摘要:
The invention relates to a process for the removal of deposits formed in a reaction apparatus by the precipitation of solids from a liquid reaction mixture, which process is characterized in that particles of a material that is inert under the reaction conditions are introduced into the reaction apparatus, which particles, by suitable mechanical circulation of the reaction mixture, are so moved through the reactor that, during the reaction, by striking the walls or other built-in elements, they abrasively remove precipitates adhered thereto.
摘要:
A process for the separation a substantially adduct-free diaryl carbonate from reaction solution is disclosed. The process entails obtaining a solution that contains diaryl carbonate, catalyst system components and an aromatic solvent, lowering the temperature of the solution, optionally in the presence of a nucleating agent, to produce a crystallization product, and washing the crystallization product with an anhydrous wash solution to remove catalyst residues and impurities.
摘要:
A process for the separation a substantially adduct-free diaryl carbonate from reaction solution is disclosed. The process entails obtaining a solution that contains diaryl carbonate, catalyst system components and an aromatic solvent, lowering the temperature of the solution, optionally in the presence of a nucleating agent, to produce a crystallization product, and washing the crystallization product with an anhydrous wash solution to remove catalyst residues and impurities.
摘要:
A process for the work up of a reaction mixture obtained from the preparation of diaryl carbonate by direct carbonylation of aromatic hydroxy compounds is disclosed. The process entails obtaining a reaction mixture that contains diaryl carbonate, aromatic hydroxy compound, water, base and quaternary salt, separating the mixture in a distillation apparatus having only one theoretical separation stage into a liquid phase and a gas phase and recycling the liquid phase without further work up to the reaction step of the direct carbonylation.
摘要:
The present invention relates to a process for the preparation of aromatic amines of the formula (I) Ar--NR.sup.1 R.sup.2 (I) in which Ar is ##STR1## and R.sup.3 to R.sup.9 independently of one another are hydrogen, C.sub.1 -C.sub.8 -alkyl, alkoxy-(C.sub.1 -C.sub.8), acyloxy-(C.sub.1 -C.sub.8), OAr, Ar, fluorine, chlorine, bromine, iodine, OH, NO.sub.2, CN, CO.sub.2 H, CHO, SO.sub.3 H, SO.sub.2 R, SOR, NH.sub.2, NH-alkyl-(C.sub.1 -C.sub.12), N-alkyl.sub.2 -(C.sub.1 -C.sub.12), NHCO-alkyl-(C.sub.1 -C.sub.12), CO-alkyl-(C.sub.1 -C.sub.12), NHCHO, COAr, CO.sub.2 Ar, CF.sub.3, CONH.sub.2, CHCHCO.sub.2 R, POAr.sub.2, PO-alkyl.sub.2 -(C.sub.1 -C.sub.12), 5-ring heteroaryl, 6-ring heteroaryl, Si-alkyl.sub.3 -(C.sub.1 -C.sub.12), where R=alkyl(C.sub.1 -C.sub.8), aryl(C.sub.5 -C.sub.10) and R.sup.1 and R.sup.2 independently of one another are hydrogen, C.sub.1 -C.sub.12 -alkyl, Ar as defined above, 5-ring heteroaryl, 6-ring heteroaryl, by reacting chloroaromatics of the formula II Ar--Cl (II) with ammonia or primary or secondary amines of the formula III R.sup.1 R.sup.2 NH (III) in which Ar and R.sup.1 and R.sup.2 are as defined above, which comprises reacting the starting materials in the presence of a palladium catalyst, a strong base and a halide cocatalyst in an inert solvent at temperatures of 80.degree.-200.degree. C.
摘要:
The preparation of quaternary salt phenolate solutions is disclosed. The preparation entails mixing an aqueous hydroxide-containing solution with an organic phase that contains phenol and quaternary salt, distilling off the water and precipitating and filtering off the resulting salt.
摘要:
A process for the removal and recovery of quaternary salt (A) and base (D) from a reaction mixture is disclosed. The reaction mixture resulting from oxidative direct carbonylation contains in addition to (A) and (D), at least one hydroxyaromatic compound (B) and at least one reaction product (C) and optionally a solvent, and the process entails a) adding acid to the reaction mixture to cause conversion of (D) into a hydroxyaromatic compound (B2) b) separating the reaction mixture into b1.) that contains (C) and optionally (B) and/or (B2) and b2.) that contains (A) and optionally (B) and/or (B2), and c) reacting b1.) with a base (E) to re-form (D).
摘要:
A process for the production of an aromatic carbonate is disclosed. Accordingly, an aromatic hydroxy compound is reacted with carbon monoxide and oxygen in the presence of a platinum group metal catalyst, a co-catalyst, a base, and optionally a quaternary salt as well as an inert organic solvent. The reaction is carried out under conditions whereby the inert organic solvent forms an azeotrope with the water arising during the reaction. The azeotrope is then removed from the reaction mixture.
摘要:
A process for the work up of reaction mixtures containing diaryl carbonate, aromatic hydroxy compound, water, base and quaternary salt, which are obtained in the preparation of diaryl carbonates by direct carbonylation of aromatic hydroxy compounds, is described. In the process of the present invention an adduct of diaryl carbonate and aromatic hydroxy compound is crystallized from the reaction mixture. A distillate comprising aromatic hydroxy compound is removed from the liquid phase either prior to or after crystallization of the adduct of diaryl carbonate and aromatic hydroxy compound. The liquid phase remaining after the crystallization and distillation steps may be recycled, without further work up, back to the direct carbonylation process step by which the diaryl carbonate is initially prepared.