CN113816400A - Preparation method of potassium nitrate - Google Patents
Preparation method of potassium nitrate Download PDFInfo
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- CN113816400A CN113816400A CN202010556887.8A CN202010556887A CN113816400A CN 113816400 A CN113816400 A CN 113816400A CN 202010556887 A CN202010556887 A CN 202010556887A CN 113816400 A CN113816400 A CN 113816400A
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- potassium nitrate
- ammonium
- nitrate
- potassium
- solid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D9/00—Nitrates of sodium, potassium or alkali metals in general
- C01D9/08—Preparation by double decomposition
- C01D9/10—Preparation by double decomposition with ammonium nitrate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/02—Froth-flotation processes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/16—Halides of ammonium
- C01C1/164—Ammonium chloride
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
A preparation method of potassium nitrate comprises the following steps: (1) putting potassium chloride and ammonium nitrate into a reaction tank, mixing the potassium chloride and the ammonium nitrate with saturated mother liquor of the ammonium chloride and the potassium nitrate at normal temperature and normal pressure, and carrying out solid-liquid phase conversion reaction to obtain a solid mixture of potassium nitrate-ammonium solid solution and ammonium chloride; (2) adding a flotation reagent into the mixture of the potassium ammonium nitrate solid solution and the solid ammonium chloride and the saturated ammonium chloride potassium nitrate mother liquor in a stirring tank, stirring, then performing flotation, wherein the supernatant is a coarse potassium nitrate solid solution, the underflow is ammonium chloride, and performing solid-liquid separation on the potassium ammonium nitrate solid solution and the ammonium chloride; (3) adding the obtained coarse potassium nitrate solid solution into an ammonium nitrate solution, stirring, filtering to obtain coarse ammonium nitrate, washing, filtering to obtain wet potassium nitrate, and drying to obtain the finished potassium nitrate. The method does not need high-temperature operation reaction, improves the yield of the potassium nitrate, reduces energy consumption and equipment failure rate, and realizes large-scale production by a conversion method.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to a preparation method of potassium nitrate.
Background
Potassium nitrate is an important inorganic chemical product, not only widely used in the fields of military affairs and fireworks, but also a high-quality chemical fertilizer with 60% of nutrient components, all of which are water-soluble nutrients, potassium ions and nitrate ions can be quickly absorbed by crops, and the potassium nitrate is a chemical nitrogen-potassium compound fertilizer which is completely composed of effective substances and has no residue after application. It is a high-quality fertilizer which is forbidden to chlorine crops such as tobacco, coffee, tomato, grape, orange, gardening, flowers, potato, avocado, tea and the like, and can obviously improve the yield and quality of economic crops.
In the large-scale industrial production of potassium nitrate, the yield is improved and the energy consumption is saved on the basis of the quality of potassium nitrate products, so that the method is a key way for reducing the production cost. In the production of preparing potassium nitrate by a conversion method, the yield is mainly related to the amount of evaporated water and high-temperature reaction operation production, and a certain yield can be achieved only when the amount of evaporated water and the temperature are in proper values, but the yield is limited due to high amount of evaporated water and high-temperature operation production, high equipment failure rate and high energy consumption. The problem of high production cost of the production method in the field can not be solved for a long time, that is, the technology of the traditional double decomposition conversion method for preparing potassium nitrate is developed to a bottleneck period for improving the yield. The potassium nitrate production is faced with the problems of potassium resource shortage, unreasonable process route, small production scale of the existing enterprises and the like, which causes high production cost, although the potential market of the potassium nitrate is large, the development of new technology and new process for producing the potassium nitrate is urgently needed to be solved because the potassium nitrate is slowly restricted by factors such as the production cost, immature large-scale production process technology and the like.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a method for preparing potassium nitrate by converting an ammonium nitrate solution and solid potassium chloride without high temperature operation reaction. The crude potassium nitrate solid solution and ammonium chloride are directly extracted by flotation. The method fully utilizes the ammonium nitrate solution to flush the coarse potassium nitrate solid solution, only needs saturated mother liquor formed by evaporating the ammonium nitrate solution and a small amount of washing water, greatly reduces the evaporation amount, improves the yield of potassium nitrate, reduces the energy consumption and the equipment failure rate, and realizes the large-scale production by the conversion method.
In order to achieve the purpose, the invention adopts the following technical scheme.
A preparation method of potassium nitrate specifically comprises the following steps.
