Method for complex processing of sea water and installation for its implementation

 

(57) Abstract:

Use: receive valuable minerals and fresh water from sea water. The essence of the invention: method for complex processing of sea water, including successive stages: mechanical filtration, excretion of calcium on a modified zeolite, the allocation of magnesium on subacid the cation and processing the received softened sea water, regeneration mentioned modified zeolite and regeneration mentioned weak acid cation exchanger, at the stage of processing softened seawater conduct its desalination with obtaining fresh water and simultaneous achievement of secondary brine with a salt concentration of at least 100 g/l, which regenerate the modified zeolite. The proposed installation for implementing the method for complex processing of sea water, comprising successively installed downstream filter with a natural zeolite, a column with modified zeolite, a column with a weak acid cation exchange resin and optionally the column selection calcium, connected in parallel with the column containing the modified zeolite. 2 S. and 1 C.p. f-crystals, 2 tab., 3 Il.

Idealny substances and fresh water.

The invention can be used to create stations, seawater desalination new generation or modification of existing desalination plants.

Known methods of processing of sea water using the methods of distillation, reverse osmosis, electrodialysis, genioplasty and crystallization by freezing with obtaining fresh water [1].

The main disadvantage of these methods is the lack of complexity in the processing of sea water associated with obtaining valuable minerals, as well as education in the desalination process significant quantities of environmentally harmful secondary brines, polluting the waters.

There is a method of processing sea water, comprising sequentially stage desalination with obtaining fresh water and secondary brines and the stage of processing of these brines with getting someproducts [2].

The disadvantage of this method is that in this way the stage desalination and recycling of brine are almost independent processes that do not provide for reducing the cost of desalination, on the one hand, and not allowing to improve the factor of concentration, etc is known a method of processing sea water, includes the successive stages of selection of salts of calcium, magnesium and bromine, desalination obtaining secondary sodium brines and processing of brines with obtaining sodium salt [3].

This method simultaneously with the release of calcium salts and magnesium provides given for seawater desalination plants of various types, which allows to increase the degree of extraction of fresh water and the factor concentration brines. The method also allows to avoid the formation of trudnoobrabatyvaemyh brines mixed type.

The main disadvantage of this method is the necessity to use at the stage of extraction of magnesium such expensive reagents, as the alkali, the cost of which is commensurate with the value of magnesium products.

Known installation sorption of water treatment, consisting of two vertical columns, the loaded sorbent with each of the columns has an input and output, branched in such a way that each entrance or exit of one of the column is connected to one input or the output of the upper part of the other columns, as well as one to enter or exit the bottom of another column, and all inputs and outputs are provided with valves [4].

Negotiable closest technical solution to the invention is a method for complex processing of sea-water, includes consistently pursued stage mechanical filtration through natural zeolite, excretion of calcium by passing the filtrate through a modified magnesium zeolite in Na+form, separation of magnesium by passing the solution through a carboxylic cation exchange resin in Na+form with obtaining softened sea water, regeneration of modified zeolite and regeneration of carboxylic cation exchange resin with a solution of baking soda followed by separation of the magnesium carbonate from the regenerate [5].

This method has the following disadvantages.

First, sea water is highly mineralized environment, and the sorbent for pre-softening, for example zeolites, it is often necessary to regenerate; to extend the regeneration cycles necessary to use a large one-time download of the sorption materials.

Secondly, the additional costs of producing or purchasing the required quantity of concentrated solution of salt for regeneration of zeolites or require additional costs for the purchase of reagents for separation of calcium from regenerating solutions for use in circulation.

Thirdly, the necessary costs sodersten to the proposed installation of complex processing of sea water is to install, includes installed sequentially downstream of the sorption filter with a natural zeolite, a vertical adsorption column excretion of calcium with modified zeolite sorption site selection magnesium with weak acid cation exchange resin, the node processing of softened water and the node processing the mixed concentrate [6].

This facility has the following disadvantages.

Installation includes expensive site for the regeneration of zeolites at the stage of selection of calcium and requires too large one-time download of the modified zeolite in the adsorption column excretion of calcium.

The most significant drawback of the scheme and the design of the installation is that it does not allow the processes of adsorption-regeneration at the stage of extraction of calcium in parallel.

