CN1056819C - Ion exchange process for producing potassium nitrate - Google Patents
Ion exchange process for producing potassium nitrate Download PDFInfo
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- CN1056819C CN1056819C CN96117207A CN96117207A CN1056819C CN 1056819 C CN1056819 C CN 1056819C CN 96117207 A CN96117207 A CN 96117207A CN 96117207 A CN96117207 A CN 96117207A CN 1056819 C CN1056819 C CN 1056819C
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Abstract
The present invention provides a process for producing potassium nitrate by ion-exchange resin. The process comprises the following steps of using industrial or agricultural ammonium nitrate and potassium chloride as raw materials and ion-exchange resin as exchange carriers, changing the sodium base of the raw materials into the kalium base, dissolving ammonium in forward flow and kalium in back flow, exchanging NH4<+> and K<+> for a solution containing ammonium nitrate, and effectively evaporating and once crystallizing a potassium nitrate solution obtained by exchange to obtain a potassium nitrate product with high purity. The process has the characteristics of cheap raw material, bland reaction conditions, low consumption, low energy consumption, low cost, high and stable product quality, good benefit, no pollution, etc., and the process is suitable for industrialization production in various scales.
Description
The invention relates to a method and a process for producing chemical raw materials or chemical fertilizers.
Potassium nitrate is an important inorganic chemical raw material and an agricultural high-efficiency binary chlorine-free compound ammonium fertilizer which is in domestic shortage. Prior to the present invention, there were generally four production methods for potassium nitrate.
Firstly, a conversion method: the double decomposition method is obtained by double decomposition of sodium nitrate and potassium chloride, has simple process flow, higher product quality and wide industrial application, but has higher production cost and low recovery value of the byproduct of the chlorax due to high compactness of sodium nitrate.
Secondly, an alkyl tertiary amine association displacement method (patent application No. 88105115.2, publication No. CN1040562A) or a method of extracting by-products of hydrogen chloride and unreacted nitric acid by using nitric acid and chlorinated water as raw materials and using an organic solvent (chemical production flow diagram, chemical industry Press, 6 months 1984). The by-product of the method is ammonium chloride, but the raw material part is added with ammonia or liquid ammonia (the latter is diluted hydrochloric acid), the equipment corrosion is serious, the process flow is long, and the product quality is low (KNO)3The content is 93.0-97.0%).
And thirdly, absorption method: the tail gas of nitric acid is absorbed by potassium carbonate or caustic potash solution, which is expensive and has high production cost, and is rarely used.
Fourthly, ammonium nitrate double decomposition method: the potassium nitrate and the ammonium chloride are subjected to double decomposition to obtain two products of agricultural grade potassium nitrate and ammonium chloride, but the industrial grade potassium nitrate and the ammonium chloride need to be subjected torecrystallization, the consumption is high, and equipment corrosion is serious when mixed mother liquor containing the ammonium nitrate, the ammonium chloride and the like is evaporated, so that the large-scale industrial production is less.
The invention aims to provide a process for producing potassium nitrate by an ion exchange method, which has the advantages of cheap and easily obtained raw materials, advanced process, short flow, low consumption, low energy consumption, high and stable product quality, basically realizes no discharge of three wastes and can realize large-scale industrial production.
The invention relates to a process for producing potassium nitrate by an ion exchange method, which adopts cation exchange resin as an exchange carrier, adopts industrial or agricultural ammonium nitrate and potassium chloride as raw materials, and carries out the ion exchange of potassium salt and ammonium salt under normal pressure to produce high-purity potassium nitrate by the following technical scheme. Namely:
1. transformation of ion exchange resin: the cation exchange resin is preferably a strongly acidic styrene cation exchange resin. Passing potassium salt water solution such as potassium chloride through sodium cation exchange resin layer to convert into potassium resin, wherein the ion exchange resin is K phase when K concentration in effluent is unchangedAnd (5) saturation and transformation are finished. The potassium, sodium salt solution remaining in the column was washed with water. The reaction formula is as follows: (wherein R represents an ion exchange resin, the same applies hereinafter)
2. Feeding ammonium in a concurrent manner: and (3) using a certain amount of ammonium nitrate solution with the temperature of-10-100 ℃ and the concentration of 5-90%, controlling the linear speed within 0.3-6 cm/min, enabling the ammonium nitrate solution to flow into the exchange column downstream to elute the potassium ion exchange resin, and eluting the potassium ion exchange resin with water at the same linear speed after the ammonium nitrate solution flows out until the potassium resin is changed into the ammonium resin. Collecting potassium nitrate exchange liquid with the concentration of 30g/L for material melting of ammonium nitrate.
