EA020502B1 - Apparatus for filtering water from different sources and method of preparing sorbent material - Google Patents

Abstract

Apparatus for filtering water from different sources and method of preparing sorbent material relate to purification of liquids from impurities by filtration and can be used in systems of production and domestic utilization and for monitoring the state of natural aqueous medium and subsequent determination concentration of some elements. An apparatus has a chamber, having an inlet and outlet for a liquid stream and a sorbent element which is hydrodynamically linked to the inlet and the outlet. The chamber is a composite column with a funnel, wherein the connecting parts of the top part of the column enter its bottom part, the structure is fastened by rods and bolts, and is connected to a receiving device fitted with a pump, the sorbent element is a removable cartridge with sorbent material therein placed inside the chamber and is supported by a grid. A method of preparing the sorbent material involves cutting discs from polyurethane, washing, drying and successively saturating the matrix with chemicals to form in the matrix a mixture of iron oxyhydroxide and manganese(IV) dioxide in ratio of 5:1 with pH ~8. The technical effect provides high efficiency and rate of concentrating elements from water, purification of liquids and easier use of the apparatus.

Description

The invention relates to the field of purification of liquids from impurities by filtration and can be used in systems of industrial and domestic purposes and to monitor the state of the natural aquatic environment, followed by determining the concentrations of certain elements.

A filter for providing drinking water and a method for using it are known [R. No. 2279910, MPK VON 20/20; publ. 20.07.2006], comprising a housing with a supply pipe and a filtering substance located inside said housing.

The disadvantages of this filter and method are that the filter design in question does not provide for the presence of an element that limits the penetration of the filtering substance into the discharge pipe. Taking into account the fact that the filtering material is formed from at least a variety of filtering granules — particles of activated carbon based on wood, particles of activated carbon based on coal, particles of activated carbon based on peat, particles of activated carbon based on pitch, particles of activated carbon on the basis of tar and their mixtures, it is necessary to ensure the retention of such particles in a limited volume.

The known method and device for multistage filtration of a liquid; the device contains a chamber having an inlet and an outlet for the flow of a liquid, and three stages of its filtration, passing through which retention of mechanical suspensions and microorganisms takes place, as filters use microglass fibers and activated carbon [of the Russian Federation, item No. 2266253, IPC С02Р 1/28, publ. December 20, 2005 (prototype)].

The disadvantages of this filter and liquid filtration method are that the use of at least three filtration stages, represented by different filtering materials, can lead to a limitation of the flow rate of the liquid in a separate stage. In addition, a tight fit of the filtering material to the walls of the filter housing is not guaranteed, which can lead to the penetration of the primary solution into the area of the purified liquid, bypassing the filtering material.

There is also known a method of sorption of macrocyclic compounds on ILU [Macrocyclic compounds in analytical chemistry / Ed. Yu.A. Zolotov, N.M. Kuzmina. - M: Science, 1993. - 320 p.], Including the following scheme. A solution of thymol blue was prepared by dissolving an exact sample in a certain volume of distilled water with the addition of a certain amount (3 ml) of 0.05 M ΝαΟΗ. ILU was used as a sorbent. The mass of ILU tablets varied from 30 to 50 mg. The ILU was purified as follows: it was kept in a 0.1 M solution of sulfuric acid for 30 minutes, then washed with water until the pH was 4-5, dried in air, washed with acetone, and dried to an air-dry state. The study of the sorption of the dye was carried out in a static mode. The detection limit is 6x 10 ^-10 mol.

The disadvantage is the significant differences in the sorption properties depending on the form of the macrocyclic compound in the studied media.

The known method for the determination of iron in the form of a complex of iron (11) with 1,10-phenanthroline on polyurethane foams used as sorbents [S.G. Dmitrienko, L.N. Pyatkova, V.K. Runes. Optical sorption molecular spectroscopic analysis methods. Sorption of ionic associates of tris (1,10-phenanthroline) of iron (11) with polyurethane foams and its analytical application // Journal of Analytical Chemistry, 1996, V. 51, 6, p. 600-604 (prototype)], which consists in the following: in polyurethane foams based on ethers and esters, discs are knocked out with a metal punch, they are washed in 0.1 M sulfuric acid for 30 minutes to clean them from metal ions and organic compounds, then washed with water to pH 4-5 with acetone and air-dried, to the test solution containing iron, add 1 ml of 1.4 M hydroxylamine hydrochloric acid, 2 ml of 1-10-2 M 1,10-phenanthroline, ammonium acetate buffer with pH 5, 8, 5 ml of 0.4 M sodium perchlorate and water to a total volume of 25 ml. Then a polyurethane foam disk is introduced, mixed vigorously for 30 minutes, the disk is removed, pressed between sheets of filter paper, dried in air, and diffuse reflectance spectra are recorded. The detection limit is 0.005 μg of iron on the disk.

