CN104310352B - A kind of production method preparing dipotassium hydrogen phosphate by-product Caulis et Folium Lactucae sativae special fertilizer - Google Patents

A kind of production method preparing dipotassium hydrogen phosphate by-product Caulis et Folium Lactucae sativae special fertilizer Download PDF

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CN104310352B
CN104310352B CN201410478361.7A CN201410478361A CN104310352B CN 104310352 B CN104310352 B CN 104310352B CN 201410478361 A CN201410478361 A CN 201410478361A CN 104310352 B CN104310352 B CN 104310352B
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caulis
lactucae sativae
folium lactucae
fertilizer
hydrogen phosphate
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CN104310352A (en
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陈肖虎
廖吉星
高贵龙
朱飞武
薛涛
彭宝林
李军旗
黄芳
金会心
唐晓宁
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Guizhou Kailin Group Co Ltd
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Guizhou University
Guizhou Kailin Group Co Ltd
Guizhou Kexin Chemical and Metallurgical Co Ltd
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Abstract

The present invention relates to chemical technology field, a kind of production method preparing dipotassium hydrogen phosphate by-product Caulis et Folium Lactucae sativae special fertilizer, by needing fertilizer according to Caulis et Folium Lactucae sativae, effective absorbtivity of n-p-k element is analyzed, and the constituent content in production process is adjusted and arranges in pairs or groups, the compound fertilizer making the compound state prepared can meet the demand of Caulis et Folium Lactucae sativae to greatest extent, and reduce in composite heat transfer because of element mismatch, the high cost caused, further avoid too much element to put among soil, cause the solidification of compound fertilizer to pollute environment.

Description

A kind of production method preparing dipotassium hydrogen phosphate by-product Caulis et Folium Lactucae sativae special fertilizer
Technical field
The present invention relates to chemical technology field, a kind of producer preparing dipotassium hydrogen phosphate by-product Caulis et Folium Lactucae sativae special fertilizer Method.
Background technology
Caulis et Folium Lactucae sativae (formal name used at school: Lactuca sativa), has another name called Caulis et Folium Lactucae sativae, spring vegetable, wheat dish, is the annual of Compositae Lactuca or two Year raw herbaceous plant, it is the most common a kind of edible vegetable;And containing abundant nutrient in lettuce haulm, according to detection: Every 100 grams of moisture contents 96.4 grams, 0.6 gram of protein, 0.1 gram of fat, carbohydrate 1.9 grams, crude fibre 0.4 gram, calcium 7 milli Gram, 31 milligrams of phosphorus, ferrum 2 milligrams, carotene 0.02 milligram, thiamine 0.03 milligram, 0.02 milligram of riboflavin, nicotinic acid 0.5 milli Gram;Wherein, possibly together with a kind of specific nutrient-" Caulis et Folium Lactucae sativae element ", Caulis et Folium Lactucae sativae element has bitter in the mouth, can strengthen gastric juice, stimulate digestion, promotes Appetite, and there is feature and the effects such as analgesia and hypnosis.
But, in Caulis et Folium Lactucae sativae cultivation with in fertile prior art, it is to carry out being mixed in proportion preparation by traditional azophoska, obtains Obtain the Chemical Mixed Fertilizer of mixed state so that azophoska meets the nutrient demand of Caulis et Folium Lactucae sativae growth course, promote the normal growth of Caulis et Folium Lactucae sativae, enter And make substantial amounts of n-p-k element because mismatch is unable to meet equilibrium absorption principle, residue among soil, enter And react with other mineral elements remained in soil among soil for a long time, cause the trophic structure of soil to become Change, even soil compaction, cause soil quality to be gradually deteriorated, cause the pollution of environment, also result in lettuce planting fertile simultaneously Amount increases, and strengthens lettuce planting cost and affects Caulis et Folium Lactucae sativae quality.
Dipotassium hydrogen phosphate is a kind of fertilizer containing phosphorus potassium element, it is possible in the environment of 20 DEG C, substantial amounts of soluble in water, with Water forms solution state, and then is sufficiently absorbed by crop, is a kind of efficient phosphorus potash fertilizer.Currently for dipotassium hydrogen phosphate Preparation technology is more, but it is low mostly to there is the product purity produced, and needs to carry out further remove impurity process so that produce The features such as cost is relatively big, and production technology tail washings discharge capacity is big, and phosphorus potassium element loss is big.
