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CN1045085A - Production method of potassium dihydrogen phosphate and potassium sulfate - Google Patents

Production method of potassium dihydrogen phosphate and potassium sulfate Download PDF

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Publication number
CN1045085A
CN1045085A CN 89106858 CN89106858A CN1045085A CN 1045085 A CN1045085 A CN 1045085A CN 89106858 CN89106858 CN 89106858 CN 89106858 A CN89106858 A CN 89106858A CN 1045085 A CN1045085 A CN 1045085A
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China
Prior art keywords
fertilizer
mother liquor
repone
ammonium
tartar
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Pending
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CN 89106858
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Chinese (zh)
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门伟
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Individual
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Individual
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Priority to CN 89106858 priority Critical patent/CN1045085A/en
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Abstract

In the production, firstly, fertilizer ammonium nitrate, fertilizer potassium chloride, industrial salt, tap water and fertilizer ammonium dihydrogen phosphate are used to prepare circulating solution, then the circulating solution is circularly acted with fertilizer potassium chloride, fertilizer ammonium dihydrogen phosphate or fertilizer ammonium sulfate and sodium chloride to produce potassium dihydrogen phosphate or potassium sulfate and fertilizer ammonium chloride as by-product.

Description

The production method of potassium primary phosphate, vitriolate of tartar
Knownly produce the production method of potassium primary phosphate with biphosphate ammonium fertilizer and Repone K fertilizer, the yield of its product potassium primary phosphate is: 60~65%, and its ammonium chloride byproduct reclaims through evaporation concentration by separating mother liquor.
The known fertilizer ammonium sulfate of using, fertilizer Repone K is produced the production method of vitriolate of tartar, is to adopt ammonia circulating process potassium sulfate making, and it separates mother liquor and reclaims the ammonium chloride byproduct through evaporation concentration.
The product yield of the production method of existing potassium primary phosphate is lower, and needs evaporation concentration to reclaim byproduct.
The objective of the invention is to improve with the fertilizer monoammonium phosphate, fertilizer Repone K is produced the product yield of potassium primary phosphate, and reclaims the ammonium chloride byproduct at normal temperatures.
The objective of the invention is to simplify to fall to have now with ammonium sulfate fertilizer, Repone K fertilizer is produced the ammonia circulating process of vitriolate of tartar, and reclaims the ammonium chloride byproduct at normal temperatures.
Implementation method of the present invention is as follows:
1. preparation circulate soln:
With fertilizer ammonium nitrate, fertilizer Repone K, industrial table salt, tap water, fertilizer primary ammonium phosphate or fertilizer ammonium sulfate, press column weight amount proportioning, mixed, be heated to 50~70 ℃ and react:
Fertilizer ammonium nitrate: 1100~730 parts; Fertilizer Repone K: 560~310 parts; Industrial table salt: 800~530 parts; 1000 parts in tap water; The fertilizer primary ammonium phosphate: 130 parts, or fertilizer ammonium sulfate: 60 parts.
The chemical equation of reaction is:
Reacted 30~60 minutes, and be cooled to 23~25 ℃, separate the KNO that contains that generates 3, NH 4The precipitation of Cl promptly gets the NaNO that contains that will prepare 3Circulate soln,
2. with circulate soln cyclic production potassium primary phosphate or vitriolate of tartar and ammonium chloride:
(1) with circulate soln and Repone K fertilizer effect precipitated sodium chloride:
