CN103332668A - Production method of monopotassium phosphate - Google Patents

Production method of monopotassium phosphate Download PDF

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Publication number
CN103332668A
CN103332668A CN2013102911353A CN201310291135A CN103332668A CN 103332668 A CN103332668 A CN 103332668A CN 2013102911353 A CN2013102911353 A CN 2013102911353A CN 201310291135 A CN201310291135 A CN 201310291135A CN 103332668 A CN103332668 A CN 103332668A
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China
Prior art keywords
pump
evaporator
tank
washing surface
reaction
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CN2013102911353A
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Chinese (zh)
Inventor
杨毅
胡国涛
赵建勇
宋子瞻
刘海
饶轶晟
周智武
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Wengfu Group Co Ltd
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Wengfu Group Co Ltd
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Priority to CN2013102911353A priority Critical patent/CN103332668A/en
Publication of CN103332668A publication Critical patent/CN103332668A/en
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Abstract

The invention discloses a production method of monopotassium phosphate. A production device comprises a feed calcium slurry tank (1), a reaction tank (2), a feed calcium slurry pump (3), a reaction slurry pump (4), a first automatic back washing surface filter (5), a primary evaporator (6), an impurity removal and desulfurization tank (7), a second automatic back washing surface filter (8), a slurry pump (9), a secondary evaporator (10), a mother solution pump (11), a crystallizer (12), a crystal mush pump (13), a flat plate scraper centrifuge (14), a drier (15), a methanol delivery pump (16), a methanol recovery storage tank (17) and a methanol condenser (18). With the adoption of the production device and a production technology flow, feed calcium hydrophosphate and potassium hydrogen sulfate generate replacement reaction, so that the content of a produced product can reach 98%, the cost is greatly lower than the production cost of a product obtained by a neutralization method production technology, and the production method is simple in technology and extensive in raw material source, and has broad market application prospects.