3. And (4) countercurrent potassium feeding: the method is used for a potassium chloride solution with equivalent ammonium nitrate of 0-100 ℃ and 5-36.2% concentration, the control line speed is controlled within 0.3-6 cm/min, the solution is fed into an exchange column in a countercurrent mode, ammonium type ion exchange resin is regenerated, after potassium chloride flows out, the ammonium type ion exchange resin is regenerated by water at the same line speed until the ammonium type ion exchange resin is changed into potassium type resin. Collecting ammonium chloride exchange liquid with the concentration of more than 15 g/L; the ammonium chloride exchange solution with the concentration less than 15g/L is used for partially dissolving potassium chloride. The reaction formula is as follows:
the concurrent feeding of ammonium and the countercurrent feeding of potassium are preferably controlled within the exchange capacity of the ion exchange resin, and the continuous and repeated operation can continuously obtain potassium nitrate and ammonium chloride solutions.
Compared with the prior art, the invention has the following advantages:
1. advanced process, short flow, high product quality and stability.
2. The raw materials are cheap and easy to obtain, the reaction is complete, the consumption is low, the utilization rate of the raw materials is improved by 5 percent, and the cost is low.
3. And by adopting equipment such as a multi-effect evaporator, high-efficiency crystallization and the like, the energy consumption is greatly reduced, and the energy is saved by more than 20%.
4. Basically realizes no three-waste discharge.
In the ion exchange process, the low-concentration potassium nitrate obtained by forward flow ammonium feeding and water washing is used for preparing the ammonium nitrate chemical material, the low-concentration ammonium chloride obtained by reverse flow potassium feeding and water washing is used for preparing part of potassium chloride chemical material, and the part of potassium chloride passes through the ammonium type ion exchange resin layer before potassium feeding, so that the closed cycle of the process is realized. Therefore, the three wastes are basically not discharged.
5. The economic benefit is remarkable.
FIG. 1 is a flow chart of a process for producing potassium nitrate by an ion exchange method.
The embodiment of the invention comprises the following steps:
dissolving potassium
1. 400Kg of potassium chloride per batch is put into a potassium melting pool according to the formula requirements, 1372.3Kg of water is added, and the potassium chloride is stirred to be completely dissolved to prepare a solution with the yield of 22.57% (the potassium solution can also adopt other soluble inorganic potassium salt solutions containing potassium ions with equivalent amount, such as potassium nitrate, potassium sulfate and other potassium solutions).
2. Weighing 2.5Kg potassium carbonate (K)2CO3) Dissolving with 1Kg of potassium hydroxide (KOH) in appropriate amount of water, gradually injecting into a potassium bath, stirring, controlling pH to 10-11 to remove calcium and magnesium ions, clarifying, and filtering.
3. Standing and clarifying. And detecting whether the contents of calcium and magnesium ions are qualified or not.
4. Pumping clear and transparent potassium chloride filtrate into a potassium chloride head tank for later use.
Ammonium salt of di (di)
1. 429.4 Kg/batch of ammonium nitrate is weighed and put into an ammonium dissolving pool, 1522.4Kg of water is added, and the solution with the yield of 22% is stirred and dissolved.
2. Standing for clarification and filtering.
3. Pumping the filtrate into an ammonium nitrate head tank for later use.
Ion exchange
1. Counter-current potassium feeding
(1) Feeding the potassium chloride solution into an exchange column in a countercurrent manner, and controlling the linear velocity within 1-2 cm/min.
(2) After the potassium chloride solution is added, water is sent in a countercurrent way at the same linear velocity until the concentration of effluent liquid at an outlet is 0, and ammonium chloride exchange liquid with the concentration of more than 15g/l is collected; ammonium chloride exchange solution with a concentration of less than 15g/l was used for partial potassiumchloride digestion.
(3) Rinsing the resin bed layer with deionized water for about 1h, and testing CL with silver nitrate (AgNO3)-And(4) whether the product is qualified.
2. Concurrent ammonium addition
(1) The ammonium nitrate solution flows into the exchange column downstream, and the line speed is controlled within 2-3 cm/min.
(2) After the ammonium nitrate solution is added and the speed is reduced, the potassium type ion exchange resin is leached by water at the same linear speed until the concentration of effluent liquid is 0, and potassium nitrate exchange liquid with the concentration of more than 30g/l is collected; the potassium nitrate exchange liquid with the concentration less than 30g/l is used for the material dissolving of the ammonium nitrate.
Fourthly, evaporation and concentration
In the evaporation concentration process, a normal pressure or vacuum method is adopted, and the liquid temperature is controlled within the range of 40-116 ℃ until the liquid is concentrated to 45 ℃ Be'.
Fifthly, crystallization and centrifugation
1. Cooling with cooling water to obtain concentrated solution, cooling for crystallization, and centrifuging when the temperature of crystallization mother liquor is reduced to below 35 deg.C.
2. After the liquid is removed by the centrifugal machine, the machine is stopped after the mother liquid flows out and continues to centrifuge for 2-3 minutes.
Sixthly, drying
And (4) centrifugally separating the crystals, and drying the crystals by a dryer to obtain the finished product.
