CN100475700C - Potassium nitrate preparing technology - Google Patents
Potassium nitrate preparing technology Download PDFInfo
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- CN100475700C CN100475700C CNB2007100621717A CN200710062171A CN100475700C CN 100475700 C CN100475700 C CN 100475700C CN B2007100621717 A CNB2007100621717 A CN B2007100621717A CN 200710062171 A CN200710062171 A CN 200710062171A CN 100475700 C CN100475700 C CN 100475700C
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Abstract
The invention relates to a kind of technique field of inorganic chemical industry, which is a kind of preparation craft of niter. To solve such problems existing preparation craft of niter as that sources of raw material is restricted, production cost and energy consumption is high and quality of products is inferior, the invention uses potassium chloride and dilute nitric acid react to form potassium chloride, dilute nitric acid, niter and hydrochloric acid, take a great of hydrochloric acid and nitric acid out through distillation, then heat and concentrate them to make the mixture turn into saturated solution which becomes neutral when put into sodium carbonate and regulated, the solution reacts with surplus little hydrochloric acid and form sodium chloride at the same time. Finally, it separates niter out making use of different solubility of niter, sodium chloride and potassium chloride at the same temperature. Sources of raw material in this invention are extensive, the production cost is relatively low; Operations such as chemistry reaction, distillation and concentration are finished at the same reaction equipment, process of operation goes on under normal atmosphere and save investment of equipment; it is easy to operate and separate; get finished product using method of mechanism filter-pressing, it is simple to operate with little investment.
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 and the metathesis crystallization process of raw material with Repone K and ammonium nitrate, their common drawback is to adopt ammonium nitrate as raw material, because ammonium nitrate has explosivity, it is the main raw material of making native explosive, so country expressly limits its use range, so that the raw material sources of above-mentioned two kinds of methods are restricted, simultaneously the ammonium nitrate price is higher, general per ton is about 1500 yuan, use cost is higher, and the byproduct ammonium chloride recovery difficult that generates is big, is easy to production unit is caused corrosion, introduces ammonium ion in the raw material simultaneously, can make the water absorbability index of finished product saltpetre not reach standard-required, product easily lumps.Be one step of the metathesis extraction process and the nitric acid conversion methdo of raw material for another example with Repone K and nitric acid, though solved above-mentioned two kinds of a series of problems that process using ammonium nitrate is brought, raw material sources are extensive, production cost is lower, it is organic solvent that but there is employed extraction agent in one step of metathesis extraction process, to the toxic effect of human body, the content of byproduct hydrochloric acid is on the low side simultaneously, is difficult to problems such as sale; And be disclosed a kind of the utilization in the technology that nitric acid conversion methdo produces saltpetre in 92106421 the patent application in the patent No., the problem of its existence is that mother liquor contains a large amount of saltpetre in the sepn process, must extract through circulation just can obtain, and therefore disposable finished product yield is lower, cause energy consumption height, cost height, because a large amount of Recycling Mother Solution are used, cause batching inaccurate, influence reaction process, increased operation easier, the sepn process complexity, product purity is lower, is unfavorable for suitability for industrialized production.For these reasons, press at present a kind of raw material sources extensively, production cost is lower, sepn process is simple and quality product saltpetre preparation method preferably.
Summary of the invention
The present invention provides a kind of potassium nitrate preparing technology for problems such as solving existing saltpetre preparation method and have that raw material sources are restricted, production cost is higher, energy consumption is high and quality product is relatively poor.
