VERFAHREN ZUR HERSTELLUNG VON ALKYLIERTEN N- BZW. AMINO-, AMMONIUM- ODER SPIROBICYCLISCHEN AMMONIUMGRUPPEN HALTIGEN, VERNETZTEN POLYMEREN

• Main Authors: STANEK, MICHAEL, SCHOPPEL, GERHARD, WRESSNEGGER, ERNST, WAGNER, MARION, RAML, WALTER, HAEUBL, GEORG
• Format: Patent
• Language: German
• Published: 15.04.2011
• Subjects: ACYCLIC OR CARBOCYCLIC COMPOUNDS; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F,C08G; CHEMISTRY; COMPOSITIONS BASED THEREON; GENERAL PROCESSES OF COMPOUNDING; MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVINGCARBON-TO-CARBON UNSATURATED BONDS; METALLURGY; ORGANIC CHEMISTRY; ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; WORKING-UP

Production of alkylated crosslinked polymer gels containing nitrogen, amino, ammonium or spiro bicyclic ammonium groups by a simplified and solvent-saving process comprising batchwise or continuous washing with a methanol/sodium chloride mixture, sodium chloride and then deionized water. Production of alkylated crosslinked polymer gels containing nitrogen, amino, ammonium or spiro bicyclic ammonium groups comprises: (i) pre-hardening an aqueous solution of the polymer at 0 - 90 degrees C and a pH of 7.5-14 using a crosslinker with stirring and then completing the hardening in a hardening vessel; (ii) cutting the gel to a definite shape; (iii) batchwise washing with methanol in a static or agitated bed; (iv) directly alkylating by adding alkylating agent(s) at 5 - 90 degrees C and 1-3 bar, adding a base and optionally re-protonizing; and (v) washing the alkylated gel either batchwise in a static or agitated bed or continuously, by washing first with methanol/sodium chloride, then with sodium chloride wash and finally with deionized water. An Independent claim is also included for a variant of the process in which the cut-to-shape gel is washed with methanol prior to being alkylated, the methanol washing comprising feeding the solvent at the bottom or top of a stirred vessel or of a stirred suction filter and suctioning of the used washing medium via a dip tube. Following the washing, alkylation is performed and the product is washed as per step (v) above with methanol/sodium chloride (MeOH/NaCl). The solvent washing comprises feeding the solvent upwards into a continuously-operating column, tower or stirred vessel containing the filtered gel cake as a static or agitated bed and suctioning off the solvent via a dip tube and then performing the sodium chloride and deionized water washes by spraying the gel bed or by suspension washing in a suction filter, stirred vessel or continuously-operating wash column.