Extraction of phenol containing sewage flows

FIELD: process engineering.

SUBSTANCE: invention relates to environmental protection and can be used for purification of phenol containing sewage flows. Phenol containing sewage flows are purified by a mix containing 60 to 99 wt % of methylisobutyl ketone, 1 to 40 wt % of anisole and, is required, up to 20 wt % of mesitylene.

EFFECT: higher degree of purification.

16 cl, 1 tbl, 3 ex

 

This application relates to a method of extraction of phenolic effluent stream.

In industrial processes, such as upon receipt of phenol using cumene, or upon receipt of bisphenol a by condensation of phenol and acetone are formed of finasteride aqueous solutions in the form of effluent stream.

Based on the solubility of phenol in water (at a temperature above 65,3°With both substances unlimited mixed with each other at room temperature is dissolved only almost 10 wt.% phenol in water) and the formation of azeotropic mixtures by distillation of such solutions is the allocation of phenol from such effluent stream is impossible by simple distillation (J.M.Sorensen, W.Arlt, Liquid-Liquid Equilibrium Data Collection, Chemistry Data Series V/I, str-361, Dechema, Frankfurt 1979; Ullmann''s Encyclopedia of Industrial Chemistry, T. 19, str-312, 5. Edition, VCH Manheim, 1991).

Upon receipt of bisphenol a using acidic ion-exchange resins produced by the reaction of water should be removed, otherwise it decreases the activity of the catalyst. First, this removal occurs by distillation separation of the reaction water from bisphenol a, its isomers and phenol used in excess as a solvent in the process of obtaining bisphenol A. This is separated by distillation water contains a large amount of phenol (1-15 wt.%), and under some circumstances also acetone (0-5 wt.%). The together is with these basic impurities in the separated water may also contain other organic compounds, such as methanol, products samarangense acetone, such as, for example, mesityloxide, used in the process of obtaining bisphenol structurai socialization (thiol), and the cleavage products, or the subsequent conversion of these compounds. However, other aqueous streams generated in this process, along with additional organic components - containing phenol (e.g., water for contact sealing rings or the vacuum unit).

Therefore, due to the toxicity of phenol and for economic reasons (regeneration of phenol) finasteridee wastewater is purified by extraction with an organic solvent. When this is used, for example, benzene, cumene, diisopropyl ether or methyl isobutyl ketone. The extraction can be performed by known technology expert (box extractor, settling and mixing system, countercurrent extraction, and so on). To reduce the residual extractant thus treated waste water, in most cases, at a later stage additionally processed in the Stripping column. This is important because the presence of residual extract leads to significant pollution of wastewater by organic substances. By reducing the content of the extractant in the waste water can economize on the use of PA is a and, therefore, to reduce energy costs. Then the thus treated waste water is subjected to biological treatment in the effluent treatment plant.

At present, it was found that extraction of phenolic aqueous solutions isobutyl ketone as a solvent, its residual content after extraction can be reduced if he will further contain an appropriate amount of anisole and, if necessary, mesitylene.

The invention relates to a method of extraction of phenolic aqueous solutions, in which as a solvent a mixture containing 60 to 99 wt.% of isobutyl ketone, 1 to 40 wt.% anisole and 0 to 20 wt.% mesitylene, considering the mixture.

This is the preferred method of extraction of phenolic aqueous solutions, in which as a solvent a mixture containing 75 to 95 wt.% of isobutyl ketone, 5 to 25 wt.% anisole and 0 to 10 wt.% mesitylene, considering the mixture.

Thanks to the extraction of phenol and acetonaemia waste water with a mixture of isobutyl ketone and anisole instead of the pure isobutyl ketone, significantly reduce the residual content of the mixture in the waste water under the same conditions of extraction. The degree of extraction of phenol and acetone remains virtually the same.

Although the use of a mixture of isobutyl ketone and anisole in waste water are small amounts of anisole, however, a reduction in the content of the mixture is significantly greater than the increase in the content of anisole, so that, in General, the result of waste water with low content of organic components. In addition, by adding to the extraction mixture mesitylene, can also reduce the amount of anisole in the water after extraction with constant extraction effect and the residual content of the mixture.

The content of phenol in aqueous solution (waste water) is preferably 1 to 15 wt.%, believing in aqueous solution.

In addition, the waste water may contain up to 5 wt.% acetone, believing in aqueous solution.

To improve the extraction of the aqueous solution may additionally contain sodium sulfate, and/or an aqueous solution is acidified to pH<7 with sulfuric acid or other acids.

The extraction can be performed by known technology expert (multi-stage extraction, while the box extractor, settling and mixing system, countercurrent extraction, and so on).

After extraction waste water can additionally be freed of residual solvent by distillation in a column, if necessary, steam.

In addition, phenolic aqueous solution before extraction subjected to distillation, in which fully or partially separated, for example, contained in ketones or other organic components.

Extracted from phenolic aqueous solution of phenol, and, under certain conditions, other extracted organic components (in particular, under certain conditions, extracted acetone) can be separated from the extractant by distillation and thus to regenerate. Thus purified extractant can be used again for extraction.

