Abstract:
The invention relates to a process for producing 4,4′-dichlorodiphenyl sulfone comprising reacting a solution comprising 4,4′-dichlorodiphenyl sulfoxide and at least one linear C6-C10 carboxylic acid as solvent with an oxidizing agent to obtain a crude reaction product comprising 4,4′-dichlorodiphenyl sulfone, wherein the concentration of water in the reaction mixture is kept below 5 wt %, the process comprising: (a) adding 0.9 to 1.05 mol oxidizing agent per mol 4,4′-dichlorodiphenyl sulfoxide uniformly distributed to the solution at a temperature in the range from 80 to 105° C. over a period from 1.5 to 5 h in a first step to obtain the reaction mixture; (b) agitating the reaction mixture after completion of the first step at the temperature of the first step for 5 to 30 min without adding oxidizing agent; (c) adding 0.05 to 0.2 mol oxidizing agent per mol 4,4′-dichlorodiphenyl sulfoxide to the reaction mixture at a temperature in the range from 80 to 105° C. over a period of less than 40 min in a second step; (d) agitating the reaction mixture after completion of the second step at the temperature of the second step for 10 to 30 min without adding oxidizing agent, (e) heating the reaction mixture to a temperature in the range from 95 to 110° C. and hold this temperature for 10 to 90 min to obtain a crude reaction product comprising 4,4′-dichlorodiphenyl sulfone.
Abstract:
The invention relates to a process for producing 4,4′-dichlorodiphenyl sulfoxide comprising: (a) reacting thionyl chloride, chlorobenzene and aluminum chloride in a molar ratio of thionyl chloride:chlorobenzene:aluminum chloride of 1:(6 to 9):(1 to 1.5) at a temperature in the range from 0 to below 20° C., forming an intermediate reaction product and hydrogen chloride, (b) mixing aqueous hydrochloric acid and the intermediate reaction product at a temperature in the range from 70 to 110° C. to obtain a crude reaction product comprising 4,4′-dichlorodiphenyl sulfoxide, (c) separating the crude reaction product into an organic phase comprising the 4,4′-dichlorodiphenyl sulfoxide and an aqueous phase, (d) washing the organic phase with an extraction liquid.
Abstract:
The invention relates to a process for producing free-flowing dicarboxylic acid crystals from an aqueous solution or suspension of the dicarboxylic acid in a crystallizer.
Abstract:
The present invention relates to an apparatus of the loop Venturi reactor type for the continuous reaction of liquids with gases, in particular for hydrogenations, oxidations or acetylations, e.g. for the preparation of toluenediamine by hydrogenation of dinitrotoluene, and a process for the continuous reaction of liquid reactants with gaseous reactants in the apparatus. In the apparatus of the invention, the diversion of an internal circulatory flow in the reactor is effected by means of a diversion pan which is arranged underneath a heat exchanger.
Abstract:
The invention relates to an apparatus (1) for producing pseudoionone and hydroxy pseudoionone. It suggests an apparatus (1) comprising first and second substantially vertically oriented reactor chambers oriented such that components flow through the first and second reactor chambers in different directions, wherein the first reactor chamber (13) is configured to receive a first component feed (C1) containing a first aqueous mixture through an inlet (15), and to produce a second aqueous mixture, and wherein the apparatus (1) comprises a mixing device (17) positioned downstream of the first component feed inlet (15) and configured to add a second component feed (C2) to the first component feed (C1) when the second aqueous mixture has formed, and the second reactor chamber (23) is configured to receive the first and second component feeds unified in the mixing device (17) from the first reactor chamber (13) and to produce a third aqueous mixture from the first and second aqueous mixtures. The invention further suggests a method and a use for producing pseudoionone and hydroxy pseudoionone.
Abstract:
The invention relates to a process for producing 4,4′-dichlorodiphenyl sulfone, comprising: (a) reacting 4,4′-dichlorodiphenyl sulfoxide and an oxidizing agent in at least one carboxylic acid as solvent to obtain a reaction mixture comprising 4,4′-dichlorodiphenyl sulfone and carboxylic acid; (b) separating the reaction mixture into a first stream comprising 4,4′-dichlorodiphenyl sulfone and a second stream comprising carboxylic acid; (c) purifying the second stream comprising carboxylic acid by distilling a part of the second stream comprising carboxylic acid stripping low boilers from at least a part of the second stream comprising carboxylic acid (d) recycling the purified carboxylic acid into the reaction (a).
Abstract:
Process for the continuous production of an optically active carbonyl compound by asymmetric hydrogenation of a prochiral α,β-unsaturated carbonyl compound with hydrogen in the presence of a homogeneous rhodium catalyst that has at least one chiral ligand, wherein a liquid reaction mixture comprising the prochiral α,β-unsaturated carbonyl compound is subjected in a first, backmixed reactor to a gas/liquid two-phase hydrogenation, and the liquid reaction mixture is then further hydrogenated in a second reactor, wherein the prochiral α,β-unsaturated carbonyl compound is employed in the first reactor in a concentration from 3% to 20% by weight. The process allows a high total conversion to the prochiral α,β-unsaturated carbonyl compound.
Abstract:
The invention relates to a process for purifying 4,4′-dichlorodiphenyl sulfone comprising: (a) providing a suspension comprising particulate 4,4′-dichlorodiphenyl sulfone in carboxylic acid, (b) carrying out a solid-liquid separation of the suspension to obtain residual moisture containing 4,4′-dichlorodiphenyl sulfone and a carboxylic acid comprising filtrate, (c) washing the residual moisture containing 4,4′-dichlorodiphenyl sulfone with an aqueous base and then with water, (d) mixing the aqueous base after being used for washing with a strong acid, or mixing the aqueous base after being used for washing, the carboxylic acid comprising filtrate and a strong acid, (e) carrying out a phase separation in which an aqueous phase and an organic phase comprising the carboxylic acid are obtained.