Method of ion-exchange purification of sewage waters and technological solutions from metal ions

FIELD: chemistry.

SUBSTANCE: invention can be used in industry at the stage of fine or additional purification of water from traces of heavy metal ions, in the purification of vapour condensate in boiler houses and TPP plants in the creation of closed technological water circulation. To realise the method of ion-exchange water purification sewage waters and technological solutions are passed through a sorbent, containing hydrazide groups. as the sorbent used is activated carbon, preliminarily processed with a gas mixture of ammonia and hydrazine, taken in volume ratios of 1:2-2.5, at a temperature of 350-450°C. The method provides the removal of ions of metals with a variable valence: Cu2+, Zn2+, Ni2+, Cr3+, Fe3+, as well as ions of metals: Bi3+, Zr4+, Sr2+, Co2+ from water, with the preservation by the sorbent of the sorption activity in a wide range of the water solution pH values.

EFFECT: purification of water from traces of heavy metal ions.

1 tbl, 1 ex

 

The invention relates to a waste water treatment technology and can be used in the industry on stage or thin with additional water purification from traces of heavy metal ions, in the purification of steam condensate to boiler houses and CHP enterprises, including the creation of a closed technological cycle.

The known method of water purification from metal ions at their joint presence by filtration through a copolymer sorbents containing ethylendiamine grouping (copyright certificate EN NO. 966023, IPC 7, CL C02F 1/42, 1982 ). The method is selective only with respect to ions of trivalent iron (Fe3+) that is his fault, as it is limited to its application and performance when the concentration of other ions in the water.

Known methods of extraction of heavy metal ions sulfonated lignite coal [Ibarra J. R. Moliner Fuel for the Removal of heavy metal ions from wastewater with lomano sulfonated lignite. 1984, 63, N3, p.377], the sorbent based on peat [Ludwig Simon G. J. Purification of industrial wastewater from heavy metals using filters with granular sorbent based on peat. "Jahrb Geol", 1983, N6a, p.365].

The disadvantages of these cleaning methods is the low absorption capacity of the sorbents, the high cost of regeneration, low strength of the sorbent and, sledovatel�till then, high losses when filtering.

The known method of purification of wastewater from heavy metal ions by extraction sorbent based on magnesia-ferrous slags [Zosin A. P. Gurevich B. I. Milovanova I. B. On the sorption properties of lakoseljac. In proc. "Chemistry and technology of silicate materials". L. Nauka, 1971, p. 100 105], [A. P. Zosin, T. I. Primak. Treatment of industrial waste water from ions of Nickel, cobalt, copper, sorbent on the basis of magnesium-iron slags of non-ferrous metallurgy // Chemistry and technology of inorganic sorbents: the Ministry of higher education. Sat. scientific. Tr. Perm. Politiche, inst. Perm, 1980, p. 92 97].

Sewage treatment from ions of metals is carried out by passing the solution through a bed of sorbent. The disadvantage of this method is low efficiency, the impossibility of regeneration of the sorbent due to the low strength of the granules.

The known method of purification of the solution containing copper, zinc and iron from ferric ions by sorption on the anion exchange resin obtained by the amination of hydrazine copolymer of methyl acrylate and divinylbenzene [Copyright certificate EN NO. 528310, IPC 7, CL C08F 226/02, C08F 8/32 1975].

The disadvantage of this method is the low degree of purification of the solution from the ferric ions.

The known method of purification of copper-zinc solutions from ferric ions by sorption on the anion exchanger obtained �mining hydroxylamine copolymer of methyl acrylate and divinylbenzene [Copyright certificate EN No. 529178, IPC 7, CL C08F 226/02, C08F 8/32, B010 15/04, 1975].

The disadvantage of this method is the low degree of purification of the solution from the ferric ions.

Closest to the invention to the technical essence and the achieved result is a method of ion-exchange purification of sewage and waste waters from ions of metals of variable valence by passing it through a mixture aminocarboxylic of cationite and onto weak-base resin curing type, taken in cationic and anionic form, wherein the mixture is used a copolymer of methyl methacrylate, diphenylsulfide, divinylbenzene and poly (methacrylic acid hydrazide, when the ratio ethylendiamine and hydrazide groups in the copolymer is 1:1 [Patent RU No. 2434811), C02F 1/42, IPC 7, 01J 43/00, B01J 20/26, 2011].

The disadvantage of this method is its limited efficiency in the purification of wastewater containing ions of metals such as Bi3+, Zr4+, Sr2+, Co2+.

The technical result of the invention is the removal of water from ions of metals of variable valence: Cu2+, Zn2+, Ni2+, Cr3+Fe3+and metal ions: Bi3+, Zr4+, Sr2+, Co2+while maintaining the sorbent in the sorption capacity, wide pH aqueous solution and number of cycles "purge - regeneration".

Delivered technical�technical result is achieved in that a method of ion-exchange purification of waste waters and technological solutions from metal ions by passing it through a sorbent containing a hydrazide group, according to the invention in the activated carbon sorbent is used, the pre-treated gas mixture of ammonia and hydrazine, taken in the ratio of 1:2-2,5, at a temperature of 350-450°C.

