CN102424374A - Production method of potassium dihydrogen phosphate - Google Patents
Production method of potassium dihydrogen phosphate Download PDFInfo
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- CN102424374A CN102424374A CN2011102638653A CN201110263865A CN102424374A CN 102424374 A CN102424374 A CN 102424374A CN 2011102638653 A CN2011102638653 A CN 2011102638653A CN 201110263865 A CN201110263865 A CN 201110263865A CN 102424374 A CN102424374 A CN 102424374A
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- primary phosphate
- dihydrogen phosphate
- potassium dihydrogen
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Abstract
A production method of potassium dihydrogen phosphate comprises the following steps: adding a potassium bisulfate solution and powdery calcium hydrogen phosphate into a potassium dihydrogen phosphate reaction tank for reaction, filtering the material slurry after the reaction, delivering the filter residues to a wet-method phosphoric acid system filter for filtration, delivering to a phosphogypsum stockyard or directly stacking in a stockyard, delivering the filtrate into an evaporation concentration device for concentration; allowing the concentrated supersaturated solution to enter a cooling crystallization tank, filtering the material slurry after cooling crystallization by a centrifugation filter, returning the filtered mother liquor to the potassium dihydrogen phosphate reaction tank and a mixed acid tank of a device for producing sulfur-base composite fertilizer, wherein the crystal obtained from filtration is potassium dihydrogen phosphate, drying to obtain the potassium dihydrogen phosphate finished product. The invention is applicable to all enterprises with a high-concentration sulfur-base composite fertilizer device, and has the advantages of low cost, good product quality, and less equipment investment.
Description
Technical field
The present invention relates to the composite fertilizer producing process technical field, be specifically related to a kind of working method of potassium primary phosphate.
Background technology
Potassium primary phosphate is a kind of high density high-quality phosphorus potassium complex fertilizer, and traditional technology generally adopts neutralisation and double decomposition, and neutralisation technology is simple, but raw materials used costliness, production cost is high, is difficult in the production of agricultural and industrial potassium primary phosphate, promote; Double decomposition mainly carries out replacement(metathesis)reaction with Repone K and phosphoric acid, makes reaction be able to carry out through the hydrogen chloride gas that shifts out the reaction generation, and there are problems such as remaining chloride ion content exceeds standard in energy consumption height and the product in this method.The potassium primary phosphate production technique also has organic extraction method, ion exchange method and direct method etc. in addition, and all high owing to production cost, quality product is defective, equipment corrosion is serious etc. failed industriallization.
Up to the present, also do not have fairly large potassium primary phosphate production equipment, cause on the market potassium primary phosphate source of goods in short supply, product price is higher.
Summary of the invention
The objective of the invention is to overcome above-mentioned deficiency; The potassium primary phosphate working method that provide that a kind of production cost is low, good product quality and facility investment reduces significantly; This method is applicable to that all have the enterprise of high density S-based compound fertilizer device, and potassium primary phosphate can form a complete production network.
The objective of the invention is to realize like this: a kind of working method of potassium primary phosphate; Comprise following process: with reacting in potassium hydrogen sulfate solution and the powdered acid hydrogen calcium adding biphosphate potassium reaction; Reacted slurry filtration; Filter residue is sent into and is sent ardealite storage yard after phosphoric acid by wet process system filtration machine filters or directly deliver in the stockyard and stack, and filtrating is sent to evaporation concentration device and concentrated; Supersaturated solution after concentrating gets into the crystallisation by cooling groove; Slip behind the crystallisation by cooling filters through centrifugal filter; Mother liquor after the filtration returns the biphosphate potassium reaction and produces in the nitration mixture groove of S-based compound fertilizer device; The crystal that filters gained is a potassium primary phosphate, is drying to obtain the potassium primary phosphate finished product.
The mol ratio of potassium hydrogen sulfate solution and powdered acid hydrogen calcium is 1:1～1:1.05.
Described potassium hydrogen sulfate solution is from sal enixum workshop section in the high density production of sulfur-based compound fertilizer flow process, in the biphosphate potassium reaction not the sal enixum of complete reaction can be back in the high density S-based compound fertilizer system and recycle.
Potassium hydrogen sulfate solution and powdered acid hydrogen calcium are added when reacting in the biphosphate potassium reaction, are 3-6 hour in the following reaction times of well-beaten situation, and temperature of reaction is at 70～90 ℃.
