Method of obtaining composition for cleaning and disinfection of water

FIELD: chemistry.

SUBSTANCE: method of obtaining the polymeric composition is proposed. It is obtained by inter-reacting a guanidine containing polymer and a natural mineral in which interaction of the water-soluble guanidine containing polymer and a natural mineral is accomplished by intercalation of the guanidine containing monomer in the interlayer space of montmorillonite and its subsequent polymerisation. The relation of components in the obtained composition is, mass%: montmorillonite 50-85, methacrylate of guanidine 15-50.

EFFECT: invention makes it possible to increase the sorption activity of the composition.

3 ex, 4 tbl

 

The invention relates to the field of composite materials with sorption and biocidal properties and are designed for cleaning and disinfection of water.

It is known that the use of polymeric guanidine derivatives for water disinfection effectiveness is equivalent to its ozonation or chlorination, however, unlike the latter, has no irritating effect on the mucous membranes and the skin, is not accompanied by the accumulation in the water carcinogenic substances, does not cause allergic reactions in people and equipment corrosion [Keskiarvo, Aggrecanases, Paganucci, In Proc. of the Problem of disinfection and sterilization (Ed. Viewaskew). VIP. VNIIAES, Moscow, 1975. P.58].

The most known and studied an analogue of the polymer used to produce the composition is polyhexamethylene guanidine (phmg), which is a high molecular weight derivative of a specific nitrogenous bases - guanidine

[Paganucci, Lofbacka, Grabadora, Shimura, Dsiec. Chemical industry, №2, 82 (1984)].

Thanks to the combination of flocculation and biocidal properties of polymeric materials on the basis of guanidine are used for cleaning and disinfection of domestic and industrial wastewater [Whittow, Miyanosawa, POSTGRADUATE the inoculum, Paganucci, Izv. Questions of balneology, physiotherapy and exercise therapy. №2, 48 (1992)].

Closest to the proposed invention is a method for biocidal sorbent conocida representing natural zeolite (clinoptilolite tuff), the surface of which pgmg fixed by means of epichlorohydrin [Vaikesena, Paganucci, AMEC, Lofbacka, Akhalinskaya. WPI. An. Serhiy., 1550 (1994)].

The method thereof is that for fixing pgmg in water-insoluble form on the zeolite used the cross-linkage reaction pgmg under the action of epichlorohydrin in the presence of alkali (0.7 to 1.5 mol of epichlorohydrin on the link pgmg). The reaction occurs according to the mechanism of sequential oxyalkylene guanidino groups. Clinical is the sorbent with respect to the ions of heavy and radioactive metals. Clinical has a cation exchange capacity (1.0 to 1.5 mEq./ml), anion exchange capacity (0,2-0,3 mg-EQ./ml) and biocidal properties [U.S. Pat. 2050971, RF; B. I.(36), 88 (1995)].

The disadvantages of the method of obtaining this composition are the need of the use of epichlorohydrin for stitching guanidinoacetate polymer and fixing it on the surface of the zeolite, the additional consumption of alkali, a multi-stage and duration of the process. The disadvantage of the polymer of the composition is low IO is obmana capacity, as sorption properties has only modified by an organic compound, the surface composition.

Tasks to be solved by the invention is:

- increased sorption activity and simplification of the adsorbents for water purification and disinfection;

- improved performance bentonite clay as adsorbent, i.e. giving patterns, allowing you to use it in dynamic mode water purification;

- reduce the cost of polymer composites due to the use as raw materials natural materials;

- greater use of sorbents for extraction of water impurities wide spectrum of inorganic impurities, organic matter, ions, dyes and so on).

The invention is characterized by the fact that to get a biocidal sorbent used layered mineral (montmorillonite) and guanidinoacetate polymer intercalated in the interlayer space of the clay mineral. As a modifier and a repellent to aqueous suspension of bentonite clay, which includes at least 70% of the mineral of the montmorillonite group, is added to the Monomeric salt based on methacrylic acid and guanidine of the formula

where R=CH3.

When this happens hydrophobicity and modificationsto a clay mineral with the formation of layered columnar clay material. Next to aqueous solution of modified thus bentonite is added radical initiator is ammonium persulfate, so that the total content of ammonium persulfate in suspension was 0.05-0.2 wt.%, and the mixture is stirred for 30 minutes at a temperature of 60-70°C. the Ratio of guanidine compounds and bentonite clay (50-85):(15-50), preferably 75:25 wt.%. As a result, the monomer is polymerized on the surface and in the interlayer space of the clay. During the polymerization reaction of the monomer in the clay composition is formed, which is a solid homogeneous mass, able to swell in water, and possesses the qualities of effective filtering material, including in dynamic conditions of water purification. Ion-exchange properties of the composition are defined as properties of polymer - polyampholyte and cation exchange properties of bentonite clay. This sorbent composition is not only in relation to heavy metal ions, but also can absorb a variety of organic pollutants such as phenol, dyes, etc. at the same time the disinfection of water.

