National Starch and Chemical Corporation

Dennis V Neigel

Martin M Tessler

Chester D Szymanski

John Kancylarz

An improved and novel process for the preparation of an aqueous 3-chloro-2-sulfopropionic acid reagent involves the formation of a reaction mixture by adding acrylic acid to chlorosulfonic acid maintained at about 45.degree. to 130.degree. C., maintaining the mixture at about 60.degree.-130.degree. C. for about 2-6 hours, and adding sufficient water to the resulting anhydrous reagent to decompose the unreacted chlorosulfonic acid and dilute the reagent to a solids content of about 50-95%, preferably 70-90%. The reagent may be vacuum stripped to remove residual hydrochloric acid. Crystalline 3-chloro-2-sulfopropionic acid may be isolated from the aqueous reagent at a solids content above 80% and below 95%, preferably at 85%.

Process for the preparation of an anhydrous and aqueous

A semi-continuous process for the manufacture of acetals of chloroacetaldehyde is described. In a preferred embodiment of the invention, chloroacetaldehyde dimethyl acetal is prepared by introducing chlorine and vinyl acetate through separate inlets into the upper opening of a cooled vertical packed column to form an intermediate product. The intermediate flows through the column, and optionally a static mixer, into a cooled batch reactor precharged with an excess of methanol to form the crude acetal product. Isolation and purification of the product is accomplished by known batch-type procedures.

Process for the manufacture of acetals of chloroacetaldehyde

A semi-continuous process for the manufacture of acetals of alpha-halogenated aldehydes is described. In a preferred embodiment of the invention, chloroacetaldehyde dimethyl acetal is prepared by introducing chlorine and a mixture of vinyl acetate and an excess of methanol through separate inlets into a reaction site of a vertical packed column and collecting a low boiling distillate formed from by-product vapors and separately collecting the crude acetal product flowing downward from the reaction site.

Process for the manufacture of chloroacetaldehyde dialkyl acetals

Quaternary ammonium monomers and monomers copolymerizable therewith are reacted in the presence of anionic polymers to directly form a dry coacervate by a process which comprises forming a solution comprising the monomer(s), the anionic polymer, solvent(s) and a free-radical initiator and simultaneously polymerizing and drying the solution at a temperature above the boiling point of the solvent.

Process for reacting quaternary ammonium monomer in the presence of

Graft copolymers of cellulose derivatives and N,N-diallyl,N-N-dialkyl ammonium chlorides or bromides are prepared using a dry or substantially solvent-free system by impregnating a concentrated aqueous solution of the N,N-diallyl-N,N-dialkyl ammonium halide, water soluble surfactant and catalyst onto the dry cellulose substrate, heating the reaction mass for sufficient time to achieve polymerization and then drying.

Process for the preparation of graft copolymers of cellulose derivatives

Quaternary ammonium monomers and monomers copoylmerizable therewith are reacted in the presence of anionic polymers to directly form a dry coacervate by a process which comprises forming a solution comprising the monomer(s), the anionic polymer, solvent(s) and a free-radical initiator and simultaneously polymerizing and drying the solution at a temperature above the boiling point of the solvent.

Process for reacting quaternary ammonium monomers in the presence of

Homo- and copolymers of quaternary ammonium monomers are prepared directly in dry form by a process which comprises forming a solution of the monomer(s), solvent and a free-radical initiator and simultaneously polymerizing the monomers and drying the solution at a temperature above the boiling point of the solvent.

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Whitehouse Station, NJ, United States of America

Dennis V Neigel