Method of producing potassium chloride with improved rheological properties

FIELD: chemistry.

SUBSTANCE: invention can be used in producing halurgic potassium chloride from sylvinite ore using a dissolution-crystallisation method. The method of producing potassium chloride involves structural agglomeration of a mixture of a wet crystallisate and dry hot potassium chloride in a mixer-granulator and then drying the mixture. For structural agglomeration of the mixture, dry hot potassium chloride is fed in amount of 25-100% of the weight of wet crystallisate. The mixture is dried at temperature 105-135°C to obtain the end product.

EFFECT: invention reduces caking capacity of potassium chloride, avoids use of structure-forming salts, reduces consumption of reagents used to prevent potassium chloride from caking, and obtain a product which does not contain extraneous impurities.

2 cl, 2 tbl, 2 ex

 

The invention relates to techniques for obtaining galilejskogo potassium chloride from sylvinite ores by the method of dissolution-crystallization.

Known methods for producing potassium chloride from sylvinite ores by dissolving by heating in a circulating solution with the release of halite, clarification hot saturated solution, followed by its cooling installations, vacuum crystallization, highlighting kristalliset and return circulating solution in the dissolution of sylvinite ores - see Mining journal, No. 8, 2007, p.27-30. In accordance with the regulatory documents to prevent caking of the target product dry crystallized treated with amines at a flow rate of 200 g/ton or ferrocyanide of potassium (sodium) at a flow rate of 50 g/t and alkaline additives to 200 g/so

The disadvantage is the relatively high consumption of these chemicals, which cause difficulties when using the product in the production of chlorine-free and complex NPK-fertilizers.

A method of obtaining agglomerated potassium chloride from fine potassium chloride fraction is 0.25 mm - see RF patent №2213078, CL C01D 3/04, 29.08.2001-27.09.2003, including the introduction of wet concentrate reagent that promotes agglomeration, mixing the mixture and dried in the drying apparatus. While in the wet concentrate enter cyclone the dust, caught at the stage of dry flue gas drying apparatus, and the mixture before drying is passed through TurboPascal mixer-granulator.

The disadvantage of this method is the contamination of the target product binder additives and elevated moisture content.

A method of obtaining potassium chloride moisture with improved rheological properties - see RF patent №2359910, CL C01D 3/22, 27.06.2007-10.01.2009, bull. No. 8 - the prototype.

The method comprises adding to galilejskogo or flotation potassium chloride minerals - structure-forming salt is selected from a carbonate, sulfate, dihydrophosphate, orthophosphate, metasilicate potassium or sodium, which are served before drying in the wet concentrate on structural stage agglomeration. Structural agglomeration is carried out at a moisture content of 3.0-5.0 percent in TurboPascal mixer-granulator in a mixture with dry hot potassium chloride, taken in an amount of 10-20% by weight of the agglomerated potassium chloride. Structure-forming salt serves in the amount of 0.5 to 5.0 kg per tonne of finished products.

The disadvantage of this method is the pollution galilejskogo potassium chloride salt structure, which is unacceptable in obtaining high-quality product with KCl content of 96-99%. In addition, when receiving moisture proof small agglomerated Gal who lieskove potassium chloride, does not contain amines, there may be a need for a processing reagent to prevent caking of the target product.

The task of the invention is to improve the quality galilejskogo potassium chloride at the expense of abandoning the use of structure-forming salt with simultaneous reduction of the consumption of reagents fed to prevent caking of the target product.

This goal is achieved by the fact that in contrast to the known method, including structural agglomeration of the mixture moist kristalliset hot and dry potassium chloride in the mixer-granulator, followed by drying the mixture, the proposed method for structural agglomeration of the mixture of the hot dry MOP served in a number of 25-100% by weight of wet kristalliset and drying of the mixture is conducted in the temperature range of 105-135°C to obtain the desired product. When this dried mixture is conducted preferably at a temperature of 110°C.

The essence of the method as a technical solution is as follows.

In contrast to the known method, the wet crystallized received at the facility vacuum crystallization, process hot dry potassium chloride, taken in an amount of 25-100% by weight of wet kristalliset in the mixer-granulator, and structural-agglomerated mixture is dried at a temperature of 105-135°C.