To this end, this research worker needs fertile requirement, in conjunction with in dipotassium hydrogen phosphate product preparation process by research Caulis et Folium Lactucae sativae growth The defect existed is studied, and the preparation technology of Caulis et Folium Lactucae sativae special fertilizer is joined in dipotassium hydrogen phosphate product preparation process, for phosphorus The preparation method of acid hydrogen dipotassium product provides a kind of new approaches.
Summary of the invention
In order to solve above-mentioned technical problem present in prior art, the present invention provides one to prepare dipotassium hydrogen phosphate by-product The production method of Caulis et Folium Lactucae sativae special fertilizer, has and can be combined with Caulis et Folium Lactucae sativae special fertilizer preparation technology by dipotassium hydrogen phosphate product preparation process Getting up, reduce the purification difficult of dipotassium hydrogen phosphate product in traditional handicraft, the double salt for Caulis et Folium Lactucae sativae a kind of compound state of offer is special simultaneously With compound fertilizer, reduce traditional Caulis et Folium Lactucae sativae fertile time, during the special fertilizer of the n p k fertilizer compound carried out, bring to environment The feature of probability of pollution.
It is achieved particular by techniques below scheme:
A kind of production method preparing dipotassium hydrogen phosphate by-product Caulis et Folium Lactucae sativae special fertilizer, uses phosphoric acid and phosphoamide according to mol ratio For (1.6-2.1): 1 mixes, and is that 15 DEG C/min is warming up to 85-105 DEG C with programming rate, stirring reaction 3-5h, obtain centre Body slip;Use this intermediate slip to mix with 2.4-2.8mol alkaline potassium salt again, and to control reaction temperature be 55 DEG C-85 DEG C, Stirring reaction 30-60min, detection pH value is when being 8-9.5, and reaction terminates, it is thus achieved that nitrogenous, the slip of phosphorus, potassium, and by nitrogenous, phosphorus, The slip of potassium is placed in cooler crystallizer and carries out decrease temperature crystalline filtration treatment, makes filtrate at circulation crystallization in cooler crystallizer Reason, and detect analysis filtrate, when nitrogen, phosphorus pentoxide, the mass ratio of potassium oxide are (2-2.4): (1-2): time (1.8-2.4), Stop crystallization also filtering, it is thus achieved that filter cake be dipotassium hydrogen phosphate product, in filtrate, add being adjusted to of trace compound He Tai compound fertilizer just finished product;And first finished product is placed in baker, using programming rate is that 3 DEG C/min is warming up to 45-55 DEG C, dry After dry 0.6-0.9h, adjustment moisture is 1-2%, can be prepared by Caulis et Folium Lactucae sativae special fertilizer.
Described phosphoric acid reacts with phosphoamide, for phosphoric acid solution and phosphoamide solid reaction.
Described phosphoric acid reacts with phosphoamide, for phosphoric acid solution and phosphoamide liquid reactions.
Described phosphoric acid reacts with phosphoamide, for phosphoric acid solid and phosphoamide liquid reactions.
Described alkaline potassium salt is the one in potassium carbonate, potassium acetate.In addition, above-mentioned alkaline potassium salt, it is also possible to At least one in the potassium compositions such as potassium chloride, potassium nitrate, potassium sulfate, potassium hydroxide is used to substitute.
Described trace compound is calcium sulfate, Fe2+Chelate, the mixture of humic acid.
Described Caulis et Folium Lactucae sativae special fertilizer is compound state compound fertilizer, and its effective ingredient has In one or more mixing Thing.
By phosphoric acid and urea reaction, and it is controlled by temperature, mol ratio and other technological parameters so that phosphoric acid There is complicated polyreaction in the structural formula of urea so that it is is formedIntermediate-ion, in the middle of this Ion has stronger stability, and there is also coordinate bond between carbon oxygen atom, in the solution that this ion exists simultaneously Containing substantial amounts of dihydrogen phosphate, therefore, when to exist this intermediate-ion solution in add potassium ion time, potassium ion gradually with Dihydrogen phosphate reaction in solution, forms potassium dihydrogen phosphate, and the amount added along with potassium ion is gradually increased, and regulated value PH Value, potassium dihydrogen phosphate progressively changes into dipotassium hydrogen phosphate, and suitably excess potassium ion, then intermediate-ion and potassium ion are carried out instead Should, replace out part ammonium radical ion so that intermediate-ion chelates intoIntermediate-ion, and With positive charge, and then when solution participates in other electronegative ions or compound, it will form rechlorination with this ion Compound, the nutritional labeling in the abundantest product.
As added potassium sulfate in solution, adjust the Determination of Potassium in solution, then can generate sulfenyl double salt compound state multiple Hefei.
