CN104310346B - A kind of production method preparing dipotassium hydrogen phosphate by-product spinach special fertilizer - Google Patents
A kind of production method preparing dipotassium hydrogen phosphate by-product spinach special fertilizer Download PDFInfo
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Abstract
The present invention relates to chemical technology field, especially a kind of production method preparing dipotassium hydrogen phosphate by-product spinach special fertilizer, by needing in fertile requirement according to spinach, effective absorbed dose of n-p-k element is analyzed, 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 spinach to greatest extent, and reduce in composite heat transfer because element mismatch, the high cost caused, too much element is further avoided to drop among soil, cause solidifying of composite fertilizer and contaminate environment.
Description
Technical field
The present invention relates to chemical technology field, especially a kind of production method preparing dipotassium hydrogen phosphate by-product spinach special fertilizer.
Background technology
Spinach, also known as field dish, formal name used at school: SpinaciaoleraceaL., belong to Amaranthaceae lamb's-quarters subfamily spinach and belong to, annual herb plant, ground is raw, level and smooth without hair, uprightly.Complete stool is smooth, and tender many moisture content, without powder.With a long history in Chinese cultivated, its leaf halberd shape or avette, tip is sharp-pointed, and petiole is elongated, and cold hardiness is comparatively strong, suitable overwintering cultivation.Stingless kind of blade oval, loose, many wrinkles, the blunt circle of tip, petiole is short, its heat hardiness is strong, output is high, suitable spring, summer or cultivation in late fall, and containing abundant nutritive element, there is abundant nutritive value, according to surveying and determination: every hectogram is containing 2 grams, protein, 0.2 gram, fat, carbohydrate 2 grams, robust fibre 0.6 gram, ash content 2 grams, calcium 70 milligrams, 34 milligrams, phosphorus, iron 2.5 milligrams, carotene 2.96 milligrams, VitB1 0.04 milligram, 0.13 milligram, riboflavin, nicotinic acid 0.6 milligram, 31 milligrams, xitix, oxalic acid is more than 0.1 gram, phytomelin 17 milligrams, 1.1 milligrams, fluorine, volume alpha-tocopherol, 6-hydroxymethyllumazin, therefore, a large amount of trace elements and other nutritive elements can be provided to human body.
But, fertilising at present for spinach plantation still adopts farm manure to use in conjunction with other chemical fertilizer mixing, and the spinach chemical combination state special fertilizer not having a kind of special nutritional needs for spinach plantation and design, but there is the proiprietary formula appearance carrying out chemical fertilizer for spinach fertilizer, this proiprietary formula is then use a large amount of existing chemical fertilizer to carry out compound together, form the fertilizer of mixed state, although the preparation of this fertilizer can meet spinach need fertile requirement, a large amount of n-p-k element mismatch can be caused, or absorbed unbalanced by spinach, the macroelement in the fertilizer used is caused to remain in soil, combination reaction is carried out with soil, soil is hardened, reduce soil property, contaminate environment, simultaneously, also a large amount of elements can be made by the waste of an innocent person, cause spinach large with fertile cost.
Dipotassium hydrogen phosphate is a kind of fertilizer containing phosphorus potassium element, can under the environment of 20 DEG C, and a large amount of is soluble in water, forms solution state, and then absorbed fully by crop with water, is a kind of phosphorus potash fertilizer efficiently.At present, the preparation technology for dipotassium hydrogen phosphate is more, but it is low mostly to there is the product purity produced, and needs to carry out removal of impurities process further, and make production cost comparatively large, production technique tail washings discharge capacity is large, the features such as phosphorus potassium element loss is large.
For this reason, need in the preparation process to dipotassium hydrogen phosphate product, while purification processes is carried out to dipotassium hydrogen phosphate product, reduce the infringement of phosphorus potassium element and other natural resourcess, and the added value of product improving whole production technique is studied.
Therefore, this researchist by effort for many years and exploration, and in conjunction with the need fertilizer requirement of spinach and the production technique of dipotassium hydrogen phosphate, provides a kind of new approaches to the preparation technology of dipotassium hydrogen phosphate product and the preparation of spinach special fertilizer.
Summary of the invention
In order to solve the above-mentioned technical problem existed in prior art, the invention provides one and can improve dipotassium hydrogen phosphate product purity, reduce production cost, and fertile requirement can be needed according to spinach, the trophic structure of the mother liquor in dipotassium hydrogen phosphate preparation technology is adjusted, and then produce spinach special fertilizer, improve the added value of product of dipotassium hydrogen phosphate production technique, reduce the production method preparing dipotassium hydrogen phosphate by-product spinach special fertilizer of environmental pollution.