The present invention adopts following technical scheme to realize: potassium nitrate preparing technology, may further comprise the steps: (1) is that rare nitric acid of 20-40% is 1 according to mol ratio with Repone K and concentration: the mixed of 1.05-1.4, under normal pressure, temperature is to react under 60-90 ℃ the condition, generates the mixing solutions that contains Repone K, rare nitric acid, saltpetre and hydrochloric acid; (2) be to distill under 80-95 ℃ the condition the above-mentioned mixing solutions that obtains in temperature, isolate the hydrochloric acid that contains nitric acid, because hydrochloric acid and nitric acid have easy volatile, so that greatly the hydrochloric acid of part and the remaining a small amount of nitric acid of reaction become gas and volatilize in the mixing solutions, obtain thick potassium solution, comprise the hydrochloric acid of Repone K, saltpetre and minute quantity in this thick potassium solution; (3) the above-mentioned thick potassium solution that obtains is continued to heat to 95-110 ℃, concentrate and obtain thick potassium saturated solution, add the yellow soda ash neutralization then, make this saturated solution be neutral, yellow soda ash and hydrochloric acid reaction generate sodium-chlor simultaneously, the dosage of yellow soda ash is determined by the residual content of hydrochloric acid in the thick potassium solution, is comprised saltpetre, Repone K and sodium-chlor in the mixed solution that this step obtains; (4) be to concentrate under 120-130 ℃ the condition the mixed solution that obtains in the step (3) in temperature, when potassium nitrate content reaches 580-750g/L in the supersaturated solution, precipitated sodium chloride and potassium chloride, remove sodium-chlor and Repone K through press filtration, obtain potassium nitrate solution, this step is to reach and separate with sodium-chlor, the different solubility of Repone K under same temperature according to saltpetre; (5) potassium nitrate solution that obtains is cooled to normal temperature, centrifuge dehydration, oven dry obtain finished product saltpetre.
The present invention is according to 1.
Chemical equation is produced saltpetre, and foundation is HCl+NaCO 2.
3→ NaCl+CO
2Remove micro-hydrochloric acid in the saltpetre.
Because 1. chemical equation is reversible reaction, carry out to the direction that generates saltpetre in order to make this reaction, the present invention has taked following way:
When 1, reacting, add excessive rare nitric acid, improve concentration of reactants;
2, distill simultaneously in reactor, the hydrochloric acid that reaction is generated is converted into the hydrogen chloride gas discharge;
3, 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 60-90 ℃.
Repone K raw material of the present invention can be buied from Salt Lake Industry, Qinghai group at least, 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 | 99.5-99.8 |
| 2 | Moisture | ≤0.10 | 0.05-0.08 |
| 3 | Chlorion (Cl -) | ≤0.020 | 0.01-0.015 |
| 4 | Water-insoluble | ≤0.020 | 0.015-0.018 |
| 5 | Sulfate ion (SO 4 2-) | ≤0.010 | 0.007-0.008 |
| 6 | Rate of moisture absorption | ≤0.30 | 0.15-0.25 |
Can find out from last table, the every index of the saltpetre that the present invention makes all near or be better than national standard.
Compared with prior art, the present invention has the following advantages:
(1) raw material sources are extensive, and production cost is lower, compare with other technologies, and cost reduces by 1000 yuan/ton;
(2) finish operations such as chemical reaction, evaporation concentration simultaneously in same conversion unit, all operations process is all carried out under normal pressure, does not need pressure exerting device, has saved facility investment;
(3) separation method that adopts of the present invention easy to operate, be easy to separate, effectively reduce Recycling Mother Solution, avoided the side reaction generation, reduce steam output, reduce processes such as washing finished product, improved yield of product;
(4) adopt method of mechanism filter-pressing to obtain the saltpetre finished product, less investment, simple to operate, and can thoroughly separate with sodium-chlor, Repone K, guaranteed the quality of saltpetre;
(5) owing to there is not the introducing of ammonium ion in the raw material, product water absorbability index does not need special control can reach standard-required, the product prevented from caking,
In a word, the saltpetre that the present invention makes is widely used in making fireworks, black powder, opticglass, special glass etc. industrial, and as fertilizer sources is mainly used in fields such as tobacco, cash crop, gardening simultaneously.
Embodiment
Embodiment 1:
Potassium nitrate preparing technology, may further comprise the steps: (1) is that rare nitric acid of 20% is 1: 1.05 mixed according to mol ratio with Repone K and concentration, under normal pressure, temperature is to react under 60 ℃ the condition, generates the mixing solutions that contains Repone K, rare nitric acid, saltpetre and hydrochloric acid; (2) be to distill under 80 ℃ the condition the above-mentioned mixing solutions that obtains, isolate the hydrochloric acid that contains nitric acid, obtain thick potassium solution in temperature; (3) the above-mentioned thick potassium solution that obtains is continued to heat to 95 ℃, concentrate and obtain thick potassium saturated solution, add the yellow soda ash neutralization then and make this saturated solution be neutral, yellow soda ash and hydrochloric acid reaction generate sodium-chlor simultaneously; (4) be to concentrate under 120 ℃ the condition in temperature with the mixed solution that obtains in the step (3), when potassium nitrate content reached 580g/L in the supersaturated solution, precipitated sodium chloride and potassium chloride were removed sodium-chlor and Repone K through press filtration, obtain potassium nitrate solution; (5) potassium nitrate solution that obtains is cooled to normal temperature, centrifuge dehydration, oven dry obtain finished product saltpetre.
