CN101182014B - Preparation technique of potassium nitrate - Google Patents
Preparation technique of potassium nitrate Download PDFInfo
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- CN101182014B CN101182014B CN2007101854485A CN200710185448A CN101182014B CN 101182014 B CN101182014 B CN 101182014B CN 2007101854485 A CN2007101854485 A CN 2007101854485A CN 200710185448 A CN200710185448 A CN 200710185448A CN 101182014 B CN101182014 B CN 101182014B
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- nitric acid
- potassium nitrate
- saltpetre
- hydrochloric acid
- rare nitric
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Abstract
The invention relates to a preparation technology of potassium nitrate, pertaining to the inorganic chemical technical field and solving the problems of restricted sources of raw materials, high production cost, high energy consumption, low one-off yield of finished products, nonrecoverable waste, etc., of the existing method. Potassium chloride and dilute nitric acid are blended according to certain proportion and react under the negative pressure of 0.01-0.02 MPa and the temperature of 30-40DEG C; the mixed solution produced from the reaction is cooled to the normal temperature and continues to be frozen and then is centrifugated to obtain crude potassium nitrate and primary mother liquor; the crude potassium nitrate can be refined to obtain the finished product while the primary mother liquor is evaporated and concentrated to precipitate hydrochloric acid and nitric acid which are separated through condensation and extraction; the concentrated secondary crude potassium nitrate is cooled, frozen and centrifugated to obtain the secondary crude potassium nitrate and secondary mother liquor which returns to the system for recycling. The one-off yield of the potassium nitrate is relatively high and is 85-90 percent, which ensures simple follow-up treatment technology, low energy consumption and relatively low cost and realizes no pollution and no wastewater discharge, thus completely solving the environment-friendly problem.
Description
Technical field
The present invention relates to technical field of inorganic chemical industry, be specially a kind of potassium nitrate preparing technology.
Background technology
Saltpetre is one of main products of sylvite series products, the industrial fields such as fireworks, black powder, opticglass, special glass that are mainly used in, what use on the agricultural is fertilizer grade saltpetre or agricultural saltpetre, it is a kind of fine potassium nitrogen binary compound fertilizer, contain potassium oxide and 13% above nitrogen greater than 44%, it all is soluble nutrient, can all be absorbed by crop, be mainly used in fields such as tobacco, cash crop, gardening, can obviously improve the yield and quality of crop, be one of required high-effective chemical fertilizer kind of development high-efficiency high-quality agricultural.
China's saltpetre is through developed recently; people have found out kinds of processes and have produced route; formed certain scale; obtained certain technical progress; but in actual production process, all there is shortcoming separately; such as being the ion exchange method of raw material with Repone K and ammonium nitrate; its shortcoming is to adopt ammonium nitrate as raw material, because ammonium nitrate has explosivity, is the main raw material of making native explosive; so country expressly limits its use range; institute is so that raw material sources are restricted, and the ammonium nitrate price is higher simultaneously, and general per ton is about 1500 yuan; use cost is higher; and having the ammonium chloride exhausted liquid of part lower concentration to generate, recovery difficult is bigger, is the protection environment; reduce pollutant emission; usually this part solution is adopted the way of evaporation concentration to reclaim, but because this strength of solution is low, evaporation concentration need consume a large amount of steam; thereby cause the whole production process energy consumption big, the cost height.Be the nitric acid conversion methdo of raw material with Repone K and nitric acid for another example, though solved a series of problems that above-mentioned process using ammonium nitrate is brought, raw material sources are extensive, production cost is lower, the problem of its existence is that mother liquor contains a large amount of saltpetre in the sepn process, must just can obtain through the circulation extraction, but the disposable finished product yield of saltpetre is lower, subsequent treatment process energy consumption height, cost height; And the mixing acid that contains nitric acid and hydrochloric acid that reaction generates in time do not reclaim, and equipment has been caused great corrosion, and severe contamination environment.
