CN104276551B - A kind of production method preparing Secondary ammonium phosphate by-product oat special fertilizer - Google Patents
A kind of production method preparing Secondary ammonium phosphate by-product oat special fertilizer Download PDFInfo
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Abstract
The present invention relates to chemical technology field, especially a kind of production method preparing Secondary ammonium phosphate by-product oat special fertilizer, by requiring to analyze to the need fertilizer of oat, and the shortcoming existed in primary ammonium phosphate product preparation process step is analyzed, and then the preparation technology of oat special fertilizer with primary ammonium phosphate product is combined, complementation is carried out by two incoherent techniques, while improving the added value in primary ammonium phosphate product preparation process, improve the purity of primary ammonium phosphate product, the element resources such as nitrogen phosphorus are saved, reduce discharging of waste liquid amount, by carrying out controlling and adjustment to the nutritive element in the waste liquid produced in primary ammonium phosphate product preparation process, while making the elements such as the nitrogen phosphorus in waste liquid can meet Oat Growth demand, the purity improving primary ammonium phosphate product reaches more than 93%, and reduce and remain in nitrogen phosphoric in waste liquid, decrease the quantity discharged of waste liquid, there is the significant value of environmental protection and economic benefit.
Description
Technical field
The present invention relates to chemical technology field, especially a kind of production method preparing Secondary ammonium phosphate by-product oat special fertilizer.
Background technology
Oat is grass, is called naked oats in China, is commonly called as naked oats, maize, bromegrass, wild wheat, is a kind of low sugar, high nutrition, high energy food.Oat is rich in food fibre, and can promote enterogastric peristalsis, be beneficial to defecation, heat is low, and glycemic index is low, blood lipid-reducing blood sugar-decreasing, is also one of high-grade tonic, is indispensable solid food in distressed area.Comprehensively analyze according to Chinese Academy of Medical Sciences's health research, Chinese naked oats reaches 15.6% containing crude protein, and fat 8.5% also has the element such as starch release heat and phosphorus, iron, calcium, compared with other 8 kinds of grains, all comes out at the top.In oat, water-soluble dietary fibre is 4.7 times and 7.7 times of wheat and maize respectively.Vitamin B group in oat, nicotinic acid, folic acid, pantothenic acid are all abundanter, particularly vitamin-E, up to 15 milligrams in every 100 grams of oatmeals.In addition the saponin (main component of ginseng) all lacked in cereal grain is also contained in oatmeal.The amino acid ratio of components of protein is comparatively comprehensive, all ranking first of 8 seed amino acid content of needed by human, especially containing Methionin up to 0.68 gram; According to " animal feeding science ", containing crude protein 5.2%, crude fat 2.2%, nitrogen free extract 44.6% in naked oats stalk, all high than millet straw, wheat straw, cornstalk; Be difficult to the fiber 28.2% digested, lower by 4.9 ~ 16.4% than wheat, corn, grain straw, be one of best forage grass.Its seed is the high-quality feed of raising cub, old poultry, ill domestic animal and weighing the draught animal and the domestic animals and fowls such as chicken, pig.It has stronger edibleness, whitening health value.
In traditional Oatplanting technology, normally adopt primary ammonium phosphate, potassium primary phosphate, ammonium nitrate, the traditional chemical combination state composite fertilizer such as ammonium sulfate carries out the composite fertilizer of the mixed state of a certain proportion of mixed preparing, and then meet the demand of cereals nutrient composition, promote the normal growth fast of oat, improve the seed output and quality of oat, but oat special fertilizer prepared according to a certain ratio by the fertilizer of this employing chemical combination state, often cause the preparation of certain element excessive, and then the nutritive element mismatch making in fertilizer, cause after certain element absorption completes, other elements of part are also had not absorbed in addition, and then remain among soil, cause the waste of fertilizer and the pollution of environment, increase peasant household's Oatplanting cost, and it is theoretical according to wooden barrel short slab, during nutritive element in Crop fertilizer, when lacking certain element, be difficult to form effective nutrient transport, also can affect to the normal growth of the crops such as oat, affect the normal growth of the farm crop such as oat.
