A kind of reactive weak base variable color azo-anthraquinone pH probe and its preparation and application
An anthraquinone and probe technology, applied to pH probes and their preparation and application fields, can solve the problems of insensitive response, high equipment requirements, poor wet handling fastness, etc., and achieves simple preparation process, low cost, color rich effects
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Embodiment 1
[0054] The synthesis process of the azo-anthraquinone pH probe with the following structure:
[0055]
[0056](1) Preparation of a condensate: 18.6g (0.1mol) of cyanuric chloride was prepared into a 20% (mass percent concentration) solution, and was beaten in an ice-water bath at 0-2°C for 0.5h. Accurately weigh 52.61g (0.099mol) of 1-amino-2-sulfonic acid-4-(3-amino-2,4,6-trimethyl-5-sulfonic acid phenylamino)anthraquinone monosodium salt to prepare 15 % solution, adjust the pH value to 5.8-6.5, and the dissolving solution is a blue clear solution, and add it dropwise to the uniformly beaten cyanuric chloride within 1 hour at 0-5°C, and keep the temperature at 5°C after the dropwise addition is completed. React for 3 hours with a pH value of 4-4.5, and detect the end point of the shrinkage reaction by thin-layer chromatography (developing solvent: n-butanol: ethanol: water = 8:2:3).
[0057] (2) Preparation of the dicondensate: Accurately weigh 23.44g (0.098mol) J acid dr...
Embodiment 2
[0063] The synthesis process of the azo-anthraquinone pH probe with the following structure:
[0064]
[0065] (1) Preparation of a condensate: 18.6g (0.1mol) of cyanuric chloride was prepared into a 20% (mass percent concentration) solution, and was beaten in an ice-water bath at 0-2°C for 0.5h. Accurately weigh 52.61g (0.099mol) of 1-amino-2-sulfonic acid-4-(3-amino-2,4,6-trimethyl-5-sulfonic acid phenylamino)anthraquinone monosodium salt to prepare 15 % solution, adjust the pH value to 5.8-6.5, and the dissolving solution is a blue clear solution, and add it dropwise to the uniformly beaten cyanuric chloride within 1 hour at 0-5°C, and keep the temperature at 5°C after the dropwise addition is completed. React for 3 hours with a pH value of 4-4.5, and detect the end point of the shrinkage reaction by thin-layer chromatography (developing solvent: n-butanol: ethanol: water = 8:2:3).
[0066] (2) Preparation of the dicondensate: Accurately weigh 23.44g (0.098mol) J acid d...
Embodiment 3
[0072] The synthesis process of the azo-anthraquinone pH probe with the following structure:
[0073]
[0074] (1) Preparation of a condensate: 18.6g (0.1mol) of cyanuric chloride was configured into a 20% solution, and beat in an ice-water bath for 0.5h at 0-2°C. Accurately weigh 52.61g (0.099mol) of 1-amino-2-sulfonic acid-4-(3-amino-2,4,6-trimethyl-5-sulfonic acid phenylamino)anthraquinone monosodium salt to prepare 15 % solution, adjust the pH value to 5.8-6.5, and the dissolving solution is a blue clear solution, and add it dropwise to the uniformly beaten cyanuric chloride within 1 hour at 0-5°C, and keep the temperature at 5°C after the dropwise addition is completed. React for 3 hours with a pH value of 4-4.5, and detect the end point of the shrinkage reaction by thin-layer chromatography (developing solvent: n-butanol: ethanol: water = 8:2:3).
[0075] (2) Preparation of the dicondensate: Accurately weigh 23.44g (0.098mol) J acid dry powder, adjust the pH value of...
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