Method of purifying phenol-containing sewage waters of rice husk processing

FIELD: chemistry.

SUBSTANCE: method of purification of phenol-containing sewage waters of alkali-hydrolysis processing of rice husk includes preliminary desiliconisation of phenol-containing sewage waters by their processing with hydrochloric acid with precipitation of solid and separation from solution of silicon-containing product and electrochemical oxidation in presence of chloride ions in electrolytic cell with application of direct current. Process of electrochemical oxidation is carried out with concentration of chloride ions 0.10-0.11 mol/l in non-diaphragm electrolytic cell with application of ruthenium-titanium oxide anode and titanium cathode for 70-90 min with current density 100-150 mA/cm2 with constant mixing. Required concentration of chloride ions is provided by dilution with water of phenol-containing sewage waters after their desiliconisation.

EFFECT: invention makes it possible to increase degree of purification of polydisperse concentrated phenol-containing sewage waters of alkali-hydrolysis processing of rice husk from phenol and other organic pollutants.

3 cl, 1 tbl, 2 ex

 

The invention relates to the treatment of industrial waste water from organic compounds that represent an environmental hazard, and can be used to clean finasterida wastewater from the production of cellulosic materials, mainly waste water recycling rice husk by alkaline hydrolysis.

The production of fibrous materials in the pulp and paper industry, in particular to obtain an intermediate for the production of cellulosic materials from rice husks, is characterized by a large flow of water to ensure environmentally safe level of water use is necessary before discharge to water bodies be cleaned in accordance with the regulations.

To clean finasterida wastewater pulp and paper industry uses a variety of methods: physical, chemical, physico-chemical (coagulation, flocculation, adsorption) and biological, at present, all the more widespread electrochemical methods that effectively remove difficultly oxidizable organic compounds.

Known purification method finaasteride wastewater (Pat. CN No. 101362677, publ. 2009.02.11) by electrochemical decomposition of phenol in solution using as a working electrode polyaniline plait�Ki, precipitated on the surface of the anode, with the oxidation-reduction mode is controlled by adjusting the potential of the electrode. Under oxidizing conditions, the membrane expands and draws phenol, or recovery it narrows, releasing phenol, and regenerates. The known method is ineffective at clearing polydisperse wastewater with high values of chemical oxygen demand (COD) and color.

Also known electrochemical method of cleaning finasterida wastewater COD=530 mg O2/l (us Pat. CN No. 101891285, publ. 2010.11.24) using boron-doped diamond film electrode with a developed surface, with which the standard indicator (150 mg/l) phenol is achieved 3,19 h. However, the known method is ineffective at clearing polydisperse wastewater with high concentrations of phenols, COD value and chroma.

The closest to the claimed is a method of cleaning finasterida wastewater by electrochemical oxidation (Pat. CN No. 102515315, publ. 2012.06.27), ensuring the achievement of standard indicators in mild reaction conditions and the absence of secondary pollution of waste waters in which use of titanium anode, previously subjected to grinding, alkaline and acid treatment, electrolysis and calcium�the probing, and a platinum cathode. The content of chloride ions in the waste water was adjusted to a concentration of not less than 0.03 mol/l, then carry out the processing at a constant current density of 500 mA/cm2for 0.5 h at controlled concentrations of chloride ions, the current density and time of electrolysis.

However, the known method is not effective enough at clearing polydisperse wastewater with high concentrations of phenols, COD value and chroma, in particular alkaline hydrolysates formed by obtaining fibrous semi-finished products from rice husk and contains in addition to phenolic compounds complex of polluting organic substances. It provides the necessary degree of purification finasteride solution with an initial concentration of not more than 200 mg of phenol/l, and the indicators of purity relate to model solutions that do not contain other pollutants.

The object of the invention is to provide an effective method of purification of highly concentrated polydisperse finasterida wastewater alkaline hydrolysis of rice husk processing, providing a high degree of purification from phenol and other environmental risk of organic substances.

The technical result of the invention is to improve PT�fines and degree of treatment of polydisperse concentrated finasterida wastewater alkaline hydrolysis of rice husk processing from phenol and other organic contaminants.

Said technical result is ensured by the method of cleaning finasterida wastewater alkaline hydrolysis of rice husk processing by electrochemical oxidation in the presence of chloride ions in the electrolytic cell with the use of direct current, in which, in contrast to the known, the electrochemical oxidation is carried out at the concentration of chloride ions 0,10-0,11 mol/l in bezdiafragmennoi electrolytic cell using an oxide ruthenium-titanium anode and titanium cathode for 70-90 min at a current density of 100-150 mA/cm2with continuous stirring, and conduct pre-obstrelyani finasterida wastewater by treatment with hydrochloric acid to settling or separation from the solid solution of silicon-containing product, with the necessary concentration of the chloride ions by dilution with water finasterida wastewater after their obstrelyany.

In a preferential embodiment of a method of processing finasterida wastewater with hydrochloric acid is carried out until the pH of the solution is 3.5-4.0.

To create optimal conditions for the electrochemical oxidation of wastewater after obstrelyany diluted with water in ratio 1:(10-12).

The method is as follows.

