CN104261377B - A kind of production method preparing potassium primary phosphate by-product shepherd's purse special fertilizer - Google Patents
A kind of production method preparing potassium primary phosphate by-product shepherd's purse special fertilizer Download PDFInfo
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Abstract
The present invention relates to chemical technology field, especially a kind of production method preparing potassium primary phosphate by-product shepherd's purse special fertilizer, by carrying out research and analysis to the demand of shepherd's purse nutrient composition content, and carry out regulating to the constituent content in production process and arrange in pairs or groups, make the composite fertilizer of the chemical combination state prepared can meet the demand of crop to greatest extent, and reduce in composite heat transfer because element mismatch, the high cost caused, further avoid too much element to drop among soil, that causes composite fertilizer solidifies soil and contaminate environment.
Description
Technical field
The present invention relates to chemical technology field, especially a kind of production method preparing potassium primary phosphate by-product shepherd's purse special fertilizer.
Background technology
Common fertilizer is after arable land applies, and a part is rising, dissipation and outflowing with water, and a part is fixed by soil and soil microorganisms and utilized, and only has a part wherein just absorbed by crops and utilize.Show after deliberation: the utilization ratio of urea, carbon ammonium is 20% one 46%, phosphate fertilizer (two ammoniums, an ammonium, coarse whiting) is 10% one 25%, potash fertilizer 45% one 60%.As can be seen here, common fertilizer utilization ratio is very low.
By the research to the demand analysis of shepherd's purse macronutrient and traditional nitrogen-phosphorus-potassium compound fertilizer nutrient composition content of use, can learn, the N P and K that shepherd's purse requires conventional composite fertilizer is nitrogen 16%, phosphorus 7%, potassium 7%, total amount reaches more than 30%, therefore, the effective absorbed dose for the nitrogen of nitrogen-phosphorus-potassium compound fertilizer, phosphorus, potassium element is 3.2-7.5%, effective absorbed dose of phosphorus is 0.7-1.75%, effective absorbed dose of potash fertilizer is 3.15-4.2%; As can be seen here, the simple combination of traditional N P and K compound and collocation, make a large amount of n p k nutrition elements can be left in soil, by the long-term conversion of soil and loss, and then cause n p k nutrition element to harden soil and contaminate environment, waste natural resources.
In addition, in the preparation process of potassium dihydrogen phosphate product, normally adopt cooling down crystallization treatment, potassium dihydrogen phosphate product in stock liquid is reached capacity after under state by crystallization, and in traditional potassium primary phosphate production technique, in order to resources such as the potassium primary phosphates that the liquid that do not waste raw material contains, be usually potassium primary phosphate is carried out circulation crystallization process, make the potassium primary phosphate in stock liquid by a large amount of crystallizations, and then improve the output of potassium dihydrogen phosphate product, , the purity of the potassium dihydrogen phosphate product prepared according to above method is lower, because, while potassium primary phosphate thoroughly crystallizes out, with a large amount of calcium in the potassium dihydrogen phosphate product process adopting phosphoric acid by wet process or thermal phosphoric acid to prepare, magnesium, aluminium, the chemical elements such as iron, and then while the thorough crystallization of potassium primary phosphate, also other metal phosphates or dihydrogen phosphate quilt crystallization is simultaneously had, and then greatly reduce the purity of the potassium dihydrogen phosphate product produced, for this reason, a separating and filtering technique will be added purification processes is carried out to potassium dihydrogen phosphate product, the cost preparing potassium dihydrogen phosphate product is strengthened greatly.
Simultaneously, for the preparation of complex fertilizer product, what generally adopt in traditional technology is that multiple compound that is organic or inorganic chemical state is obtained by mixing, and the component content of various compound is adjusted according to the demand of crop n p k nutrition element, and then guarantee to provide the demand of the nutritive element meeting certain plant growth, but a large amount of n-p-k elements will be caused in the process to arrange in pairs or groups unreasonable because of element, cause running off in soil, make soil compaction, waste natural resources and contaminate environment.
For this reason, this researchist is by effort for many years and discussion, in conjunction with existing isomorph technology, analyze the mechanism formed between multiple potash fertilizer, phosphate fertilizer, again in conjunction with the demand of the nutritive ingredient of shepherd's purse, to in the process of preparation potassium dihydrogen phosphate product, prepare shepherd's purse composite fertilizer special and provide a kind of new approaches.
