Method for preparation of polymer-clayish composition for water purification and decontamination

FIELD: chemistry.

SUBSTANCE: invention refers to the method for preparation of polymer-clayish composition which can be used in different branches of industry as sorbent for water purification and decontamination. According to the invention the surface activator - guanidine-containing salt with quaternary nitrogen atom is added to bentonite clay and then the activated surface is treated with unsaturated organic acid (acrylic or metacrylic) in presence of radical initiator of polymerisation - ammonium persulphate. The mixture is heated at temperature 60-70°C with stirring up to polymerisation of unsaturated organic acid. The mass ratio of activated bentonite clay to unsaturated organic acid is 1:1÷2.

EFFECT: simplifying of the process of bentonite surface activation, enhancing of sorption activity, improvement of bentonite performance as well as transfer to bentonite composition of biocide properties.

3 tbl, 9 ex, 1 dwg

 

The invention relates to the field of production of chemically modified clays, which can be used as sorbents for purification and disinfection of water in various industries.

Bentonite is related to the layered clay minerals group of smectites, is widely used in the manufacture of materials for various industries: oil production, metallurgy, water treatment. The possibility of bentonite as raw material for the synthesis of new materials, multi-purpose, far from being exhausted. High content in bentonite montmorillonite, structural elements which are the aluminosilicate layers with a thickness of 1 nm, provides a very significant scientific and technological potential of this mineral. At the present time, in connection with the loss-rich montmorillonite deposits of the Caucasus, is actual involvement in industrial use Russian bentonites and the creation of physico-chemical principles of production and use polymersilicate compositions with the necessary complex technological properties.

Closest to the proposed invention is a method of obtaining organic cation [Eli, Amorebieta, Adevarul. Plastic masses, No. 10, 2005].

The method thereof is that the bentonite Manaccora IU the prospect (Kazakhstan), the main rock-forming mineral is montmorillonite, activate 20% sulfuric acid under heating for 6 hours in a water bath. Then the bentonite treated with a solution of benzoyl peroxide as an initiator and dried in vacuum to constant weight. The dried bentonite is placed in the reaction flask, add an aqueous solution of acrylic acid and rinsed with an inert gas. The reaction system with stirring is heated at a temperature of 60-70°C. the resulting activated polyacrylic acid bentonite, which shows properties of weak acid cation exchanger.

The disadvantage of this method of obtaining activated bentonite is that the processing of clay minerals inorganic acids leads to a profound change in their structure and properties. These changes are primarily expressed in significant destruction of the octahedral layers as a result of dissolution of the oxides of aluminum, magnesium and iron. When this N-form of bentonite enters Al-uniform, especially when heated and the moisture that is accompanied by a significant loss of activity. In addition, this method is multi-stage and duration of the process.

The problem solved by the invention is the use of bentonite clay in the Russian field, simplifying the process of activating the surface of the be the will set, the increase in sorption activity, improving performance characteristics of bentonite clay, giving the composition of the biocidal properties.

The inventive method is that for chemically activated surface of bentonite clay, clay mineral Russian field "garbages" (Kabardino-Balkaria), containing 80% of montmorillonite subjected to activating guanidinoacetate salts, which leads to the hydrophobization of the particles of clay and the best combination with organic materials. As activator use of biocidal guanidinoacetate salt with the Quaternary nitrogen atom, for example: diallylmalonate (DAG), cialisgenericpriceat (DATTA), methacrylamides (MAG), acrylathane (AG).

To obtain polymer-clay composition to the aqueous suspension of bentonite clay add the activator surface guanidinoacetate salt with the Quaternary nitrogen atom, is treated with an activated surface of an unsaturated organic acid, acrylic (AA) or methacrylic (IAC) acid, in the presence of a radical polymerization initiator ammonium persulfate, with activated bentonite clay and unsaturated organic acid taken in a mass ratio of 1:1÷2, further heated at a temperature of 60-70°C under stirring until polymeris the tion of unsaturated organic acids.

The method is as follows:

Example 1. In the bentonite suspension containing 10 g of clay and 50 ml of water, prepared by stirring at room temperature on a magnetic stirrer for 30 minutes, add diallylmalonate and stirred for further 2 hours at room temperature. The ratio of guanidine compounds and bentonite clay 15:85 wt.%. The resulting organogeny washed with water by repeated decantation and dried at room temperature. Then 40 ml of aqueous suspension containing 5 g of organogeny placed in chetyrehosnuju flask 0.5 l equipped with a stirrer, reflux condenser, thermometer, poured 5 ml of methacrylic or acrylic acid, and ammonium persulfate so that its concentration in the total solution volume of 50 ml was 5×10-3M. the Reaction mixture was stirred at 60-70°C. until the polymerization of unsaturated organic acids. The resulting product is removed from the flask, washed repeatedly with distilled water and dried at room temperature for 48 hours.

Example 2. In the bentonite suspension containing 10 g of clay and 50 ml of water, prepared by stirring at room temperature on a magnetic stirrer for 30 minutes, add cialisgenericpriceat and stirred for further 2 hours at room temperature. The ratio of the guanidine compound and b is nanitoboy clay 15:85 wt.%. The resulting organogeny washed with water by repeated decantation and dried at room temperature. Then 40 ml of aqueous suspension containing 5 g of organogeny placed in chetyrehosnuju flask 0.5 l equipped with a stirrer, reflux condenser, thermometer, poured 8 ml of methacrylic or acrylic acid, and ammonium persulfate so that its concentration in the total solution volume of 50 ml was 5×10-3M. the Reaction mixture was stirred at 60-70°C. until the polymerization of unsaturated organic acids. The resulting product is removed from the flask, washed repeatedly with distilled water and dried at room temperature for 48 hours.

