CN1083034A - The production method of ammonium potassium dihydrogen phosphate - Google Patents
The production method of ammonium potassium dihydrogen phosphate Download PDFInfo
- Publication number
- CN1083034A CN1083034A CN 92108206 CN92108206A CN1083034A CN 1083034 A CN1083034 A CN 1083034A CN 92108206 CN92108206 CN 92108206 CN 92108206 A CN92108206 A CN 92108206A CN 1083034 A CN1083034 A CN 1083034A
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- CN
- China
- Prior art keywords
- ammonium
- controlled
- dihydrogen phosphate
- repone
- phosphate
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B13/00—Fertilisers produced by pyrogenic processes from phosphatic materials
- C05B13/06—Alkali and alkaline earth meta- or polyphosphate fertilisers
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- Organic Chemistry (AREA)
- Fertilizers (AREA)
Abstract
A kind of production method of ammonium potassium dihydrogen phosphate comprises following technical process: 1. be the feedstock production ammonium dihydrogen phosphate with the phosphoric acid by wet process; 2. primary ammonium phosphate and Repone K metathesis; 3. crystallisation by cooling; 4. centrifugation; 5. dry.When ammonium dihydrogen phosphate and Repone K metathesis, Repone K: primary ammonium phosphate=0.7～1,50 ℃～80 ℃ of temperature of reaction, crystallisation by cooling temperature-10 °～30 ℃.Method provided by the invention has been widened raw material sources, helps the development and use of China's phosphate rock resource, and product contains N＞5%, P
2O
5＞50%, K
2O＞18%, total recovery rate has reached 60～80%, and cl content is less than 2%, production cost reduces by 20～30%.
Description
The invention belongs to high-concentration fertilizer and make the field, relate to a kind of production method of ammonium potassium dihydrogen phosphate.
The suitability for industrialized production ammonium potassium dihydrogen phosphate mainly contains two kinds of methods at present: a kind of is with preparing primary ammonium phosphate with thermal phosphoric acid in the bicarbonate of ammonia, then primary ammonium phosphate and Repone K being carried out metathesis and obtain ammonium potassium dihydrogen phosphate; Another kind is to be raw material with agricultural ammonium phosphate, with its water extraction, gets its extraction liquid and Repone K reaction production ammonium potassium dihydrogen phosphate.The weak point of above-mentioned two kinds of methods is that raw materials cost is higher, causes the cost height of product.
The objective of the invention is to overcome the deficiencies in the prior art, providing a kind of is the method for raw material production ammonium potassium dihydrogen phosphate with phosphoric acid by wet process, to reduce production costs, widens the starting material source, makes full use of china natural resources.
Phosphoric acid by wet process is directly by phosphorus ore extraction and obtain, and more in view of the mid low grade phosphate rock of China, so the content of impurity is also more in the phosphoric acid by wet process, and its major impurity is silicofluoric acid (H
2SiF
6), aluminium sesquioxide (Al
2O
3), ferric oxide (Fe
2O
3) and magnesium oxide (MgO).At the characteristics of phosphoric acid by wet process, method provided by the present invention comprises following technical process:
1, with the phosphoric acid by wet process is the feedstock production ammonium dihydrogen phosphate
The operation of this flow process is defluorinate, filtration, neutralization, filtration and concentrates.
The defluorinate of phosphoric acid by wet process adds Repone K or sodium sulfate, makes silicofluoric acid generate potassium silicofluoride (sodium) precipitation and removes.Required by defluorinate, the add-on of potassium hydride KH is that 100～140%(is by stoichiometry), the add-on of sodium sulfate is that 120～160%(is by stoichiometry), temperature of reaction is controlled at 25 °～50 ℃.
Filtering for the first time is to remove potassium silicofluoride or Sodium Silicofluoride, can adopt centrifugal separation.