The installation also does not allow for continuous monitoring of regeneration of the modified zeolite secondary brine obtained at the stage of desalination.

The problem to be solved in the present invention is to increase the efficiency and reduce the cost of complex processing of sea water through the creation of "samoreguliruemaja" SOCA of the present invention is to develop a method for complex processing of sea-water, which would allow using the solutions obtained in the process in closed loop mode without involving the purchase of reagents and apparatus for carrying out this method.

Additionally the invention aims to improve the environmental safety of complex processing of sea water through the use of closed circuit and the elimination of liquid waste.

The task is solved by the fact that in the method for complex processing of sea water, including consistently pursued stage mechanical filtration through natural zeolite, excretion of calcium by passing the filtrate through a modified magnesium zeolite in Na+form, separation of magnesium by passing the solution through a carboxylic cation exchange resin in Na+form with obtaining softened sea water, regeneration of modified zeolite and regeneration of carboxylic cation exchange resin with a solution of baking soda followed by separation of the magnesium carbonate from the regenerate, is conducted additionally stage desalination softened sea water to obtain fresh water and secondary brine with a concentration of not less than 100 g/l, the latter is directed to the stage of regeneration of the modified zeolite magasanik potassium brines, which is directed to the additional stage processing of natural zeolite with obtaining potassium form of zeolite and circulating brine returned to the stage of processing of the regenerate.

The tasks are solved also by the fact that the installation of complex processing of sea water according to the invention, including installed sequentially downstream of the sorption filter with a natural zeolite, a vertical adsorption column excretion of calcium with modified zeolite sorption site selection magnesium with weak acid cation exchange resin, the node processing of softened water and the node processing the mixed concentrate further comprises a sorption column excretion of calcium, connected in parallel with the first column selection calcium, and mentioned columns provided in the upper and lower parts of the blocks with input and output valves, the node processing softened water is made in the form of a desalination module, having the inlet and two outlet pipe for fresh water and secondary brine, respectively, with the outlet of the sorption filter is connected to the input valve blocks the upper part of the sorption columns highlight calsci sorption columns excretion of calcium, the outlet for the secondary brine desalination module is connected to the input valve blocks the lower part of the sorption columns excretion of calcium, the input port of node processing mixed concentrate connected with the output valve blocks the upper part of the sorption columns excretion of calcium.

Appropriate setting to provide sorption column with the natural zeolite, the inlet of which is connected to the output socket of a node processing mixed concentrate, and the outlet connected to the inlet side of the above-mentioned node processing mixed concentrate.

In Fig. 1 shows the output curves of sorption on synthetic zeolite; Fig. 2 - output curves of the artificial regeneration of the zeolite, and Fig. 3 is a block diagram of plant for complex processing of sea water.

The proposed solution "samoreguliruemaja" adsorption-desalination systems based on the combination of the following conditions: the use of modified zeolites and the effect of isothermal supersaturation for their regeneration. Achieved a fundamental result that was not achieved anywhere previously, is that the conditions are Platonism for complete regeneration of the zeolites with simultaneous separation of calcium salts. For example, if the sorption cycle Omakaitse V0the volume of sea water, and the concentration degree of the secondary brines equal to P, the last equal to V=V0/P, provides a comprehensive desorption of calcium from the zeolite and to restore it to its sodium form for use in a subsequent cycle softening. Modification of zeolites produced as follows. The zeolites of type a sequentially process of 0.05-0.5 M solution of magnesium chloride to saturation and 2-3 M solution of sodium chloride [6]. Modified zeolites have a unique combination of properties required (as shown by theoretical study) for the efficient sorption of preliminary preparation: high selectivity to ions of calcium than magnesium ionsCaMg25, the low value of the equilibrium constant for ion exchange of calcium and sodium, KCaNa= 1, the high value of the total capacitance and 5 g-EQ/liter