Example 3. In the bentonite suspension containing 10 g of clay and 50 ml of water, prepared by stirring at room temperature on a magnetic stirrer for 30 minutes, add acrylathane or methacrylamide and stirred for further 2 hours at room temperature. The ratio of guanidine compounds and bentonite clay 15:85 wt.%. The resulting organogeny washed with water by repeated decantation and dried at room temperature. Then 40 ml of aqueous suspension containing 5 g of organogeny placed in chetyrehosnuju flask 0.5 l equipped with a stirrer, reflux condenser, thermometer, poured 10 ml of methacrylic or acrylic acid and persulfate so, to its concentration in the total solution volume of 50 ml was 5×10-3M. the Reaction mixture was stirred at 60-70°C. until the polymerization of unsaturated organic acids. The resulting product is removed from the flask, washed repeatedly with distilled water and dried at room temperature for 48 hours.

The technical result is achieved due to the application to activate the clay biocidal guanidinoacetic salts with Quaternary nitrogen atom, the improvement of consumer properties by increasing the sorption activity and impart biocidal properties, simplify the process by reducing time modification of clay.

The study of sorption activity of the obtained compositions was carried out by traditional methods commonly used to evaluate the activity of sorbents: adsorption of methylene blue and iodine from the aqueous solution, in static conditions. The equilibrium concentration of methylene blue was determined by photocolorimetric method. The equilibrium iodine concentration was determined by titration with sodium thiosulfate solution. Adsorption activity of the material was carried out through the determination of adsorption capacity in mg×g-1(table 1).

The possibility of extracting a synthesized composite materials of some heavy metals from wastewater and natural waters research and using model solutions. Measurement of the mass concentration of metals in water samples before and after processing of the composites was performed by atomic absorption method with electrothermal atomization using atomic adsorption spectrometer "MGA-915". The research results are summarized in table 2.

To test the effectiveness of cleaning the model waste water from toxic organic compounds showed that the proposed material has a high absorption capacity for toxic organic compounds, in particular phenol. The equilibrium concentration of phenol was determined by photocolorimetric method. Were built adsorption isotherms of phenol from its aqueous solutions at room temperature. These studies indicate that the absorption ability of the obtained sorbents towards phenol increases for composite materials, which were obtained by processing a higher concentration of acrylic or methacrylic acid. When the content of the phenol of less than 1 mg/l to remove it from solution is 80-95% (see drawing).

Studies of bactericidal activity and toxicity of the synthesized composite materials, held in conjunction with the Bacteriological laboratory of SSES CBD and pharmaceutical Association "Elfare (KBR, Nalchik)showed that these drugs are very active and on adut biocidal activity against gram-negative (E. coli) microorganisms and also have a low toxicity (table 3).

Thus, the combination of the submissions received high bactericidal activity with increased ability to bind with heavy metals and organic pollutants opens the possibility of their use as effective sorbents for water purification and disinfection.

Table 1
Evaluation of adsorption capacity of polymer composites
№/№sampleorganogen: AK(MAC)Adsorption capacity, mg×g-1
iodinefor MS
1the original bentonite clay(BG)-412
2BG/DAG+AK1:14772
3BG/DAG+MAC1:14268
4 BG/DITTA+AK1:1,65270
5BG/DITTA+MAC1:1,65067
6BG/MAG+AK1:26388
7BG/MAG+MAC1:25584
8BG/AG+AK1:26690
9BG/AG+MAC1:26492

Table 2
Measurement of the mass concentration of metals in water samples before and after processing composites
No., p/pMe2+The concentration of the metal, mg/l
Before cleaningP the following cleanup The degree of sorption, %
BG/MAG+MAC(1:2)
1C2,910,37287,2
2Pb1,380,14989,2
3Cd1,640,27383,3
4Ni1,520,37075,6
5Co1,280,40568,3
BG/MAG+AK (1:2)
1C2,910,10796,3
2Pb1,380,164at 88.1
3 Cd1,640,21686,8
4Ni1,520,46069,7
5Co1,280,38270,1

Table 3
Data biocenose and toxicity of polymer-clay compositions
no PPConnectionorganogen: AK(MAC)ItThe number of E. coli colonies grown on 1 cm3waterThe diameter of the zone of growth inhibition (mm)
1the original bentonite clay67,512060
2BG/DAG+AK1:1to 75.23210
3 BG/DAG+MAC1:198,8359,6
4BG/DITTA+MAC1:1,6122,41215
5BG/DITTA+AK1:1,693,21613
6BG/MAG+AK1:276,1476,5
7BG/MAG+MAC1:279,2369.8
8BG/AG+AK1:2100,2398,2
9BG/AG+MAC1:2104,6427,8
Note. I t- toxicity index (considered non-toxic sample, where 120>It>60)

A method of obtaining a polymer-clay composition for cleaning and disinfection of water, which consists in the fact that the aqueous slurry bentonite clay add the activator surface guanidinoacetate salt with the Quaternary nitrogen atom, is treated with an activated surface of an unsaturated organic acid, acrylic or methacrylic acid, in the presence of a radical polymerization initiator ammonium persulfate, with activated bentonite clay and unsaturated organic acid taken in a mass ratio of 1:1÷2, further heated at a temperature of 60-70°C under stirring until the polymerization of unsaturated organic acids.



 

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