CN112939032A - Method for preparing potassium nitrate by nitric acid method - Google Patents
Method for preparing potassium nitrate by nitric acid method Download PDFInfo
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- CN112939032A CN112939032A CN202110316151.8A CN202110316151A CN112939032A CN 112939032 A CN112939032 A CN 112939032A CN 202110316151 A CN202110316151 A CN 202110316151A CN 112939032 A CN112939032 A CN 112939032A
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- nitric acid
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- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 title claims abstract description 332
- 239000004323 potassium nitrate Substances 0.000 title claims abstract description 166
- 235000010333 potassium nitrate Nutrition 0.000 title claims abstract description 166
- 238000000034 method Methods 0.000 title claims abstract description 90
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 229910017604 nitric acid Inorganic materials 0.000 title claims abstract description 60
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims abstract description 212
- 238000006243 chemical reaction Methods 0.000 claims abstract description 110
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract description 106
- 238000003825 pressing Methods 0.000 claims abstract description 67
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 62
- 238000002425 crystallisation Methods 0.000 claims abstract description 48
- 239000000047 product Substances 0.000 claims abstract description 43
- 230000008025 crystallization Effects 0.000 claims abstract description 36
- 238000005406 washing Methods 0.000 claims abstract description 34
- 239000001103 potassium chloride Substances 0.000 claims abstract description 31
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 31
- 238000001704 evaporation Methods 0.000 claims abstract description 30
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 28
- 230000008020 evaporation Effects 0.000 claims abstract description 27
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 27
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000007710 freezing Methods 0.000 claims abstract description 23
- 230000008014 freezing Effects 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 238000000926 separation method Methods 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 238000005119 centrifugation Methods 0.000 claims abstract description 8
- 239000012452 mother liquor Substances 0.000 claims description 59
- 239000013078 crystal Substances 0.000 claims description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 230000000694 effects Effects 0.000 claims description 22
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 22
- 238000004064 recycling Methods 0.000 claims description 19
- 238000003860 storage Methods 0.000 claims description 19
- 239000002002 slurry Substances 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 14
- 239000012295 chemical reaction liquid Substances 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 208000005156 Dehydration Diseases 0.000 claims description 9
- 230000018044 dehydration Effects 0.000 claims description 9
- 238000006297 dehydration reaction Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 4
- 230000002378 acidificating effect Effects 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims 1
- 239000006227 byproduct Substances 0.000 abstract description 10
- 239000000243 solution Substances 0.000 description 35
- 238000004519 manufacturing process Methods 0.000 description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 11
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical group OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 5
- 238000000354 decomposition reaction Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 239000012047 saturated solution Substances 0.000 description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- 238000005342 ion exchange Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- 235000002639 sodium chloride Nutrition 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 235000019270 ammonium chloride Nutrition 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- 159000000003 magnesium salts Chemical class 0.000 description 2
- 239000010413 mother solution Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 159000000000 sodium salts Chemical class 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- DHKHZGZAXCWQTA-UHFFFAOYSA-N [N].[K] Chemical compound [N].[K] DHKHZGZAXCWQTA-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000005008 domestic process Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011403 purification operation Methods 0.000 description 1
- 238000005185 salting out Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- 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
- C01D9/04—Preparation with liquid nitric acid
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/26—Magnesium halides
- C01F5/30—Chlorides
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Geology (AREA)
- Agronomy & Crop Science (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention aims to provide a method for preparing potassium nitrate by a nitric acid method, which takes potassium chloride, dilute nitric acid and magnesium oxide as raw materials, produces a main product of potassium nitrate by the processes of proportioning, filter pressing, crystallization, washing, centrifugation and drying, comprises the steps of proportioning, heating reaction, plate-and-frame filter pressing, freezing crystallization, washing, centrifugal separation of magnesium chloride solution evaporation and the like, and simultaneously produces magnesium chloride as a byproduct.
Description
The technical field is as follows:
the invention relates to the field of production of inorganic chemical products, mainly relates to an inorganic salt, and particularly relates to a method for preparing potassium nitrate by a nitric acid method.
Background art:
potassium nitrate and magnesium chloride are one of the important chemical raw materials, and potassium nitrate is widely applied to various fields of national defense and military industry such as black powder, industry, agriculture, food additives, medicines, feed additives, optical glass, electronic industry and the like. The fertilizer grade potassium nitrate used in agriculture is a high-quality potassium-nitrogen binary compound fertilizer. At present, domestic methods for producing potassium nitrate mainly comprise a double decomposition method and an ion exchange method.