Simultaneously, in preparation technology for Secondary ammonium phosphate product, normally adopt thermal phosphoric acid and phosphoric acid by wet process, no matter but be that thermal phosphoric acid or phosphoric acid by wet process prepare primary ammonium phosphate product, all can have in its technique a large amount of impurity elements pure, make the purity of the primary ammonium phosphate product prepared poor, and, the primary ammonium phosphate product adopting thermal phosphoric acid or phosphoric acid by wet process to prepare out is carrying out in crystallization treatment step, often also need the waste being reduced starting material element by degree of depth crystallization treatment, economize in raw materials resource, reduce the preparation cost of primary ammonium phosphate product, reduce the quantity discharged of waste liquid, but this process can make primary ammonium phosphate bring other impurity into when degree of depth crystallization, and then affect the purity of primary ammonium phosphate product, do not carry out degree of depth crystallization, the output of primary ammonium phosphate product is lower, and a large amount of nitrogen phosphor resources can be wasted, production cost is caused to improve.
For this reason, this investigator is by the production process of primary ammonium phosphate product, analyze in conjunction with to oat special fertilizer feature, and carry out analyzing to cereals nutrient value and understand, through long-term Exploration & stu dy, the preparation technology of primary ammonium phosphate product is combined with the preparation technology of oat special fertilizer, for the preparation technology of oat special fertilizer and primary ammonium phosphate product provides 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 Secondary ammonium phosphate by-product oat special fertilizer, have and the preparation technology of primary ammonium phosphate product is combined with the preparation technology of oat special fertilizer, and then provide feasible scheme for the liquid waste disposal in primary ammonium phosphate product preparation process, and pass through the liquid waste disposal in primary ammonium phosphate product preparation process, avoid the degree of depth crystallization of primary ammonium phosphate product, improve the purity of primary ammonium phosphate product, reduce waste liquid amount discharge, improve the added value of product of primary ammonium phosphate product preparation process, there is the features such as the significant value of environmental protection and economic benefit.
Be achieved particular by following technical scheme:
Prepare a production method for Secondary ammonium phosphate by-product oat special fertilizer, adopt phosphoric acid and urea to be (1.4-1.9) according to mol ratio: 1, be 80-130 DEG C in temperature, after stirring reaction 2-3h, obtain intermediate slurry; Again intermediate slurry and ammonia are carried out hybrid reaction, and control temperature is 50-80 DEG C, when adjustment pH value is 7.8-8.2, after stirring reaction 30-50min, obtains the slip of phosphoric acid hydrogen two ammonium, and the slip of phosphoric acid hydrogen two ammonium is carried out circulation temperature lowering crystallization treatment, and the N∶P ratio detected in analysis and regulation solution is 1:(1.1-1.3) time, stop crystallization and filter, filter cake is Secondary ammonium phosphate product; In filtrate, add potassium composition and medium trace element compound be adjusted to chemical combination state composite fertilizer just finished product, the content of the potassium component content wherein added and nitrogen phosphoric is 1.1:(1.1-1.3 than for n-p-k element forms mol ratio): (1.3-1.9); 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 0.5-2h, adjustment moisture content is 1-4%, can obtain oat special chemical combination state composite fertilizer.
Specifically comprise the following steps:
(1) raw material preparation mixing: be (1.4-1.9) according to mol ratio by phosphoric acid and urea: 1 in stirring-type reactor, be 80-130 DEG C in temperature, the stirring velocity controlling stirring tank is that 180-200r/min is uniformly mixed reaction 2-3h, obtains intermediate slip;
(2) Secondary ammonium phosphate is prepared: to step 1) pass into ammonia in the intermediate slip that obtains, and the temperature controlled in reactor is 50-80 DEG C, when adjustment pH value is 7.8-8.2, be 60-80r/min according to stirring velocity, stirring reaction 30-50min, obtains the slip of phosphoric acid hydrogen two ammonium product;
(3) circulation crystallization filters: by step 2) slip that obtains phosphoric acid hydrogen two ammonium is placed in cooling crystallizer 15s and is cooled to temperature≤40 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, treat nitrogen component, the mol ratio of phosphorus composition is 1:(1.1-1.3) time, stop crystallization and filter, acquisition filter cake is Secondary ammonium phosphate, potassium composition is added and medium trace element compound adjustment fertilizer structure becomes chemical combination state composite fertilizer just finished product in filtrate, the ratio that the potassium component content wherein added is n-p-k element with the content ratio of nitrogen phosphoric is 1.1:(1.1-1.3): (1.3-1.9),
(4) filtrate dries: by step 3) the chemical combination state composite fertilizer that obtains just finished product be placed in baker, heat-up rate is adopted to be that 3 DEG C/min is warming up to 40-50 DEG C, after dry 0.5-2h, adjustment moisture content is 1-4%, can obtain oat special chemical combination state composite fertilizer.
