A kind of synthetic method of hydroxypropanesulfonic acid pyridinium salt
A technology of hydroxypropane sulfonate pyridinium salt and hydroxypropane sulfonate, which is applied in the field of nickel plating intermediate hydroxypropane sulfonate pyridinium salt, can solve the problem that it is difficult to produce high-end refined products, and the product color has a great influence , waste of production raw materials and other issues, to achieve the effect of avoiding product discoloration, improving application effect and reducing product cost
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example 1
[0036] Add deionized water (335g, 18.59mol) and sodium pyrosulfite (97g, 0.51mol) to a 500ml four-necked flask with mechanical stirring, a thermometer, a reflux condenser, and a constant pressure dropping funnel, and stir thoroughly to dissolve it. , add auxiliary sulfonating agent sodium sulfite (11.57g, 0.091mol) to adjust the pH of the system to 5.5, add 0.2552g catalyst polyether F-6 (allyl alcohol and ethylene oxide, propylene oxide polymer), citric acid 0.0028g . After the system is heated to 60-65°C, nitrogen protection is introduced, and epichlorohydrin (92.31g, 1.0mol) is slowly added dropwise, and the dropping temperature is controlled to be between 60-65°C. The heat preservation reaction was carried out for 4 hours, and then the temperature was raised to 70-75° C. for 1 hour heat preservation reaction. At the end of the heat preservation reaction, pyridine (73.77 g, 0.93 mol) was added, and the temperature was raised to 90-105° C. for reflux reaction for 10 hours. ...
example 2
[0039]Add deionized water (775g, 43mol) and sodium pyrosulfite (194.20g, 1.02mol) to a 2000ml four-necked flask with mechanical stirring, a thermometer, a reflux condenser, and a constant pressure dropping funnel, and fully stir to dissolve it. , add auxiliary sulfonating agent sodium sulfite (20.42g, 0.162mol) to adjust the pH value of the system to 5.35, add 0.933g catalyst polyether F-6 (ie: allyl alcohol and ethylene oxide, propylene oxide polymer), complex Mixture citric acid 0.058g. After the temperature of the system was raised to 65-70° C., nitrogen protection was introduced, and epichlorohydrin (185.07 g, 2.0 mol) was slowly added dropwise. After the dropwise addition is completed, the temperature is kept at 65-70°C for 3 hours, and then the temperature is raised to 75-80°C for 1 hour. Add pyridine (147.66 g, 1.86 mol) after the heat preservation reaction, and heat up to 95-105° C. for reflux reaction, and add 11.07 g of impurity remover triethylamine at the end of r...
example 3
[0042] Add 1600kg of deionized water to a 3000L standard reaction kettle, add sodium metabisulfite (500Kg, 2.63kmol) under stirring, add sodium sulfite (38kg, 0.3kmol) to adjust the pH value to 5.35, add catalyst 2.06kg polyether F-6 (ie : allyl alcohol and ethylene oxide, propylene oxide polymer), complexing agent citric acid 0.15kg. The temperature was raised to 60-70° C. and nitrogen protection was introduced, and epichlorohydrin (470 kg, 5.07 kmol) was slowly added dropwise, at which time the heat release was obvious. After the dropwise addition, the temperature was controlled at 65-70°C for 4 hours, and then the temperature was raised to 80-90°C for 1 hour. After the reaction, pyridine (375kg, 4.74kmol) was added. After heating up to 100-110° C. for reflux reaction for 14 hours, 18.75 kg of impurity remover triethylamine was added. After dehydration and decolorization, adjust the pH value to 3.5 with hydrochloric acid, add 5.88kg of stabilizer 4-hydroxy-2,2,6,6-tetrameth...
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