Method of extracting ortho-vanilin and iso-vanilin from aqueous solutions

FIELD: chemistry.

SUBSTANCE: invention relates to a method of extracting ortho-vanilin and iso-vanilin from aqueous solutions. The method involves addition of a salting-out agent - sodium chloride to aqueous solutions of ortho-vanilin and iso-vanilin and a solution of polyvinyl caprolactam prepared beforehand, having concentration of 5-15 wt % until achieving 34-35 wt % content of salt in the solution, with volume ratio of the aqueous phase to organic phase equal to 10:1. The organic phase is extracted and separated, analysed spectrophotometrically and the recovery ratio (R, %) of ortho-vanilin and iso-vanilin is calculated using the formula: R=DĚ100/(D+r), where D is coefficient of distribution of ortho-vanilin and iso-vanilin between the solution of polyvinyl caprolactam and the aqueous solution, r is the ratio of equilibrium volumes of the aqueous and organic phases.

EFFECT: method increases recovery ratio of ortho-vanilin and iso-vanilin from aqueous solutions.

1 tbl, 2 ex

 

The invention relates to analytical chemistry of organic compounds and can be used to extract ortho-vanillin and ISO-vanillin from aqueous solutions.

The closest in technical essence and the achieved effect is the method of extraction of ortho-vanillin and ISO-vanillin from aqueous solutions [Aigurande. The distribution coefficients of organic compounds. - Voronezh: Publishing house of Voronezh state University, 1992. - 336 S.].

An object of the invention is to develop a way to extract ortho-vanillin and ISO-vanillin from aqueous solutions of non-toxic hydrophilic polymer (polyvinylcaprolactam).

The disadvantage of this method is the low degree of extraction of ortho-vanillin and ISO-vanillin from aqueous media, and the use of toxic extractants for retrieval.

For the technical solution of the invention, a method for extraction of ortho-vanillin and ISO-vanillin from aqueous solutions, characterized by the fact that aqueous solutions of ortho-vanillin and ISO-vanillin add visivel - sodium chloride to the salt content in the solution 34-35 wt.% and pre-prepared solution of polyvinylcaprolactam with a concentration of 5-15 wt.%, when a volume ratio of water-salt and organic phases and 10:1, extracted within 20-30 minutes, the organic phase is separated and analyze the spectrum of the photometrically, the distribution coefficient is found by calibration curve, the degree of recovery (R %) of ortho-vanillin and ISO-vanillin calculated by the formula:

R=DĚ100/(D+r),

where D is the distribution coefficient of ortho-vanillin and ISO-vanillin between the solution of polyvinylcaprolactam and water solution, r is the ratio of the equilibrium volumes of aqueous and organic phases.

The technical result is to increase the degree of extraction of ortho-vanillin and ISO-vanillin in aqueous solution, saturated sodium chloride solution polyvinylcaprolactam.

The proposed method of extraction of ortho-vanillin and ISO-vanillin from aqueous solutions is as follows.

To analyze aqueous solution of ortho-vanillin and ISO-vanillin add visivel crystalline sodium chloride to the salt content in the solution 34-35 wt.%. Select the 10 cm3the resulting solution, add 1 cm3solution polyvinylcaprolactam with a concentration of 5-15 wt.%, extracted 20-30 min, the extract is separated. The equilibrium concentration of ortho-vanillin and ISO-vanillin in aqueous solution determined spectrophotometrically.

To aqueous solutions of ortho-vanillin or ISO-vanillin concentrations (with) 0,01; 0,02; 0,03; 0,04; 0,05; 0,06; 0,07; 0,08; 0,09, 0,1 g/cm3add visivel - crystalline sodium chloride to the salt content in the solution 34-35 wt.%. Select the 10 cm3 the resulting solution, add 1 cm3solution polyvinylcaprolactam with a concentration of 5-15 wt.%, extracted 20-30 min, the extract is separated. The equilibrium concentration of ortho-vanillin or ISO-vanillin in aqueous solution determined spectrophotometrically. The data and construct a graph of the dependence D=f(c).

The recovery (R %) of ortho-vanillin and ISO-vanillin calculated by the formula:

R=DĚ100/(D+r),

where D is the distribution coefficient of ortho-vanillin and ISO-vanillin between solution polyvinylcaprolactam and water solution, r is the ratio of the equilibrium volumes of aqueous and organic phases.

The organic phase transitions 84% ortho-vanillin and 77% ISO-vanillin.

Examples of the method.

Example 1.

To 10 cm3aqueous solution of ortho-vanillin add visivel - crystalline sodium chloride to the salt content in the solution 34 wt.% and 1 cm3solution polyvinylcaprolactam with a concentration of 10 wt.%, extracted with 20 min, a volume ratio of water-salt and organic phases 10:1 extract is separated, the equilibrium concentration of ortho-vanillin in aqueous solution determined spectrophotometrically in the range of wavelength 190-400 nm.

The recovery (R %) of ortho-vanillin calculated by the formula:

R=DĚ100/(D+r),

where D is the distribution coefficient of ortho-vanillin between solution polyvinylcaprolactam aqueous solution, r is the ratio of the equilibrium amounts of water-salt and organic phases.

The organic phase transitions 84% ortho-vanillin.

Way feasible.

Example 2.

To 10 cm3aqueous solution of ISO-vanillin add visivel crystalline sodium chloride to salt in a solution of 35 wt.%, and 1 cm3solution polyvinylcaprolactam with a concentration of 10%, extracted for 30 min at a volume ratio of aqueous and organic phases 10:1 extract is separated, the equilibrium concentration of ISO-vanillin in aqueous solution determined spectrophotometrically in the range of wavelength 190-400 nm.

The degree of extraction of ISO-vanillin calculated analogously to example 1.

The organic phase transitions 77% ISO-vanillin.

Way feasible.

Table.
The degree of extractionThe known methodThe degree of extraction examples
Example 1Example 2
Ortho-vanillin5484-
ISO-vanilla33-/td> 77

As can be seen from the table, the degree of extraction of ortho-vanillin and ISO-vanillin in aqueous solution, saturated sodium chloride, rises to 84% for ortho-vanillin, to 77% for ISO-vanillin when removing solution polyvinylcaprolactam.

In the absence or decrease of the concentration of sodium chloride in the analyzed water solution, the organic phase is not formed, when the content of polyvinylcaprolactam less than 5% is not achieved more or less complete extraction, increasing the concentration of polymer is more than 15% of the economically impractical.

The proposed method of extraction of ortho-vanillin and ISO-vanillin from aqueous solutions allows to increase the degree of extraction of ortho-vanillin and ISO-vanillin from aqueous solutions and used as extractant non-toxic polyvinylcaprolactam.

The method of extraction of ortho-vanillin and ISO-vanillin from aqueous solutions, characterized by the fact that aqueous solutions of ortho-vanillin and ISO-vanillin add visivel sodium chloride to the salt content in the solution 34-35 wt.% and pre-prepared solution of polyvinylcaprolactam with a concentration of 5-15 wt.%, when a volume ratio of aqueous and organic phases 10:1, is extracted, the organic phase is separated and analyzed spectrophotometrically, the degree of recovery (R %) of ortho-vanillin and ISO-Vani is ina calculated by the formula:
R=DĚ100/(D+r),
where D is the distribution coefficient of ortho-vanillin and ISO-vanillin between solution polyvinylcaprolactam and water solution, r is the ratio of the equilibrium volumes of aqueous and organic phases.



 

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