Method of extraction recovery of phenol, nitrophenol or halogensubstituted of nitrophenol from aqueous solutions containing 4-nitrocresols

 

(57) Abstract:

The invention relates to analytical chemistry of organic compounds. When analytical control of wastewater containing phenol, NITROPHENOL or halogensubstituted NITROPHENOL and 4-nitrocresols, the water sample is acidified to pH 2 to 3, then enter the ammonium sulfate in the amount of 38.5 - 40.0% from the mass of the solution and lead extraction with acetone. table 2.

The invention relates to analytical chemistry of organic compounds and can be used for pre-separation in analytical control of wastewater containing phenol (NITROPHENOL or halogen-substituted) and 4-nitrocresols.

As an analogue of the selected extraction method extraction of nitro - and nitrosophenol the octanol-1 of water samples (Korenman I. I. the distribution Coefficients of organic compounds. - Voronezh: publishing house. Voronezh. University, 1992, 336 C. ). The disadvantage of analogue is the low degree of extraction of phenol and nitrophenols and the impossibility of separating them with 4-nitrosobenzene in the extraction step in a joint presence in a water sample.

The prototype can serve as the extraction of phenol and 4-nitrosobenzene allylacetate of acidified water Rast is I and chem. technology, 1978, T. 21, N2, S. 182 - 185). The disadvantage of this method is the low degree of extraction of phenol, do not provide for a full transition extractable compounds in the organic phase for the single extraction and 10-fold concentration. In addition, when the extraction of the specified method is the simultaneous extraction of 4-nitrosobenzene in case of its presence in the analyzed water sample.

The objective of the invention is to increase the degree single extraction phenol (nitrophenols or halogen-substituted) of the analyzed water solution and separation of these compounds and 4-nitrosobenzene when their joint presence in a water sample in the extraction step.

This object is achieved in that in the method of extraction recovery of phenol (nitrophenols or halogensubstituted) from aqueous solutions containing 4-nitrocresols, to analyze the water sample is added to the extract as acetone in the presence of ammonium sulfate in the amount of 38.5 - 40.0 wt.% with respect to the sample was acidified to pH 2

Based on the research of patent and scientific literature, we can conclude that the set of essential features is new and allows to improve the and the extraction step.

The technical result is that the proposed method can achieve almost complete removal of phenol (nitrophenols or halogen-substituted) and to separate them from 4-nitrosobenzene at the stage of extraction with an organic solvent in an acid environment.

The distribution coefficients D of these compounds and factors division 4-nitrosobenzene =D1/D2where D1and D2the distribution coefficients of phenols and 4-nitrosobenzene respectively, are given in table. 1.

How is that to 200 ml of a water sample containing phenol (NITROPHENOL or halogen-substituted) and 4-nitrocresols, acidified with sulfuric acid ( = to 1.187 g/cm3) to pH 2, add visivel - ammonium sulfate in the amount of 38.5 - 40.0 wt.% in relation to the analyzed water sample and 25 ml of acetone, ekstragiruyut on vibromaster until the salt is completely dissolved and the self-selection of the organic phase (10 - 15 min). After separation of phases (10 - 15 min) to separate the extract containing phenol (NITROPHENOL or halogen-substituted), not grasping the aqueous layer, and determine the concentration of phenols in aqueous and organic phases.

The distribution coefficients (D) and flat the

Caboutthe concentration of phenol in the organic phase;

K is the ratio of the equilibrium volumes of aqueous and organic phases;

C2the concentration of phenol in the aqueous phase.

An example of the prototype. To 200 ml of a water sample containing phenol and 4-nitrocresols, acidified to pH 2, add 20 ml of butyl acetate, extracted within 10 - 15 minutes to establish the interfacial equilibrium. After separation of phases (10 - 15 min) to separate the organic phase from the water and determine the concentration of phenols in aqueous and organic phases. The ratio of the equilibrium volumes of aqueous and organic phases is 10 : 1.

The distribution coefficients (D) of phenol and 4-nitrosobenzene are 58,00 and 1,77, the degree of extraction - 85,3 and 15.0%, respectively.

The proposed method is illustrated by the following examples.

Example 1. To 200 ml of a water sample containing phenol (NITROPHENOL or halogen-substituted) and 4-nitrocresols and acidified to pH 2, add the ammonium sulfate in the amount of 40.0 wt.% with respect to the sample and 25 ml of acetone, stirred until the salt is completely dissolved and the self-selection of the organic phase. The ratio of the equilibrium volumes of aqueous and organic phases is 10 : 1. Factors raspredelitelnogo or halogen-substituted) and 4-nitrosobenzene, as well as the transition of phenol (nitrophenols or halogen-substituted) in the organic phase with a high degree of extraction.

Example 2. To 200 ml of acidified water samples (pH 3) containing phenol and 4-nitrocresols add the ammonium sulfate in the amount of 40.0 wt.% with respect to the sample and 25 ml of acetone, extracted until the salt is completely dissolved. Next, similarly to example 1. The distribution coefficient D of phenol 900, the recovery rate of 99.0%, the separation factor of 104. Way feasible.

Example 3. To 200 ml of acidified water samples (pH 4) containing phenol and 4-nitrocresols add the ammonium sulfate in the amount of 40.0 wt.% with respect to the sample and 25 ml of acetone, extracted until the salt is completely dissolved. Next, similarly to example 1. The distribution coefficient D of phenol 830, the degree of extraction 98,8%, the separation factor is less than 104. The method is not feasible.

Example 4. To 200 ml of acidified water samples (pH 2) containing phenol and 4-nitrocresols add the ammonium sulfate in the amount of 41.0 wt.% with respect to the sample and 25 ml of acetone. The method is not feasible, visivel dissolved completely and significantly adsorb phenols.

Example 5. To 200 ml of acidified water samples (pH 2) containing phenol and 4-nitro what about the complete dissolution of the salt. Next, similarly to example 1. The distribution coefficient D of phenol 985, the recovery was 99.2%, the separation factor of 104. Way feasible.

Example 6. To 200 ml of acidified water samples (pH 2) containing phenol and 4-nitrocresols add the ammonium sulfate in the amount of 37.5 wt.% with respect to the sample and 25 ml of acetone, extracted until the salt is completely dissolved. Next, similarly to example 1. The distribution coefficient D of phenol and 4-nitrosobenzene are 780 and 0.08, respectively. The separation factor is less than 104. The method is not feasible.

Comparative characteristics of known and proposed methods are given in table. 2.

Method of extraction recovery of phenol, NITROPHENOL or halogensubstituted of NITROPHENOL from aqueous solutions containing 4-nitrocresols, including extraction with an organic solvent in an acidic medium, characterized in that the starting solution is acidified to pH 2 to 3, then add the ammonium sulfate in the amount of 38.5 - 40.0% from the mass of the solution and the extractant used acetone.

 

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