CN105060317A - Potassium chloride and ammonium nitrate double decomposition and circulation method for producing high quality potassium nitrate - Google Patents
Potassium chloride and ammonium nitrate double decomposition and circulation method for producing high quality potassium nitrate Download PDFInfo
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Abstract
The invention discloses a potassium chloride and ammonium nitrate double decomposition and circulation method for producing high quality potassium nitrate. According to the method, potassium chloride and ammonium nitrate are taken as the raw materials, and the method comprises steps of raw material preparation, potassium nitrate crystallization, foam floatation and separation, potassium nitrate refinement, and ammonium chloride crystallization. The method is developed on the basis of conventional potassium nitrate production technology by improving part of the technology; wherein in the foam flotation and separation technology, in the presence of a floatation reagent (C12-C20 higher straight-chain aliphatic amine) and in a certain pH value range, the ammonium chloride and coarse potassium nitrate can be separated through foam entrainment; in the potassium nitrate refinement, the refined potassium mother liquid in the previous circulation is used to wash the coarse potassium nitrate, and then potassium nitrate is purified by sodium carbonate. In one aspect, the conventional potassium nitrate production technology is optimized, the potassium nitrate quality is improved, and the impurity content of the potassium nitrate product is greatly reduced. In the other aspect, the water using amount is reduced, the labor intensity is also reduced, and the production cost is saved. The industrial grade KNO3 mass content is not less than 99.7%, the content of Cl<-> is not more than 0.01%, and the content of NH4<+> is not more than 0.03%. the method has a wide application value and can generate prominent social benefit and economic benefit.
Description
Technical field
The present invention relates to a kind of method by Repone K and ammonium nitrate double decomposition circulation process production high-quality saltpetre.
Background technology
Saltpetre is colourless rhombic system crystallization or white powder, is a kind of important inorganic chemical product.According to the effect purposes of saltpetre, saltpetre can be divided into agriculture level saltpetre and technical grade saltpetre.Agricultural level saltpetre, is applied to farm crop to chlorine sensitivity mainly as a kind of high-quality without chlorine potassium, nitrogen binary compound fertilizer, and is referred to as world's " green potash fertilizer " in short supply; Technical grade saltpetre, is compared to agriculture level saltpetre, quality is high, excellent property, and its purity, higher than 99.0%, is widely used in national defence, military project, special glass preparation and other electronics processing industry.In recent years, along with the development of science and technology, the demand of Chinese market to saltpetre constantly increases, and has higher requirement to the quality of saltpetre.
At present, domestic Production of Potassium Nitrate mainly contains several techniques such as SODIUMNITRATE-Repone K conversion method, Repone K-nitric acid (ammonium nitrate) ion exchange method and ammonium nitrate-Repone K metathesis conversion method.SODIUMNITRATE-Repone K conversion method is the industrial method adopted the earliest, this processing method has the advantages such as simple, the easy to operate and good product quality of flow process, but there is the expensive and shortcoming of raw material anxiety of raw material SODIUMNITRATE simultaneously, in the long run consider, this production technique does not meet the strategic requirement of China's Sustainable development.Ion exchange method is owing to exchanging that liquid saltpetre concentration is low, evaporation cost is high and requiring that high unfavorable factor limits the large-scale production of this technique to equipment performance, and domestic at present only have Shanxi Deng Jijia enterprise of Wen Tong sylvite Group Co., Ltd still to adopt this technique.Ammonium nitrate-Repone K double decomposition is developed by French Auby company the earliest, and because possessing simultaneously, raw material availability is high, processing unit simple and the advantage such as environmentally safe and enjoy the favor of entrepreneur, and current domestic Production of Potassium Nitrate producer adopts this technology mostly.
