반응식
[Na+].[Na+].[N+:3]([C:6]1[CH:7]=[C:8]([S:27]([O-:30])(=[O:29])=[O:28])[C:9]([CH:12]=[CH:13][C:14]2[C:15]([S:23]([O-:26])(=[O:25])=[O:24])=[CH:16][C:17]([N+:20]([O-:22])=[O:21])=[CH:18][CH:19]=2)=[CH:10][CH:11]=1)([O-:5])=[O:4]>O>[N+:20]([C:17]1[CH:16]=[C:15]([S:23]([OH:26])(=[O:25])=[O:24])[C:14]([CH:13]=[CH:12][C:9]2[C:8]([S:27]([OH:30])(=[O:29])=[O:28])=[CH:7][C:6]([N+:3]([O-:5])=[O:4])=[CH:11][CH:10]=2)=[CH:19][CH:18]=1)([O-:22])=[O:21]참가 물질
실험 절차
Solid 4,4′-dinitro-2,2′-stilbenedisulfonic acid disodium salt (2550 parts) is dissolved in hot water to produce a nominal 8% w/w solution (7.8-8.2% expressed as 4,4′-dinitro-2,2′-stilbenedisulfonic acid). Then 2375 parts of 50% sodium hydroxide solution is added. The temperature of the solution is adjusted to 60-62° C. A self-condensation reaction is carried out in a pH range from about 11 to 13 and in the temperature range from 60 to 65° C. by the addition in equal increments over 2 hours of 700 parts of 93% paraformaldehyde. After the condensation is complete, the reaction mixture is then acidified with 90-96% sulfuric acid. For convenience half the reaction mass is fed to an extraction vessel containing methyl isobutyl ketone (12,850 parts) and triisooctylamine (11,600 parts) which is preheated to 55-60° C. The neutralized dye slurry is fed concurrently with concentrated sulfuric acid (1600 parts) to the extraction solvents with agitation. The vessel contents thus achieve a temperature of 65-80° C. After 15 minutes, the agitation is stopped and the phases separate immediately.
출처 및 근거
- ORD 기록
- ord-a9c144a4427945c7b1a542a6ce9f316c
- 출처 데이터셋
- uspto-grants-2002_12
- 특허 번호
- US06491731B1
연결된 노트
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