Potassium primary phosphate working method provided by the invention has following beneficial effect:
1, adopting the potassium hydrogen sulfate solution that sal enixum workshop section produces in the high density production of sulfur-based compound fertilizer flow process is raw materials for production, has reduced the input of sal enixum production equipment during potassium primary phosphate is produced, and has promptly significantly reduced facility investment.
2, in the biphosphate potassium reaction unreacted completely sal enixum can be back to recycle in the high density production of sulfur-based compound fertilizer system, improved the recovery of potassium, reduced production cost.
3, the present invention includes two-step approach; Synthesizing in the production of sulfur-based compound fertilizer device of the first step sal enixum accomplished; The second step sal enixum and the reaction of powdered acid hydrogen calcium generate potassium primary phosphate; Chloride ion content in the sal enixum product that high density S-based compound fertilizer device is produced is low, so the product that the more traditional Repone K double decomposition of the chloride ion content in the potassium primary phosphate of producing is produced is lower, the potassium dihydrogen sulfate product reaches industrial salable product standard and feed grade standard.
4, secondary calcium phosphate is as one of main raw material that reacts, and the source is wide, and price is low, thereby has reduced production cost.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
Through specific embodiment the present invention is done further introduction below, but embodiment can not be construed as limiting the invention.
The reaction equation that the present invention relates to is:
KHSO
4+CaHPO
4·2H
2O?=KH
2PO
4+CaSO
4·2H
2O
Embodiment 1:
The potassium hydrogen sulfate solution of sal enixum workshop section in the high density production of sulfur-based compound fertilizer flow process (S-NPK device) is taken out in the part adding biphosphate potassium reaction; Adding is the powdered acid hydrogen calcium of 1:1～1:1.05 with the sal enixum mol ratio in reactive tank again; Reaction is 6 hours under well-beaten situation; Temperature of reaction is 70～85 ℃, and reacted slip filters through full-automatic chamber(filter)press, and filter residue is sent into and sent ardealite storage yard after phosphoric acid by wet process system filtration machine filters or directly deliver in the stockyard and stack; Filtrating is potassium dihydrogen phosphate, sends to evaporation concentration device and concentrates; Supersaturated solution after concentrating gets into crystallisation by cooling groove crystallisation by cooling; Slip after the crystallization is sent to piston material pushing formula centrifugal filter and is filtered; Mother liquor after the filtration returns the biphosphate potassium reaction and produces in the nitration mixture groove of S-based compound fertilizer device; The crystal that filters gained is a potassium primary phosphate, sends to the vibra fluidized bed drying system and is drying to obtain the potassium primary phosphate finished product, sends to the automatic packing machine packing.
Embodiment 2:
The potassium hydrogen sulfate solution of sal enixum workshop section in the high density production of sulfur-based compound fertilizer flow process (S-NPK device) is taken out in the part adding biphosphate potassium reaction; Adding is the powdered acid hydrogen calcium of 1:1～1:1.05 with the sal enixum mol ratio in reactive tank again; Reaction is 3 hours under well-beaten situation; Temperature of reaction is 80～90 ℃, and reacted slip filters through full-automatic chamber(filter)press, and filter residue is sent into and sent ardealite storage yard after phosphoric acid by wet process system filtration machine filters or directly deliver in the stockyard and stack; Filtrating is potassium dihydrogen phosphate, sends to evaporation concentration device and concentrates; Supersaturated solution after concentrating gets into crystallisation by cooling groove crystallisation by cooling; Slip after the crystallization is sent to piston material pushing formula centrifugal filter and is filtered; Mother liquor after the filtration returns the biphosphate potassium reaction and produces in the nitration mixture groove of S-based compound fertilizer device; The crystal that filters gained is a potassium primary phosphate, sends to the vibra fluidized bed drying system and is drying to obtain the potassium primary phosphate finished product, sends to the automatic packing machine packing.