Summary of the invention
In order to solve the above-mentioned technical problem existed in prior art, the invention provides a kind of production method preparing potassium primary phosphate by-product shepherd's purse special fertilizer, have by preparation potassium dihydrogen phosphate product process, the content of the n-p-k element in the mother liquor after separating out potassium primary phosphate carries out Detection & Controling, passing through Addition ofelements, the nutritive ingredient structure in the mother liquor after potassium dihydrogen phosphate product is separated out in adjustment, making to prepare need not degree of depth crystallization in the process of potassium dihydrogen phosphate product, also the waste of raw material resources can not be caused, shepherd's purse use composite fertilizer special can also be suitable for by by-product simultaneously, reduce the loss of elements that in composite fertilizer, various nutritive element causes because of mismatch and the feature of wasting soil compaction probability and the products production cost brought.
Be achieved particular by following technical scheme:
A kind of production method preparing potassium primary phosphate by-product shepherd's purse special fertilizer, phosphoric acid is adopted to be (1.4-1.8) with carboxamide according to mol ratio: 1 mixes, and be that 15 DEG C/min is warming up to 100-120 DEG C with heat-up rate, stirring reaction 4-5h, obtains intermediate slip, this intermediate slip is adopted to mix with 1.4-1.5mol alkaline potassium salt again, after reaction terminates, obtain nitrogenous, phosphorus, the slip of potassium, and by nitrogenous, phosphorus, the slip of potassium is placed in cooling crystallizer and carries out decrease temperature crystalline filtration treatment, make filtrate circulation crystallization process in cooling crystallizer, and detect analysis filtrate, when the content of nitrogen component is 3.2-7.5%, Vanadium Pentoxide in FLAKES component content is 1-2%, when potassium oxide component content is 3-5%, stop crystallization and filter, the filter cake obtained is potassium dihydrogen phosphate product, in filtrate, add trace compound adjustment become chemical combination state composite fertilizer just finished product, and first finished product is placed in baker, adopt heat-up rate to be that 3 DEG C/min is warming up to 45-55 DEG C, after dry 0.5-1h, adjustment moisture content is 2-3%, can obtain shepherd's purse special fertilizer.
Described phosphoric acid and carboxamide react, and are phosphoric acid solution and carboxamide solid reaction.
Described phosphoric acid and carboxamide react, and are phosphoric acid solution and carboxamide liquid reactions.
Described phosphoric acid and carboxamide react, and are phosphoric acid solid and carboxamide liquid reactions.
Described alkaline potassium salt is one or both mixtures in Repone K, saltpetre, potassium sulfate, and when for two kinds of mixtures, mol ratio is followed successively by 1:2, and the total moles of potassium ion is 1.3-1.4mol; Described trace compound is CaSO
4, MgSO
4, Fe
2+inner complex, one or more mixtures in humic acid.
Described sponge gourd special fertilizer is chemical combination state composite fertilizer, and wherein effective constituent is for containing
ionic state structural formula, the dotted line wherein between carbon atom and Sauerstoffatom represents to there is coordinate bond between C atom and O atom.
Urea and phosphoric acid are reacted under heat-up rate is the temperature environment of 15 DEG C/min, generates Ureaphil, and along with the progressively rising of temperature, and then make the coordinate bond dialysis between Ureaphil and form two kinds of ion like materials, be namely exactly
when
ion is in phosphoric acid environment, will be close with phosphoric acid, and then carries out ionic polymerization under temperature environment when the dialysis of Ureaphil coordinate bond, makes
ion and phosphoric acid generate
intermediate-ion, make containing a large amount of dihydrogen phosphates in solution, when adding potassium ion compound, dihydrogen phosphate and potassium ion react and generate potassium primary phosphate, and in succession reach capacity simultaneously; When potassium content is excessive, will reacts with the ammonium radical ion in intermediate-ion, further make intermediate-ion chelating become
intermediate-ion, and with positive charge, and then when participating in other electronegative ions or compound in solution, compound salt will be formed with this ion, further enriching the nutritive ingredient in product.
Meanwhile, when in solution containing a large amount of affect the element of fertilizer impurity time, it not easily generates colloid, and then makes the character of fertilizer unaffected:
In process as Wet-process Phosphoric Acid Production potassium dihydrogen phosphate product, the elements such as a large amount of iron, magnesium, aluminium can produce colloid in the solution, and then affect the technique ease of potassium dihydrogen phosphate product preparation process, make in potassium dihydrogen phosphate product preparation process, removal of impurities cost is larger; Iron ion, magnesium ion, aluminum ion are positively charged gas ions, and then interference can not be formed to intermediate-ion, solution and another formation with elements such as iron, magnesium, aluminium of intermediate-ion easily decompose intermediate-ion body on the contrary, make fully to be absorbed by crop.