Summary of the invention
There are problems such as raw material sources are restricted, production cost is higher, energy consumption is high and disposable finished product yield is lower, waste can't reclaim in the present invention in order to solve existing saltpetre preparation method, and a kind of potassium nitrate preparing technology is provided.
The present invention adopts following technical scheme to realize: a kind of potassium nitrate preparing technology, may further comprise the steps: (1) is that rare nitric acid of 30-40% is 1 according to mol ratio with Repone K and concentration: the mixed of 1.4-1.5, in negative pressure is that 0.01-0.02Mpa, temperature are to react under 30-40 ℃ the condition, generation contains the mixing solutions of saltpetre, rare nitric acid and hydrochloric acid, in the reaction process, rare nitric acid is excessive, the Repone K complete reaction; (2) the above-mentioned mixing solutions that obtains is cooled to normal temperature, continue to be refrigerated to 0～-5 ℃ then, disposablely separate out most of crude product saltpetre, be approximately 85-90%, and carry out centrifugation, obtain crude product saltpetre and comprise a mother liquor of saltpetre, hydrochloric acid and rare nitric acid, the content of saltpetre only is 10-15% in mother liquor; (3) a crude product saltpetre is carried out obtaining finished product after the refinement treatment, be that 0.01-0.02Mpa, temperature are to evaporate under 70-80 ℃ the condition and make a mother liquor be concentrated into 50-55 degree Beaume (° B é) with mother liquor in negative pressure simultaneously, obtain comprising the mixed gas and the secondary crude product potassium nitrate solution of hydrochloric acid, rare nitric acid, this step is utilized the volatility of hydrochloric acid and nitric acid, both are evaporated separation, the secondary crude product potassium nitrate solution after obtaining concentrating; (4) the secondary crude product potassium nitrate solution that obtains is cooled to normal temperature, continues to be refrigerated to 0～-5 ℃ then, and carry out centrifugation, obtain secondary crude product saltpetre and secondary mother liquid, the content of saltpetre and hydrochloric acid, nitric acid still less in the secondary mother liquid; (5) secondary crude product saltpetre is carried out obtaining finished product after the refinement treatment, simultaneously secondary mother liquid is returned evaporation, enrichment process in the step (3), to recycle, so that the yield of saltpetre and purity are more and more higher, the rate of recovery of hydrochloric acid and rare nitric acid is also more and more higher.
In the said process, the refinement treatment operation of crude product saltpetre is that those of ordinary skill in the art is easy to realize, carries out drying after refining, packing gets final product; Described reaction and cooling apparatus adopt the jacketed type enamel reaction still, and evaporation equipment adopts graphite modified polypropylene shell and tube heating chamber, and extraction equipment adopts CTL type centrifugal extractor, and refrigerating apparatus adopts YSBLG type brine freezing unit.
The spent acid that generates for fear of reaction causes corrosion and contaminate environment to equipment, the present invention with the Mixed Gas Condensation that comprises hydrochloric acid and rare nitric acid that obtains in the above-mentioned steps (3) to 40-50 ℃, obtain comprising the mixing acid of hydrochloric acid and rare nitric acid, extract with tributyl phosphate then, obtain rare nitric acid and hydrochloric acid respectively, rare nitric acid recycles as the reaction raw materials retrieval system, and the hydrochloric acid that obtains is carried through rectifying and is used to produce 30% technical hydrochloric acid after dense.In addition, because hydrochloric acid and nitric acid itself all have volatility, also can produce the mixed gas of minute quantity in the reaction process, this mixed gas adopts method same as described above to absorb and utilizes.
Known, potassium chloride particle is thin more, helps the carrying out that react more, but cost is higher simultaneously, and the present invention is through test of many times and summary of experience, and the order number of determining Repone K is the 160-170 order.