The technological principle of ammonium nitrate-Repone K preparing potassium nitrate by means of double decomposition is the quarternary phase diagram based on being made up of Repone K, ammonium nitrate, saltpetre, ammonium chloride, the crystallization completing saltpetre and ammonium chloride successively by selecting rational condition be separated.Technical process mainly comprises following four steps: one is in circulating mother liquor, add Repone K complete batching; Two is that after potassium nitrate solution crystallisation by cooling, centrifugation obtains saltpetre; Three is add ammonium nitrate in the mother liquor after saltpetre is separated; Four be solution after adding ammonium nitrate after evaporation concentration, crystallisation by cooling, centrifugation ammonium chloride, the Recycling Mother Solution after separation uses.Through the development of decades, Repone K-ammonium nitrate metathesis is produced saltpetre technology and is reached its maturity, but for a long time, the drawbacks such as the loaded down with trivial details and energy consumption of by-product ammonium chloride and saltpetre separation difficulty that this technique exists, poor product quality, slightly potassium process for refining is high do not obtain substantial improvement yet.
In recent years, numerous enterprises person skilled is produced saltpetre process optimization with regard to ammonium nitrate-Repone K replacement(metathesis)reaction and has been done unremitting effort, and proposes kinds of processes optimization method.These achievements in research are in the majority with patent report, only account for small part with academic paper form report, and these reports relate generally to technical fields such as improving raw material availability, purifying products and energy-saving and emission-reduction.
China's open patent of invention 200910115890.X " method of saltpetre is produced in metathesis " discloses a kind of method that saltpetre is produced in metathesis.This processing method by utilizing the rinsing of various different concns, relief liquor rinses work in-process, finished product saltpetre, and by the mode of heat of solution multiple junction produce quality up to 99.9% potassium nitrate product.This processing method optimizes traditional metathesis production technique, greatly improve the quality product of saltpetre, reduce the consumption of ammonium chloride sepn process clear water to a certain extent simultaneously, but the method for the rinsing potassium nitrate product of this rinsing by different concns, relief liquor different batches, the person's labour intensity that enhances enterprise work, extend the production cycle, reduce production efficiency.
China's publication 01114497.1 " three-step circular metathesis process of producing potassium nitrate " discloses a kind of method of three-step circular metathesis process of producing potassium nitrate.In this processing method implementation process, improved quality and the product yield of product by the mode adding auxiliary agent SODIUMNITRATE in reaction solution, its effect essence is the SODIUMNITRATE added promotes saltpetre precipitation as crystalline reagents.Patent public data shows, and after potassium nitrate crystal, in mother liquor, the content of SODIUMNITRATE is up to 4.5% ~ 11%, and this adds production cost on the one hand, may cause the Na in potassium nitrate product on the other hand
+the rising of content, causes difficulty to follow-up impurity removal process.Meanwhile, the potassium nitrate product that this inventive method is produced is agriculture level saltpetre, can not meet the service requirements of high-quality technical grade saltpetre.
The open patent of invention 201410310839.5 " metathesis air cooling crystallization method produces saltpetre technique " of China has openly been invented a kind of metathesis air cooling crystallization method and has been produced saltpetre technique.This invention adopts air to do heat-eliminating medium to realize the crystallization of saltpetre and ammonium chloride.In ammonium chloride sepn process, adopt smart potassium mother liquor and clear water to rinse saltpetre, wherein only in treating process, rinse dosage is 15% ~ 30% of saltpetre amount.This processing method remains the mode separating ammonium chloride that have employed conventional washing, and the homework burden that, labour intensity high to water resources consumption is large still fails to propose effective solution.
The open patent of invention of China 201310140425.8 " preparation method of a kind of high purity, saltpetre in enormous quantities " discloses a kind of preparation method of high-purity potassium nitrate.The method relates generally to the method for purification of saltpetre, by to the saltpetre of mass content 99.4% to dissolve, the unit operation such as crystallization and washing obtain 99.8% high-purity potassium nitrate, wherein dissolving water is the pure water prepared by double-stage reverse osmosis water manufacturing system, and the quality of its consumption and saltpetre is suitable.Found by public data, the Cl in the potassium nitrate product after purifying
-content be only 0.001%, for before purifying 0.02% 1/20th.This preparation method significantly reduces Cl in product
-content, improve the quality of potassium nitrate product.But, this patented method only relates to saltpetre purge process, and the not mentioned process being prepared saltpetre by the raw material such as ammonium nitrate and Repone K, and purge process water is pure water, described saltpetre preparation method invests greatly, cost is high, is unfavorable for commercial scale production.
