CN105800575B - A kind of method using half water law Wet-process Phosphoric Acid Production fertilizer potassium dihydrogen phosphate - Google Patents
A kind of method using half water law Wet-process Phosphoric Acid Production fertilizer potassium dihydrogen phosphate Download PDFInfo
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- CN105800575B CN105800575B CN201610132577.7A CN201610132577A CN105800575B CN 105800575 B CN105800575 B CN 105800575B CN 201610132577 A CN201610132577 A CN 201610132577A CN 105800575 B CN105800575 B CN 105800575B
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- phosphoric acid
- potassium
- dihydrogen phosphate
- half water
- potassium hydroxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/30—Alkali metal phosphates
- C01B25/301—Preparation from liquid orthophosphoric acid or from an acid solution or suspension of orthophosphates
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
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Abstract
A kind of method using half water law Wet-process Phosphoric Acid Production fertilizer potassium dihydrogen phosphate, it is characterized in that, including following technical process：Half water law phosphoric acid by wet process is added into ground phosphate rock and carries out desulfurization, the slurry after desulfurization is filtered, filter residue feeding phosphoric acid system, filtrate enters a neutralization chamber, adds potassium hydroxide and neutralizes, and neutralize slip pH value of regulation is 2.0 2.5 etc., and beneficial effect of the invention is：Half water phosphoric acid by wet process and dry ground phosphate rock reaction desulfuration, reduce by half water phosphoric acid by wet process SO4 2‑, while dissolving in 2 5% CaO.The consumption of first and second neutralization removal of impurities potassium hydroxide can be reduced.So that phosphorus and potassium are fully used.P is improved with this2O5Yield.Three neutralization filtrated stocks return to the first and second preparation water for neutralizing potassium hydroxide, reduce production process water consumption, while reclaiming the phosphorus and potassium of the residual of mother liquor so that phosphorus and potassium make full use of, improve the yield of phosphorus and potassium.
Description
Technical field
The invention belongs to phosphorous chemical industry field, and in particular to a kind of half water law Wet-process Phosphoric Acid Production fertilizer potassium dihydrogen phosphate
(KH2PO4) method.
Background technology
Potassium dihydrogen phosphate (KH2PO4) it is phosphatic one big branch, potassium dihydrogen phosphate is phosphatic staple product, pure
Potassium dihydrogen phosphate is the (K containing potassium oxide2O) 34.60%, phosphorus pentoxide (P2O5) 52.20%.Potassium dihydrogen phosphate is a kind of colourless
Or the rhomboidal crystal of white gloss, water can be dissolved in, is reacted acid, insoluble in alcohol.Potassium dihydrogen phosphate is a kind of high concentration high-quality
Phosphorus potassium complex fertilizer, traditional handicraft typically uses neutralisation and double decomposition, and neutralisation technique is simple, but cost of material used
It is expensive, it is difficult to be promoted in the production of agricultural potassium dihydrogen phosphate；Double decomposition mainly carries out double decomposition with potassium chloride and phosphoric acid
Reaction, by remove react produce hydrogen chloride gas reaction is carried out, this exist exist in high energy consumption and product chlorine from
The problems such as sub- content overproof.In addition potassium dihydrogen phosphate production technology also has direct method, conversion method, organic extraction, ion exchange
Method etc., fails to industrialize because cost of material is expensive, production cost is high, product quality is unqualified, equipment corrosion is serious etc..
To at present therefore, also without fairly large potassium dihydrogen phosphate process units, causing in the market potassium dihydrogen phosphate goods
Supply falls short of demand in source, and product price is higher.
The content of the invention
The purpose of the present invention overcome it is above-mentioned it is not enough there is provided a kind of production cost is low, good product quality and equipment investment
The Methods For The Manufacture of Potassium Dihydrogen Phosphate being greatly reduced, the method possesses calcium hydrophosphate fodder and composite heat transfer dress suitable for all
The enterprise put, can form a complete production network potassium dihydrogen phosphate.
