CN1765746A - Method for making potassium nitrate using magnesium hydroxide circular reaction method - Google Patents
Method for making potassium nitrate using magnesium hydroxide circular reaction method Download PDFInfo
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- CN1765746A CN1765746A CN 200510099753 CN200510099753A CN1765746A CN 1765746 A CN1765746 A CN 1765746A CN 200510099753 CN200510099753 CN 200510099753 CN 200510099753 A CN200510099753 A CN 200510099753A CN 1765746 A CN1765746 A CN 1765746A
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Abstract
This invention discloses a method to prepare potassium nitrate and ammonium chloride by nitric acid, potassium chloride and ammonia. Wherein, with cycling magnesium hydroxide, mixing nitric acid, magnesium hydroxide, and potassium chloride to react; cooling, crystallizing, centrifugal separating, drying, and obtaining potassium nitrate; adding ammonia to the mother liquid of potassium nitrate to generate magnesium hydroxide deposition for cycling and ammonium chloride solution to obtain crystal. This technique is convenient to operation without pollution.
Description
1, technical field
The present invention relates to a kind of is the technical field that raw material is produced saltpetre and produced ammonium chloride with nitric acid, Repone K and ammonia.
2, technical background
At present, China's Production of Potassium Nitrate method mainly is to be raw material with ammonium nitrate and Repone K, adopts ion exchange method or preparing potassium nitrate by means of double decomposition.
Ion exchange method is that Klorvess Liquid and ammonium nitrate solution are alternately passed through ion exchange resin, obtains potassium nitrate solution and ammonium chloride solution respectively, obtains desired product through evaporation concentration, crystallisation by cooling, drying then.This law product solution concentration is low, evaporation energy consumption height, and the byproduct ammonium chloride solution is little because of concentration, corrosion is big, reclaims difficulty.
Double decomposition is to be raw material with ammonium nitrate and Repone K, adopts the replacement(metathesis)reaction legal system to get saltpetre, pays and produces ammonium chloride product.Practice shows, though this method technology and equipment are simple, pollution-free, technology maturation, it is prosperous to pay the product ammonium chloride market requirement, but this method has the following disadvantages: the first, raw material ammonium nitrate belongs to the dangerous and explosive articles of national stringent regulations control, and supply is restricted with transportation, price is high, causes Production of Potassium Nitrate cost height; The second, in the replacement(metathesis)reaction process, 50% left and right sides potassium ion of only having an appointment in the reaction soln is converted into saltpetre, and the Recycling Mother Solution amount is bigger in the production process, and evaporated quantity of water is also higher, and equipment and process cost are also high, cause the production cost height.
Therefore researching and developing new raw material route and modern technique, to produce saltpetre be an important topic.The object of the present invention is to provide a kind ofly can overcome the insufficient new production saltpetre method of above technology, technology is simple, and is easy to operate, totally-enclosed closed cycle production, and the no three wastes produce.
3, summary of the invention
With nitric acid, Repone K and ammonia is that raw material reaction is produced saltpetre and ammonia chloride craft, at first be in salpeter solution, to add magnesium hydroxide to mix with Repone K and react, mainly be that magnesium nitrate is produced in the reaction of nitric acid and magnesium hydroxide, emit a large amount of heats simultaneously, its chemical equation is as follows:
The reaction liberated heat raises solution temperature, accelerate the Repone K dissolving simultaneously, then solution is cooled, because saltpetre is along with temperature reduces, its solubleness sharply descends, and magnesium chloride solubleness is little along with temperature decline rangeability, therefore, solution temperature constantly reduces, and magnesium nitrate and Repone K complex decomposition reactive crystallization are separated out potassium nitrate crystals, generate magnesium chloride solution simultaneously, its chemical equation is as follows:
Then the saltpetre feed liquid is sent from the scheming centrifugation and gets saltpetre and mother liquor I, separate to such an extent that saltpetre is finished product saltpetre after drying.Major ingredient is magnesium chloride and minute quantity saltpetre among the mother liquor I, adds ammoniacal liquor in solution, sinks reactive magnesium under agitation condition, and reaction generates magnesium hydrate precipitate, and heavy reactive magnesium chemical equation is as follows:
In order to make strainability magnesium hydroxide preferably, in heavy reactive magnesium process, in solution, add an amount of magnesium oxide powder earlier, the MgO of adding is slightly soluble in water, and reaction equation is as follows:
MgO and the Mg (OH) that reacts generation
2As crystal seed in the heavy reactive magnesium process, also be simultaneously the loss amount that replenishes magnesium in the technological cycle process.And then add high-polymerization degree anion-polyacrylamide (being called for short PAM) and as flocculation agent, magnesium hydroxide is had coagulation effect preferably, can accelerate precipitation and filtration velocity so greatly, the flocculation agent add-on is to add the 10-20 gram in the 100kg solution.