Product of seven, potassium nitrate
The potassium nitrate exchange liquid prepared by exchange is subjected to multi-effect evaporation concentration at 40-120 ℃ and-0.09-1 Mpa until the specific gravity is 1.4g/cm2And then cooling to-15-40 ℃, crystallizing for the first time, separating and drying to obtain 99.6% industrial first-grade potassium nitrate or 99.8% military potassium nitrate products.
Ammonium chloride product
And (3) carrying out multi-effect evaporation and concentration on the exchanged ammonium chloride exchange solution at 40-116 ℃ and-0.09-1 Mpa until the specific gravity is 1.2g/cm, cooling to 15-40 ℃, carrying out primary crystallization, separating and drying to obtain a 99.3% industrial first-grade ammonium chloride product.
Ninth, the ion exchange method is used for producing industry and can also produce products such as potassium carbonate, potassium bicarbonate, sodium nitrate, potassium dihydrogen phosphate, potassium sulfate and the like.
Claims (2)
1. A process for preparing potassium nitrate by ion exchange method, which is to prepare potassium nitrate solution by ion exchange resin, then to obtain high-purity potassium nitrate product by multi-effect vacuum evaporation concentration, crystallization, separation and drying, is characterized in that:
(1) adopting cation exchange resin, transforming before use, and placing in an exchange column in any way;
(2) carrying out concurrent ammonium feeding and countercurrent potassium feeding;
(3) preparing potassium nitrate solution by adopting ammonium nitrate solution with the temperature of-10 to 100 ℃ and the concentration of 5 to 90 percent;
(4) adding potassium chloride solution with concentration of 5-36.2% at 0-100 deg.C to obtain ammonium chloride solution;
(5) the linear speed of the ammonium on the forward flow is controlled within 0.3-6 cm/min, and the potassium on the reverse flow is controlled within 0.3-6 cm/min.
2. The process for producing potassium nitrate by the ion exchange method according to claim 1, which is characterized in that: the amount of co-current ammonium or counter-current potassium is controlled within the exchange capacity of the ion exchange resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96117207A CN1056819C (en) | 1996-12-06 | 1996-12-06 | Ion exchange process for producing potassium nitrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96117207A CN1056819C (en) | 1996-12-06 | 1996-12-06 | Ion exchange process for producing potassium nitrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1184077A CN1184077A (en) | 1998-06-10 |
| CN1056819C true CN1056819C (en) | 2000-09-27 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN96117207A Expired - Fee Related CN1056819C (en) | 1996-12-06 | 1996-12-06 | Ion exchange process for producing potassium nitrate |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102951661A (en) * | 2011-08-19 | 2013-03-06 | 交城县并盛化工有限公司 | Production method of potassium nitrate |
| CN102585779B (en) * | 2011-11-18 | 2014-02-05 | 牟邦志 | Preparation method of high-purity heat-conduction energy storage molten salt |
| CZ2013234A3 (en) | 2013-03-28 | 2014-06-04 | Membrain S.R.O. | Process for preparing potassium nitrate by employing electrodialysis method and apparatus for making the same ya |
| CN104876248B (en) * | 2015-05-15 | 2016-09-14 | 中南大学 | A kind of method preparing potassium sulfate co-production ammonium chloride |
| CN105905928B (en) * | 2016-05-03 | 2017-11-07 | 四川福思达生物技术开发有限责任公司 | A kind of handling process for preparing waste liquid during 3,6 dichlorosalicylic acids |
| CN106219581A (en) * | 2016-07-22 | 2016-12-14 | 中国科学院青海盐湖研究所 | A kind of method utilizing selection absorption method to prepare magnesium nitrate |
| CN107140660B (en) * | 2017-07-20 | 2018-05-04 | 台山市化工厂有限公司 | A kind of preparation method of potassium carbonate |
| CN109384251A (en) * | 2018-12-12 | 2019-02-26 | 青海盐湖工业股份有限公司 | A kind of prilling process of potassium nitrate and its potassium nitrate granules of preparation |
| CN109437247A (en) * | 2018-12-21 | 2019-03-08 | 滑县大潮林物产有限责任公司 | Potassium carbonate recovery method in the production of super capacitor carbon |
| CN111111793B (en) * | 2020-01-02 | 2023-09-19 | 黎明化工研究设计院有限责任公司 | Ion exchange device and application thereof in preparation of hydroxylamine nitrate or hydroxylamine perchlorate |
| 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5110578A (en) * | 1989-10-05 | 1992-05-05 | Monomeros Colombo Venezolanos, S.A. (E.M.A.) | Continuous production of potassium nitrate via ion exchange |
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1996
- 1996-12-06 CN CN96117207A patent/CN1056819C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5110578A (en) * | 1989-10-05 | 1992-05-05 | Monomeros Colombo Venezolanos, S.A. (E.M.A.) | Continuous production of potassium nitrate via ion exchange |
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| CN1184077A (en) | 1998-06-10 |
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