The object of the present invention is achieved like this：A kind of side using half water law Wet-process Phosphoric Acid Production fertilizer potassium dihydrogen phosphate
Method, feature of present invention is, including following technical process：Half water law phosphoric acid by wet process is added into ground phosphate rock and carries out desulfurization, after desulfurization
Slurry is filtered, filter residue feeding phosphoric acid system so, filtrate enters neutralization chamber, adds potassium hydroxide and neutralizes, regulation one
Secondary neutralize slip pH value, one time neutralize slip is filtered, and filter residue is added in nitrogen-phosphorus-potassium compound fertilizer by 2%-10%, and not shadow
Nitrogen-phosphorus-potassium compound fertilizer index is rung, filtrate enters secondary neutralization chamber, add the secondary neutralization of potassium hydroxide, adjust secondary neutralize slip pH
Value, secondary neutralize slip filtered, filter residue as calcium hydrophosphate fodder additive, filtrate into three neutralization chambers, plus
Enter three neutralizations of potassium hydroxide, adjust three neutralization pH value, three neutralize slips are delivered to evaporation concentration device concentration, after concentration
Supersaturated solution enter crystallisation by cooling groove, the slurry after crystallisation by cooling is through filtering, and mother liquor, which returns one, two, three and neutralized, is used as hydrogen
Potassium oxide preparation water, the crystal obtained by filtering is potassium dihydrogen phosphate, and drying, metering, packaging produce potassium dihydrogen phosphate finished product.
The amount of half water law phosphoric acid by wet process desulfurization addition ground phosphate rock is 1 according to the mol ratio of sulphur and calcium oxide:1~1：3. reaction
Time 1.0-3.0 hour.30-80 DEG C of of reaction temperature
Neutralize slip pH value 2.0-2.5, reaction time 1.5-3.0 hour.30-50 DEG C of of reaction temperature
Secondary neutralize slip pH value 3.0-3.5, reaction time 1.5-3.0 hour.30-50 DEG C of of reaction temperature
Three neutralize slip pH value 4.2-4.7, reaction time 2.0-6.0 hour.50-70 DEG C of of reaction temperature
First and second neutralizes concentration of potassium hydroxide 15-30%.
Three neutralization filtrated stocks are used as potassium hydroxide preparation water.
The present invention provides Methods For The Manufacture of Potassium Dihydrogen Phosphate, has the advantages that：
1st, half water phosphoric acid by wet process and dry ground phosphate rock reaction desulfuration, reduce by half water phosphoric acid by wet process SO4 2-, while dissolving in 2-5%'s
CaO. (table 1 is index before and after half water phosphoric acid by wet process desulfurization)
Table 1
2nd, because half water phosphoric acid by wet process desulfurization can dissolve in 2-5% CaO, Ca is provided for first and second neutralization removal of impurities2+, one
Secondary neutralization removal of impurities mainly generates CaSO4.2H2O、CaF2、K2SiF6And ferric phosphate magnalium sylvite.Secondary neutralization is mainly generated
CaHPO4.H2O, because of Ca2+It is excessive, reduce by first and second consumption for neutralizing removal of impurities potassium hydroxide.
3rd, once in and in potassium hydroxide is added and while removal of impurities, generate CaSO4.2H2O、CaF2、K2SiF6And phosphoric acid
Iron magnalium sylvite, can as nitrogen-phosphorus-potassium compound fertilizer additive so that phosphorus and potassium are fully used.
4th, in secondary and in adding potassium hydroxide and when, generate substandard products calcium monohydrogen phosphate, the substandard products calcium monohydrogen phosphate can add
It is added in calcium hydrophosphate fodder finished product, the amount of addition can be added by 2-10%, the calcium hydrophosphate fodder finished product after addition
Index can be up to state standards so that phosphorus is fully used, and P is improved with this2O5Yield.
5th, three neutralization filtrated stocks return to the first and second preparation water for neutralizing potassium hydroxide, reduce production process water
Amount, while reclaiming the phosphorus and potassium of the residual of mother liquor so that phosphorus and potassium make full use of, improves the yield of phosphorus and potassium.
Brief description of the drawings
Fig. 1 is the process flow diagram of the present invention.