In recent years, systematically reported seldom by the research of academic paper form to ammonium nitrate and Repone K preparing potassium nitrate by means of double decomposition.Wherein, the separation of product is related generally to from the report of aspect to preparing potassium nitrate by means of double decomposition of production practice.Relevant report has:
F.HERNAINZ etc. are at " SeparationofthesolublesaltsKNO
3andNH
4clbyflotationwitholeicacid " report using oleic acid as collecting agent in (TransIChemE, 2003,81.A:963-970.), ammonia is pH adjusting agent, controls solution optimal ph=8, by three step flotation NH
4the mode of Cl realizes the separation method of product saltpetre and ammonium chloride in Production of Potassium Nitrate.Result shows, KNO after flotation
3total yield be 93%, massfraction is 98%.Similarly, Chemical Design Inst., Qinghai Prov company limited is in " research of saltpetre reverse flotation separation method " (chemical industry mineral and processing, 2010, (7) to report: 17-20.) with sodium oleate be collecting agent, NaOH is pH value adjusting agent, adjustment optimal ph is 8.0, is realized the separation of ammonium chloride by the mode of multiple-grooved connection choosing.It is consistent with people such as F.HERNAINZ that it probes into result.But, in actual production, be but difficult to obtain the ideal effect described in document.
The pertinent literature of other Production of Potassium Nitrate by Double Decomposition-Circulation Method that can find, how inquire into the feasibility of this production method from crystallization, phasor, Efficiency Calculation scheduling theory angle, mainly contain:
Li Tianwen etc. are at " Phase Diagram Analysis in double decomposition Production of Potassium Nitrate " (sea lake salt and chemical industry, 2001,30 (2): 7-11) in the quarternary phase diagram be made up of Repone K, ammonium nitrate, saltpetre and ammonium chloride for foundation, analyze the distribution in production process and influence factor thereof; Zhang Yifu etc. are in " producing 20000 t potassium nitrate unit Efficiency Calculation per year " (inorganic chemicals industry, 2004,36 (1): 43-44) according to the processing parameter of 20,000 t preparing potassium nitrate by means of double decomposition and the physical parameter of each material in, calculating the heat often produced needed for 1t Agricultural Potassium Nitrate, to instructing saltpetre industrial design, there is certain reference role; Zhang Gang etc. are at " novel process of crystallisation by cooling manufacture saltpetre " (Yunnan chemical, 2005,32 (5): 29-31) describe Demountable spiral-plate heat exchanger in as the application of Outer Cooler in Production of Potassium Nitrate, achieve serialization cooling and crystallization.Report like this also has a lot, but reports that the representative paper of preparing potassium nitrate by means of double decomposition technique is subordinate to the people such as Zhang Gang all sidedly.If Zhang Gang etc. is at " Repone K and ammonium nitrate Production of Potassium Nitrate by Double Decomposition-Circulation Method " (sea lake salt and chemical industry, 1994,23 (1): 41-42) literary composition comprehensively describes technological principle and the technological process of Production of Potassium Nitrate by Double Decomposition-Circulation Method, and the potassium nitrate product of producing reaches the industrial potassium nitrate first grade quality standard that the national GB/T1981-86 " industrial potassium nitrate " that performed at that time arranges.
Through the development of decades, although current domestic Production of Potassium Nitrate enterprise has carried out optimize and improve in various degree to traditional process for producing potassium nitrate, the serial drawback existed in traditional mode of production has not obtained the solution of essence yet.Sum up, be mainly reflected in two aspects: on the one hand, ammonium chloride separating technology is loaded down with trivial details, and energy consumption is high, and labour intensity is large; On the other hand, potassium nitrate product foreign matter content is high, poor quality, and quality product can not reach technical grade saltpetre quality standard.
