Reaction #433584

ord-0423e525c6e84d15bca13a31ff875520

Reaction equation

Cl.N=C(N)N
guanidine hydrochloride
NCCCCCCN
hexamethylene diamine
CCCCN=C(N)NCCCC
polyhexamethyleneguanidine

Solvents

Conditions

Temperature
120°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Temperaturewas then raised to 150–170° C. for a further 5 hours
  2. 2
    TemperatureThe mixture was cooled to 80° C.
  3. 3
    Temperaturemaintaining the temperature at 80° C.
  4. 4
    workup.DISSOLUTIONuntil dissolution
  5. 5
    TemperatureThe mixture was then cooled

Procedure

A mixture of guanidine hydrochloride (200 parts) and hexamethylene diamine (292 parts) were heated to 120° C. for 4 hours under a nitrogen atmosphere The temperature was then raised to 150–170° C. for a further 5 hours. The mixture was cooled to 80° C. and water (400 parts) was added, maintaining the temperature at 80° C. until dissolution occurred. The mixture was then cooled to give a solution in water of polyhexamethyleneguanidine, referred to as Prepolymer 1, having a weight average molecular weight (Mw) of 1010 and a number average molecular weight (Mn) of 710, as determined by aqueous gel permeation chromatography.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07172274B2uspto-grants-2007_02