Described potassium composition is the one in potassium hydroxide, potassium sulphide, Repone K.
Described medium trace element compound is the mixture of calcium ion EDTA inner complex, iron ion EDTA inner complex, zine ion EDTA inner complex, plasma selenium EDTA inner complex, magnesium ion EDTA inner complex, borax, humic acid, plant ash.
The concentration of described potassium composition is 30%.
The total addition level of described medium trace element compound is about 12% of filtrate gross weight.
Described chemical combination state composite fertilizer, containing following N P and K chemical combination state structural formula in its composition:
wherein, the dotted line between carbon atom and Sauerstoffatom represents to there is coordinate bond between C atom and O atom.
The nutrient content of described Secondary ammonium phosphate product is: total nitrogen 12.01-12.23%, Vanadium Pentoxide in FLAKES are 61.05-61.25%.
When carrying out potassium composition and medium trace element adds, the animal excretion become thoroughly decomposed can also be added wherein, other organic or inanimate matter materials such as natural pond slag and straw powder.
Compared with prior art, the technique effect of technical scheme of the present invention is embodied in:
1, by requiring to analyze to the need fertilizer of oat, and the shortcoming existed in primary ammonium phosphate product preparation process step is analyzed, and then the preparation technology of oat special fertilizer with primary ammonium phosphate product is combined, complementation is carried out by two incoherent techniques, while improving the added value in primary ammonium phosphate product preparation process, improve the purity of primary ammonium phosphate product, saved the element resources such as nitrogen phosphorus, reduced discharging of waste liquid amount.
2, by carrying out controlling and adjustment to the nutritive element in the waste liquid produced in primary ammonium phosphate product preparation process, while making the elements such as the nitrogen phosphorus in waste liquid can meet Oat Growth demand, the purity improving primary ammonium phosphate product reaches more than 93%, and reduce and remain in nitrogen phosphoric in waste liquid, decrease the quantity discharged of waste liquid, there is the significant value of environmental protection and economic benefit.
3, 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 absorbed by crops, 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 oat 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)
-(CO
5pN
2h
8)
+ion, when adding excessive and appropriate ammonium radical ion, dihydrogen phosphate and ammonium radical ion form Secondary ammonium phosphate crystal and are precipitated, and by detecting the content of the nitrogen phosphoric analyzed in filtrate, and add potassium element, magnesium elements, ferro element and other medium trace element according to the demand of oat, trophic structure in adjustment filtrate, makes trophic structure layer meet the demand of oat, then dries the oat special chemical combination state composite fertilizer that can obtain containing N, P, K and other elements.
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:
Secondary ammonium phosphate product to be crystallized out after, then in filtrate, add potassium element and other elements, then can with the dihydrogen phosphate remained in filtrate, hydrogen phosphate and
intermediate-ion react, generate the chemical combination state oat composite fertilizer special of Multiple salts forms.
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 Secondary ammonium phosphate by-product oat special fertilizer, comprise the following steps:
(1) raw material preparation mixing: by phosphoric acid and urea according to mol ratio be 1.4:1 in stirring-type reactor, be 80 DEG C in temperature, the stirring velocity controlling stirring tank is that 180r/min is uniformly mixed and reacts 2h, obtains intermediate slip;
(2) Secondary ammonium phosphate is prepared: to step 1) pass into ammonia in the intermediate slip that obtains, and the temperature controlled in reactor is 50 DEG C, when adjustment pH value is 7.8, be 60r/min according to stirring velocity, stirring reaction 30min, obtains the slip of phosphoric acid hydrogen two ammonium product;
(3) circulation crystallization filters: by step 2) slip that obtains phosphoric acid hydrogen two ammonium is placed in cooling crystallizer 15s and is cooled to temperature 40 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, treat nitrogen component, when the mol ratio of phosphorus composition is 1:1.1, stop crystallization and filter, acquisition filter cake is Secondary ammonium phosphate, potassium composition is added and medium trace element compound adjustment fertilizer structure becomes chemical combination state composite fertilizer just finished product in filtrate, the ratio that the potassium component content wherein added is n-p-k element with the content ratio of nitrogen phosphoric is 1.1:1.1:1.3,
(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, after dry 0.5h, adjustment moisture content is 1%, can obtain oat special chemical combination state composite fertilizer.
