Method for preparation of filter-sorption material

FIELD: technological processes; chemistry.

SUBSTANCE: method for preparation of filter-sorption material includes application of silica-alumina mineral on substrate. Substrate used is basalt fibers, and silica-alumina mineral is bentonitic clay with montmorillonite content of at least 80%. Basalt fibers are processed by 5-7% water solution of alkali, bentonitic clay that has been previously exposed to soda activation is added, then mixed with addition of binding agent selected from aluminium salts, at ratio of bentonitic clay and binding agent equal to 1:3, heated at temperature of 50-100°C for 2 hours, material is cooled, flushed by water and exposed to thermal activation at the temperature of 110-120°C.

EFFECT: higher sorption capacity of filter-sorption material capable of regeneration, and expansion of material application sphere.

3 tbl

 

The invention relates to a method for filter sorption material and can be used in chemical, metallurgical or pulp and paper industry, the electroplating industry wastewater treatment for removing heavy metal ions, mainly ions of lead, chromium and iron.

A method of obtaining sorption-filtering material, including the processing of bentonite clay, previously subjected to a heat and acid activated sequentially with solutions of salts of divalent manganese and potassium permanganate (RF Patent No. 2229336, IPC 01J 20/12, B01J 20/06, publ. 2004).

The disadvantage of this method is the narrow field of use due to the use for water purification from iron ions.

The closest in technical essence and the achieved result is a method for filter sorption material, comprising applying to the substrate of aluminosilicate mineral. This application aluminosilicate mineral carry out hydrodynamic method, the substrate used is porous, in particular, ceramic cartridges, as aluminosilicate mineral is used, for example, vermiculite, glauconite, pyrolusite or diatomite (Kuznetsov Basics of water purification from radioactive contamination / Yevtushenkov, Vonderembse, A. Trusov. - M.: Atomizdat, 1974. - P. 203).

The disadvantages of the described method are the low efficiency of treatment and the short period of the cycle due to the low sorption capacity of the filter-sorptive material, due to the small specific surface and poor adhesion to the substrate and aluminosilicate mineral due to hydrodynamic deposition, which leads to the entrainment of mineral in the process of working with the substrate surface, causing the need for periodic replenishment of aluminosilicate minerals, the inability to regenerate after working sorption capacity, which necessitates disposal of material after each cycle of wastewater treatment, as well as a narrow field of use due to the application for removal of radioactive ions of metals.

The invention solves the problem of increasing the sorption capacity of the filter-sorptive material, the possibility of regeneration and expansion of use.

To achieve the technical result in the production method of the filter-sorptive material, comprising applying to the substrate of aluminosilicate mineral, as a substrate using basalt fiber, and as aluminosilicate mineral used bentonite clay containing montmorillonite is not less than 80%, when it is basalt fiber handle 5-7% aqueous solution of alkali, add bentonite clay, previously subjected soda activation, stirred mechanically with the addition of a binder in the form of one of aluminum salts in the ratio of bentonite clay and a binder component, equal to 1:3, is heated at a temperature of 50-100°C for 2 h, and then the resulting material is cooled, washed with water and subjected to thermal activation at a temperature of 110-120°C.

The increase in sorption capacity of the filter-sorptive material, caused by the use of basalt fibers with advanced structure, high specific surface area and the presence of strong coupling bentonite clay with basalt fibers, the possibility of multiple regeneration, helping to create a closed water cycles and water reuse in industrial processes, and expanding the use of provided that the substrate using basalt fiber, and as aluminosilicate mineral used bentonite clay containing montmorillonite is not less than 80%, while basalt fiber handle 5-7% aqueous alkali solution, add bentonite clay, previously subjected soda activation, stirred mechanically with the addition of a binder in the form of one of aluminum salts with the respect of bentonite clay and a binder component, equal to 1:3, is heated at a temperature of 50-100°C for 2 h, and then the resulting material is cooled, washed with water and subjected to thermal activation at a temperature of 110-120°C.