Compared with prior art, the technique effect of technical scheme of the present invention is embodied in:
1, by carrying out research and analysis to the demand of shepherd's purse nutrient composition content, and carry out regulating to the constituent content in production process and arrange in pairs or groups, make the composite fertilizer of the chemical combination state prepared can meet the demand of crop to greatest extent, and reduce in composite heat transfer because element mismatch, the high cost caused, further avoid too much element to drop among soil, that causes composite fertilizer solidifies soil and contaminate environment.
2, by controlling the processing condition of producing, make in sponge gourd special fertilizer preparation process, highly purified potassium dihydrogen phosphate product can be produced, compensate for removal of impurities cost when traditional wet phosphoric acid prepares potassium dihydrogen phosphate product, make the purity of the potassium dihydrogen phosphate product prepared reach more than 95%, production cost reduces 93%; Make each element in the shepherd's purse composite fertilizer special prepared equal proportion amount to be absorbed by shepherd's purse fully simultaneously, can't remain in soil and easily be combined with soil with other, the state of matter that soil is hardened exists, and then avoids environmental pollution.
3, by production process, the mol ratio of raw material, in crystallisation step, the accurate analysis of filtrate and detection, the quality of the shepherd's purse composite fertilizer produced is guaranteed, and with adjusting the mode of filtrate component content, using the raw material of the waste liquid in Chemicals production process as composite heat transfer, avoid the discharge of waste liquid, reduce composite heat transfer cost.
4, by technical parameter in chemical combination state compound fertilizer production technology, namely be exactly temperature, the control of material concentration and proportioning, after making phosphoric acid and urea reaction, generate Ureaphil product, Ureaphil product itself has stronger acidity, and between phosphoric acid and urea, be the chemical combination state double salt be combined together to form by the mode of coordinate bond, also be fertile as crop in conventional art, and crop is to the specific absorption comparison urea of this chemical combination state double salt, volatile salt, the unitary such as ammonium nitrate, binary fertilizer specific absorption is a kind of chemical combination state composite fertilizer all preferably, but, under the environment that this chemical combination state double salt exists at phosphoric acid, at the temperature of 80-250 DEG C, complicated decomposition polyreaction can be there is, Ureaphil is made to form (H
2pO
4)
-(H
2nCONH
3)
+two ions, (H
2nCONH
3)
+ion and phosphoric acid close, and be under the environment of 80-160 DEG C in temperature, formed
intermediate-ion and dihydrogen phosphate, and coordinate bond is formed between C and O, this intermediate-ion can form multielement intermediate-ion with centering element compound chelating, and then the compound electronegative with other can be continued or ion forms inner complex, improve constituent content in double salt, and then the nutrient content that can adjust in the double salt of this ion existence, simultaneously, this inner complex can be hydrolyzed again and by crop, and then fertilizer efficiency can be provided for crop effectively for a long time, simultaneously, in conjunction with the mensuration of constituent content in the solution existed this ion, and then each constituent content during formation of adjustment double salt, dry and obtain chemical combination state double salt composite fertilizer, make the quality product of chemical combination state double salt composite fertilizer can meet the requirement composite fertilizer special of shepherd's purse nutritive ingredient.
Embodiment
Below in conjunction with concrete embodiment, further restriction is done to technical scheme of the present invention, but claimed scope is not only confined to done description.
Principle illustrates:
The present invention carries out research and discussion by the mechanism of reacting phosphoric acid and carboxamide, and arrives in conjunction with prior art literature, and phosphoric acid and carboxamide react and generate Ureaphil, and its molecular formula is: CO (NH
2)
2.H
3pO
4under the environment of comparatively high temps, the chemical bond meeting dialysis between H and O in phosphoric acid, hydrogen ion is combined the ionic state formed containing positive charge with urea, the ion double salt making Ureaphil form a kind of positive and negative charge to attract mutually, its mechanism structural response following expression: CO (NH
2)
2.H
3pO
4→ (H
2pO
4)
-● (H
2nCONH
3)
+
Further, under the environment that Ureaphil ion double salt exists at phosphoric acid, (H wherein
2nCONH
3)
+positive ion and phosphoric acid close, form the intermediate-ion of C → O coordinate bond, be (CO
5pN
2h
8)
+, and then make in Ureaphil intermediate containing a large amount of (H
2pO
4)
-(CO
5pN
2h
8)
+ion, when adding excessive and appropriate potassium ion, dihydrogen phosphate and potassium ion form potassium dihydrogen phosphate crystal and are precipitated, unnecessary potassium ion and (CO
5pN
2h
8)
+ionic reaction, and displace part NH
4 +, make in solution containing (CO
5pNH
4k)
+double salt ion, and analyze by detecting and control the content of N in solution, P, K element, the chemical combination state composite fertilizer containing N, P, K element can be obtained at heat drying.
