Synthetic method of pyridinium hydroxy propyl sulfobetaine

A technology of hydroxypropane sulfonate pyridinium salt and hydroxypropane sulfonate, which is applied in the field of preparation of nickel-plating intermediate hydroxypropane sulfonate pyridinium salt, can solve problems such as difficulty in producing high-end refined products, and avoid product Effects of discoloration, accelerated reaction rate, and improved conversion rate

Active Publication Date: 2014-07-16
湖北吉和昌化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] Today, as the nickel plating industry develops more and more refined, it is difficult to produce high-end refined products that can meet the needs of the industry through the above synthetic routes

Method used

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  • Synthetic method of pyridinium hydroxy propyl sulfobetaine
  • Synthetic method of pyridinium hydroxy propyl sulfobetaine
  • Synthetic method of pyridinium hydroxy propyl sulfobetaine

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0036] Add deionized water (335g, 18.59mol) and sodium metabisulfite (97g, 0.51mol) to a 500ml four-necked flask with a mechanical stirrer, 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 (polymer of allyl alcohol and ethylene oxide, propylene oxide), citric acid 0.0028g . After the system is heated up 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 1...

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. , 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 (namely: 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 (147.66g, 1.86mol) at the end of the heat preservation reaction, and raise the temperature to 95-105°C for reflux reaction, and add 11.07g of impurity remover triethylamine at the end of reflux. Afte...

example 3

[0042] Add 1600kg of deionized water into the 3000L standard reaction kettle, put in sodium metabisulfite (500Kg, 2.63kmol) under stirring to dissolve, 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. Raise the temperature to 60-70°C and pass through nitrogen protection, slowly add epichlorohydrin (470kg, 5.07kmol) dropwise, at this time the heat release is 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 DEG C of reflux reaction for 14 hours, add 18.75kg of impurity remover triethylamine. 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-tetramethylpiperidi...

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Abstract

The invention relates to a synthetic method of pyridinium hydroxy propyl sulfobetaine. The synthetic method comprises the following steps: sufficiently dissolving hydrosulphite or pyrosulfite in water at normal temperature, adding sodium sulfite as an auxiliary sulfonating agent to adjust the pH value of the system to be 5.2-5.5, and then adding polyether F-6 as a catalyst; then adding a complexing agent, controlling the environment conditions, adding epichlorohydrin, and carrying out loop-opening reaction to obtain 3-chloro-2-hydroxy propanesulfonate; adding pyridine to the system, controlling the temperature to carry out reflux reaction, adding triethylamine as an impurity removing agent, reacting for 1 hour, then dehydrating and decoloring, adjusting the pH to 2-5, and adding 4-hydroxyl-2, 2, 6, 6-tetramentylniperidine-1-oxygen radical as a stabilizer and a vitamin C derivative to obtain an aqueous solution of the pyridinium hydroxy propyl sulfobetaine. The pyridinium hydroxy propyl sulfobetaine synthesized by the synthetic method is produced by adopting a one-pot method, which accords with the electroplating industry development demands at present; the pyridinium hydroxy propyl sulfobetaine is low in impurity content, good in appearance and low in production cost.

Description

technical field [0001] The invention belongs to a new method for preparing nickel-plating intermediate hydroxypropanesulfonic acid pyridinium salt, which is an electroplating additive with bright and excellent leveling performance in the high current density area. Background technique [0002] Hydroxypropane sulfonate pyridinium salt is an electroplating intermediate, the pure product is white crystal, the common colorless to pale yellow liquid product with content between 40%-50% and pH value between 3-5. CAS number: 3918-73-8, molecular formula: C 8 h 11 NaO 4 S, molecular weight: 217.24. [0003] Pyridinium hydroxypropanesulfonate (PPS-OH) has excellent brightening and leveling effects in nickel plating, especially in high current density areas. As a basic additive in the nickel plating bath, its consumption is 20-50g / kAH, and the dosage is 50-500mg / L, and the market demand is large. At present, the liquid products of pyridinium hydroxypropanesulfonate (PPS-OH) are o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/04
CPCC07D213/04
Inventor 高成杨威黄开伟陈彰评周世骏宋文超
Owner 湖北吉和昌化工科技有限公司
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