High speed and completeness of ion exchange reactions on the surface of the proposed filter-sorptive material is achieved through the use of bentonite clay containing montmorillonite is not less than 80%, subjected to preliminary soda activation. High content of montmorillonite leads to high ion-exchange capacity of the bentonite clay. Soda activation leads to an increase of the active surface of montmorillonite and accelerates the reaction rate of ion exchange, which allows the cleaning process at high speeds, thus reducing the adhesion of the particles of the mineral and the solvate shell extractable heavy metal ions are well kept on its surface, providing a high cleaning effect even at low concentrations of pollutants in the wastewater.

This material provides high efficiency in a wide range of concentrations of heavy metal ions in waste water and its application reduces operating costs. The proposed material can purify wastewater to the maximum permissible concentrations, which allows you to use the e is for water purification.

The higher efficiency of cleaning provides a high ion-exchange capacity of montmorillonite, part of bentonite clay, and due to the fact that basalt fibers with a diameter of from 0.5 to 3 μm, the surface area approaching the inside area. This structure basalt fibers allows the same unit volume of the filter-sorptive material to obtain a much greater surface area of the exchange. The matrix of the adsorbent, in which the nodes are active centers, is more affordable, and the utilization of the working surface it high.

The application of the proposed filter-sorptive material can reduce the production area by improving the efficiency of wastewater treatment plants. The consumption of the apparatus can be reduced through the use of this filter sorption material with negligible weight.

When using basalt fibers operating costs of the washing, loading, and transportation of the material is significantly reduced compared with the use of heavy loads due to low resistance (lost power) and low density of the proposed filter-sorptive material.

The regeneration process of the material is characterized by simple is that and low cost. For example, in the case of water purification of lead ions from the filter-sorptive material regenerate 5-8% solutions of caustic soda or sodium chloride, which considerably reduces the cleaning process. Regeneration when removing chromate ions (anion exchange) spend 4-6% sodium hydroxide solution. Thanks to the highly developed surface and low resistivity material, a rapid saturation of the filter-sorptive material by ions of the above salts, reduces the time and cost of recovery. The filter-sorptive material can be regenerated many times, thus there is a slight decrease in sorption capacity, which is 2-5%. The washing water with high content of lead ions and chromium can be used as a commercial product that allows you to reduce the discharge of toxic substances into water bodies, save valuable raw materials, and create enterprises closed water circulation loops.

Expansion of use is achieved through the possibility of applying the proposed material for water purification from metal ions, for example, the CA2+, Mg2+, Mn2+Ni2+, oil, polyvinyl alcohol, humic and fulvic acids, sparingly soluble organochlorine pesticides, isotopes:90Sr91Y95Zr,134Cs144Ce147 Pm,235U and products of their division. All this makes it a universal filter-sorptive material for wastewater treatment in many industries.

Processing of basalt fibers 5-7% aqueous solution of alkali increases the adhesion of bentonite clay on the surface of basalt fibers. When leaching specific surface basalt fibers significantly increases due to the formation of pores, resulting in partial dissolution of the metal oxides included in the composition of basalt fibers. The use of 5-7% aqueous alkali solution is optimal. When the concentration of the aqueous alkali solution is less than 5% is incomplete and long-term dissolution of the oxides of calcium, magnesium and iron that are included with basalt fibers. When the concentration of the aqueous solution of alkali over 7% - dissolution is faster, but it causes a decrease in strength of basalt fibers, since there is a partial destruction of the skeleton of the silicon dioxide, and unnecessary consumption of reagent leaching.

Increase the efficiency of wastewater treatment is provided through the use of soda activated bentonite clay, increasing the sorption capacity due to the increase in porosity and increase in specific surface bentonite clay.

Adding a binder is omponent in the form of one of aluminum salts contributes to the increase of the adhesion forces between basalt fiber and bentonite clay at the expense of complex compounds, formed by the interaction of the binder component with the surface of basalt fibers and montmorillonite. The result is a thin layer of montmorillonite is well fixed on the treated 5-7% aqueous solution of alkali surface of basalt fiber, which prevents the entrainment of bentonite clay with a stream of treated water.