1 circulate soln of being prepared is added fertilizer Repone K, and heat temperature raising is with the NaNO in the circulate soln 3Following reaction takes place:
Reaction conditions is:
1. the charging capacity of fertilizer Repone K: 185~125 grams per liters.
2. temperature of reaction: 50~70 ℃, the reaction times: 30~60 minutes.
After reaction finishes, separate and use after the NaCl that generates is left to, will separate mother liquor and be cooled to 35~40 ℃, separate the KCl crystallization that generates, separate mother liquor and enter next step production, use after isolated KCI is left to.
(2) produce potassium primary phosphate or vitriolate of tartar with circulating mother liquor:
The separation mother liquor that to produce in (1) adds biphosphate ammonium fertilizer or ammonium sulfate fertilizer, and following reaction takes place:
Reaction conditions is:
1. the charging capacity of fertilizer phosphoric acid=hydrogen ammonium: 205~115 grams per liters,
Or the charging capacity of fertilizer ammonium sulfate: 120~65 grams per liters,
2. temperature of reaction: 40~45 ℃, the reaction times: 30~60 minutes; Be cooled to 28~32 ℃ after reaction finishes, after reaction finishes, separate the crystal that generates, be potassium primary phosphate or potassium product, separate mother liquor and be used to produce ammonium chloride:
(3) produce ammonium chloride with circulating mother liquor:
To produce in (1) isolating NaCL and put into production in (2) isolating circulating mother liquor, following reaction will take place:
Reaction conditions is:
(1) charging capacity of sodium-chlor: for producing 1.02~1.05 times of isolated NaCL weight in (1).
(2) temperature of reaction: 28~32 ℃, reacted 30~60 minutes, after finishing, reaction is cooled to 23~25 ℃.
After reaction finishes, separate the NH that generates 4The CL precipitation is byproduct fertilizer ammonium chloride.
So far, produce and finished a circulation, this circulation separates NH 4Mother liquor behind the CL drops into Repone K fertilizer (comprising isolating Repone K in the production (1)) again and produces by the method for (1), (2), (3) again, so constantly repeats, and finishes the successive production process.
Example:
1. preparation circulate soln:
Fertilizer ammonium nitrate, fertilizer Repone K, industrial table salt, tap water, fertilizer primary ammonium phosphate or fertilizer ammonium sulfate are pressed mixed, the dissolving of column weight amount proportioning, are heated to 60 ℃, react:
Ammonium nitrate: 816 grams; Repone K: 340.2 grams; Salt: 600 grams; Tap water: 900 grams; Phosphoric acid=hydrogen ammonium: 117 grams or ammonium sulfate 54 grams.
Reacted 30 minutes, and after reaction finishes, be cooled to 23 ℃, isolate and contain KNO 3, NH 4Precipitation 726 grams or 666 grams of CL must separate 1430 milliliters in mother liquor, and this mother liquor is circulate soln.
2. carry out the cyclic production first time:
(1) separate out NaCl with circulate soln and the effect of fertilizer Repone K:
Fertilizer Repone K (KCl that contains 98% weight) 143 grams per liter solution 204.5 are restrained totally, drop in 1 circulate soln of being prepared, be warming up to 60 ℃, reacted 30 minutes, separate the NaCl precipitation, get 84 grams, be cooled to 37 ℃, separate the KCl crystallization, get 58 grams, 1460 milliliters in mother liquor.
(2) produce potassium primary phosphate or vitriolate of tartar:
(purified contains the NH of 97% weight to add the fertilizer primary ammonium phosphate 4H 2PO 4) 155.5 grams per liters totally 227 grams, in producing (1) mother liquor after separating KCl, keep 40 ℃ of reactions 30 minutes, be cooled to 28 ℃, separate the KH that separates out 2PO 4Crystallization gets 262.5 grams, 1435 milliliters in mother liquor.
Or: add the fertilizer ammonium sulfate ((NH that contains 98% weight 4) 2SO 4) 89.2 grams totally 130 grams, in producing (1) mother liquor after separating KCl, keep 40 ℃ of reactions 30 minutes, be cooled to 28 ℃, separate the K that separates out 2SO 4Crystallization gets 155 grams, 1435 milliliters in mother liquor.
(3) produce ammonium chloride:
Add the isolated NaCl of production (1), and excessive 2% 86 restrain in producing (2) isolating mother liquor totally, keep 28 ℃ of reactions 30 minutes, be cooled to 23 ℃, separate the NH that generates 4The Cl precipitation gets 124 grams, 1400 milliliters in mother liquor.
3. carry out the cyclic production second time:
(1) separate out NaCl with circulating mother liquor and the effect of fertilizer Repone K:
The production (3) that will circulate separates NH 4Mother liquor behind the Cl adds fertilizer Repone K, and it measures 152.5 grams per liters totally 214 grams (comprising circulation one production (1) isolating KCl crystallization), is warming up to 65 ℃, reacts 30 minutes, after reaction finishes, separate the NaCl precipitation, get 78 grams, be cooled to 37 ℃, separate the KCl crystallization, get 68 grams, 1455 milliliters in mother liquor.
(2) produce potassium primary phosphate or vitriolate of tartar:
Add fertilizer primary ammonium phosphate 155.5 grams per liters in totally 226 mother liquors that restrain after this cyclic production (1) is separated KCl, keep 40 ℃ of reactions 30 minutes, be cooled to 28 ℃, separate KH 2PO 4Crystal gets 253 grams, 1435 milliliters in mother liquor.
Or: add fertilizer ammonium sulfate 89.2 grams per liters in totally 130 mother liquors that restrain after this cyclic production (1) is separated KCl, keep 40 ℃ of reactions 30 minutes, be cooled to 28 ℃, separate K 2SO 4Crystal gets 155 grams, 1435 milliliters in mother liquor.
(3) produce ammonium chloride:
Add the isolated NaCl of this cyclic production (1), and excessive 2.5% 75 restrain in producing (2) isolating mother liquor totally, keep 28 ℃ of reactions 30 minutes, be cooled to 23 ℃, separate the NH that generates 4The Cl precipitation gets 120 grams, 1400 milliliters in mother liquor.
Later cyclic production is just undertaken by the method for circulation two.
4. production effect:
The production of circulation two:
The product potassium primary phosphate corresponding to the yield of raw material primary ammonium phosphate is: 94.4%
Product K H 2PO 4Content be: the 97.4%(butt), meet agricultural quality standard,
The product vitriolate of tartar is 97.6% corresponding to the yield of raw material sulphuric acid ammonium
K in the product 2SO 4Content be: the 98.5%(butt), meet agricultural quality standard.
The content of NaCl is in the byproduct ammonium chloride: 1.8%, meet the agricultural fertilizer standard.
Potassium primary phosphate is a kind of water-soluble no chlorine phospho potash complex fertilizer that contains high component nutrient for plants, has good performance, physicochemical property are stable, salt index is low, can not burn during use leaf or the root system of crop, its dilute solution is usually used in foliage fertilization, also be the raw material of obtaining liq fertilizer, but, fail on the agricultural at present to widely apply because production cost is higher than other chemical fertilizer, the existing the simplest method of potassium primary phosphate of producing, be neutralisation, but cost is very high, in addition with phosphoric acid and potassium hydroxide or salt of wormwood direct reaction, also has the preparation method of directly removing HCL with the Repone K and the phosphatase reaction of cheapness, but, do not obtain satisfied result so far, the double decomposition close with the inventive method owing to the severe corrosive of reaction medium under the high temperature and the disproportionation under the high temperature, be to carry out metathesis, again at NH with Repone K and primary ammonium phosphate 4-KH 2PO 4-H 2The O system phase diagram is isolated potassium primary phosphate, but yield is not high, and need high temperature evaporation to reclaim the ammonium chloride byproduct, with method of the present invention can be raw material with fertilizer Repone K cheap and easy to get and biphosphate ammonium fertilizer, simply, produce potassium primary phosphate with high yield, and reclaim the ammonium chloride byproduct at normal temperatures, its production technique is simple, production cost is low, can obtain the production cost close with other fertilizer, is a kind of Perfected process of production potassium dihydrogen phosphate product, enforcement of the present invention, can be simply, mass production is potassium primary phosphate cheaply, satisfies the demand of agricultural sector, has significant industry and economic results in society.