The present invention is 1. HNO of basis
3+ KCl
KNO
3+ HCl chemical equation is produced saltpetre, because 1. chemical equation is reversible reaction, carries out to the direction that generates saltpetre in order to make this reaction, and the present invention has taked following way:
When 1, reacting, add excessive rare nitric acid, improve concentration of reactants;
2, the suitable temperature of reaction of control guarantees normally carrying out of chemical reaction, and is too high as temperature, and the nitric acid volatilization increases, and causes evaporable nitric acid to sneak in the hydrogenchloride, causes not easily separated and waste; Temperature is low excessively, and chemical reaction is insufficient, and the saltpetre composition is few, and product purity is poor, and temperature of reaction of the present invention is controlled at 30-40 ℃.
Repone K raw material of the present invention can be buied from Salt Lake Industry, Qinghai group, and described rare nitric acid wide material sources can directly be buied from the market.
After adopting saltpetre that preparation technology of the present invention obtains after testing, its every performance index and national standard compare, and be as shown in the table:
| Numbering | Project | National standard (%) | The saltpetre that the present invention obtains (%) |
| 1 | Saltpetre | ≥99.4 | 99.6-99.8 |
| 2 | Moisture | ≤0.10 | 0.05-0.06 |
| 3 | Chlorion (Cl -) | ≤0.020 | 0.01-0.015 |
| 4 | Water-insoluble | ≤0.020 | 0.01-0.015 |
| 5 | Sulfate ion (SO 4 2-) | ≤0.010 | 0.002-0.005 |
| 6 | Rate of moisture absorption | ≤0.30 | 0.15-0.20 |
Can find out that from last table the every index of the saltpetre that the present invention makes all reaches or is better than national standard.
Compared with prior art, the present invention utilizes nitric acid and Repone K to get the mixing solutions of saltpetre and hydrochloric acid through replacement(metathesis)reaction, with mixing solutions through the cooling, freezing, centrifugal after, a large amount of potassium nitrate crystals are separated out, disposable yield is higher, be 85-90%, make that subsequent treatment process is simple, energy consumption is low, cost is lower; Mother liquor is after evaporation concentration simultaneously, utilize the volatility of hydrochloric acid and nitric acid that its evaporation is separated, by extraction hydrochloric acid is separated, reclaims with nitric acid then, realized pollution-free, non-wastewater discharge, thoroughly solve environmental issue, and reclaimed the rare nitric acid retrieval system recycling again that obtains, greatly reduced production cost.
Description of drawings
Fig. 1 is a process flow sheet of the present invention
Embodiment
Embodiment 1:
A kind of potassium nitrate preparing technology, may further comprise the steps: (1) is that rare nitric acid of 30% is 1: 1.4 mixed according to mol ratio with Repone K and concentration, in negative pressure is that 0.01Mpa, temperature are to react under 30 ℃ the condition, generation contains the mixing solutions of saltpetre, rare nitric acid and hydrochloric acid, and the order number of Repone K is 160 orders; (2) the above-mentioned mixing solutions that obtains is cooled to normal temperature, continues to be refrigerated to 0 ℃ then, and carry out centrifugation, obtain crude product saltpetre and contain a mother liquor of saltpetre, hydrochloric acid and rare nitric acid; (3) a crude product saltpetre is carried out obtaining finished product after the refinement treatment, dry then, packing gets final product, be to evaporate under 70 ℃ the condition and make a mother liquor be concentrated into 50 degree Beaume simultaneously with mother liquor, obtain comprising the mixed gas and the secondary crude product potassium nitrate solution of hydrochloric acid, rare nitric acid in negative pressure 0.01Mpa, temperature; (4) the secondary crude product potassium nitrate solution that obtains is cooled to normal temperature, continues to be refrigerated to 0 ℃ then, and carry out centrifugation, obtain secondary crude product saltpetre and the secondary mother liquid that contains a small amount of saltpetre, hydrochloric acid and rare nitric acid; (5) secondary crude product saltpetre is carried out obtaining finished product after the refinement treatment, dry then, packing gets final product, and simultaneously secondary mother liquid is returned evaporation, enrichment process in the step (3), to recycle.With evaporable Mixed Gas Condensation to 40 in the mixed gas that comprises hydrochloric acid, rare nitric acid that obtains in the step (3) and the reaction process ℃, obtain comprising the mixing acid of hydrochloric acid and rare nitric acid, extract with tributyl phosphate then, obtain rare nitric acid and hydrochloric acid respectively, rare nitric acid recycles as the reaction raw materials retrieval system, and hydrochloric acid is carried through rectifying and is used to produce 30% technical hydrochloric acid after dense.
