RU1808832C - Method of hexamethylene guanidine polymer producing - Google Patents

Abstract

Usage: in systems for the preparation of highly pure waters. SUMMARY OF THE INVENTION: guanidine hydrochloride is mixed with hexamethylenediamine in a molar ratio of 1: 1.2-1.5, respectively, the mixture is heated for 10 hours at 150-160 ° C, cooled to a foamy solid mass, ground and washed. 6 tab.

Description

The invention relates to the field of synthesis of ion exchange resins, in particular to the synthesis of a structured polymer of hexamethylene guenidine having anion exchange properties, which can be used in highly pure water treatment systems.

The aim of the invention is to provide ion-exchange properties of the target product while maintaining its bactericidal activity.

The goal is achieved by the fact that the proposed polymer is obtained with an excess of HMDA against equimolar. Based on the trifunctionality of GHC and the bifunctionality of HMDA, the mutual saturation during the interaction of the groups contained in them occurs when the ratio of GHC: HMDA is 1: 1.5 and can be expressed by the following equation:

1,5H2N (CH2) 6NH2 + H2NCNH2iNHCNH (CH2) T

And NH HCI HC1M (CH2) bg

At a ratio of GTC: HMDA of 1: 1, a water-soluble compound is formed.

As the GHC: HMDA ratio increases from 1: 1.15 to 1: 1.5, crosslinking density and stiffness increase, and the degree of swelling in water decreases.

The guanidine group in the molecule of the claimed water-insoluble polymer creates a high positive charge and causes pronounced ion-exchange properties, while maintaining the bactericidal properties inherent in the guanidine group.

Example 1 In a metal beaker, 95.5 g (1 mol) of GHC are mixed with 139.2 g (1.2

00

about

00

00

00

Yu

mole) HMDA: the mixture is heated in an oil bath with periodic stirring for 10 hours at a temperature of 150-160 ° C. At the end of this period, the mixture is cooled and a foamy solid mass is obtained which is easily crushed to produce particles of any size. The resulting particles are placed in water for swelling, then in a column and washed with distilled water to remove the soluble fraction (sol),

Table 1 shows the ratios of the starting components for preparing the inventive hexamethylene guanidine polymer.

PRI me R 2, Determination of the degree of swelling of the polymer.

To determine the degree of swelling, a sample of dry resin is weighed, placed in a cylinder and poured with a 10-fold excess of water. The resin is left to swell for 15-20 hours and the degree of swelling is determined by the increase in volume.

. The results are presented in table 2,

Freeze, Determination of static exchange capacity.

To determine the static exchange capacity, 2 g of the polymer obtained in Example 1 are taken, placed in a conical flask, 200 ml of 0.1 N are added. NaOH solution, close with a ground stopper and leave for 24 hours with constant stirring. After that, an aliquot was taken from the flask and titrated with 0.1 N HCI solution. Full static exchange capacity is determined by the formula:

(V -a -Vi) 100., - Ps v., Lg. ...- -N, mEq / g, m (100 - W)

where V is the volume of the solution, taken for context, ml;

Vt is the volume spent on titration of an aliquot after contact, ml;

V a - rm-; t - mass of ion exchanger, taken for

contact, g;

W is the mass fraction of moisture,%; N is the normality of the solution. Equilibrium Static Exchange

capacity is determined by the formula

Pc

and VL- 100 m (100 -W)

N, mEq / g.

The results of determining the exchange capacity of the claimed polymer are presented in Table 3.

PRI me R 4. Determination of the bactericidal activity of the polymer hexamethylene guanidine.

To determine the bactericidal activity, 250 ml of water containing E. coli (E. col) in an amount of 4 x 108 col / l was placed in a flask, then 5 g of a swollen hexamethylene guanidine polymer was placed in the flask. The flask was closed and, with constant stirring, at regular intervals, samples were taken for the presence of microbial contaminants in the water. Determination of microbial contamination by E. Coli is carried out by filtering 1 ml of the sample through an No. 1 ashless membrane filter, then placing it on Endo medium in a Petri dish and incubating the culture at 37 ° C for 20-24 hours. Thereafter, colony grown on filters is counted. The results are presented in tables 4 and 5.

From table 6 it is seen that in comparison with the prototype, the proposed polymer has ion-exchange properties while maintaining bactericidal activity,

Claims (1)

SUMMARY OF THE INVENTION A method for producing a polymer of hexamethylene guanidine by reacting hexamethylene diamine and guanidine hydrochloride by heating, characterized in that, in order to ensure the ion-exchange properties of the target product while maintaining its bactericidal ™, the reaction is carried out at a molar ratio of guanidine hydrochloride with hexamethylene diamine 1 min , 2-1.5), respectively, for 10 hours at 150-160 ° C, followed by cooling to obtain a foamy solid mass, grinding and washing with water. Table 1 Table 4 Determination of bactericidal properties by polymers of hexamethylene guanidine with a ratio of starting components G GC: HMDA 1: 1.4 table 2 Table 3 Determination of the bactericidal properties of guanidine hydrochloride copolymer at various ratio of starting components Table 5 Table 6