Method for optimizing crystallization of potassium chloride based on online monitoring system

A monitoring system and potassium chloride technology, applied in chemical instruments and methods, solution crystallization, crystallization separation, etc., can solve problems such as inability to achieve optimal crystallization effect, secondary nucleation, spontaneous nucleation, etc.

Inactive Publication Date: 2019-08-23
QINGHAI UNIV FOR NATITIES
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is: in order to solve the present optimal treatment of potassium chloride crystallization process, often concentrate on the influence of supersaturation, impurity and other ions on the crystal habit of potassium chloride crystal, but can not reach good optimized crystallization effect, there will still be spontaneous nucleation and secondary nucleation problems, and a method based on an online monitoring system to optimize the crystallization of potassium chloride is proposed

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  • Method for optimizing crystallization of potassium chloride based on online monitoring system
  • Method for optimizing crystallization of potassium chloride based on online monitoring system
  • Method for optimizing crystallization of potassium chloride based on online monitoring system

Examples

Experimental program
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Effect test

Embodiment 1

[0050] The present embodiment provides determination of solubility:

[0051] Using the static method, from high temperature to low temperature, to measure the solubility of potassium chloride at different temperatures, add 100mL of high-purity water to the jacketed crystallizer, open the program-controlled constant temperature bath, and set the temperature to 10°C, 20 ℃, 30 ℃, 40 ℃, a total of four groups, keep warm for 30 minutes respectively, add 50g of potassium chloride, turn on the electromagnetic stirrer and stir at constant temperature for 1 hour, so that the system can fully reach the state of solid-liquid two-phase equilibrium, turn off the magnetic stirring, and let it stand 1h, and read the temperature T, the mass of the pipette with the tip of the pipette is m 1 Pipette gun to pipette 10mL supernatant, weigh the total mass of the pipette and the solution m 11 , move the solution into the crucible, then the total mass is m 2 , and rinse the straw with pure solvent...

Embodiment 2

[0054] In this embodiment, without adding seed crystals, the metastable zone of potassium chloride is determined.

[0055] Take potassium chloride and water into the crystallizer according to the mass ratio of 1:5, turn on the stirrer, FBRM, PVM online monitoring system, and insert the temperature probe, heat up to 55°C to completely dissolve potassium chloride in the crystallizer, and then Measure the supersolubility data at a cooling rate of 5-15°C / h and a rotating speed of 200-400r / min. When tiny crystals appear, the temperature will change suddenly. Write down the temperature T when the sudden change occurs, and then the prepared potassium chloride solution will be The mass ratio is the supersolubility at this temperature. (there are 6 groups of tests in this embodiment, with stirring rate and cooling rate as variables, respectively: the stirring speed is 300r / min, and the cooling rate is 5°C / h; the stirring speed is 300r / min, 10°C / h; the stirring speed 300r / min, 15°C / h; ...

Embodiment 3

[0061] In this embodiment, crystal seeds are added to measure the metastable zone of potassium chloride.

[0062] Under the condition of a rotating speed of 300r / min, the temperature of 100g of potassium chloride solution with a mass fraction of 20% is raised to 70-90°C and then lowered to its saturation temperature T 1 After 30 minutes of heat preservation, potassium chloride seed crystals were added (two sets of data, when the seed crystal masses were 2g and 6g respectively), and the FBRM and PVM online monitoring systems were turned on at the same time, and the temperature probe was inserted, and the temperature was lowered at a rate of 5°C / h until the temperature suddenly changed. , FBRM, and PVM systems detect that the number of crystals increases, and record the corresponding temperature at this time as T 2 , the metastable zone data of the potassium chloride solution of this concentration can be obtained under the conditions of stirring rate, cooling rate and seed cryst...

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Abstract

The invention discloses a method for optimizing the crystallization of potassium chloride based on an online monitoring system, and belongs to the field of potassium chloride production. A static technology is adopted to detect solubility data and supersolubility data of potassium chloride, the focused beam reflectance measurer (FBRM) and online particle size analyzer (PVM) monitoring system to detect the metastable zone of potassium chloride crystallization, the solubility of the potassium chloride gradually increases with the increase of the temperature, increase of the cooling rate widens the width of the metastable zone of potassium chloride, increase of the stirring speed narrows the width of the metastable zone of potassium chloride, and reduction of the addition amount of seed crystals narrows the width of the metastable zone of potassium chloride. The problem that existing optimization of the crystallization process of potassium chloride tends to focus on the influences of supersaturation, impurities and other ions on the crystal habits of potassium chloride crystal, but does not achieve a good crystallization optimization effect and spontaneous nucleation and secondary nucleation still exist is solved in the invention.

Description

technical field [0001] The invention relates to the field of potassium chloride production, in particular to a method for optimizing potassium chloride crystallization based on an online monitoring system. Background technique [0002] Potassium chloride is not only an important potassium fertilizer, but also an important chemical raw material. According to the survey, 84% of the land in our country is deficient in potassium, and our country is relatively deficient in potassium resources. There is a large gap between the supply and demand of potassium resources, and we have long relied on imports. We are the second largest importer of potassium fertilizer in the world. In the production process of salt chemical industry in our country, due to the constraints of production technology and equipment conditions, the produced potassium chloride products are of low grade and high impurity content, which makes the resources not optimally utilized. Therefore, the research on the cr...

Claims

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Application Information

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IPC IPC(8): B01D9/02C01D3/24
CPCB01D9/0031B01D2009/0086C01D3/24
Inventor 王刚解玉龙张莉媛杨小波
Owner QINGHAI UNIV FOR NATITIES
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