Under the real situation that industrial market is growing to high-quality saltpetre demand, based on the difficult problem that the process implementing process of existing preparing potassium nitrate by means of double decomposition exists, probe into and less investment is proposed, the technique of energy consumption is low, labour intensity is little double decomposition production high-quality saltpetre seems particularly necessary.The present invention produces on the basis of saltpetre technique in traditional metathesis, probes into, the practice such as pilot scale and suitability for industrialized production through laboratory, provides a kind of novel process by Repone K and ammonium nitrate double decomposition production high-quality saltpetre.The enforcement of present method, by the limitation of the conventional unit operations that the restriction Production of Potassium Nitrate technology existed in the production technique that breaks traditions further develops, the production that can be high-quality saltpetre provides certain directive function.Method technique of the present invention is simple, and level of automation is high, shortens the production cycle.The potassium nitrate product quality adopting the method to produce is high, and foreign matter content is low, saltpetre mass content KNO
3>=99.7%, wherein Cl
-≤ 0.01%, NH
4 +≤ 0.03%, saltpetre quality meets the requirement of the industrial premium grads saltpetre that technical grade saltpetre state quality standard GB/T1918-2011 retrains, and can meet all conglomeraties such as high-end thin glass preparation to the demand of high-quality saltpetre.
Summary of the invention
For solving the above-mentioned technical barrier that current China Production of Potassium Nitrate by Double Decomposition-Circulation Method technique exists, the object of the present invention is to provide a kind of method of double decomposition circulation process production high-quality saltpetre.
In order to realize foregoing invention object, the present invention is achieved in the following ways:
A kind of method by Repone K and ammonium nitrate double decomposition circulation process production high-quality saltpetre of the present invention, described method is undertaken by following technical process:
By a method for Repone K and ammonium nitrate double decomposition circulation process production high-quality saltpetre, its technical characteristic is to carry out according to following steps:
(1) prepare burden: Repone K, ammonium nitrate and water are hybridly prepared into KNO
3reaction solution, places in dosing vessel, KNO
3nH in reaction solution
4 +with Cl
-mol ratio be 1 ~ 1.6: 1, steam heating also stirs;
(2) the adding of flotation reagent: treat dosing vessel KNO
3reaction solution is warming up to>=40 DEG C time, in dosing vessel, drop into flotation reagent, continue to heat up, make it at KNO
3disperse completely in reaction solution, dissolve; In this process, adjustment system pH is between 4.0 ~ 7.0;
(3) KNO
3crystallization: control KNO
3reacting liquid temperature 70 DEG C ~ 110 DEG C, treats KNO
3reaction solution is evaporated to 38Be ~ 44Be, after filtering and impurity removing, is cooled to 30 DEG C ~ 36 DEG C, must separates out potassium nitrate crystals mother liquor;
(4) pneumatic flotation is separated: the mother liquor of separating out potassium nitrate crystals is pumped to centrifugal filter device by pump, the ammonia chloride crystal be mixed in potassium nitrate crystals mother liquor floats to the upper strata of separating out potassium nitrate crystals mother liquor naturally with foam, by the mode of overflow, foam layer is separated, the mother liquor centrifuge dehydration of potassium nitrate crystals will be separated out, obtain crude product potassium nitrate crystals, after being separated, foam solution is containing ammonium chloride mother liquor, stand-by;
(5) dehydration of crude product potassium nitrate crystals and washing: crude product potassium nitrate crystals is put into the whizzer being lined with filter cloth, rinse the residual chloride ammonium being adsorbed on crude product saltpetre top layer with clear water after whizzer filter dehydration; Through whizzer filter dehydration, obtain crude product saltpetre; Together with parting liquid converges with washings, be mother liquor I, stand-by;
(6) crude product saltpetre is refined: dissolved by separating obtained crude product saltpetre, determine wherein NH
4 +amount, and with n (Na
2cO
3): n (NH
4 +the mol ratio of)=1:2, adds sodium carbonate in potassium nitrate solution; Control steam heating temperature between 100 DEG C ~ 115 DEG C, strength of solution 48Be ~ 52Be; Until solution cooling, after recrystallization, after centrifugal, drying, namely obtain fine work saltpetre; Mother liquor III part that recrystallization is separated out will be used for the washing of crude product saltpetre in next circulation, and a part and ammonium chloride mother liquor converge;
(7) NH
4cl crystallization: ammonium chloride mother liquor and mother liquor I, mother liquor III are mixed and heated to 120-130 DEG C, evaporation concentration, and drop into ammonium nitrate, control NH
4 +with Cl
-mol ratio be 2:1, adjustment reaction solution concentration is 36Be ~ 38Be, cooling, separate out ammonia chloride crystal;
(8) NH
4cl product: the whizzer solution of separating out ammonia chloride crystal being put into liner filter cloth, obtains ammonium chloride product after centrifuge dehydration; Be separated NH
4cl joins KNO as mother liquor II
3in reaction solution, Substitute For Partial ammonium nitrate.
