Method for preparing sodium nitrate through solvent extraction

A potassium nitrate 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., and achieve easy control of extraction and stripping operations, simplify extraction and Back-extraction operation, good extraction effect

Active Publication Date: 2015-11-11
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

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  • Method for preparing sodium nitrate through solvent extraction
  • Method for preparing sodium nitrate through solvent extraction

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Effect test

Embodiment 1

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

[0029] (1) Add potassium chloride 100g, water 233g and raffinate water phase (the raffinate water phase is water at the initial stage of process start-up) into the reaction vessel, prepare a potassium chloride saturated solution with a temperature of 50°C, and add Concentration is 103g of nitric acid of 68wt%, under normal pressure, under agitation, react at 50 ℃ for 60min, the gained reaction liquid is naturally cooled to 25 ℃, filter, the gained filter cake is washed with 20g water and dried to obtain 1 # Potassium nitrate product 63g, productive rate is 56%;

[0030] (2) step (1) is filtered to obtain filtrate 364g, and in this filtrate, H + Content is 0.30wt%, Cl - The content is 12.89wt%, NO 3 - Content is 8.75wt%, in this filtrate, add extraction agent, the volume ratio of extraction agent and filtrate is 1.5:1, carry out extraction at 25 ℃, extraction residence ...

Embodiment 2

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

[0042] (1) Add potassium chloride 100g, water 218g and raffinate water phase (at the initial stage of process start-up, the raffinate water phase is water) into the reaction vessel, prepare a potassium chloride saturated solution with a temperature of 60°C, and add Concentration is 83g of nitric acid of 68wt%, under normal pressure, under agitation, react at 60 ℃ for 45min, the gained reaction liquid is naturally cooled to 30 ℃, filter, the gained filter cake is washed with 25g water and dried to obtain 1 # Potassium nitrate product 49g, productive rate is 54%;

[0043] (2) step (1) is filtered to obtain filtrate 341g, and in this filtrate, H + The content is 0.26wt%, Cl - The content is 13.54wt%, NO 3 - Content is 7.79wt%, in this filtrate, add extraction agent, the volume ratio of extraction agent and filtrate is 1:1, extract at 30 ℃, extraction retention time is 20m...

Embodiment 3

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

[0053] (1) Add potassium chloride 100g, water 208g, and raffinate water phase (in the initial stage of process start-up, the raffinate water phase is water) into the reaction vessel, prepare a potassium chloride saturated solution with a temperature of 70°C, and add Concentration is 130g of nitric acid of 65wt%, at normal pressure, 70 ℃ stirring reaction 30min, the gained reaction liquid is naturally cooled to 20 ℃, filter, the gained filter cake is washed with 15g water and dried to obtain 1 # Potassium nitrate product 72g, productive rate is 53%;

[0054] (2) step (1) is filtered to obtain filtrate 361g, and in this filtrate, H + The content is 0.37wt%, Cl - The content is 13.22wt%, NO 3 - Content is 11.21wt%, adds extractant in this filtrate, the volume ratio of extractant and filtrate is 3:1, extracts at 20 ℃, extraction residence time is 30min, returns the raffina...

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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, in particular to a method for preparing potassium nitrate by solvent extraction. Background technique [0002] Potassium nitrate is a chlorine-free high-grade nitrogen and potassium binary compound fertilizer. Its total nutrient content is as high as 60wt%. It is universally applicable and non-volatile. After application, it can be completely absorbed by plants and soil without being brought Chemical residues, which can effectively improve the quality and yield of plants, are called "true green fertilizers". There are many production methods of potassium nitrate, currently the main methods used in 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 etc. have reported a method for preparing agricultural po...

Claims

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Application Information

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Patent Type & Authority Applications(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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