The disadvantages of the method include the multistage and duration of the method of determination, the complexity of obtaining sorbent and reproducible results, the impossibility of sorption concentration of iron from large volumes of solutions.

The technical result of the invention is to improve the quality and speed of the concentration of the desired elements, purification of liquids and ease of operation.

The technical result is achieved by the fact that in the method of manufacturing a cartridge for the sorption of elements of the uranium-thorium series, according to which the base is cut in the form of polyurethane foam discs, washing, drying and saturating these discs with the reactive substance, a new process is that sequential processing of polyurethane foam discs is carried out with solutions hydrochloric acid, Fe ^{+ 2} compounds, ammonium hydroxide at pH 8, then potassium permanganate and Mn ² compounds, to form a mixture of iron oxyhydrate and manganese dioxide in soo With a ratio of 5: 1.

Also new is the fact that the device for filtering water of different genesis contains a cartridge manufactured by the above method.

- 1 020502

Comparative analysis with the prototypes made it possible to identify a set of essential features in relation to the technical result for each of the claimed objects set forth in the formulas. Therefore, each of the claimed inventions meets the criterion of novelty.

Signs that distinguish the proposed technical solutions from the prototypes are not identified in other technical solutions when studying data and related areas of technology and, therefore, provide the proposed solutions according to the criterion of inventive step.

In this application for the grant of a patent, the requirement of unity of the invention is met, since a device for filtering water of various genesis and method of preparing the sorbent material is claimed. The claimed inventions solve the same problem, due to the same technical result in the implementation of the inventions - improving the quality and speed of the concentration of the desired elements, cleaning liquids and ease of operation.

The invention is illustrated by drawings

FIG. 1 is a drawing of a filtering device. FIG. 2 shows a general view of the filtering device. FIG. 3 is a longitudinal section of the assembly column of the device. FIG. 4a, b - the upper and lower parts of the sorption container.

A device for filtering water of various genesis (Fig. 1) consists of a funnel (1), a combined column (2), the whole structure is installed on the receiving device (3) using an adapter (4) that is screwed onto the neck of the receiving device. A sorption container with a grate bottom (5) and a lid (6) is installed inside the column. If necessary, the number of containers can be increased. The whole structure is assembled as a pyramid, and the connecting parts of the upper part enter the lower part, thereby preventing water from leaking out of the device. The whole structure is reinforced with the help of three rods (7) installed on the outside of the structure. Parts are fixed with screws (8). Filtering is carried out using a vacuum pump (9), which is attached to the receiving device (3).

The sorbent material used in the inventive device is a synthetic material previously impregnated with organic and inorganic substances, for example a mixture of oxyhydroxide Pe (III) and MnO ₂ oxide.

All reagents must have a classification not lower than ch.d.a. and comply with the regulations of GOST and technical conditions.

The prepared base, usually a PPU plate with a thickness of 1 cm and dimensions of 100 by 100 cm, is placed in a suitable container, for example, a crystallizer, 3 liters in volume, into which a solution of HC1 is pre-poured, with a concentration of 3 M, and 1.5 liters. Carefully and slowly, the PPU plate is immersed in the solution until it is completely wetted. After that, the plate is squeezed out using special rollers, washed with a large amount of running water to flush away dissolved dirt and mechanical mud with polyurethane foam. After that, the washed and pressed plate is again lowered into the crystallizer with a fresh acid solution, where the full saturation of the polyurethane foam with hydrochloric acid occurs. Then the plate is squeezed from an excess of acid and placed in a crystallizer with a solution of iron salt, the concentration of which in the crystallizer is 15 μg / l. The PPU plate, impregnated with a salt of iron, becomes light yellow in color. After that, the plate is easily wrung out from excess reagent, placed in ammonia water (distilled water with ammonia added to pH ~ 8) and completely moistened with this water with constant stirring. When this occurs, the process of oxidation of iron (11) to iron (111) with the formation of iron oxyhydroxide and the PPU plate acquires a light brown color.