In the proposed method the effect of improved water treatment is achieved by the improved structure of activated carbon. This process was carried out under the following conditions: a temperature of 350-450°C, the processing gas mixture of ammonia and hydrazine, taken in volume ratio of 1:2-2,5, the processing time was 2-5 minutes. Such process conditions allow you to modify the porous structure of coal and to increase the porosity, which gives conditions for the acquisition of coal properties on sorption from the aqueous phase not only ions of metals of variable valence: Cu2+, Zn2+, Ni2+, Cr3+Fe3+and ions of the following metals: Bi3+, Zr4+, Sr2+, Co2+.

The technical result achieved by the above set of essential features, due to the fact that this method of cleaning is manifested integrated activity of the sorbent using, in addition to available active carbon structures, amino groups-NH2and Hijazi�governmental groupings-NH-NH 2.

The sorbent does not lose mechanical strength in a cycle of work - regeneration. The set of active groups allows you to hold a wide variety of metal ions: Bi3+, Zr4+, Sr2+, Co2+without compromising with the degree of purification from ions of metals of variable valence: Cu2+, Zn2+, Ni2+, Cr3+Fe3+. In this case, the water removed from, among others, contamination of the ionic character, it is clean, usable water cycle. The method was tested in laboratory settings.

The test results are shown in the table.

Example 1

500 ml of an aqueous solution containing ions of Cu2+, Zn2+, Ni2+, Cr3+and Fe3+when the content of 1.40 mg/l and metal ions of Bi3+, Zr4+, Sr2+, Co2+when the content above 0.01 mg/l (traces) (see table), by gravity flow through the column with a height of 100 mm and a diameter of 11.3 mm, filled to 80% activated carbon is pretreated with a gas mixture of ammonia and hydrazine, in the ratio 1:2 by volume at a temperature of 350°C. In purified water solution according to the results of liquid chromatographic analysis of ions of Cr3+and Fe3+no, ions of Cu2+, Zn2+, Ni2+do not exceed permissible values, environmentally hazardous metal ions Bi3+, Zr4+, Sr2 , Co2+no, that is the quality of water treatment is greatly improved.

Example 2

500 ml of the technological solution used in the metal produced by "Volgogradneftemash", containing ions of Cu2+, Zn2+, Ni2+, Cr3+Fe3+, Bi3+, Zr4+, Sr2+and Co2+(see table), by gravity flow through the column with a height of 100 mm and a diameter of 11.3 mm, filled to 80% activated carbon is pretreated with a gas mixture of ammonia and hydrazine, in the ratio 1:2 by volume at a temperature of 350°C. In purified technological solution according to the results of liquid chromatographic analysis of ions of Cr3+and Fe3+no, ions of Cu2+, Zn2+, Ni2+do not exceed permissible values, environmentally hazardous metal ions Bi3+, Zr4+, Sr2+, Co2+no, that is the quality of the cleaning process solution is significantly improved. Results in comparison with the prototype presented in the table.

Example 3

500 ml of wastewater produced by "Metalware plant" containing ions of Cu2+, Zn2+, Ni2+, Cr3+Fe3+, Bi3+, Zr4+, Sr2+and Co2+(see table), by gravity flow through the column with a height of 100 mm and a diameter of 11.3 mm, filled to 80% activated carbon, pre-obrabotannoi mixture of ammonia and hydrazine, taken in the ratio 1:2.5 by volume, at a temperature of 450°C. the Treated waste water contains ions of Cu2+, Zn2+, Ni2+in concentrations not exceeding the permissible values of environmentally hazardous metal ions Bi3+, Zr4+, Sr2+, Co2+no, that is the quality of wastewater treatment is greatly improved.

tr> no
The proposed method
Composition (mg/l) and parametersExample 1Example 2Example 3Prototype
Cu2+1,401,391,431,40
Zn2+1,401,401,441,40
Ni2+1,401,361,421,40
Cr3+1,401,401,401,40
Fe3+1,401,381,431,40
Metal ions (
more than 0.01 mg/l)
Bi3+++++
Zr4+++++
Sr2+++++
Co2+++++
the pH of the solution3,5-53,5-53,5-53,5-5
The volume of purified water ml/ml �Anita 300300300300
the pH of the treated water7,0777
The change in volume of the sorbent, %0,0÷+0,40,0÷+0,40,0÷+0,40,0÷+0,4
The number of cycles "work-regeneration" without deterioration of the treated water22222222"
Bi3+nononothere
Zr4+nononothere
Sr2+nononothere
Co2+nonothere
Cu2+(mg/l)0,0050,0050,0050,005
Zn2+(mg/l)0,0070,0070,0070,007
Ni2+(mg/l)0,0010,0010,0010,001
Cr3+nononono
Fe3+nononono

Thus, the developed technical solution provides the features, sufficient to obtain a new technical result specified by the claims.

Method of ion-exchange purification of waste waters and technological solutions from metal ions by p�lowering through the sorbent, containing a hydrazide group, characterized in that the activated carbon sorbent is used, the pre-treated gas mixture of ammonia and hydrazine, taken in the ratio of 1:2-2,5, at a temperature of 350-450°C.



 

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