EA036588B1 - Solid composite reagent for treatment of aqueous solutions and method for aqueous solution treatment - Google Patents

Abstract

The invention relates to water treatment and water disposal procedures, and can be used for treatment of surface, underground, industrial, waste waters and other contaminated waters, using chemical reagents. The objective of the invention is development of compositions for solid composites and a method for treatment of aqueous solutions having a various contamination level, allowing for improvement of treatment efficiency: achieving the regulated parameters of the treated water quality while reducing the dose of chemicals injected and reducing the residual coagulant content. Said objective is attained by the use of a solid composite reagent for aqueous solution treatment in the form of powders, grains, tablets, pellets, containing a coagulant and a flocculant, at their mass ratio of 5:1 to 20:1, wherein aluminum sulfate or aluminum polyhydroxochloride is used as a coagulant, the coagulant particles dispersion degree being from 0.006 to 0.016 m-1, cationic flocculant is used as a flocculant, the flocculant particles dispersion degree being from 0.003 to 0.03 m-1, and additionally containing zeolite sorbent NaX in the amount of at least 31% of the total reagent weight, pH regulator sodium hydrocarbonate in the amount of at least 32% of the total reagent weight, decontamination agent sodium dichloroisocyanurate in the amount of at least 6% of the total reagent weight, wherein zeolite NaX particles have a dispersion degree of 0.02 m-1, the dispersion degree of sodium hydrocarbonate is 0.008 m-1, and the dispersion degree of dichloroisocyanurate is 0.014 m-1. The proposed invention includes a method for treatment of aqueous solutions using a solid composite reagent as claimed in claim 1, comprising injection of the solid composite reagent to the treated water being mixed intensely during 0.5-1.5 min at a speed gradient of 40 to 370 s-1, which ensures formation of floccules with an average size from 200 to 1,550 m at the stage of slow mixing.

Description

The invention relates to the processes of water treatment and wastewater disposal and can be used for the purification of surface, underground, technological, waste and other contaminated waters using chemical reagents.

The main stages of reagent technologies for the purification of aqueous solutions are the processes of coagulation, flocculation, sorption and disinfection [1]. In most cases, these stages are carried out by sequentially introducing reagents in the form of powders, granules, tablets, suspensions, or aqueous solutions into polluted water [2]. The latter method is most widely used in the treatment of large volumes of surface and waste water [3]. Despite the apparent correctness of water treatment with pre-prepared aqueous solutions of reagents, this method has a number of significant disadvantages:

the use of large quantities of previously purified water for the stage of dissolving reagents;

the presence of large containers and storage facilities for storing solutions;

increased requirements for the chemical resistance of container materials to acidic solutions of coagulants (mandatory anti-corrosion coating of the inner surfaces of containers for storing acidic solutions of coagulants);

aging of solutions of coagulants and flocculants during their long-term storage, leading to deterioration of their coagulation-flocculation properties and precipitation.

The known method of sequential dry dosing of reagents: disinfecting tablets [4], powder sorbents and coagulants [5-8], introduced into the treated water at different stages of its purification. The disadvantage of this method is the need for separate introduction of reagents at different points of the technological process of water purification, which significantly complicates and increases the cost of the purification process as a whole [3].

To eliminate the disadvantages of the above-described wet and dry dosing methods, it is proposed to premix the reagents and obtain liquid or powder compositions. Known formulations and methods for obtaining liquid coagulating-flocculating compositions MOF based on polyoxychloride aluminum grades Aqua-Aurat 18 and Aqua-Aurat 30 and cationic flocculants [9]. The disadvantage of such systems is that when mixing solutions of a coagulant with solutions of flocculants, before their interaction with contaminated water, the flocculant begins to react with the still unformed coagulation products, which reduces their coagulation ability in relation to water pollutants and leads to an increase in the dose of coagulant required for cleaning water. It is known that between the onset of the action of the coagulant and the time of introduction of the flocculant should pass from 1 to 4 minutes [10-12]. If this condition is not met, then cleaning becomes ineffective and costly.

