RU2077955C1 - Method and apparatus for liquid heterogeneous system separation - Google Patents

Abstract

FIELD: separation of liquid mediums with heterogeneous additions. SUBSTANCE: separation is exercised using liquid systems passing through column, that has dispersion material with particles size of 0.1 - 3.0 mm and inhomogeneous surface and polarized by electric field with intensity of no less than 1 V/cm. Apparatus for liquid heterogeneous systems separation has electrical sorption column filled with sorbent of no more than 95 % of volume and provided with feeding, removing and draining pipelines. In the case draining pipeline capacity of passage at least is three fold higher, than feeding pipeline capacity of passage. Removing pipeline is located in upper part of body forming clearance between it and sorbent. EFFECT: increase quality of separation. 9 cl, 1 dwg, 7 tbl

Description

 The invention relates to the field of physicochemical means for the separation of heterogeneous systems, and in particular to methods and devices for purifying a liquid, in particular water, from heterogeneous impurities.

 The prototype of the claimed invention are the method and device described in Japanese application N 63-7117, 1989, which proposes to combine the advantages of filtration and electrolytic methods.

 The device comprises a housing in which two electrodes are installed, between which a nozzle is placed, which ensures both the flow of filtration and the release of metal ions under the action of electrolytic processes, which provide additional water treatment due to adsorption and flocculation processes.

 The disadvantage of the prototype is the enrichment of water with undesirable substances, the need for purification from the released substances, low resource working filter elements.

 The objective of the invention was to create a simpler, more efficient installation of a method for cleaning liquids from impurities.

 The problem is solved by a method consisting in passing a fluid to be cleaned through a container filled with dispersed non-conductive material having a non-uniform surface with a particle size of 0.1 3.0 mm, which is polarized by an electric field with a voltage of at least 1 V / cm.

The indicated minimum field strength provides an effective purification of a liquid (water) heavily contaminated with bio- and oil products, when it is pumped at a space velocity of up to 20 h ^-1 . At higher fluid rates or increased requirements for purified water, the effective field strength is set based on the characteristics of the medium being cleaned.

 Fragments or granules of ceramics, in particular ferroceramics, ion exchange resins, pieces of polymeric materials, for example, granules of polyvinyl alcohol with inclusions, quartz, sand, dispersions of cellulose, chitosan, shungite, etc., are used as dispersed material.

 The presence of surface inhomogeneities of both a chemical and geometric nature is necessary for the purification of a liquid, the mechanism of which is based on the ingress of particles contained in it when passing through a material into zones with different values and signs of a charge, as well as amplification of flow irregularities in a liquid.

 As a result of the first process, electrically non-polar particles contained in a liquid are uneven in volume, which sharply enhances their coagulation, and processes leading to flow irregularities provide the appearance of "stagnant" zones in the filter material, where these conglomerates are delayed, further increasing the degree of heterogeneity material and, accordingly, separation efficiency. This is proved, in particular, by the fact that the best results were achieved when separation was carried out in a field, the intensity of which at the beginning of operation (the first 10 minutes) exceeds the working one by more than 5 times, which allows for optimal charge distribution.

 For aqueous systems, the optimal speed of passage of the cleaned mixture through a polarizable material (PM) is 0.1 to 20 cm / s, however, deviations from these parameters are possible, based on the properties of the components to be separated (for example, when switching to viscous liquids).

 These materials can be used individually, in a mixture with each other and in combination with other traditional materials. The use of larger dispersed particles reduces the processing efficiency due to a decrease in their surface area and the volume of stagnant zones, the use of more dispersed particles leads to an undesirable increase in hydrodynamic resistance and also to a decrease in the volume of stagnant zones.

 To implement the method, a device was created, a diagram of which is shown in the drawing.