Embodiment 3:
The potassium hydrogen sulfate solution of sal enixum workshop section in the high density production of sulfur-based compound fertilizer flow process (S-NPK device) is taken out in the part adding biphosphate potassium reaction; Adding is the powdered acid hydrogen calcium of 1:1 with the sal enixum mol ratio in reactive tank again; Reaction is 5 hours under well-beaten situation; Temperature of reaction is 80～85 ℃, and reacted slip filters through full-automatic chamber(filter)press, and filter residue is sent into and sent ardealite storage yard after phosphoric acid by wet process system filtration machine filters or directly deliver in the stockyard and stack; Filtrating is potassium dihydrogen phosphate, sends to evaporation concentration device and concentrates; Supersaturated solution after concentrating gets into crystallisation by cooling groove crystallisation by cooling; Slip after the crystallization is sent to piston material pushing formula centrifugal filter and is filtered; Mother liquor after the filtration returns the biphosphate potassium reaction and produces in the nitration mixture groove of S-based compound fertilizer device; The crystal that filters gained is a potassium primary phosphate, sends to the vibra fluidized bed drying system and is drying to obtain the potassium primary phosphate finished product, sends to the automatic packing machine packing.
Evaporation concentration device among the embodiment 1,2 and 3 is made up of vapo(u)rization system, well heater, recycle pump and atmospheric cooler etc., and wherein vapo(u)rization system adopts double-effect evaporation.
Claims (4)
1. the working method of a potassium primary phosphate; It is characterized in that: comprise following process: with reacting in potassium hydrogen sulfate solution and the powdered acid hydrogen calcium adding biphosphate potassium reaction; Reacted slurry filtration; Filter residue is sent into and is sent ardealite storage yard after phosphoric acid by wet process system filtration machine filters or directly deliver in the stockyard and stack, and filtrating is sent to evaporation concentration device and concentrated; Supersaturated solution after concentrating gets into the crystallisation by cooling groove; Slip behind the crystallisation by cooling filters through centrifugal filter; Mother liquor after the filtration returns the biphosphate potassium reaction and produces in the nitration mixture groove of S-based compound fertilizer device; The crystal that filters gained is a potassium primary phosphate, is drying to obtain the potassium primary phosphate finished product.
2. the working method of potassium primary phosphate according to claim 1, it is characterized in that: the mol ratio of potassium hydrogen sulfate solution and powdered acid hydrogen calcium is 1:1～1:1.05.
3. the working method of potassium primary phosphate according to claim 1; It is characterized in that: described potassium hydrogen sulfate solution is from sal enixum workshop section in the high density production of sulfur-based compound fertilizer flow process, in the biphosphate potassium reaction not the sal enixum of complete reaction can be back in the high density S-based compound fertilizer system and recycle.
4. the working method of potassium primary phosphate according to claim 1; It is characterized in that: potassium hydrogen sulfate solution and powdered acid hydrogen calcium are added when reacting in the biphosphate potassium reaction; In the following reaction times of well-beaten situation is 3-6 hour, and temperature of reaction is at 70～90 ℃.
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| CN2011102638653A CN102424374A (en) | 2011-09-07 | 2011-09-07 | Production method of potassium dihydrogen phosphate |
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| CN2011102638653A CN102424374A (en) | 2011-09-07 | 2011-09-07 | Production method of potassium dihydrogen phosphate |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102862964A (en) * | 2012-09-08 | 2013-01-09 | 湖北三宁化工股份有限公司 | Device and method for producing monopotassium phosphate by using double decomposition |
| CN102901327A (en) * | 2012-10-23 | 2013-01-30 | 常熟市圆启晶体材料有限公司 | Centrifugal dehydrating method of potassium dihydrogen phosphate in solid solution state |
| CN102963874A (en) * | 2012-11-26 | 2013-03-13 | 四川川恒化工股份有限公司 | Method for producing industrial-grade potassium dihydrogen phosphate (KH2PO4) by wet method purified phosphoric acid and potassium sulfate |
