence of phosphoric acid of at least 75% strength by weight and, additionally to the acid, in the presence of an organic compound irradiated with light of 2000 to 8000 Š and capable of absorbing the said light.

    Preparation of 1,6-hexan:diol and epsilon-caprolactone from carboxylic acid mixture

    公开(公告)号:DE19647349A1

    公开(公告)日:1998-05-20

    申请号:DE19647349

    申请日:1996-11-15

    Applicant: BASF AG

    Abstract: Preparation of 2,6-hexandiol and iota -caprolactone from a carboxylic acid mixture containing adipic acid, 6-hydroxycaproic acid and small amounts of 1,4-cyclohexandiols. The mixture is obtained as a by-product of the oxidation of cyclohexane into cyclohexanone and cyclohexanol with oxygen or oxygen-containing gases, water extraction, esterification and hydrogenation into hexandiol and cyclisation of 6-hydroxycaproic acid esters into caprolactone. Steps involved are: (a) esterification of the monocarboxylic and dicarboxylic acids in the aqueous reaction mixture with low molecular mass alcohols, (b) excess alcohol and low b.pt. substances are distilled off, (c) a second distillation step separates the mixture into an ester fraction substantially free of 1,4-cyclohexandiols and one containing at least the greater part of the 1,4-cyclohexandiols, (d) at least part of a substantially 6-hydroxycaproic acid ester stream is separated from the ester fraction in a third distillation stage, (e) the ester fraction from (d) from which the 6-hydroxycaproic acid ester was at least partially removed, is hydrogenated catalytically and 1,6-hexandiol is extracted by distillation and (f) the substantially 6-hydroxycaproic acid ester containing stream is heated above 200 deg C at reduced pressure so as to effect cyclisation. Pure iota -caprolactone is recovered by distillation. Preferably water is removed from the carboxylic acid mixture before esterification. Alcohol for esterification is either 1-3C (preferably MeOH) or 4-10C (preferably iso-BuOH or tert.-BuOH) and a variety of distillation, collection and separation arrangements are used depending on the relative b.pts. of the intermediate products involved. A Cu, Co and/or Re based catalyst is used for the hydrogenation step, or one of type CuaAlbZrcMndOx (a > 0, b > 0, c \- 0, d > 0, a > b/2, b > a/4, a > c, a > d and x = a number to balance the formula).

    29.
    发明专利
    未知

    公开(公告)号:DE19536178A1

    公开(公告)日:1997-04-03

    申请号:DE19536178

    申请日:1995-09-28

    Applicant: BASF AG

    Abstract: The continuous prodn. of alkyl(meth)acrylates (I) by the reaction of (meth)acrylic acid (II) and 1-8C monohydric alcohols (III) in homogeneous liq. phase at elevated temp. in the absence of solvent and in presence of an acid esterification catalyst (IV). The process comprises (a) feeding (II), (III) and (IV) continuously into a reaction zone (RZ), (b) removing (I) after a residence time in the form of an azeotrope contg. water or water and (III) in addn. to (I) at the top of a rectifier column (RC) mounted over the RZ, (c) separating the distillate into an organic phase contg. (I) and aq. phase(s) contg. water, (d) recycling part of the organic phase via the top of the column and opt. returning water to the RZ, (e) separating (I) from the rest of the organic phase and removing part of the reaction mixt. continuously from the RZ. The RZ consists of a cascade of at least two reactors in series, and the outflow from one reactor provides the input flow for the next reactor. Also claimed is an appts. for this process.

    30.
    发明专利
    未知

    公开(公告)号:DE19510891A1

    公开(公告)日:1996-09-26

    申请号:DE19510891

    申请日:1995-03-24

    Applicant: BASF AG

    Abstract: A continuous prepn. process for (meth)acrylic acid alkyl esters in a homogeneous, liq., organic solvent-free phase, comprises the following steps : (1) a 1-8C monovalent alcohol and (meth)acrylic acid are reacted in a mol. ratio of 1-2:1 at high temp. in the presence of sulphuric acid or an organic sulphonic acid catalyst, with the acid, alkanol and catalyst all being continuously supplied to a reactor ; (2) following several hours reaction time the azeotrope consisting of a (meth)acrylic acid alkyl ester and water or water / alkanol starting material is passed out of the top of the reactor where the pressure is 0.1-1 atmos. and sepd. in a rectification zone ; (3) the distillate is sepd. into at least one organic phase contg. the ester and at least one aq. phase ; (4) some of the organic phase is returned to the rectification zone and opt. water is returned to the reactor ; (5) the excess alkyl ester is sepd. from the organic phase by known methods ; and (6) some of the reaction mixt. is continuously removed from the reactor. The reaction temp. is 100-150 degrees C, the dwell time is 1-6 h and the reaction mixt. contains 5-20 wt.% acid catalyst.

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