Flotation reagent is C
12~ C
20one or more of high straight chain aliphatic amide.
During batching, the weight of Repone K is according to 100%, flotation reagent C
12~ C
20the gross weight of high straight chain aliphatic amide is 0.02% ~ 0.06%.
PH value regulator is hydrochloric acid, potassium hydroxide or sodium hydroxide.
KNO
3crystallization mode can be air natural crystallisation by cooling, also can be vacuum cooling crystallization.
Add the amount of sodium carbonate according to the NH in crude product saltpetre
4 +content is according to the ratio-dependent of material mol ratio 1:2.
Sum up, the present invention adopts Repone K, water and ammonium nitrate or separates out the circulating mother liquor after ammonium chloride is raw material, comprises the technological processs such as the refining and ammonium chloride crystals of preparation of raw material, potassium nitrate crystal, flotation separation, saltpetre.Wherein, floatation separation process is that the mode of being carried secretly by foam under the effect of flotation reagent completes being separated of ammonium chloride and crude product saltpetre, and the refining of saltpetre is realized through operations such as sodium carbonate purifications by the upper one smart potassium mother liquor washing circulated again.
The present invention is compared to prior art, following technique effect can be produced: 1, adopt the flotation reagents such as high straight chain aliphatic amide by the mode separating ammonium chloride of pneumatic flotation, optimize the ammonium chloride separating technology in traditional mode of production thoroughly, dosing is few, good separating effect, significantly reduces NH in crude product saltpetre
4 +, Cl
-deng the content of impurity.2, flotation separation process naturally completes under floatation of foam effect, without the need to extra energy consumption, significantly saved bath water.3, the present invention adopts the smart potassium mother liquor washing of part to be adsorbed on the residual chloride ammonium on crude product saltpetre top layer due to flotation, reduces the loss of saltpetre, improves product recovery rate.4, the present invention is in saltpetre treating process, adds sodium carbonate to remove the NH of trace in product
4 +.Most of NaCl that reaction process generates separates out in ammonium chloride crystals process thereupon, and a small amount of sodium-chlor is stayed in the mother liquor after ammonium chloride precipitation, and forms stable circulation in system.In circulating system, sodium-chlor is as crystalline reagents, facilitates the precipitation of potassium nitrate crystals, improves saltpetre productive rate, and does not affect the quality of saltpetre.5, present invention process process is simple, easy to operate, reduces labour intensity, is conducive to realizing large scale continuous prod.6, the potassium nitrate product foreign matter content of the inventive method production is low, and quality is high, saltpetre mass content KNO
3>=99.7%, meet the technical grade premium grads saltpetre quality standard that national GB/T1918-2011 " industrial potassium nitrate " retrains.
Double decomposition circulation process production high-quality saltpetre method of the present invention, pollution-free, energy consumption is low, technique is simple, level of automation is high, meets the general requirements of National Sustainable Development Strategies.This inventive method is applied to suitability for industrialized production, can be society and enterprise creates high economic benefit.
Accompanying drawing explanation
Fig. 1 is the present invention by the process flow diagram of Repone K and ammonium nitrate double decomposition circulation process production high-quality saltpetre method.