The effect of supersaturation allows you to use the concentrate after the desalination of sea water, which is a mixture of chloride and sodium sulfate, without precipitation of gypsum in the zeolite layer. When this regeneration efficiency increases, and complete desorption of calcium is achieved by volume of the concentrate, is equal to neobmenennogo supersaturation - is illustrated in Fig. 1 and 2. It is evident from Fig. 1, which shows the output curves of sorption of magnesium (1 and 1') and calcium (2 and 2') from seawater 0.8 l of modified zeolite (curves 1 and 2) in comparison with the same number of commercial cation exchange resin KU-2 (curves 1' and 2') shows that the sorption of calcium these sorbents are practically identical. At the same time, as shown in Fig. 2, the number of secondary chloride - sulfate brine 3.2 liters (obtained after concentration 5 times 16 liters of softened water in accordance with Fig.1) with a concentration of 175 g/l, is achieved through the comprehensive regeneration of the modified zeolite (curve 1), with the resulting supersaturated solution spontaneously decomposes residual concentration of calcium in the solution in accordance with curve 1. As shown by curve 3, the same number of the same secondary brine is not capable of regenerating the cation exchange resin KU-2. As shown by curve 2, the same amount of pure chloride solution with a concentration that does not lead to saturation, is not capable of regenerating the modified zeolite. It is advisable to carry out the regeneration process of the modified zeolite secondary brine with a concentration of not less than 100 g/l, since at lower concentrations the efficiency regenertive desorption of calcium. Traditional desalination technologies do not provide a secondary brine with a concentration of more than 60 to 90 g/L. the Proposed method for deep softening allows to increase the degree of concentration (and consequently, the efficiency of desalination).

"Samoreguliruemaja" scheme implemented during the creation process waste complex processing of sea-water, is shown in Fig. 3. In this scheme, the preliminary preparation of sea water is mechanically filtered on natural zeolite 1, then used two layers 2 and 3 of the modified zeolite, running in parallel to stages of adsorption and regeneration. Then, the solution is passed through the carboxylic cation exchange resin in Na+-form. Then fully softened the solution is fed to the desalination module 5. The regeneration of carboxylic cation exchanger spend soda solution and regeneration of the modified zeolite is a solution of the concentrate is continuously supplied with a desalination module 5. Reclaim obtained after desorption of calcium from layer 2 or 3 of the modified zeolite, is fed to a fractional crystallization, where traditional methods produce calcium sulfate, sodium chloride and sodium sulfate, residual brines enriched caliea by fractional crystallization. When this natural zeolite becomes saturated potassium composite, which is chlorine-free fertilizer with prolonged action. As the zeolite layer 7, it is advisable to use exhaust during operation zeolite in stage 1. The feature of the circuit shown in Fig. 3, is that simultaneous loading of sorbents is not dictated by their capacity. Multiple reduction of the duration of the filtration cycle will be affected ultimately only on the frequency of the switching valves of ion-exchange columns containing modified zeolite.

As desalination module 5 can be used electrodialyzer, as well as various types of thermal distillation. The most promising is developed in recent years, the method of membrane distillation, built on the effect of permeability of hydrophobic membranes for water vapor and impermeable their liquid solutions.

"Samoreguliruemaja" scheme implemented for complex processing of sea-water, is shown in Fig.3.

Installation of complex processing of sea water contains installed in series along the process of sorption filter 1 of calcium with modified zeolite, sorption site 4 allocation of magnesium with a weak acid cation exchange resin, the node 5 processing of softened water, the node 6 processing of mixed concentrate and additional column 7 with the natural zeolite for the disposal of potash brine.

The column selection calcium 2 and 3 provided in the upper and lower parts of the blocks with the input 8, 9, 10, 11 and output 12, 13, 14, 15 of the vehicle.

The node processing softened water 5 made in the form of desalination module, having an inlet pipe 16 and two output pipe 17 and 18 for freshwater and secondary brine, respectively.

The outlet 19 of the sorption filter 1 is connected with the inlet valves 8 and 9 blocks the upper part of the sorption columns 2 and 3 highlight of calcium.

The inlet 20 of the sorption site 7 allocation of magnesium connected to the output valves 14 and 15 blocks the lower part of the sorption columns 2 and 3 highlight of calcium.

Outlet 18 for the secondary brine node 5 is connected with the inlet valves 10 and 11 blocks the lower part of the sorption columns 2 and 3 highlight of calcium.

Inlet pipe 21 site 6 processing mixed concentrate connected with the output valves 12 and 13 blocks the upper part of the sorption columns 2 and 3 provide what trubka 23 additional columns 7 with natural zeolite, and the outlet 24 of the column 7 is connected to the inlet side 25 of node 6.