The existing double decomposition method usually adopts double decomposition of ammonium nitrate and potassium chloride to prepare potassium nitrate and produce ammonium chloride as a byproduct, but the method has higher requirements on production equipment, mainly because the method has serious corrosion on the equipment in the production process, the operation difficulty in the operation process of the equipment is higher, and the prepared potassium nitrate product has lower purity, high purification operation cost and high energy consumption. The method adopts an ion exchange method to prepare a product by carrying out ion exchange reaction on ammonium nitrate and potassium chloride and produces ammonium chloride as a byproduct, wherein one of the used raw materials is ammonium nitrate, the use and purchase range of the ammonium nitrate is limited, namely the raw material source is controlled by the state, so the price is relatively high, the production cost is increased invisibly, and secondly, the equipment for ion exchange is huge, the corresponding equipment investment is larger, the yield of a primary finished product of potassium nitrate is lower, the subsequent treatment cost is high, and the mixed acid formed by the nitric acid and the hydrochloric acid generated in the production process has great influence on the equipment, so the equipment cannot be well recovered and the environment is easily polluted.
For example, the method for producing potassium nitrate by using dilute nitric acid disclosed in Chinese patent publication No. CN1064063A, comprises the steps of carrying out a chemical reaction between 35-40% dilute nitric acid and potassium chloride at a high temperature of 70-105 ℃ and a negative pressure of 300-400mm Hg to generate potassium nitrate, cooling, crystallizing, drying and the like. Also, chinese patent publication No. CN101070167A, a potassium nitrate preparation process, includes reacting potassium chloride with dilute nitric acid to produce potassium chloride, potassium nitrate, and a mixture of dilute nitric acid and hydrochloric acid, then distilling to remove a large amount of hydrochloric acid and nitric acid, heating and concentrating to make the mixed solution become a saturated solution, adding sodium carbonate to adjust the solution to neutrality, simultaneously adding a small amount of hydrochloric acid to react to produce sodium chloride, and finally separating potassium nitrate by using the difference of the solubilities of potassium nitrate, sodium chloride and potassium chloride at the same temperature.
As another example, chinese patent publication No. CN107651697A, discloses a method for preparing potassium nitrate, which specifically comprises adding solid potassium chloride into 55-68% by mass of nitric acid, stirring for 10-20 minutes, adding an extractant at 4-10 ℃, standing for 25-40 minutes, and separating an oil phase from a water phase; the obtained aqueous phase was centrifuged to obtain a solid as coarse potassium nitrate crystals, which were washed and dried to obtain potassium nitrate.
Chinese publication No. CN103771461A, a method for preparing potassium nitrate by double decomposition, which comprises using ammonium nitrate and potassium chloride as raw materials, recycling mother liquor, because the potassium chloride as the raw material brings impurities such as sodium chloride, magnesium chloride and the like, and the accumulation and treatment problems of the impurities in the mother liquor in long-term circulation are not solved, the invention is characterized in that a shunting impurity removal production line is arranged close to a production device, a sodium removal unit and a magnesium removal unit are arranged on the production line, the two units can run simultaneously or independently, 1-30% of the total circulation amount of the mother liquor is introduced into the production line for impurity removal treatment, the main components of the impurities are water-soluble sodium salt and magnesium salt, removing part of sodium salt by using magnesium chloride as a salting-out agent, removing part of magnesium salt by using ammonium bicarbonate as a precipitating agent, wherein the temperature of the solution is 10-90 ℃, and returning the mother solution after impurity removal treatment to a mother solution circulating system.
It can be seen from the above-mentioned technical solutions that the existing potassium nitrate preparation method still uses the double decomposition method and/or ion exchange resin method, some of them also need to add extractant or complexing agent, etc. in the course of preparation, and in the course of chemical reaction, every addition of a substance can correspondingly increase the cost of its subsequent treatment, at the same time, it still has the problems of low yield of primary product, high production cost and large equipment investment, and the produced dilute nitric acid and dilute hydrochloric acid can cause a certain pollution to environment. The separation of nitric acid and hydrochloric acid is difficult.
Therefore, how to provide a method for preparing potassium nitrate, the prepared potassium nitrate has high purity, low preparation cost, convenient separation operation, small equipment investment, less influence on the environment, simple preparation process and realization of the recycling of filtrate resources.
The invention content is as follows:
the invention aims to provide a method for preparing potassium nitrate by a nitric acid method, which takes potassium chloride, dilute nitric acid and magnesium oxide as raw materials, produces a main product of potassium nitrate by the processes of proportioning, filter pressing, crystallization, washing, centrifugation and drying, comprises the steps of proportioning, heating reaction, plate-and-frame filter pressing, freezing crystallization, washing, centrifugal separation of magnesium chloride solution evaporation and the like, and simultaneously produces magnesium chloride as a byproduct.