Be achieved particular by following technical scheme:
A kind of production method preparing dipotassium hydrogen phosphate by-product spinach special fertilizer, phosphoric acid is adopted to be (1.3-1.9) with carboxamide according to mol ratio: 1 mixes, and be that 5 DEG C/min is warming up to 90-140 DEG C with heat-up rate, stirring reaction 3-5h, obtains intermediate slip, this intermediate slip is adopted to mix with 2.2-2.6mol alkaline potassium salt again, and to control temperature of reaction be 60 DEG C-80 DEG C, stirring reaction 20-70min, when detection pH value is 8-9.5, 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, work as nitrogen, Vanadium Pentoxide in FLAKES, the mass ratio of potassium oxide is (5-6): (3-4): time (3-5), stop crystallization and filter, the filter cake obtained is dipotassium hydrogen phosphate product, in filtrate, add trace compound be adjusted to 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 3-4%, can obtain spinach 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 the one in Repone K, saltpetre, potassium sulfate, potassium hydroxide, salt of wormwood, Potassium ethanoate.
Described trace compound is calcium sulfate, magnesium chloride, zinc chloride, Selenium monochloride, Fe
2+inner complex, humic acid mixture.
Described spinach special fertilizer is chemical combination state composite fertilizer, and its effective constituent has
in one or more mixtures.
By phosphoric acid and urea reaction, and controlled by temperature, mol ratio and other processing parameters, make the structural formula of Ureaphil that complicated polyreaction occur, make it be formed
intermediate-ion, this intermediate-ion has stronger stability, and between carbon Sauerstoffatom, also there is coordinate bond, a large amount of dihydrogen phosphates is contained in the solution that this ion exists simultaneously, therefore, when adding potassium ion in the solution to this intermediate-ion of existence, potassium ion reacts with the dihydrogen phosphate in solution gradually, form potassium primary phosphate, the amount added along with potassium ion increases gradually, and adjustable value pH value, potassium primary phosphate progressively changes into dipotassium hydrogen phosphate, and suitable excessive potassium ion, then intermediate-ion and potassium ion react, replace out part ammonium radical ion, intermediate-ion chelating is 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.
As added potassium sulfate in solution, the Determination of Potassium in adjustment solution, then can generate sulfenyl double salt chemical combination state composite fertilizer.
As added saltpetre in solution, the Determination of Potassium in adjustment solution and nitrogen element content, then can generate nitrate compound salt composite fertilizer.
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 dipotassium hydrogen 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 dipotassium hydrogen phosphate product preparation process, make in dipotassium hydrogen 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 needing fertilizer according to spinach, effective absorbed dose of n-p-k element is analyzed, 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 spinach to greatest extent, and reduce in composite heat transfer because element mismatch, the high cost caused, further avoids too much element to drop among soil, causes solidifying of composite fertilizer and contaminate environment.
(2) by controlling the processing condition of producing, make in fertilizer special for tobacco preparation process, highly purified dipotassium hydrogen phosphate product can be produced, compensate for removal of impurities cost when traditional wet phosphoric acid prepares dipotassium hydrogen phosphate product, the purity of the dipotassium hydrogen phosphate product prepared is made to reach more than 95%, production cost reduces 93%, has significant economic benefit.
(3) by production process, the mol ratio of raw material, in crystallisation step, the accurate analysis of filtrate and detection, make the quality of the spinach composite fertilizer produced be 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, there is the significant value of environmental protection and economic benefit.
(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 the composite fertilizer obtained containing chemical combination state double salt structure, improve the quality of spinach special fertilizer.
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)-and (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.
Reaction formula five:
obtain phosphoric acid hydrogen ammonia potassium double salt, the potassium ion in ammonium hydrogen phosphate potassium generates dipotassium hydrogen phosphate and phosphoric acid hydrogen ammonia radical ion with biphosphate nak response again, phosphoric acid hydrogen ammonia radical ion again with
intermediate-ion is combined to the Nitrogen-and Phosphorus-containing potassium double salt structure of chemical combination state, and then can adjust the N P and K chemical combination state composite fertilizer being suitable for spinach and using.
