Sulfuric Acid → Ammonium Persulfate

温度

60 °C

The following materials were added to a 500 ml. reaction flask: 40.7 g D.I. water, 0.1 g Versene 220, 0.01 g 93% sulfuric acid and 0.04 g iron sulfate-heptahydrate (Mixture 1). The flask was equipped with a reaction flask head, reflux condenser and agitator. Then a second mixture of 80 g D.I. water, 0.6 g Versene 220, 5.17 g of 58% NaAMPS, 5.1 g Sipex EST-30, 5.4 g Igepal CA-887, 0.15 g 93% sulfuric acid, 1.5 g Potomac Yellow Dye, 0.44 g Rhodamine F5G, and 0.22 g Rhodamine F3B were added to a second container. Both mixtures were purged for 30 minutes with nitrogen to remove residual oxygen. Next 60 g of Styrene, 27 g of Acrylonitrile, and 10 g of Hydroxypropylmethacrylate were added to the second mixture and the resulting mixture was agitated to form a stable preemulsion. Mixture I was then heated to 60° C. using a temperature controlled water bath. Ammonium Persulfate (0.6 g of APS in 3.6 g of D.I. water) and Erythorbic acid (0.93 g of EA in 3.8 g D.I. water) initiator solutions were prepared and 1/3 of each solution was added to mixture 1. Mixture 2 and the remaining 2/3 of the initiator solutions were then pumped into the reactor containing Mixture I at such a rate as to maintain the temperature of Mixture I at 60° C. without using additional heating. When the addition was complete, the polymer emulsion was heated for an additional 1 hr. and the post polymerization monomer reduction step was begun. t-Butylhydroperoxide (0.25 g t-BHP in 1.75 g D.I. water) and Erythorbic acid (0.34 g EA in 2.0 g D.I. water) solutions were then added to the emulsion polymer. The temperature was maintained at 60° C. for an additional hour. The resulting orange fluorescent dispersion possessed excellent color strength, shade and brightness.

1. additionThe following materials were added to a 500 ml
2. customreaction flask
3. customThe flask was equipped with a reaction flask head
4. temperaturereflux condenser
5. additionThen a second mixture of 80 g D.I
6. customBoth mixtures were purged for 30 minutes with nitrogen
7. customto remove residual oxygen
8. additionNext 60 g of Styrene, 27 g of Acrylonitrile, and 10 g of Hydroxypropylmethacrylate were added to the second mixture
9. customto form a stable preemulsion
10. additioncontaining Mixture I at such a rate as
11. temperatureto maintain the temperature of Mixture I at 60° C.
12. additionWhen the addition
13. temperaturethe polymer emulsion was heated for an additional 1 hr
14. customand the post polymerization monomer reduction step
15. temperatureThe temperature was maintained at 60° C. for an additional hour

ORDレコード

ord-aefa65e78007486892f44256ac4d9e49

出典データセット

uspto-grants-1994_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05294664