Described potassium composition is potassium hydroxide.
Described medium trace element compound is the mixture of 0.05% calcium ion EDTA inner complex, 0.07% iron ion EDTA inner complex, 0.09% zine ion EDTA inner complex, 0.02% plasma selenium EDTA inner complex, 0.03% magnesium ion EDTA inner complex, 0.6% borax, 3.7% humic acid, 4.5% plant ash.
The concentration of described potassium composition is 30%.
By detecting, the nutrient content of Secondary ammonium phosphate product is: total nitrogen 12.01%, Vanadium Pentoxide in FLAKES are 61.05%.
Embodiment 2
Prepare a production method for Secondary ammonium phosphate by-product oat special fertilizer, comprise the following steps:
(1) raw material preparation mixing: by phosphoric acid and urea according to mol ratio be 1.9:1 in stirring-type reactor, be 130 DEG C in temperature, the stirring velocity controlling stirring tank is that 200r/min is uniformly mixed and reacts 3h, obtains intermediate slip;
(2) Secondary ammonium phosphate is prepared: to step 1) pass into ammonia in the intermediate slip that obtains, and the temperature controlled in reactor is 80 DEG C, when adjustment pH value is 8.2, be 80r/min according to stirring velocity, stirring reaction 50min, obtains the slip of phosphoric acid hydrogen two ammonium product;
(3) circulation crystallization filters: by step 2) slip that obtains phosphoric acid hydrogen two ammonium is placed in cooling crystallizer 15s and is cooled to temperature 30 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, treat nitrogen component, when the mol ratio of phosphorus composition is 1:1.3, stop crystallization and filter, acquisition filter cake is Secondary ammonium phosphate, potassium composition is added and medium trace element compound adjustment fertilizer structure becomes chemical combination state composite fertilizer just finished product in filtrate, the ratio that the potassium component content wherein added is n-p-k element with the content ratio of nitrogen phosphoric is 1.1:1.3:1.9,
(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, after dry 2h, adjustment moisture content is 4%, can obtain oat special chemical combination state composite fertilizer.
Described potassium composition is potassium sulphide.
Described medium trace element compound is the mixture of 0.07% calcium ion EDTA inner complex, 0.05% iron ion EDTA inner complex, 0.04% zine ion EDTA inner complex, 0.05% plasma selenium EDTA inner complex, 0.06% magnesium ion EDTA inner complex, 0.2% borax, 5.5% humic acid, 3.2% plant ash.
The concentration of described potassium composition is 30%.
The total addition level of described medium trace element compound is 11% of filtrate gross weight.
The nutrient content of described Secondary ammonium phosphate product is: total nitrogen 12.23%, Vanadium Pentoxide in FLAKES are 61.05%.
Embodiment 3
Prepare a production method for Secondary ammonium phosphate by-product oat special fertilizer, comprise the following steps:
(1) raw material preparation mixing: by phosphoric acid and urea according to mol ratio be 1.65:1 in stirring-type reactor, temperature 115 DEG C, the stirring velocity controlling stirring tank is that 190r/min is uniformly mixed and reacts 2.5h, obtains intermediate slip;
(2) Secondary ammonium phosphate is prepared: to step 1) pass into ammonia in the intermediate slip that obtains, and the temperature controlled in reactor is 65 DEG C, when adjustment pH value is 8, be 70r/min according to stirring velocity, stirring reaction 40min, obtains the slip of phosphoric acid hydrogen two ammonium product;
(3) circulation crystallization filters: by step 2) slip that obtains phosphoric acid hydrogen two ammonium is placed in cooling crystallizer 15s and is cooled to temperature 35 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, treat nitrogen component, when the mol ratio of phosphorus composition is 1:1.2, stop crystallization and filter, acquisition filter cake is Secondary ammonium phosphate, potassium composition is added and medium trace element compound adjustment fertilizer structure becomes chemical combination state composite fertilizer just finished product in filtrate, the ratio that the potassium component content wherein added is n-p-k element with the content ratio of nitrogen phosphoric is 1.1:1.2:1.6,
(4) filtrate dries: by step 3) the chemical combination state composite fertilizer that obtains just finished product be placed in baker, heat-up rate is adopted to be that 3 DEG C/min is warming up to 45 DEG C, after dry 1.5h, adjustment moisture content is 2.5%, can obtain oat special chemical combination state composite fertilizer.