As added potassium nitrate in solution, adjust the Determination of Potassium in solution and nitrogen element content, then can generate nitric acid Salt compound salt compound fertilizer.
The present invention is by being adjusted the nutrient in crystalline mother solution, and is controlled reaction process condition, makes Solution progressively generates substantial amounts of phosphoric acid ammonia potassium root, phosphoric acid hydrogen ammonia root, then with intermediate-ionAnd other intermediate-ion react, formed The double salt Caulis et Folium Lactucae sativae dedicated fertilizer of compound state.
Meanwhile, when in solution containing the substantial amounts of element affecting fertilizer impurity, it is difficult to generate colloid, and then makes The character of fertilizer is unaffected:
During Wet-process Phosphoric Acid Production dipotassium hydrogen phosphate product, the element such as substantial amounts of ferrum, magnesium, aluminum can be given birth in the solution Produce colloid, and then affect the technique ease of dipotassium hydrogen phosphate product preparation process so that be prepared by dipotassium hydrogen phosphate product During, remove impurity cost is bigger;Iron ion, magnesium ion, aluminium ion are positively charged gas ions, so will not to centre from Son forms interference, and solution and intermediate-ion form another with elements such as ferrum, magnesium, aluminum and easily decompose intermediate-ion on the contrary Body so that fully absorbed by crop.
Compared with prior art, the technique effect of technical scheme is embodied in:
1. by needing fertilizer according to Caulis et Folium Lactucae sativae, effective absorbtivity of n-p-k element is analyzed, and to production process In constituent content be adjusted and arrange in pairs or groups so that the compound fertilizer of the compound state prepared can meet Caulis et Folium Lactucae sativae to greatest extent Demand, and reduce in composite heat transfer because element mismatch, the high cost caused, further avoid too much unit Element puts among soil, causes the solidification of compound fertilizer to pollute environment.
2. by the process conditions produced are controlled so that in Caulis et Folium Lactucae sativae special fertilizer preparation process, it is possible to produce height The dipotassium hydrogen phosphate product of purity, compensate for remove impurity cost when traditional wet phosphoric acid prepares dipotassium hydrogen phosphate product, makes The purity of the dipotassium hydrogen phosphate product that must prepare reaches more than 95%, and production cost reduces 93%, has significant warp Ji benefit.
3. by production process, the mol ratio of raw material, in crystallisation step, the accurate of filtrate is analyzed and detection, makes The quality of the Caulis et Folium Lactucae sativae compound fertilizer that must produce is guaranteed, and with adjusting the mode of filtrate component content, chemical products are raw Waste liquid during product is as the raw material of composite heat transfer, it is to avoid the discharge of waste liquid, reduces composite heat transfer cost, has The significantly value of environmental protection and economic benefit.
4. by technical parameter in compound state compound fertilizer production technology, it is exactly i.e. the control of temperature, material concentration and proportioning System so that after phosphoric acid and urea reaction, generates urea phosphate product, and urea phosphate product itself has stronger acidity, and phosphoric acid with It is again the compound state double salt being combined together to form by the way of coordinate bond between carbamide, is also that conventional art is used as crop Fertilizer, and crop is equal to the unitary such as the absorbance comparison carbamide of this compound state double salt, ammonium carbonate, ammonium nitrate, binary fertilizer absorbance Preferably a kind of compound state compound fertilizer, but, this compound state double salt is in the environment of phosphoric acid exists, at a temperature of 80-250 DEG C, The decomposition polyreaction of complexity can occur so that urea phosphate forms (H2PO4)-(H2NCONH3)+Two ions, (H2NCONH3)+ Ion is close with phosphoric acid, and in the environment of temperature is 80-160 DEG C, is formedIntermediate-ion And dihydrogen phosphate, and between C and O, forming coordinate bond, this intermediate-ion can be formed with centering element compound chelating Multielement intermediate-ion, and then can continue to the compound electronegative with other or ion formation chelate, improve double salt Middle constituent content, and then the nutrient content in the double salt that this ion exists can be adjusted, meanwhile, this chelate can carry out again water Solve and by crop, and then effectively for a long time can provide fertilizer efficiency for crop, meanwhile, in conjunction with element in the solution that this ion is existed The mensuration of content, and then adjust each constituent content when double salt is formed, dry and obtain the compound fertilizer containing compound state double salt structure, Improve the quality of Caulis et Folium Lactucae sativae special fertilizer.
Detailed description of the invention
Below in conjunction with specific embodiment, technical scheme is further limited, but claimed Scope is not only limited to description.
