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Production method of high-purity PPS-OH

A technology of pure hydroxypropane sulfonate pyridinium salt and hydroxypropane sulfonate pyridinium salt, which is applied in the production field of high-purity hydroxypropane sulfonate pyridinium salt, can solve the problem of unfavorable transportation and increase of hydroxypropane sulfonate pyridinium salt solution Difficulty in handling Plating parts are brittle and affect the brightness of the nickel layer, etc.

Inactive Publication Date: 2012-06-13
ZHUZHOU TIMES ELECTRIC INSULATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] One is that there is a small amount of pyridine remaining in the solution, and pyridine makes the coating black in the low current area, and the brittleness of the coating increases at the same time;
[0007] Second, there is a large amount of sodium chloride remaining in the solution, and the presence of sodium ions affects the brightness of the nickel layer, and increases the difficulty of post-treatment of the nickel plating solution and the brittleness of the plated parts;
[0008] The third is that the resulting hydroxypropanesulfonate pyridinium salt solution is not conducive to transportation

Method used

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  • Production method of high-purity PPS-OH
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  • Production method of high-purity PPS-OH

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Example 1: Add 50ml of water, 0.153mol of sodium 3-chloro-2-hydroxypropanesulfonate into a three-necked flask, then drop in 0.304mol of pyridine (1:2), raise the temperature to 94~102°C, keep warm and reflux for 5~10 Hour. After the reaction is complete, pyridine and water are removed under reduced pressure at 80-85°C to obtain a white solid. Add 1.59 mol of formic acid (1:10) to the white solid, filter with suction, add 0.99 mol of methanol (1:6.47) to the obtained filtrate, a large number of crystals are precipitated, filter with suction, and dry in vacuum to obtain high-purity pyridine hydroxypropanesulfonate The onium salt is 0.138mol, the yield is 90%, the sodium chloride content is 0.9%, and the infrared is shown in the accompanying drawing.

[0019] 1 HNMR (D 2 O, 600 MHz): δ 8.806 (d, 2 H, aromatic ring H), 8.544 (t, 1H, aromatic ring H), 8.044 (2H, aromatic ring H), 4.905 (d, OH), 4.471~4.586 ( t, 2H, CH2), 3.185 (t, 2H, CH2), 2.161 (s, 1H, CH).

[0020] ...

Embodiment 2

[0022] Example 2: Add 60ml of water, 0.153mol of sodium 3-chloro-2-hydroxypropanesulfonate into a three-necked flask, then drop in 0.158mol of pyridine (1:1), raise the temperature to 94~102°C, keep warm and reflux for 5~10 Hour. After the reaction is complete, pyridine and water are removed under reduced pressure at 80-85°C to obtain a white solid. Add 2.55m0l of acetic acid (1:17) to the white solid, filter with suction, add 0.71mol of ethanol (1:4.64) to the obtained filtrate, a large amount of crystals are precipitated, filter with suction, and dry in vacuum to obtain high-purity pyridine hydroxypropanesulfonate The onium salt is 0.12mol, the yield is 78.6%, and the sodium chloride content is 0.9%. The infrared is shown in the accompanying drawing.

[0023] 1 HNMR (D 2 O, 600 MHz): δ 8.806 (d, 2 H, aromatic ring H), 8.544 (t, 1H, aromatic ring H), 8.044 (t, 2H, aromatic ring H), 4.905 (d, OH), 4.471~ 4.586 (t, 2H, CH2), 3.185 (t, 2H, CH2), 2.161 (s, 1H, CH2).

[0024]...

Embodiment 3

[0026] Example 3: Add 60ml of water and 0.153mol of sodium 3-chloro-2-hydroxypropanesulfonate into a three-necked flask, then drop in 0.757 (1:4.95)mol of pyridine, raise the temperature to 94-102°C, keep warm and reflux for 5-10 Hour. After the reaction was completed, pyridine and water were removed under reduced pressure at 80-85°C to obtain a white solid. Add 0.78 mol of DMF (1:5) to the white solid, filter with suction, add 0.52 mol of propanol (1:3.39) to the obtained filtrate, a large number of crystals are precipitated, filter with suction, and dry in vacuum to obtain high-purity hydroxypropanesulfonic acid The pyridinium salt is 0.127mol, the yield is 83%, the sodium chloride content is 0.9%, and the infrared is shown in the accompanying drawing.

[0027] 1 HNMR (D 2 O, 600 MHz): δ 8.806 (d, 2 H, aromatic ring H), 8.544 (t, 1H, aromatic ring H), 8.044 (t, 2H, aromatic ring H), 4.905 (d, OH), 4.471~ 4.586 (t, 2H, CH2), 3.185 (t, 2H, CH2), 2.161 (s, 1H, CH2).

[002...

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Abstract

The invention discloses a production method of high-purity PPS-OH. The production method of the high-purity PPS-OH comprises the following steps of dropwisely adding pyridine into a sodium 3-chloro-2-hydroxypropanesulfonate aqueous solution, carrying out a reflux reaction process for multiple hours, removing the pyridine and water by pressure reduction, carrying out drying to obtain white solids, dissolving the white solids in one or more organic solvents, filtering to remove inorganic salts, adding one or more organic solvents into the filtrate, filtering, and drying to obtain the high-purity PPS-OH. The PPS-OH obtained by the production method has high purity, is convenient for transportation, has low common salt content, does not contain pyridine and has good electroplating effects.

Description

technical field [0001] The invention relates to a production method of onium salt, in particular to a production method of high-purity hydroxypropanesulfonic acid pyridinium salt. Background technique [0002] Pyridinium hydroxypropanesulfonate (PPS-OH) is a white crystalline powder, CAS: 3918-73-8, molecular formula C 8 h 11 NO 4 S, molecular weight: 217.23, belongs to pyridine derivatives, is one of the main products of nickel plating intermediates, and has strong brightening and leveling effects. The most common and widely used in nickel plating process is bright nickel plating solution. Nickel plating can provide devices with a flat and glossy coating. Therefore, device processing can be continuously produced, production cost can be reduced, and labor productivity can be improved. Hydroxypropane sulfonate pyridinium salt is used as a high-efficiency bright additive and powerful leveling agent in the plating solution, which makes the coating uniformity good in elec...

Claims

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Application Information

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IPC IPC(8): C07D213/20
Inventor 刘含茂周升
Owner ZHUZHOU TIMES ELECTRIC INSULATION
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