Describe content of the present invention below in detail:
1. in reactor, the salpeter solution of adding 25% to 45%, under continuous agitation condition, slowly adding magnesium hydroxide and Repone K miscellany again in the salpeter solution in reactor reacts, reactant ratio is: nitric acid: Repone K: magnesium hydroxide=1: 1: 0.5 (mol ratio), temperature of reaction is controlled to be 70-95 ℃, and the solution pH value is controlled to be 5-7; Generate magnesium nitrate and Repone K mixed solution after reaction is finished, send strainer to remove by filter impurity solution.
The solution that 2. will remove by filter impurity send in the cooling crystallizer, make solution temperature be reduced to-15 to 0 ℃ by cooling or freezing mode, a large amount of potassium nitrate crystals are separated out in crystallization in the solution, then the saltpetre feed liquid is sent from the scheming, get saltpetre and mother liquor I through centrifugation, separate to such an extent that saltpetre send drying machine to be finished product saltpetre after drying.
3. mother liquor I major ingredient is a magnesium chloride, mother liquor I is sent in the heavy magnesium device, under continuous agitation condition, in mother liquor I, add magnesium oxide powder, the magnesium oxide add-on is the 10-20% of magnesium chloride mole number in the solution, slowly feeding concentration in solution again is the ammoniacal liquor of 15-25%, reaction generates magnesium hydrate precipitate, the ammonia add-on is the 200-240% of magnesium chloride mole number in the solution, feed in the ammoniacal liquor process, add the anion-polyacrylamide flocculation agent simultaneously, it is 10-20g/100kg solution that flocculation agent adds concentration, and flocculation agent concentration is 0.01-0.02% in the ie in solution.Feed in the ammoniacal liquor reaction process, control solution pH value is 10, and temperature of reaction 30-70 ℃, reaction times 2-5 hour, solution reaction generated the magnesium hydrate precipitate that particle is big, the filtration washing performance is good.
4. will contain magnesium hydrate precipitate solution be sent from scheming centrifuging separate magnesium hydrate precipitate and the mother liquor II of the about 15-35% of water content, recycle with Repone K is mixed during 1. magnesium hydrate precipitate returns, participate in circulating reaction.Major ingredient is an ammonium chloride among the mother liquor II, and minute quantity saltpetre and magnesium chloride.
5. mother liquor II send in the vaporizer with returning mother liquor III, is 70% to 75% through evaporation concentration to terminal point concentration, again evaporation concentration liquid is sent and cool 30-50 ℃ in the cooling crystallizer, ammonia chloride crystal is separated out in crystallization, separate out and contain a small amount of magnesium salts and sylvite in the ammonia chloride crystal, so can be described as nitrogen potassium magnesium compound fertilizer again, be sent from the scheming centrifugation then and get ammonium chloride and mother liquor III, separation mother liquor III returns to send in the vaporizer with mother liquor II and recycles.
With Repone K, nitric acid, ammonia is main raw material, produces saltpetre and ammonia chloride craft flow diagram as shown in Figure 1.
4, invention advantage
The present invention has following advantage:
The first, main raw material Repone K, nitric acid, the ammonia of the present invention's employing are all cheap and easy to get, and raw materials cost is low, for Production of Potassium Nitrate provides a good raw material route.
The second, technical process of the present invention is simple, easy to operate, totally-enclosed closed cycle production, and all mother liquors all circulate and participate in reaction, finally all are converted into product, and therefore, raw material availability is higher, and energy consumption is low, and production cost is low.
Three, the present invention utilizes magnesium hydroxide as the intermediate reaction thing, magnesium hydroxide recycles in solution all the time and reacts, make each step reaction carry out comparatively fully, potassium ion is converted into potassium nitrate crystals basically in the solution, thereby saves process cost in the technological process.
Four, product saltpetre quality of the present invention reaches requirement, contains KNO
3〉=96.0%, Cl≤1.0%, moisture content≤1.0% meets agricultural saltpetre standard and requirement, and further purification can get industrial potassium nitrate; Ammonium chloride contains N 〉=18.80%, K
2O≤3.80%, MgO≤6.60%, moisture content≤5.0% meets agrochemical standard and requirement, is a kind of nitrogen potassium magnesium compound fertilizer of the market requirement.
Five, the present invention does not have " three wastes " generation, environmentally safe.
5, description of drawings:
Fig. 1 is a technological process block-diagram of the present invention.
