Chemical and Petroleum Engineering, Vol. 47, Nos. 56, September, 2011 (Russian Original Nos.

56, MayJune, 2011)

INDUSTRIAL VACUUM-EVAPORATION UNIT FOR CONCENTRATING MAGNESIUM CHLORIDE SOLUTION

Yu. V. Kartovskii,1 V. B. Chernozubov,1 K. V. Glushko,1 V. A. Chemezov,1 D. S. Tretyakov,1 A. Yu. Serkin,1 N. E. Chernykh,1* S. M. Tokarev,1 A. A. Shchelkonogov,2* V. A. Kiselev,2 and A. I. Potekha2

Production equipment layout is described for a three-vessel evaporation unit fitted with descending film equipment. The device is intended for concentrating magnesium chloride solution before carnallite synthesis, from which magnesium metal is subsequently prepared by electrolysis. Engineering properties of the equipment, composition of the starting and evaporated solutions, and also the planned operating regime are noted. Features of the bahavior of magnesium chloride solution, which should be considered for provision of successful operation without crystallization of salts within it, are mentioned.

The company Ruskii Magnii (Rusmag) has started development and construction of a plant for producing magnesium metal, prepared by electrolysis of synthetic carnallite (KClMgCl26H2O). The raw material for production is serpentinite (2SiO24MgO4H2O), contained in asbestos production dumps. A magnesium chloride solution, obtained in the sepentinite treatment stage, is evaporated in a vacuum-evaporation unit (VEU) and is aimed at the production stage of preparing synthetic carnallite [1]. Technical characteristics of the evaporation unit Productivity for starting chromium-magnesium solution, tons/h . . Productivity for evaporated water, tons/h . . . . . . . . . . . . . . . . . . . . Heated steam consumption with P = 0.42 MPa, tons/h . . . . . . . . . Cooling water consumption with t = 23C, m3/h . . . . . . . . . . . . . . Pump electric motor power, kW: included simultaneously . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . total (taking account of reserve pumps) with U = 380 V . . . . . Weight of newly developed equipment, kg: total . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . of titanium . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
1 2

70.5 29.5 15.5 486 238 344 21610 15900

Sverdlovskii Research and Design Institute of Chemical Machine Building (SverdNIIkhimmash), Ekaterinburg, Russia. Rusmag Company, Asbest, Russia. * Deceased. Translated from Khimicheskoe i Neftegazovoe Mashinostroenie, No. 5, pp. 810, May, 2011.

0009-2355/11/0506-0301 2011 Springer Science+Business Media, Inc.

301

Heated steam AB1 2s

1co 1wa AB2 2s CK1 2s 1co T4 T3 T5 AB3 1wa WIU1 BC1 1co WU1

Cooling water

1co

T2 1e 1e H2

1e 1e 1c 1c

1e 1e 1e H6 H3

1e 1e

1e

1e 1e 1e 1e H5 1e

H10

1e

T6 H2 1e 1co 1co H11 Technical condensate Hydrochloric acid To HS technical condensate tank To oxidation-reduction system Starting magnesium chloride solution

H4 To carnallite synthesis

H8 To boiler or to production

1e

1co cooling water 1e evaporation solution 1wa washing solution 2 self-evaporation steam 2h heated steam 2s secondary steam 3 uncondensed gas

H9 1e H1 T1

1co

Fig. 1. Basic layout of the vacuum-evaporation unit.

of corrosion-resistant steel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3925 of carbon steel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1785 Overall equipment dimensions, m: length width height . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24 6 12 Two VEU are proposed in order to provide production continuity for carnallite preparation in the evaporation stage, one of which is in reserve. The chemical composition and the magnesium chloride solution in the VEU according to the All-Russia Institute of Galurgie (VNII Galurgiya) procedure is provided in Table 1. An evaporation unit has been developed in the technical planning stage. The basic layout of the VEU scheme is provided in Fig. 1. The device operates in a counterflow scheme of production flow movements of steam and evaporation solution. During operation in this regime, the starting magnesium chloride solution from tank T1 is fed by pump H1 into the upper solution chamber of the evaporation equipment AB1. The starting solution at the equipment inlet AB3 is mixed with partly evaporated solution circulating within this equipment. Circulation is provided by pump H5. With flow of mixed solution over the inner surface of the heat exchanger pipes in the form of a descending thin film, there is partial evaporation of water from the solution. Solution is pumped by pump H2 from unit AB3 into the second unit AB2, and then from AB2 by pump H3 into a third unit AB1, whose concentrated solution is organized in the same way as in unit AB3. Solution evaporated to a final prescribed concentration is pumped from unit AB1 by pump H4 into a service vessel, from which it passes to carnallite synthesis. Heated steam from an outside source is supplied to the heating chamber of unit AB1, where it condenses, and evaporates the magnesium chloride solution to a final concentration. The condensate of heated steam is removed to receiving tank T2, fitted with a level controller, and then through a hydraulic shut-off, fitted with a control valve, into self-evaporator CK. 302

TABLE 1
Component content, wt.% Name MgCl2 CaCl2 NaCl KCl H2O Value of temperature depression, C