 The device consists of a housing 1, in the inner container of which electrodes 2 are installed and a polarizable material (PM) 3 is placed, occupying no more than 95% of its volume. The housing is equipped with pipelines 4 6, of which pipeline 4, equipped with a valve 7, is connected to a water source (inlet 16), pipeline 5 (outlet) is located above the PM level and is connected to a tap or tank for storing purified water 8, pipeline 6 with a valve 9 connects the housing to the drain 10. Polarization is carried out using block 17.

 An additional container with a regenerating solution 14 can be connected to the housing 1 through a valve 12 and a pipe 13, as a solution of detergents, solvents, alkalis, acids, etc., depending on the properties of the liquids being cleaned and the nature of the impurities. At the inlet and outlet, the housing can be additionally equipped with electrode cells 15, designed to clean the liquid from ionized impurities, degradation of the sludge and prevent the entrainment of PM.

 The distinctive features of this device, along with the placement of a material capable of polarization in a volume of not more than 95% of its volume, is the installation of an output pipe 5 in the upper part of the housing 1 while at the same time exceeding the throughput of the drainage pipeline by at least 3 times the input parameter .

 The device operates as follows.

 PM 3 is poured into the housing 1, voltage is applied to the electrodes 2, after which the liquid through the valve 7 and the inlet pipe 4 enters the lower part of the housing, and then, passing through the PM, completely (or partially) fills the upper part of the housing and enters through the output pipeline 5 for consumption.

 The impurities contained in it during passage through the PM under the influence of an electric field are electrified, coagulated and sorbed by the upper layers of PM 3.

 To regenerate the sorbent, the power is usually turned off or the electrodes 2 are switched on and the valve 9 of the pipeline 6 is opened. Moreover, due to the difference in the throughput of the pipelines, the liquid from the pipeline 4 enters the pipeline 6, and the PM is freed from adsorbed contaminants by a combination of repelling charged impurities from PM particles that have changed sign when switching the field of electrodes, with washing the PM with a layer of absorbent liquid 11 or simply washing them off (when the current is turned off).

 If it is necessary to reduce fluid loss during regeneration, valve 7 is shut off before opening valve 9. It is possible to regenerate only the liquid contained in the PM column that is contained in the housing as a result of opening valve 12. In this case, use smaller pipelines 4 and 6 or reduce the volume of flushing liquid less than 1 10 with respect to sometimes it does not provide a sufficient degree of regeneration to the volume of PM without the introduction of special cleaning agents. The latter, if necessary, come from the tank 14 when opening the valve 7.

 Further operation of the device is carried out by simply closing the valve 9 and, if necessary, the valve 12 and opening, if it was closed, the valve 7.

 The specified regeneration scheme in relation to the material of the declared nature allows, in particular, to carry out water purification for at least two years without changing the sorbent material.

 During industrial tests of the device, which received the name "Cascade", it was shown that with small dimensions (weight 5 25 kg) it allows cleaning of liquids with a capacity of up to 100 l / h, ensuring complete removal from the water of both mechanical and almost any organic impurities from microorganisms to petroleum products, as well as from toxic materials to the permitted level.

 In addition, if necessary, it can be easily converted to produce cathode or anode ("living" or "dead") water.

 The practical applicability of the method and device is illustrated by examples.

 Example 1

Water taken from the Neva River (St. Petersburg) in the winter mooring area of ships from a depth of 5 m was passed through a column containing ferroceramic granules with a dielectric constant of 15,000 placed in a constant electric field of strength 1,200 V / cm. The volume of the working chamber was 1x1x50 cm ³ , the water flow rate of 0.5 2500 forces / h 0.1 50 h ^-1 /, the granule size of 0.25 0.4 mm

Water analysis was carried out by turbidity using an SF-26 spectrophotometer (LOMO Rossiya company) at λ 460 nm, as well as by plating on nutrient media in order to determine coli index and total microbial contamination (OMO). Sowing was carried out by placing 0.1 ml of liquid in Petri dishes with nutrient media (Endo, meat-peptone agar, etc.) and incubating them for 24 hours at 36 -38 ^o C.

 The cleaning results are shown in table. 1, from which it follows that unsuitable drinking water contaminated with microorganisms after said treatment meets the requirements for drinking water, being essentially sterile.