A known method of producing reagents by mixing an aqueous colloidal solution of aluminum pentahydroxochloride with a 0.1-1.0% aqueous solution of polyacrylamide [13]. This method also does not allow achieving a consistent effect of coagulant and flocculant on contaminated water with a time interval of 1-4 min. Therefore, when the solutions of these reagents are mixed, the positively charged colloidal particles of the coagulant interact with the negatively charged macroions of the flocculant, which prevents the process of neutralizing the surface negative charges of the particles of pollutants dispersed in the water being purified, and reducing the degree of its purification.

A known method of purification of natural and waste water using a reagent obtained by radical polymerization of acrylamide in aluminum hydroxochloride in the presence of oxyalkyl-tert-butyl peroxide [14].

Also known is a composite reagent for obtaining water for communal drinking purposes from natural surface sources [15]. It contains polyacrylamide gel (flocculant), aluminum sulfate and activated carbon.

The methods described in [12-14] for the preparation of composite reagents are complex and do not make it possible to regulate their composition depending on the parameters of the water being purified, which does not allow using these compositions as universal reagents for purifying waters of various compositions.

Known solid composition for the disinfection and purification of water based on polyhydroxochlorides of aluminum and dichloroisocyanuric acid, used as a disinfectant in the form of a single dosage package [16]. This composition is proposed for obtaining drinking water in the field and in conditions where there is no centralized water treatment system. The composition is expensive and is only intended for treating small volumes of water.

The prototype of the proposed technical solution is a pellet-shaped composition containing a coagulant based on multivalent metal compounds having a particle size of 25 to 2000 μm, and an organic polymer flocculant with a particle size of 10 to 750 μm [17]. Upon contact with water, the pellets are destroyed with the formation of a solution of a mixture of a coagulant with a flocculant. The disadvantages of such a molded composition are: a) high polydispersity of each of the components, which leads to uneven release of reagents into water and does not allow creating a uniform distribution of coagulant and flocculant in the volume of water; b) significant excess of particle sizes

- 1 036588 coagulant (2.5-2.7 times) in relation to the particles of the flocculant, which leads to their simultaneous dissolution and interaction with each other at the stage when the coagulation process is not completed. This determines the inefficiency of using this composition for the purification of large volumes of aqueous solutions at water treatment plants.

The objective of this invention is to develop compositions of solid compositions and a method for purifying aqueous solutions with varying degrees of contamination, allowing to increase the purification efficiency: to achieve standardized quality indicators of purified water, while reducing the dose of introduced reagents and reducing the residual coagulant content.

The problem is solved by using a solid composite reagent for the purification of aqueous solutions in the form of powders, granules, tablets, pellets containing a coagulant and a flocculant at a mass ratio of 5: 1 to 20: 1, and aluminum sulfate or aluminum polyhydroxochloride is used as a coagulant, the degree of dispersion of the coagulant particles is from 0.006 to 0.016 μm ^-1 , a cationic flocculant is used as a flocculant, the degree of dispersion of the flocculant particles is from 0.003 to 0.03 μm ^-1 , and additionally containing the sorbent NaX zeolite in an amount of at least 31% of the total mass reagent, pH regulator sodium bicarbonate in an amount of not less than 32% of the total mass of the reagent, disinfectant sodium dichloroisocyanurate in an amount of not less than 6% of the total mass of the reagent, and the particles of NaX zeolite have a degree of dispersion of 0.02 μm ^-1 , sodium bicarbonate - 0.008 μm ^-1 , sodium dichloroisocyanurate - 0.014 μm ^-1 . The present invention includes a method for purifying aqueous solutions using a solid composite reagent according to claim 1, which consists in the fact that the solid composite reagent is introduced into the water to be purified with vigorous stirring for 0.5-1.5 minutes with a speed gradient from 40 to 370 s ^-1 , providing the formation of floccules with an average size of 200 to 1550 microns at the stage of slow mixing.