Its concrete reaction principle will carry out further instruction by following reaction structure formula and reaction mechanism:
Reaction formula one:
CO(NH
2)
2+H
3PO
4→CO(NH
2)
2.H
3PO
4
Reaction formula two:
Reaction formula three:
Wherein, the dotted line between carbon atom and Sauerstoffatom represents to there is coordinate bond between C atom and O atom.
Reaction formula four:
Wherein, the dotted line between carbon atom and Sauerstoffatom represents to there is coordinate bond between C atom and O atom.
Noun illustrates:
Ureaphil (Ureaphosphate, UP), No. CAS is 4861-19-2, and molecular formula is CH
7n
2o
5p, can be expressed as CO (NH
2)
2h
3pO
4:
It is a kind of fine chemical product being widely used in the fields such as livestock industry, industry, agricultural, its solid is white crystals or crystalline powder, and soluble in water and alcohol is insoluble to ethers, toluene and tetracol phenixin, the aqueous solution, in acid, start during melting to decompose and releases carbonic acid gas and ammonia.Embodiment: with concrete operation embodiment, the present invention is further elaborated below.
Embodiment: with concrete operation embodiment, the present invention is further elaborated below.
Phosphoric acid is prepared in potassium dihydrogen phosphate product process in a wet process, to be combined with urea by phosphoric acid and react, after obtained Ureaphil intermediate, adopt intermediate with carry out containing the compound of potassium element reacting prepare potassium dihydrogen phosphate product processing step based on, adjusting process parameter, its temperature is made to reach the temperature of reaction of 100-120 DEG C, and adopt the heat-up rate of 15 DEG C/min to carry out the process of intensification stirring reaction, stirring velocity controls at 140-200r/min, and then make temperature-controllable in reaction process, and regulate pH value, make the product state in reaction process controlled, and by crystallisation process, the control of the amount of potassium dihydrogen phosphate product, the impurity in filtrate is made to be difficult to be crystallized out, and then purifying potassium dihydrogen phosphate product, and in conjunction with Addition ofelements adjustment filtrate structure in filtrate, make in filtrate, to form a kind of Chelating state compound, and by after drying, obtain the special efficient composite fertilizer being suitable for shepherd's purse and using.
Embodiment 1
Prepare a production method for potassium primary phosphate by-product shepherd's purse special fertilizer, comprise the following steps:
(1) raw material preparation mixing: be that 1.4:1 is in stirring-type reactor according to mol ratio by phosphoric acid and carboxamide, be that 15 DEG C/min is warming up to 120 DEG C with heat-up rate, the stirring velocity controlling stirring tank is that 200r/min is uniformly mixed reaction 5h, obtains intermediate slip;
(2) KH is prepared
2pO
4: again the alkaline potassium salt 4h of 1.5mol is at the uniform velocity added containing in steps 1) in the reactor of obtained intermediate slip, and employing stirring speed is 200r/min stirring reaction 60min, obtains nitrogenous, phosphorus, potassium slip;
(3) circulation crystallization filters: by step 2) obtain nitrogenous, phosphorus, potassium slip and be placed in cooling crystallizer and be cooled to temperature 20 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, until nitrogen component content be 7.5%, Vanadium Pentoxide in FLAKES component content is 2%, potassium oxide component content is 5% time, stop crystallization and filter, acquisition filter cake is potassium primary phosphate, and in filtrate, add other trace compounds adjustment fertilizer structure becomes chemical combination state composite fertilizer just finished product;
(4) filtrate dries: by step 3) the chemical combination state composite fertilizer that obtains just finished product be placed in baker, adopt heat-up rate to be that 3 DEG C/min is warming up to 55 DEG C, dry 1.2h, adjustment moisture content is 2%, detects packaging, can obtain shepherd's purse special fertilizer.
Described phosphoric acid and carboxamide react, and are phosphoric acid solution and carboxamide solid reaction.
Described alkaline potassium salt is Repone K.