 Example 2

In the conditions of example 1, using as a nozzle a material based on Nb ₂ O ₅ with a dielectric constant of 4000 and at E 100 V / cm, an artificial mixture was pumped at a rate of 1 h ^-1 containing 100 mg of a petroleum product mixture per 1 liter of tap water, consisting of engine oil M-5 (10%), M-10 (10%) M-20 (10%), fuel oil (20%), diesel fuel (50%).

 The water-hydrocarbon mixture was homogenized using a magnetic stirrer and fed into an electrocolumn. Every 30 minutes, filtrate samples were analyzed using a laser spectrometer for the total content of petroleum products.

When the filtrate characteristics deteriorated, saline water containing 1–4% NaCl or KNO _{3 was} pumped in the opposite direction through the electrocolumn in the opposite direction for 0.5–10.0 min. The nature of the regenerating solution practically did not affect the efficiency of the process.

 The effectiveness of water purification from petroleum products is given in table. 2 and 3.

 Example 3

 In the conditions of example 1, the sea water of the Gulf of Finland was purified from impurities of oil products. Regeneration was carried out with a 2% NaCl solution, E 10 V / cm. The results are shown in table. 4.

 Example 4

имитировали вариант аварийного выброса в природный водоем сточных вод, для чего использовали суспензию клеток E. coli М-17 в концентрации 2,2•10⁹ кл./мл. После проведения очистки при E 150 В/см при скорости подачи 1 ч^-1 в пробах роста E.crli не обнаружено, что свидетельствует о полной очистке воды от микроорганизмов в данных условиях.In the conditions of example 1, using ferroceramics based on the material T-10000, coated with a film of polyvinylpyrrolidone 1000 thickness

They simulated a variant of emergency discharge of wastewater into a natural water body, for which a suspension of E. coli M-17 cells at a concentration of 2.2 • 10 ⁹ cells / ml was used. After purification at E 150 V / cm at a feed rate of 1 h ⁻¹ , no growth of E.crli was found in the growth samples, indicating a complete purification of water from microorganisms under these conditions.

 Example 5

Spent the breeding of influenza A virus / Texas / 1024 GE / 0.2 ml / and ballast proteins in the virus-containing allantoic fluid of chicken embryos (IMPORTANT). Distribution conditions: polyvinyl alcohol granules with their ratio of 8 1 ferroceramics with inclusion, field strength 50 V / cm, flow rate 0.15 cm / s, regenerating solution or eluent: 0.1 M phosphate buffer, against 0.5 n. NaCl at pH 8.5. The output of the active virus is 82%, which indicates complete carrier regeneration, the degree of protein purification is more than 40 times (0.05 mg / m protein in the viral fraction instead of 2.1 mg / ml in the initial IMPORTANT), the protein yield in the ballast fraction 93 %
Example 6

The blood cells and plasma proteins from citrate blood were separated, except that the flow rate was 0.1 h ^{−1 and the} pH of the second eluent was 7.5. The separation conditions are similar to those taken in Example 5. Protein yield 96% cell mass yield 78% protein purification from cells 68 times.

 Example 7

A suspension of Sach yeast cells was passed through an electrocolumn, as in Example 1, filled with granules of the “sphadex G-15” sorbent, Pharmacia Sweden. cerevisiae at a concentration of 3 • 10 ⁸ cells / ml, containing 30 mg / l FeCl ₃ . When applying an electric field with E 40 V / cm, the concentration of iron ions in the filtrate fell to the level of 1 2 mg / L. The concentration of yeast cells in this case decreased by about 10 ⁶ times.

 Example 8

Through the electrocolumn of example 1, filled with a combined filler based on T-10000 ferroceramics, wastewater was passed from the city system. The output was controlled by the content of microbial cells and phosphates, the initial levels of which were 3 • 10 ⁷ cells / ml and 11 mg / l. When applying an electric field with a strength in the range of 10 50 V / cm, the concentration of microorganisms decreased to zero, and the phosphate level dropped to 0.2 mg / L.