6, embodiment:
Embodiment 1: in 1000 kilogram 25% salpeter solution, gradual slow adds 165 kilograms of moisture 30% magnesium hydroxides, 300 kilograms in Repone K (〉=98%, following quality all with), and continuous stirring reaction, temperature of reaction is controlled to be 70 ℃, and the solution pH value is 5; After reaction is finished, solution is removed by filter impurity, cool-15 ℃ again, then the centrifugation of saltpetre feed liquid is got saltpetre and mother liquor I, separate to such an extent that saltpetre send drying machine to be finished product saltpetre after drying, contain KNO
3〉=97.25%, Cl≤0.80%, moisture content≤0.92%.Under continuous agitation condition, in mother liquor I, add magnesium oxide powder (MgO 〉=90%, following quality all with) 9 kilograms, slowly in solution, add concentration again and be 15% ammoniacal liquor reaction, add 0.1 kilogram of anion-polyacrylamide flocculation agent simultaneously, control solution reaction temperature is 70 ℃, and control solution pH value is 10,2 hours reaction times.To contain magnesium hydrate precipitate solution be sent from scheming centrifuging separate the magnesium hydrate precipitate and the mother liquor II of water content 32%, magnesium hydrate precipitate is used for embodiment 2 to be used, mother liquor II is 70% through evaporation concentration to terminal point concentration, again the evaporation concentration liquid cooling is but cooled to 30 ℃, ammonium chloride is separated out in crystallization, be sent from the scheming centrifugation then and get ammonium chloride and mother liquor III, ammonium chloride contains N 〉=19.52%, K
2O≤3.22%, MgO≤4.21%, moisture content≤4.52% separates mother liquor III and is used for embodiment 2 uses.
Embodiment 2: in 555 kilogram 45% salpeter solution, gradual slow adds the magnesium hydroxide among the embodiment 1,300 kilograms in Repone K, continuous stirring reaction, temperature of reaction is controlled to be 95 ℃, after reaction is finished, solution is removed by filter impurity, cool 0 ℃ again, then the centrifugation of saltpetre feed liquid is got saltpetre and mother liquor I, separate to such an extent that saltpetre send drying machine to be finished product saltpetre after drying, contain KNO
3〉=96.13%; Under continuous agitation condition, in mother liquor I, add 18 kilograms of magnesium oxide powders, slowly adding concentration again in solution is the reaction of 25% ammoniacal liquor, adds 0.2 kilogram of anion-polyacrylamide flocculation agent simultaneously, control solution reaction temperature is 30 ℃; Control solution pH value is 10,5 hours reaction times.To contain magnesium hydrate precipitate solution be sent from scheming centrifuging separate magnesium hydrate precipitate and mother liquor II, magnesium hydrate precipitate is used for embodiment 3 to be used, mother liquor III is mixed among mother liquor II and the embodiment 1, is 75% through evaporation concentration to terminal point concentration, again the evaporation concentration liquid cooling is but cooled to 50 ℃, be sent from the scheming centrifugation then and get ammonium chloride and mother liquor III, ammonium chloride contains N 〉=18.88%, K
2O≤3.80%, MgO≤6.55% separates mother liquor III and is used for embodiment 3 uses.
Embodiment 3: in 700 kilogram 36% salpeter solution, gradual slow adds the magnesium hydroxide among the embodiment 2,310 kilograms in Repone K, continuous stirring reaction, temperature of reaction is controlled to be 95 ℃, after reaction is finished, solution is removed by filter impurity, cool-10 ℃ again, then the centrifugation of saltpetre feed liquid is got saltpetre and mother liquor I, separate to such an extent that saltpetre send drying machine to be finished product saltpetre after drying, contain KNO
3〉=96.85%; Under continuous agitation condition, in mother liquor I, add 18 kilograms of magnesium oxide powders, slowly adding concentration again in solution is the reaction of 20% ammoniacal liquor, adds 0.1 kilogram of anion-polyacrylamide flocculation agent simultaneously, control solution reaction temperature is 40 ℃; Control solution pH value is 10,3 hours reaction times.To contain magnesium hydrate precipitate solution be sent from scheming centrifuging separate magnesium hydrate precipitate and mother liquor II, mother liquor III is mixed among mother liquor II and the embodiment 2, after evaporation concentration, be 75% to terminal point concentration, again the evaporation concentration liquid cooling is but cooled to 40 ℃, be sent from the scheming centrifugation then and get ammonium chloride and mother liquor III, ammonium chloride contains N 〉=18.85%, K
2O≤3.78%, MgO≤6.61%.