The invention discloses a method for preparing potassium nitrate by a nitric acid method, which takes potassium chloride, dilute nitric acid and magnesium oxide as raw materials, produces a main product of potassium nitrate by the working procedures of batching, filter pressing, crystallization, washing, centrifugation and drying, and comprises the following steps:
2) preparing materials: firstly, nitric acid is metered and pumped into an acid metering tank, then magnesium oxide and potassium chloride are conveyed to a feeding port of a reaction device tank through an automatic feeder,
2) heating and reacting: adding process water into the reaction device tank in the step 1), adding magnesium oxide in batches, slowly adding nitric acid for reaction, controlling the pH of the reaction solution to be carried out under an acidic condition, keeping the reaction temperature at 100 ℃ and 140 ℃, continuously stirring for reaction, adding potassium chloride for continuous stirring reaction after magnesium nitrate is generated, and obtaining a mixture reaction liquid of potassium nitrate and magnesium chloride;
3) plate and frame filter pressing: transferring the reaction liquid obtained in the step 2) into a heat preservation device tank, carrying out multiple filter pressing on the reaction liquid by a plate-and-frame filter press to obtain filter pressing mother liquid and filter pressing filter residues,
4) freezing and crystallizing: putting the filter pressing mother liquor obtained in the step 3) into a mother liquor storage tank, transferring the mother liquor storage tank into a freezing tank for cooling treatment, controlling the mother liquor storage tank to cool to-8 to-15 ℃, transferring the mother liquor storage tank into a crystallizing tank, and slowly crystallizing to obtain potassium nitrate crystals and magnesium chloride solution;
5) washing: putting the potassium nitrate crystals obtained in the step 4) into a washing tank, washing to obtain potassium nitrate crystal slurry, and returning washing mother liquor to the reaction device tank for recycling;
6) centrifuging: placing the potassium nitrate crystal slurry obtained in the step 4) into a centrifuge for centrifugal separation to obtain centrifugal potassium nitrate crystal solid, and returning centrifugal mother liquor to the reaction device tank for recycling;
7) drying: drying the solid potassium nitrate crystals by a dryer to obtain potassium nitrate with the water content less than or equal to 0.1 percent, namely a potassium nitrate product;
8) evaporation of magnesium chloride solution: transferring the magnesium chloride solution obtained in the step 4) into a magnesium chloride storage tank, conveying the magnesium chloride solution into a magnesium chloride evaporation crystallizer device through a centrifugal pump to perform downstream evaporation operation, and continuously feeding, continuously evaporating and continuously discharging through a separation chamber and a crystallizer to obtain a magnesium chloride coarse material;
9) magnesium chloride dehydration: and (3) carrying out centrifugal dehydration treatment on the magnesium chloride coarse material obtained in the step 8) to obtain a magnesium chloride product, and refluxing the separated mother liquor to a reaction device tank for recycling.
The method for preparing the potassium nitrate by the nitric acid method comprises the step 1) of controlling the mass concentration of a nitric acid solution to be 45-52 Wt%.
According to the method for preparing potassium nitrate by the nitric acid method, in the heating reaction in the step 2), magnesium oxide is uniformly added for 2-4 times after process water is added, the pH is controlled to be 3-4, the reaction time is 1.5-2.5 hours, and the heating reaction is controlled to be steam heating.
The method for preparing the potassium nitrate by the nitric acid method comprises the step 3) of plate-frame filter pressing, wherein the filter pressing is carried out when the temperature of a reaction solution is controlled to be 65-85 ℃, and the filter pressing frequency is controlled to be 1-3 times.
Preferably, in the step 4), the freezing crystallization is carried out by controlling the mass ratio of potassium nitrate to magnesium chloride of the filter pressing mother liquor entering the freezing tank to be 2-2.5: 1, controlling the cooling treatment temperature to be-9 to-12 ℃.
Further, the evaporation in the step 8) adopts triple effect evaporation, single effect natural circulation, double effect and triple effect forced circulation, and a triple effect separation chamber adopts a DTB crystallizer.
Preferably, step 8) controls the moisture content of the magnesium chloride product to be less than or equal to 4 percent.
Preferably, the heating reaction in step 2) is carried out under normal pressure or under a micro-pressure condition.
The method for preparing potassium nitrate by a nitric acid method comprises the step 4) of freezing crystallization, wherein a potassium nitrate crystallization agent is added into a filter-pressing mother liquor to crystallize and separate out potassium nitrate crystals, and the potassium nitrate crystallization agent is a potassium nitrate saturated/or supersaturated solution or high-purity potassium nitrate crystals.