Principle illustrates:
The present invention carries out research and discussion by the mechanism reacting phosphoric acid and phosphoamide, and combines prior art literature Solution arrives, and phosphoric acid and phosphoamide react generation urea phosphate, and its molecular formula is: CO (NH2)2.H3PO4, in the environment of higher temperature, Chemical bond meeting dialysis between H and O in phosphoric acid, hydrion is combined with carbamide and forms the ionic state containing positive charge so that phosphorus Acid urea forms the ion double salt that a kind of positive and negative charge attracts mutually, its mechanism structural response following expression: CO (NH2)2.H3PO4→ (H2PO4)-.(H2NCONH3)+
Further, urea phosphate ion double salt phosphoric acid exist in the environment of, (H therein2NCONH3)+Cation and phosphorus Acid is close, forms the intermediate-ion of C → O coordinate bond, is (CO5PN2H8)+, and then make in urea phosphate intermediate containing a large amount of (H2PO4)-(CO5PN2H8)+Ion, when adding excessive and appropriate potassium ion, dihydrogen phosphate is formed with potassium ion Potassium dihydrogen phosphate crystal is precipitated, unnecessary potassium ion and (CO5PN2H8)+Ionic reaction, and displace part NH4 +So that molten Containing (CO in liquid5PNH4K)+Double salt ion, and analyzed and control the content of N in solution, P, K element by detection, in heating It is dried and can be prepared by containing N, P, the compound state compound fertilizer of K element.
Its concrete reaction principle will carry out further instruction by following reaction structure formula and reaction mechanism:
Reaction equation one:
CO(NH2)2+H3PO4→CO(NH2)2.H3PO4
Reaction equation two:
Reaction equation three:
Wherein, the dotted line between carbon atom and oxygen atom represents and there is coordinate bond between C atom and O atom.
Reaction equation four:
Wherein, the dotted line between carbon atom and oxygen atom represents and there is coordinate bond between C atom and O atom.
Reaction equation five:
Obtain phosphoric acid hydrogen ammonia potassium double salt, in ammonium hydrogen phosphate potassium Potassium ion generate dipotassium hydrogen phosphate and phosphoric acid hydrogen ammonia radical ion with biphosphate nak response again, phosphoric acid hydrogen ammonia radical ion again withIntermediate-ion is combined to the Nitrogen-and Phosphorus-containing potassium double salt structure of compound state, and then can adjust suitable The N P and K compound state compound fertilizer used together in Caulis et Folium Lactucae sativae.
Noun illustrates:
Urea phosphate (Urea phosphate, UP), No. CAS is 4861-19-2, and molecular formula is CH7N2O5P, is represented by CO (NH2)2·H3PO4:
Being a kind of fine chemical product being widely used in the fields such as animal husbandry, industry, agricultural, its solid is white crystals Or crystalline powder, soluble in water and alcohol, insoluble in ethers, toluene and carbon tetrachloride, aqueous solution is acidity, starts point time melted Solve and release carbon dioxide and ammonia.
Embodiment: with concrete operation embodiment, the present invention is further elaborated below.
Embodiment 1
A kind of production method preparing dipotassium hydrogen phosphate by-product Caulis et Folium Lactucae sativae special fertilizer, comprises the following steps:
(1) raw material preparation mixing: by phosphoric acid and phosphoamide according to mol ratio be 1.6:1 in stirring-type reactor, to rise Temperature speed is that 15 DEG C/min is warming up to 85 DEG C, and the mixing speed controlling stirred tank is that 170r/min stirs hybrid reaction 3h, it is thus achieved that Intermediate slip;
(2) K is prepared2HPO4: again the alkaline potassium salt 2h of 2.4mol is at the uniform velocity added containing in steps 1) the intermediate slip for preparing Reactor in, and to control reaction temperature be 55 DEG C, and stirring reaction 30min, when detection pH value is 8, reaction terminates, it is thus achieved that contain Nitrogen, phosphorus, the slip of potassium;
(3) circulation crystallization filters: by step 2) obtain slip nitrogenous, phosphorus, potassium and be placed in cooler crystallizer cooling in 20s To temperature 7 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, treat nitrogen component, phosphorus pentoxide When composition, the mass ratio of potassium oxide composition are 2:1:1.8, stop crystallization and filter, it is thus achieved that filter cake is dipotassium hydrogen phosphate, to filtrate Middle addition trace compound adjusts fertilizer structure becomes compound state compound fertilizer just finished product;
(4) filtrate dries: by step 3) the compound state compound fertilizer that obtains just finished product is placed in baker, uses programming rate Being that 3 DEG C/min is warming up to 45 DEG C, be dried 0.6h, adjusting moisture is 1%, and detection packaging can be prepared by Caulis et Folium Lactucae sativae special fertilizer.