The phenol-containing waste water, �Brazauskas upon receipt of fibrous cellulosic prefabricated from rice husk by processing by the method of alkaline hydrolysis and containing more than 1000 mg/l phenol in, and other organic pollution, including in the form of polydisperse particles of organic origin, was treated with hydrochloric acid to obtain the silicon-containing solid residue. Almost complete obstrelyani is carried out with the pH value of the solution is 3.5-4.0. Obtained by processing silicon-containing sludge separated from wastewater by using one of known methods, and the remaining obescity solution was diluted with water, providing the concentration of the chloride ions of about 4 g/l (0,10-0,11 mol/l), which required a dilution of 10-12 times.

Then carried out the electrochemical oxidation of dilute wastewater in bezdiafragmennoi temperature-controlled electrolytic cell at a current density of 100-150 mA/cm2for 70-90 min with constant stirring. As the anode was used ruthenium oxide-titanium (ORT) electrode and a titanium cathode.

Quality indicators derived from the processing of rice husk by the method of alkaline hydrolysis of wastewater prior to their treatment by the proposed method and after, and technology standards for wastewater treatment in accordance with the recommendations of Helsinki Commission (HELCOM, 1992.04.09) for wastewater pulp production are given in the table. The content of impurities is given in mg/DM3and for �normiruemyh on the recommendations of HELCOM in kilograms per tonne of product (air-dried pulp).

The destruction efficiency of organic substances, which clearly shows the degree of purification was assessed by color, biochemical oxygen demand BOD5, chemical oxygen demand COD and phenolic equivalent. The removal efficiency of organic compounds in COD was 66%, phenolic compounds are oxidized almost completely within 80 min. the decolorization Efficiency after 60 min reaches over 99%.

Peeled proposed method, the effluents before discharge to water in places of drinking and household water use by the existing standards (maximum permissible concentrations of 15 and 30 mg O2/l respectively) and HELCOM standards require advanced treatment to remove organic substances (COD. They can be used as process water in the corresponding production, in particular for cleaning the intermediate products in the processing of rice husk.

Examples of specific implementation method

To determine the color was applied fotoelektrokalorimetry method with spectrophotometer UNICO-1201 GOST 3351-74 "drinking Water. Methods for determination of taste, odour, colour and turbidity". COD was determined by the PND f (environmental�this regulatory document Federal) No. 14.1:2:4.190-03 dated 27.02.2003 "Quantitative chemical analysis of water. The method of determining bichromate oxidability (chemical oxygen demand) in samples of natural, drinking and waste water by the photometric method with application fluid analyzer "Fluorat-02"". The content of phenolic compounds was determined photometrically using the Folin reaction (Standard Methods for the Examination of Water and Wastewater/American Water Works Association, and Water Pollution Control Federation. 20th Edition. Washington, DC, 1998. Vol. 5550. P. 988-992). The optical density of the solution was measured on a UV spectrophotometer Shimadzu UV-1800. The chloride concentration in the solution was determined by potentiometric titration with silver chloride electrode according to GOST 18190-72. "Drinking water. Methods for determination of residual active chlorine" (valid).

Example 1

Waste water alkaline hydrolysis of rice husk after separation of the cellulosic semi-finished product, subsequent processing of the resulting solution with hydrochloric acid (d=1,175 g/cm3) to pH 4.0 with settling or filtering out of silicon-containing product was diluted with water 1:10. The diluted solution with a content of chloride ions of 0.11 mol/l (4 g/l) were subjected to electrochemical oxidation in bezdiafragmennoi temperature-controlled electrolytic cell with continuous stirring at a constant current density of 100 mA/cm2within 90 min using as the anode oxide ruthenium-year - �anew electrode, consisting of 30% of RuO2and 70% of TiO2as a cathode electrode made of titanium grade VT1-0.

The results of processing are shown in the table. The decolorization efficiency of 99.93%.

Example 2

Waste water recycling rice husk alkaline hydrolysis was treated according to example 1 under the following conditions: treatment with hydrochloric acid to pH 3.5, diluted with water obschetvennogo solution of 1:12 to the content in the diluted solution of the chloride ions of 0.10 mol/l, electrochemical oxidation at a current density of 150 mA/cm2for 70 min.

The similar results obtained in example 1.

1. Method of cleaning finasterida wastewater alkaline hydrolysis of rice husk processing by electrochemical oxidation in the presence of chloride ions in the electrolytic cell with the use of direct current, characterized in that the electrochemical oxidation is carried out at the concentration of chloride ions 0,10-0,11 mol/l in bezdiafragmennoi electrolytic cell using an oxide ruthenium-titanium anode and titanium cathode for 70-90 min at a current density of 100-150 mA/cm2with continuous stirring, and conduct pre-obstrelyani finasterida wastewater by treatment with hydrochloric acid and precipitation of solid separation from the solution kremnistaya�his product the necessary concentration of the chloride ions by dilution with water finasterida wastewater after their obstrelyany.

2. A method according to claim 1, characterized in that the processing finasterida wastewater with hydrochloric acid is carried out until the pH of the solution is 3.5-4.0.

3. A method according to claim 1, characterized in that the waste water after obstrelyany diluted with water in ratio 1:(10-12).



 

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