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 1
Prepare a production method for dipotassium hydrogen phosphate by-product spinach special fertilizer, comprise the following steps:
(1) raw material preparation mixing: be that 1.3:1 is in stirring-type reactor according to mol ratio by phosphoric acid and carboxamide, be that 5 DEG C/min is warming up to 90 DEG C with heat-up rate, the stirring velocity controlling stirring tank is that 180r/min is uniformly mixed reaction 3h, obtains intermediate slip;
(2) K is prepared
2hPO
4: again the alkaline potassium salt 2h of 2.2mol at the uniform velocity being added containing in steps 1) in the reactor of obtained intermediate slip, and to control temperature of reaction be 60 DEG C, stirring reaction 20min, when to detect pH value be 8, reaction terminates, and obtains nitrogenous, phosphorus, potassium slip;
(3) circulation crystallization filters: by step 2) obtain nitrogenous, phosphorus, potassium slip and be placed in cooling crystallizer 10s and be cooled to temperature 5 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, when the mass ratio of nitrogen component, Vanadium Pentoxide in FLAKES composition, potassium oxide composition is 5:3:3, stop crystallization and filter, acquisition filter cake is dipotassium hydrogen phosphate, and in filtrate, add trace compound 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 0.5h, adjustment moisture content is 3%, detects packaging, can obtain spinach special fertilizer.
Described phosphoric acid and carboxamide react, and are phosphoric acid solution and carboxamide solid reaction.
Described alkaline potassium salt is Repone K, and concentration is 30%.
Described trace compound is 0.05% calcium sulfate, 0.005% magnesium chloride, 0.007% zinc chloride, 0.004% Selenium monochloride, 0.006%Fe
2+inner complex, 0.08% humic acid mixture.
Detect the effective constituent of spinach special fertilizer, it is
Embodiment 2
Prepare a production method for dipotassium hydrogen phosphate by-product spinach special fertilizer, comprise the following steps:
(1) raw material preparation mixing: be that 1.9:1 is in stirring-type reactor according to mol ratio by phosphoric acid and carboxamide, be that 5 DEG C/min is warming up to 140 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) K is prepared
2hPO
4: again the alkaline potassium salt 3h of 2.6mol at the uniform velocity being added containing in steps 1) in the reactor of obtained intermediate slip, and to control temperature of reaction be 80 DEG C, stirring reaction 70min, when to detect pH value be 9.5, reaction terminates, and obtains nitrogenous, phosphorus, potassium slip;
(3) circulation crystallization filters: by step 2) obtain nitrogenous, phosphorus, potassium slip and be placed in cooling crystallizer 10s and be cooled to temperature 4 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, when the mass ratio of nitrogen component, Vanadium Pentoxide in FLAKES composition, potassium oxide composition is 5:4:5, stop crystallization and filter, acquisition filter cake is dipotassium hydrogen phosphate, and in filtrate, add trace compound 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 1h, adjustment moisture content is 4%, detects packaging, can obtain spinach special fertilizer.
Described phosphoric acid and carboxamide react, and are phosphoric acid solution and carboxamide liquid reactions.
Described alkaline potassium salt is potassium hydroxide, and concentration is 30%.
Described trace compound is 0.04% calcium sulfate, 0.003% magnesium chloride, 0.006% zinc chloride, 0.005% Selenium monochloride, 0.005%Fe
2+inner complex, 0.09% humic acid mixture.
Detect the effective constituent of spinach special fertilizer, it is
Embodiment 3
Prepare a production method for dipotassium hydrogen phosphate by-product spinach 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 5 DEG C/min is warming up to 100 DEG C with heat-up rate, the stirring velocity controlling stirring tank is that 190r/min is uniformly mixed reaction 3.5h, obtains intermediate slip;
(2) K is prepared
2hPO
4: again the alkaline potassium salt 2.3h of 2.3mol at the uniform velocity being added containing in steps 1) in the reactor of obtained intermediate slip, and to control temperature of reaction be 65 DEG C, stirring reaction 40min, when to detect pH value be 8.5, reaction terminates, and obtains nitrogenous, phosphorus, potassium slip;
(3) circulation crystallization filters: by step 2) obtain nitrogenous, phosphorus, potassium slip and be placed in cooling crystallizer 10s and be cooled to temperature 3 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, when the mass ratio of nitrogen component, Vanadium Pentoxide in FLAKES composition, potassium oxide composition is 5:3:4, stop crystallization and filter, acquisition filter cake is dipotassium hydrogen phosphate, and in filtrate, add trace compound 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 0.8h, adjustment moisture content is 3.3%, detects packaging, can obtain spinach special fertilizer.