The ratio of bentonite clay and a binder component, equal to 1:3 is optimal, as it is with the high dosage of the binder component provides maximum surface contact bentonite clay with the surface of basalt fibers. When applying the smaller the ratio is incomplete reaction of complex formation with aluminum, forming part of montmorillonite (octahedral layer montmorillonite), this reduces the strength of the applied layer of montmorillonite on the surface of basalt fibers. Use a larger ratio results in excessive reagent and adhesion of particles due to coagulation of an aluminum salt in an aqueous alkali solution.

Heating at a temperature of 50-100°C for 2 h is optimal, so as to ensure complete reaction of dissolution of the binder component and a hydrogenation montmorillonite, necessary for the formation of complex compounds and relationships on the surface of montmorillonite and basalt the fibers. Heating at a temperature below 50°and a short time does not ensure complete dissolution of the binder component and the best hydrogenation of montmorillonite, which reduces the filtering qualities of the material obtained. Heating at temperatures above 100°and more time is not conducive to the improvement of the properties of the obtained material, but increases the cost.

Thermal activation can increase the adhesive strength of the binder component with basalt fibers and montmorillonite, and also increases the porosity of bentonite clay.

Conducting thermal activation at 110-120°C is optimal for the formation of pores of various sizes, which allows for the simulation of wastewater treatment processes depending on the radii of ions of heavy metals. At temperatures above 120°reduces pore size bentonite clay and, therefore, the decrease of the sorption capacity of the filter-sorptive material and the reduction of the period of the work cycle.

The invention is illustrated by tables, where table 1 shows the dependence of the efficiency of cleaning solution from the ions of chromium(VI) and duration of the work cycle on the filter-sorptive material from different initial concentration of chromium(VI); table 2 shows the same, PR is the condition for receiving the filter-sorptive material with the use of bentonite clay, not subjected soda activation; table 3 shows the same, subject to obtaining the filter-sorptive material without the use of soda activation, adding a binder and conducting thermal activation.

The method of obtaining the filter-sorptive material is as follows.

On a substrate applied aluminosilicate mineral. The substrate uses basalt fibres with a diameter of 0.5-3 μm, and as aluminosilicate mineral used bentonite clay containing montmorillonite is not less than 80%.

Bentonite clay is subjected to soda activated by any known method.

Basalt fiber is treated with 5-7% aqueous solution of alkali, e.g. sodium hydroxide or potassium hydroxide, is placed in a flask and add bentonite clay, previously subjected soda activation. Mix mechanically with the addition of a binder in the form of one of aluminum salts, such as chloride or sulfate, with a ratio of bentonite clay and a binder component, equal to 1:3. Heated at a temperature of 50-100°C for 2 h, and then the resulting material is cooled, washed with water and subjected to thermal activation at a temperature of 110-120°C.

A specific example of the proposed method.

Bentonite clay is subjected with the new activation. The original sample bentonite clay mass 15 g placed in a round bottom flask with a capacity of 250 ml with 200 ml of 5% sodium carbonate solution. When the concentration of the aqueous solution of sodium carbonate less than 5% is incomplete and long-term substitution of ions of calcium and magnesium in the crystal lattice of montmorillonite with sodium ions. When the concentration of the aqueous solution of sodium carbonate more than 5% of the replacement takes place fully, but this results in excessive reagent for activation and subsequently requires a more thorough cleaning of the residual ash. Stirred for 2 h on a mixer type THYS-2. After the flask is left in the day to complete the course soda activation. Then bentonite clay is separated from the coarse fraction insoluble clay substance and washed with distilled water to remove excess sodium carbonate.

The original sample of basalt fibres by weight of 50 g was placed in a flat-bottomed flask with a capacity of 500 ml and pour 300 ml of 5% aqueous solution of alkali, e.g. sodium hydroxide or potassium. Stirred to wet the entire surface of the basalt fibers and remove air trapped between the fibers. Add bentonite clay subjected soda activation, and stirred mechanically with the addition of a binder in the form of chloride or sulfate of aluminum with a mass of 5 g (when the ratio of the drop bentonite clay and a binder component, equal to 1:3). After stirring the flask is heated on a hotplate at a temperature of 80°C for 2 hours and Then the resulting material is cooled, washed with water until the absence of alkaline reaction. Lay out the material in a porcelain bowl and subjected to thermal activation in a drying Cabinet at a temperature of 110-120°within 2 hours.