After that, the already painted PPU plate is placed in a bath with potassium permanganate solution, the concentration of the latter should be 1 g / l. The plate is completely immersed in the solution and, with stirring, evenly turns dark purple. After that, practically without pressing, the plate is transferred to the crystallizer with the salt solution Μη (ΙΙ), where the final stage of formation of the sorbent material takes place, which is indicated by the color transition to a dark brown color due to the reduction of the permanganate ion to manganese dioxide. In the last solution, the PPU plate is very thoroughly mixed with the solution and impregnated until the violet color completely disappears.

The finished plate is squeezed, thoroughly washed with water to remove loose sediment particles. Then placed in a drying chamber for further drying.

After the mold is dried, suitable cylinder disks are cut out of the plate, which are then packaged for transportation or storage in an appropriate container.

A device for filtering water of different genesis is assembled and working as follows: first, a filtering device is assembled from component parts (1, 2 and 4), a sorption container (5) is placed into it, which is a cylinder with a grate bottom and a lid (6) filled with sorbent material, and all this is wound on the neck of the receiving device (3). The pump (9) is connected to the nozzle (10) of the receiving device (3) and the water sample is filtered, which is fed into the funnel (1). The filtration rate is regulated by the vacuum created in the receiving bottle. After passing the required amount of water (3-8 liters), the cartridge is removed and

- 2 020502 is packed in a plastic cellular container for subsequent transportation. Such packaging should ensure the safety, integrity and purity of the sorption element during transportation before and after use.

Example 1

Polyurethane foam (PUF) was used as the basis for the sorbent material for concentrating elements of the uranovotorium series. PU foam was processed according to the procedure described above, i.e. consistently with solutions of the reacting substances: HC1, Ee (11), ΝΗ ₄ ΟΗ, ΚΜηΟ ₄ , Μη (). At the end of the treatment process, the resulting sorbent material was thoroughly washed with water, then dried. Shelf life in appropriate storage conditions - 5 years. The resulting sorbent material is stable when operating in the ambient air temperature range from -40 to + 80 ° C, easy to use, easy to dispose of, has a low cost, does not deform during the preparation of the sorbent material and in the filtering process. Immediately before work, soak in water for 10 minutes. Before filtering in a sample of water, bring the pH to ~ 8 with ammonia solution (conc.).

Example 2

As a basis for the sorbent material for the concentration of elements of the uranium-rotor row, silica gel of a certain granulation was used (the optimal grain size is 3 μm). Silica gel was saturated with the reactant according to the procedure described above. A significant drawback of the sorbent material obtained is the obligatory hermetic packing of silica gel into a fabric pouch having a pore size of less than 3 microns, in order to eliminate its precipitation into the filtrate. In spite of this, it can be used for a static concentration mode, i.e. direct addition in the form of a dry material to the water sample, followed by shaking and separating the separated layer of liquid over the sorbent material.

Example 3

Synthetic fiber (rayon, polyamidacryl, etc.) was used as the basis for the sorbent material. The fiber was saturated with the reactant according to the procedure described above. As a result of processing, the fiber fell into a clump, which unevenly covered the filtering area, i.e. the lattice (6) was not completely closed, therefore, unfiltered sample flowed into the receiving device (3).

The advantages of the inventive device for filtering water of different genesis and the method of preparing the sorbent material are that the filtering device is universal, since it can be used to concentrate a significant list of substances dissolved in water. The device is easy to operate and transport. Does not require highly skilled operator. The use of the proposed device will significantly expand the field of monitoring of aquatic ecosystems, reduce the volume of samples transported and speed up the analysis of the objects under study.

In addition, the sorbent material is a ready-made billet, which can be placed in the sorption container without additional preparations, and the shape can be set arbitrarily depending on the filtering device used.

Claims (2)

CLAIM 1. A method of manufacturing a cartridge for sorption of elements of the uranium-thorium series, according to which the base is cut in the form of polyurethane foam disks, rinsing, drying and saturating these disks with the reactant, characterized in that the polyurethane disks are sequentially treated with hydrochloric acid solutions, Her compounds, ammonium hydroxide at pH 8, then potassium permanganate and Μη + ² compounds to form a mixture of iron oxyhydrate and manganese dioxide in a ratio of 5: 1. 2. A device for filtering water of various genesis, containing a cartridge made by the method according to claim 1.