The method according to the invention will become clearer from the description of the operation of the plant.

The device operates as follows. Sea water is subjected to mechanical filtration by passing through the column 1 with the natural zeolite. A suspension remains in the layer of natural zeolite and periodically, as calmative filter, wash the reverse, wrigleys flow of sea water into the marine waters. Next, the filtered sea water passes through one of the columns 2 or 3, loaded artificial modified zeolite, in which the sorption of calcium. Columns 2 and 3 simultaneously, and one - on-stage sorption, and the other at the stage of regeneration. The sorption process continues to the "breakthrough" of calcium through the sorption column (2 or 3), after which there is simultaneous switching columns mode sorption on regeneration and Vice versa, that is automatic switching of input and output valves 8 - 15. Switching is carried out, for example, the signal analyzer of calcium (Fig. 3 not shown) installed in the line connecting the inlet pipe 20 of node 4 output valves 12 IEC switching valve shown in the table. 1.

Freed from calcium partially softened sea water after columns 2 or 3 stages of sorption is supplied through the pipe 20 site 4 excretion of magnesium, which is designed in such a way that allows parallel processes of sorption of magnesium on carboxylic cation exchange resin and the regeneration of the cation exchange resin with a solution of soda. In the process the specified regeneration is obtained reclaim from which to extract the product is magnesium carbonate.

Freed from calcium and magnesium fully softened sea water then exits through pipe 16 on node 5 (desalination module). In desalination module obtained fresh water as the product is fed through the outlet 17, and a secondary brine supplied through the outlet 18. Last continuously upon receipt fed through the outlet 18 and the valve 10 or 11 blocks in the lower part of columns 2 and 3 and is used for regeneration, i.e. desorption of calcium with layers of modified zeolite.

Reclaim obtained after desorption of calcium in the stages of regeneration of the modified zeolite in columns 2 and 3, which is a mixed concentrate salts of calcium, sodium and potassium through the valves 12 or 13 BA, where is subjected to fractional crystallization with sequential selection of products: calcium sulphate, sodium chloride, sodium sulfate, and the residual brine enriched in potassium.

Potassium-enriched brine is continuously upon receipt of the node 6 is supplied through the pipe 22 to the secondary column 7 with the natural zeolite, passing through which is transformed into sodium - calcium-potassium brine, similar in composition to the mixed concentrate after regeneration columns 2 and 3, and therefore, together with the specified mixed concentrate is supplied to the node 6 processing mixed concentrate. In the process, an additional column 7 in her natural zeolite becomes saturated potassium composite, which is chlorine-free potassium fertilizer of prolonged action. The latter is discharged from the column 7 in the quality of the product, specified in column 7 is loaded with fresh natural zeolite together with the spent substandard natural zeolite formed as columns 1 mechanical filtration.

Example 1.

a) Preparing ion-exchange columns with parameters given in table. 2.

b) Through the columns 1, 2, 4 consistently miss the sea UB>2; 0.01 g - EQ/l KCl. The transmission rate of the sea water 10 l/h Time of transmission - 4 PM

in) Columns 2 and 4 off on regeneration, and the sea water continues to pass sequentially through the columns 1-3-5 at a rate of 10 l/h, and then through laboratory electrodialysis installation, collected from 10 pairs of cation-exchange and anion-exchange membranes 15 x 30 cm, when applying a common voltage sequentially to all the cells in the 12th century by the concentrate (secondary brine with a salinity of 20 g/l with the speed of 1.73 l/h and diluate (fresh water) salt 0.5 g/l with a rate of 8.27 l/h

Fresh water is directed to the further concentration and use. Secondary brine is directed to the regeneration of zeolite A in column 3, the waste stage sorption in accordance with section b).

