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

Active Publication Date: 2016-02-10
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

[0013] After HPLC analysis, it is found that the impurity content is relatively high, which shows that the coating is brittle and dark in electroplating applications; secondly, the high impurity content has a greater impact on the color of the product, which means that the produced product is darker and lighter than foreign products. Yellow to yellow; the products produced according to the above method are prone to discoloration after being placed for a long time, showing red / yellow; in the above scheme, the amount of pyridine is large and recovery is difficult, resulting in serious waste of raw materials
[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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  • A kind of synthetic method of hydroxypropanesulfonic acid pyridinium salt
  • A kind of synthetic method of hydroxypropanesulfonic acid pyridinium salt
  • A kind of synthetic method of hydroxypropanesulfonic acid pyridinium salt

Examples

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Effect test

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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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] Hydroxypropanesulfonic acid pyridinium salt is an electroplating intermediate, the pure product is a white crystal, and the common one is a colorless to light yellow liquid product with a content of 40%-50% and a pH value of 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 (P...

Claims

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Application Information

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Patent Type & Authority Patents(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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