Preparation method of polyhexamethyleneguanidine hydrochloride

A technology of polyhexamethylene guanidine hydrochloride and guanidine hydrochloride, which is applied in the field of polymer preparation, can solve problems such as product quality impact, and achieve the effects of simplifying production process, improving product yield and being convenient to use.

Active Publication Date: 2016-08-03
HUNAN XUETIAN FINE CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this process, because polyethylene glycol and toluene-4-sulfonic acid do not participate in the polymerization reaction, they still remain in the solid product after the reaction, thus affecting the product quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Put the raw materials 1,6-hexamethylenediamine and guanidine hydrochloride into a three-necked flask, wherein the molar ratio of 1,6-hexamethylenediamine and guanidine hydrochloride is 1.05:1, raise the temperature of the material to 140°C for 6 hours, then raise the temperature to 190°C and then Reaction 2h. Cool the material, lower the material temperature to 150°C, add 15% sodium hydroxide solution in an equimolar ratio to 1,6-hexanediamine, and keep the temperature at 100°C for 2 hours. The aqueous solution of the lower layer was separated, and the upper layer of polyhexamethyleneguanidine was rinsed twice with deionized water. Dissolve the rinsed polyhexamethyleneguanidine with 15% hydrochloric acid, adjust the pH of the polyhexamethyleneguanidine hydrochloride solution to 6.5, and vacuum-dry the solution at 120°C to obtain a solid polyhexamethyleneguanidine hydrochloride product. The product has a purity of 96.7%, a yield of 92.3%, Mn=1105.9, Mw=1198.3.

Embodiment 2

[0036]Put the raw materials 1,6-hexamethylenediamine and guanidine hydrochloride into a three-neck flask, wherein the molar ratio of 1,6-hexamethylenediamine and guanidine hydrochloride is 1.05:1, raise the temperature of the material to 150°C for 5 hours, then raise the temperature to 185°C Reaction 3h. Cool the material, lower the material temperature to 150°C, add 15% sodium hydroxide solution in an equimolar ratio to 1,6-hexanediamine, and keep the temperature at 105°C for 2 hours. The aqueous solution of the lower layer was separated, and the upper layer of polyhexamethyleneguanidine was rinsed twice with deionized water. The rinsed polyhexamethyleneguanidine was dissolved with 15% hydrochloric acid, the pH of the polyhexamethyleneguanidine hydrochloride solution was adjusted to 6.5, and the solution was vacuum-dried at 120°C to obtain a solid polyhexamethyleneguanidine hydrochloride product. The product has a purity of 97.2%, a yield of 93.5%, Mn=1015.4, Mw=1156.7.

Embodiment 3

[0038] Put the raw materials 1,6-hexamethylenediamine and guanidine hydrochloride into a three-necked flask, wherein the molar ratio of 1,6-hexamethylenediamine and guanidine hydrochloride is 1.10:1, raise the temperature of the material to 140°C for 8 hours, then raise the temperature to 185°C Reaction 3h. Cool the material, lower the material temperature to 150°C, add 10% sodium hydroxide solution in an equimolar ratio to 1,6-hexanediamine, and keep the temperature at 100°C for 2 hours. The aqueous solution of the lower layer was separated, and the upper layer of polyhexamethyleneguanidine was rinsed twice with deionized water. The rinsed polyhexamethyleneguanidine was dissolved with 15% hydrochloric acid, the pH of the polyhexamethyleneguanidine hydrochloride solution was adjusted to 6.5, and the solution was vacuum-dried at 120°C to obtain a solid polyhexamethyleneguanidine hydrochloride product. Product purity 97.4%, yield 91.8%, Mn=997.3, Mw=1147.2.

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Abstract

The invention discloses a preparation method of polyhexamethyleneguanidine hydrochloride. The method comprises the following steps: (1) polycondensation reaction: adding raw materials guanidine hydrochloride and 1,6-hexamethylenediamine into a reactor, stirring and heating to react in two stages, wherein the reaction is carried out for 2-10 hours after the material temperature is raised to 130-150 DEG C in the first stage, and the reaction is carried out for 1-5 hours after the material temperature is raised to 185-195 DEG C in the second stage; (2) saponification reaction: lowering the material temperature to 140-160 DEG C, adding a sodium hydroxide solution to regulate the pH value to 12 or above, and after finishing adding the sodium hydroxide solution, keeping the temperature at 90-120 DEG C for 1 hour or above; (3) skimming and washing: separating out the lower water layer of the reaction solution, and washing the upper layer with water to obtain water-insoluble polyhexamethyleneguanidine; (4) salification: dissolving the polyhexamethyleneguanidine in a hydrochloric acid solution, and regulating the pH value of the solution to obtain the polyhexamethyleneguanidine hydrochloride water solution; and (5) drying: drying the water solution to obtain the high-purity polyhexamethyleneguanidine hydrochloride product. The method has the advantages of mild reaction conditions and simple preparation process. The purity of the obtained product is 96% or above, the yield can reach 90% or above, and the product is suitable for large-scale production and application.

Description

technical field [0001] The invention belongs to the technical field of polymer preparation, in particular to a preparation method of polyhexamethyleneguanidine hydrochloride. Background technique [0002] Polyhexamethyleneguanidine hydrochloride (PHMG) is a broad-spectrum antimicrobial agent. It is an environmentally friendly and multi-purpose new cationic polymer. It is easily soluble in water and its aqueous solution is colorless and odorless. Wide range of uses. The mechanism of its fungicide is: due to the high activity of the guanidine group, the polymer becomes positively charged, and is easily adsorbed by various bacteria and viruses that are usually negatively charged, thereby inhibiting the splitting function of bacteria and viruses, and making bacteria and viruses lose Reproductive ability, and polymeric organic guanidine concentrates multiple guanidine groups on the same molecule to strengthen this effect; at the same time, because it is a high molecular polymer,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/00
CPCC08G73/00
Inventor 曾平谢维跃魏盼中蒋健任立亚张浴沂阳亚玲许筠
Owner HUNAN XUETIAN FINE CHEM IND
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