CN104261375A - Production method for preparing ammonium dihydrogen phosphate and byproduct special fertilizer for radix scutellariae - Google Patents
Production method for preparing ammonium dihydrogen phosphate and byproduct special fertilizer for radix scutellariae Download PDFInfo
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Abstract
The invention relates to the technical field of chemical engineering, and particularly relates to a production method for preparing ammonium dihydrogen phosphate and a byproduct special fertilizer for radix scutellariae. Through analysis on requirements on nutritional elements in the radix scutellariae growth process, analysis and realization of fertilization conditions of traditional radix scutellariae planting, research and discussion of the absorption conditions of crops on nitrogen, phosphorus and potassium, and analysis by combining with the defects in the preparation process of an ammonium dihydrogen phosphate product, the production process of the special fertilizer for the radix scutellariae is combined with the preparation process of the ammonium dihydrogen phosphate product, so that the preparation process of the ammonium dihydrogen phosphate product and the preparation process of the special fertilizer for the radix scutellariae are complementary; production of the special fertilizer for the radix scutellariae is carried out by using liquid waste generated in the preparation process of the ammonium dihydrogen phosphate product; the added value of the product in the preparation process of the ammonium dihydrogen phosphate product is increased; the discharge of the liquid waste is lowered; and meanwhile, deep crystallization of the ammonium dihydrogen phosphate product in the ammonium dihydrogen phosphate process is unnecessary, thus waste of nitrogen and phosphorus resources can also be avoided.
Description
Technical field
The present invention relates to chemical technology field, especially a kind of production method preparing the yellow Siberian cocklebur special fertilizer of primary ammonium phosphate by-product.
Background technology
Huang Ling, another name: bar Siberian cocklebur, sub-Siberian cocklebur, withered Siberian cocklebur, stalwart Siberian cocklebur, camellia root, perennial herb.Be born in dry endroit, can control seasonal febrile diseases heating, cough due to lung-heat, jaundice due to damp-heat, rush down the disease such as dysentery, threatened abortion, and have the effects such as antibacterial, antipyretic, step-down.Usually in the growing and cultivation technology of yellow Siberian cocklebur, adopt a large amount of miscellaneous fertilizers mixing, using phosphate fertilizer as base manure, and then be reached for the technique means that Huang Ling plantation provides nutritive ingredient, but, more than adopt a large amount of miscellaneous fertilizers mixing, Huang Lingshi is planted as base manure again using phosphate fertilizer, due to the native defect of crop itself, (specific absorption for nitrogenous fertilizer is about 20-46%, the specific absorption of phosphate fertilizer is about 10-25%, the specific absorption of potash fertilizer is about 46-60%), a large amount of n-p-k elements is made to remain in soil, cause the increase of fertilising cost, simultaneously so residual for a long time, Soil structure layer can be made to change, and then contaminate environment, increase the input of fertilizer nutrient, reduce the seed output and quality of Huang Ling.
Simultaneously, the preparation technology of primary ammonium phosphate product normally adopts phosphoric acid by wet process and thermal phosphoric acid to carry out producing, but be no matter that thermal phosphoric acid or Wet Processes of Phosphoric Acid are to prepare primary ammonium phosphate product, impact all can to the purity of primary ammonium phosphate product, make the purity of primary ammonium phosphate product poor, be difficult to meet industrial requirement, for this reason, in the process preparing primary ammonium phosphate product, the larger one-tenth of cost is needed originally to carry out the purification of primary ammonium phosphate product; For this reason, investigator is had to adopt intermediate substitute mode, with phosphoric acid and urea reaction to this, prepare Ureaphil intermediate, but this reaction completes below 80 DEG C, and then again by decrease temperature crystalline process, separate out primary ammonium phosphate product, and then raising primary ammonium phosphate product purity; ; often the needing of this processing step carries out degree of depth crystallization to primary ammonium phosphate; and then reduce the waste in the solution of nitrogen phosphoric to greatest extent, thus cost prepared by reduction primary ammonium phosphate product, relatively large discharging of waste liquid also can be avoided to cause certain pollution to environment; And in degree of depth crystallisation process, often along with the generation of other products, with primary ammonium phosphate crystallized mixed, and then can again have impact on the purity of primary ammonium phosphate product again.