Described phosphoric acid and carboxamide react, and are phosphoric acid solid and carboxamide liquid reactions.
Described alkaline potassium salt is salt of wormwood, and concentration is 15%.
Described trace compound is 0.05% calcium sulfate, 0.003% magnesium chloride, 0.004% zinc chloride, 0.006% Selenium monochloride, 0.005%Fe
2+inner complex, 0.07% humic acid mixture.
Detect the effective constituent of spinach special fertilizer, it is
Described spinach special fertilizer is chemical combination state composite fertilizer, and its effective constituent has
mixture.
Embodiment 4
Prepare a production method for dipotassium hydrogen phosphate by-product spinach 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 5 DEG C/min is warming up to 130 DEG C with heat-up rate, the stirring velocity controlling stirring tank is that 195r/min is uniformly mixed reaction 4h, obtains intermediate slip;
(2) K is prepared
2hPO
4: again the alkaline potassium salt 2.5h of 2.4mol at the uniform velocity being added containing in steps 1) in the reactor of obtained intermediate slip, and to control temperature of reaction be 70 DEG C, stirring reaction 50min, when to detect pH value be 9, reaction terminates, and obtains nitrogenous, phosphorus, potassium slip;
(3) circulation crystallization filters: by step 2) obtain nitrogenous, phosphorus, potassium slip and be placed in cooling crystallizer 10s and be cooled to temperature 2 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, when the mass ratio of nitrogen component, Vanadium Pentoxide in FLAKES composition, potassium oxide composition is 5.5:3.5:4, stop crystallization and filter, acquisition filter cake is dipotassium hydrogen phosphate, and in filtrate, add trace compound 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 0.6h, adjustment moisture content is 3.8%, detects packaging, can obtain spinach special fertilizer.
Described phosphoric acid and carboxamide react, and are phosphoric acid solid and carboxamide liquid reactions.
Described alkaline potassium salt is Potassium ethanoate, and concentration is 35%.
Described trace compound is 0.03% calcium sulfate, 0.005% magnesium chloride, 0.006% zinc chloride, 0.002% Selenium monochloride, 0.001%Fe
2+inner complex, 0.05% humic acid mixture.
Detect the effective constituent of spinach special fertilizer, it is
Embodiment 5
Prepare a production method for dipotassium hydrogen phosphate by-product spinach 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 5 DEG C/min is warming up to 120 DEG C with heat-up rate, the stirring velocity controlling stirring tank is that 190r/min is uniformly mixed reaction 4.5h, obtains intermediate slip;
(2) K is prepared
2hPO
4: again the alkaline potassium salt 2.8h of 2.5mol at the uniform velocity being added containing in steps 1) in the reactor of obtained intermediate slip, and to control temperature of reaction be 75 DEG C, stirring reaction 60min, when to detect pH value be 8.8, reaction terminates, and obtains nitrogenous, phosphorus, potassium slip;
(3) circulation crystallization filters: by step 2) obtain nitrogenous, phosphorus, potassium slip and be placed in cooling crystallizer 10s and be cooled to temperature 4 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, when the mass ratio of nitrogen component, Vanadium Pentoxide in FLAKES composition, potassium oxide composition is 6:3:5, stop crystallization and filter, acquisition filter cake is dipotassium hydrogen phosphate, and in filtrate, add trace compound 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 0.9h, adjustment moisture content is 3.6%, detects packaging, can obtain spinach special fertilizer.
Described phosphoric acid and carboxamide react, and are phosphoric acid solution and carboxamide liquid reactions.
Described alkaline potassium salt is potassium sulfate, and concentration is 22%.
Described trace compound is 0.05% calcium sulfate, 0.003% magnesium chloride, 0.004% zinc chloride, 0.006% Selenium monochloride, 0.005%Fe
2+inner complex, 0.07% humic acid mixture.
Detect the effective constituent of spinach special fertilizer, it is
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.
Test example 1 dipotassium hydrogen phosphate product purity detects
Embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5 are sampled 5g respectively, is placed in the beaker of 50ml, adopt distilled water to carry out dissolving and stirring, then adopt concentration to be that 30% hydrochloric acid carries out titration, the consumption V1 of record hydrochloric acid; Adopt again concentration be 30% sodium hydroxide solution titration concentration be 30% hydrochloric acid V1, record hydrochloric acid consumption; Carry out the calculating of dipotassium hydrogen phosphate content again according to equivalent alternate form, so calculate embodiment 1, embodiment 2, embodiment 3, embodiment 4, dipotassium hydrogen phosphate product obtained by embodiment 5 purity be respectively shown in table 1:
Table 1:
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| Dipotassium hydrogen phosphate (%) | 97.1 | 95.6 | 96.8 | 96.3 | 98.9 |
From in table, the dipotassium hydrogen phosphate that technical scheme of the present invention directly obtains, without the need to the process by removal step, namely can make the purity of dipotassium hydrogen phosphate product reach more than 95%, have significant progress.
