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Method of controlling process of sylvinite ore dissolution

Method of controlling process of sylvinite ore dissolution
IPC classes for russian patent Method of controlling process of sylvinite ore dissolution (RU 2352385):
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FIELD: chemistry.

SUBSTANCE: invention relates to technique of controlling processes of sylvinite ores dissolution and can be used in production of potassium chloride by dissolution-crystallisation method. Method of controlling processes of sylvinite ores dissolution includes regulation of ore supply depending on content of useful component in input flows, measuring ready solution temperature and determining sodium chloride content in solution by calculation method. Additionally determined are density, temperature and consumption of dissolving solution, content of sodium chloride in it is determined by content of useful component, density and temperature. Ore supply is calculated according to suggested equation and calculated value is given as task to system of weigher control.

EFFECT: invention allows to simplify controlling process of sylvinite ores dissolution.

2 cl, 8 tbl, 3 ex

 

The invention relates to a technique of managing the processes of dissolution of sylvinite ore containing potassium salts, and can be used in the production of potassium chloride by the method of dissolution-crystallization.

The known method for automatic process control leaching of potassium chloride of potash, by changing the flow rate input streams - see A.S. USSR №1060569, CL C01D 3/08; G05D 27/00. Publ. 15.12.83, bull. No. 46. In the proposed method the total flow of water to the composition of the input streams, regulate, depending on the consumption of liquor with correction for water consumption for washing machine, consumption, recycling salt solution, the density of the salt solution and the circulating liquor, the total consumption of potassium chloride in the composition of the input streams, the concentration of potassium chloride in a saturated liquor and the temperature of the liquor will impact on the flow of liquor into the machine.

The method has a high complexity, since its implementation is impossible without the implementation of a complete chemical analysis of the input streams to determine the water content of the system. Analytical control is a lengthy process, as it involves sampling, preparation for analysis and determination of components in the system KCl-NaCl-H2O in the presence of MgCl2and other impurities. The results of the analysis comes to the production of chlorine is East of potassium delayed for 3-4 hours, and in terms of large-scale production (for example, BY Uralkali flows reach 1500 m3/h) they have a significant impact on the progress of the process does not have. Therefore, the full chemical analysis used statistical material.

Wide application of analytical control does not allow for operational control of the technological process, and in terms of the low content of chlorides of magnesium and calcium in the sylvinite ore is accumulated in the circulating liquor is practically not observed and the conclusion of the process of cold saturated liquor is not required.

A known method of controlling the process of dissolution of the salt ore such as potash, by stabilizing the flow of the original solution and controlling the feed of ore depending on the content of useful component in the input flow and temperature measurement of a ready solution - prototype - see A.S. USSR №1256776, CL B01F 1/00; G05D 27/00. Publ. 15.09.86. Bull. No. 34. The proposed method additionally measure the mineral content in the finished solution, and depending on the temperature of the prepared solution and the contents of the received component, it determines the content of sodium chloride in the finished solution. The content of useful component in source and finished solutions and the calculated value of the content of sodium chloride on Radelet the ratio of the water content in the initial and final solutions and regulate the flow of ore in addiction, cited in A.S.

The method is complex because the definition of the content of sodium chloride in the finished solution is determined by the method of calculation depending on the temperature and content in the solution of potassium chloride. The calculation assumes that the degree of saturation of the prepared solution of sodium chloride equal to 1. However, operating experience potash production shows that in the finished solution is always an excessive amount of solid sodium chloride, the presence of which in solution is determined by the removal of particles of halite ore in the clarification process, the evaporation of water from the surface of the thickeners at a temperature of clarification and crystallization of sodium chloride by cooling and evaporation of the solution. Therefore, the proposed method requires the use of methods of analytical control to determine the NaCl in the finished solution. In addition, stabilization of the flow of the original solution is complex, as is the need to install a buffer tank of large volume (up to 1500 m3for smooth flows changes in working solution by unloading clay-saline sludge and concentrate, leaching equipment, etc.

The task of the invention is its simplified through the use of modern low-inertia automatic controls and automatic control process is ω dissolution of sylvinite ores.

The problem is solved in that in contrast to the known method further measure the density, temperature and flow rate of the solvent of a solution, determine the content of sodium chloride in mineral content, density and temperature and regulate the flow of ore dependencies:

,

where Qore- ore consumption, t/h;

QR.R-Rthe flow of solvent solution, t/h;

Tgtr-Rthe temperature of this solution, °C;

WithKClR. R-R- mass fraction of KCl in solvent solution;

ρR.R.-p- the density of the solvent solution, t/m3;

TR. R-R- the temperature of the solvent solution, °C;

Ini- constant coefficients, i=0, 1, 2, 3, 4, 5, 13, 34,

Andi- empirical coefficients, i=0, 1, 2, 3.

