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公开(公告)号:DE2801578A1
公开(公告)日:1979-07-19
申请号:DE2801578
申请日:1978-01-14
Applicant: BASF AG
Inventor: MUELLER HERBERT DIPL CHEM DR , HUCHLER OTTO HERMANN DIPL CHEM , HOFFMANN HERWIG DIPL CHEM DR
Abstract: Polybutyleneglycol carboxylic acid diesters R-CO-O-(-CH2CH2CH2CH2-O-)n-CO-R' (I) (in which R and R1 are alkyl, COOH-contg. opt. unsaturated aliphatic gp. or COOH-contg. aromatic gp. and n is a 2-200) are made by first treating tetrahydrofuran with strong mineral acids, organic sulphonic acids, silica gel and/or fuller's earth. The treated THF is then polymerised in the presence of >=1 carboxylic acid or carboxylic acid anhydride and a polymerisation catalyst to form the (I). The pretreatment of the THF removes traces of impurities present in technical THF and gives higher rates of polymerisation, reproducible molecular weights and avoidance of discoloured prods. The (I) can be transesterified e.g. with methanol to give the corresponding dihydroxy cpds., which are useful raw materials for the prodn. of polyurethanes.
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公开(公告)号:DE2743345A1
公开(公告)日:1979-04-05
申请号:DE2743345
申请日:1977-09-27
Applicant: BASF AG
IPC: B01J21/00 , B01J27/00 , C07B61/00 , C07D307/08 , C07D307/935
Abstract: Cyclic ethers, especially tetrahydrofuran, are manufactured by dehydrating diols in the liquid phase in the presence of a bleaching earth as the catalyst and of a minor amount of an alkali metal or alkaline earth metal carbonate or bicarbonate.
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公开(公告)号:DE2624286A1
公开(公告)日:1977-12-22
申请号:DE2624286
申请日:1976-05-31
Applicant: BASF AG
Inventor: MUELLER HERBERT DIPL CHEM DR , HOFFMANN HERWIG DIPL CHEM DR , WINDERL SIEGFRIED DIPL CHEM DR , HUCHLER OTTO HERMANN DIPL CHEM
IPC: C08G65/20
Abstract: Tetrahydrofuran (I) is polymerised using SbCl5 as catalyst in presence of >=1 carboxylic acid or anhydride in which the SbCl5 is pref. dissolved, allowing a reduction in catalyst concn. The catalyst also contains an alcohol as activator. Catalyst activity is substantially increased, the polymerisation rate and output being approx. doubled.
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公开(公告)号:DE2445962A1
公开(公告)日:1976-04-08
申请号:DE2445962
申请日:1974-09-26
Applicant: BASF AG
Inventor: HUCHLER OTTO HERMANN DIPL CHEM , MESCH WALTER DIPL CHEM DR , WINDERL SIEGFRIED , MUELLER HERBERT DIPL CHEM DR , HOFFMANN HERWIG DIPL CHEM DR
IPC: C08F8/12 , C08G65/324 , C08G65/332
Abstract: Hydroxylated polymers, esp. polyetrahydrofuran, for polyurethane prepn. are prepd. by saponifying acyloxylated polymers at 10-200 degrees C in an aq. salt soln. contg. a catalyst consisting of an acid or an acid-forming cpd. (pref. a halo acid). The reaction mixt. may contain an alcohol which is immiscible, or only partly miscible with water. The simple, economic process avoids the use and recovery of special solvents, and leads to less pollution by by-prods.
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公开(公告)号:DE2930144A1
公开(公告)日:1981-02-19
申请号:DE2930144
申请日:1979-07-25
Applicant: BASF AG
Inventor: MUELLER HERBERT , HOFFMANN HERWIG DIPL CHEM DR , WINDERL SIEGFRIED DIPL CHEM DR , HUCHLER OTTO HERMANN DIPL CHEM
IPC: B01J21/04 , C07B61/00 , C07D307/06 , C07D307/08 , C07D309/04 , C07D313/04 , C07D305/06
Abstract: Prodn. of cyclic ethers (I) comprises liq. phase dehydration of alpha, omega-diols (II) in presence of alumina suspended in the reaction mixt. The alumina is prepd. by pptn. of an alkali aluminate soln. with acid, then heating at 300-1000 deg. C. The method is used to prepare ethers (I) (A is 4-8C alkylene, opt. interrupted by heteroatoms) e.g. 1,4-dioxan from diethylene glycol or 2,5-dihydrofuran from cis-buten-2- diol-1,4. The catalyst gives almost quantitative yields and works effectively even with relatively impure diols. Catalyst consumption is low; it is not corrosive so relatively inexpensive materials can be used for the reactors, and the reaction rate is high e.g. at 210 deg. C 1-3 pts. THF per hr. per pt. catalyst.