Test example 2 spinach special fertilizer is on the growing state impact experiment of spinach culturing process
2.1 experiment process and methods
Experimental group: adopt the obtained spinach special fertilizer+animal excretion of embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5 to carry out experimental group and cultivate spinach, other culturing steps are with traditional culture scheme.
Control group 1: the preparation+animal excretion adopting traditional composite fertilizer to carry out NPK fertilizers cultivates spinach, and other culturing steps are with traditional culturing step.
Control group 2: adopt animal excretion to cultivate spinach, other steps are with traditional culturing step.
Consumption: fertilizer amount is 5kg.
Incubation time: incubation time is 2 months, and the leaf look upgrowth situation looking over spinach every 10 days.
2.2 experimental result
Table 2:
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Control group 1 | Control group 2 | |
| 10 days | Pale yellow | Pale yellow | Pale yellow | Pale yellow | Pale yellow | Pale yellow | Pale yellow |
| 20 days | Green | Green | Green | Green | Green | Green | Green |
| 30 days | Dark green | Dark green | Dark green | Dark green | Dark green | Dark green | Dark green |
| 40 days | Dark green | Dark green | Dark green | Dark green | Dark green | Dark green | Pale yellow |
| 50 days | Dark green | Dark green | Dark green | Dark green | Dark green | Pale yellow | Pale yellow |
| 60 days | Dark green | Dark green | Dark green | Dark green | Dark green | Pale yellow | Huang Ye |
As can be seen from data presentation in table, spinach special fertilizer of the present invention can meet the fertile requirement of need in spinach growth process, is supplied to spinach nutritive element in time, promotes the normal growth of spinach.
The Element detection simultaneous test in soil is remained in after test example 3 spinach special fertilizer is absorbed by spinach
3.1 test process
Experimental group: the employing embodiment of the present invention 1, embodiment 2, embodiment 3, embodiment 4, the spinach composite fertilizer special that the production method of embodiment 5 is produced carry out nutritive medium soilless culture to spinach.
Control group: adopt traditional spinach composite fertilizer formulated according to the demand of spinach n p k nutrition element to carry out nutritive medium soilless culture.
Method: until cultivation spinach 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.
3.2 test-results
| Nutritive medium nutrient composition content % before cultivation | Nutritive medium nutrient composition content % after cultivation |
| Nitrogen | Phosphorus | Potassium | Nitrogen | Phosphorus | Potassium | |
| Embodiment 1 | 3.8 | 1.8 | 3.3 | 3.82 | 1.9 | 3.35 |
| Embodiment 2 | 3.5 | 1.7 | 3.2 | 3.54 | 1.78 | 3.3 |
| Embodiment 3 | 3.2 | 1.9 | 3.5 | 3.28 | 1.89 | 3.57 |
| Embodiment 4 | 3.7 | 2.1 | 3.7 | 3.71 | 2.13 | 3.65 |
| Embodiment 5 | 3.6 | 1.8 | 3.6 | 3.61 | 1.91 | 3.69 |
| Control group | 3.5 | 1.7 | 3.2 | 3.71 | 1.92 | 3.65 |
As can be seen from upper table data presentation, spinach special fertilizer of the present invention can be absorbed in a large number by spinach, 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, visible, spinach special fertilizer of the present invention can better be absorbed by spinach, and then keeps the nutritive ingredient in 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.
Simultaneously, again integrated is carried out to the amount of the n-p-k element remained in nutritive medium, can find out that the n-p-k element remained in nutritive medium can meet the element collocation in the chemical structure of effective constituent, and then can be overall remain in nutritive medium, after avoiding Term Fertilization, resolve into single-element and cause the technical barrier of element waste and contaminate environment to occur.
