Patent GB-678211-A (GB)
Title: Improvements in and relating to the conducting of chemical processes and apparatus therefor
IPC: B01J19/00
Filed: 1949-05-02
Abstract: Liquid phase chemical reactions in which at least one of the reactants is a gas are carried out under superatmospheric pressure and within controlled ranges of temperature by introducing the reactants into a zone containing heat transfer coils, passing a controlled portion of the reactant gas through the coils, mixing the streams of gas from the reaction zone and the coils, and recycling the combined stream partly to the reaction zone and partly to the coils (see Group III).  When all the reactants are gaseous an inert liquid medium is maintained in the reaction zone.  The molar ratio of gas to liquid used is such that little vaporization of the liquid occurs.  The process may be used for the carbonylation of mono-olefines containing 2-18 carbon atoms, or cyclohexene, by means of carbon monoxide and hydrogen, using a cobalt catalyst (e.g. cobalt naphthenate or acetate) at a temperature of 100-180 DEG  C. and a pressure of 200-300 atmospheres to form oxygen-containing compounds, especially aldehydes.  When the olefines are gaseous an inert liquid medium, e.g. saturated butane trimer, 3,5,5-trimethyl hexanol, or dinonyl ether, is present.  An example describes the carbonylation of diisobutylene to form a product comprising 3,5,5-trimethyl-hexanal-1 and 3,5,5-trimethylhexanol-1.  Other reactions referred to are: liquid-phase Fischer-Tropsch reaction; synthesis of glycollic acid from aqueous formaldehyde and carbon monoxide; synthesis of propionic acid from ethylene, carbon monoxide and water; reductive alkylation of aromatic nitro-bodies and amines to give alkyl substituted amines, e.g. N,N1-dialkyl-phenylene-diamines; and amination of high boiling aldehydes and ketones.ALSO:<PICT:0678211/III/1> Liquid phase chemical reactions in which at least one of the reactants is a gas are carried out under superatmospheric pressure and within controlled ranges of temperature by introducing the reactants into a zone containing heat transfer coils, passing a controlled portion of a reactant gas through the coils, mixing the streams of gas from the reaction zone and the coils, and recycling the combined stream partly to the reaction zone and partly to the coils.  When all the reactants are gaseous an inert liquid medium is maintained in the reaction zone. The molar ratio of gas to liquid used is such that little vaporization of the liquid occurs; the theoretical molar ratio is preferably 2 : 1 to 4 : 1, but the actual ratio used may be increased to 7 : 1. The ratio of the volume of gas passed through the coils to the volume fed to the reaction zone is preferably greater than 9 : 1 In the apparatus shown reactant gas is fed through pipes 2, and reactant liquid through pipe 3a heat transfer gas passes from inlet 11 via headers 10 through serpentine coils 8 to outlet 12; the reaction products are withdrawn through pipe 13 and the liquid portion separated.  When the reaction is exothermic, the gases from the coils and from the reaction zone are cooled before recycling; for endothermic reactions the circulating gases are heated.  The process may be used for the carbonylation of mono-olefines containing 2-18 carbon atoms, or cyclohexene, by means of carbon monoxide and hydrogen, using a cobalt catalyst (e.g. cobalt naphthenante or acetate) at a temperature of 100 DEG -180 DEG C and a pressure of 200-300 atmospheres to form oxygen-containing compounds, especially aldehydes.  When the olefines are gaseous, an inert liquid medium, e.g. saturated butane trimer, 3, 5, 5-trimethyl hexanol, or dinonyl ether, is present.  An example describes the carbonylation of diisobutylene to form a product comprising 3, 5, 5-trimethylhexanal-1 and 3, 5, 5-trimethylhexanol-1.  Other reactions referred to are: liquid phase Fischer Tropsch reaction; synthesis of glycollic acid from aqueous formaldehyde and carbon monoxide; synthesis of propionic acid from ethylene, carbon monoxide and water; reductive alkylation of aromatic nitro-bodies and amines to give alkyl substituted amines, e.g. NN1-dialkyl-phenylene diamines; and amination of high boiling aldehydes and ketones.