The invention discloses a method for preparing potassium nitrate by a nitric acid method, which is used for preparing potassium nitrate products and by-producing magnesium chloride and has the following technical characteristics,
firstly, the reaction can be carried out under the normal pressure condition, the reaction condition is mild, and the cost for producing and preparing the potassium nitrate is low;
secondly, the invention has mild reaction conditions, small equipment investment, simple working operation, greatly reduced labor intensity of workers, no need of large-scale workplaces and facilities,
thirdly, in the process of freezing crystallization, a potassium nitrate crystallization agent is added, and the potassium nitrate crystallization agent can be a high-purity potassium nitrate crystal or a saturated or supersaturated solution of potassium nitrate, so that potassium nitrate in a filter-pressing mother liquor formed by a mixture reaction liquid of potassium nitrate and magnesium chloride in a freezing tank is easy to crystallize and separate out, the purification content of potassium nitrate is further ensured, the purity of the prepared potassium nitrate is higher under the same other process conditions, the maximum content of potassium nitrate can reach 99.99%, and the general content can also reach 99.9% through actual production detection;
fourthly, the invention adopts a circulating device and a plate-frame type filter pressing device, so that the filtering is more thorough, and the corrosivity to equipment is smaller, thereby prolonging the service life of the equipment such as a reaction device, and the like, and recycling the recovered water or wastewater generated by each process reaction, achieving the purpose of recycling, saving resources and realizing the production function of environmental protection.
The specific implementation mode is as follows:
the present invention is further illustrated by the following specific examples; the mass or mass ratio of each raw material used in the present invention may be obtained commercially, unless otherwise specified, and the meaning of the reaction tank or the reaction apparatus tank in the following embodiments is the same.
The specific embodiment of the invention is prepared as follows: the main reaction equation of the invention is as follows:
2KCl+2HNO3+5H2O+MgO＝＝＝2KNO3+MgCl2·6H2O。
the invention relates to a method for preparing potassium nitrate by a nitric acid method, which takes potassium chloride, dilute nitric acid and magnesium oxide as raw materials, produces a main product of potassium nitrate by the working procedures of batching, filter pressing, crystallization, washing, centrifugation and drying, and comprises the following steps:
3) preparing materials: firstly, nitric acid with the mass concentration of 45-52Wt% is metered and pumped into an acid metering tank, then magnesium oxide and potassium chloride are conveyed to a feeding port of a reaction device tank through an automatic feeding machine,
2) heating and reacting: adding process water or recycled solution and the like recovered in the original reaction process into a reaction device tank in the step 1), then uniformly feeding magnesium oxide for each time by 2-4 times, slowly adding nitric acid for reaction, controlling the pH of the reaction solution under an acidic condition, generally controlling the pH to be 3-4, the reaction temperature to be 100-; the reaction in the step is carried out under normal pressure or under the condition of micro-pressure, wherein the micro-pressure condition means that the tank body of the reaction device is carried out under the sealing condition under the condition of the reaction temperature, and the reaction device is not subjected to additional pressurization reaction;
3) plate and frame filter pressing: transferring the reaction solution obtained in the step 2), namely the mixture reaction solution of potassium nitrate and magnesium chloride, into a heat preservation device tank, performing filter pressing on the reaction solution at the temperature of 65-85 ℃ by using a plate and frame filter press, controlling the filter pressing frequency to be 1-3 times, obtaining filter pressing mother liquor and filter pressing filter residues,
4) freezing and crystallizing: placing the filter pressing mother liquor obtained in the step 3) in a mother liquor storage tank, then transferring the mother liquor storage tank into a freezing tank for cooling treatment, and controlling the mass ratio of potassium nitrate to magnesium chloride of the filter pressing mother liquor entering the freezing tank to be 2-2.5: controlling and cooling to-8 to-15 ℃, transferring to a crystallization tank, and preferably adding a potassium nitrate crystallization agent into the pressure filtration mother liquor of potassium nitrate and magnesium chloride in the crystallization tank at the same time, wherein the potassium nitrate crystallization agent can be a high-purity potassium nitrate crystal such as a chemically pure potassium nitrate crystal or a saturated or supersaturated solution of potassium nitrate so as to improve the crystallization purity of potassium nitrate, and slowly crystallizing to obtain a potassium nitrate crystal and a magnesium chloride solution;
5) washing: putting the potassium nitrate crystals obtained in the step 4) into a washing tank, washing to obtain potassium nitrate crystal slurry, and returning washing mother liquor to the reaction device tank for recycling;
6) centrifuging: placing the potassium nitrate crystal slurry obtained in the step 4) into a centrifuge for centrifugal separation to obtain centrifugal potassium nitrate crystal solid, and returning centrifugal mother liquor to the reaction device tank for recycling;
7) drying: drying the solid potassium nitrate crystals by a dryer to obtain potassium nitrate with the water content less than or equal to 0.1 percent, namely a potassium nitrate product;
8) evaporation of magnesium chloride solution: transferring the magnesium chloride solution obtained in the step 4) into a magnesium chloride storage tank, conveying the magnesium chloride solution into a magnesium chloride evaporative crystallizer device through a centrifugal pump to perform downstream evaporation operation, continuously feeding, continuously evaporating and continuously discharging through a separation chamber and a crystallizer, wherein generally, triple-effect evaporation, single-effect natural circulation, double-effect and triple-effect forced circulation are adopted, and a DTB crystallizer is adopted in a triple-effect separation chamber to obtain a magnesium chloride coarse material;
9) magnesium chloride dehydration: and (3) carrying out centrifugal dehydration treatment on the magnesium chloride coarse material obtained in the step 8) to obtain a magnesium chloride product, and refluxing the separated mother liquor to a reaction device tank for recycling. The content of potassium nitrate prepared by the method can reach 99.98-99.99 percent at most.
