Process for preparing polysuccinimide derivatives-based microcapsules
A polysuccinimide, microcapsule technology, applied in microcapsule preparations, microsphere preparation, chemical instruments and methods, etc.
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Embodiment 1
[0274] Preparation of Polysuccinimide Derivatives
[0275] Preparation of polysuccinimide (PSI, 1)
[0276]
[0277] In a 250 mL beaker, orthophosphoric acid (10 g, 0.114 mmol) and L-aspartic acid (100 g, 751 mmol) were added separately and mixed in a mortar to obtain a white solid. The solid was heated under vacuum at 120° C. for 1 hour in a three-neck reactor. The solid was crushed in a mortar and heated at 200° C. under vacuum for 2 hours and 30 minutes. The obtained powder was washed 3 times with 500 mL of water, then with 30% by weight NaOH, and filtered to obtain an aqueous phase with a pH of 4. The solid was then dried under vacuum at 50°C for at least 24 hours.
[0278] Preparation of polysuccinimide-co-poly(n-dodecylsuccinamide) (2)
[0279]
[0280] In a 250 mL round bottom flask, 1 (15 g, 155 mmol of repeating unit) was dissolved in NMP (150 mL) and heated at 80 °C to obtain an orange-yellow solution. 1-Dodecylamine (DDA) (5, 10 or 20 mole % relative to...
Embodiment 2
[0289] Preparation of microcapsules according to the invention
[0290] Will N-100 (4.76 g, 24.5 mmol NCO) and acridine (0.25 g - compound added after deposition) were diluted into perfume oil (20.74 g, Table 2). Copolymer 2 or 3 (0.7 g) was diluted into an aqueous buffer solution at pH 7 (31.57 g). The oil and water phases were mixed together and then dispersed with an Ultra Turax at 24000 rpm for 3 minutes. The emulsion was put into a 250 mL glass jacketed reactor and stirred at 350 rpm at room temperature. A solution of guanidine carbonate (24.5 mmol) in pH 7 buffered aqueous solution (10.85 g) was added dropwise to the emulsion for 1 hour. Then, the temperature of the reaction mixture was slowly raised from room temperature to 70°C in 4 times of 15 minutes each (room temperature; 40°C; 50°C; 60°C; 70°C) and then kept at 70°C for 2 hours. Finally, the stirring speed was reduced to 100 rpm, and the dispersion was cooled to room temperature.
[0291] Table 2: Compositio...
Embodiment 3
[0298] Preparation of comparative microcapsules X
[0299] A solution of poly(vinyl alcohol) in water (45 g, 0.5% by weight, Mowiol 18-88, source: Aldrich, Switzerland) was introduced into the beaker. Perfume oil A (see Table 1, 38g) and polyisocyanate (0.27g, D-110N, source: Mitsui Chemicals, Japan) was introduced into the beaker. The reaction mixture was stirred with an UltraTurrax at 24,000 rpm for 2 minutes at room temperature (RT). A solution of guanidine carbonate (0.88 g, source: Aldrich, Switzerland) in water (4 g) was added dropwise with a syringe pump within 1 hour at room temperature. The resulting emulsion was warmed to 70°C over the course of 1 hour. The temperature was maintained at 70° C. for 2 hours and then cooled to room temperature to obtain a white dispersion (pH=9.7).
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