* 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] Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 4, p. 148
[2] Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 4, p. 149
2
[ 91-20-3 ]
[ 6654-64-4 ]
[ 86-66-8 ]
[ 85-49-4 ]
Yield
Reaction Conditions
Operation in experiment
80%
at 65 - 150℃;
Sulfonation treatment: the liquid naphthalene and concentration of 100percent sulfuric acid solution was continuously added to the kettle sulfonated, sulfonated kettle temperature rose to 90 , for the first time sulfonated, after the first sulfonated products were continuously fed to the buffer tank indexable sulfonated column, the column transposition sulfonated temperature rose to 150 , conducted transfer reaction;The complete material transfer reaction mass concentration of 100percent sulfuric acid solution and the mass concentration of 65percent oleum sulfonation continuously fed to the reactor, the reactor temperature sulfonation was 65 , second sulfonated;And materials will be sent to the concentration after the second sulfonated completed 65percent oleum sulfonated three towers, three towers sulfonation the temperature rose to 150 , a third sulfonated, sulfonated generation, sulfonated sulfonated and into the buffer storage tank.Sulfonated as nitrification spare
80%
With sulfuric acid; sulfur trioxide In water at 65 - 150℃; Autoclave
When said device 1 is sulfonated, the liquid naphthalene and concentration of 100percent sulfuric acid solution was continuously added to the kettle 101 sulfonated, sulfonated kettle temperature of 101 90 , for the first time sulfonated. The product was first sulfonated after the buffer tank 102 are continuously fed to the tower 103 indexable sulfonation, sulfonation translocation temperature within the column 103 is 150 deg.] C, the reaction carried translocation. The complete material transfer reaction mass concentration of 100percent sulfuric acid solution and the mass concentration of 65percent fatOleum sulfonation continuously fed to the reactor 104, the internal temperature was 104 sulphonation reactor 65 , second sulfonation. It will be sent three times a sulfonated column 105, a temperature of 105 within three sulfonated tower 150 , a third sulfonated to produce sulfonated and sulfonated material was sent after the completion of the second and sulfonated oleum sulfonated into the buffer storage tank 106. Chemical reaction occurs in the sulfonated apparatus 1 is as follows:The above-described embodiment, the means 2 for generating nitrification nitrification. As a preferred option, such as, The nitrification device according to FIG. 12 comprises a nitration reactor 201, two nitrification tank202 and nitrites buffer tank 203, a nitrification reactor inlet and sulfonated buffer 201Tank outlet 106 is connected to an outlet 201 of the nitration reaction with the secondary nitrification tank 202Inlet connection, two nitrification and nitrification tank outlet buffer tank inlet 202 of 203 connections.
Reference:
[1] Patent: CN105669500, 2016, A, . Location in patent: Paragraph 0058; 0059; 0060; 0061; 0062
[2] Patent: CN105566171, 2016, A, . Location in patent: Paragraph 0025; 0026
[3] Patent: CN105693560, 2016, A, . Location in patent: Paragraph 0042; 0043; 0044; 0045; 0046
3
[ 120-18-3 ]
[ 6654-64-4 ]
[ 86-66-8 ]
[ 85-49-4 ]
Reference:
[1] Canadian Journal of Chemistry, 1983, vol. 61, p. 1453 - 1455
4
[ 131-27-1 ]
[ 6654-64-4 ]
Reference:
[1] Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 3, p. 420
[2] Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 3, p. 421
5
[ 91-20-3 ]
[ 5724-16-3 ]
[ 525-37-1 ]
[ 6654-64-4 ]
[ 81-04-9 ]
Reference:
[1] Recueil des Travaux Chimiques des Pays-Bas, 1994, vol. 113, # 9, p. 403 - 410
Reference:
[1] Recueil des Travaux Chimiques des Pays-Bas, 1994, vol. 113, # 9, p. 403 - 410
[2] Recueil des Travaux Chimiques des Pays-Bas, 1994, vol. 113, # 9, p. 403 - 410
[3] Recueil des Travaux Chimiques des Pays-Bas, 1994, vol. 113, # 9, p. 403 - 410
Synthesis of compound 4: Nitration of commercially available 2 (1 g) is according to the procedure described (for literature conditions see U.S. Pat. No. 4,534,905; Allison, F. et al. Helv. Chim. Acta 4:2139 (1952)).
The yield of naphthalene-1,3,5-trisulphonic acid is 82%, based on naphthalene.