For this reason, this investigator passes through in yellow Siberian cocklebur planting process, yellow Siberian cocklebur nutrient demand situation, and in conjunction with the defect existed in primary ammonium phosphate product preparation process, the preparation technology of yellow Siberian cocklebur special fertilizer preparation technology and primary ammonium phosphate product is combined, for the preparation technology of primary ammonium phosphate and Huang Ling special fertilizer 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 the yellow Siberian cocklebur special fertilizer of primary ammonium phosphate by-product, have and the preparation technology of yellow Siberian cocklebur special fertilizer preparation technology and primary ammonium phosphate product is combined, the waste liquid in primary ammonium phosphate product preparation process is adopted to carry out the preparation of yellow Siberian cocklebur special fertilizer, improve the added value in primary ammonium phosphate product preparation process, avoid simultaneously and degree of depth crystallization is carried out to reduce production cost to primary ammonium phosphate, further improve purity and the quality of primary ammonium phosphate product, also can prepare simultaneously and meet Huang Ling growth demand, and can guarantee to remain in the feature of the less N P and K double salt composite fertilizer of n-p-k element content in soil.
Be achieved particular by following technical scheme:
A kind of production method preparing the yellow Siberian cocklebur special fertilizer of primary ammonium phosphate by-product, phosphoric acid is adopted to be (1.5-1.7) with urea according to mol ratio: 1 mixes, and to adjust temperature be 90-140 DEG C, stirring reaction 1-3h, obtain intermediate slip, and ammonia is passed in intermediate slip, control temperature of reaction is 70-80 DEG C, stirring reaction 30-40min, reaction end pH value is 4.2-4.6, obtain phosphoric acid ammonium dihydrogen slip, and the product of phosphoric acid ammonium dihydrogen slip is placed in circulation temperature lowering crystallizer, carry out circulation temperature lowering crystallization treatment, and detect the nitrogen phosphorus element content analyzed in filtrate, adjustment nitrogen phosphorus element content reaches (1.2-1.5): when 1, stop the crystallization of primary ammonium phosphate product and filter, filter cake is primary 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 potassium component content wherein added and the content of nitrogen phosphoric compare for n-p-k element forms mol ratio for (1.2-1.5): 1:(1.1-1.3), 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 (1.5-1.7) according to mol ratio by phosphoric acid and urea: 1 in stirring-type reactor, be 90-140 DEG C in temperature, the stirring velocity controlling stirring tank is that 180-200r/min is uniformly mixed reaction 1-3h, obtains intermediate slip;
(2) primary ammonium phosphate is prepared: to step 1) pass into ammonia in the intermediate slip that obtains, and the temperature controlled in reactor is 70-80 DEG C, be 60-80r/min according to stirring velocity, stirring reaction 30-40min, reaction end pH value is 4.2-4.6, obtains the slip of phosphoric acid ammonium dihydrogen product;
(3) circulation crystallization filters: by step 2) slip that obtains phosphoric acid ammonium dihydrogen is placed in cooling crystallizer 10s 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 (1.2-1.5): when 1, stop crystallization and filter, acquisition filter cake is primary 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 (1.2-1.5): 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, heat-up rate is adopted to be that 3 DEG C/min is warming up to 45-55 DEG C, after dry 0.5-1h, adjustment moisture content is 1-3%, can obtain yellow Siberian cocklebur special chemical combination state composite fertilizer.
Described potassium composition is the one in potassium hydroxide, potassium sulfate, 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 10% of filtrate total amount.
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 primary ammonium phosphate product is: total nitrogen 13.01-13.32%, Vanadium Pentoxide in FLAKES are 60.05-61.15%.
When adding potassium composition and medium trace element compound, natural pond slag, slag liquid, the poultry manure that becomes thoroughly decomposed, Chinese medicine residue or other amino acid can also be added or amino acid is received.