In the following examples, the same as the above-described embodiments are not described except for the following description of examples.
Example 1:
the invention discloses a method for preparing potassium nitrate by a nitric acid method, which comprises the following steps of,
the method takes potassium chloride, dilute nitric acid and magnesium oxide as raw materials and produces a main product of potassium nitrate and a byproduct of magnesium chloride through the working procedures of proportioning, filter pressing, crystallization, washing, centrifugation, drying and the like, and the specific reaction process is as follows:
1) preparing materials: pumping nitric acid with the mass concentration of 50% into a dilute nitric acid metering tank, and conveying magnesium oxide and potassium chloride to a reaction tank or the same feeding port below a reaction device tank through an automatic feeding machine;
2) reaction: adding process water into a reaction tank, adding magnesium oxide for 3 times, adding excessive magnesium oxide in the reaction, slowly adding nitric acid, controlling the pH to 3.5, performing the reaction at normal pressure, controlling the reaction temperature to 120 ℃, heating by using steam, controlling stirring reaction for 2 hours, adding potassium chloride for stirring reaction when the magnesium nitrate is fully reacted to generate magnesium nitrate, and controlling the magnesium nitrate and the potassium chloride to be fully reacted to generate a mixture reaction liquid of potassium nitrate and magnesium chloride, or called a reaction liquid;
3) plate and frame filter pressing: after the reaction is finished, transferring the reaction solution in the previous step into a heat-preserving tank, controlling the reaction solution to carry out first filter pressing by a plate-and-frame filter press at 70-80 ℃ to obtain filter pressing mother liquor, namely mixed liquor of potassium nitrate and magnesium chloride, and simultaneously obtain filter pressing filter residues, carrying out second filter pressing on the filter pressing mother liquor, wherein steam is generated in the filter pressing process;
4) freezing and crystallizing: in the mixed liquid of potassium nitrate and magnesium chloride of the filter pressing mother liquid, the mass ratio of potassium nitrate to magnesium chloride is 2.1: after the reaction is finished, mainly utilizing the fact that the solubility of potassium nitrate changes greatly along with the temperature, but the solubility of magnesium chloride does not change greatly along with the temperature, then transferring the filter pressing mother liquor into a freezing tank through a mother liquor storage tank for cooling, transferring the mother liquor into a crystallizing tank for slowly crystallizing and separating out to obtain potassium nitrate crystals and magnesium chloride solution byproducts; generally, magnesium chloride hexa-crystal aquatic products;
5) washing: transferring the potassium nitrate crystals obtained in the step 4) into a washing tank, washing to obtain potassium nitrate crystal slurry or called potassium nitrate crystal slurry, and returning washing mother liquor to the reaction tank for recycling;
6) centrifuging: separating solid from the washed potassium nitrate solid-containing crystal slurry, namely potassium nitrate crystal slurry, by using a centrifugal machine, and returning centrifugal mother liquor to the reaction tank for recycling;
7) drying: drying the finished potassium nitrate product in a dryer until the water content of the product is less than or equal to 0.1 percent to obtain a potassium nitrate product;
8) evaporation of magnesium chloride solution: the magnesium chloride obtained by cooling crystallization is generally the same as magnesium chloride hexa-crystallization aqueous solution, transferred into a magnesium chloride hexa-crystallization water storage tank and conveyed to the first effect of a three-effect magnesium chloride hexa-crystallization water evaporation crystallizer through a centrifugal pump, wherein the three-effect evaporator of the magnesium chloride hexa-crystallization water adopts concurrent flow operation, natural circulation of the first effect and forced circulation of the second effect and the third effect, a DTB crystallizer is adopted in a three-effect separation chamber, and continuous feeding, continuous evaporation and continuous discharging are adopted for evaporation crystallization; obtaining a magnesium chloride product;
9) magnesium chloride dehydration: and (4) centrifugally dewatering the magnesium chloride obtained in the step (8) to obtain a magnesium chloride product, controlling the water content of the magnesium chloride product to be 4%, and refluxing the removed mother liquor to a reaction tank. The potassium nitrate prepared by the embodiment has the content of 99.95 percent.
