Preparation method of guanidine polymer fungicides

Abstract

The invention discloses a preparation method of guanidine polymer fungicides. The preparation method includes that mass polymerization is adopted, and polymerization reaction is divided into two stages: prepolymerization and condensation; guanidine salt and endamine-based polymers are placed in a reaction kettle to be evenly mixed; the mass ratio of the guanidine salt to the endamine-based polymers is 1:10-1:1; under nitrogen protection, temperature is raised to 70-100DEG C for refluxing reaction in stirring, and guanidyl containing low polymers are obtained; polyamine small molecules are added to the reaction kettle to be evenly mixed; the mass ratio of the polyamine small molecules to the guanidine salt is 1:4-2:1; under nitrogen protection, temperature is raised to 120-200DEG C for refluxing reaction in stirring, and the guanidine polymers are obtained. The preparation method is simple in process and easy to implement and high in yield; the guanidine polymers contain a great deal of reactive amine on the basis of retaining fungicidal-group guanidyl, grafting to the surface of the product in the subsequent steps is facilitated, and the fungicides are good in practicability and application prospect.

Description

technical field

[0001] The invention belongs to the field of polymer bactericides, and in particular relates to a preparation method of guanidine polymer bactericides. Background technique

[0002] Bacteria are widely distributed in nature, and the diseases caused by bacterial transmission and infection have caused great troubles to people's healthy life. With the increasing awareness of safety, health and environmental protection, people put forward higher requirements for antibacterial materials. The current antibacterial materials can be divided into inorganic and organic in terms of structure and properties, and can be divided into anti-bacterial adhesion, contact sterilization and release sterilization in terms of antibacterial mechanism. Inorganic antibacterial materials mainly use silver, copper, zinc and other metals or their ions, and use the antibacterial ability of metal ions to achieve the purpose of sterilization and antibacterial through slow release. Among t...

Examples

Embodiment 1

[0025] Take 5g of guanidinium hydrochloride and 50g of polyethyleneimine (molecular weight: about 600), put them into a three-necked flask, mix well, under the protection of nitrogen, raise the temperature to 70°C, reflux under stirring for 2 hours, then add 1,6-hexanedi amine 2.5g, continue to heat up to 120 ℃ under the protection of nitrogen, stop after reflux reaction under stirring for 5 hours, obtain guanidine polymer, its molecular weight is about 1.2×10 4 , the minimum bactericidal concentration detected by the agar dilution method is 12ppm.

Embodiment 2

[0027] Take 5 g of guanidinium nitrate salt and 10 g of polyethyleneimine (molecular weight is about 1800), put them into a three-necked flask, mix well, under the protection of nitrogen, raise the temperature to 90 ° C, stir and reflux for 1 hour, then add 10 g of triethylenetetramine, Continue to heat up to 160°C under the protection of nitrogen, and stop the reflux reaction after stirring for 6 hours to obtain a guanidine polymer with a molecular weight of about 1.0×10 4 , using the agar dilution method to detect the minimum inhibitory concentration of 25ppm.

Embodiment 3

[0029] Take 5g of aminoguanidine hydrochloride and 25g of polyoxyethylene diamine (molecular weight about 1000), put them into a three-necked flask, mix well, under the protection of nitrogen, heat up to 100°C, reflux under stirring for 2 hours, then add trimethyl Hexamethylenediamine 5g, continue to heat up to 150 ℃ under the protection of nitrogen, stop after reflux reaction under stirring for 8 hours, obtain the polymer containing guanidine group, its molecular weight is about 2.2 * 10 4 , using the agar dilution method to detect the minimum inhibitory concentration of 45ppm.

technical field

[0001] The invention belongs to the field of polymer bactericides, and in particular relates to a preparation method of guanidine polymer bactericides. Background technique

[0002] Bacteria are widely distributed in nature, and the diseases caused by bacterial transmission and infection have caused great troubles to people's healthy life. With the increasing awareness of safety, health and environmental protection, people put forward higher requirements for antibacterial materials. The current antibacterial materials can be divided into inorganic and organic in terms of structure and properties, and can be divided into anti-bacterial adhesion, contact sterilization and release sterilization in terms of antibacterial mechanism. Inorganic antibacterial materials mainly use silver, copper, zinc and other metals or their ions, and use the antibacterial ability of metal ions to achieve the purpose of sterilization and antibacterial through slow release. Among t...

Examples

Embodiment 1

[0025] Take 5g of guanidinium hydrochloride and 50g of polyethyleneimine (molecular weight: about 600), put them into a three-necked flask, mix well, under the protection of nitrogen, raise the temperature to 70°C, reflux under stirring for 2 hours, then add 1,6-hexanedi amine 2.5g, continue to heat up to 120 ℃ under the protection of nitrogen, stop after reflux reaction under stirring for 5 hours, obtain guanidine polymer, its molecular weight is about 1.2×10 4 , the minimum bactericidal concentration detected by the agar dilution method is 12ppm.

Embodiment 2

[0027] Take 5 g of guanidinium nitrate salt and 10 g of polyethyleneimine (molecular weight is about 1800), put them into a three-necked flask, mix well, under the protection of nitrogen, raise the temperature to 90 ° C, stir and reflux for 1 hour, then add 10 g of triethylenetetramine, Continue to heat up to 160°C under the protection of nitrogen, and stop the reflux reaction after stirring for 6 hours to obtain a guanidine polymer with a molecular weight of about 1.0×10 4 , using the agar dilution method to detect the minimum inhibitory concentration of 25ppm.

Embodiment 3

[0029] Take 5g of aminoguanidine hydrochloride and 25g of polyoxyethylene diamine (molecular weight about 1000), put them into a three-necked flask, mix well, under the protection of nitrogen, heat up to 100°C, reflux under stirring for 2 hours, then add trimethyl Hexamethylenediamine 5g, continue to heat up to 150 ℃ under the protection of nitrogen, stop after reflux reaction under stirring for 8 hours, obtain the polymer containing guanidine group, its molecular weight is about 2.2 * 10 4 , using the agar dilution method to detect the minimum inhibitory concentration of 45ppm.

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