Compared with prior art, the technique effect of technical scheme of the present invention is embodied in:
1. by analyzing the demand of yellow Siberian cocklebur process of growth Middle nutrition element, and undertaken analyzing by fertile situation to traditional yellow Siberian cocklebur plantation and understand, and to the absorbing state of n-p-k element, research and discussion is carried out to crop, analyze in conjunction with the shortcoming in primary ammonium phosphate product preparation process, and then the production technique of yellow Siberian cocklebur special fertilizer and the preparation technology of primary ammonium phosphate product are combined, the preparation technology of primary ammonium phosphate product and the preparation technology of Huang Ling special fertilizer is made to carry out complementation, the waste liquid produced in primary ammonium phosphate product preparation process is adopted to carry out the production of yellow Siberian cocklebur special fertilizer, improve the added value of product in primary ammonium phosphate product preparation process, reduce discharging of waste liquid amount, also make the waste also can avoiding nitrogen phosphor resource of unnecessary degree of depth crystalline ammonium dihydrogen product in primary ammonium phosphate technique simultaneously.
2. by the control of the processing parameter in phosphoric acid and urea reaction process, make the structural formula of Ureaphil that complicated change occur, and then form the complexity polymerization phosphorus urea gas ions of Nitrogen-and Phosphorus-containing, this gas ions can compared with the content of the n-p-k element in the control chemical combination state double salt structure of limits, and then the obtained azophoska salt chemical combination state composite fertilizer meeting yellow Siberian cocklebur process of growth needs, and the seed output and quality of Huang Ling is improved largely, reduce the planting cost of peasant household, avoid the environmental pollution that Fertilization Effect is brought, there is the significant value of environmental protection and economic benefit, , the purity of primary ammonium phosphate product is substantially increased meanwhile, the quality of primary ammonium phosphate product is guaranteed.
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 yellow Siberian cocklebur 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 ammonium dihydrogen 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 yellow Siberian cocklebur, trophic structure in adjustment filtrate, makes trophic structure layer meet the demand of yellow Siberian cocklebur, then dries the yellow Siberian cocklebur 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:
Primary 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 yellow Siberian cocklebur composite fertilizer special of chemical combination state of Multiple salts forms.
Noun illustrates:
Ureaphil (Urea phosphate, 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 the yellow Siberian cocklebur special fertilizer of primary ammonium phosphate by-product, comprise the following steps:
(1) raw material preparation mixing: by phosphoric acid and urea according to mol ratio be 1.5:1 in stirring-type reactor, be 90 DEG C in temperature, the stirring velocity controlling stirring tank is that 180r/min is uniformly mixed and reacts 1h, obtains intermediate slip;
(2) primary ammonium phosphate is prepared: to step 1) pass into ammonia in the intermediate slip that obtains, and the temperature controlled in reactor is 70 DEG C, is 60r/min according to stirring velocity, stirring reaction 30min, reaction end pH value is 4.2, obtains the slip of phosphoric acid ammonium dihydrogen product;
(3) circulation crystallization filters: by step 2) slip that obtains phosphoric acid ammonium dihydrogen is placed in cooling crystallizer 10s 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 1.2:1, stop crystallization and filter, acquisition filter cake is primary 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 1.2:1:1.1,
(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, after dry 0.5h, adjustment moisture content is 1%, can obtain yellow Siberian cocklebur special chemical combination state composite fertilizer.
Described potassium composition is potassium hydroxide.
Described medium trace element compound is the mixture of 0.7% calcium ion EDTA inner complex, 0.05% iron ion EDTA inner complex, 0.03% zine ion EDTA inner complex, 0.02% plasma selenium EDTA inner complex, 0.01% magnesium ion EDTA inner complex, 0.07% borax, 3.5% humic acid, 5.3% plant ash.
The concentration of described potassium composition is 30%.
By detecting, the nutrient content of primary ammonium phosphate product is: total nitrogen 13.01%, Vanadium Pentoxide in FLAKES are 60.05%.
Embodiment 2
Prepare a production method for the yellow Siberian cocklebur special fertilizer of primary ammonium phosphate by-product, comprise the following steps:
(1) raw material preparation mixing: by phosphoric acid and urea according to mol ratio be 1.7:1 in stirring-type reactor, be 140 DEG C in temperature, the stirring velocity controlling stirring tank is that 200r/min is uniformly mixed and reacts 3h, obtains intermediate slip;
(2) primary 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, is 80r/min according to stirring velocity, stirring reaction 40min, reaction end pH value is 4.6, obtains the slip of phosphoric acid ammonium dihydrogen product;
(3) circulation crystallization filters: by step 2) slip that obtains phosphoric acid ammonium dihydrogen is placed in cooling crystallizer 10s 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 1.5:1, stop crystallization and filter, acquisition filter cake is primary 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 1.5:1:1.3,
(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 1h, adjustment moisture content is 3%, can obtain yellow Siberian cocklebur special chemical combination state composite fertilizer.