Example 2:
the invention discloses a method for preparing potassium nitrate by a nitric acid method, the rest of the following embodiments are the same as the embodiment 1 or the above embodiment except the following description, the embodiment mainly comprises the steps that the concentration of nitric acid is 51%, and simultaneously, a potassium nitrate crystallization agent is added into filter-pressing mother liquor during step 4) freeze crystallization to form a potassium nitrate saturated solution;
the method takes potassium chloride, dilute nitric acid and magnesium oxide as raw materials and produces a main product of potassium nitrate and a byproduct of magnesium chloride through the working procedures of proportioning, filter pressing, crystallization, washing, centrifugation, drying and the like, and the specific reaction process is as follows:
2) preparing materials: pumping nitric acid with mass concentration of 51 Wt% into a dilute nitric acid metering tank, and feeding magnesium oxide and potassium chloride to a reaction tank or a same feeding port below a reaction device tank through an automatic feeding machine;
2) reaction: adding process water into a reaction tank, adding magnesium oxide for 3 times, adding excessive magnesium oxide in the reaction, slowly adding nitric acid, controlling the pH to 3-4, performing the reaction at normal pressure, controlling the reaction temperature to 120 ℃, heating by using steam, controlling stirring reaction for 2 hours, adding potassium chloride for stirring reaction when the magnesium nitrate is fully reacted to generate magnesium nitrate, and controlling the magnesium nitrate and the potassium chloride to be fully reacted to generate a mixture reaction liquid of potassium nitrate and magnesium chloride, or called a reaction liquid;
3) plate and frame filter pressing: after the reaction is finished, transferring the reaction solution in the previous step into a heat-preserving tank, controlling the reaction solution to carry out first filter pressing by a plate-and-frame filter press at 70-80 ℃ to obtain filter pressing mother liquor, namely mixed liquor of potassium nitrate and magnesium chloride, and simultaneously obtain filter pressing filter residues, carrying out second filter pressing on the filter pressing mother liquor, wherein steam is generated in the filter pressing process;
4) freezing and crystallizing: in the mixed liquid of potassium nitrate and magnesium chloride of the filter pressing mother liquid, the mass ratio of potassium nitrate to magnesium chloride is 2.1: after the reaction is finished, simultaneously adding a potassium nitrate saturated solution, continuously stirring, controlling the addition amount of the potassium nitrate saturated solution to ensure that potassium nitrate is completely separated out after the potassium nitrate is changed along with the temperature, mainly utilizing the fact that the solubility of potassium nitrate is changed greatly along with the temperature, and the solubility of magnesium chloride is not changed greatly along with the temperature, then transferring the filter pressing mother liquor into a freezing tank through a mother liquor storage tank for cooling, transferring the mother liquor into a crystallizing tank after being cooled to-10 ℃, adding a potassium nitrate crystallization agent, namely the potassium nitrate saturated solution into the crystallizing tank, controlling the addition amount to be about 0.5-1% of the quality of the filter pressing mother liquor, slowly crystallizing to obtain potassium nitrate crystals, and simultaneously obtaining a magnesium chloride solution byproduct; generally, magnesium chloride hexa-crystal aquatic products;
5) washing: transferring the potassium nitrate crystals obtained in the step 4) into a washing tank, washing to obtain potassium nitrate crystal slurry or called potassium nitrate crystal slurry, and returning washing mother liquor to the reaction tank for recycling;
6) centrifuging: separating solid from the washed potassium nitrate solid-containing crystal slurry, namely potassium nitrate crystal slurry, by using a centrifugal machine, and returning centrifugal mother liquor to the reaction tank for recycling;
7) drying: drying the finished potassium nitrate product in a dryer until the water content of the product is less than or equal to 0.1 percent to obtain a potassium nitrate product;
8) evaporation of magnesium chloride solution: the magnesium chloride obtained by cooling crystallization is generally the same as magnesium chloride hexa-crystallization aqueous solution, transferred into a magnesium chloride hexa-crystallization water storage tank and conveyed to the first effect of a three-effect magnesium chloride hexa-crystallization water evaporation crystallizer through a centrifugal pump, wherein the three-effect evaporator of the magnesium chloride hexa-crystallization water adopts concurrent flow operation, natural circulation of the first effect and forced circulation of the second effect and the third effect, a DTB crystallizer is adopted in a three-effect separation chamber, and continuous feeding, continuous evaporation and continuous discharging are adopted for evaporation crystallization; obtaining a magnesium chloride product;
9) magnesium chloride dehydration: and (4) centrifugally dewatering the magnesium chloride obtained in the step (8) to obtain a magnesium chloride product, controlling the water content of the magnesium chloride product to be 4%, and refluxing the removed mother liquor to a reaction tank. The potassium nitrate prepared by the embodiment has the content of 99.99 percent.