Described potassium composition is Repone K.
Described medium trace element compound is the mixture of 0.8% calcium ion EDTA inner complex, 0.01% iron ion EDTA inner complex, 0.02% zine ion EDTA inner complex, 0.08% plasma selenium EDTA inner complex, 0.06% magnesium ion EDTA inner complex, 0.06% borax, 4.5% humic acid, 2.8% plant ash.
The concentration of described potassium composition is 30%.
The total addition level of described medium trace element compound is about 12% of filtrate gross weight.
By detecting, the nutrient content of Secondary ammonium phosphate product is: total nitrogen 12.12%, Vanadium Pentoxide in FLAKES are 61.15%.
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: oat of the present invention special chemical combination state composite fertilizer is on the impact of amount of oat yield
Experimental group: adopt the obtained oat special chemical combination state composite fertilizer of embodiment 1, embodiment 2, embodiment 3 traditionally implantation methods add this composite fertilizer 100kg/ mu and carry out Oatplanting 5 mu, single fertilization process completes, and weighing oat weight is 208.45kg/ mu.
Control group: the composite fertilizer adopting traditional technology to prepare implantation methods traditionally adds composite fertilizer 100kg/ mu and carries out Oatplanting 5 mu, and single fertilization process completes, and weighing oat weight is 197.12kg/ mu.Note: the composite fertilizer that traditional technology of employing prepares is that to carry out N P and K by existing chemical fertilizer such as ammonium fertilizer, phosphate fertilizer, potash fertilizer, ammonium fertiliser containing magnesiums be the formulated composite fertilizer of 1:1.1-1.3:1.3-1.9, and experimental group and control group are all added with farm manure as base manure.
Can be drawn by simultaneous test, oat composite fertilizer special of the present invention is than traditional composite every mu of volume increase about 11.33kg, and stimulation ratio reaches about 5.75%, has significant economic benefit.
It is important to point out at this; above embodiment and test example are only limitted to do further explaination to the technique effect that technical scheme of the present invention can reach and understand; it is not limitation of the invention further; therefore the amendment of the essential characteristics of the non-protruding made on this basis and non-significant progress and improvement, still belong to protection category of the present invention.
Claims (6)
1. prepare a production method for Secondary ammonium phosphate by-product oat special fertilizer, it is characterized in that, adopt phosphoric acid and urea to be (1.4-1.9) according to mol ratio: 1, be 80-130 DEG C in temperature, after stirring reaction 2-3h, obtain intermediate slurry; Again intermediate slurry and ammonia are carried out hybrid reaction, and control temperature is 50-80 DEG C, when adjustment pH value is 7.8-8.2, after stirring reaction 30-50min, obtains the slip of phosphoric acid hydrogen two ammonium, and the slip of phosphoric acid hydrogen two ammonium is carried out circulation temperature lowering crystallization treatment, and the N∶P ratio detected in analysis and regulation solution is 1:(1.1-1.3) time, stop crystallization and filter, filter cake is Secondary ammonium phosphate product; In filtrate, add potassium composition and medium trace element compound be adjusted to chemical combination state composite fertilizer just finished product, the content of the potassium component content wherein added and nitrogen phosphoric is 1.1:(1.1-1.3 than for n-p-k element forms mol ratio): (1.3-1.9); 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 0.5-2h, adjustment moisture content is 1-4%, can obtain oat special chemical combination state composite fertilizer.
