Patent GB-835977-A (GB)
Title: Method of separating non-ionized organic solutes from one another in aqueous solution
IPC: B01J47/00
Filed: 1958-02-12
Abstract: An aqueous solution of at least two of the weakly or non-ionized organic compounds hereinafter referred to is fed to a bed of an ion-exchange resin immersed in an aqueous liquid, an aqueous solution of one of the inorganic electrolytes hereinafter referred to is then fed to the bed and successive fractions of the eluate are collected whereby there are obtained certain fractions each of which contains the major portion of one of said organic compounds.  Organic compounds which are separated are lower alkyl alcohols (methyl, ethyl, n-propyl, i-propyl, n-butyl, sec.-butyl, tert.-butyl), glycols (ethylene glycol, propylene glycol, diethylene glycol, triethylene glycol, dipropylene glycol), glycerol, aldehydes (formaldehyde, acetaldehyde, acetal methylal), ketones, amines (methylamine, ethyl-, amine, n-propylamine, isopropylamine, n-butylamine, sec.-butylamine, diethylamine, monoethanolamine) and lignins.  Electrolytes which are used for elution are chlorides of sodium, potassium, ammonium, calcium, barium and aluminium, bromides of sodium and ammonium, sulphates of sodium, potassium, ammonium, magnesium and aluminium, sodium borate and potassium phosphate; basic salts such as the last mentioned (K3PO4) are preferred when separating amines from each other.  Suitable concentrations are from 0.1 N to saturated. Initially the bed is flooded normally with water or the eluting solution.  The process is preferably conducted at from 20-85 DEG  C. and may be repeated many times using the same bed of resin; by employing two or more beds in parallel and loading one whilst eluting another, the process may be carried out continuously.  Examples describe the separation of individual alcohols, glycols, and amines from mixtures comprising only alcohols, glycols and amines respectively.  Cation and anion exchange resins may be employed; strongly basic quaternary ammonium resins may be used in basic or salt form. For separating aliphatic hydroxy compounds using ammonium sulphate eluent solution, the preferred resin is the reaction product of an insoluble copolymer of a major amount of styrene and minor amounts of ar-ethyl vinyl benzene, and divinyl benzene, said copolymer containing chloromethyl groups on aromatic nuclei, with trimethylamine; for separating aliphatic amines using potassium phosphate eluent solution, the preferred resin is the alkali metal salt form of a nuclear sulphonated insoluble copolymer of a major proportion of styrene and minor proportions of ar-ethyl vinyl benzene and divinyl benzene.  Other specified resins are (a) the reaction product of an insoluble copolymer of a major proportion of at least one monovinyl aromatic compound and a minor proportion of divinyl benzene, said copolymer containing chloromethyl groups on aromatic nuclei, and a tertiary amine; and (b) a nuclear sulphonated copolymer of a polymerizable monoalkenyl aromatic hydrocarbon, e.g. styrene, vinyl-toluene or ar-ethyl-vinyl benzene and a divinyl benzene. Specifications 577,707, 654,706, 679,850 and 709,550 are referred to.ALSO:An aqueous solution of at least two of the weakly or non-ionized organic compounds hereinafter referred to is fed to a bed of an ion exchange resin immersed in an aqueous liquid, an aqueous solution of one of the inorganic electrolytes hereinafter referred to is then fed to the bed and successive fractions of the eluate are collected whereby there are obtained certain fractions each of which contains the major portion of one of said organic compounds.  Organic compounds which are separated are lower alkyl alcohols (methyl, ethyl, n-propyl, i-propyl, n-butyl, sec.-butyl, tert.-butyl), glycols (ethylene glycol, propylene glycol, diethylene glycol, triethylene glycol, dipropylene glycol), glycerol, aldehydes (formaldehyde, acetaldehyde, acetal, methylal), ketones, amines (methylamine, ethylamine, n-propylamine, isopropylamine, n - butylamine, sec. - butylamine, diethylamine, monoethanol-amine) and lignins. Electrolytes which are used for elution are chlorides of sodium, potassium, ammonium, calcium, barium and aluminium, bromides of sodium and ammonium, sulphates of sodium, potassium, ammonium, magnesium and aluminium, sodium borate and potassium phosphate; basic salts such as the last mentioned (K3PO4) are preferred when separating amines from each other.  Suitable concentrations are from 0.1 N to saturated.  Initially the bed is flooded normally with water or the eluting solution.  The process is preferably conducted at from 20-85 DEG  C. and may be repeated many times using the same bed of resin: by employing two or more beds in parallel and loading one whilst eluting another, the process may be carried out continously. Examples describe the separation of individual alcohols, glycols, and amines from mixtures comprising only alcohols, glycols and amines respectively.  Cation and anion exchange resins may be employed; strongly basic quaternary ammonium resins may be used in basic or salt form. For separating aliphatic hydroxy compounds using ammonium sulphate eluent solution, the preferred resin is the reaction product of an insoluble copolymer of a major amount of styrene and minor amounts of ar-ethyl vinyl benzene and divinyl benzene, said copolymer containing chloromethyl groups on aromatic nuclei, with trimethylamine; for separating aliphatic amines using potassium phosphate eluent solution, the preferred resin is the alkali metal salt form of a nuclear sulphonated insoluble copolymer of a major proportion of styrene and minor proportions of ar-ethyl vinyl benzene and divinyl benzene.  Other resins are (a) the reaction product of an insoluble copolymer of a major proportion of at least one monovinyl aromatic compound and a minor proportion of divinyl benzene, said copolymer containing chloromethyl groups on aromatic nuclei; and a tertiary amine, and (b) a nuclear sulphonated copolymer of a polymerizable monoalkenyl aromatic hydrocarbon e.g. styrene, vinyl-toluene or ar-ethyl vinyl benzene and a minor proportion of divinyl benzene.  Specifications 577,707, 654,706, 679,850 and 709,550 are referred to.