Comparative example:
the invention discloses a method for preparing potassium nitrate by a nitric acid method, which changes the adding mode of magnesium oxide,
the method takes potassium chloride, dilute nitric acid and magnesium oxide as raw materials and produces a main product of potassium nitrate and a byproduct of magnesium chloride through the working procedures of proportioning, filter pressing, crystallization, washing, centrifugation, drying and the like, and the specific reaction process is as follows:
3) preparing materials: pumping nitric acid with the mass concentration of 50% into a dilute nitric acid metering tank, and conveying magnesium oxide and potassium chloride to a reaction tank or the same feeding port below a reaction device tank through an automatic feeding machine;
2) reaction: adding process water into a reaction tank, adding magnesium oxide for 1 time, adding excessive magnesium oxide in the reaction, slowly adding nitric acid, controlling the pH to 3.5, performing the reaction at normal pressure, controlling the reaction temperature to 120 ℃, heating by using steam, controlling stirring reaction for 2 hours, adding potassium chloride for stirring reaction when the magnesium nitrate is fully reacted to generate magnesium nitrate, and controlling the magnesium nitrate and the potassium chloride to be fully reacted to generate a mixture reaction liquid of potassium nitrate and magnesium chloride, or called a reaction liquid;
3) plate and frame filter pressing: after the reaction is finished, transferring the reaction solution in the previous step into a heat-preserving tank, controlling the reaction solution to carry out first filter pressing by a plate-and-frame filter press at 70-80 ℃ to obtain filter pressing mother liquor, namely mixed liquor of potassium nitrate and magnesium chloride, and simultaneously obtain filter pressing filter residues, carrying out second filter pressing on the filter pressing mother liquor, wherein steam is generated in the filter pressing process;
4) freezing and crystallizing: in the mixed liquid of potassium nitrate and magnesium chloride of the filter pressing mother liquid, the mass ratio of potassium nitrate to magnesium chloride is 2.1: after the reaction is finished, mainly utilizing the fact that the solubility of potassium nitrate changes greatly along with the temperature, but the solubility of magnesium chloride does not change greatly along with the temperature, then transferring the filter pressing mother liquor into a freezing tank through a mother liquor storage tank for cooling, transferring the mother liquor into a crystallizing tank for slowly crystallizing and separating out to obtain potassium nitrate crystals and magnesium chloride solution byproducts; generally, magnesium chloride hexa-crystal aquatic products;
5) washing: transferring the potassium nitrate crystals obtained in the step 4) into a washing tank, washing to obtain potassium nitrate crystal slurry or called potassium nitrate crystal slurry, and returning washing mother liquor to the reaction tank for recycling;
6) centrifuging: separating solid from the washed potassium nitrate solid-containing crystal slurry, namely potassium nitrate crystal slurry, by using a centrifugal machine, and returning centrifugal mother liquor to the reaction tank for recycling;
7) drying: drying the finished potassium nitrate product in a dryer until the water content of the product is less than or equal to 0.1 percent to obtain a potassium nitrate product;
8) evaporation of magnesium chloride solution: the magnesium chloride obtained by cooling crystallization is generally the same as magnesium chloride hexa-crystallization aqueous solution, transferred into a magnesium chloride hexa-crystallization water storage tank and conveyed to the first effect of a three-effect magnesium chloride hexa-crystallization water evaporation crystallizer through a centrifugal pump, wherein the three-effect evaporator of the magnesium chloride hexa-crystallization water adopts concurrent flow operation, natural circulation of the first effect and forced circulation of the second effect and the third effect, a DTB crystallizer is adopted in a three-effect separation chamber, and continuous feeding, continuous evaporation and continuous discharging are adopted for evaporation crystallization; obtaining a magnesium chloride product;
9) magnesium chloride dehydration: and (4) centrifugally dewatering the magnesium chloride obtained in the step (8) to obtain a magnesium chloride product, controlling the water content of the magnesium chloride product to be 4%, and refluxing the removed mother liquor to a reaction tank. The potassium nitrate prepared by the embodiment has the content of 98.9 percent, and the potassium nitrate content is lower, so that the reaction is possibly incomplete and the like.
The following table shows the quality indexes of potassium nitrate prepared by the method example of the present invention and the comparative example as shown in table 1,
description of the drawings: the detection basis is GB1918-2011, and it can be seen from the table above that the purity of the potassium nitrate prepared by adding the potassium nitrate crystallization agent in the method for preparing the potassium nitrate by the nitric acid method is higher.
The above-mentioned embodiments are only examples of the present invention, and should not be construed as limiting the scope of the present invention, and all the modifications and the decoration made by the skilled in the art using the principles and technical features of the present invention should be covered by the protection scope defined by the appended claims.
