* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Reference:
[1] Patent: CN105272886, 2016, A, . Location in patent: Paragraph 0008; 0027
2
[ 59572-10-0 ]
[ 6358-69-6 ]
Yield
Reaction Conditions
Operation in experiment
245 g
With sodium hydroxide In water for 5 h;
In 2000 ml three-necked flask into 1200 grams of concentrated sulfuric acid, stirring into the 120 grams of flowers, a little warming to promoteAfter all the dissolved, slowly warming to 90 ° C for 1 hour, three bottles with a water bath to cool below 40 ° C, drop the liquid sulfur black 480 grams, 3 hours drop finished. And then to maintain the temperature of about 100 ° C reaction for 5 hours, down to room temperature, the three bottles of material into the 720 grams of ice water, into a sticky material, filter dry filter cake, get pyrene tetrasulfonic acid tetrasodium salt. And then the pyrene tetrasulfonic acid tetrasodium salt dissolved in 1000 ml of water into the 2000 ml three-necked flask, stirring with a plate of sodium hydroxide to neutral, then add 300 grams of flaky sodium hydroxide, slowly warming To micro-boiling state for 5 hours. After cooling, the first with hydrochloric acid and PH value of 7 or so, then add 100 grams of sodium chloride stirring dissolved, slowly precipitated light yellow solid, filtered and dried to get 8-hydroxy-1,3, 6-pyrene three Sodium sulfonate salt about 245 grams.
Reference:
[1] Patent: CN105272886, 2016, A, . Location in patent: Paragraph 0013; 0026; 0027
In 2000 ml three-necked flask into 1200 grams of concentrated sulfuric acid, stirring into the 120 grams of flowers, a little warming to promoteAfter all the dissolved, slowly warming to 90 C for 1 hour, three bottles with a water bath to cool below 40 C, drop the liquid sulfur black 480 grams, 3 hours drop finished. And then to maintain the temperature of about 100 C reaction for 5 hours, down to room temperature, the three bottles of material into the 720 grams of ice water, into a sticky material, filter dry filter cake, get pyrene tetrasulfonic acid tetrasodium salt. And then the pyrene tetrasulfonic acid tetrasodium salt dissolved in 1000 ml of water into the 2000 ml three-necked flask, stirring with a plate of sodium hydroxide to neutral, then add 300 grams of flaky sodium hydroxide, slowly warming To micro-boiling state for 5 hours. After cooling, the first with hydrochloric acid and PH value of 7 or so, then add 100 grams of sodium chloride stirring dissolved, slowly precipitated light yellow solid, filtered and dried to get 8-hydroxy-1,3, 6-pyrene three Sodium sulfonate salt about 245 grams.
In 2000 ml three-necked flask into 1200 grams of concentrated sulfuric acid, stirring into the 120 grams of flowers, a little warming to promoteAfter all the dissolved, slowly warming to 90 C for 1 hour, three bottles with a water bath to cool below 40 C, drop the liquid sulfur black 480 grams, 3 hours drop finished. And then to maintain the temperature of about 100 C reaction for 5 hours, down to room temperature, the three bottles of material into the 720 grams of ice water, into a sticky material, filter dry filter cake, get pyrene tetrasulfonic acid tetrasodium salt. And then the pyrene tetrasulfonic acid tetrasodium salt dissolved in 1000 ml of water into the 2000 ml three-necked flask, stirring with a plate of sodium hydroxide to neutral, then add 300 grams of flaky sodium hydroxide, slowly warming To micro-boiling state for 5 hours. After cooling, the first with hydrochloric acid and PH value of 7 or so, then add 100 grams of sodium chloride stirring dissolved, slowly precipitated light yellow solid, filtered and dried to get 8-hydroxy-1,3, 6-pyrene three Sodium sulfonate salt about 245 grams.