Description

A kind of production method of potassium primary phosphate
Technical field
The present invention relates to a kind of production technology of chemical fertilizer, be specifically related to a kind of production method of potassium primary phosphate.
Background technology
Potassium primary phosphate is efficient phosphorus potash fertilizer, use range is very wide, demand is big, market value is about 4 times of single Repone K potash fertilizer, the utilization ratio of potassium primary phosphate almost can reach 100%, because have the dual function of phosphate fertilizer and potash fertilizer concurrently, effect of increasing production is fine, the application of phosphoric acid potassium dihydrogen can obtain few input fecund and go out the result.Though China is potassium primary phosphate production and consumption big country, mainly all be single setting up factories in the past, adopt the higher neutralisation production technique of cost, production technology is also relatively backward.Because the products production cost is higher, cause its price higher, applying certain degree of difficulty in addition, therefore, the Methods of Producing Potassium Dihydrogen Phosphate route that research has low cost, high purity or production special purpose is significant to having applied in China's agriculture production.
Summary of the invention
Purpose of the present invention is devoted to seek the technology of the high-quality potassium primary phosphate of a kind of low cost production, be characterized in utilizing calcium hydrophosphate fodder and sal enixum to produce replacement(metathesis)reaction, produce potassium primary phosphate, simultaneously, the corresponding potassium primary phosphate production equipment of exploitation one cover guarantees high-quality potassium primary phosphate production.
Method of the present invention adopts following production equipment to realize:
Mainly by raising calcium slurry vessel 1, reactive tank 2 is raised calcium shurry pump 3 to the potassium primary phosphate production equipment, reaction material stock pump 4, the first automatic back-washing surface filters 5, single vaporization device 6, removal of impurities desulfurizer 7, the second automatic back-washing surface filters 8, shurry pump 9, second evaporator 10, mother liquor pump 11, crystallizer 12, magma pump 13, dull and stereotyped scraper centrifugal machine 14, moisture eliminator 15, methyl alcohol transferpump 16, Methanol Recovery storage tank 17, methanol condenser 18 is formed; Wherein raise calcium slurry vessel 1 by raising calcium shurry pump 3, ligation groove 2, the sal enixum Preparation tank is by pipe connection reactive tank 2, reactive tank 2 is connected with the first automatic back-washing surface filter 5 by reaction material stock pump 4, be connected with single vaporization device 6 with pipeline again, the single vaporization device feeds removal of impurities desulfurizer 7 with pipeline again, removal of impurities desulfurizer 7 connects the second automatic back-washing surface filter 8 by shurry pump 9 and is connected with second evaporator 10 with pipeline, after second evaporator 10 concentrated mother liquors are switched to crystallizer 12 crystallizations by mother liquor pump 11, deliver to dull and stereotyped scraper centrifugal machine 14 by magma pump 13 by pipeline, isolated crystallization is delivered to moisture eliminator 15 usefulness steam dryings and is obtained potassium dihydrogen phosphate product; In addition, the gas that second evaporator 10 evaporates when concentrating arrives methanol condenser 18 with pipe connection, the methyl alcohol that reclaims is connected to Methanol Recovery storage tank 13 with pipeline, and the methyl alcohol that removal of impurities desulfurizer 7 needs is connected with Methanol Recovery storage tank 17 with methyl alcohol transferpump 16 with pipeline; The technology of invention production equipment adopts following technical measures to realize, 1. enter from the slip of raising calcium device thickener and raise calcium slurry vessel 1, to raise calcium slip and potassium hydrogen sulfate solution and pump into reactive tank 2,55 ℃~60 ℃ of control temperature of reaction, reaction times 1.5~2h, reaction is squeezed into the first automatic back-washing surface filter with reaction material stock pump 4 with slip after finishing, filtrate enters the single vaporization device, and filter residue turns back to phosphogypsum slag field; 2. filtrate in single vaporization device 6, be concentrated to original volume 50% after pump into the impurity desulfurization groove, add methyl alcohol and carry out desulfurization, the slip after desulfurization is finished enters the second automatic back-washing surface filter, and filtrate enters second evaporator, filter residue returns the sal enixum Preparation tank, carries out recycle; 3. the steam that contains methyl alcohol of secondary concentration generation reclaims, filtrate in the second evaporator 10 is concentrated into 25% of its volume, solution after concentrating enters crystallizer tank 14, slip enters dull and stereotyped scraper centrifugal machine 15 after the crystallization, centrifugal back mother liquor returns second evaporator 10, crystallization enters moisture eliminator, and drying obtains product.
Beneficial effect of the present invention: adopt the high-quality Methods of Producing Potassium Dihydrogen Phosphate flow process of production equipment of the present invention and this low cost production, be characterized in utilizing calcium hydrophosphate fodder and sal enixum to produce replacement(metathesis)reaction, producing its content of potassium primary phosphate can the 98%(mass percentage concentration), cost is significantly less than the products production cost that the neutralisation production technique obtains, technology is simple, raw material sources are extensive, have wide market application prospect.
Description of drawings
Fig. 1 is production technique block diagram of the present invention;
Fig. 2 is production equipment structural representation of the present invention.
In Fig. 2,1. raise the calcium slurry vessel, 2. reactive tank is 3. raised the calcium shurry pump, 4. reaction material stock pump, the 5. first automatic back-washing surface filter, 6. single vaporization device, 7. removal of impurities desulfurizer, 8. second automatic back-washing surface filter, the 9. shurry pump, 10. second evaporator, 11. mother liquor pumps, 12. crystallizers, 13. the magma pump, 14. dull and stereotyped scraper centrifugal machines, 15. moisture eliminators, 16. the methyl alcohol transferpump, 17. Methanol Recovery storage tanks, 18. methanol condensers.
 