CNaCl R. R-R- mass fraction of NaCl in solvent solution for a range of temperatures 60-75°C.

When the flow solvent solution between the main solvents and apparatus for heat recovery, for example, when discharge of the mixer, in which heat recovery is carried out halite blade cold solvent solution, the second solvent consumption, solvent of the solution is determined by the relationship:

where FR.R.-P1and FR.R.-the 2 threads solvent liquor between devices, m3/h;

ρR. R-P2the density of cold solvent solution, t/m3.

The method consists in the following. In contrast to the known method, the proposed method of managing the process of dissolution of sylvinite ore is that the amount of potassium chloride introduced into the cycle with the ore, is equivalent capacity for potassium chloride solvent solution at a temperature of dissolution with variations in the flow rate and composition.

The flow of ore extinguish all the perturbations that occur in the technological cycle of production of potassium chloride, which affect the flow rate and solvent composition of the solution. The proposed method to measure the density, temperature and flow rate of the solvent of a solution, determine the content of potassium chloride and content of useful component is potassium chloride, density and temperature determine its content of sodium chloride. In the ore also determine the content of potassium chloride.

The supply of ore to the dissolution adjust for dependencies:

where Qore- ore consumption, t/h;

WithKCl ore- mass fraction of KCl in the ore;

Tgtr-Rthe temperature of this solution, °C;

CKCl R. R-R- mass fraction of KCl in solvent solution;

<> ρR.R-R- the density of the solvent solution, t/m3;

TR.R-R- the temperature of the solvent solution, °C;

QR.R-Rthe flow of solvent solution, t/h;

Ini- constant coefficients, i=0, 1, 2, 3, 4, 5, 13, 34.

The calculated mass fraction of NaCl in the solvent solution for the temperature interval from 60 to 75°C is determined by dependencies

,

where Qore- managed the flow of ore, t/h;

QR.R-Rthe flow of solvent solution, t/h;

CKCl ore- mass fraction of KCl in the ore;

Tgtr-Rthe temperature of this solution, °C;

CKCl R. R-R- mass fraction of KCl in solvent solution, %;

ρR R-R- the density of the solvent solution, t/m3;

TR. R-R- the temperature of the solvent solution, °C;

Andi- empirical coefficients, i=0, 1, 2, 3.

The dependences show that all the parameters of the equation of flow can be quickly determined with the help of modern sensors, low inertia, and the result processed in the controller, where the signal is sent to control the dosing flow rate of sylvinite ore. This control system is almost instantaneous.

When developing a mathematical model of the stages of dissolution of sylvinite ore was shown that one of nazimah factors which must be considered in the management process, is the mass fraction of NaCl in the solvent solution. Direct measurement of mass fraction of NaCl using the instrumentation is not possible. Therefore, the implemented calculation method for the determination of NaCl on the basis of the automatically measured parameters: the mass fraction of KCl, density and temperature of the solvent liquor application developed in VNIIG "Method of coefficient - see Method of calculation of the density of the complex salt systems. Proceedings of VNIIG, vol.No. 36, Goskomizdat, 1959. This method allows to determine the empirical coefficients Andi.

Applying a known method three-factor experiment (see, for example, Planning of experiment in chemistry and chemical technology". The Sautin S.N. Ed. "Chemistry", L., 1975) when processing the resulting technological calculations of data received basic equation relating the density of the solvent liquor with its composition and temperature:

.

Transforming this equation, we obtain the dependence of the mass fraction of NaCl in solvent solution WithNaCl R. R.-R.

This equation is valid for an interval of 60-75°C and in the range is the temperature of the solvent solution after heat recovery. However, the temperature interval if necessary, the can is to be expanded.

Through the use of automatic analyzers for determining the content of KCl in the ore and solutions, as well as the use of the calculation method of determining the content of NaCl in solutions based on indirect parameters: density and temperature, these parameters are determined by the automatic control means with sufficient accuracy. Kinetic regularities of the process of dissolution of sylvinite ore taking into account factors such as the residence time of the solid phase in the solvent, the rate of leaching of KCl ore, etc. incorporated in the project setup dissolution and taken into account when selecting equipment. Therefore, to control the stage of dissolution of the proposed method using a static model. Development of mathematical model is made using the method of mathematical planning of the full factorial experiment based on actual statistical data of existing facilities involving mathematical description of the process in the diagram, the solubility of the water-salt system KCl-NaCl-H2O in the presence of MgCl2. To determine the coefficients Iniin the above equation, calculate material balances process of dissolution of sylvinite ores based on, for example, from a condition of receipt of the final solution with a degree of saturation on KCl equal to 0.98, the temperature drop of the prepared solution from optimalnoe, equal to 2°C, the degree of leaching of KCl ore - not less than 0.95.