Embodiment
Embodiment 1：
Half water law phosphoric acid by wet process is added into ground phosphate rock and carries out desulfurization, additional proportion is 1 according to the mol ratio of sulphur and calcium oxide:
2 reactions, 1.5 hours reaction time.Slurry after 50 DEG C of desulfurization of reaction temperature is filtered, filter residue feeding phosphoric acid system so,
Filtrate enters a neutralization chamber, adds concentration and is neutralized for 15% potassium hydroxide, a neutralize slip pH value 2.2 is adjusted, during reaction
Between 1.5 hours, 60 DEG C of reaction temperature, one time neutralize slip is filtered, filter residue add nitrogen-phosphorus-potassium compound fertilizer in, filtrate enters two
Secondary neutralization chamber, it is the secondary neutralization of 15% potassium hydroxide to add concentration, adjusts secondary neutralize slip pH value 3.0, the reaction time 1.5 is small
When, 60 DEG C of reaction temperature, secondary neutralize slip is filtered, and filter residue adds calcium hydrophosphate fodder drying system, and filtrate enters
Three neutralization chambers, it is 15% potassium hydroxide, three neutralizations to add concentration, adjusts three neutralization pH value 4.2, and the reaction time 2.0 is small
When, 70 DEG C of reaction temperature, three neutralize slips are delivered to evaporation concentration device concentration, and the supersaturated solution after concentration enters cooling
Slurry after crystallization tank, crystallisation by cooling is through filtering, and it is potassium hydroxide preparation water that mother liquor, which returns one, two, three neutralization, filtering gained
Crystal be potassium dihydrogen phosphate, dry, measure, packing and to obtain the more excellent potassium dihydrogen phosphate product of quality.Potassium dihydrogen phosphate product index
It is shown in Table 1
The potassium dihydrogen phosphate product Indexs measure table of the present invention of table 1
| Project | Agriculture Grade A | This product |
| Potassium dihydrogen phosphate (KH2PO4In terms of butt) content >=, % | 96 | 96.2 |
| Shui Fen≤, % | 4 | 3.8 |
| PH value | 4.3-4.7 | 4.5 |
| Potassium oxide (K2O is in terms of butt) content >=, % | 33.2 | 33.25 |
Embodiment 2：
Half water law phosphoric acid by wet process is added into ground phosphate rock and carries out desulfurization, additional proportion is 1 according to the mol ratio of sulphur and calcium oxide:
3 reactions, 1.5 hours reaction time.Slurry after 50 DEG C of desulfurization of reaction temperature is filtered, filter residue feeding phosphoric acid system so,
Filtrate enters a neutralization chamber, adds concentration and is neutralized for 15% potassium hydroxide, a neutralize slip pH value 2.2 is adjusted, during reaction
Between 1.5 hours, 30 DEG C of reaction temperature, one time neutralize slip is filtered, filter residue add nitrogen-phosphorus-potassium compound fertilizer in, filtrate enters two
Secondary neutralization chamber, it is the secondary neutralization of 15% potassium hydroxide to add concentration, adjusts secondary neutralize slip pH value 3.2, the reaction time 1.5 is small
When, 30 DEG C of reaction temperature, secondary neutralize slip is filtered, and obtains substandard products calcium monohydrogen phosphate, and substandard products calcium monohydrogen phosphate 5% adds feed
Calcium hydrophosphate drying system, by drying metering packing, obtains the qualified calcium hydrophosphate fodder product of quality.Filtrate enters
Three neutralization chambers, it is 15% potassium hydroxide, three neutralizations to add concentration, adjusts three neutralization pH value 4.2, and the reaction time 2.0 is small
When, 50 DEG C of reaction temperature, three neutralize slips are delivered to evaporation concentration device concentration, and the supersaturated solution after concentration enters cooling
Slurry after crystallization tank, crystallisation by cooling is through filtering, and it is potassium hydroxide preparation water that mother liquor, which returns one, two, three neutralization, filtering gained
Crystal be potassium dihydrogen phosphate, dry, measure, packing and to obtain the more excellent potassium dihydrogen phosphate product of quality.Substandard products calcium monohydrogen phosphate adds by 5%
Enter calcium hydrophosphate fodder drying system, calcium hydrophosphate fodder index is shown in Table 2.