Embodiment
Below further specify the present invention by specific embodiment, but be not used for limiting the scope of the invention.
Embodiment 1
Mainly by raising calcium slurry vessel 1, reactive tank 2 is raised calcium shurry pump 3 to the potassium primary phosphate production equipment, reaction material stock pump 4, the first automatic back-washing surface filters 5, single vaporization device 6, removal of impurities desulfurizer 7, the second automatic back-washing surface filters 8, shurry pump 9, second evaporator 10, mother liquor pump 11, crystallizer 12, magma pump 13, dull and stereotyped scraper centrifugal machine 14, moisture eliminator 15, methyl alcohol transferpump 16, Methanol Recovery storage tank 17, methanol condenser 18 is formed; Wherein raise calcium slurry vessel 1 by raising calcium shurry pump 3, ligation groove 2, the sal enixum Preparation tank is by pipe connection reactive tank 2, reactive tank 2 is connected with the first automatic back-washing surface filter 5 by reaction material stock pump 4, be connected with single vaporization device 6 with pipeline again, the single vaporization device feeds removal of impurities desulfurizer 7 with pipeline again, removal of impurities desulfurizer 7 connects the second automatic back-washing surface filter 8 by shurry pump 9 and is connected with second evaporator 10 with pipeline, after second evaporator 10 concentrated mother liquors are switched to crystallizer 12 crystallizations by mother liquor pump 11, deliver to dull and stereotyped scraper centrifugal machine 14 by magma pump 13 by pipeline, isolated crystallization is delivered to moisture eliminator 15 usefulness steam dryings and is obtained potassium dihydrogen phosphate product; In addition, the methyl alcohol that the gas that second evaporator 10 evaporates when concentrating reclaims to methanol condenser 18 with pipe connection, connect Methanol Recovery storage tank 13 again with pipeline, the methyl alcohol that removal of impurities desulfurizer 7 needs is connected with Methanol Recovery storage tank 17 with methyl alcohol transferpump 16 with pipeline; The technology of invention production equipment adopts following technical measures to realize, 1. enter from the slip of raising calcium device thickener and raise calcium slurry vessel 1, to raise calcium slip and potassium hydrogen sulfate solution and pump into reactive tank 2,55 ℃~60 ℃ of control temperature of reaction, reaction times 1.5~2h, reaction is squeezed into the first automatic back-washing surface filter with reaction material stock pump 4 with slip after finishing, filtrate enters the single vaporization device, and filter residue turns back to phosphogypsum slag field; 2. filtrate in single vaporization device 6, be concentrated to original volume 50% after pump into the impurity desulfurization groove, add methyl alcohol and carry out desulfurization, the slip after desulfurization is finished enters the second automatic back-washing surface filter, and filtrate enters second evaporator, filter residue returns the sal enixum Preparation tank, carries out recycle; 3. the steam that contains methyl alcohol of secondary concentration generation reclaims, filtrate in the second evaporator 10 is concentrated into 25% of its volume, solution after concentrating enters crystallizer tank 14, slip enters dull and stereotyped scraper centrifugal machine 15 after the crystallization, centrifugal back mother liquor returns second evaporator 10, crystallization enters moisture eliminator, and drying obtains product.
Specifically, take by weighing 172g mash feed calcium hydrophosphate, add water in the ratio of liquid-solid ratio 3.5:1 and stir.The potassium hydrogen sulfate solution for preparing is slowly added in the calcium hydrophosphate fodder solution by certain flow velocity, potassium phosphorus mol ratio is 1:1, temperature of reaction is at 60 ℃, reaction times is 2h, cooling-sedimentation filtered after reaction was finished, filter residue is the very low calcium sulfate of foreign matter content, filtrate is carried out impurity and purification again, regulate ph value to 4~5, concentrate crystallisation by cooling, filtration, crystal after the filtration is potassium primary phosphate, the moisture of its crystal can be lower than 10%, carries out drying again and can obtain the product potassium primary phosphate, and the content of its potassium primary phosphate can be greater than 98%.

Claims (1)