Composite reagents of the specified degree of dispersion allow not only to fully preserve the coagulating ability of coagulants and flocculating ability of flocculants, but also to additionally obtain a synergistic effect, which consists in reducing the consumption of coagulant and reducing the content of residual aluminum in the treated water. The use of powders of coagulant and flocculant with a degree of dispersion outside the range specified in the claims leads to the loss of the synergistic effect and other advantages described above. The ratio of the masses of the coagulant and the flocculant given in the formula is optimal for the formation of rapidly sedimenting floccules. With a lower sorbent content in the composite reagent, the required degree of removal of dissolved pollutants is not achieved. The content of the pH regulator in the composite reagent in an amount of less than 32% of the reagent weight does not allow increasing the degree of hydrolysis of the coagulant. The introduction of a disinfectant in an amount of less than 6% of the total mass of the reagent does not allow reaching the concentration of active chlorine required to obtain water that is safe in terms of microbiological indicators. Mixing with an intensity that differs from the interval given in the formula, as well as non-observance of the mixing time interval, does not allow the formation of floccules of the required size for their precipitation, which also negatively affects the degree of purification of contaminated water. When floccules with an average size of less than 200 microns are formed, the required sedimentation rate is not achieved, while the process of removing impurities from the water being purified slows down. On the contrary, the sedimentation rate of floccules with a size exceeding 1550 μm is very high. In this case, sedimentation can occur ahead of time, not in the clarifier, but, for example, in the flocculation chamber or pipeline, which is undesirable.

Below are examples confirming the possibility of carrying out the invention.

Example 1.

A solid composite reagent is made by mixing a coagulant powder of aluminum sulfate with a fineness of 0.014 µm ^-1 and a powder of a cationic flocculant with a fineness of 0.003 µm ^-1 in a ratio of 6: 1 by weight. The resulting composite reagent in the amount of 70 mg is introduced into 1 DM ^{3 of the} model dispersion of kaolin. The introduction of the powdery reagent is carried out by metering in dry form with vigorous stirring with a speed gradient of 210 s ^-1 in (speed 500 rpm) for 1 min, and then stirring is continued for 30 min with a speed gradient of 9 s ^-1 (speed 50 rpm). The average size of the formed floccules is 640 µm. The resulting dispersion is defended for 30 minutes to precipitate the formed floccules, then a sample is taken from the middle of the water layer and the turbidity is determined (see Table 1).

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Table 1

Comparison of the results of coagulation of a model dispersion of kaolin using a solid composite, a reagent and solutions of a coagulant and a flocculant

Samples Concentration of reagents, mg / dm ³ Turbidity, mg / dm ³ Initial variance - 47 ± 1 A1 ₂ (SO ₄ ) ₃ (sol.) "Magnafloc" (sol.) by 10 1.3 ± 0.1 A1 ₂ (SO ₄ ) ₃ (TV) "Magnafloc" (TV) 60 ten 1.1 ± 0.2

Table 1 shows the results of coagulation of a model dispersion using a composite reagent and solutions of a coagulant and a flocculant, and in order to achieve comparable indices of the turbidity of purified water, the dose of the coagulant in the form of a solution was increased by 1.8 times in comparison with the composite reagent.

Example 2.

A solid composite reagent is made by mixing a coagulant powder of aluminum sulfate with a fineness of 0.014 μm ^-1 and a powder of a cationic flocculant with a fineness of 0.003 μm ^-1 in a ratio of 5: 1 by weight. The resulting composite reagent in the amount of 36 mg is introduced into 1 dm ^{3 of a} model dispersion of kaolin with a volume of 1 dm ³ . The introduction of the powdery reagent is carried out by dosing in dry form with vigorous stirring with a speed gradient of 370 s ^-1 (speed 750 rpm) for 0.5 min, and then stirring is continued for 30 min with a speed gradient of 9 s ^-1 ( speed 50 rpm). The average size of the formed floccules is 200 microns. The resulting dispersion is defended for 30 minutes to precipitate the formed floccules, then a sample is taken from the middle of the water layer and the water turbidity is determined. Table 2 shows a comparison of the results of coagulation of a model dispersion using a composite reagent and using solutions of a coagulant and a flocculant.

table 2

Comparison of the results of coagulation of a model dispersion of kaolin using a solid composite, a reagent and solutions of a coagulant and a flocculant

Samples Concentration of reagents, mg / dm ³ Turbidity, mg / dm ³ Initial variance - 40 ± 1 A1 ₂ (SO ₄ ) ₃ (sol.) "Magnafloc" (sol.) 50 6 0.2 ± 0.1 A1 ₂ (SO ₄ ) ₃ (solid) Magnafloc (solid, shredded) 30 6 0.2 ± 0.1

From the data table. 2 it is seen that the dose of the coagulant in the form of a solution is 1.7 times higher than the dose of the coagulant introduced with the composite reagent, while identical indicators of purified water are achieved.