As independent variables are:

- mass fraction of KCl in the ore;

the temperature of this solution (the temperature of the drain of the first solvent);

the flow of solvent solution;

- mass fraction of KCl in solvent solution;

- mass fraction of NaCl in the solvent solution.

The total number of material balance calculations in the planning matrix was 25or 32. Material balances that determine the flow of ore, were calculated according to standard techniques (see, for example, "Technology of potash fertilizers". Kashkarov OD, Sokolov, I., Ed. "Chemistry", D., 1978) and is not contained in the description because of grimscote and widely known methods of calculation.

Material balances flow of ore to the dissolution taking into account the zero error of the instrument, with which they control the value of process parameters, made in the traditional way using charts solubility of salts in the system KCl-NaCl-H2O in the presence of MgCl2.

Next, perform a calculation taking into account the lower and upper levels of the maximum permissible error of the instrument, make the assessment of the technological reproducibility of the calculations, the calculation of the regression coefficients, assess their significance and adequacy of the regression equations.

Table 1 shows the levels facto is impressive and ranges of their variation for dissolution of sylvinite ore, for example, for the conditions of the ore processing at the Verkhnekamskoye field.

Table 1
The name of the parameter Level factors
Basic level The intervals of variation The lower level The top level
Mass fraction of KCl in the ore, %
Mass fraction of KCl in
solvent solution, %
Mass flow
solvent solution, t/h
Mass fraction of NaCl in
solvent solution, %
Temperature ready
solution, °C
24,00
11,50
834
19,50
93
4,00
1,00
231
1.00
2
20,00
10,50
603
18,50
91
28,00
12,50
1065
20,50
95

Table 2 shows the results of determination of the coefficients Initaking into account the exceptions to the equation insignificant coefficients.

Table 2
Factor In0,t/h In1t/h In 2t/(h*grad) In3 In4t/h In5t/h In34 In13
Its value 339,446 35,5774 6.27135 1,44301 3,8405 1161,81 5360216 1,663777

After substitution of the above factors the addiction to control the flow of ore to the process of dissolution of sylvinite ores will be:

When the flow solvent solution between the main solvent and apparatus for heat recovery, for example, when discharge of the mixer, in which heat recovery is carried out halite blade cold solvent solution, the second solvent consumption, solvent of the solution is determined by the relationship:

,

where Fp.p-p1,2threads solvent solution between devices, m3/h;

ρp.p-p2- flux solvent solution into the mixer for heat recovery, t/m3.

Table 3 shows the levels of the factors and their intervals argirova the Oia to determine the empirical coefficients And i.

Table 3
The name of the parameter Level factors
Basic level The intervals of variation The lower level The top level
Mass fraction of KCl in solvent dissolved, % 11,50 1,00 10,50 12,50
Mass fraction of NaCl in the solvent solution, % 19,50 1,00 18,50 20,50
The temperature of the solvent solution, °C 67.5 7,5 60 75

Its value
Table 4
Factor And0 And1 And2m3/t And3, 1/deg
1,6494 0,0075 1 0,0006

After substitution of the coefficients Andiin equation (2) with the variables expressed in coded form, the dependence for the calculation of the mass fraction of NaCl in the solution will have the form:

.

When changing the process parameters, the mass fraction of KCl in the ore and solvent solution, temperature, mass fraction of NaCl in the solvent solution over intervals of varying the numerical values of the coefficients Iniit should be correct.

In tables 5 and 6 show additional new intervals varying factors of technological parameters (table 5), the values of the coefficients Ini(table 6), the intervals of variation and experimental values of the coefficients Andiare shown in tables 7 and 8.

Table 5
The name of the parameter Level factors
Basic level The intervals of variation The lower level The top level
M is Sova fraction of KCl in the ore, %
Mass fraction of KCl in
solvent solution, %
Mass flow
solvent solution, t/h
Mass fraction of NaCl in
solvent solution, %
Temperature ready
solution, °C
31,70
12,00
1340
18,00
97
1,50
2,00
280
2,00
1
30.20mm
10,00
1060
16,00
96
33,20
14,00
1620
20,00
98

Table 6 shows the results of determination of the coefficients Initaking into account the exceptions to the equation insignificant coefficients.

Table 6
Factor In0t/h In1t/h In2t/(h*grad) In3 In4t/h B5t/h In34
Its value 43,0042 1475,787 8,0817 0,85014 5,125 1436,52 4,20325

After substitution of the above factors the addiction to control races who Odom ore dissolution process of sylvinite ores will be:

Table 7 shows the levels of the factors and ranges of their variation to determine the empirical coefficients Andi.