| CN103058158A (en) * | 2013-02-05 | 2013-04-24 | 瓮福（集团）有限责任公司 | Method for preparing monopotassium phosphate from fertilizer grade calcium hydrophosphate |
| CN103159194A (en) * | 2013-04-10 | 2013-06-19 | 河北诺达化工设备有限公司 | Continuous crystallization process for monopotassium phosphate |
| CN103332668A (en) * | 2013-07-11 | 2013-10-02 | 瓮福（集团）有限责任公司 | Production method of monopotassium phosphate |
| CN107188146A (en) * | 2017-07-18 | 2017-09-22 | 禄丰天宝磷化工有限公司 | A kind of production technology of feed grade potassium dihydrogen phosphate |
| CN107265424A (en) * | 2017-07-18 | 2017-10-20 | 禄丰天宝磷化工有限公司 | A kind of production technology that feed grade potassium dihydrogen phosphate is produced by phosphorus ore containing |
| CN115676788A (en) * | 2022-10-18 | 2023-02-03 | 新希望化工投资有限公司 | High-purity monopotassium phosphate and preparation method thereof |
Citations (4)
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|---|---|---|---|---|
| CN1412107A (en) * | 2001-10-19 | 2003-04-23 | 四川宏达(集团)有限公司 | Production method of potassium dihydrogen phosphate |
| CN1830762A (en) * | 2006-03-30 | 2006-09-13 | 云南省化工研究院 | Method of continuously preparing potassium dihydrogen phosphate |
| US20060222581A1 (en) * | 2005-03-31 | 2006-10-05 | Cargill, Incorporated Of Wayzata, Mn | Process for producing high purity phosphates |
| CN100999312A (en) * | 2007-01-05 | 2007-07-18 | 黄尚勋 | Coproduction method of potassium dihydrogen phosphate, sulfur base composite fertilizer and aluminium polychloride |
-
2011
- 2011-09-07 CN CN2011102638653A patent/CN102424374A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1412107A (en) * | 2001-10-19 | 2003-04-23 | 四川宏达(集团)有限公司 | Production method of potassium dihydrogen phosphate |
| US20060222581A1 (en) * | 2005-03-31 | 2006-10-05 | Cargill, Incorporated Of Wayzata, Mn | Process for producing high purity phosphates |
| CN1830762A (en) * | 2006-03-30 | 2006-09-13 | 云南省化工研究院 | Method of continuously preparing potassium dihydrogen phosphate |
| CN100999312A (en) * | 2007-01-05 | 2007-07-18 | 黄尚勋 | Coproduction method of potassium dihydrogen phosphate, sulfur base composite fertilizer and aluminium polychloride |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102862964B (en) * | 2012-09-08 | 2014-07-23 | 湖北三宁化工股份有限公司 | Device and method for producing monopotassium phosphate by using double decomposition |
| CN102862964A (en) * | 2012-09-08 | 2013-01-09 | 湖北三宁化工股份有限公司 | Device and method for producing monopotassium phosphate by using double decomposition |
| CN102901327A (en) * | 2012-10-23 | 2013-01-30 | 常熟市圆启晶体材料有限公司 | Centrifugal dehydrating method of potassium dihydrogen phosphate in solid solution state |
| CN102901327B (en) * | 2012-10-23 | 2014-09-03 | 常熟市圆启晶体材料有限公司 | Centrifugal dehydrating method of potassium dihydrogen phosphate in solid solution state |
| CN102963874A (en) * | 2012-11-26 | 2013-03-13 | 四川川恒化工股份有限公司 | Method for producing industrial-grade potassium dihydrogen phosphate (KH2PO4) by wet method purified phosphoric acid and potassium sulfate |
| CN102963874B (en) * | 2012-11-26 | 2015-04-15 | 贵州川恒化工有限责任公司 | Method for producing industrial-grade potassium dihydrogen phosphate (KH2PO4) by wet method purified phosphoric acid and potassium sulfate |
| CN103058158A (en) * | 2013-02-05 | 2013-04-24 | 瓮福（集团）有限责任公司 | Method for preparing monopotassium phosphate from fertilizer grade calcium hydrophosphate |
| CN103159194A (en) * | 2013-04-10 | 2013-06-19 | 河北诺达化工设备有限公司 | Continuous crystallization process for monopotassium phosphate |
| CN103332668A (en) * | 2013-07-11 | 2013-10-02 | 瓮福（集团）有限责任公司 | Production method of monopotassium phosphate |
| CN107188146A (en) * | 2017-07-18 | 2017-09-22 | 禄丰天宝磷化工有限公司 | A kind of production technology of feed grade potassium dihydrogen phosphate |
| CN107265424A (en) * | 2017-07-18 | 2017-10-20 | 禄丰天宝磷化工有限公司 | A kind of production technology that feed grade potassium dihydrogen phosphate is produced by phosphorus ore containing |
| CN115676788A (en) * | 2022-10-18 | 2023-02-03 | 新希望化工投资有限公司 | High-purity monopotassium phosphate and preparation method thereof |
| CN115676788B (en) * | 2022-10-18 | 2024-02-02 | 新希望化工投资有限公司 | High-purity potassium dihydrogen phosphate and preparation method thereof |
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Application publication date: 20120425 |