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A kind of method that solvent extraction prepares potassium nitrate

A potassium nitrate and extraction technology, applied in the field of solvent extraction to prepare potassium nitrate, can solve the problems of unsatisfactory extraction effect, high separation cost, large consumption of isoamyl alcohol, etc., achieve easy control of extraction and back-extraction operations, simplify extraction and Stripping operation, good extraction effect

Active Publication Date: 2017-01-18
SICHUAN UNIV
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Problems solved by technology

This method has the following disadvantages: (1) high energy consumption: the reaction temperature is controlled at about 5°C, and a large amount of refrigeration energy consumption is required in the production process, resulting in high production costs; (2) HCl and HNO cannot be effectively separated 3 , the extraction and separation operation is complex and cumbersome: due to the mutual solubility between isoamyl alcohol and TBP and water, there will be the phenomenon that TBP contains isoamyl alcohol and isoamyl alcohol contains TBP, resulting in unsatisfactory extraction effect and separation process. Complex, separation of HCl and HNO 3 The process of the process has become the main part of the whole potassium nitrate production process, and the separation cost is high; (3) the consumption of extractant is large: the method adopts isoamyl alcohol to extract HCl, and the distribution coefficient of HCl in isoamyl alcohol and water is about 0.058~0.57, That is, isoamyl alcohol has a better selectivity to HCl when the HCl concentration is higher, but usually the HCl concentration in the potassium nitrate crystallization mother liquor is not high, so the extraction rate of isoamyl alcohol to hydrochloric acid is low, and isoamyl alcohol is in water. Solubility is bigger, and part isoamyl alcohol is dissolved in aqueous phase and causes loss during extraction, therefore, to reach certain extraction effect, the consumption of isoamyl alcohol is big, causes production cost height; (4) the concentration of by-product hydrochloric acid is very low , is 7.5% to 8.5%, and contains impurity HNO 3 , although the hydrochloric acid with a concentration of about 20% can be obtained through further concentration, the concentrated hydrochloric acid still cannot be sold as a product, and the concentration operation needs to consume a large amount of energy, and there is also the problem of high energy consumption. The by-product hydrochloric acid contains HNO 3 also caused raw material NO 3 - waste of

Method used

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  • A kind of method that solvent extraction prepares potassium nitrate
  • A kind of method that solvent extraction prepares potassium nitrate

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Experimental program
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Embodiment 1

[0028] The process flow of this embodiment is as figure 1 As shown, the steps are as follows:

[0029] (1) Add 100g of potassium chloride, 233g of water and the raffinate aqueous phase (at the beginning of the process, the raffinate aqueous phase is water) into the reaction vessel, prepare a saturated potassium chloride solution at a temperature of 50℃, and add it to the reaction vessel 103g nitric acid with a concentration of 68wt% was reacted at 50℃ for 60min under normal pressure and stirring. The resulting reaction solution was naturally cooled to 25℃, filtered, and the resulting filter cake was washed with 20g of water and dried to obtain 1 # 63g of potassium nitrate product, with a yield of 56%;

[0030] (2) Step (1) Filter to obtain 364g filtrate, in which H + The content is 0.30wt%, Cl - The content is 12.89wt%, NO 3 - The content is 8.75% by weight, the extractant is added to the filtrate, the volume ratio of the extractant to the filtrate is 1.5:1, the extraction is perfor...

Embodiment 2

[0041] The process flow of this embodiment is as figure 1 As shown, the steps are as follows:

[0042] (1) Add 100 g of potassium chloride, 218 g of water and the raffinate aqueous phase (at the beginning of the process, the raffinate aqueous phase is water) into the reaction vessel, prepare a saturated potassium chloride solution at a temperature of 60°C, and add it to the reaction vessel 83g of nitric acid with a concentration of 68wt%, reacted at 60°C for 45min under normal pressure and stirring, the resulting reaction liquid was naturally cooled to 30°C, filtered, and the resulting filter cake was washed with 25g of water and dried to obtain 1 # 49g of potassium nitrate product, with a yield of 54%;

[0043] (2) Step (1) filter to obtain 341g filtrate, in which H + The content is 0.26wt%, Cl - The content is 13.54wt%, NO 3 - The content is 7.79wt%, the extractant is added to the filtrate, the volume ratio of the extractant to the filtrate is 1:1, the extraction is carried out at...

Embodiment 3

[0052] The process flow of this embodiment is as figure 1 As shown, the steps are as follows:

[0053] (1) Add 100 g of potassium chloride, 208 g of water and the raffinate aqueous phase (at the beginning of the process, the raffinate aqueous phase is water) into the reaction vessel, prepare a saturated potassium chloride solution at a temperature of 70°C, and add it to the reaction vessel 130g of nitric acid with a concentration of 65% by weight, stirred and reacted at 70°C under normal pressure for 30min, the resulting reaction liquid was naturally cooled to 20°C, filtered, and the resulting filter cake was washed with 15g of water and dried to obtain 1 # 72g of potassium nitrate product, with a yield of 53%;

[0054] (2) Step (1) Filter to obtain 361g filtrate, in which H + The content is 0.37wt%, Cl - The content is 13.22wt%, NO 3 - The content is 11.21wt%, the extractant is added to the filtrate, the volume ratio of the extractant to the filtrate is 3:1, the extraction is carri...

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Abstract

The invention provides a method for preparing sodium nitrate through solvent extraction. The method includes the following steps that step1, a potassium chloride saturated solution with the temperature of 50 DEG C-70 DEG C is prepared, nitric acid is added to react with the potassium chloride saturated solution at the temperature of 50 DEG C-70 DEG C, cooling crystallization and solid-liquid separation are performed, and an obtained solid phase is washed with water and dried to obtain a potassium nitrate product; step2, an extraction agent is added into a liquid phase obtained in solid-liquid separation in the step1, and a raffinate water phase is returned into a reaction vessel in the step1; 3, an organic phase obtained in extraction in the step2 is mixed with water or a second mother solution, ammonia gas is led into the mixture for reverse extraction, and a reverse extraction organic phase is returned to the step2; 4, condensation crystallization and solid-liquid separation are performed on a reverse extraction water phase in the step3 to obtain ammonium chloride and a first mother solution, potassium chloride is added into the first mother solution and reacts with the first mother solution at the temperature of 60 DEG C-80 DEG C, cooling crystallization and solid-liquid separation are performed to obtain a solid phase and the second mother solution, the obtained solid phase is washed and dried to obtain a potassium nitrate product, and the second mother solution is returned to the step3.

Description

Technical field [0001] The invention belongs to the field of agricultural fertilizer production, and particularly relates to a method for preparing potassium nitrate by solvent extraction. Background technique [0002] Potassium nitrate is a high-grade nitrogen and potassium binary compound fertilizer containing no chlorine. Its total nutrient content is as high as 60wt%. It is universally applicable and has no volatility. After application, it can be completely absorbed by plants and soil without being brought into it. Chemical residues can effectively improve the quality and yield of plants and are called "true green fertilizers". There are many production methods of potassium nitrate, and the main methods currently used in the industry are: sodium nitrate-potassium chloride conversion method, ammonium nitrate-potassium chloride double decomposition method, ion exchange method, nitric acid and potassium chloride preparation method. [0003] Wang Guiyun et al. reported a method f...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01D9/04C01D9/08
Inventor 李军马誉景金央陈明罗建洪
Owner SICHUAN UNIV
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