2. prepare the production method of Secondary ammonium phosphate by-product oat special fertilizer as claimed in claim 1, it is characterized in that, comprise the following steps:
(1) raw material preparation mixing: be (1.4-1.9) according to mol ratio by phosphoric acid and urea: 1 in stirring-type reactor, be 80-130 DEG C in temperature, the stirring velocity controlling stirring tank is that 180-200r/min is uniformly mixed reaction 2-3h, obtains intermediate slip;
(2) Secondary ammonium phosphate is prepared: to step 1) pass into ammonia in the intermediate slip that obtains, and the temperature controlled in reactor is 50-80 DEG C, when adjustment pH value is 7.8-8.2, be 60-80r/min according to stirring velocity, stirring reaction 30-50min, obtains the slip of phosphoric acid hydrogen two ammonium product;
(3) circulation crystallization filters: by step 2) slip that obtains phosphoric acid hydrogen two ammonium is placed in cooling crystallizer 15s and is cooled to temperature≤40 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, treat nitrogen component, the mol ratio of phosphorus composition is 1:(1.1-1.3) time, stop crystallization and filter, acquisition filter cake is Secondary ammonium phosphate, potassium composition is added and medium trace element compound adjustment fertilizer structure becomes chemical combination state composite fertilizer just finished product in filtrate, the ratio that the potassium component content wherein added is n-p-k element with the content ratio of nitrogen phosphoric is 1.1:(1.1-1.3): (1.3-1.9),
(4) filtrate dries: by step 3) the chemical combination state composite fertilizer that obtains just finished product be placed in baker, heat-up rate is adopted to be that 3 DEG C/min is warming up to 45-55 DEG C, after dry 0.5-2h, adjustment moisture content is 1-4%, can obtain oat special chemical combination state composite fertilizer.
3. prepare the production method of Secondary ammonium phosphate by-product oat special fertilizer as claimed in claim 1 or 2, it is characterized in that, described potassium composition is the one in potassium hydroxide, potassium sulphide, Repone K.
4. prepare the production method of Secondary ammonium phosphate by-product oat special fertilizer as claimed in claim 1 or 2, it is characterized in that, described medium trace element compound is the mixture of calcium ion EDTA inner complex, iron ion EDTA inner complex, zine ion EDTA inner complex, plasma selenium EDTA inner complex, magnesium ion EDTA inner complex, borax, humic acid, plant ash.
5. prepare the production method of Secondary ammonium phosphate by-product oat special fertilizer as claimed in claim 1 or 2, it is characterized in that, described chemical combination state composite fertilizer, containing following N P and K chemical combination state structural formula in its composition:
wherein, the dotted line between carbon atom and Sauerstoffatom represents to there is coordinate bond between C atom and O atom.
6. prepare the production method of Secondary ammonium phosphate by-product oat special fertilizer as claimed in claim 1 or 2, it is characterized in that, the nutrient content of described Secondary ammonium phosphate product is: total nitrogen 12.01-12.23%, Vanadium Pentoxide in FLAKES are 61.05-61.25%.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1060648A (en) * | 1990-10-08 | 1992-04-29 | 邢新华 | Polybasic fertilizer |
| CN1127738A (en) * | 1995-01-26 | 1996-07-31 | 杨馥成 | Full nutritive element plant growth regulating composition and preparing process thereof |
| CN101215202A (en) * | 2007-12-27 | 2008-07-09 | 山东大学 | Leaf vegetable release-controlling fertilizer |
| CN104016322A (en) * | 2014-05-20 | 2014-09-03 | 贵阳中化开磷化肥有限公司 | Production method for diammonium hydrogen phosphate |
-
2014
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1060648A (en) * | 1990-10-08 | 1992-04-29 | 邢新华 | Polybasic fertilizer |
| CN1127738A (en) * | 1995-01-26 | 1996-07-31 | 杨馥成 | Full nutritive element plant growth regulating composition and preparing process thereof |
| CN101215202A (en) * | 2007-12-27 | 2008-07-09 | 山东大学 | Leaf vegetable release-controlling fertilizer |
| CN104016322A (en) * | 2014-05-20 | 2014-09-03 | 贵阳中化开磷化肥有限公司 | Production method for diammonium hydrogen phosphate |
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