Example 3.

Solid composite reagent is made in the form of tablets from a mixture of coagulant powders of aluminum pentahydroxochloride (relative basicity 83%) with a degree of dispersion of 0.015 μm ^-1 , a powder of a cationic flocculant with a degree of dispersion of 0.003 μm ^-1 and a powder of an ion-exchange sorbent NaX zeolite with a degree of dispersion of 0.02 μm ^-1 in a ratio of 10: 1: 5 by mass, while the mass of the sorbent is 31% of the total mass of the reagent. The composition is formed into tablets. The resulting composite reagent in the form of a 60 mg tablet is dosed directly into 1 dm ^{3 of a} model dispersion containing kaolin, humic compounds and calcium and magnesium salts, with vigorous stirring with a speed gradient of 370 s ^-1 (speed 750 rpm) for 0 , 5 min, and then - for 30 min with a speed gradient of 9 s ^-1 (speed 50 rpm). The average size of the formed floccules is 830 microns. The resulting dispersion is defended for 30 minutes to precipitate the formed floccules, then a sample is taken from the middle of the water layer and the turbidity, color and the content of hardness salts (Ca ²⁺ and Mg ^{2+ ions} ) are determined. The results of purification of a model aqueous dispersion are presented in table. 3.

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Table 3

Results of purification of a model aqueous dispersion containing kaolin, humic compounds and hardness salts

Parameter Source water Purified water Purification degree,% Turbidity, mg / dm ³ 4.0 0.8 80 Chromaticity, hail 86 19 78 Ca ²⁺ , mg / dm ³ 28 5.4 81 Mg ²⁺ , mg / dm ³ 28 16 43

The results obtained (see Table 3) indicate a high degree of removal of suspended impurities (80%), organic compounds (78%), and hardness salts from water using a solid composite reagent.

Example 4.

A solid composite reagent is made by mixing a powder of a coagulant polyhydroxochloride aluminum (relative basicity 43%) with a degree of dispersion 0.006 μm ^-1 , a powder of a cationic flocculant with a degree of fineness of 0.03 μm ^-1 and a powder of a pH regulator of sodium bicarbonate with a degree of dispersion of 0.008 μm ^-1 in a ratio of 20: 1: 10 by weight, while the weight of the pH regulator is 32% of the total weight of the reagent. The resulting composite reagent in the amount of 12 mg is introduced into 1 dm ^{3 of} natural water taken from a surface source. The introduction of a powdery reagent is carried out by dosing in dry form with vigorous stirring with a speed gradient of 40 s ^-1 (speed 150 rpm) for 1.5 min, and then within 30 minutes with a speed gradient of 9 s ^-1 (speed 50 rpm). The average size of the formed floccules is 860 microns. The resulting dispersion is defended for 30 minutes to precipitate the formed floccules, then a sample is taken from the middle of the water layer and the required parameters are determined. Table 4 shows the results of water purification using a solid composite reagent containing a pH regulator and in its absence.

Table 4

The effect of the pH regulator in the composition of the composite reagent on the degree of purification

Parameter Originally I am water Purified water Maximum permissible values in accordance with SanPiN 10-124 RB 99 Composite reagent with pH regulator Composite reagent without pH regulator pH 8.0 7.9 7.9 6-9 Turbidity, mg / dm ³ 1,2 0.2 0.5 1.5 Chromaticity, hail 33 eleven 12 twenty Permanganate oxidizability, mg О ₂ / dm ³ 4.5 2.9 3.6 5 Residual aluminum, mg / dm ³ - 0.3 0.6 0.5

According to the table. 4, the introduction of a pH regulator into the composition of the composite reagent made it possible to increase the efficiency of the coagulant, the use of which initially did not allow obtaining the water quality indicators required by SanPiN 10-124 RB 99 in terms of residual aluminum content.