Embodiment
As shown in Figure 1, the method for double decomposition circulation process production high-quality saltpetre of the present invention, with Repone K, ammonium nitrate and water for raw material, adopts Recycling Mother Solution method production high-quality saltpetre, implements especially by with under type:
(1) prepare burden: when first time produces, Repone K, ammonium nitrate and water are mixed with saltpetre reaction solution, control NH
4 +with Cl
-amount than for (1.6 ~ 1): 1, under constantly stirring, pass through steam heating; Circulation time is then according to conservation of matter, and circulating mother liquor in Repone K, water and step (8) is mixed into dosing vessel by a certain percentage, is mixed with the state that when producing with first time, saltpetre reaction solution is consistent;
(2) the adding of flotation reagent: treat dosing vessel KNO
3during reacting liquid temperature>=40 DEG C, according to the input amount of Repone K, in dosing vessel, drop into one or more C of Repone K weight ratio 0.02% ~ 0.06%
12~ C
20high straight chain aliphatic amide, continues to heat up, makes it at KNO
3disperse completely in reaction system, dissolve; In this process, to, by hydrochloric acid or potassium hydroxide adjustment system pH, make it to guarantee between 4.0 ~ 7.0 simultaneously;
(3) KNO
3crystallization: control KNO
3reacting liquid temperature 70 DEG C ~ 110 DEG C, question response liquid is evaporated to 38Be ~ 44Be when reaching saltpetre hypersaturated state, by reacting liquid filtering removal of impurities, ensure that reaction solution is cooled to 30 DEG C ~ 36 DEG C in the mode of spontaneous nucleation or vacuum cooling crystallization, separate out potassium nitrate crystals;
(4) ammonium chloride is separated: the solid-liquid system of separating out potassium nitrate crystals is pumped to centrifugal filter device by pump, and the ammonia chloride crystal be mixed in potassium nitrate crystals together floats to KNO by under the effect of carrying secretly of foam with foam
3mother liquor upper strata after precipitation, and completed and being separated of potassium nitrate crystals by the mode of overflow, the ammonium chloride after separation imports mother liquor I;
(5) dehydration of crude product saltpetre and washing: the potassium nitrate crystals isolating ammonium chloride is put into the whizzer being lined with filter cloth, rinse with a small amount of clear water after whizzer filter dehydration, recentrifuge dewaters, and removes the residual chloride ammonium being adsorbed on crude product saltpetre top layer due to flotation.Mother liquor I after separation and lotion liquid converge together, will be used for the circulation of subsequent step (7);
(6) crude product saltpetre is refined: dissolved by crude product saltpetre separating obtained in step (5), determine wherein NH
4 +amount, and with n (Na
2cO
3): n (NH
4 +the mol ratio of)=1:2, to KNO
3a certain amount of sodium carbonate is added in solution.Control steam heating temperature between 100 DEG C ~ 115 DEG C, strength of solution 48Be ~ 52Be.Until solution cooling, after recrystallization, after centrifugal, drying, namely obtain mass content KNO
3the fine work saltpetre of>=99.7%.Wherein, Cl
-≤ 0.01%, NH
4 +≤ 0.03%.The mother liquor III part that recrystallization is separated out will be used for the washing of crude product saltpetre in next circulation, and rest part will converge with mother liquor I;
(7) NH
4cl crystallization: about 125 DEG C will be heated to containing ammonium mother liquor, evaporation concentration, and drop into a certain amount of ammonium nitrate, control NH
4 +with Cl
-mol ratio be 2:1, adjustment ammonium chloride reaction solution concentration is 36Be ~ 38Be, cooling, separates out ammonia chloride crystal;
(8) NH
4cl product: the whizzer solution of separating out ammonia chloride crystal being put into liner filter cloth, obtains ammonium chloride product after centrifuge dehydration.Mother liquor II after separation will get back to step (1) and recycle.