Step 1, carrying out solid-liquid phase reaction at normal temperature and normal pressure: putting solid potassium chloride and ammonium nitrate solution into a reaction tank with stirring, mixing the solid potassium chloride and the ammonium nitrate solution with saturated mother liquor of the potassium nitrate chloride at normal temperature and normal pressure, controlling the solid-phase concentration to be 20-40%, then guiding the mixture into a ball mill, a colloid mill, an emulsifying machine or other wet milling equipment for milling, guiding the mixture into the stirring tank, and stirring and reacting for 3 hours, wherein the reaction product is a mixture of potassium nitrate solid solution and ammonium chloride.
And the saturated mother liquor of the potassium ammonium nitrate chloride is recycled.
Step 2, the flotation separation method of the mixture of the potassium nitrate solid solution and the ammonium chloride comprises the following steps: adding a flotation reagent into the mixture of the potassium nitrate solid solution and the ammonium chloride and the mixed slurry of the saturated mother liquor of the potassium nitrate and the ammonium chloride, stirring for 10 minutes, and then introducing the mixture into a flotation machine for flotation, wherein the supernatant (concentrate) is coarse potassium nitrate solid solution, the underflow (tailings) is ammonium chloride, the coarse potassium nitrate solid solution and the ammonium chloride are respectively subjected to solid-liquid separation in a vacuum filter or a centrifuge, the saturated mother liquor of the potassium nitrate is recycled, and only the residual saturated mother liquor formed by evaporating the ammonium nitrate solution is needed.
The flotation reagent comprises a potassium nitrate collecting agent, a foaming agent and a regulator, wherein the collecting agent is sodium dodecyl sulfate, the foaming agent is sodium dodecyl diphenyl ether disulfonate, and the regulator is sodium carbonate.
And 3, adding the coarse potassium nitrate solid solution obtained by separation in the step 2 into an ammonium nitrate solution, stirring, filtering to obtain low-chlorine wet ammonium nitrate, adding the obtained coarse ammonium nitrate into secondary condensed water obtained by evaporation (saturated mother liquor formed by the ammonium nitrate solution), stirring and washing, filtering to obtain wet potassium nitrate, drying to obtain finished potassium nitrate, and adding the washing mother liquor into the mixed ammonium nitrate solution as a raw material to perform secondary production feeding.
Cl in solid potassium chloride in the step 1-And NH in ammonium nitrate solution4 +In a molar ratio of 1.97: 1.
and the adding amount of the flotation reagent in the step 2 is two ten-thousandth of the mass of the mixed slurry.
The nitrogen content of the ammonium chloride in the step 2 is 18-22%.
And 3, adding the coarse potassium nitrate solid solution (concentrate) and the ammonium nitrate solution (feeding weight) obtained by separation in the step 2 into a stirring tank for stirring for 1min, then carrying out solid-liquid separation on a material paddle in a vacuum filter to obtain low-chlorine ammonium potassium nitrate, adding the low-chlorine ammonium potassium nitrate obtained by separation and water into the stirring tank, stirring for 1min, then carrying out solid-liquid separation on the material paddle in the vacuum filter to obtain wet potassium nitrate, drying the wet potassium nitrate to obtain an agricultural potassium nitrate product, and adding washing mother liquor into the mixed ammonium nitrate solution as a raw material for feeding the next secondary production.
In the step 3, the potassium nitrate contains more than or equal to 46 percent of potassium oxide, contains more than or equal to 13.5 percent of nitrogen, contains less than or equal to 0.2 percent of chloride ions and contains less than or equal to 0.5 percent of water, thereby achieving the standard of agricultural potassium nitrate.
The low-chlorine ammonium potassium nitrate and the water separated in the step 3 are mixed according to a mass ratio of 4: 1 is added into a stirring tank.
The flotation machine is a stirring flotation machine.
Compared with the prior art, the invention has the beneficial effects.
According to the preparation method of potassium nitrate, potassium nitrate is prepared by converting the ammonium nitrate solution and the solid potassium chloride, so that the problems that the traditional ammonium nitrate conversion method runs at high temperature in the process of producing potassium nitrate and a large amount of saturated ammonium chloride potassium nitrate mother liquor is evaporated are solved. The production operation process of the invention is carried out at normal temperature and normal pressure. The mother liquor is recycled, and only the residual saturated mother liquor formed by evaporating the ammonium nitrate solution is needed, so that the yield of the potassium nitrate is improved, and the large-scale production of the potassium nitrate by a potassium nitrate conversion method is realized. In addition, the preparation method uses normal-temperature and normal-pressure solid-liquid phase reaction to prepare the potassium nitrate solid solution and the ammonium chloride in one step, the potassium nitrate solid solution and the ammonium chloride solid are separated by a flotation method, water and heat are not added in the reaction process, the mother solution is recycled and is safely operated at normal temperature and normal pressure, the prepared potassium nitrate only needs the saturated mother solution formed by evaporating the ammonium nitrate solution, the energy consumption is reduced, the operation is easy, and the preparation method is safe and environment-friendly.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
The embodiment provides a preparation method of potassium nitrate, which comprises the following steps.