Example 5.

A solid composite reagent is made by mixing a coagulant powder of aluminum sulfate with a degree of dispersion of 0.016 μm ^-1 , a powder of a cationic flocculant with a degree of dispersion of 0.003 μm ^-1 and a powder of a disinfectant sodium dichloroisocyanurate with a degree of dispersion of 0.014 μm ^-1 in a ratio of 20: 1: 1.4 by mass, while the mass of the disinfectant is 6% of the total mass of the reagent. Pellets are formed from the composition. The resulting composite reagent in the form of a pellet weighing 200 mg is introduced into 1 dm ^{3 of} natural water taken from a surface source during the flood period, with vigorous stirring with a speed gradient of 370 s ^-1 (speed 750 rpm) for 0.5 min, and then - for 30 minutes with a speed gradient of 9 s ^-1 (speed 50 rpm). The average size of the formed floccules is 580 microns. The resulting dispersion is defended for 30 minutes to precipitate the formed floccules, then a sample is taken from the middle of the water layer and the main characteristics are determined. Table 5 shows the results of purification of water with a high degree of pollution by substances of organic origin using a solid composite reagent containing a disinfectant and without it.

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Table 5

Results of purification of natural surface waters using a solid composite reagent containing a disinfectant and the same reagent without it

Parameter Source water Purified water Maximum permissible values in accordance with SanPiN 10-124 RB 99 Composite reagent with disinfectant Composite reagent without disinfectant UV absorption (254 nm) characterizes the content of organic matter 0.86 0.12 0.16 - Total iron, mg / dm ³ 0.93 0.1 0.3 0.3 Total microbial count (TMC) - the number of plaque-forming bacterial colonies in 1 cm ³ 2.0 · 10 ³ 0 twenty no more than 50

From the data table. 5 it follows that the introduction of sodium dichloroisocyanurate into the composition of the composite reagent of the disinfecting agent makes it possible to obtain water that is safe in terms of microbiological parameters (TMP not more than 50).

Example 6.

Solid composite reagent is made by mixing powder of coagulant pentahydroxochloride aluminum (relative basicity 83%) with a degree of dispersion of 0.015 μm ^-1 , powder of a cationic flocculant with a degree of dispersion of 0.003 μm ^-1 in a ratio of 20: 1 by weight. The resulting composite reagent in the amount of 100 mg is introduced into 1 dm ^{3 of} storm wastewater. The introduction of a powdery reagent is carried out by metering in dry form with vigorous stirring with a speed gradient of 40 s ^-1 (speed 150 rpm) for 1.5 min, and then within 30 minutes with a speed gradient of 9 s ^-1 (speed 50 rpm). The average size of the formed floccules is 1400 microns. The resulting dispersion is defended for 30 minutes to precipitate the formed floccules, then filtered and the main characteristics are determined. Table 6 shows the results of storm wastewater treatment.

Table 6

Stormwater treatment results

Indicator, units measurements Initial stock Purified water Limit value pH 7.0 6.6 6-9 Suspended substances, mg / dm ³ 34.2 <0.5 400 Dry residue, mg / dm ³ 484.0 455.0 1000 COD, mg O ₂ / dm ³ 1934 440 1000 BOD ₅ , mg O ₂ / dm ³ 780.0 472 400 Ammonium nitrogen, mg / dm ³ 2.8 4.83 thirty Phosphates, mg / dm ³ 2.2 0.063 one hundred Chlorides, mg / dm ³ 23.5 16.8 350 Total iron, mg / dm ³ 2.5 <0.2 2.0 Petroleum products, mg / dm ³ 0.5 0.2 0.9

Table data. 6 indicate a high degree of water purification by all indicators, including COD (chemical oxygen demand) and BOD (biochemical oxygen demand), which in the original wastewater exceeded the maximum permissible values by almost 2 times.