Table 7
The name of the parameter Level factors
Basic level The intervals of variation The lower level The top level
Mass fraction of KCl in solvent solution, % 12,00 2,00 10,00 14,00
Mass fraction of NaCl in the solvent solution, % 18,00 2,00 16,00 20,00
The temperature of the solvent solution, °C 67,5 7,5 60 75

Table 8
Factor And0 And1 And2m3/g And3i/deg
Its value 1,1958 0,01525 0,01625 0,00450

After substitution of the coefficients Andiin equation (2) with the variables expressed in coded form, the dependence for the calculation of the mass fraction of NaCl in the solution will have the form:

These parameters cover almost the whole area of work gallerycheck enterprises for the processing of sylvinite ores.

Thus, the task of simplifying the management process of dissolution of sylvinite ores by replacing long analytical control automatic analyzer potassium and low-inertia automatic sensors of process parameters - temperature, flow, and density using the results of measurement for automatic control of the flow of ore from the application of PC in the supervisor mode.

The method is as follows. Solvent solution after heat recovery at the UWC with a temperature of 60-75°C is directed to the dissolution, the solution determines the temperature of thermocouple with the University of fitiavana output signal - for example, TSMU-055; density - for example, using a primary Converter MFS2000 and signal Converter MFS081 consumption and the solvent of the solution - for example, by the induction flow meter type SORA HEH.

Mass fraction of potassium in the ore and solvent solution is determined by measuring potassium, for example, the company "Bertold" LB 377-62. The temperature of this solution is also determined with the aid of thermocouple.

The received signals are sent to the controller and the PC, where the signal goes to automatic tape dispenser, which belt speed controls the flow of ore in the automatic mode the dependencies (1) and (2).

Examples of the method

Example 1

1. The readings for determining the mass fraction of NaCl have the values:

0,115 - mass fraction of KCl in solvent solution;

1,205 - density solvent solution, g/cm3;

68,3 - temperature solvent solution, °C.

The calculation of the mass fraction of NaCl in the solvent solution:

.

Mass fraction of NaCl used in the calculation of consumption of ore.

2. The performance of devices for determining the flow of ore have values:

0,239 - mass fraction of KCl in the ore;

92,2 - temperature ready solution, °C;

853,20 - flow solvent solution, m3/PM

Calculation of ore consumption:

The calculated value of the flow of ore served as the task management system weighing feeder, and sylvinite ore is fed into the solvent. A survey of automatic devices produced with an interval of 10 seconds.

Example 2

The performance of devices for determining the flow rate of the solvent of the solution have the values:

771,30 - flow solvent solution in basic solvents, m3/h;

80,04 - flow solvent solution in the apparatus for heat recovery halite blade, m3/h;

1,205 - density solvent solution in the main solvent, g/cm3;

1,233 - density solvent solution in the apparatus for heat recovery halite blade, g/cm3.

.

.

Example 3

3. The readings for determining the mass fraction of NaCl have the values:

0,120 - mass fraction of KCl in solvent solution;

1,205 - density solvent solution, g/cm3;

67,7 - temperature solvent solution, °C.

The calculation of the mass fraction of NaCl in the solvent solution:

.

.

Mass fraction of NaCl used in the calculation of consumption of ore.

4. Instrument readings to determine flow of ore have values:

0,308 - mass fraction of KCl in p is de;

of 97.8 - temperature ready solution, °C;

1118 - flow solvent solution, m3/PM

The calculation flow of ore:

.

1. The process control method of dissolution of sylvinite ores, including the regulation of feeding ore depending on the content of useful component in the input streams, the temperature measurement of the prepared solution and the determination of the content of sodium chloride in the solution design method, characterized in that it further measure the density, temperature and flow rate of the solvent of a solution, determine the content of sodium chloride in mineral content, density and temperature, calculate the ore feed to the following dependence and the calculated value serves as the task management system weight batcher:


where Qore- ore consumption, t/h;
CKCl ore- mass fraction of KCl in the ore;
Tgoth. R-Rthe temperature of this solution, °C;
CKCl R. R-R- mass fraction of KC1 in solvent solution;
ρR.R-R- the density of the solvent solution, t/m3;
TR. R-R- the temperature of the solvent solution, °C;
QR.R-Rthe flow of solvent solution, t/h;
Bi- constant coefficients, i=0, 1, 2, 3, 4, 5, 13, 34;
CNaCl p. p-p- mass fraction of NaCl in the solvent solution for the temperature range from 60 to 75°C;
Andi- empirical coefficients, i=0, 1, 2, 3.

2. The method according to claim 1, characterized in that when the division of the flow of solvent solution between the main solvents and apparatus for heat recovery amount is governed by the dependence:
Qp.p-p=FR. p-p1·ρp.p-p+FR. R-P2·ρR. R-P2,
where Fp.p.p1and Fp.p.p2threads solvent solution between devices, m3/h;
ρp.p-p2the density of cold solvent solution of the heat recovery, t/m3.

 

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