Described potassium composition is potassium sulfate.
Described medium trace element compound is the mixture of 0.5% calcium ion EDTA inner complex, 0.03% iron ion EDTA inner complex, 0.04% zine ion EDTA inner complex, 0.03% plasma selenium EDTA inner complex, 0.03% magnesium ion EDTA inner complex, 0.06% borax, 2.5% humic acid, 3.3% plant ash.
The concentration of described potassium composition is 30%.
By detecting, the nutrient content of primary ammonium phosphate product is: total nitrogen 13.32%, Vanadium Pentoxide in FLAKES are 60.05%.
Embodiment 3
Prepare a production method for the yellow Siberian cocklebur special fertilizer of primary ammonium phosphate by-product, comprise the following steps:
(1) raw material preparation mixing: by phosphoric acid and urea according to mol ratio be 1.6:1 in stirring-type reactor, be 125 DEG C in temperature, the stirring velocity controlling stirring tank is that 190r/min is uniformly mixed and reacts 2h, obtains intermediate slip;
(2) primary ammonium phosphate is prepared: to step 1) pass into ammonia in the intermediate slip that obtains, and the temperature controlled in reactor is 75 DEG C, is 70r/min according to stirring velocity, stirring reaction 35min, reaction end pH value is 4.4, obtains the slip of phosphoric acid ammonium dihydrogen product;
(3) circulation crystallization filters: by step 2) slip that obtains phosphoric acid ammonium dihydrogen is placed in cooling crystallizer 10s 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 1.35:1, stop crystallization and filter, acquisition filter cake is primary 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 1.3:1:1.2,
(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 0.8h, adjustment moisture content is 2%, can obtain yellow Siberian cocklebur special chemical combination state composite fertilizer.
Described potassium composition is Repone K.
Described medium trace element compound is the mixture of 0.4% calcium ion EDTA inner complex, 0.03% iron ion EDTA inner complex, 0.01% zine ion EDTA inner complex, 0.01% plasma selenium EDTA inner complex, 0.02% magnesium ion EDTA inner complex, 0.03% borax, 6.5% humic acid, 2.3% plant ash.
The concentration of described potassium composition is 30%.
By detecting, the nutrient content of primary ammonium phosphate product is: total nitrogen 13.15%, Vanadium Pentoxide in FLAKES are 60.64%.
Test example: the technique effect of technical scheme of the present invention and product performance are described further below in conjunction with specific embodiment content.
The yellow Siberian cocklebur of test example the present invention special chemical combination state composite fertilizer is to yellow Siberian cocklebur growth situation and qualitative effects situation.
1.1 experiment process
Experimental group: adopt the yellow Siberian cocklebur special chemical combination state composite fertilizer traditionally planting technology that the embodiment of the present invention 1, embodiment 2, embodiment 3 prepare, plant yellow Siberian cocklebur, according to every mu of fertilising 97kg yellow Siberian cocklebur special chemical combination state composite fertilizer prepared of the present invention, and using traditional farm manure as base manure.
Control group: adopt traditional compounded technology, carries out proportionally mixed preparing with traditional chemical fertilizer such as potassium primary phosphate, primary ammonium phosphate, dipotassium hydrogen phosphate, ammonium nitrate, potassium sulfate, and according to every mu of fertilising 97kg, and using farm manure as base manure.
Note: experimental group is consistent with the amount of the farm manure that control group adopts.
1.2 experimental result
Take the root weight of Huang Ling, and the root choosing the yellow Siberian cocklebur of experimental group and control group carries out the detection of nutrient substance, its result is as shown in table 1:
Table 1:
As can be seen from data presentation result in table, the present invention can improve the content of the inner nutrient substance of yellow Siberian cocklebur, improves the quality of yellow Siberian cocklebur, and yellow Siberian cocklebur root growth can be made better, improves yellow Siberian cocklebur product, and then changes the quality and yield of Huang Ling, have significant progress.