Embodiment 2:
A kind of potassium nitrate preparing technology, may further comprise the steps: (1) is that rare nitric acid of 40% is 1: 1.5 mixed according to mol ratio with Repone K and concentration, in negative pressure is that 0.02Mpa, temperature are to react under 40 ℃ the condition, generation contains the mixing solutions of saltpetre, rare nitric acid and hydrochloric acid, and the order number of Repone K is 170 orders; (2) the above-mentioned mixing solutions that obtains is cooled to normal temperature, continues to be refrigerated to-5 ℃ then, and carry out centrifugation, obtain crude product saltpetre and contain a mother liquor of saltpetre, hydrochloric acid and rare nitric acid; (3) a crude product saltpetre is carried out obtaining finished product after the refinement treatment, dry then, packing gets final product, be to evaporate under 80 ℃ the condition and make a mother liquor be concentrated into 55 degree Beaume simultaneously with mother liquor, obtain comprising the mixed gas and the secondary crude product potassium nitrate solution of hydrochloric acid, rare nitric acid in negative 0.02Mpa, temperature; (4) the secondary crude product potassium nitrate solution that obtains is cooled to normal temperature, continues to be refrigerated to-5 ℃ then, and carry out centrifugation, obtain secondary crude product saltpetre and the secondary mother liquid that contains a small amount of saltpetre, hydrochloric acid and rare nitric acid; (5) secondary crude product saltpetre is carried out obtaining finished product after the refinement treatment, dry then, packing gets final product, and simultaneously secondary mother liquid is returned evaporation, enrichment process in the step (3), to recycle.With evaporable Mixed Gas Condensation to 50 in the mixed gas that comprises hydrochloric acid, rare nitric acid that obtains in the step (3) and the reaction process ℃, obtain comprising the mixing acid of hydrochloric acid and rare nitric acid, extract with tributyl phosphate then, obtain rare nitric acid and hydrochloric acid respectively, rare nitric acid recycles as the reaction raw materials retrieval system, and hydrochloric acid is carried through rectifying and is used to produce 30% technical hydrochloric acid after dense.
Embodiment 3:
A kind of potassium nitrate preparing technology, may further comprise the steps: (1) is that rare nitric acid of 30% is 1: 1.5 mixed according to mol ratio with Repone K and concentration, in negative pressure is that 0.02Mpa, temperature are to react under 30 ℃ the condition, generation contains the mixing solutions of saltpetre, rare nitric acid and hydrochloric acid, and the order number of Repone K is the 160-170 order; (2) the above-mentioned mixing solutions that obtains is cooled to normal temperature, continues to be refrigerated to-5 ℃ then, and carry out centrifugation, obtain crude product saltpetre and contain a mother liquor of saltpetre, hydrochloric acid and rare nitric acid; (3) a crude product saltpetre is carried out obtaining finished product after the refinement treatment, dry then, packing gets final product, be that 0.01Mpa, temperature are to evaporate under 80 ℃ the condition and make a mother liquor be concentrated into 55 degree Beaume with mother liquor in negative pressure simultaneously, obtain comprising the mixed gas and the secondary crude product potassium nitrate solution of hydrochloric acid, rare nitric acid; (4) the secondary crude product potassium nitrate solution that obtains is cooled to normal temperature, continues to be refrigerated to 0 ℃ then, and carry out centrifugation, obtain secondary crude product saltpetre and the secondary mother liquid that contains a small amount of saltpetre, hydrochloric acid and rare nitric acid; (5) secondary crude product saltpetre is carried out obtaining finished product after the refinement treatment, dry then, packing gets final product, and simultaneously secondary mother liquid is returned evaporation, enrichment process in the step (3), to recycle.With evaporable Mixed Gas Condensation to 50 in the mixed gas that comprises hydrochloric acid, rare nitric acid that obtains in the step (3) and the reaction process ℃, obtain comprising the mixing acid of hydrochloric acid and rare nitric acid, extract with tributyl phosphate then, obtain rare nitric acid and hydrochloric acid respectively, rare nitric acid recycles as the reaction raw materials retrieval system, and hydrochloric acid is carried through rectifying and is used to produce 30% technical hydrochloric acid after dense.