Described phosphoric acid reacts with phosphoamide, for phosphoric acid solution and phosphoamide solid reaction.
Described alkaline potassium salt uses potassium hydroxide this potassium composition to replace, and concentration is 30%.
Described trace compound is 0.05% calcium sulfate, 0.005%Fe2+Chelate, 0.0.9% humic acid Mixture.
Embodiment 2
A kind of production method preparing dipotassium hydrogen phosphate by-product Caulis et Folium Lactucae sativae special fertilizer, comprises the following steps:
(1) raw material preparation mixing: by phosphoric acid and phosphoamide according to mol ratio be 2.1:1 in stirring-type reactor, to rise Temperature speed is that 15 DEG C/min is warming up to 105 DEG C, and the mixing speed controlling stirred tank is that 205r/min stirs hybrid reaction 5h, it is thus achieved that Intermediate slip;
(2) K is prepared2HPO4: again the alkaline potassium salt 3h of 2.8mol is at the uniform velocity added containing in steps 1) the intermediate slip for preparing Reactor in, and to control reaction temperature be 85 DEG C, and stirring reaction 60min, when detection pH value is 9.5, reaction terminates, it is thus achieved that contain Nitrogen, phosphorus, the slip of potassium;
(3) circulation crystallization filters: by step 2) obtain slip nitrogenous, phosphorus, potassium and be placed in cooler crystallizer cooling in 20s To temperature 6 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, treat nitrogen component, phosphorus pentoxide When composition, the mass ratio of potassium oxide composition are 2:2:2.4, stop crystallization and filter, it is thus achieved that filter cake is dipotassium hydrogen phosphate, to filtrate Middle addition trace compound adjusts fertilizer structure becomes compound state compound fertilizer just finished product;
(4) filtrate dries: by step 3) the compound state compound fertilizer that obtains just finished product is placed in baker, uses programming rate Being that 3 DEG C/min is warming up to 55 DEG C, be dried 0.9h, adjusting moisture is 2%, and detection packaging can be prepared by Caulis et Folium Lactucae sativae special fertilizer.
Described phosphoric acid reacts with phosphoamide, for phosphoric acid solution and phosphoamide liquid reactions.
Described alkaline potassium salt is potassium carbonate, and concentration is 15%.
Described trace compound is 0.04% calcium sulfate, 0.003%Fe2+Chelate, 0.6% humic acid mixed Compound.
Embodiment 3
A kind of production method preparing dipotassium hydrogen phosphate by-product Caulis et Folium Lactucae sativae special fertilizer, comprises the following steps:
(1) raw material preparation mixing: by phosphoric acid and phosphoamide according to mol ratio be 1.7:1 in stirring-type reactor, to rise Temperature speed is that 15 DEG C/min is warming up to 95 DEG C, and the mixing speed controlling stirred tank is that 180r/min stirs hybrid reaction 4h, it is thus achieved that Intermediate slip;
(2) K is prepared2HPO4: again the alkaline potassium salt 2.5h of 2.6mol is at the uniform velocity added containing in steps 1) the intermediate material for preparing In the reactor of slurry, and to control reaction temperature be 65 DEG C, stirring reaction 40min, and when detection pH value is 8.5, reaction terminates, it is thus achieved that Nitrogenous, the slip of phosphorus, potassium;
(3) circulation crystallization filters: by step 2) obtain slip nitrogenous, phosphorus, potassium and be placed in cooler crystallizer cooling in 20s To temperature 5 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, treat nitrogen component, phosphorus pentoxide Composition, potassium oxide composition mass ratio 2.4:1:2.4 time, stop crystallization and also filter, it is thus achieved that filter cake is dipotassium hydrogen phosphate, to filtrate Middle addition trace compound adjusts fertilizer structure becomes compound state compound fertilizer just finished product;
(4) filtrate dries: by step 3) the compound state compound fertilizer that obtains just finished product is placed in baker, uses programming rate Being that 3 DEG C/min is warming up to 50 DEG C, be dried 0.75h, adjusting moisture is 1.5%, and detection packaging can be prepared by Caulis et Folium Lactucae sativae special Fertile.
Described phosphoric acid reacts with phosphoamide, for phosphoric acid solid and phosphoamide liquid reactions.
Described alkaline potassium salt uses potassium chloride this potassium composition to replace, and concentration is 30%.
Described trace compound is 0.07% calcium sulfate, 0.008%Fe2+Chelate, 0.4% humic acid mixed Compound.