The method is as follows.

Example 1. In chetyrehosnuju flask 0.5 l equipped with a stirrer, reflux condenser, thermometer, place 100 ml of distilled water, 5 g of montmorillonite and mixed what about a homogeneous suspension. Then, the suspension is added 2.5 g of methacrylate guanidine, 1 ml of freshly prepared solution of persulfate ammonium containing 0.12 g (NH4)2S2O8and raise the temperature in the reaction medium up to 60-70°C. the Reaction mixture is stirred until the formation of a solid homogeneous mass. The resulting product is removed from the flask, washed repeatedly with distilled water and dried at room temperature for 48 hours.

Example 2. In chetyrehosnuju flask 0.5 l equipped with a stirrer, reflux condenser, thermometer, place 100 ml of distilled water, 5 g of montmorillonite and mixed until a homogeneous suspension. Then, the suspension is added to 1.25 g of methacrylate guanidine, 1 ml of freshly prepared solution of persulfate ammonium containing 0.12 g (NH4)2S2O8and raise the temperature in the reaction medium up to 60-70°C. the Reaction mixture is stirred until the formation of a solid homogeneous mass. The resulting product is removed from the flask, washed repeatedly with distilled water and dried at room temperature for 48 hours.

Example 3. In chetyrehosnuju flask 0.5 l equipped with a stirrer, reflux condenser, thermometer, place 100 ml of distilled water, 5 g of montmorillonite and mixed until a homogeneous suspension. Then in suspe is the Zia add 0.75 g of methacrylate guanidine, 1 ml of freshly prepared solution of persulfate ammonium containing 0.12 g (NH4)2S2O8and raise the temperature in the reaction medium up to 60-70°C. the Reaction mixture is stirred until the formation of a solid homogeneous mass. The resulting product is removed from the flask, washed repeatedly with distilled water and dried at room temperature for 48 hours.

Use in the invention as a repellent and a modifier in the interlayer space of the clay guanidinoacetate monomer capable of further polymerization, greatly simplifies the method of obtaining the polymer of the composition and reduces the duration of the process.

The technical result of the invention is expressed in improving the quality of biocidal sorbents on the basis of natural materials and polymers, reducing the consumption of expensive reagents, the improvement of consumer properties, there is no need to create special devices for purification and disinfection of water.

The possibility of extracting a synthesized polymer composites of some heavy metals from wastewater and natural waters was investigated 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 and what emitatsiey using atomic adsorption spectrometer "MGA-915". The research results are summarized in table 1.

Table 1
No., p/pThe concentration of the metal, mg/l
the original solutionafter the introduction of the sorbentThe degree of sorption, %
polymer composition
1copper (II)2,910,04798,3
2lead (II)1,380,19286,08
3cadmium (II)1,840,20588,85

As can be seen from the table, synthesized guanidinoacetate composite materials exhibit a sufficiently high sorption activity against the studied metals.

The results of the study of sorption activity of iodine and methylene blue are presented in table 2.

3
Table 2
No., p/pThe designated substanceThe original mass of matter,

mg
The final mass of the substance mgThe specific activity of the sorbent, g/100 g
1methyleneof 0.01252,98
blue
2iodine25421044,45

Preliminary studies of bactericidal activity of the synthesized composite materials, held in conjunction with the Bacteriological laboratory of SSES CBD, showed that they are very active and have biocidal activity against both gram-positive and gram-negative microorganisms.

Table 3

The dependence of the number of colonies of E. coli concentration sample
C, g/l0,00030,0030,030,33sample
The number of colonies3028231512polymer composition
5442362923Pgmg

The diameter of zone of growth inhibition of microorganisms

Table 4
SampleThe diameter of the zone of growth inhibition (mm) Qualitative assessment of biocides
Polymer composition15+++
Pgmg11++

Thus, the present invention provides a receiving guanidinoacetic polymer-clay compositions for cleaning and disinfection of natural and waste waters, with the necessary sorption properties, using cheap and available raw material is bentonite clay.

A method of obtaining a composition for cleaning and disinfection of water, including the modification of the natural mineral guanidinoacetate polymer, characterized in that as a natural mineral take bentonite clay containing not less than 70% of the mineral of the montmorillonite group, to the aqueous slurry which is added to the Monomeric salt based on methacrylic acid and guanidine in the amount of 15-50% by weight of montmorillonite, and a radical polymerization initiator, carry out stirring at 60-70° before polymerization of the monomer on the surface and in the interlayer space of the clay.



 

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