d) Regeneration of the zeolite And the secondary brine is conducted simultaneously with the operations of the sorption softening on the columns 1-3-5 and desalination by electrodialysis installation in accordance with p. in). Bandwidth brine 8,2 l/h, the process time is 4 o'clock

d) Simultaneously with the regeneration of the zeolite And p. g) conduct the regeneration column 4 with a cation exchange resin KB-4, an elaborate stage sorption in accordance with section b). DL is3(baking soda) - 0, 59 g - EQ/l Total concentration of the solution by the sodium - of 3.73 g - ion/l, the molar ratio of carbonate and bicarbonate - 1:0,376, the pH of 9.6. Further, the name of the mixture of this composition is "AL". Bandwidth "AL" - 6 l/h, the time bandwidth - 2 hours the Filtrate, which is supersaturated solution of magnesium carbonate, after the column stand for 1 h, during which there is a spontaneous crystallization of poorly soluble compounds MgCO33H2O with a crystal size of 0.3-1 mm, the Precipitate is filtered off, the solution of Na2CO3+ NaHCO3residual contents of Mg2+= 0.05 g - EQ/l is collected in a container for use in the next cycle of regeneration after doreplace a mixture of "AL" in the amount exactly equivalent to the amount of desorbed magnesium (4.5 g - EQ by Na+). After the precipitate it is dried at a temperature of 100oC. Total for the cycle obtained 280 g of the product MgCO33H2O (4 g - EQ magnesium) with a purity not less than 99.5% pure. The duration of all operations on the item - 4 PM

d) Columns 2 and 4 switch on the sorption and begin to let sea water scheme 1-2-4. Columns 3 and 5 switch on regeneration and repeat all the processes in accordance with PP b), C), d) and dei reverse flow of sea water at 50 l/h for 2 minutes Stream discharge or direct the waters (source) of sea water.

(e) After each cycle of regeneration of the zeolite And in accordance with p. in) get a 33 litre concentrate, which is supersaturated solution of the sulphate of calcium, of which over 1 h begins spontaneous crystallization of gypsum CaSO42H2O. Obtained after each cycle, the concentrate is evaporated 1.2 times (in the laboratory) a rotary evaporator at 50oC with a pressure of 0.05-0.10 kg/cm or under infra-red lamps simulating solar evaporation until it reaches a saturation state by sodium chloride (330 g/l and the density of a solution of 1.9 g/cm). The precipitate of sodium sulfate (gypsum) is separated and dried at a temperature of 100oC. for Only one cycle (4 hours) the process of complex processing of sea water get to 54.5 g CaSO42H2O in terms of dry salt.

f) the Filtrate after separation of the precipitate gypsum 1 l/h at an average flow subjected to further evaporation 6.7 times for allocation of common salt NaCl. Oparka is to achieve a state close to saturation on sodium sulfate at a temperature of 50oC (up to a total flow of liquid brines 150 ml/h). The precipitated sodium chloride is separated and dried at there not more than 1% and an admixture of sodium bromide no longer than 0,35%.

C) the Filtrate after separation of the sodium chloride (salt concentration = 400 g/l) is cooled to a temperature of - 5oC and incubated for 1 h, resulting in the precipitation of sodium sulfate in the form of Glauber's salt Na2SO410H2O. In the process of crystallization of sodium sulfate reduced the total concentration of salts in the residual bitter brines up to 250 g/L. the Precipitate was separated by filtration on cold and dried first by blowing air through the filter, and then at a temperature of 80oC. for Only one cycle obtain 46 g of Glauber's salt with NaCl impurity not more than 5%.

and) Bitter brines after separation of sodium sulfate, potassium-enriched, the total flow of 130 ml/h and a concentration of 250 g/l is passed through an additional column with clinoptilolite with parameters 1 = 25 cm S = 20 cm (PL. 2 N 6) for the sorption separation of potassium. The obtained filtrate (130 ml/hour), Na - brine having a composition close to the composition of secondary brine after electrodialysis, add in the regeneration solution to zeolite And in columns 3 and 4.

K) After 10 cycles of the process column with clinoptilolite (table. 2 N-6) is processed bitter brines in accordance with item and), saturated potassium and replaced by a fresh download with prolonged action, can be used in Agrochemistry.

Thus, when conducting operations in PP (a) - K) provides a comprehensive waste-free processing of sea water for the production of useful products: H2O MgCO33H2O, NaCl, NaSO4, CaSO4and K-clinoptilolite.

Example 2.