Embodiment 4
A kind of production method preparing dipotassium hydrogen phosphate by-product Caulis et Folium Lactucae sativae special fertilizer, comprises the following steps:
(1) raw material preparation mixing: by phosphoric acid and phosphoamide according to mol ratio be 2:1 in stirring-type reactor, to heat up Speed is that 15 DEG C/min is warming up to 100 DEG C, and the mixing speed controlling stirred tank is that 200r/min stirs hybrid reaction 3.5h, it is thus achieved that Intermediate slip;
(2) K is prepared2HPO4: again the alkaline potassium salt 2.4h of 2.5mol is at the uniform velocity added containing in steps 1) the intermediate material for preparing In the reactor of slurry, and to control reaction temperature be 75 DEG C, and stirring reaction 50min, when detection pH value is 9, reaction terminates, it is thus achieved that contain Nitrogen, phosphorus, the slip of potassium;
(3) circulation crystallization filters: by step 2) obtain slip nitrogenous, phosphorus, potassium and be placed in cooler crystallizer cooling in 20s To temperature 5 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, treat nitrogen component, phosphorus pentoxide When composition, the mass ratio of potassium oxide composition are 2.4:2:1.8, stop crystallization and filter, it is thus achieved that filter cake is dipotassium hydrogen phosphate, to filter Liquid adds trace compound adjustment fertilizer structure and becomes compound state compound fertilizer just finished product;
(4) filtrate dries: by step 3) the compound state compound fertilizer that obtains just finished product is placed in baker, uses programming rate Being that 3 DEG C/min is warming up to 48 DEG C, be dried 0.8h, adjusting moisture is 1.8%, and detection packaging can be prepared by Caulis et Folium Lactucae sativae special fertilizer.
Described phosphoric acid reacts with phosphoamide, for phosphoric acid solution and phosphoamide liquid reactions.
Described alkaline potassium salt is potassium acetate, and concentration is 35%.
Described trace compound is 0.06% calcium sulfate, 0.009%Fe2+Chelate, 0.06% humic acid Mixture.
Embodiment 5
A kind of production method preparing dipotassium hydrogen phosphate by-product Caulis et Folium Lactucae sativae special fertilizer, comprises the following steps:
(1) raw material preparation mixing: by phosphoric acid and phosphoamide according to mol ratio be 1.85:1 in stirring-type reactor, to rise Temperature speed is that 15 DEG C/min is warming up to 90 DEG C, and the mixing speed controlling stirred tank is that 190r/min stirs hybrid reaction 4.5h, obtains Obtain intermediate slip;
(2) K is prepared2HPO4: again the alkaline potassium salt 2.8h of 2.7mol is at the uniform velocity added containing in steps 1) the intermediate material for preparing In the reactor of slurry, and to control reaction temperature be 70 DEG C, stirring reaction 45min, and when detection pH value is 8.8, reaction terminates, it is thus achieved that Nitrogenous, the slip of phosphorus, potassium;
(3) circulation crystallization filters: by step 2) obtain slip nitrogenous, phosphorus, potassium and be placed in cooler crystallizer cooling in 20s To temperature 4 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, treat nitrogen component, phosphorus pentoxide When composition, the mass ratio of potassium oxide composition are 2.4:2:2.4, stop crystallization and filter, it is thus achieved that filter cake is dipotassium hydrogen phosphate, to filter Liquid adds trace compound adjustment fertilizer structure and becomes compound state compound fertilizer just finished product;
(4) filtrate dries: by step 3) the compound state compound fertilizer that obtains just finished product is placed in baker, uses programming rate Being that 3 DEG C/min is warming up to 53 DEG C, be dried 0.8h, adjusting moisture is 1.4%, and detection packaging can be prepared by Caulis et Folium Lactucae sativae special fertilizer.
Described phosphoric acid reacts with phosphoamide, for phosphoric acid solid and phosphoamide liquid reactions.
Described alkaline potassium salt uses potassium sulfate this potassium composition to replace, and concentration is 18%.
Described trace compound is 0.01% calcium sulfate, 0.003%Fe2+Chelate, 0.09% humic acid Mixture.
Test example: come the technique effect to technical scheme and product below in conjunction with specific embodiment content Characteristic is described further.