Step 1, solid-liquid phase normal temperature and normal pressure reaction: adding 1000ml of ammonium chloride potassium nitrate saturated mother liquor into a 5000ml organic glass reaction tank, starting a stirrer (XJT type variable frequency speed regulation, Jiangxi silver acute mining and metallurgy equipment Limited company), and adjusting the rotating speed of the stirrer to be more than 4000 revolutions per minute; weighing 585g of solid potassium chloride (containing 62% of potassium oxide, produced by Russia) and 1000g of ammonium nitrate solution (containing 63% of ammonium nitrate, a byproduct of the Chinese synthetic oil inner Mongolia company, Ltd.), putting the ammonium nitrate solution and the potassium chloride into an organic glass stirring tank, stirring and mixing at normal temperature and normal pressure, then guiding into a colloid mill (JM-L50, Guangzhou Hengdong mechanical equipment science and technology Co., Ltd.), grinding for 10 minutes, then guiding into the stirring tank, adding 2000ml of saturated mother liquor of potassium ammonium nitrate chloride (controlling the solid-phase concentration to be 20-40%), starting stirring and reacting for 3 hours, wherein the reaction products are a mixture of normal-temperature potassium nitrate solid solution and ammonium chloride, and normal-temperature saturated mother liquor of potassium nitrate.
The reaction chemical equation is: KCL + NH4NO3= KNO3+ NH4 CL.
The saturated mother liquor of the ammonium nitrate potassium chloride is recycled, because the saturated mother liquor only plays a role of a medium in the reaction process, the components of the saturated mother liquor are not changed, and the residual saturated mother liquor formed by the ammonium nitrate solution is evaporated.
The traditional method comprises the steps of carrying out high-temperature reaction on potassium chloride, ammonium nitrate and saturated ammonium chloride and potassium nitrate mother liquor to generate a potassium nitrate solid solution and ammonium chloride solid mixture and also high-temperature circulating saturated ammonium chloride and potassium nitrate mother liquor.
Step 2, the flotation separation method of the mixture of the potassium nitrate solid solution and the ammonium chloride comprises the following steps: adding 10 ml of a flotation agent into a mixture containing the potassium nitrate solid solution and the ammonium chloride and the saturated mother solution of the potassium nitrate (the solid-to-liquid ratio is controlled to be 20-40%) in an organic glass reaction tank, stirring for 10min, and then introducing the mixture into a flotation machine (0.51, Jiangxi mining and metallurgy test equipment factory) in batches for flotation, wherein the roughing condition is as follows: stirring for flotation for 3-4min, and filtering with vacuum pump (SHZ-D111, manufactured by Zhang province instruments Co., Ltd.) to obtain 661g of foam product containing Cl-16.13%; the underflow (middlings) contained Cl-41.61% in 107 g. Then, 661g of roughed foam product and 2500ml of saturated mother liquor are subjected to paddle regulation in a stirring tank, and are led into a flotation machine in batches for fine selection, and the fine selection condition is as follows: the conditions are the same as those of rough concentration, and after filtration, 537g of concentrated foam product containing Cl-12.93% and 108g of underflow (middlings) containing Cl-32.88% are obtained. 537g of foam product of first concentration and 1800ml of saturated mother liquor are adjusted in a stirring tank and are led into a flotation machine in batches for second concentration under the same conditions of rough concentration, and 448g of foam product is obtained after filtration, wherein Cl is 10.27%, and bottom flow (middling) is 70g, wherein Cl is 27.98%. And (2) adjusting the pulp of the foam product 448g of the second concentration and 1500ml of saturated mother liquor in a stirring tank, introducing the foam product 448g of the second concentration and the saturated mother liquor into a flotation machine in batches for third concentration, performing rough concentration under the same conditions, filtering to obtain 373g of foam product (concentrate) with Cl-8.26% and underflow (middling 60g with Cl-21.13%. the rough concentration underflow, the first concentration underflow, the second concentration underflow and the third concentration underflow are mixed 345g and are adjusted with 1500ml of saturated mother liquor in the stirring tank, adding 5 ml of a flotation agent, stirring for 10min, and then introducing the mixture into the flotation machine in batches for scavenging, wherein the conditions are the same as that of rough concentration, scavenging time is 3-4min, and filtering to obtain 214g of scavenging foam (middling) with Cl-22.36%, wherein the scavenging foam (middling) is used for next rough concentration, and underflow (tailing) 122g with Cl-51.04%, ammonium ions are 25.66%, potassium oxide is 7.43%, and water is 6.81%.