Described trace compound is 0.05%CaSO
4, 0.008%MgSO
4, 0.007%Fe
2+inner complex, 0.8% humic acid mixture.
Embodiment 2
Prepare a production method for potassium primary phosphate by-product shepherd's purse special fertilizer, comprise the following steps:
(1) raw material preparation mixing: be that 1.8:1 is in stirring-type reactor according to mol ratio by phosphoric acid and carboxamide, be that 15 DEG C/min is warming up to 100 DEG C with heat-up rate, the stirring velocity controlling stirring tank is that 180r/min is uniformly mixed reaction 4h, obtains intermediate slip;
(2) KH is prepared
2pO
4: again the alkaline potassium salt 3h of 1.4mol is at the uniform velocity added containing in steps 1) in the reactor of obtained intermediate slip, and employing stirring speed is 160r/min stirring reaction 40min, obtains nitrogenous, phosphorus, potassium slip;
(3) circulation crystallization filters: by step 2) obtain nitrogenous, phosphorus, potassium slip and be placed in cooling crystallizer and be cooled to temperature 19 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, until nitrogen component content be 3.2%, Vanadium Pentoxide in FLAKES component content is 1%, potassium oxide component content is 3% time, stop crystallization and filter, acquisition filter cake is potassium primary phosphate, and in filtrate, add other trace compounds adjustment fertilizer structure becomes chemical combination state composite fertilizer just finished product;
(4) filtrate dries: by step 3) the chemical combination state composite fertilizer that obtains just finished product be placed in baker, adopt heat-up rate to be that 3 DEG C/min is warming up to 45 DEG C, dry 1.1h, adjustment moisture content is 1%, detects packaging, can obtain shepherd's purse special fertilizer.
Described phosphoric acid and carboxamide react, and are phosphoric acid solution and carboxamide liquid reactions.
Described alkaline potassium salt is saltpetre.
Described trace compound is 0.008%MgSO
4, 0.007%Fe
2+inner complex, 0.8% humic acid mixture.
Embodiment 3
Prepare a production method for potassium primary phosphate by-product shepherd's purse special fertilizer, comprise the following steps:
(1) raw material preparation mixing: be that 1.5:1 is in stirring-type reactor according to mol ratio by phosphoric acid and carboxamide, be that 15 DEG C/min is warming up to 105 DEG C with heat-up rate, the stirring velocity controlling stirring tank is that 190r/min is uniformly mixed reaction 4.2h, obtains intermediate slip;
(2) KH is prepared
2pO
4: again the alkaline potassium salt 3.3h of 1.45mol is at the uniform velocity added containing in steps 1) in the reactor of obtained intermediate slip, and employing stirring speed is 180r/min stirring reaction 50min, obtains nitrogenous, phosphorus, potassium slip;
(3) circulation crystallization filters: by step 2) obtain nitrogenous, phosphorus, potassium slip and be placed in cooling crystallizer and be cooled to temperature 18 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, until nitrogen component content be 5.5%, Vanadium Pentoxide in FLAKES component content is 1.5%, potassium oxide component content is 4% time, stop crystallization and filter, acquisition filter cake is potassium primary phosphate, and in filtrate, add other trace compounds adjustment fertilizer structure becomes chemical combination state composite fertilizer just finished product;
(4) filtrate dries: by step 3) the chemical combination state composite fertilizer that obtains just finished product be placed in baker, adopt heat-up rate to be that 3 DEG C/min is warming up to 50 DEG C, dry 1.1h, adjustment moisture content is 1.5%, detects packaging, can obtain shepherd's purse special fertilizer.
Described phosphoric acid and carboxamide react, and are phosphoric acid solid and carboxamide liquid reactions.
Described alkaline potassium salt is potassium sulfate.
Described trace compound is 0.05%CaSO
4, 0.8% humic acid mixture.