Neutralization is under agitation to feed gas ammonia in filtrate, and the pH value of solution value is controlled at 3.0～5.0.This operation can form primary ammonium phosphate, the also further removal of impurity, and in this kind basic solution, Fe
++, Al
++, Mg
++The phosphoric acid salt that can generate Deng impurity and precipitating.
Filtering for the second time is to remove Fe
++, Al
++, Mg
++Deng the phosphoric acid salt that impurity generates, adopt vacuum filtration or centrifuging, filter residue can send phosphorus ammonium Workshop Production ammophos.
Concentrating is to remove water unnecessary in the filtrate, makes the water content in the ammonium dihydrogen phosphate just in time satisfy metathetic requirement, and this is one critical process, and it directly has influence on the carrying out of next flow process.Through repetition test, the content of primary ammonium phosphate should be controlled at 40～60% in the solution.
2, primary ammonium phosphate and Repone K metathesis
This flow process is will solid potassium chloride directly to add to concentrate in the good ammonium dihydrogen phosphate and under agitation carry out, and the add-on of Repone K is according to Repone K (Kcl): primary ammonium phosphate (NH
4H
2PO
4)=0.7～1(mol ratio) calculates, but, only be applicable to the Repone K that purity is high according to the determined Repone K add-on of following formula,, then need after suitable purifying treatment, to press earlier following formula and calculate for impure more Repone K (as agricultural potassium chloride).Metathetic temperature of reaction is controlled at 50 °～80 ℃.
3, crystallisation by cooling
The Tc of this flow process is controlled at-10 °～30 ℃, and cooling rate is controlled at 0.3 °～3 ℃/minute, stops 0.5～1 hour in Tc during crystallization.
4, centrifugation
This flow process is that the ammonium potassium dihydrogen phosphate precipitation is separated with mother liquor, and isolated mother liquor can be used as other multiple fertile raw material, also can directly be condensed into the multiple fertilizer of solid nitrogen potassium phosphorus.
5, drying
The present invention has the following advantages:
1, compare with existing method, cost can reduce by 20～30%.
2, go out ammonium potassium dihydrogen phosphate with impure more Wet-process Phosphoric Acid Production, help the development and use of China's phosphate rock resource, widened the starting material source.
3, determined the optimum concn of ammonium dihydrogen phosphate and the add-on of Repone K, the product that metathesis is obtained has reached 60～80% recovery rates, and cl content meets the requirement of no chlorine fertilizer less than 2%.
Fig. 1 is a process flow sheet of the present invention.
Embodiment:
The composition of used phosphoric acid by wet process is: P
2O
522%, F1.0%, Al
2O
30.86%, MgO 0.85%, Fe
2O
30.25%.
Get 1000 kilograms of phosphoric acid by wet processes, add the required Repone K of defluorinate by stoichiometry 120%, in 50 ℃ of reactions, precipitation, the elimination potassium silicofluoride, the feeding gas ammonia is till the pH=3.5 in filtrate, and vacuum filtration calcium phosphate precipitation impurity contains NH with filtrate being concentrated to
4H
2PO
440% is standby.
At 70 ℃, slowly add Repone K under constantly stirring, reach Kcl: NH
4H
2PO
4After=0.7 promptly the speed with 1 ℃/minute cool to 25 ℃ of Tcs, and insulated and stirred 0.5 hour.At last with the ammonium potassium dihydrogen phosphate centrifugation of separating out and be drying to obtain 220 kilograms of products.Contain N5%, P in the product
2O
554%, K
2O18%, Cl＜2%.
Claims (3)
1, a kind of production method of ammonium potassium dihydrogen phosphate, technical process comprises primary ammonium phosphate and Repone K metathesis, crystallisation by cooling, centrifugation and drying, the crystallisation by cooling temperature is controlled at-10 °～30 ℃, cooling rate is controlled at 0.3 °～3 ℃/minute, stopped 0.5～1 hour in Tc during crystallization, it is characterized in that:
(1) preparation of ammonium dihydrogen phosphate is a raw material with the phosphoric acid by wet process that contains plurality of impurities, its operation is defluorinate, filtration, neutralization, filtration and concentrates, in and the time ammonification, pH value is controlled at 3.0～5.0, when concentrated in the solution content of primary ammonium phosphate be controlled at 40～60%.