The three-flotage (concentrate) is coarse potassium nitrate solid solution, the bottom flow (tailing) is ammonium chloride, the coarse potassium nitrate solid solution and the ammonium chloride are respectively subjected to solid-liquid separation in a vacuum filter or a centrifuge, saturated mother liquor of the ammonium chloride and the potassium nitrate is recycled, and the residual mother liquor formed by the ammonium nitrate solution is evaporated.
The flotation reagent comprises a potassium nitrate collecting agent, a foaming agent and a regulator, wherein the collecting agent is sodium dodecyl sulfate, the foaming agent is sodium dodecyl diphenyl ether disulfonate, and the regulator is sodium carbonate; the preparation process of the flotation reagent comprises the following steps: heating 100ml water to 80 deg.C, weighing 5g sodium dodecyl sulfate, 0.5g sodium dodecyl diphenyl ether disulfonate, 0.5g sodium carbonate, adding into the above hot water, stirring and dissolving to obtain the final product.
The traditional potassium nitrate separation method is to wash by a large amount of secondary condensed water evaporated to obtain a coarse potassium nitrate solid solution.
Step 3, leaching 373g of the crude potassium nitrate solid solution (concentrate) obtained by separation in the step 2 with an ammonium nitrate solution (1000 g, 63%) to obtain 183g of low-chlorine ammonium potassium nitrate, wherein Cl is 0.27%, adding 183g of low-chlorine ammonium potassium nitrate obtained by separation and 100ml of water into a stirring tank to stir for 5 min, then performing solid-liquid separation on a material paddle in a vacuum filter to obtain 105g of wet potassium nitrate, and drying 105g of wet potassium nitrate to obtain 101g of agricultural potassium nitrate product, wherein Cl is 0.087%, K is 0.087%, and K is 0% of potassium nitrate2O-46.3 percent and water content-3.05 percent. And adding the washing mother liquor into the mixed ammonium nitrate solution as a raw material for secondary production and feeding.
The nitrogen content of the ammonium chloride in the step 2 is 18-22%.
In the step 3, the potassium nitrate contains more than or equal to 46 percent of potassium oxide, contains more than or equal to 13.5 percent of nitrogen, contains less than or equal to 0.2 percent of chloride ions and contains less than or equal to 0.5 percent of water, thereby achieving the standard of agricultural potassium nitrate.
Claims (10)
1. The preparation method of potassium nitrate is characterized by comprising the following steps:
step 1, carrying out solid-liquid phase reaction at normal temperature and normal pressure: putting solid potassium chloride and ammonium nitrate solution into a reaction tank with stirring, mixing the solid potassium chloride and the ammonium nitrate solution with saturated mother liquor of the potassium nitrate chloride at normal temperature and normal pressure, controlling the solid-phase concentration to be 20-40%, then guiding the mixture into a ball mill, a colloid mill, an emulsifying machine or other wet milling equipment for milling, guiding the mixture into the stirring tank for stirring and reacting for 3 hours, wherein the reaction product is a mixture of potassium nitrate solid solution and ammonium chloride;
step 2, the flotation separation method of the mixture of the potassium nitrate solid solution and the ammonium chloride comprises the following steps: adding a flotation reagent into the mixture of the potassium nitrate solid solution and the ammonium chloride and the mixed slurry of the saturated mother liquor of the potassium nitrate and the ammonium chloride and the potassium nitrate in a stirring tank, stirring for 10 minutes, then introducing the mixture into a flotation machine for flotation, wherein the upper floating object is a coarse potassium nitrate solid solution, the bottom flow is the ammonium chloride, the coarse potassium nitrate solid solution and the ammonium chloride are respectively subjected to solid-liquid separation in a vacuum filter or a centrifuge, the saturated mother liquor of the potassium nitrate is recycled, and only the residual saturated mother liquor formed by evaporating the ammonium nitrate solution is needed;
and 3, adding the coarse potassium nitrate solid solution obtained by separation in the step 2 into an ammonium nitrate solution for stirring, filtering to obtain low-chlorine wet potassium ammonium nitrate, adding the obtained coarse potassium ammonium nitrate into secondary condensed water obtained by evaporation for stirring and washing, filtering to obtain wet potassium nitrate, drying to obtain finished potassium nitrate, and adding washing mother liquor into the mixed ammonium nitrate solution as a raw material for feeding next secondary production.