High efficiency water purification filter obtained sorption material is illustrated as follows.

Aqueous solutions containing 0.5, 2.5 and 5 mg/l of potassium bichromate, individually passed through the filter column with a diameter of 90 mm with a speed of 5 m/h, loaded with 65 g of filter-sorptive material. In each case, the filter column load fresh filter-sorptive material. As a binder used aluminum sulfate. The results of the experiment are presented in table 1. From table 1 it is evident that the duration of the cycle decreases with increasing initial concentration of the solution, but the cleaning efficiency of ions of chromium(VI) is high at different initial concentrations of the solution.

Aqueous solutions containing 0.5, 2.5 and 5 mg/l of potassium bichromate, individually passed through the filter column with a diameter of 90 mm with a speed of 5 m/h, loaded with 65 g of filter-sorptive material. In each case, fil is revelou column load fresh filter-sorptive material. As a binder used aluminum sulfate. Used bentonite clay is not subject soda activation. The results of the experiment are presented in table 2. Table 2 shows that the duration of the cycle is reduced. This is due to the decrease in sorption capacity of the material due to the use of bentonite clay, not previously subjected to soda activation, contributing to the increase in the porosity of the material.

Aqueous solutions containing 0.5, 2.5 and 5 mg/l of potassium bichromate, individually passed through the filter column with a diameter of 90 mm with a speed of 5 m/h, loaded with 65 g of filter-sorptive material. In each case, the filter column load fresh filter-sorptive material. Used bentonite clay is not subject soda activation. Adding the binder component is not performed. The resulting material is not subjected to thermal activation. The results of the experiment are presented in table 3.

From table 3 it can be seen that the duration of the filtering cycle is significantly reduced. This is due to the decrease in sorption capacity of the material due to receipt of suboperator filter-sorptive material. No additives binder causes a partial ablation of the material flow PTS is returned water.

Thus, the proposed method allows to obtain the filter-sorptive materials with high sorption capacity, providing effective cleaning in a wide range of concentrations of heavy metal ions, to carry out the regeneration and expansion of use of the filter-sorptive material.

Table 1

The dependence of the efficiency of cleaning solution from the ions of chromium(VI) and duration of the work cycle on the filter-sorptive material from different initial concentration of chromium(VI)
The initial concentration of bichromate of potash in solution, mg/lThe amount of purified water V, lThe cleaning efficiency e, %The duration of the cycle τ, h
0,54095-997
2,51695-983
5,0493-980,75

Table 2

The dependence of the efficiency of cleaning solution from the ions of chromium(VI) and duration of the work cycle on the filter-sorptive material from different initial concentration of chromium(VI) without the applications of soda activation
The initial concentration of bichromate of potash in solution, mg/lThe amount of purified water V, lThe cleaning efficiency e, %The duration of the cycle τ, h
0,52990-915
2,51083-891,9
5,0262-780,4

Table 3

The dependence of the efficiency of cleaning solution from the ions of chromium(VI) and duration of the work cycle on the filter-sorptive material from different initial concentratie solution without the use of soda and thermal activation without the addition of binder - aluminium salts
The initial concentration of bichromate of potash in solution, mg/lThe amount of purified water V, lThe cleaning efficiency e, %The duration of the cycle τ, h
0,52586-894,3
2,5778-831,3
5,01,667-700,3

The method of obtaining the filter-sorptive material, including nasenyana substrate of aluminosilicate mineral, characterized in that the substrate using basalt fiber, and as aluminosilicate mineral used bentonite clay containing montmorillonite is not less than 80%, while basalt fiber handle 5-7%aqueous solution of alkali, add bentonite clay, previously subjected soda activation, stirred mechanically with the addition of a binder in the form of one of aluminum salts in the ratio of bentonite clay and a binder component, equal to 1:3, is heated at a temperature of 50-100°C for 2 h, and then the resulting material is cooled, washed with water and subjected to heat activation at a temperature of 110-120°C.



 

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