Embodiment 4:
A kind of potassium nitrate preparing technology, may further comprise the steps: (1) is that rare nitric acid of 35% is 1: 1.45 mixed according to mol ratio with Repone K and concentration, in negative pressure is that 0.015Mpa, temperature are to react under 35 ℃ the condition, generation contains the mixing solutions of saltpetre, rare nitric acid and hydrochloric acid, and the order number of Repone K is 165 orders; (2) the above-mentioned mixing solutions that obtains is cooled to normal temperature, continues to be refrigerated to-3 ℃ then, and carry out centrifugation, obtain crude product saltpetre and contain a mother liquor of saltpetre, hydrochloric acid and rare nitric acid; (3) a crude product saltpetre is carried out obtaining finished product after the refinement treatment, dry then, packing gets final product, be that 0.02Mpa, temperature are to evaporate under 76 ℃ the condition and make a mother liquor be concentrated into 52 degree Beaume with mother liquor in negative pressure simultaneously, obtain comprising the mixed gas and the secondary crude product potassium nitrate solution of hydrochloric acid, rare nitric acid; (4) the secondary crude product potassium nitrate solution that obtains is cooled to normal temperature, continues to be refrigerated to-2 ℃ then, and carry out centrifugation, obtain secondary crude product saltpetre and the secondary mother liquid that contains a small amount of saltpetre, hydrochloric acid and rare nitric acid; (5) secondary crude product saltpetre is carried out obtaining finished product after the refinement treatment, dry then, packing gets final product, and simultaneously secondary mother liquid is returned evaporation, enrichment process in the step (3), to recycle.With evaporable Mixed Gas Condensation to 43 in the mixed gas that comprises hydrochloric acid, rare nitric acid that obtains in the step (3) and the reaction process ℃, obtain comprising the mixing acid of hydrochloric acid and rare nitric acid, extract with tributyl phosphate then, obtain rare nitric acid and hydrochloric acid respectively, rare nitric acid recycles as the reaction raw materials retrieval system, and hydrochloric acid is carried through rectifying and is used to produce 30% technical hydrochloric acid after dense.
Embodiment 5:
A kind of potassium nitrate preparing technology, may further comprise the steps: (1) is that rare nitric acid of 38% is 1: 1.48 mixed according to mol ratio with Repone K and concentration, in negative pressure is that 0.02Mpa, temperature are to react under 37 ℃ the condition, generation contains the mixing solutions of saltpetre, rare nitric acid and hydrochloric acid, and the order number of Repone K is 162 orders; (2) the above-mentioned mixing solutions that obtains is cooled to normal temperature, continues to be refrigerated to-4 ℃ then, and carry out centrifugation, obtain crude product saltpetre and contain a mother liquor of saltpetre, hydrochloric acid and rare nitric acid; (3) a crude product saltpetre is carried out obtaining finished product after the refinement treatment, dry then, packing gets final product, be that 0.01Mpa, temperature are to evaporate under 72 ℃ the condition and make a mother liquor be concentrated into 54 degree Beaume with mother liquor in negative pressure simultaneously, obtain comprising the mixed gas and the secondary crude product potassium nitrate solution of hydrochloric acid, rare nitric acid; (4) the secondary crude product potassium nitrate solution that obtains is cooled to normal temperature, continues to be refrigerated to-5 ℃ then, and carry out centrifugation, obtain secondary crude product saltpetre and the secondary mother liquid that contains a small amount of saltpetre, hydrochloric acid and rare nitric acid; (5) secondary crude product saltpetre is carried out obtaining finished product after the refinement treatment, dry then, packing gets final product, and simultaneously secondary mother liquid is returned evaporation, enrichment process in the step (3), to recycle.With evaporable Mixed Gas Condensation to 48 in the mixed gas that comprises hydrochloric acid, rare nitric acid that obtains in the step (3) and the reaction process ℃, obtain comprising the mixing acid of hydrochloric acid and rare nitric acid, extract with tributyl phosphate then, obtain rare nitric acid and hydrochloric acid respectively, rare nitric acid recycles as the reaction raw materials retrieval system, and hydrochloric acid is carried through rectifying and is used to produce 30% technical hydrochloric acid after dense.