Claims (9)
1. A method for preparing potassium nitrate by a nitric acid method, which takes potassium chloride, dilute nitric acid and magnesium oxide as raw materials and produces a main product of potassium nitrate by the working procedures of batching, filter pressing, crystallization, washing, centrifugation and drying, comprises the following steps:
preparing materials: firstly, nitric acid is metered and pumped into an acid metering tank, then magnesium oxide and potassium chloride are conveyed to a feeding port of a reaction device tank through an automatic feeder,
2) heating and reacting: adding process water into the reaction device tank in the step 1), adding magnesium oxide in batches, slowly adding nitric acid for reaction, controlling the pH of the reaction solution to be carried out under an acidic condition, keeping the reaction temperature at 100 ℃ and 140 ℃, continuously stirring for reaction, adding potassium chloride for continuous stirring reaction after magnesium nitrate is generated, and obtaining a mixture reaction liquid of potassium nitrate and magnesium chloride;
3) plate and frame filter pressing: transferring the reaction liquid obtained in the step 2) into a heat preservation device tank, carrying out multiple filter pressing on the reaction liquid by a plate-and-frame filter press to obtain filter pressing mother liquid and filter pressing filter residues,
4) freezing and crystallizing: putting the filter pressing mother liquor obtained in the step 3) into a mother liquor storage tank, transferring the mother liquor storage tank into a freezing tank for cooling treatment, controlling the mother liquor storage tank to cool to-8 to-15 ℃, transferring the mother liquor storage tank into a crystallizing tank, and slowly crystallizing to obtain potassium nitrate crystals and magnesium chloride solution;
5) washing: putting the potassium nitrate crystals obtained in the step 4) into a washing tank, washing to obtain potassium nitrate crystal slurry, and returning washing mother liquor to the reaction device tank for recycling;
6) centrifuging: placing the potassium nitrate crystal slurry obtained in the step 4) into a centrifuge for centrifugal separation to obtain centrifugal potassium nitrate crystal solid, and returning centrifugal mother liquor to the reaction device tank for recycling;
7) drying: drying the solid potassium nitrate crystals by a dryer to obtain potassium nitrate with the water content less than or equal to 0.1 percent, namely a potassium nitrate product;
8) evaporation of magnesium chloride solution: transferring the magnesium chloride solution obtained in the step 4) into a magnesium chloride storage tank, conveying the magnesium chloride solution into a magnesium chloride evaporation crystallizer device through a centrifugal pump to perform downstream evaporation operation, and continuously feeding, continuously evaporating and continuously discharging through a separation chamber and a crystallizer to obtain a magnesium chloride coarse material;
9) magnesium chloride dehydration: and (3) carrying out centrifugal dehydration treatment on the magnesium chloride coarse material obtained in the step 8) to obtain a magnesium chloride product, and refluxing the separated mother liquor to a reaction device tank for recycling.
2. The method for preparing potassium nitrate by the nitric acid method according to claim 1, wherein the mass concentration of the nitric acid solution in the step 1) is controlled to be 45-52 Wt%.
3. The method for preparing potassium nitrate by the nitric acid method as claimed in claim 1, wherein the heating reaction in step 2) is that magnesium oxide is uniformly added in 2-4 times after process water is added, the pH is controlled to be 3-4, the reaction time is 1.5-2.5h, and the heating reaction is controlled to be steam heating.
4. The method for preparing potassium nitrate by the nitric acid method according to claim 1, wherein the plate-and-frame filter pressing in the step 3) is performed while controlling the temperature of the reaction solution to be 65-85 ℃, and the filter pressing frequency is controlled to be 1-3 times.
5. The method for preparing potassium nitrate by the nitric acid method according to claim 1, wherein the step 4) of freezing crystallization is that the mass ratio of potassium nitrate to magnesium chloride of the filter-pressing mother liquor entering the freezing tank is controlled to be 2-2.5: 1, controlling the cooling treatment temperature to be-9 to-12 ℃.
6. The method for preparing potassium nitrate by the nitric acid method according to claim 1, wherein the evaporation in the step 8) is triple effect evaporation, single effect natural circulation, double effect and triple effect forced circulation, and a DTB crystallizer is adopted in a triple effect separation chamber.
7. The method for preparing potassium nitrate by the nitric acid method according to claim 1, wherein the moisture content of the magnesium chloride product is controlled to be less than or equal to 4% in step 8).
8. The method for preparing potassium nitrate by the nitric acid method according to claim 1 or 3, wherein the heating reaction in the step 2) is performed under normal pressure or under a micro-pressure condition.
9. The method for preparing potassium nitrate by the nitric acid method according to claim 1 or 5, wherein the step 4) of freezing crystallization is to add a potassium nitrate crystallization agent into the filter-pressing mother liquor to crystallize and precipitate potassium nitrate crystals, wherein the potassium nitrate crystallization agent is a saturated/supersaturated solution of potassium nitrate or high-purity potassium nitrate crystals.
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| CN114873614A (en) * | 2022-06-10 | 2022-08-09 | 山西金兰化工股份有限公司 | Method for preparing potassium nitrate and by-producing potassium carnallite and magnesium chloride |
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