2. The method for preparing potassium nitrate according to claim 1, wherein the solid potassium chloride in the step 1 contains Cl-And NH in ammonium nitrate solution4 +In a molar ratio of 1.97: 1.
3. the method for preparing potassium nitrate according to claim 1, wherein the reaction of potassium chloride and ammonium sulfate in the step 1 is a solid-liquid phase reaction, and a saturated mother solution of potassium ammonium chloride and potassium nitrate is recycled.
4. The method for preparing potassium nitrate according to claim 1, wherein the flotation agent is added in an amount of two ten-thousandths of the mass of the mixed slurry in the step 2.
5. The method for preparing potassium nitrate according to claim 1, wherein the flotation reagent in the step 2 comprises a potassium nitrate collector, a foaming agent and a regulator, wherein the collector is sodium dodecyl sulfate, the foaming agent is sodium dodecyl diphenyl ether disulfonate, and the regulator is sodium carbonate.
6. The method for preparing potassium nitrate according to claim 1, wherein the nitrogen content of ammonium chloride in the step 2 is 18-22%.
7. The method for preparing potassium nitrate according to claim 1, wherein the specific operation of the step 3 is to add the coarse potassium nitrate solid solution and the ammonium nitrate solution obtained by separation in the step 2 into a stirring tank to stir for 1min, then perform solid-liquid separation on the slurry in a vacuum filter to obtain low-chlorine ammonium potassium nitrate, add the low-chlorine ammonium potassium nitrate obtained by separation and water into the stirring tank to stir for 1min, then perform solid-liquid separation on the slurry in the vacuum filter to obtain wet potassium nitrate, dry the wet potassium nitrate to obtain an agricultural potassium nitrate product, and add the washing mother liquor into the mixed ammonium nitrate solution as a raw material to perform secondary production and feeding.
8. The method for preparing potassium nitrate according to claim 1, wherein in the step 3, the potassium nitrate contains more than or equal to 46 percent of potassium oxide, contains more than or equal to 13.5 percent of nitrogen, contains less than or equal to 0.2 percent of chloride ions and contains less than or equal to 0.5 percent of water, and reaches the standard of agricultural potassium nitrate.
9. The method for preparing potassium nitrate according to claim 1, wherein the low-chlorine ammonium potassium nitrate separated in the step 3 and water are mixed in a mass ratio of 4: 1 is added into a stirring tank.
10. The method for preparing potassium nitrate according to claim 1, wherein the flotation machine is an agitation type flotation machine.
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| CN202010556887.8A CN113816400A (en) | 2020-06-18 | 2020-06-18 | Preparation method of potassium nitrate |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB411587A (en) * | 1933-01-28 | 1934-06-14 | Ig Farbenindustrie Ag | Improvements in the separation of mixtures of alkali metal nitrates with ammonium chloride |
| CN101628723A (en) * | 2009-08-18 | 2010-01-20 | 湖南丹化农资有限公司 | Method for preparing potassium nitrate and ammonium chloride employing double decomposition reaction |
| CN105060317A (en) * | 2015-07-30 | 2015-11-18 | 湖南丹化农资有限公司 | Potassium chloride and ammonium nitrate double decomposition and circulation method for producing high quality potassium nitrate |
| CN106629781A (en) * | 2015-10-28 | 2017-05-10 | 绥芬河市石英经贸有限公司 | Potassium sulfate preparation method |
-
2020
- 2020-06-18 CN CN202010556887.8A patent/CN113816400A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB411587A (en) * | 1933-01-28 | 1934-06-14 | Ig Farbenindustrie Ag | Improvements in the separation of mixtures of alkali metal nitrates with ammonium chloride |
| CN101628723A (en) * | 2009-08-18 | 2010-01-20 | 湖南丹化农资有限公司 | Method for preparing potassium nitrate and ammonium chloride employing double decomposition reaction |
| CN105060317A (en) * | 2015-07-30 | 2015-11-18 | 湖南丹化农资有限公司 | Potassium chloride and ammonium nitrate double decomposition and circulation method for producing high quality potassium nitrate |
| CN106629781A (en) * | 2015-10-28 | 2017-05-10 | 绥芬河市石英经贸有限公司 | Potassium sulfate preparation method |
Non-Patent Citations (2)
| Title |
|---|
| 吴朝香: "硝酸钾反浮选分离方法研究", 《化工矿物与加工》 * |
| 陈坤等: "氯化钾-硝酸铵复分解法制备硝酸钾工艺进展", 《化肥工业》 * |
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