Test example 1 dipotassium hydrogen phosphate product purity test experience
By embodiment 1, embodiment 2, embodiment 3, embodiment 4, the separately sampled 5g of embodiment 5, it is placed in the beaker of 50ml, Use distilled water dissolve and stir, then to use concentration be that 30% hydrochloric acid titrates, the consumption V of record hydrochloric acid;Again The hydrochloric acid V that sodium hydroxide solution titration concentration is 30% using concentration to be 30%, the consumption of record hydrochloric acid;Replace further according to equivalent The formula of changing carries out the calculating of dipotassium hydrogen phosphate content, and then calculates embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment The purity of the dipotassium hydrogen phosphate product obtained by 5 is respectively shown in table 1:
Table 1:
Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5
Dipotassium hydrogen phosphate (%) 98.1 95.4 97.8 96.3 99.1
From in table, the dipotassium hydrogen phosphate that technical scheme directly prepares is without by the place of removal step Reason, i.e. can make the purity of dipotassium hydrogen phosphate product reach more than 95%, has the most progressive.
Test example 2 Caulis et Folium Lactucae sativae special fertilizer remains in the Element detection contrast test in soil after being absorbed by Caulis et Folium Lactucae sativae
2.1 tests process
Experimental group: use the production method life of the embodiment of the present invention 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5 The Caulis et Folium Lactucae sativae composite fertilizer special that output is come carries out nutritional solution soilless culture to Caulis et Folium Lactucae sativae.
Matched group: the Caulis et Folium Lactucae sativae compound fertilizer using traditional demand according to Caulis et Folium Lactucae sativae n p k nutrition element formulated is carried out Nutritional solution soilless culture.
Method: after cultivating Caulis et Folium Lactucae sativae 1 month, the content of n p k nutrition composition in determination experiment group and matched group.
Fertilising consumption: experimental group and matched group fertilizer are 0.3kg.
2.2 result of the test
Shown it can be seen that the Caulis et Folium Lactucae sativae special fertilizer of the present invention can be absorbed in a large number by Caulis et Folium Lactucae sativae by upper table data, and matched group Nutritional solution in the content of n-p-k element compare cultivation before all have large range of raising, it is seen then that the Caulis et Folium Lactucae sativae of the present invention is special Fertilizer can preferably be absorbed by Caulis et Folium Lactucae sativae, and then keeps the nutritional labeling in initial soil, it is ensured that the quality in soil, the most not The state that Nitrogen In Soils phosphorus potassium element can be caused too much to harden occurs, and compared with traditional compounding fertilizer, has significant effect.
Meanwhile, then to the amount of the n-p-k element remained in nutritional solution it is integrated processing, it can be seen that remain in battalion N-p-k element in nutrient solution disclosure satisfy that the element collocation in the chemical constitution of effective ingredient, and then can overall remaining in In nutritional solution, it is to avoid after Term Fertilization, resolve into single-element and cause element waste and pollute the technical barrier of environment and go out Existing.
It is important to point out at this, above example and test example are only limitted to do technical scheme further Elaboration and understanding, it is impossible to being interpreted as the further restriction to technical scheme, those skilled in the art are basis at this On the essential characteristics of non-protruding made and the most progressive innovation and creation, still fall within the protection category of the present invention.

Claims (8)

1. the production method preparing dipotassium hydrogen phosphate by-product Caulis et Folium Lactucae sativae special fertilizer, it is characterised in that use phosphoric acid and phosphoamide It is (1.6-2.1) according to mol ratio: 1 mixing, and is that 15 DEG C/min is warming up to 85-105 DEG C with programming rate, stirring reaction 3- 5h, obtains intermediate slip;Use this intermediate slip to mix with 2.4-2.8mol alkaline potassium salt again, and control reaction temperature and be 55 DEG C-85 DEG C, stirring reaction 30-60min, when detection pH value is 8-9.5, reaction terminates, it is thus achieved that nitrogenous, the slip of phosphorus, potassium, and The slip of nitrogenous, phosphorus, potassium is placed in cooler crystallizer and carries out decrease temperature crystalline filtration treatment, make filtrate follow in cooler crystallizer Ring crystallization treatment, and detect analysis filtrate, when nitrogen, phosphorus pentoxide, the mass ratio of potassium oxide are (2-2.4): (1-2): (1.8- 2.4), time, stop crystallization and also filter, it is thus achieved that filter cake be dipotassium hydrogen phosphate product, in filtrate, add trace compound adjust Whole for compound state compound fertilizer just finished product;And first finished product is placed in baker, using programming rate is that 3 DEG C/min is warming up to 45- 55 DEG C, after being dried 0.6-0.9h, adjustment moisture is 1-2%, can be prepared by Caulis et Folium Lactucae sativae special fertilizer.