At about the existence from the flotation of potassium chloride, particles which are crushed natural mineral sylvite (KCl), the surface of which has a significant amount of flotation agents (amines and other), glogicheski potassium chloride is formed from the hot clarified saturated solution when it is cooled at facilities regulated (RWCU) or unregulated vacuum crystallization (ICD).

KCl content crystallizatio is adjusted in the range 95-99% by adding water in the housing units crystallization. Particles kristalliset after RUKU have an average size of 0.5-0.7 mm, depending on the conditions of crystallization, and after ICD - 0.2-0.3 mm and represent aggregates of crystals of irregular shape ("hedgehogs").

Crystallized usually filtered on a centrifuge, after which the content of moisture is ~3% (RWCU) or ~5% (internals). Drying kristalliset having a temperature of 30-40°C, as a rule, is carried out in the fluidized bed apparatus (COP) at a temperature of 120-150°C until the content of moisture of 0.1-0.3%, after which the product is treated to prevent caking of the amine or the ferrocyanide of potassium (sodium) in alkaline medium. The product is used mainly for technical purposes, for example in the production of potassium nitrate, potassium sulfate, KOH, NPK fertilizers and other purposes, so the presence of extraneous salts unacceptable, and the content of sodium chloride limit is regulated.

Regulatory documentation content-caking agent, such as an amine, in gallerycheck potassium chloride should not exceed 200 g/t, but many consumers ask about reducing its content in the target product to a minimum.

Gallaratese potassium chloride belongs to the class of hydrophilic substances, for which the caking is caused by traces of hygroscopic water "sucked" concave surfaces intergrowths of crystals from the external environment with the formation on the surface of the crystals saturated in KCl solution. When migration solution in the dispersion medium during the storage of material due to fluctuations in ambient temperature occurs secondary crystallization of KCl and hardening of the dispersed product. This process occurs repeatedly during storage and transportation of potassium chloride, which leads to caking and loss of flowability.

Our experiments showed the possibility of a sharp decrease in the content of the target product reagents-anti-caking agent due to structural agglomeration of kristalliset in the mixer-granulator by processing it filtered wet kristalliset hot dry potassium chloride, obtained after drying the mixture. Particles of potassium chloride after internals and drying have an irregular shape that is substantially different from ravnovesnoi - cubic. Therefore, the surface energy of the particles is excessive, the system has a high sorption activity and are able to agglomeration of crystals with particle formation with minimum surface energy. The water plays the role of surfactants in the process of formation of the phase contacts.

The proposed method for obtaining particles of potassium chloride this effect is achieved by forcing the packing dispersed material in the mixer-granulator. When structural agglomeration is a mechanical leveling the surface of the crystals ("hedgehogs") and elimination of defects in the crystals due to their enveloping fine product, formed by abrasion of polydisperse particles. When interacting wet kristalliset with a large number of hot, dry potassium chloride on the border of the particles is the formation of a vapor phase, which leads to migration of the solution contained in crystallizatio, to the surface of the crystals. It also facilitates alignment of the entire surface of the solid phase and reduces the effect of the destruction of the crystals at their sudden heat in the drying zone, for example, in the apparatus of the constitutional court. "Soft" heat of the mixture and its mechanical processing in the mixer-granulator reduces the effect of thermal deformation of crystals, which occurred is carried out with the crystallization of potassium chloride from the solution and drying of kristalliset.

Table 1 shows the compositions of galilejskogo potassium chloride, subjected to structural agglomeration.

Table 1
Material nameContent, wt. %The average particle size, mm
KClNaClMgCl2CaSO4H2O
Crystallized after installation, vacuum crystallization, and filtering91,713,020,050,025,200,26
Crystallized after installing the adjustable vacuum crystallization and filtering96,300,710,030,012,950,65

Table 2 shows data on the rheological properties galilejskogo potassium chloride, subjected to structural agglomeration and drying.