Vitriolate of tartar is a potash fertilizer kind maximum except that the chlorination potassic fertilizer, is used for happiness potassium fear-chlorion crops such as tobacco, potato, beet, grape in a large number.China does not have the production of this fertilizer for a long time, in a large number from external import, expend huge foreign exchange, with ammonium sulfate fertilizer and Repone K fertilizer is the traditional technology of raw material production vitriolate of tartar, need the ammonia circulating process to produce vitriolate of tartar, and need high temperature evaporation to concentrate recovery ammonium chloride byproduct, and its complex manufacturing, production cost is higher.Use method of the present invention, can simplify the deammoniation circulating process, and reclaim the ammonium chloride byproduct at normal temperatures, its production technique is simple, and energy consumption is few, and production cost is low, be a kind of with fertilizer ammonium sulfate, fertilizer Repone K is the Perfected process of raw material production vitriolate of tartar, and enforcement of the present invention can be simply, mass production vitriolate of tartar cheaply, substituting import one satisfies the demand of agricultural sector, has significant industry and economic results in society.
Realize that process flow of the present invention has been a mode as described in the accompanying drawing, its worker:
1. prepare the circulate soln operation:
With fertilizer ammonium nitrate a, fertilizer Repone K B, industrial table salt D, tap water C, fertilizer primary ammonium phosphate A or fertilizer ammonium sulfate C drop in the reactive tank 1, react through metering, mixing, heating by aforementioned preparation circulate soln method partly, after reaction finishes, separate the precipitation that generates with pressure filter 2, separate mother liquor and be the circulate soln that to prepare.
2. the production process of sodium-chlor:
The circulate soln of production process 1 preparation is put into reactive tank 3, add fertilizer Repone K F, by aforementioned production method, react, after reaction finishes with circulate soln and fertilizer Repone K effect precipitated sodium chloride part, separate the NaCID that generates with pressure filter 4, this sodium-chlor is used to produce ammonium chloride, separates sodium-chlor post precipitation separation mother liquor and enters in the crystallization groove 5, through cooling, separate the KCl crystallization H that separates out with pressure filter 6, this Repone K is used for the production of sodium-chlor.
3. potassium primary phosphate or vitriolate of tartar production process:
Mother liquor behind the production process 2 separation KCl crystal is squeezed in the reactive tank 7, add fertilizer primary ammonium phosphate A or fertilizer ammonium sulfate C, by the production method of aforementioned potassium primary phosphate or vitriolate of tartar part produce finish after, separate the crystal of separating out with whizzer 8, be potassium primary phosphate M or vitriolate of tartar N finished product.
4. Production of Ammonium Chloride operation:
Mother liquor behind the production process 3 separation finished products is squeezed in the reactive tank 1, added production process 1 isolating sodium-chlor D, produce by the production method of aforementioned ammonium chloride part, after reaction finished, the precipitation with pressure filter 2 separation generate was ammonium chloride finished product E.
More than produce and finished a circulation, later production just constantly repeats by above-mentioned 234 production method, finishes the successive production process.