 Example 9

Through the electrocolumn of example 1, filled with a dispersion based on chitosan, water was passed containing flakes of oxides in a concentration of 0.5% iron and 1% CuSO ₄ . At the output, the content of the components was controlled by the photometric and sitrometric method. The filler was saturated with dissolved components in the absence of a field. When applying an electric field with a strength in the range of 5 -20 V / cm, the concentration of iron oxides in water decreased almost to zero, and the ionized components by 9 10 times. When removing the field, the concentration at the outlet of the electrocolumn increased, exceeding the initial level, which indicated the regeneration of the filler. Upon repeated application of the electric field, the effect of cleaning the aqueous solution was repeated.

 Example 10

A suspension of E. coli K-12 cells at a concentration of 5 × 10 ⁹ cells / ml was pumped through an electrocolumn with crushed schungite, whose anode is approximately 100 times larger than the cathode. At the output of the electrocolumn, the cell concentration and the pH of the liquid were monitored. The average electric field strength was set in the range from 50 to 200 V / cm. In all cases, the effect of complete purification of the liquid from microbial cells was observed, however, the pH of the medium depended on the electrical mode of operation (see Table 5).

 Example 11

A suspension of Bac cells was pumped through a crushed quartz electrocolumn. thuringiensis at a concentration of 2 • 10 ⁸ cells / ml. The electric field was set at 10 V / cm. The concentration of cells at the outlet of the electrocolumn was reduced to 5 • 10 ⁶ cells / ml. After that, the cleaning process was repeated under the following conditions.

 For 1 min, a voltage of 150 V / cm was established between the electrodes of the column, and then it was reduced to 10 V / cm, as in the first part of the experiment. As a result, no cells were observed at all at the output of the electrocolumn.

 Example 12

In the conditions of example 8, wastewater from an urban sewer system was passed through an electrocolumn. Identical electrode cells with an effective electrode area of 1200 cm ² and a volume of 50 cm ^{3 were} installed at the inlet and outlet of the electrocolumn. The cells were connected to a power source parallel to the electrocolumn. In addition to example 8, the amount of sludge in the drainage (per 1 liter of treated effluents), chlorides and nitrates in the filtrate was controlled. The results are shown in table. 6.

Claims (9)

 1. The method of separation of liquid heterogeneous systems, including passing liquid through a filter material placed in an electric field, characterized in that the liquid is passed through a dispersed material with a particle size of 0.1 3.0 mm, having an inhomogeneous surface and placed in an alternating electrical field with a strength of at least 1 V / cm.  2. The method according to claim 1, characterized in that ferroceramics are used as filter material.  3. The method according to claim 1, characterized in that as the filter material using sand or crushed quartz.  4. The method according to claim 1, characterized in that shungite is used as a filter material.  5. The method according to claim 1, characterized in that dispersions based on chitosan or resins are used as filter material.  6. The method according to PP.1 to 5, characterized in that at the beginning of the separation for 0.5 to 10 minutes using an electric field with a strength of more than 5 times the operating value.  7. Device for separating liquid heterogeneous systems, consisting of a housing containing electrodes installed in it, connected to a direct current source, and filter material, as well as a piping system including inlet and outlet pipelines, characterized in that the filter material is in the form of dispersed particles with a non-uniform surface of polarized material is placed in the housing in an amount of not more than 95% of its volume, the discharge pipe is located in the upper part of the housing, providing a gap between it and the upper m layer of filter material, and below the lower part of the filter material, the casing is equipped with a pipeline connected to a drainage having a throughput of at least 3 times higher than the supply pipe.  8. The device according to claim 7, characterized in that it is additionally equipped with a tank with a regeneration solution connected by a pipeline equipped with a valve connecting the tank with the upper part of the housing.  9. The device according to PP.7 and 8, characterized in that at the input and output of the housing additionally installed electrode cells.

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