Starting solution Evaporated solution

20.06 34.5

0.42 0.72

1.2 2.08

1.39 2.4

76.93 60.3

7.2 for t = 48.5 28 for t = 126 1

Condensate of heated steam from the self-evaporator enters either the heating chamber of unit AB2, or it is returned to the boiler. Choice of the type of hydraulic shut-off is due to the large pressure drop of steam between AB1 and AB2, caused by the high temperature depression of the solution. Condensate from AB2 passes into AB3 through a U-shaped hydraulic shutoff. Condensate from the heating chamber of unit AB3 is poured by gravity flow in tank T3, from which it is pumped by pump H9. Secondary steam, forming during evaporation of solution in unit AB1, and steam from self-evaporation of condensate in self-evaporator CK1, enters as heated steam into the heating chamber of unit AB2. Secondary steam, obtained with evaporation of solution in unit AB2, is heated for unit AB3. Secondary steam, obtained in unit AB3, enters into barometric condenser BC1 of a jet-bubble type, where it condenses. A steam and air mixture from units AB1AB3 and barometric condenser BC1, is removed into a water-injection unit (WIU1, providing the vacuum operating regime for the device. Evacuation of the equipment is accomplished through drawing the starting solution into tank T1. A system is provided for washing the inner surfaces of both the heat exchange tubes of the heating chambers, and the actual units AB1AB3, and also their separation devices from contamination and deposits of distillate or acid solution. Washing of the equipment is performed using a tank T6 and pump H11. Washing may be carried out either through a closed loop: tank T6 pump H11 units AB1 (AB2, AB3), or by filling to the working level of the washing equipment with washing solution and its subsequent circulation in the units by means of pump H7 (H6, H5). After washing, the washing solution is pumped into the hydrochloric acid preparation cycle. Separation devices may be washed additionally by condensate fed by pump H9 from tank T3. The device is fitted with control and measuring instruments, and systems for automatic regime management. The type, design, and construction and use of VEU production equipment were determined by a requirement for providing operational reliability and convenience of repair for equipment, and also the corrosion resistance of structural materials in contact with magnesium chloride solution evaporated in a prescribed temperature and slat regime. In order to concentrate magnesium chloride solution, equipment was used with a descending film. This equipment, compared with that used traditionally in mineral salt production equipment with induced circulation, is more effective with respect to heat transfer, less metal content, it has markedly lower solution volume, and it is distinguished by low inertia. The low inertia makes it possible to use a more reliable system for automated control of the production process. In addition, there is a significant reduction in the expenditure of operating time for preparation and carrying out prophylactic washing of heat exchange surfaces. In addition, the equipment with a descending film exhibits a greater tendency towards crystallization on a heat exchange surface compared with equipment with induced circulation. This is due to the fact that within equipment with a descending film evaporation of solution occurs in tubes, and the wall layer of solution is more saturated than in equipment with induced circulation. The lack of experimental data for the operation of equipment with a descending film of magnesium chloride solution predetermines a requirement for experimental verification of the evaporation equipment of this type in order to concentrate magnesium chloride solution of planned composition. This verification was carried out in a test unit [2], whose results confirmed the suitability of equipment with a descending film for evaporation of magnesium chloride solution. The equipment construction developed consists of a heating chamber and removable separator. The surface of the heat exchange equipment is 390 m2, and for the heat exchanger tubes it 38 1 6000 mm. The equipment has the follow303

TABLE 2
Equipment Parameters AB1 AB2 AB3

Productivity for evaporated water, tons/h Heated steam consumption, tons/h Heated steam temperature, C Boiling temperature, C Temperature depression, deg Available temperature difference, deg Heat transfer coefficient, W/(m deg)
2

10.86 13.38 133.2 123 28 10.2 2350

9.37 11.80 94.9 85.6 15 9.2 2080

9.27 10.44 70.3 58.5 7.2 11.2 1550

ing internal devices: a slow flow shutter distillation safety trap, located in a separator and made of vertical bundles, intended for cleaning from droplet carry over; a nozzle for washing the shutter bundles from salt crystals, as result of carry of them into the shutters. Pumps have frequency control for the number of rotations, i.e., in order to provide solution circulation in the equipment and removal of evaporated solution from the equipment. Stable film flow of solution over the surface of heat exchange tube is provided by a nozzle-jet device. The equipment is made entirely from titanium alloy VT1-0. Water evaporated from the solution is not a commercial product. Therefore in order to concentrate secondary steam, entering from unit AB3, a surface-free contact jet-bubble barocondenser BC1 was developed. The construction of the barometric condenser was made with two jet condensation stages. The jet forming tray was perforated with holes 15 mm in diameter, which almost prevents their blockage by mechanically suspended matter. The barometric condenser and elements of the water injector unit (water injector, tank T5, connecting pipes) are manufactured from steel 12Kh18N10T. Self-evaporator CK1 and tanks T2, T3, and T4 are made from carbon steel VSt3sp. The pipelines and connections in fittings in lines are: for magnesium chloride solution made of titanium alloy VT1-0; for drainage and acid solution made from polymer material; for condensate made from carbon steel. Production pumps pumping magnesium chloride solution are made of titanium alloy VT1-0. The General Designer selected the type of pump H1 and material used for tank T1. The planned temperature-salt regime for VEU operation, calculated from starting data of VNII Galurgiya [1], is provided in Table 2. It is demonstrated in article [2] that the planned operating regime for the VEU may be realized in vacuum-evaporation equipment with a descending film without crystallization in them of salts from solution. In addition, if the permissible concentration limit of salt in the starting magnesium chloride solution is not maintained, then early concentration of solution is possible in unit AB1, which may lead to mass crystallization in the heat exchanger tubes up to complete blockage with salt crystals. Considering that during industrial operation the salt composition of the solution is as a rule not maintained, therefore the version developed replaces the first vessel of a VEU in equipment with induced circulation.

REFERENCES 1. 2. Vacuum-Evaporation Equipment for Concentrating Magnesium Chloride Solution. PZ for Technical Plan A.29.970.000 PZ, SverdNIIkhimmash (2008). Yu. V. Kartovskii, S. M. Tokarev, S. G. Vasiliev, et al., Experimental study of the behavior of magnesium chloride solution with concentration in equipment with a descending film.

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