Claims (6)
1., by a method for Repone K and ammonium nitrate double decomposition circulation process production high-quality saltpetre, it is characterized in that: carry out according to following steps:
(1) prepare burden: Repone K, ammonium nitrate and water are hybridly prepared into KNO
3reaction solution, places in dosing vessel, KNO
3nH in reaction solution
4 +with Cl
-mol ratio be 1 ~ 1.6: 1, steam heating also stirs;
(2) the adding of flotation reagent: treat dosing vessel KNO
3reaction solution is warming up to>=40 DEG C time, in dosing vessel, drop into flotation reagent, continue to heat up, make it at KNO
3disperse completely in reaction solution, dissolve; In this process, adjustment system pH is between 4.0 ~ 7.0;
(3) KNO
3crystallization: control KNO
3reacting liquid temperature 70 DEG C ~ 110 DEG C, treats KNO
3reaction solution is evaporated to 38Be ~ 44Be, after filtering and impurity removing, is cooled to 30 DEG C ~ 36 DEG C, must separates out potassium nitrate crystals mother liquor;
(4) pneumatic flotation is separated: the mother liquor of separating out potassium nitrate crystals is pumped to centrifugal filter device by pump, the ammonia chloride crystal be mixed in potassium nitrate crystals mother liquor floats to the upper strata of separating out potassium nitrate crystals mother liquor naturally with foam, by the mode of overflow, foam layer is separated, the mother liquor centrifuge dehydration of potassium nitrate crystals will be separated out, obtain crude product potassium nitrate crystals, after being separated, foam solution is containing ammonium chloride mother liquor, stand-by;
(5) dehydration of crude product potassium nitrate crystals and washing: crude product potassium nitrate crystals is put into the whizzer being lined with filter cloth, rinse the residual chloride ammonium being adsorbed on crude product saltpetre top layer with clear water after whizzer filter dehydration; Through whizzer filter dehydration, obtain crude product saltpetre; Together with parting liquid converges with washings, be mother liquor I, stand-by;
(6) crude product saltpetre is refined: dissolved by separating obtained crude product saltpetre, determine wherein NH
4 +amount, and with n (Na
2cO
3): n (NH
4 +the mol ratio of)=1:2, adds sodium carbonate in potassium nitrate solution; Control steam heating temperature between 100 DEG C ~ 115 DEG C, strength of solution 48Be ~ 52Be; Until solution cooling, after recrystallization, after centrifugal, drying, namely obtain fine work saltpetre; Mother liquor III part that recrystallization is separated out will be used for the washing of crude product saltpetre in next circulation, and a part and ammonium chloride mother liquor converge;
(7) NH
4cl crystallization: ammonium chloride mother liquor and mother liquor I, mother liquor III are mixed and heated to 120-130 DEG C, evaporation concentration, and drop into ammonium nitrate, control NH
4 +with Cl
-mol ratio be 2:1, adjustment reaction solution concentration is 36Be ~ 38Be, cooling, separate out ammonia chloride crystal;
(8) NH
4cl product: the whizzer solution of separating out ammonia chloride crystal being put into liner filter cloth, obtains ammonium chloride product after centrifuge dehydration; Be separated NH
4cl joins KNO as mother liquor II
3in reaction solution, Substitute For Partial ammonium nitrate.
2. a kind of method by Repone K and ammonium nitrate double decomposition circulation process production high-quality saltpetre according to claim 1, is characterized in that: flotation reagent is C
12~ C
20one or more of high straight chain aliphatic amide.
3. strengthen the method that by-product ammonium chloride is separated in preparing potassium nitrate by means of double decomposition according to claim 1, it is characterized in that: during batching, the weight of Repone K is according to 100%, flotation reagent C
12~ C
20the gross weight of high straight chain aliphatic amide is 0.02% ~ 0.06%.
4. a kind of method by Repone K and ammonium nitrate double decomposition circulation process production high-quality saltpetre according to claim 1, is characterized in that: pH value regulator is hydrochloric acid, potassium hydroxide or sodium hydroxide.
5. a kind of method by Repone K and ammonium nitrate double decomposition circulation process production high-quality saltpetre according to claim 1, is characterized in that: KNO
3crystallization mode can be air natural crystallisation by cooling, also can be vacuum cooling crystallization.
6. a kind of method by Repone K and ammonium nitrate double decomposition circulation process production high-quality saltpetre according to claim 1, is characterized in that: add the amount of sodium carbonate according to the NH in crude product saltpetre
4 +content is according to the ratio-dependent of material mol ratio 1:2.
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