Embodiment 4
Prepare a production method for potassium primary phosphate by-product shepherd's purse special fertilizer, comprise the following steps:
(1) raw material preparation mixing: be that 1.7:1 is in stirring-type reactor according to mol ratio by phosphoric acid and carboxamide, be that 15 DEG C/min is warming up to 110 DEG C with heat-up rate, the stirring velocity controlling stirring tank is that 195r/min is uniformly mixed reaction 4.5h, obtains intermediate slip;
(2) KH is prepared
2pO
4: again the alkaline potassium salt 3.8h of 1.48mol is at the uniform velocity added containing in steps 1) in the reactor of obtained intermediate slip, and employing stirring speed is 190r/min stirring reaction 55min, obtains nitrogenous, phosphorus, potassium slip;
(3) circulation crystallization filters: by step 2) obtain nitrogenous, phosphorus, potassium slip and be placed in cooling crystallizer and be cooled to temperature 17 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, until nitrogen component content be 6.5%, Vanadium Pentoxide in FLAKES component content is 1.8%, potassium oxide component content is 4.5% time, stop crystallization and filter, acquisition filter cake is potassium primary phosphate, and in filtrate, add other trace compounds adjustment fertilizer structure becomes chemical combination state composite fertilizer just finished product;
(4) filtrate dries: by step 3) the chemical combination state composite fertilizer that obtains just finished product be placed in baker, adopt heat-up rate to be that 3 DEG C/min is warming up to 48 DEG C, dry 1.2h, adjustment moisture content is 1.3%, detects packaging, can obtain shepherd's purse special fertilizer.
Described phosphoric acid and carboxamide react, and are phosphoric acid solution and carboxamide solid reaction.
Described alkaline potassium salt is the mixture of Repone K, saltpetre, and mol ratio is 1:2.
Described trace compound is 0.05%CaSO
4, 0.8% humic acid mixture.
Embodiment 5
Prepare a production method for potassium primary phosphate by-product shepherd's purse special fertilizer, comprise the following steps:
(1) raw material preparation mixing: be that 1.6:1 is in stirring-type reactor according to mol ratio by phosphoric acid and carboxamide, be that 15 DEG C/min is warming up to 115 DEG C with heat-up rate, the stirring velocity controlling stirring tank is that 185r/min is uniformly mixed reaction 4.3h, obtains intermediate slip;
(2) KH is prepared
2pO
4: again the alkaline potassium salt 3.3h of 1.48mol is at the uniform velocity added containing in steps 1) in the reactor of obtained intermediate slip, and employing stirring speed is 170r/min stirring reaction 53min, obtains nitrogenous, phosphorus, potassium slip;
(3) circulation crystallization filters: by step 2) obtain nitrogenous, phosphorus, potassium slip and be placed in cooling crystallizer and be cooled to temperature 16 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, until nitrogen component content be 3.8%, Vanadium Pentoxide in FLAKES component content is 1.9%, potassium oxide component content is 3.8% time, stop crystallization and filter, acquisition filter cake is potassium primary phosphate, and in filtrate, add other trace compounds adjustment fertilizer structure becomes chemical combination state composite fertilizer just finished product;
(4) filtrate dries: by step 3) the chemical combination state composite fertilizer that obtains just finished product be placed in baker, adopt heat-up rate to be that 3 DEG C/min is warming up to 53 DEG C, dry 1.1h, adjustment moisture content is 1.6%, detects packaging, can obtain shepherd's purse special fertilizer.
Described phosphoric acid and carboxamide react, and are phosphoric acid solid and carboxamide liquid reactions.
Described alkaline potassium salt is the mixture of saltpetre, potassium sulfate, and mol ratio is 1:2.
Described trace compound is 0.007%Fe
2+inner complex, 0.8% humic acid mixture.
Test example: the technique effect of technical scheme of the present invention and product performance are described further below in conjunction with specific embodiment content.
The simultaneous test of test example 1 composite fertilizer's consumption and shepherd's purse growing state
1.1 test process
Traditional plantation technique that all adopts of following test group and control group is planted, and consumption is 0.24kg.
Experimental group: adopt the shepherd's purse specific complex fertilizer product for preparing of embodiments of the invention 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5 to carry out experimental group test.
Control group 1: adopt the patent No. be 200410073243.4 " isomorphically synthesized ammonium-potassium phosphate sosoloid compound manure and preparation method thereof " preparing product carry out the planting experiment of shepherd's purse.
Control group 2: adopt traditional multiple chemical fertilizer according to the fertile planting experiment carrying out shepherd's purse of demand preparation mixing of shepherd's purse nutritive element.
Control group 3: what adopt farm manure equal proportion amount uses the planting experiment carrying out shepherd's purse.