Table 2
The name of the indicator and its dimensionMaterial name
Control sample of the prototype with the addition of sodaCrystallized after internals and filteringCrystallized after RUKU and filtering
1234
1. Consumption of dry hot potassium chloride, %2025/10025/100
2. Drying temperature, °C85135110/105
3. The KCl content in the target product, %95,8296,7599,10/99,05
4. The content of H2O in the target product, %0,450,090,12/0,17
5. The average particle size, mm0,270,280,67
6. The content of the fraction is 0.1 mm %1,00,70,01
7. Friability, %100100100
8. Caking (stress fracture), kg3,22,8/1,72,4/1,5

As a control sample investigated glogicheski potassium chloride, obtained from stage vacuum crystallization and filtration (see table 1), treated with soda ash in accordance with the recommendations of the prototype.

Cyclone dust on the prototype was returned to the agglomeration, and upon receipt of KCl on the proposed method in the process in accordance with production requirements. When drying control sample in the temperature range of 70-110°C was observed clogging of the ducts of the apparatus of the COP due to the condensation of vapors. When drying the samples at temperatures above 135°C was observed cracking of the crystals and the growth fraction content -0,1 mm in the target product because of the intense boiling of the liquid phase inside and on the surface of the particles. The boiling point of the solution is ~107°C, therefore, the optimal drying temperature should be considered ~110°C, which provides a "soft" warm-Krista is fishing, reduce the risk of their destruction.

In accordance with the regulatory documents deemed to be significant indicators according to claim 3, 4, 6, 7, 8 - see table 2.

From the table 2 data shows that the proposed method is obtained glogicheski potash higher quality, which does not contain impurities.

In the proposed method the hot dry MOP served in a number of 25-100% by weight of wet kristalliset. From paragraph 8 of table 2 shows that the main indicator of rheological properties - caking decreases with the increase in the share of dry hot potassium chloride in the mixture. Additional costs for drying material is not required, but increase retur requires maintenance costs of equipment for transportation reture and structural agglomeration of the material. Therefore, in the present material, the upper limit of the flow rate of retur adopted 100%, but it can be increased. Reducing consumption of dry hot potassium chloride less than 25% affects the rheological properties of the target product and requires the use of structure-forming additives.

At the request of consumers obtained target product can be treated with conventional-caking agent such as amines, but their consumption should be reduced by 2-3 times, i.e. instead of the standard 200 g/t must be given not more than 100 g/so

That is they way the proposed method solves the problem of improving the quality galilejskogo potassium chloride due to the departure from the use of structure-forming additives, reduction or waiver of reagents added to prevent caking of the target product and improve the rheological properties of the material due to the reduction in him particulate fractions of potassium chloride.

The method is as follows. Crystallized obtained by dissolving sylvinite ores, the clarification of a hot saturated solution, cooling installations, vacuum crystallization and separation of the resulting suspension by filtration, subjected to structural agglomeration in the mixer-granulator by adding thereto a dry hot potassium chloride in the amount of 25-100% by weight of kristalliset.

The resulting agglomerate was dried at a temperature of 105-135°C, for example, in a fluidized bed apparatus (COP), preferably at a temperature of 110°C. the dry Part of the target product was returned for structural agglomeration filtered kristalliset.

Examples of the method.

Example 1.

100 tons filtered kristalliset after RUKU with a moisture content of 3.8% and a temperature of 40°C was subjected to structural agglomeration in the mixer-granulator by adding thereto 100 tonnes of dry potassium chloride with a temperature of 110°C and the content of H2O - 0,1%. Received the initial material was dried at 110°C in the fluidized bed apparatus with obtaining the target product. The content in the product fraction is less than 0.1 mm to 0.02%. Caking of 1.5 kg

Example 2.

The method was carried out in accordance with example 1, but the finished product was treated with amine hydrochloric acid in the amount of 60 g/t was Received material from caking 0,9 kg

1. The method of obtaining galilejskogo potassium chloride with improved rheological properties, including structural agglomeration of the mixture moist kristalliset hot and dry potassium chloride in the mixer-granulator, followed by drying the mixture, characterized in that the structural agglomeration of the mixture of the hot dry MOP served in a number of 25-100% by weight of wet kristalliset and drying of the mixture is conducted in the temperature range of 105-135°C To produce the target product.

2. The method according to claim 1, characterized in that the drying of the mixture is conducted preferably at a temperature of 110°C.



 

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