The biphosphate calcium product Indexs measure table of the present invention of table 2
Embodiment 3：
Half water law phosphoric acid by wet process is added into ground phosphate rock and carries out desulfurization, additional proportion is 1 according to the mol ratio of sulphur and calcium oxide:
2.5 reactions, 1.5 hours reaction time.Slurry after 50 DEG C of desulfurization of reaction temperature is filtered, filter residue feeding phosphoric acid system institute
So that filtrate enters a neutralization chamber, adds concentration and is neutralized for 15% potassium hydroxide, adjusts a neutralize slip pH value 2.2, reaction
1.5 hours time, 30 DEG C of reaction temperature, one time neutralize slip is filtered, and filter residue is added in nitrogen-phosphorus-potassium compound fertilizer, and filtrate enters
Secondary neutralization chamber, it is the secondary neutralization of 15% potassium hydroxide to add concentration, adjusts secondary neutralize slip pH value 3.2, reaction time 1.5
Hour, 30 DEG C of reaction temperature, secondary neutralize slip is filtered, and obtains substandard products calcium monohydrogen phosphate, and substandard products calcium monohydrogen phosphate adds by 10%
Enter calcium hydrophosphate fodder drying system, by drying metering packing, obtain the qualified calcium hydrophosphate fodder product of quality.Filter
Liquid enters three neutralization chambers, and it is 15% potassium hydroxide, three neutralizations to add concentration, adjusts three neutralization pH value 4.2, reaction time
2.0 hours, 50 DEG C of reaction temperature, three neutralize slips were delivered to evaporation concentration device concentration, and the supersaturated solution after concentration enters
Enter the slurry after crystallisation by cooling groove, crystallisation by cooling through filtering, it is potassium hydroxide preparation water, mistake that mother liquor, which returns one, two, three neutralization,
Crystal obtained by filter is potassium dihydrogen phosphate, dries, measures, packing and to obtain the more excellent potassium dihydrogen phosphate product of quality.Substandard products calcium monohydrogen phosphate
Calcium hydrophosphate fodder drying system is added by 10%, calcium hydrophosphate fodder index is shown in Table 3
The biphosphate calcium product Indexs measure table of the present invention of table 3
Embodiment 4：
Half water law phosphoric acid by wet process is added into ground phosphate rock and carries out desulfurization, additional proportion is 1 according to the mol ratio of sulphur and calcium oxide:
1.2 reactions, 1.5 hours reaction time.Slurry after 50 DEG C of desulfurization of reaction temperature is filtered, filter residue feeding phosphoric acid system institute
So that filtrate enters a neutralization chamber, adds concentration and is neutralized for 15% potassium hydroxide, adjusts a neutralize slip pH value 2.2, reaction
1.5 hours time, 30 DEG C of reaction temperature, one time neutralize slip is filtered, and filter residue is added one in nitrogen-phosphorus-potassium compound fertilizer according to 5%
Drying is played, filtrate enters secondary neutralization chamber, add concentration and neutralized for 15% potassium hydroxide is secondary, adjust secondary neutralize slip pH value
3.2,1.5 hours reaction time, 30 DEG C of reaction temperature, secondary neutralize slip is filtered, and filter residue adds calcium hydrophosphate fodder
Drying system, by drying metering packing, obtains the qualified calcium hydrophosphate fodder product of quality.Filtrate enters three neutralizations
Groove, it is 15% potassium hydroxide, three neutralizations to add concentration, adjusts three neutralization pH value 4.2,2.0 hours reaction time, reaction temperature
50 DEG C of degree, three neutralize slips are delivered to evaporation concentration device concentration, and the supersaturated solution after concentration enters crystallisation by cooling groove, cold
But the slurry after crystallizing is through filtering, and it is potassium hydroxide preparation water that mother liquor, which returns one, two, three neutralization, and the crystal obtained by filtering is
Potassium dihydrogen phosphate, dries, measures, packing and to obtain the more excellent potassium dihydrogen phosphate product of quality.