Example 7.

A solid composite reagent is made by mixing a coagulant powder of aluminum pentahydroxochloride (relative basicity 83%) with a dispersion degree of 0.015 μm ^-1 , a cationic flocculant powder with a dispersion degree of 0.003 μm ^-1 , a sorbent powder (OU-A grade activated carbon) with a dispersion degree of 0, 05 μm ^-1 and disinfectant powder dichlo

- 5 036588 sodium rhizocyanurate with a degree of dispersion of 0.014 μm ^-1 in a ratio of 20: 1: 10: 5 by weight, while the weight of the sorbent is 28% of the total weight of the reagent, the weight of the disinfectant is 14% of the total weight of the reagent. The resulting composite reagent in the amount of 74 mg is introduced into 1 dm ^{3 of} natural water taken from a surface source. The introduction of the powdery reagent is carried out by dosing in dry form with vigorous stirring with a speed gradient of 40 s ^-1 (speed 150 rpm) for 1.5 min, and then within 30 minutes with a speed gradient (speed 50 rpm ). The average size of the formed floccules is 1550 microns. After the end of stirring, the resulting dispersion is settled for 30 minutes to precipitate the formed floccules, then filtered and the main characteristics are determined. Table 7 shows the results of natural water purification using a solid composite reagent containing a coagulant, a flocculant, a sorbent and a disinfectant.

Table 7

The results of natural water purification using a solid composite reagent containing a coagulant, flocculant, sorbent and disinfectant

Indicator, units measurements Initial waste water Purified water Maximum permissible values in accordance with SanPiN 10-124 RB 99 pH 8.5 8.0 6-9 Turbidity, mg / dm ³ 28 1.0 1.5 Chromaticity, hail 300 15 twenty Total microbial count (TMC) - the number of plaque-forming bacterial colonies in 1 cm ³ 3.0 10 ³ 0 twenty

Thus, composite reagents have a number of advantages over traditional aqueous solutions of coagulants and flocculants: they allow to achieve standardized indicators of the quality of purified water, while reducing the dose of introduced reagents (by 1.5-1.7 times), reducing the content of residual coagulant by purified water, to drastically simplify the process of water purification by reducing (2-3 times) the number of stages of the introduction of reagents. The use of composite reagents at water treatment plants will also make it possible to reduce the area of storage facilities, abandon corrosion-resistant pumping and storage equipment, and reduce the cost of transporting reagents.

Information sources.

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8. Astrelin, IM Powdery floccoagulant-sorbent / IM.

Astrelin, N.M. Tolstopalova, Yu.V. Artyukh // 17th Mendeleev Congress on General and Applied Chemistry, Kazan, September 21-26, 2003: Abstracts. T. 3.

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Claims (2)

CLAIM 1. Solid composite reagent for the purification of aqueous solutions in the form of powders, granules, tablets or pellets, containing a coagulant and a flocculant at a mass ratio of 5: 1 to 20: 1, and as a coagulant used aluminum sulfate or polyhydroxochloride aluminum, the degree of dispersion of particles coagulant is from 0.006 to 0.016 μm ^-1 , a cationic flocculant is used as a flocculant, the degree of dispersion of the flocculant particles is from 0.003 to 0.03 μm ^-1 , and additionally containing a sorbent NaX zeolite in an amount of at least 31% of the total mass of the reagent, the regulator pH sodium bicarbonate in an amount of not less than 32% of the total mass of the reagent, the disinfectant sodium dichloroisocyanurate in an amount of not less than 6% of the total mass of the reagent, and the particles of the NaX zeolite have a degree of dispersion of 0.02 μm ^-1 , sodium hydrogen carbonate 0.008 μm ^-1 , sodium dichloroisocyanurate - 0.014 μm ^-1 . 2. A method for purifying aqueous solutions using a solid composite reagent according to claim 1, which consists in the fact that the solid composite reagent is introduced into the water to be purified with vigorous stirring for 0.5-1.5 minutes with a speed gradient from 40 to 370 s ^{- 1} , providing the formation of floccules with an average size of 200 to 1550 μm at the stage of slow stirring.