Embodiment 2:
Potassium nitrate preparing technology, may further comprise the steps: (1) is that rare nitric acid of 40% is 1: 1.4 mixed according to mol ratio with Repone K and concentration, under normal pressure, temperature is to react under 90 ℃ the condition, generates the mixing solutions that contains Repone K, rare nitric acid, saltpetre and hydrochloric acid; (2) be to distill under 95 ℃ the condition the above-mentioned mixing solutions that obtains, isolate the hydrochloric acid that contains nitric acid, obtain thick potassium solution in temperature; (3) the above-mentioned thick potassium solution that obtains is continued to heat to 110 ℃, concentrate and obtain thick potassium saturated solution, add the yellow soda ash neutralization then and make this saturated solution be neutral, yellow soda ash and hydrochloric acid reaction generate sodium-chlor simultaneously; (4) be to concentrate under 130 ℃ the condition in temperature with the mixed solution that obtains in the step (3), when potassium nitrate content reached 750g/L in the supersaturated solution, precipitated sodium chloride and potassium chloride were removed sodium-chlor and Repone K through press filtration, obtain potassium nitrate solution; (5) potassium nitrate solution that obtains is cooled to normal temperature, centrifuge dehydration, oven dry obtain finished product saltpetre.
Embodiment 3:
Potassium nitrate preparing technology, may further comprise the steps: (1) is that rare nitric acid of 30% is 1: 1.2 mixed according to mol ratio with Repone K and concentration, under normal pressure, temperature is to react under 70 ℃ the condition, generates the mixing solutions that contains Repone K, rare nitric acid, saltpetre and hydrochloric acid; (2) be to distill under 85 ℃ the condition the above-mentioned mixing solutions that obtains, isolate the hydrochloric acid that contains nitric acid, obtain thick potassium solution in temperature; (3) the above-mentioned thick potassium solution that obtains is continued to heat to 105 ℃, concentrate and obtain thick potassium saturated solution, add the yellow soda ash neutralization then and make this saturated solution be neutral, yellow soda ash and hydrochloric acid reaction generate sodium-chlor simultaneously; (4) be to concentrate under 125 ℃ the condition in temperature with the mixed solution that obtains in the step (3), when potassium nitrate content reached 620g/L in the supersaturated solution, precipitated sodium chloride and potassium chloride were removed sodium-chlor and Repone K through press filtration, obtain potassium nitrate solution; (5) potassium nitrate solution that obtains is cooled to normal temperature, centrifuge dehydration, oven dry obtain finished product saltpetre.
Embodiment 4:
Potassium nitrate preparing technology, may further comprise the steps: (1) is that rare nitric acid of 35% is 1: 1.3 mixed according to mol ratio with Repone K and concentration, under normal pressure, temperature is to react under 80 ℃ the condition, generates the mixing solutions that contains Repone K, rare nitric acid, saltpetre and hydrochloric acid; (2) be to distill under 90 ℃ the condition the above-mentioned mixing solutions that obtains, isolate the hydrochloric acid that contains nitric acid, obtain thick potassium solution in temperature; (3) the above-mentioned thick potassium solution that obtains is continued to heat to 98 ℃, concentrate and obtain thick potassium saturated solution, add the yellow soda ash neutralization then and make this saturated solution be neutral, yellow soda ash and hydrochloric acid reaction generate sodium-chlor simultaneously; (4) be to concentrate under 128 ℃ the condition in temperature with the mixed solution that obtains in the step (3), when potassium nitrate content reached 700g/L in the supersaturated solution, precipitated sodium chloride and potassium chloride were removed sodium-chlor and Repone K through press filtration, obtain potassium nitrate solution; (5) potassium nitrate solution that obtains is cooled to normal temperature, centrifuge dehydration, oven dry obtain finished product saltpetre.