1. the production method of a potassium primary phosphate, it is characterized in that implementing the production equipment of the inventive method by raising calcium slurry vessel (1), reactive tank (2) is raised calcium shurry pump (3), reaction material stock pump (4), the first automatic back-washing surface filter (5), single vaporization device (6), removal of impurities desulfurizer (7), the second automatic back-washing surface filter (8), shurry pump (9), second evaporator (10), mother liquor pump (11), crystallizer (12), magma pump (13), dull and stereotyped scraper centrifugal machine (14), moisture eliminator (15), methyl alcohol transferpump (16), Methanol Recovery storage tank (17), methanol condenser (18) is formed; Wherein raise calcium slurry vessel (1) by raising calcium shurry pump (3), ligation groove (2), the sal enixum Preparation tank is by pipe connection reactive tank (2), reactive tank (2) is connected with the first automatic back-washing surface filter (5) by reaction material stock pump (4), use pipeline to be connected with single vaporization device (6) again, the single vaporization device feeds removal of impurities desulfurizer (7) with pipeline again, removal of impurities desulfurizer (7) connects the second automatic back-washing surface filter (8) by shurry pump (9) and uses pipeline to be connected with second evaporator (10) again, after second evaporator (10) concentrated mother liquor is switched to crystallizer (12) crystallization by mother liquor pump (11), deliver to dull and stereotyped scraper centrifugal machine (14) by magma pump (13) by pipeline, isolated crystallization is delivered to moisture eliminator (15) and is obtained potassium dihydrogen phosphate product with steam drying; In addition, vaporized gas reclaimed methyl alcohol with pipe connection to methanol condenser (18) when second evaporator (10) concentrated, be connected to Methanol Recovery storage tank (13) with pipeline, the methyl alcohol that removal of impurities desulfurizer (7) needs is connected with Methanol Recovery storage tank (17) with methyl alcohol transferpump (16) with pipeline; The technology of production equipment of the present invention adopts following technical measures to realize, 1. enter from the slip of raising calcium device thickener and raise calcium slurry vessel (1), to raise calcium slip and potassium hydrogen sulfate solution and pump into reactive tank (2), 55 ℃~60 ℃ of control temperature of reaction, reaction times 1.5~2h, reaction is squeezed into the first automatic back-washing surface filter with reaction material stock pump (4) with slip after finishing, filtrate enters single vaporization device (6), and filter residue turns back to phosphogypsum slag field; 2. filtrate in the single vaporization device, be concentrated to original volume 50% after pump into the impurity desulfurization groove, add methyl alcohol and carry out desulfurization, the slip after desulfurization is finished enters the second automatic back-washing surface filter, and filtrate enters second evaporator (10), filter residue returns the sal enixum Preparation tank, carries out recycle; 3. the steam that contains methyl alcohol of secondary concentration generation reclaims, filtrate in the second evaporator is concentrated into 25% of its volume, solution after concentrating enters crystallizer tank (14), slip enters dull and stereotyped scraper centrifugal machine (15) after the crystallization, centrifugal back mother liquor returns second evaporator, crystallization enters moisture eliminator, and drying obtains product.
CN2013102911353A 2013-07-11 2013-07-11 Production method of monopotassium phosphate Pending CN103332668A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103738931A (en) * 2013-11-26 2014-04-23 瓮福(集团)有限责任公司 Method for production of potassium dihydrogen phosphate from phosphorus-containing acidic wastewater
CN104787738A (en) * 2015-04-29 2015-07-22 瓮福(集团)有限责任公司 Purification method of dilute acid in wet-process phosphoric acid production
CN104891465A (en) * 2015-05-29 2015-09-09 湖北三宁化工股份有限公司 Method for preparing potassium dihydrogen phosphate from industrial monoammonium phosphate mother solution
CN106629645A (en) * 2016-11-15 2017-05-10 华东理工大学 Method for double solution decomposition in the production process of monopotassium phosphate purification
CN106744764A (en) * 2016-11-15 2017-05-31 华东理工大学 A kind of method for producing potassium dihydrogen 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

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102424374A (en) * 2011-09-07 2012-04-25 湖北三宁化工股份有限公司 Production method of potassium dihydrogen phosphate

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102424374A (en) * 2011-09-07 2012-04-25 湖北三宁化工股份有限公司 Production method of potassium dihydrogen phosphate

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103738931A (en) * 2013-11-26 2014-04-23 瓮福(集团)有限责任公司 Method for production of potassium dihydrogen phosphate from phosphorus-containing acidic wastewater
CN104787738A (en) * 2015-04-29 2015-07-22 瓮福(集团)有限责任公司 Purification method of dilute acid in wet-process phosphoric acid production
CN104891465A (en) * 2015-05-29 2015-09-09 湖北三宁化工股份有限公司 Method for preparing potassium dihydrogen phosphate from industrial monoammonium phosphate mother solution
CN106629645A (en) * 2016-11-15 2017-05-10 华东理工大学 Method for double solution decomposition in the production process of monopotassium phosphate purification
CN106744764A (en) * 2016-11-15 2017-05-31 华东理工大学 A kind of method for producing potassium dihydrogen phosphate
CN106744764B (en) * 2016-11-15 2019-05-14 华东理工大学 A method of producing potassium dihydrogen 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

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Application publication date: 20131002