Patent ID: 11926703
Assignee: THOMAS FLECHSIG
Field: Macromolecular chemistry, polymers (Chemistry)
Classification: CPC C | IPC C

Claim 0:
1. A method for the production of poly(alkylene) guanidines, comprising at least the following steps:
a) providing an alkylene diamine of the formula NH2—(CH2)mNH2 where m=4-12, in a reaction vessel and heating of the alkylene diamine to a temperature equal to or above a melting temperature of the alkylene diamine, as a result of which a melt of the alkylene diamine is formed;
b) portion-wise adding of a guanidinium salt and reacting with the alkylene diamine until formation of alkylene(guanidine) monomers is concluded, wherein the formation of the alkylene(guanidine) monomers can be ascertained to be concluded by a cessation of foaming as a result of NH3 release and a vacuum is generated in the reaction vessel for a predetermined period of time in order to promote foaming, and optionally any unreacted alkylene diamine is distilled off prior to step c);
c) reacting the monomers formed in step b) at at least a minimum polymerization temperature at which a polymerization to a desired poly(alkylene) guanidine begins, with the minimum polymerization temperature being at least 120° C., until a formation of the poly(alkylene) guanidine is concluded;
wherein a molar ratio of alkylene diamine to guanidinium salt lies in a range from 1.2:1 to 1:1, and steps a) and b) for the formation of alkylene(guanidine) monomers are performed at a temperature within a range from 25° C. to 115° C., and all of the steps are carried out while stirring,
wherein step (b) is conducted while stirring at a temperature in a range from 41° C. to 110° C., for a period of time of 15 mm to 25 h, until the formation of alkylene(guanidine) monomers is concluded, and wherein step (c) comprises the following steps;
c1) heating the monomers formed in step b) while stirring to the minimum temperature at which the polymerization to the desired poly(alkylene) guanidine begins;
c2) keeping the reaction mixture at this temperature for a predetermined period of time;
c3) slowly increasing the reaction temperature in steps, and after each increasing step keeping the reaction mixture at the respective increased temperature for a predetermined period of time;
c4) keeping the reaction mixture at a predetermined maximum temperature for a predetermined period of time;
c5) reducing the temperature of the reaction mixture to a predetermined value below the maximum temperature, but above the minimum temperature for polymerization and keeping the reaction mixture at this temperature for a predetermined period of time; and
c6) cooling the reaction mixture to a temperature below the minimum polymerization temperature for the termination of polymerization, as a result of which the desired homogeneous poly(alkyene) guanidine is directly obtained.