Claims (5)
1, a kind ofly produce the method for saltpetre, it is characterized in that may further comprise the steps with nitric acid, Repone K and ammonia:
1. magnesium hydroxide that adding is returned in salpeter solution and Repone K are mixed reacts, and after reaction is finished, solution is removed by filter impurity;
2. the solution crystallisation by cooling is separated out potassium nitrate crystals, then the saltpetre feed liquid is sent from the scheming centrifugation and gets saltpetre and mother liquor I, separate to such an extent that saltpetre is finished product saltpetre after drying;
3. in mother liquor I, add magnesium oxide powder, slowly feed the ammoniacal liquor that concentration is 15-25%, add the anion-polyacrylamide flocculation agent simultaneously, control solution pH value is 10, temperature of reaction 30-70 ℃, reaction times 2-5 hour, solution reaction generated magnesium hydrate precipitate;
4. will contain magnesium hydrate precipitate solution filtering separation and get magnesium hydrate precipitate and mother liquor II, mix the participation circulating reaction with Repone K during 1. magnesium hydrate precipitate returns;
5. mother liquor II send in the vaporizer with returning mother liquor III, is 70% to 75% through evaporation concentration to concentration, cool 30-50 ℃ again, ammonia chloride crystal is separated out in crystallization, be sent from the scheming centrifugation then and get ammonium chloride and mother liquor III, separate mother liquor III and return to send in the vaporizer and recycle with mother liquor II.
2, the described method of root a tree name claim 1, it is characterized in that adding in the magnesium hydroxide and Repone K reaction process that returns in the salpeter solution, salpeter solution concentration is 25-45%, reactant ratio is a nitric acid: Repone K: magnesium hydroxide=1: 1: 0.5 (mol ratio), temperature of reaction are controlled to be 70-95 ℃.
3, the described method of root a tree name claim 1 is characterized in that the solution crystallisation by cooling separates out in the potassium nitrate crystals process, and solution crystallisation by cooling terminal temperature is-15 ℃ to 0 ℃.
4, the described method of root a tree name claim 1 is characterized in that the magnesium oxide add-on is the 10-20% of magnesium chloride mole number among the mother liquor I among the mother liquor I.
5, the described method of root a tree name claim 1 is characterized in that adding the anion-polyacrylamide flocculant concentration and is controlled to be 0.01-0.02%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111204779A (en) * | 2020-03-10 | 2020-05-29 | 余荣华 | Fused salt production method for co-producing high-purity magnesium hydroxide, magnesium carbonate and nitrogen-potassium fertilizer |
| CN112897554A (en) * | 2021-02-04 | 2021-06-04 | 中国科学院过程工程研究所 | Method for preparing potassium nitrate and by-product crystalline aluminum chloride |
| CN112939032A (en) * | 2021-03-24 | 2021-06-11 | 江西金利达钾业有限责任公司 | Method for preparing potassium nitrate by nitric acid method |
| CN113233480A (en) * | 2021-06-29 | 2021-08-10 | 郭建文 | Magnesium refining slag recovery equipment and recovery process thereof |
| CN117088444A (en) * | 2023-08-28 | 2023-11-21 | 武汉天源环保股份有限公司 | High ammonia nitrogen organic wastewater treatment system and method |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109721082A (en) * | 2019-03-22 | 2019-05-07 | 青海爱能森新材料科技有限公司 | A kind of production method of high purity magnesium hydroxide and potassium nitrate coproduction |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1721016A1 (en) * | 1989-01-09 | 1992-03-23 | Государственный научно-исследовательский и проектный институт метанола и продуктов органического синтеза | Method of producing potassium nitrate |
| CN1043750C (en) * | 1995-08-31 | 1999-06-23 | 夏文建 | Process for producing potassium nitrate |
| IL135611A0 (en) * | 2000-04-12 | 2001-05-20 | Pipko Gregory | A process for the production of potassium nitrate |
| CN1194893C (en) * | 2001-05-29 | 2005-03-30 | 沈晃宏 | Three-step circular metathesis process of producing potassium nitrate |
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- 2005-09-06 CN CNB2005100997533A patent/CN1302992C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111204779A (en) * | 2020-03-10 | 2020-05-29 | 余荣华 | Fused salt production method for co-producing high-purity magnesium hydroxide, magnesium carbonate and nitrogen-potassium fertilizer |
| CN112897554A (en) * | 2021-02-04 | 2021-06-04 | 中国科学院过程工程研究所 | Method for preparing potassium nitrate and by-product crystalline aluminum chloride |
| CN112939032A (en) * | 2021-03-24 | 2021-06-11 | 江西金利达钾业有限责任公司 | Method for preparing potassium nitrate by nitric acid method |
| CN113233480A (en) * | 2021-06-29 | 2021-08-10 | 郭建文 | Magnesium refining slag recovery equipment and recovery process thereof |
| CN117088444A (en) * | 2023-08-28 | 2023-11-21 | 武汉天源环保股份有限公司 | High ammonia nitrogen organic wastewater treatment system and method |
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