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 (8)
1. prepare the production method of dipotassium hydrogen phosphate by-product spinach special fertilizer for one kind, it is characterized in that, adopt phosphoric acid to be (1.3-1.9) with carboxamide according to mol ratio: 1 mixes, and is that 5 DEG C/min is warming up to 90-140 DEG C with heat-up rate, stirring reaction 3-5h, obtains intermediate slip, this intermediate slip is adopted to mix with 2.2-2.6mol alkaline potassium salt again, and to control temperature of reaction be 60 DEG C-80 DEG C, stirring reaction 20-70min, when detection pH value is 8-9.5, 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, work as nitrogen, Vanadium Pentoxide in FLAKES, the mass ratio of potassium oxide is (5-6): (3-4): time (3-5), stop crystallization and filter, the filter cake obtained is dipotassium hydrogen phosphate product, in filtrate, add trace compound be adjusted to 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 3-4%, can obtain spinach special fertilizer.
2. prepare the production method of dipotassium hydrogen phosphate by-product spinach special fertilizer as claimed in claim 1, it is characterized in that, comprise the following steps:
(1) raw material preparation mixing: be (1.3-1.9) according to mol ratio by phosphoric acid and carboxamide: 1 in stirring-type reactor, be that 5 DEG C/min is warming up to 90-140 DEG C with heat-up rate, the stirring velocity controlling stirring tank is that 180-200r/min is uniformly mixed reaction 3-5h, obtains intermediate slip;
(2) K is prepared
2hPO
4: again the alkaline potassium salt 2-3h of 2.2-2.6mol is at the uniform velocity added containing in steps 1) in the reactor of obtained intermediate slip, and to control temperature of reaction be 60 DEG C-80 DEG C, stirring reaction 20-70min, when to detect pH value be 8-9.5, reaction terminates, and obtains nitrogenous, phosphorus, potassium slip;
(3) circulation crystallization filters: by step 2) obtain nitrogenous, phosphorus, potassium slip and be placed in cooling crystallizer 10s and be cooled to temperature≤5 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, mass ratio until nitrogen component, Vanadium Pentoxide in FLAKES composition, potassium oxide composition is (5-6): (3-4): time (3-5), stop crystallization and filter, acquisition filter cake is dipotassium hydrogen phosphate, and in filtrate, add trace compound 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 0.5-1h, adjustment moisture content is 3-4%, detect packaging, spinach special fertilizer can be obtained.
3. prepare the production method of dipotassium hydrogen phosphate by-product spinach 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 dipotassium hydrogen phosphate by-product spinach 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 dipotassium hydrogen phosphate by-product spinach 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 dipotassium hydrogen phosphate by-product spinach special fertilizer as claimed in claim 1 or 2, it is characterized in that, described alkaline potassium salt is the one in salt of wormwood, Potassium ethanoate.
7. prepare the production method of dipotassium hydrogen phosphate by-product spinach special fertilizer as claimed in claim 1 or 2, it is characterized in that, described trace compound is calcium sulfate, magnesium chloride, zinc chloride, Selenium monochloride, Fe
2+inner complex, humic acid mixture.
8. prepare the production method of dipotassium hydrogen phosphate by-product spinach special fertilizer as claimed in claim 1 or 2, it is characterized in that, described spinach special fertilizer is chemical combination state composite fertilizer, and its effective constituent has
in one or more mixtures.
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| CN101811684A (en) * | 2009-11-23 | 2010-08-25 | 瓮福（集团）有限责任公司 | Method for co-production of granular monoammonium phosphate by using powdery monoammonium phosphate production device |
| CN103803518A (en) * | 2014-01-24 | 2014-05-21 | 贵阳中化开磷化肥有限公司 | Method for preparing monopotassium phosphate by using wet-process phosphoric acid |
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|---|---|---|---|---|
| CN101811684A (en) * | 2009-11-23 | 2010-08-25 | 瓮福（集团）有限责任公司 | Method for co-production of granular monoammonium phosphate by using powdery monoammonium phosphate production device |
| CN103803518A (en) * | 2014-01-24 | 2014-05-21 | 贵阳中化开磷化肥有限公司 | Method for preparing monopotassium phosphate by using wet-process phosphoric acid |
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Effective date of registration: 20160301 Address after: 550000 Huaxi District, Guizhou, Guiyang Applicant after: Guizhou University Applicant after: Phosphorylcholine group limited-liability company is opened in Guizhou Applicant after: Guizhou Ke Xinhua smelting company limited Address before: 550000 Huaxi District, Guizhou, Guiyang Applicant before: Guizhou University Applicant before: Zhonghuakai Phosphorous Chemical Fertilizer Co., Ltd., Guiyang Applicant before: Guizhou Ke Xinhua smelting company limited |
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