Claims (5)

1, potassium primary phosphate, the production method of vitriolate of tartar is characterized in that: at first be mixed with the circulate soln that contains SODIUMNITRATE; This circulate soln of reheat and fertilizer Repone K effect precipitated sodium chloride; Mother liquor behind the separation sodium-chlor cools and separates out Repone K; Potassium primary phosphate or potassium product are produced in mother liquor behind the separation Repone K and fertilizer primary ammonium phosphate or fertilizer ammonium sulfate effect; Mother liquor behind separation potassium primary phosphate or the vitriolate of tartar and production begin to separate out isolating sodium-chlor effect and produce ammonium chloride, and this ammonium chloride is byproduct.Mother liquor behind the separating ammonium chloride contains SODIUMNITRATE, this mother liquor as circulate soln again with the effect of fertilizer Repone K, carry out above-mentioned production again.
2, according to the production method of the described potassium primary phosphate vitriolate of tartar of claim 1, it is characterized in that:
The circulate soln that contains SODIUMNITRATE is mixed with following reactants and weight proportion warp thereof, reacting by heating, and precipitation separation is prepared:
Fertilizer ammonium nitrate: 1100~730 parts; Fertilizer Repone K: 560~310 parts; Industrial table salt: 800~530 parts; Tap water: 1000 parts; Fertilizer primary ammonium phosphate: 130 parts; Or fertilizer ammonium sulfate: 60 parts.
3, according to the described potassium primary phosphate of claim 1, the production method of vitriolate of tartar is characterized in that: with circulate soln and fertilizer Repone K effect precipitated sodium chloride, the mother liquor behind the separation sodium-chlor is separated out Repone K:
(1) charging capacity of fertilizer Repone K: 205~125 grams per liters.
(2) temperature of reaction: 50~70 ℃, the reaction times: 30~60 minutes; After reaction finishes, separate the sodium-chlor of separating out, mother liquor is cooled to 35~40 ℃, separate the Repone K of separating out.
4, according to the described potassium primary phosphate of claim 1, the production method of vitriolate of tartar is characterized in that: separate out mother liquor and primary ammonium phosphate or ammonium sulfate effect production potassium primary phosphate or vitriolate of tartar behind the Repone K with separating;
(1) charging capacity of primary ammonium phosphate: 205~115 grams per liters, or the charging capacity of ammonium sulfate: 120~65 grams per liters.
(2) temperature of reaction: 40~45 ℃, the reaction times: 30~60 minutes, after finishing, reaction is cooled to 28~32 ℃, separate the potassium primary phosphate or the vitriolate of tartar of separating out.
5, according to the described potassium primary phosphate of claim 1, the production method of vitriolate of tartar is characterized in that: produce ammonium chloride with mother liquor and sodium-chlor effect behind separation potassium primary phosphate or the vitriolate of tartar:
(1) drops into participation reaction in the circulating mother liquor with producing the isolating sodium-chlor of beginning excessive 2~5%.
(2) temperature of reaction: 28~32 ℃, the reaction times: 30~60 minutes, after finishing, reaction is cooled to 23~25 ℃, separate the ammonium chloride of separating out.
CN 89106858 1989-11-23 1989-11-23 Production method of potassium dihydrogen phosphate and potassium sulfate Pending CN1045085A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 89106858 CN1045085A (en) 1989-11-23 1989-11-23 Production method of potassium dihydrogen phosphate and potassium sulfate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 89106858 CN1045085A (en) 1989-11-23 1989-11-23 Production method of potassium dihydrogen phosphate and potassium sulfate

Publications (1)

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CN1045085A true CN1045085A (en) 1990-09-05

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CN 89106858 Pending CN1045085A (en) 1989-11-23 1989-11-23 Production method of potassium dihydrogen phosphate and potassium sulfate

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101277901B (en) * 2005-08-11 2013-01-23 克鲁有限公司 Methods of producing fertilizer and CO2
CN101395103B (en) * 2005-12-01 2013-03-13 克鲁有限公司 A method for the combined production of a sulfur oxide containing product and a fertilizer
CN106430132A (en) * 2016-11-04 2017-02-22 湖北三宁化工股份有限公司 Method for preparing monopotassium phosphate and co-product ammonium sulfate by circulation method

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101277901B (en) * 2005-08-11 2013-01-23 克鲁有限公司 Methods of producing fertilizer and CO2
CN101395103B (en) * 2005-12-01 2013-03-13 克鲁有限公司 A method for the combined production of a sulfur oxide containing product and a fertilizer
CN106430132A (en) * 2016-11-04 2017-02-22 湖北三宁化工股份有限公司 Method for preparing monopotassium phosphate and co-product ammonium sulfate by circulation method

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