Prepare the production method of dipotassium hydrogen phosphate by-product Caulis et Folium Lactucae sativae special fertilizer the most as claimed in claim 1, it is characterised in that include Following steps:
(1) raw material preparation mixing: be (1.6-2.1) according to mol ratio by phosphoric acid and phosphoamide: 1 in stirring-type reactor, with Programming rate is that 15 DEG C/min is warming up to 85-105 DEG C, and the mixing speed controlling stirred tank is that 170-205r/min stirring mixing is anti- Answer 3-5h, it is thus achieved that intermediate slip;
(2) K is prepared2HPO4: again the alkaline potassium salt 2-3h of 2.4-2.8mol is at the uniform velocity added containing in steps 1) the intermediate material for preparing In the reactor of slurry, and to control reaction temperature be 55 DEG C-85 DEG C, stirring reaction 30-60min, when detection pH value is 8-9.5, instead Should terminate, it is thus achieved that nitrogenous, the slip of phosphorus, potassium;
(3) circulation crystallization filters: by step 2) obtain slip nitrogenous, phosphorus, potassium and be placed in cooler crystallizer and in 20s, be cooled to temperature Spend≤7 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, treat that nitrogen component, phosphorus pentoxide become Divide, the mass ratio of potassium oxide composition is (2-2.4): (1-2): time (1.8-2.4), stops crystallization and also filters, it is thus achieved that filter cake is phosphorus Acid hydrogen dipotassium, adding trace compound adjustment fertilizer structure in filtrate becomes compound state compound fertilizer just finished product;
(4) filtrate dries: by step 3) the compound state compound fertilizer that obtains just finished product is placed in baker, and using programming rate is 3 DEG C/min is warming up to 45-55 DEG C, is dried 0.6-0.9h, adjustments moisture is 1-2%, and detection is packed, and can be prepared by Caulis et Folium Lactucae sativae special With fertilizer.
Prepare the production method of dipotassium hydrogen phosphate by-product Caulis et Folium Lactucae sativae special fertilizer the most as claimed in claim 1 or 2, it is characterised in that Described phosphoric acid reacts with phosphoamide, for phosphoric acid solution and phosphoamide solid reaction.
Prepare the production method of dipotassium hydrogen phosphate by-product Caulis et Folium Lactucae sativae special fertilizer the most as claimed in claim 1 or 2, it is characterised in that Described phosphoric acid reacts with phosphoamide, for phosphoric acid solution and phosphoamide liquid reactions.
Prepare the production method of dipotassium hydrogen phosphate by-product Caulis et Folium Lactucae sativae special fertilizer the most as claimed in claim 1 or 2, it is characterised in that Described phosphoric acid reacts with phosphoamide, for phosphoric acid solid and phosphoamide liquid reactions.
Prepare the production method of dipotassium hydrogen phosphate by-product Caulis et Folium Lactucae sativae special fertilizer the most as claimed in claim 1 or 2, it is characterised in that Described alkaline potassium salt is the one in potassium carbonate, potassium acetate.
Prepare the production method of dipotassium hydrogen phosphate by-product Caulis et Folium Lactucae sativae special fertilizer the most as claimed in claim 1 or 2, it is characterised in that Described trace compound is calcium sulfate, Fe2+Chelate, the mixture of humic acid.
Prepare the production method of dipotassium hydrogen phosphate by-product Caulis et Folium Lactucae sativae special fertilizer the most as claimed in claim 1 or 2, it is characterised in that Described Caulis et Folium Lactucae sativae special fertilizer is compound state compound fertilizer, and its effective ingredient has In one or more mix Compound, carbon oxygen dotted line represents coordinate bond.
CN201410478361.7A 2014-09-19 2014-09-19 A kind of production method preparing dipotassium hydrogen phosphate by-product Caulis et Folium Lactucae sativae special fertilizer Expired - Fee Related CN104310352B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1191635A (en) * 1966-07-27 1970-05-13 Marchon Products Ltd Improvements in the manufacture of Orthophosphates
CN1060648A (en) * 1990-10-08 1992-04-29 邢新华 Polybasic fertilizer
CN1343186A (en) * 1999-03-18 2002-04-03 Oms投资公司 Processes for preparing granular composite fertilizer compositions and products produced thereby
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1191635A (en) * 1966-07-27 1970-05-13 Marchon Products Ltd Improvements in the manufacture of Orthophosphates
CN1060648A (en) * 1990-10-08 1992-04-29 邢新华 Polybasic fertilizer
CN1343186A (en) * 1999-03-18 2002-04-03 Oms投资公司 Processes for preparing granular composite fertilizer compositions and products produced thereby
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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