(2) will solid potassium chloride directly add and concentrate in the good ammonium dihydrogen phosphate and under agitation carry out metathesis, its add-on is according to Repone K (KCl): primary ammonium phosphate (NH
4H
2PO
4Calculate)=0.7～1 (mol ratio), and temperature of reaction is controlled at 50 °～80 ℃.
2, production method according to claim 1 is characterized in that adding the Repone K defluorinate, and its add-on is that 100～140%(is by stoichiometry), temperature of reaction is controlled at 25 °～50 ℃.
3, production method according to claim 1 is characterized in that adding the sodium sulfate defluorinate, and its add-on is that 120～160%(is by stoichiometry), temperature of reaction is controlled at 25 °～50 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92108206 CN1083034A (en) | 1992-07-13 | 1992-07-13 | The production method of ammonium potassium dihydrogen phosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92108206 CN1083034A (en) | 1992-07-13 | 1992-07-13 | The production method of ammonium potassium dihydrogen phosphate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1083034A true CN1083034A (en) | 1994-03-02 |
Family
ID=4943328
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 92108206 Pending CN1083034A (en) | 1992-07-13 | 1992-07-13 | The production method of ammonium potassium dihydrogen phosphate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1083034A (en) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343206B (en) * | 2008-09-05 | 2011-05-04 | 中国-阿拉伯化肥有限公司 | Process for preparing circular particle kalium based fertilizer |
| CN103011122A (en) * | 2012-12-28 | 2013-04-03 | 山东金正大生态工程股份有限公司 | Method for producing water-soluble potassium ammonium phosphate from wet-process phosphoric acid |
| CN103030129A (en) * | 2012-12-28 | 2013-04-10 | 贵州金正大生态工程有限公司 | Method for producing water-soluble ammonium potassium phosphate fertilizer with wet-method phosphoric acid |
| CN103641574A (en) * | 2013-12-25 | 2014-03-19 | 黄明科 | Method for producing chemically synthesized water soluble fertilizer |
| CN104386664A (en) * | 2014-10-30 | 2015-03-04 | 成都化工股份有限公司 | Method for producing ammonium potassium dihydrogen phosphate from fertilizer grade ammonium dihydrogen phosphate |
| CN104744175A (en) * | 2015-04-03 | 2015-07-01 | 武汉工程大学 | Method for producing nitrogen-phosphorus-potassium mixed fertilizer by utilizing phosphorus-potassium associated ore |
| CN105000539A (en) * | 2015-08-17 | 2015-10-28 | 四川大学 | Method for producing potassium dihydrogen phosphate and potassium-ammonium dihydrogen phosphate through wet process phosphoric acid |
| CN105149016A (en) * | 2015-10-29 | 2015-12-16 | 黄尚勋 | Method for achieving replacement reaction through resin-free autologous bed ion exchange method |
| CN105174237A (en) * | 2015-09-22 | 2015-12-23 | 贵州开磷集团股份有限公司 | Method for preparing sodium dihydrogen phosphate by means of phosphoric acid obtained by wet process |
| CN107161968A (en) * | 2017-05-31 | 2017-09-15 | 攀枝花火凤凰再生资源回收利用有限责任公司 | The method of comprehensive utilization of potassium in a kind of sintering flue dust |
| CN107720713A (en) * | 2017-10-29 | 2018-02-23 | 贵阳开磷化肥有限公司 | A kind of method that phosphoric acid by wet process prepares ammonium dihydrogen phosphate co-production potassium dihydrogen phosphate |
