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Process for producing sulfinate with low content exogenous salt

A sulfinate, low-content technology, applied in the electrolysis process, electrolysis components, etc., can solve the problems of separation, difficulty in zinc salt, etc., and achieve the effect of inhibiting the formation of by-products

Inactive Publication Date: 2005-07-13
BASF AG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the known preparation methods have the disadvantage that the obtained sulfinate solution contains substances formed during the preparation
Zinc salts are often difficult to remove by filtration, which makes them difficult to separate during the separation of the resulting sulfinate from dithionite

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Reaction of crystalline sodium dithionite containing exotic salts with formalin solution to form NaHMS

[0039]In a stirred tank, 880 g of 88% crystalline sodium dithionite (BASF AGHydrosulfite, the balance of foreign salts), ie 4.5 moles of sodium dithionite, was dissolved in about 3.6 L of water. At room temperature, 4.5 moles of formaldehyde (30% (w / w) in formalin) were added over 20 minutes while stirring. After the addition of 4.3 molar NaOH, sodium dithionite had been converted quantitatively (on-line UV spectroscopy) and the pH of the solution was 9.7. A total of 4.31 moles of NaHMS were formed. The corresponding NaHMS yield was 95%, based on the dithionite initially charged.

Embodiment 2

[0041] Sodium dithionite solution (electrolysis effluent) containing foreign salts reacts with formalin solution to form HMS

[0042] Add 2.24 moles of sodium dithionite and 0.6 moles of foreign salts (NaHSO 3 , Na 2 SO 3 ) of electrolytic wastewater. Add 50% NaOH to adjust the pH to pH>8 and pH<10. Then 2.3 moles of formaldehyde (30% (w / w) in formalin) were added over 20 minutes at room temperature while stirring. The final pH was adjusted to pH=11.5 by adding 50% (w / w) NaOH. Sodium dithionite has been converted quantitatively after addition (online UV spectroscopy). In total 2.21 moles of NaHMS were formed. The corresponding NaHMS yield was 98%, based on the initially charged dithionite.

Embodiment 3

[0044] Electrodialysis of NaHMS aqueous solution containing foreign salts

[0045] In the electrodialysis cell (Osmota100, 5 pairs of cells, the electrodes are composed of RA2 and expanded metal titanium, and the electrolyte is 5% (w / w) Na 2 CO 3 , cation exchanger CMX, anion exchanger ASV, film CMB) add the reaction solution to be purified, wherein in the dilution circuit contains 89g / L NaHMS and 116g / L NaHMS 2 SO 3 . At the start of the run, the product loop contained a very dilute salt solution (5.6 g / L NaHMS and 10.6 g / L NaHMS 2 SO 3 ). A current of I = 1.81 A was applied at T = 35°C while circulating both circuits through the pump. After the run, the following concentrations were present in the dilution loop: 5.4 g / L NaHMS and 120 g / L NaHMS 2 SO 3 . Concentrations in the product loop are 94g / L NaHMS and 27.3g / L NaHMS 2 SO 3 .

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PUM

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Abstract

The present invention relates to a process for the preparation of sulfinate salts with low levels of foreign salts by reducing alkali metal or alkaline earth metal or ammonium dithionite salts using carbonyl compounds or imines at pH > 6. The molar ratio of dithionite to carbonyl or imine compound is preferably in the range of 0.75-1.3. The present method provides a sulfinate product with low levels of foreign salts. If desired, the foreign salts formed can be further removed using conventional techniques. The method is particularly useful for the preparation of hydroxymethyl sulfinate.

Description

field of invention [0001] The present invention relates to a process for the preparation of sulfinates with a low content of extraneous salts by reducing dithionites of alkali metals or alkaline earth metals or ammonium with carbonyl compounds or imine compounds at pH > 6. By maintaining a specific concentration ratio between the reactants, a product with a low content of foreign salts can be obtained, and the foreign salts can further be easily removed by conventional methods. Background technique [0002] Sulfinates are widely used in industry as reducing agents and as free radical generators. Examples include dyeing and dye-stripping operations, and polyaddition reactions. [0003] Sulfinates are usually prepared by reacting dithionite with an aldehyde in the presence of a base. However, the known preparation methods have the disadvantage that the obtained sulfinate solutions contain substances formed during the preparation. Usually, these solutions are sold without...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C313/04C25B1/22
CPCC07C313/04
Inventor H·伯恩克J·弗朗克H·普特尔H·舍林R·施耐德S·塔特
Owner BASF AG
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