Claims (2)
1. potassium nitrate preparing technology is characterized in that may further comprise the steps:
(1) be that rare nitric acid of 30-40% is 1 according to mol ratio with Repone K and concentration: the mixed of 1.4-1.5 is that 0.01-0.02MPa, temperature are to react under 30-40 ℃ the condition in negative pressure, generates the mixing solutions that contains saltpetre, rare nitric acid and hydrochloric acid;
(2) the above-mentioned mixing solutions that obtains is cooled to normal temperature, continues to be refrigerated to 0～-5 ℃ then, and carry out centrifugation, obtain a crude product saltpetre and a mother liquor;
(3) a crude product saltpetre is carried out obtaining finished product after the refinement treatment, be that 0.01-0.02MPa, temperature are to evaporate under 70-80 ℃ the condition and make a mother liquor be concentrated into the 50-55 degree Beaume with mother liquor in negative pressure simultaneously, obtain comprising the mixed gas and the secondary crude product potassium nitrate solution of hydrochloric acid, rare nitric acid; The Mixed Gas Condensation that comprises hydrochloric acid, rare nitric acid that will obtain then is to 40-50 ℃, obtain comprising the mixing acid of hydrochloric acid and rare nitric acid, extract with tributyl phosphate then, obtain rare nitric acid and hydrochloric acid respectively, rare nitric acid recycles as the raw material retrieval system of reaction;
(4) the secondary crude product potassium nitrate solution that obtains is cooled to normal temperature, continues to be refrigerated to 0～-5 ℃ then, and carry out centrifugation, obtain secondary crude product saltpetre and secondary mother liquid;
(5) secondary crude product saltpetre is carried out obtaining finished product after the refinement treatment, simultaneously secondary mother liquid is returned evaporation, enrichment process in the step (3), to recycle.
2. potassium nitrate preparing technology according to claim 1, the order number that it is characterized in that Repone K is the 160-170 order.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101854485A CN101182014B (en) | 2007-12-15 | 2007-12-15 | Preparation technique of potassium nitrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101854485A CN101182014B (en) | 2007-12-15 | 2007-12-15 | Preparation technique of potassium nitrate |
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| Publication Number | Publication Date |
|---|---|
| CN101182014A CN101182014A (en) | 2008-05-21 |
| CN101182014B true CN101182014B (en) | 2010-09-15 |
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|---|---|---|---|
| CN2007101854485A Expired - Fee Related CN101182014B (en) | 2007-12-15 | 2007-12-15 | Preparation technique of potassium nitrate |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2477946A4 (en) * | 2009-06-25 | 2017-07-12 | IMI Tami Institute For Research And Development Ltd. | Polyhalite imi process for kno3 production |
| CN103539167B (en) * | 2012-07-09 | 2015-07-15 | 虎尾科技大学 | Method of continuously purifying potassium nitrate in batch in waste generated by glass hardening process |
| CN103466664B (en) * | 2013-09-17 | 2015-07-08 | 蓝思科技股份有限公司 | Fully-automatic production line type potassium nitrate recovering process |
| CN105036158B (en) * | 2015-07-21 | 2017-01-18 | 四川大学 | Method for preparing sodium nitrate through solvent extraction |
| CN105439175A (en) * | 2015-12-30 | 2016-03-30 | 山东天一化学股份有限公司 | Method for directly producing potassium nitrate |
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