EXAMPLE 3 The procedure is as in Example 1 except that the reaction mixture is stirred for 12 hours at 80 C. after adding 42 g of 65% oleum. The yield of naphthalene-1,3,5-trisulphonic acid was 80%, based on naphthalene.
EXAMPLE 5 The procedure is as in Example 4 except that 388 g of crude sulphonation reaction mixture and 350 g of 100% H2 SO4 are initially introduced into the separate flask and mixed. For the trisulphonation, the reaction mixture is stirred at 100 C. for 4 hours. 85% of the methylene chloride employed is recovered by decanting and 15% was recovered by distillation. The yield of naphthalene-1,3,5-trisulphonic acid is 81%, based on naphthalene.
The yield of naphthalene-1,3,5-trisulphonic acid is 68%, based on naphthalene.
16
[ 91-20-3 ]
[ 6654-64-4 ]
[ 86-66-8 ]
[ 85-49-4 ]
Yield
Reaction Conditions
Operation in experiment
6%; 80%; 13%
With sulfuric acid; sulfur trioxide; at 65 - 150℃;
Sulfonation treatment: the liquid naphthalene and concentration of 100% sulfuric acid solution was continuously added to the kettle sulfonated, sulfonated kettle temperature rose to 90 , for the first time sulfonated, after the first sulfonated products were continuously fed to the buffer tank indexable sulfonated column, the column transposition sulfonated temperature rose to 150 , conducted transfer reaction;The complete material transfer reaction mass concentration of 100% sulfuric acid solution and the mass concentration of 65% oleum sulfonation continuously fed to the reactor, the reactor temperature sulfonation was 65 , second sulfonated;And materials will be sent to the concentration after the second sulfonated completed 65% oleum sulfonated three towers, three towers sulfonation the temperature rose to 150 , a third sulfonated, sulfonated generation, sulfonated sulfonated and into the buffer storage tank.Sulfonated as nitrification spare
6%; 80%; 13%
With sulfuric acid; sulfur trioxide; In water; at 65 - 150℃;Autoclave;
When said device 1 is sulfonated, the liquid naphthalene and concentration of 100% sulfuric acid solution was continuously added to the kettle 101 sulfonated, sulfonated kettle temperature of 101 90 , for the first time sulfonated. The product was first sulfonated after the buffer tank 102 are continuously fed to the tower 103 indexable sulfonation, sulfonation translocation temperature within the column 103 is 150 deg.] C, the reaction carried translocation. The complete material transfer reaction mass concentration of 100% sulfuric acid solution and the mass concentration of 65% fatOleum sulfonation continuously fed to the reactor 104, the internal temperature was 104 sulphonation reactor 65 , second sulfonation. It will be sent three times a sulfonated column 105, a temperature of 105 within three sulfonated tower 150 , a third sulfonated to produce sulfonated and sulfonated material was sent after the completion of the second and sulfonated oleum sulfonated into the buffer storage tank 106. Chemical reaction occurs in the sulfonated apparatus 1 is as follows:The above-described embodiment, the means 2 for generating nitrification nitrification. As a preferred option, such as, The nitrification device according to FIG. 12 comprises a nitration reactor 201, two nitrification tank202 and nitrites buffer tank 203, a nitrification reactor inlet and sulfonated buffer 201Tank outlet 106 is connected to an outlet 201 of the nitration reaction with the secondary nitrification tank 202Inlet connection, two nitrification and nitrification tank outlet buffer tank inlet 202 of 203 connections.
With sulfuric acid; sulfur trioxide; at 65 - 150℃;
Continuously add liquidnaphthalene and 100% concentrated sulfuric acid solution into the sulfonationkettle. Raise the temperature of thesulfonation kettle to 90. Undergo firstsulfonation. The product after the firstsulfonation and after going through the buffer tank, is continuously fed to thetransposition sulfonation column. Raisethe temperature of the column to 150 and undergo transposition reaction; Continuously fed thematerial obtained after undergoing transposition reaction, the 100% concetratedsulfuric acid solution and the 65% concentrated fuming sulfuric acid into thesulfonation reactor. The temperatureinsude the sulfonation reactor is 65, undergo second sulfonation; Send the materialobtained after undergoing second sulfonation and the 65% concentrated fumingsulfuric acid to the third sulfonation tower.The tower's temperature is 150, undergo third sulfonation, producingthe sulfonated compound. Then, send thesulfonated compound to the sulfonated buffer tank. The stored sulfonated compound is the sparefor nitrification.