| CN115490541A (en) * | 2022-11-22 | 2022-12-20 | 云南缁磷工业技术有限公司 | Method for continuously producing ammonium potassium phosphate |
-
1992
- 1992-07-13 CN CN 92108206 patent/CN1083034A/en active Pending
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343206B (en) * | 2008-09-05 | 2011-05-04 | 中国-阿拉伯化肥有限公司 | Process for preparing circular particle kalium based fertilizer |
| CN103030129B (en) * | 2012-12-28 | 2015-04-08 | 贵州金正大生态工程有限公司 | Method for producing water-soluble ammonium potassium phosphate fertilizer with wet-method phosphoric acid |
| CN103011122A (en) * | 2012-12-28 | 2013-04-03 | 山东金正大生态工程股份有限公司 | Method for producing water-soluble potassium ammonium phosphate from wet-process phosphoric acid |
| CN103030129A (en) * | 2012-12-28 | 2013-04-10 | 贵州金正大生态工程有限公司 | Method for producing water-soluble ammonium potassium phosphate fertilizer with wet-method phosphoric acid |
| CN103011122B (en) * | 2012-12-28 | 2014-08-20 | 金正大生态工程集团股份有限公司 | Method for producing water-soluble potassium ammonium phosphate from wet-process phosphoric acid |
| CN103641574B (en) * | 2013-12-25 | 2016-03-30 | 黄明科 | A kind of production method of chemosynthesis water-soluble fertilizer |
| CN103641574A (en) * | 2013-12-25 | 2014-03-19 | 黄明科 | Method for producing chemically synthesized water soluble fertilizer |
| CN104386664A (en) * | 2014-10-30 | 2015-03-04 | 成都化工股份有限公司 | Method for producing ammonium potassium dihydrogen phosphate from fertilizer grade ammonium dihydrogen phosphate |
| CN104386664B (en) * | 2014-10-30 | 2016-02-17 | 成都化工股份有限公司 | The method of ammonium potassium dihydrogen phosphate produced by fertilizer grade primary ammonium phosphate |
| CN104744175A (en) * | 2015-04-03 | 2015-07-01 | 武汉工程大学 | Method for producing nitrogen-phosphorus-potassium mixed fertilizer by utilizing phosphorus-potassium associated ore |
| CN104744175B (en) * | 2015-04-03 | 2017-09-29 | 武汉工程大学 | The method that nitrogen-phosphorus-potassium compound fertilizer is produced using phosphorus potassium associated minerals |
| CN105000539A (en) * | 2015-08-17 | 2015-10-28 | 四川大学 | Method for producing potassium dihydrogen phosphate and potassium-ammonium dihydrogen phosphate through wet process phosphoric acid |
| CN105174237A (en) * | 2015-09-22 | 2015-12-23 | 贵州开磷集团股份有限公司 | Method for preparing sodium dihydrogen phosphate by means of phosphoric acid obtained by wet process |
| CN105149016A (en) * | 2015-10-29 | 2015-12-16 | 黄尚勋 | Method for achieving replacement reaction through resin-free autologous bed ion exchange method |
| CN107161968A (en) * | 2017-05-31 | 2017-09-15 | 攀枝花火凤凰再生资源回收利用有限责任公司 | The method of comprehensive utilization of potassium in a kind of sintering flue dust |
| CN107720713A (en) * | 2017-10-29 | 2018-02-23 | 贵阳开磷化肥有限公司 | A kind of method that phosphoric acid by wet process prepares ammonium dihydrogen phosphate co-production potassium dihydrogen phosphate |
| CN107720713B (en) * | 2017-10-29 | 2020-11-20 | 贵阳开磷化肥有限公司 | Method for preparing ammonium dihydrogen phosphate and co-producing potassium dihydrogen phosphate by wet-process phosphoric acid |
| CN115490541A (en) * | 2022-11-22 | 2022-12-20 | 云南缁磷工业技术有限公司 | Method for continuously producing ammonium potassium phosphate |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |