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    3.
    发明专利
    未知

    公开(公告)号：DE1238028B

    公开(公告)日：1967-04-06

    申请号：DEB0071578

    申请日：1963-04-20

    Applicant: BASF AG

    Inventor： MERKEL DR KARL ,  HAARER DR ERICH ,  CORR DR HUBERT

    IPC: C07B61/00

    Abstract: 1,054,685. #-Cyanoethyl ethers and thioethers. BADISCHE ANILIN- & SODAFABRIK A.G. April 10, 1964 [April 20, 1963]. No. 14855/64. Heading C2C. #-Cyanoethyl ethers and thioethers of monohydric or polyhydric alcohols, phenols or thiols are prepared continuously by reacting monohydric or polyhydric alcohols, phenols or thiols with stoichiometric or substantially stoichiometric amounts of acrylonitrile in the liquid phase in at least two separate containers arranged in series, with intense stirring and simultaneous supply of the reactants to the first reactor, the residence period in the first reactor being such that at the most 80% of the total conversion takes place therein and the reaction being completed in the last reactor at a higher temperature than in the first reactor. The intense mixing may be achieved by recirculation of the liquid phase. An excess of alcoholic, phenolic or thiolic reactant may be supplied to the first reactor and a further amount of acylonitrile to balance this excess may be fed to the second reactor. The reaction may be conducted both in the presence of an alkaline catalyst and in the presence of a polymerization inhibitor. Specified products include #-cyanoethyl methyl ether, #-cyanoethyl tertiary-butyl ether, tri-#-cyanoethoxypropane- (1,2,3), tetra - (# - cyanoethoxymethyl) - methane, di - # -cyanoethoxyethane - (1,2), di- (# 1 -cyanoethyl) diethyl ether, #-cyanoethyl phenyl ether, #-cyanoethyl benzyl ether, #- cyanoethyl cyclohexyl ether, 1,4-(di-#-cyanoethoxymethyl) - cyclohexane, # - cyanoethyl allyl ether, #-cyanoethyl propargyl ether, di-#- cyanoethoxy - (1,4) - butene - (2), di - #- cyanoethoxybutyne - (2), 4 - amino - 1 - #- cyanoethoxybutane, di- # cyanoethyl ether and #-cyanoethyl dodecyl thioether.

    5.
    发明专利
    未知

    公开(公告)号：DE1272913B

    公开(公告)日：1968-07-18

    申请号：DEB0072428

    申请日：1963-06-26

    Applicant: BASF AG

    Inventor： WEGERICH DR ANTON ,  FUERST DR ERNST ,  HAARER DR ERICH ,  CORR DR HUBERT

    IPC: C07C51/44

    Abstract: A mixture of succinic, glutaric and adipic acids, such as obtained by the oxidation of cyclohexanol, cyclohexanone or cyclohexane is separated by fractional distillation under subatmospheric pressure in the presence of steam. The mixture is introduced from tank 1 into evaporator 2, which is heated to about 200 DEG C. and is maintained at an absolute pressure of 40 to 100 mm. Hg. The mixture then flows down column 4 into a still 5 at 195 DEG to 220 DEG C. into which superheated steam is injected through line 7. The steam laden with acid vapours is conducted from the head of the column into the evaporator, the vapours then passing through line 8 into a condenser 9 and being sprayed therein with an aqueous solution from a receiver 10. Crystals of succinic acid suspended in an aqueous solution are obtained by cooling in a vessel 14, are separated out in a centrifuge 15. The mother liquid is evaporated and the residue is returned to the crude product. The product received in vessel 6 from the still is substantially glutaric and adipic acids. Water is added to convert anhydrides into acids before preheating in 17 and passing the mixture into a column 18. The still 19 of the column is heated to 200 DEG C., a vacuum of 40-50 mm. Hg is maintained at the top of the column, and superheated steam is passed through line 20 into the still. The vapours leaving the head of the column are cooled in a condenser 21 and liquid glutaric acid so formed flows into a receiver 22 while steam with a small amount of succinic acid flows into a condenser 23. A mixture of adipic acid with a small amount of glutaric acid is withdrawn at 27 from the still from which adipic acid may be recovered by crystallization. The columns are provided with packings, baffles, spirals or bubble trays.

    9.
    发明专利
    未知

    公开(公告)号：DE1188572B

    公开(公告)日：1965-03-11

    申请号：DEB0057889

    申请日：1960-05-18

    Applicant: BASF AG

    Inventor： CORR DR HUBERT ,  HAARER DR ERICH ,  HORNBERGER DR PAUL

    IPC: C07C29/149

    Abstract: Catalysts for the hydrogenation of carboxylic acids to alcohols consist of a metal hydrogenation catalyst, the catalytic activity of which is impaired by sulphur, and which is prepared by sintering the metals which may be used are preferably copper, silver, manganese, iron, nickel and especially cobalt and may be supported on pumice, alumina, kieselguhr, silica gel, synthetic or natural silicates, porcelain or quartz. The "sintering" is defined as heating the catalyst to a temperature which is not high enough to melt the catalyst but high enough to unite the particles in order to reduce the surface area and to improve the mechanical strength. If desired the oxide of the metal may be sintered and then reduced to the metal.ALSO:Carboxylic acids are hydrogenated in the liquid phase to alcohols at elevated temperature and at atmospheric or increased pressure by means of hydrogen in the presence of a metal hydrogenation catalyst, the catalytic activity of which is impaired by sulphur, and which has been prepared by sintering. The term "prepared by sintering" is defined as heating the catalyst to a temperature which is not high enough to melt the catalyst but high enough to unite the particles to reduce the surface area and to improve the mechanical strength. The process is particularly suitable for the hydrogenation of fatty acids with 3-20 carbon atoms, alkanoic dicarboxylic acids with 3-12 carbon atoms, aliphatic hydroxycarboxylic acids with 4-8 carbon atoms, aromatic hydroxycarboxylic acids with 7-9 carbon atoms, mononuclear aromatic monoor dicarboxylic acids and cycloalkanoic monoand dicarboxylic acids with 5 or 6 carbon atoms in the ring. The acids are preferably treated in aqueous or alcoholic solution at 150-300 DEG C The preferred catalysts are copper, silver, manganese, iron, nickel and especially cobalt. The catalyst may be sintered, if desired, in admixture with carrier substances such as pumice, alumina, kieselguhr, silica gel, silicates, porcelain or quartz, at temperatures which preferably lie only just below the melting-point of the metal used. The oxides of the metals may be used as starting materials for the catalysts and in this case they are sintered and then reduced to the metal. Examples are given of the conversion of (a) adipic acid to hexane-diol-(1,6); (b) glutaric acid to pentane-diol-(1,5); (c) the acid-containing product obtained by the oxidation of cyclohexane to a mixture of hexanediol-(1,6), pentanediol-(1,5) and butane-diol-(1,4); (d) propionic acid to n-propyl alcohol; (e) benzoic acid to benzyl alcohol; (f) cyclohexyl carboxylic acid to cyclohexyl carbinol; (g) salicylic acid to salicyl alcohol and (h) o -hydroxycaproic acid to hexanediol-(1,6).

    10.
    发明专利
    未知

    公开(公告)号：DE1172268B

    公开(公告)日：1964-06-18

    申请号：DEB0066040

    申请日：1962-02-21

    Applicant: BASF AG

    Inventor： WINDERL DR SIEGFRIED ,  HAARER DR ERICH ,  CORR DR HUBERT ,  HORNBERGER DR PAUL

    IPC: B01J23/38 ,  B01J23/70 ,  C07C209/16 ,  C07C211/10 ,  C07C211/11 ,  C07C211/12

    Abstract: Catalysts for the production of diamines (see Division C2) comprise at least one of the metals silver, copper, iron, cobalt and nickel prepared by sintering the metal powder or by reducing the sintered metal oxide or hydroxide, carbonate, nitrate or nitrite before or after shaping. Examples employ sintered Co, (Co + Ni), and (Co + Cu) or Ni. The powdered metal is sintered in admixture with a carrier such as pumice, alumina, corundum, diatomaceous earth, silica gel, silicon carbide, silicates, porcelain or quartz. Promoters such as alkali metal compounds, alkaline earth metal compounds, titanium dioxide, antimony, bismuth, or compounds of Group V or V1 of the Periodic System may also be added.ALSO:Open-chain diamines are prepared by passing a dihydric aliphatic alcohol, an alkanolamine, alkylene oxide or hexamethyleneimine or mixtures thereof, with a stoichiometric excess of ammonia or a primary or secondary amine, in the presence of at least 2 litres of hydrogen per mole of alcohol, alkanolamine, alkylene oxide or hexamethyleneimine, in the presence or absence of water, at 150-300 DEG C. at a pressure of at least 10 atmospheres, over a catalyst containing at least one of the metals silver, copper, iron, cobalt and nickel, said catalyst having been prepared by sintering. Examples prepare (1) ethylene diamine and piperazine from ethylene glycol and ammonia, and 1,2-diaminopropane similarly from 1,2-propanediol; (2) ethylene diamine and piperazine from ethanolamine, diethanolamine and ammonia, or from ethylene oxide and ammonia; (3), (4), (5) 1,6-hexamethylenediamine and hexamethyleneimine from 1,6-hexanediol and ammonia or hexamethyleneimine and ammonia; (6) N,N,N1,N1 - tetra ethyl ethylenediamine and N,N-diethylethanolamine from ethylene glycol and diethylamine; and (7) N-isopropyl-1,3-diaminopropane from 1,3-propanolamine and isopropylamine. Other reactants are listed.ALSO:Catalysts for the production of diamines (see Division C2) contain at least one of the metals silver, copper, iron, cobalt and nickel and are prepared by sintering the powdered metal in admixture with a carrier such as pumice, alumina, corundum, diatomaceous earth, silica gel, silicon carbide, silicates, porcelain or quartz, or by sintering oxides of the metal or compounds converted into oxides at sintering temperature, such as hydroxides, carbonates, nitrates and nitrites, in the presence of a carrier as above and/or a promoter such as alkali metal compounds, alkaline earth metal compounds, titanium dioxide, antimony, bismuth, or compounds of metals of Group V or VI of the Periodic System, and then reducing the sintered oxide with hydrogen.

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