Formed after extraction or after distillation of the aqueous phase before processing in a biological effluent treatment plant can be treated in addition with activated charcoal.

The method according to the invention preferably is used in the treatment of wastewater from the production of bisphenol A. In the method of producing bisphenol a, for example, phenol and acetone to expose turning on sulfanilic ion-exchange resins as catalysts, optionally in the presence of thiol as socializaton obtained bisphenol a fully or partially crystallizes in the form of an adduct of bisphenol a - phenol, which is filtered off and then the filtrate is partially or fully released from water distils the Oia. You can also use the method of producing bisphenol a in which the separation of the reaction water, unlike the above-described method, fully or partially occurs before the crystallization of the adduct of bisphenol a - phenol. In addition, this method is suitable for the extraction of effluent from the process of obtaining bisphenol a, in which at or before the stage of crystallization add water (if necessary, in a mixture with phenol or other organic solvents).

Examples

Example 1 (comparative)

In a separating funnel 500 ml shake 170 ml of phenolic aqueous solution (waste water from the production of bisphenol a) within 15 seconds with 100 ml of isobutyl ketone. Then leave the funnel for 5 minutes without shaking, after which the aqueous phase is drained and examined using gas chromatography. The results are shown in table 1.

Example 2 (according to the invention)

Example 2 carried out analogously to example 1 with the difference that instead of 100 ml of isobutyl ketone, a mixture of 80 ml of isobutyl ketone and 20 ml of anisole. The results are shown in table 1.

Example 3 (according to the invention)

Example 3 carried out analogously to example 1 with the difference that instead of 100 ml of isobutyl ketone, a mixture of 83 ml of isobutyl ketone, 12 ml of anisole and 5 ml of mesitylene. The results are shown is table 1.

Table 1
The results of experiments on extraction [wt.% in the aqueous phase after extraction].
ConnectionExample 1Example 2Example 3
phenol0,210,230,25
methylisobutyl-ketone1,401,001,05
acetone0,0170,0150,017
the anisole<0,0050,0440,025
mesitylene<0,005<0,005<0,005
amountabout 1,63about 1,29about 1.35

1. The method of extraction of phenolic aqueous solutions, characterized in that as a solvent, a mixture containing from 60 to 99 wt.% of isobutyl ketone, from 1 to 40 wt.% anisole and from 0 to 20 wt.% mesitylene, considering the mixture.

2. The method according to claim 1, characterized in that the phenol content in the extractable phenolic aqueous solutions is 1-15 wt.%.

3. The method according to claim 1, characterized in that finasteride aqueous solutions of fully or partly comes from the production of bisphenol A.

4. The method according to claim 1, characterized in that finasteride aqueous solutions contain sodium sulfate.

5. The method according to claim 1, characterized in that phenolic aqueous solutions additionally contain even up to 5 wt.% of acetone.

6. The method according to claim 5, characterized in that finasteride aqueous solutions before extraction is subjected to distillation, and separating at least part of the acetone.

7. The method according to one of claims 1 to 6, characterized in that the content of isobutyl ketone in aqueous solution after extraction is reduced by distillation.

8. The method according to one of claims 1 to 6, characterized in that the phenol and, optionally, other organic components recovered by distillation from the resulting extraction mixture containing methyl isobutyl ketone.

9. The method according to claim 7, characterized in that the phenol and, optionally, other organic components recovered by distillation from the resulting extraction mixture containing methyl isobutyl ketone.

10. The method according to onomous claims 1 to 6 and 9, characterized in that the content of organic components in aqueous solution after extraction is additionally reduced by passing over activated charcoal.

11. The method according to claim 7, characterized in that the content of organic components in aqueous solution after extraction is additionally reduced by passing through activated charcoal.

12. The method according to claim 8, characterized in that the content of organic components in aqueous solution after extraction is additionally reduced by passing through activated charcoal.

13. The method according to one of claims 1 to 6, 9, 11 and 12, characterized in that the aqueous solutions before extraction of acidified to pH<7.

14. The method according to claim 7, characterized in that the aqueous solutions before extraction of acidified to pH<7.

15. The method according to claim 8, characterized in that the aqueous solutions before extraction of acidified to pH<7.

16. The method according to claim 10, characterized in that the aqueous solutions before extraction of acidified to pH<7.



 

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FIELD: devices for purification of household and industrial sewage.

SUBSTANCE: the invention is dealt with devices for purification of household and industrial sewage and intended for electrical and cavitational treatment of sewage containing a large quantity of organic compounds. The device for purification of sewage consists of a body made out of a dielectric material partitioned by diaphragms for two electrode chambers and one working chamber, that contains a filtering material. The electrode chambers have cavitational field sources installed and the working chamber is supplied with a the bubbler installed in it. The technical result consists in an increase of recuperation of the filtering material at the expense of application of a cavitational field to it, decrease of the microbiological semination, and an increase of cavitational effect on particles.

EFFECT: the invention ensures an increase of the filtering material recuperation, decreased microbiological semination and increased the cavitational effect on particles.

1 dwg

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