Conduct a process as in example 1 in accordance with items a) - C), except that the waste water containing salts of calcium, magnesium, after columns 1-2-4 or 1-3-5 flow 10 l/h is subjected to evaporation in the ferry apparatus equipped with a refrigerator and a collection of water at a temperature of 110oC for 1 h to a residual flow of secondary brine 1.8 l/h with a salt concentration of 210 g/L. thus receive 8,2 l/h of fresh water with salt content of 0.24 g/l

Secondary brine is subjected to conversion in accordance with PP (e) - (K) of example 1.

Example 3.

Carry out the process as described in example 1, except that the empty sea water flow of 10 l/h is passed through the laboratory of membrane distillation apparatus HMM, consisting of ten identical polacek separated by a hydrophobic microporous membrane type "Vladipor MMF-2" with the following parmitano sea water is passed through a hot polyacene (60oC) at a rate of 30 l/h in the circulation mode in the selection of cold half cell to 8.45 l/h of fresh water with salt content of 0.01 g/L. thus receive 1.55 l/h secondary brine with a total salt content of 225 g/l Secondary brine is subjected to further conversion in accordance with PP (e) - (K) of example 1.

The proposed method for complex processing of sea water through the use of a special set of processes and new conditions of their use and combination with each other allows you to:

- to ensure environmental safety by creating a closed circuit without liquid wastes;

- reduce the cost of produced fresh water due to the simultaneous receipt of commercial products in the form of salts of sodium, magnesium, potassium, calcium;

- reduce the cost of complex processing of sea water through the creation of "samoreguliruyuschaya the scheme of" separation of calcium, not requiring the use of imported reagents for regeneration and allowing to greatly reduce simultaneous loading of sorbents.

Thus, the described setup allows you to work in basegenerated mode ("regeneration") at the stage of selection of calcium from sea water, which ultimately Ave is tion, their service, as well as requiring the purchase of reagents. Additional savings associated with the feature schema, as shown in Fig.3. Simultaneous loading of sorbents can be significantly reduced compared to conventional designs, since in the proposed setting a minimum duration of regeneration cycles is not limited to the technological requirements associated with carrying out in practice of the process of regeneration. There is no need to elongation of regeneration cycles dictated by the small capacity of the modified zeolite. Multiple reduction of the filtration cycle will be affected ultimately only on the switching frequency of the input and output valves 8 - 15.

1. Method for complex processing of sea water, including consistently pursued stage mechanical filtration through natural zeolite, excretion of calcium by passing the filtrate through a modified magnesium zeolite in PA+form, separation of magnesium by passing the solution through a carboxylic cation exchange resin in PA+form with obtaining softened sea water, regeneration of modified zeolite and regeneration of carboxylic cation exchange resin with a solution of baking soda followed by separation of the magnesium carbonate from the regenerate,th water and secondary brine with a concentration of not less than 100 g/l, the last is directed to a stage of regeneration of the modified zeolite and subsequent processing of the regenerate fractional crystallization from getting dry salts of sodium and calcium, and potassium-enriched brines, which is directed to the additional stage processing of natural zeolite with obtaining potassium form of zeolite and circulating brine returned to the stage of processing of the regenerate.

2. Installation of complex processing of sea water, including installed sequentially downstream of the sorption filter with a natural zeolite, a vertical adsorption column excretion of calcium with modified zeolite sorption site selection magnesium with weak acid cation exchange resin, the node processing of softened water and the node processing the mixed concentrate, characterized in that the installation further comprises a sorption column excretion of calcium, connected in parallel with the first column selection calcium, and mentioned columns provided in the upper and lower parts of the blocks with input and output valves, the node processing softened water is made in the form of a desalination module, having the inlet and two outlet pipe for fresh wee valves blocks the upper part of the sorption columns excretion of calcium, the inlet of the sorption columns excretion of magnesium is connected with the output valve blocks the lower part of the sorption columns excretion of calcium, the outlet for the secondary brine desalination module is connected to the input valve blocks the lower part of the sorption columns excretion of calcium, the input port of node processing mixed concentrate connected with the output valve blocks the upper part of the sorption columns excretion of calcium.

3. Installation under item 1, characterized in that the unit is supplied through the sorption column with the natural zeolite, the inlet of which is connected to the output socket of a node processing mixed concentrate, and the outlet connected to the inlet side of the node processing the mixed concentrate.

 

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1 dwg

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