1.2 test-results
| To apply fertilizer internal lobe look changing conditions in a January (6 days test once) | Strain fabric width degree | Per mu yield | |
| Embodiment 1 | Light green → green → dark green → dark green → dark green | 8-9.1cm | 540kg |
| Embodiment 2 | Light green → light green → green → dark green → dark green | 8.3-8.8cm | 495kg |
| Embodiment 3 | Light green → light green → light green → green → dark green | 8.2-9.4cm | 521kg |
| Embodiment 4 | Light green → green → dark green → dark green → dark green | 8.1-9.2cm | 532kg |
| Embodiment 5 | Light green → green → dark green → dark green → dark green | 8.7-9.3cm | 529kg |
| Control group 1 | Light green → green → dark green → pale yellow → yellowing | 6.5-8.9cm | 487kg |
| Control group 2 | Light green → green → dark green → pale yellow → yellow | 6.3-7.8cm | 468kg |
| Control group 3 | Light green → green → green → pale yellow → yellow | 5.4-6.9cm | 459kg |
As can be seen from feature instantiation and data presentation in table, chemical combination state composite fertilizer of the present invention can promote the growth of shepherd's purse, improves the per mu yield of shepherd's purse, and the effect of the composite fertilizer of preparing than traditional composite fertilizer, base manure, isomorph is comparatively remarkable.
Test example 2 shepherd's purse is to nutritive ingredient absorbing state simultaneous test
2.1 test process
Experimental group: the employing embodiment of the present invention 1, embodiment 2, embodiment 3, embodiment 4, the shepherd's purse composite fertilizer special that the production method of embodiment 5 is produced carry out nutritive medium soilless culture to shepherd's purse.
Control group: adopt traditional shepherd's purse composite fertilizer formulated according to the demand of shepherd's purse n p k nutrition element to carry out nutritive medium soilless culture.
Method: until cultivation shepherd's purse after 1 month, the content of n p k nutrition composition in determination experiment group and control group.
Fertilising consumption: experimental group and control group fertilizer are 0.5kg.
2.2 test-results
As can be seen from upper table data presentation, shepherd's purse special fertilizer of the present invention can be absorbed in a large number by shepherd's purse, and the content of n-p-k element all has raising in a big way in the nutritive medium of control group before comparing cultivation, simultaneously, in conjunction with shepherd's purse upgrowth situation feature, visible, shepherd's purse special fertilizer of the present invention can better be absorbed by shepherd's purse, and then the nutritive ingredient in maintenance primary soil, guarantee the quality in soil, the state that Nitrogen In Soils phosphorus potassium element also can not be caused too much to harden occurs, and compared with traditional composite fertilizer, has significant effect.
Test example 3 potassium dihydrogen phosphate product purity detecting is tested
3.1 experimental techniques:
Adopt traditional colorimetry content detection respectively, the purity obtaining potassium dihydrogen phosphate product in embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5 is detected.
3.2 experimental result
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| KH 2PO 4(％) | 98.1 | 98.5 | 98.9 | 98.8 | 99.3 |
As can be seen from upper table data presentation, the purity of the potassium dihydrogen phosphate product produced can reach more than 98%, simultaneously, in conjunction with production craft step, the technological method that the present invention purifies is comparatively simple, and is combined with purification process by potassium dihydrogen phosphate product crystallisation process, shortens technical process, shorten the production cycle, reduce production cost; Also can not make to remain in potassium primary phosphate in crystal solution and other nutritive element is not wasted simultaneously, after drying, and acquisition meets the fertile standard of shepherd's purse, and the intermediate-ion body containing polymer phosphate urea, enhance the chemical combination rate of composite fertilizer, the technical problem of traditional Chemical Mixed Fertilizer technology is solved by intermediate-ion body, visible, the present invention, while potassium dihydrogen phosphate product is purified, avoids the tail liquid emissions of chemical technique, has the remarkable value of environmental protection.
It is important to point out at this; above embodiment and test example are only limitted to be further elaborated technical scheme of the present invention and understand; the further restriction to technical scheme of the present invention can not be interpreted as; the essential characteristics of the non-protruding that those skilled in the art make on this basis and significant progressive innovation and creation, still belong to protection category of the present invention.
Claims (7)
1. prepare the production method of potassium primary phosphate by-product shepherd's purse special fertilizer for one kind, it is characterized in that, adopt phosphoric acid to be (1.4-1.8) with carboxamide according to mol ratio: 1 mixes, and is that 15 DEG C/min is warming up to 100-120 DEG C with heat-up rate, stirring reaction 4-5h, obtains intermediate slip, this intermediate slip is adopted to mix with 1.4-1.5mol alkaline potassium salt again, after reaction terminates, obtain nitrogenous, phosphorus, the slip of potassium, and by nitrogenous, phosphorus, the slip of potassium is placed in cooling crystallizer and carries out decrease temperature crystalline filtration treatment, make filtrate circulation crystallization process in cooling crystallizer, and detect analysis filtrate, when the content of nitrogen component is 3.2-7.5%, Vanadium Pentoxide in FLAKES component content is 1-2%, when potassium oxide component content is 3-5%, stop crystallization and filter, the filter cake obtained is potassium dihydrogen phosphate product, in filtrate, add trace compound adjustment become chemical combination state composite fertilizer just finished product, and first finished product is placed in baker, adopt heat-up rate to be that 3 DEG C/min is warming up to 45-55 DEG C, after dry 0.5-1h, adjustment moisture content is 2-3%, can obtain shepherd's purse special fertilizer.
