Patent GB-911223-A (GB)
Title: Diethylyaminoethyl celluloses
Inventor: LOCKWOOD ARTHUR RONALD
IPC: C09D127/06
Filed: 1959-10-26
Abstract: An ion-exchange material comprises diethylaminoethyl cellulose, the cellulose having an essentially amorphous structure.  It is made by reacting amorphous cellulose with an alkali metal hydroxide to form alkali cellulose, which is then reacted with a diethylhaloethylamine. Amorphous cellulose is made by very slow extrusion of viscose into an acid coagulating bath, no tension being applied to the filaments, which suitably are monofils of 1,000-60,000 denier and preferably of 25,000 denier. The monofils may be cut into pieces 1/4 inch in length, and milled to form particles not greater than 10 B.S. mesh, preferably between 16 and 52 B.S. mesh.  The cellulose particles may then be treated with caustic soda, followed by diethylchloroethylamine. The material so made may be filled into a glass column as a suspension in water, buffered with 0,1 M sodium dihydrogen phosphate at pH 6,6, and used for purification or concentration of proteinceous material, e.g. a -amylase (see Group IV(b) or of poliomyelitis virus, Vitamin B12 acid (by adsorption) and Vitamin B12 (by adsorption of impurities while the vitamin passes through the column), or for the demineralisation of water.ALSO:Diethylaminoethyl cellulose, in which the cellulose residue has an essentially amorphous structure, is made by reacting amorphous cellulose with an alkali metal hydroxide to form alkali cellulose which is then reacted with a diethylhaloethylamine. Amorphous cellulose is made by very slow extrusion of viscose into an acid coagulating bath, no tension being applied to the filaments, which suitably are monofils of 1,000-60,000 denier and preferably of 25,000 denier.  The monofils may be cut into pieces 1/4 inch in length, and milled to form particles not greater than 10 B.S. mesh, preferably between 16 and 52 B.S. mesh.  The cellulose particles may then be treated with caustic soda, followed by diethylchloroethylamine.  In an example, 1,058 Kg. of amorphous cellulose particles between 16 and 52 B.S. mesh are mixed at 11 DEG C. for one hour with 5,3:1 of 6N NaOH.  A solution of 1,058 Kg. of diethylchloroethylamine hydrochloride in 1,6:1 of water is then added, and the whole mixed continuously for 35 minutes at 85 DEG C. The mixture is then cooled to room temperature and acidified with 2,5:1 concentrated hydrochloric acid, filtered, and the residue washed with 12:1 tap water, 5,3:1 N.NaOH and then with tap water until the washings are almost neutral.  For the application of the product as an ion-exchange material, (see Group III).ALSO:a -Amylase may be separated, purified and concentrated by means of an ion-exchange material comprising diethylaminoethyl cellulose the cellulose having an essentially amorphous structure.  The ion-exchange material is made by reacting amorphous cellulose with an alkali metal hydroxide to form alkali cellulose, which is then reacted with a diethylhaloethylamine. Amorphous cellulose is made by very slow extrusion of viscose into an acid coagulating bath, no tension being applied to the filaments, which suitably are monofils of 1,000-60,000 denier and preferably of 25,000 denier.  The monofils may be cut into pieces 1/4 inch in length, and milled to form particles not greater than 10 B.S. mesh, preferably between 16 and 52 B.S. mesh.  The cellulose particles may then be treated with caustic soda, followed by diethylchloroethylamine.  In an example, 1.058 Kg. of amorphous cellulose particles between 16 and 52 B.S. mesh are mixed at 11 DEG C. for one hour with 5.3 l. of 6N NaOH.  A solution of 1.058 Kg. of diethylchloroethylamine hydrochloride in 1.6 l. of water is then added, and the whole mixed continuously for 35 minutes at 85 DEG C.  The mixture is then cooled to room temperature and acidified with 2.5 l. concentrated hydrochloric acid, filtered, and the residue washed with 12 l. tap water, 5.3 l. N.NaOH and then with tap water until the washings are almost neutral.  The material so made may be filled into a 10 ft. X 2 in. glass column as a suspension in water to give a 7 ft. bed of about 4.2 l. volume.  The bed is then buffered with 8.4 l. 0.1 M sodium dihydrogen phosphate at pH 6.6 fed downflow at 8.4 l./hr.  In an example, 75 l. of fungal a -amylase broth at a dextrinising activity of 14.0 units/ml., equivalent to 1,050 kilo units total activity, are adjusted to pH 6.6 with acetic acid, passed through a sterilising grade of filter paper and fed downflow through the bed at 4.2 l./hr. followed by 4.2 l. water as displacement wash at 4.2 l./hr.  Analysis of the column effluent showed 1.7 kilo units total dextrinising activity, giving 1,048.3 kilo units adsorbed, equivalent to 99.8% efficiency.  The adsorbed amylase is recovered by downflow elution with 4.2 l. 0.8 M sodium acetate/0.8 M sodium chloride buffer at pH 4.7 followed by a 4.2 l. displacement water wash, all at 2.1 l./hr.  A 7 l. portion of the eluate contained 992.2 kilo units total dextrinising activity, representing 94.6% efficiency and a ten fold concentration of the original broth.ALSO:Poliomyelitis virus may be purified or concentrated by means of an ion-exchange material comprising diethylaminoethyl cellulose, the cellulose having an essentially amorphous structure.  The ion-exchange material is made by reacting amorphous cellulose with an alkali metal hydroxide to form alkali cellulose, which is then reacted with a diethylhaloethyl amine. The material so made may be filled into a 10 feet x 2 inches glass column as a suspension in water to give a 7 feet bed of about 4.2 1. volume. The bed is then buffered with 8.4 1. 0.1 M sodium dihydrogen phosphate at pH 6.6 fed downflow at 8.4 1/hr.