Once neutralize filter residue and add nitrogen-phosphorus-potassium compound fertilizer by 5%, nitrogen-phosphorus-potassium compound fertilizer index is shown in Table 4
Claims (4)
1. a kind of method using half water law Wet-process Phosphoric Acid Production fertilizer potassium dihydrogen phosphate, it is characterized in that, including following technique mistake
Journey：Half water law phosphoric acid by wet process is added into ground phosphate rock and carries out desulfurization, the slurry after desulfurization is filtered, filter residue feeding phosphoric acid system,
Filtrate enters a neutralization chamber, adds potassium hydroxide and neutralizes, and neutralize slip pH value of regulation is 2.0-2.5, reaction time
1.5-3.0 hour；30-50 DEG C of reaction temperature；One time neutralize slip is filtered, and filter residue adds N P and K by 2%-10% and is combined
In fertilizer, and nitrogen-phosphorus-potassium compound fertilizer index is not influenceed, filtrate enters secondary neutralization chamber, add the secondary neutralization of potassium hydroxide, regulation
Secondary neutralize slip pH value is 3.0-3.5, reaction time 1.5-3.0 hour, 30-50 DEG C of reaction temperature；Secondary neutralize slip is entered
Row filtering, filter residue is as the additive of calcium hydrophosphate fodder, and filtrate enters three neutralization chambers, adds in potassium hydroxide three times
With, adjust three times and neutralize pH value for 4.2-4.7, reaction time 2.0-6.0 hour, 50-70 DEG C of reaction temperature；Three neutralize slips
Evaporation concentration device concentration is delivered to, the slurry that the supersaturated solution after concentration enters after crystallisation by cooling groove, crystallisation by cooling passes through
Filter, mother liquor, which returns one, two, three and neutralized, is used as potassium hydroxide preparation water, and the crystal obtained by filtering is potassium dihydrogen phosphate, dry,
Metering, packaging produce potassium dihydrogen phosphate finished product.
2. a kind of method using half water law Wet-process Phosphoric Acid Production fertilizer potassium dihydrogen phosphate according to claim 1, it is special
Levying is, half water law phosphoric acid by wet process desulfurization add ground phosphate rock amount according to sulphur and calcium oxide mol ratio be 1:1~1：3. during reaction
Between 1.0-3.0 hours；30-80 DEG C of reaction temperature.
3. a kind of method using half water law Wet-process Phosphoric Acid Production fertilizer potassium dihydrogen phosphate according to claim 1, it is special
Levying is, first and second neutralizes concentration of potassium hydroxide for 15-30%.
4. a kind of method using half water law Wet-process Phosphoric Acid Production fertilizer potassium dihydrogen phosphate according to claim 1, it is special
Levying is, three neutralization filtrated stocks are used as potassium hydroxide preparation water.
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| CN106744762A (en) * | 2017-01-20 | 2017-05-31 | 昆明川金诺化工股份有限公司 | One kind with half water phosphoric acid multistage be directly produced industrial grade monoammonium phosphate method |
| CN108046226B (en) * | 2017-12-22 | 2020-11-20 | 贵阳开磷化肥有限公司 | Production method for co-production of industrial-grade ammonium dihydrogen phosphate and water-soluble fertilizer |
| CN116216673A (en) * | 2022-12-29 | 2023-06-06 | 瓮福（集团）有限责任公司 | Production process of monopotassium phosphate |
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| CN103072963B (en) * | 2012-12-28 | 2014-11-05 | 金正大生态工程集团股份有限公司 | Method for producing potassium dihydrogen phosphate through wet-process phosphoric acid |
| CN103159195A (en) * | 2013-04-12 | 2013-06-19 | 成都川科化工有限公司 | Method for preparing potassium dihydrogen phosphate from low-concentration wet-process phosphoric acid |
| CN103771380B (en) * | 2013-11-08 | 2016-06-29 | 昆明川金诺化工股份有限公司 | A kind of method utilizing Wet-process Phosphoric Acid Production industrial phosphoric acid salt |
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