2. prepare the production method of potassium primary phosphate by-product shepherd's purse special fertilizer as claimed in claim 1, it is characterized in that, comprise the following steps:
(1) raw material preparation mixing: be (1.4-1.8) according to mol ratio by phosphoric acid and carboxamide: 1 in stirring-type reactor, be that 15 DEG C/min is warming up to 100-120 DEG C with heat-up rate, the stirring velocity controlling stirring tank is that 180-200r/min is uniformly mixed reaction 4-5h, obtains intermediate slip;
(2) KH is prepared
2pO
4: again the alkaline potassium salt 3-4h of 1.4-1.5mol is at the uniform velocity added containing in steps 1) in the reactor of obtained intermediate slip, and employing stirring speed is 160-200r/min stirring reaction 40-60min, obtains nitrogenous, phosphorus, potassium slip;
(3) circulation crystallization filters: by step 2) obtain nitrogenous, phosphorus, potassium slip and be placed in cooling crystallizer and be cooled to temperature≤20 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, until nitrogen component content be 3.2-7.5%, Vanadium Pentoxide in FLAKES component content is 1-2%, potassium oxide component content is 3-5% time, stop crystallization and filter, acquisition filter cake is potassium primary phosphate, and in filtrate, add other trace compounds adjustment fertilizer structure becomes chemical combination state composite fertilizer just finished product;
(4) filtrate dries: by step 3) the chemical combination state composite fertilizer that obtains just finished product be placed in baker, adopt heat-up rate to be that 3 DEG C/min is warming up to 45-55 DEG C, dry 1.1-1.2h, adjustment moisture content is 1-2%, detect packaging, shepherd's purse special fertilizer can be obtained.
3. prepare the production method of potassium primary phosphate by-product shepherd's purse special fertilizer as claimed in claim 1 or 2, it is characterized in that, described phosphoric acid and carboxamide react, and are phosphoric acid solution and carboxamide solid reaction.
4. prepare the production method of potassium primary phosphate by-product shepherd's purse special fertilizer as claimed in claim 1 or 2, it is characterized in that, described phosphoric acid and carboxamide react, and are phosphoric acid solution and carboxamide liquid reactions.
5. prepare the production method of potassium primary phosphate by-product shepherd's purse special fertilizer as claimed in claim 1 or 2, it is characterized in that, described phosphoric acid and carboxamide react, and are phosphoric acid solid and carboxamide liquid reactions.
6. prepare the production method of potassium primary phosphate by-product shepherd's purse special fertilizer as claimed in claim 1 or 2, it is characterized in that, described alkaline potassium salt is one or both mixtures in Repone K, saltpetre, potassium sulfate, when for two kinds of mixtures, mol ratio is followed successively by 1:2, and the total moles of potassium ion is 1.3-1.4mol; Described trace compound is CaSO
4, MgSO
4, Fe
2+inner complex, one or more mixtures in humic acid.
7. prepare the production method of potassium primary phosphate by-product shepherd's purse special fertilizer as claimed in claim 1 or 2, it is characterized in that, described shepherd's purse special fertilizer is chemical combination state composite fertilizer, and wherein effective constituent is for containing
ionic state structural formula, the dotted line wherein between carbon atom and Sauerstoffatom represents to there is coordinate bond between C atom and O atom.
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| US7588744B1 (en) * | 2008-12-08 | 2009-09-15 | Layne Christensen Company | Method of recovering phosphate for reuse as a fertilizer |
| CN102951623B (en) * | 2012-11-15 | 2014-11-26 | 贵阳中化开磷化肥有限公司 | Production process for monopotassium phosphate |
| CN103754853A (en) * | 2014-01-24 | 2014-04-30 | 贵阳中化开磷化肥有限公司 | Method for preparing disodium hydrogen phosphate from wet-process phosphoric acid |
| CN104003362A (en) * | 2014-05-20 | 2014-08-27 | 贵阳中化开磷化肥有限公司 | Production method of dipotassium phosphate |
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