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公开(公告)号:DE2801792A1
公开(公告)日:1979-07-19
申请号:DE2801792
申请日:1978-01-17
Applicant: BASF AG
Inventor: MUELLER HERBERT DIPL CHEM DR , HUCHLER OTTO HERMANN DIPL CHEM , HOFFMANN HERWIG DIPL CHEM DR
Abstract: Polybutyleneglycol carboxylic acid diesters R-CO-O-(-CH2CH2CH2CH2-O-)n-CO-R' (I) (in which R and R1 are alkyl, COOH-contg. opt. unsaturated aliphatic gp. or COOH-contg. aromatic gp. and n is a 2-200) are made by first treating tetrahydrofuran with strong mineral acids, organic sulphonic acids, silica gel and/or fuller's earth. The treated THF is then polymerised in the presence of >=1 carboxylic acid or carboxylic acid anhydride and a polymerisation catalyst to form the (I). The pretreatment of the THF removes traces of impurities present in technical THF and gives higher rates of polymerisation, reproducible molecular weights and avoidance of discoloured prods. The (I) can be transesterified e.g. with methanol to give the corresponding dihydroxy cpds., which are useful raw materials for the prodn. of polyurethanes.
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公开(公告)号:DE2445961A1
公开(公告)日:1976-04-08
申请号:DE2445961
申请日:1974-09-26
Applicant: BASF AG
Inventor: HUCHLER OTTO HERMANN DIPL CHEM , MESCH WALTER DIPL CHEM DR , WINDERL SIEGFRIED DIPL CHEM DR , MUELLER HERBERT DIPL CHEM DR , HOFFMANN HERWIG DIPL CHEM DR
IPC: C08G65/20 , C08G65/30 , C08G65/324 , C08G65/332
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公开(公告)号:DE2509968A1
公开(公告)日:1976-09-16
申请号:DE2509968
申请日:1975-03-07
Applicant: BASF AG
Inventor: HUCHLER OTTO HERMANN DIPL CHEM , WINDERL SIEGFRIED DIPL CHEM DR , MUELLER HERBERT DIPL CHEM DR , HOFFMANN HERWIG DIPL CHEM DR
IPC: C07D307/08 , C07D307/28 , C07D309/04 , C07D315/00 , C07D307/00
Abstract: Cyclic ethers having >=5 ring members are prepd. from >=4C diols in the presence of an acid, esp. aq. H2SO4, as catalyst, by a process in which a water content of >=30 (>40) wt % is kept up in reaction mixt. Cyclic ethers obtd. are useful as monomers, synthesis intermediates and solvents. Use of process for prepn, of tetrahydrofuran from butanediol-1, 4 is specifically claimed. Process allows (i) use of undistilled butanediol without requiring a high catalyst consumption, (ii) working with appreciable aq. dilution. Yields are almost quantitative. Process can be carried out continuously, e.g. for months, without interruption.
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公开(公告)号:DE2445960A1
公开(公告)日:1976-04-15
申请号:DE2445960
申请日:1974-09-26
Applicant: BASF AG
Inventor: HUCHLER OTTO HERMANN DIPL CHEM , MESCH WALTER DIPL CHEM DR , WINDERL SIEGFRIED DIPL CHEM DR , MUELLER HERBERT DIPL CHEM DR , HOFFMANN HERWIG DIPL CHEM DR
IPC: C08F8/12 , C08G65/324 , C08G65/332
Abstract: Hydroxylated polymers, esp. polyetrahydrofuran, for polyurethane prepn. are prepd. by saponifying acyloxylated polymers at 10-200 degrees C in an aq. salt soln. contg. a catalyst consisting of an acid or an acid-forming cpd. (pref. a halo acid). The reaction mixt. may contain an alcohol which is immiscible, or only partly miscible with water. The simple, economic process avoids the use and recovery of special solvents, and leads to less pollution by by-prods.
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