Embodiment 5:
Potassium nitrate preparing technology, may further comprise the steps: (1) is that rare nitric acid of 25% is 1: 1.35 mixed according to mol ratio with Repone K and concentration, under normal pressure, temperature is to react under 75 ℃ the condition, generates the mixing solutions that contains Repone K, rare nitric acid, saltpetre and hydrochloric acid; (2) be to distill under 93 ℃ the condition the above-mentioned mixing solutions that obtains, isolate the hydrochloric acid that contains nitric acid, obtain thick potassium solution in temperature; (3) the above-mentioned thick potassium solution that obtains is continued to heat to 102 ℃, concentrate and obtain thick potassium saturated solution, add the yellow soda ash neutralization then and make this saturated solution be neutral, yellow soda ash and hydrochloric acid reaction generate sodium-chlor simultaneously; (4) be to concentrate under 122 ℃ the condition in temperature with the mixed solution that obtains in the step (3), when potassium nitrate content reached 685g/L in the supersaturated solution, precipitated sodium chloride and potassium chloride were removed sodium-chlor and Repone K through press filtration, obtain potassium nitrate solution; (5) potassium nitrate solution that obtains is cooled to normal temperature, centrifuge dehydration, oven dry obtain finished product saltpetre.
Claims (1)
1, a kind of potassium nitrate preparing technology is characterized in that may further comprise the steps:
(1) be that rare nitric acid of 20-40% is 1 according to mol ratio with Repone K and concentration: the mixed of 1.05-1.4, under normal pressure, temperature is to react under 60-90 ℃ the condition, generates the mixing solutions that contains Repone K, rare nitric acid, saltpetre and hydrochloric acid;
(2) be to distill under 80-95 ℃ the condition the above-mentioned mixing solutions that obtains, isolate the hydrochloric acid that contains nitric acid, obtain thick potassium solution in temperature;
(3) the above-mentioned thick potassium solution that obtains is continued to heat to 95-110 ℃, concentrate and obtain thick potassium saturated solution, add the yellow soda ash neutralization then, make this saturated solution be neutral, yellow soda ash and hydrochloric acid reaction generate sodium-chlor simultaneously;
(4) be to concentrate under 120-130 ℃ the condition the mixed solution that obtains in the step (3) in temperature, when potassium nitrate content reaches 580-750g/L in the supersaturated solution, precipitated sodium chloride and potassium chloride are removed sodium-chlor and Repone K through press filtration, obtain potassium nitrate solution;
(5) potassium nitrate solution that obtains is cooled to normal temperature, centrifuge dehydration, oven dry obtain finished product saltpetre.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100621717A CN100475700C (en) | 2007-06-14 | 2007-06-14 | Potassium nitrate preparing technology |
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|---|---|---|---|
| CNB2007100621717A CN100475700C (en) | 2007-06-14 | 2007-06-14 | Potassium nitrate preparing technology |
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| CN101070167A CN101070167A (en) | 2007-11-14 |
| CN100475700C true CN100475700C (en) | 2009-04-08 |
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| CNB2007100621717A Expired - Fee Related CN100475700C (en) | 2007-06-14 | 2007-06-14 | Potassium nitrate preparing technology |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103130248A (en) * | 2013-03-06 | 2013-06-05 | 昆明理工大学 | Method for preparing potassium salt from biomass fuel boiler ash |
| CN107128953A (en) * | 2017-06-19 | 2017-09-05 | 青海盐湖工业股份有限公司 | A kind of method for producing fused salt level potassium nitrate |
| CN107601532A (en) * | 2017-10-25 | 2018-01-19 | 安徽胜达化工科技有限公司 | A kind of method of coproduction technical grade potassium nitrate and complex fertilizer |
| CN108046270A (en) * | 2017-12-14 | 2018-05-18 | 江西渠成氟化学有限公司 | A kind of recovery and treatment method of nitration mixture |
| CN111410938A (en) * | 2020-01-21 | 2020-07-14 | 山西沃锦新材料股份有限公司 | Binary molten salt and preparation method thereof |
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