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; be not limited to the further restriction to technical scheme of the present invention; those skilled in the art make the improvement of non-protruding essential characteristics and non-significant progress on this basis, all belong to protection category of the present invention.
Claims (6)
1. prepare the production method of the yellow Siberian cocklebur special fertilizer of primary ammonium phosphate by-product for one kind, it is characterized in that, phosphoric acid is adopted to be (1.5-1.7) with urea according to mol ratio: 1 mixes, and to adjust temperature be 90-140 DEG C, stirring reaction 1-3h, obtain intermediate slip, and ammonia is passed in intermediate slip, control temperature of reaction is 70-80 DEG C, stirring reaction 30-40min, reaction end pH value is 4.2-4.6, obtain phosphoric acid ammonium dihydrogen slip, and the product of phosphoric acid ammonium dihydrogen slip is placed in circulation temperature lowering crystallizer, carry out circulation temperature lowering crystallization treatment, and detect the nitrogen phosphorus element content analyzed in filtrate, adjustment nitrogen phosphorus element content reaches (1.2-1.5): when 1, stop the crystallization of primary ammonium phosphate product and filter, filter cake is primary 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 potassium component content wherein added and the content of nitrogen phosphoric compare for n-p-k element forms mol ratio for (1.2-1.5): 1:(1.1-1.3), 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 the yellow Siberian cocklebur special fertilizer of primary ammonium phosphate by-product as claimed in claim 1, it is characterized in that, comprise the following steps:
(1) raw material preparation mixing: be (1.5-1.7) according to mol ratio by phosphoric acid and urea: 1 in stirring-type reactor, be 90-140 DEG C in temperature, the stirring velocity controlling stirring tank is that 180-200r/min is uniformly mixed reaction 1-3h, obtains intermediate slip;
(2) primary ammonium phosphate is prepared: to step 1) pass into ammonia in the intermediate slip that obtains, and the temperature controlled in reactor is 70-80 DEG C, be 60-80r/min according to stirring velocity, stirring reaction 30-40min, reaction end pH value is 4.2-4.6, obtains the slip of phosphoric acid ammonium dihydrogen product;
(3) circulation crystallization filters: by step 2) slip that obtains phosphoric acid ammonium dihydrogen is placed in cooling crystallizer 10s 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 (1.2-1.5): when 1, stop crystallization and filter, acquisition filter cake is primary 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 (1.2-1.5): 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, heat-up rate is adopted to be that 3 DEG C/min is warming up to 45-55 DEG C, after dry 0.5-1h, adjustment moisture content is 1-3%, can obtain yellow Siberian cocklebur special chemical combination state composite fertilizer.
3. prepare the production method of the yellow Siberian cocklebur special fertilizer of primary ammonium phosphate by-product as claimed in claim 1 or 2, it is characterized in that, described potassium composition is the one in potassium hydroxide, potassium sulfate, Repone K.
4. prepare the production method of the yellow Siberian cocklebur special fertilizer of primary ammonium phosphate by-product 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 the yellow Siberian cocklebur special fertilizer of primary ammonium phosphate by-product 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 the yellow Siberian cocklebur special fertilizer of primary ammonium phosphate by-product as claimed in claim 1 or 2, it is characterized in that, the nutrient content of described primary ammonium phosphate product is: total nitrogen 13.01-13.32%, Vanadium Pentoxide in FLAKES are 60.05-61.15%.
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| CN108046226A (en) * | 2017-12-22 | 2018-05-18 | 贵阳开磷化肥有限公司 | A kind of production method of PHOSPHORIC ACID TECH.GRADE dihydro coproducing ammonium Water soluble fertilizer |
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| CN1060648A (en) * | 1990-10-08 | 1992-04-29 | 邢新华 | Polybasic fertilizer |
| CN103787293A (en) * | 2014-01-24 | 2014-05-14 | 贵阳中化开磷化肥有限公司 | Method for preparing sodium dihydrogen phosphate by utilizing phosphoric acid by wet process |
| CN104016323A (en) * | 2014-05-20 | 2014-09-03 | 贵阳中化开磷化肥有限公司 | Production method for monoammonium phosphate |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108046226A (en) * | 2017-12-22 | 2018-05-18 | 贵阳开磷化肥有限公司 | A kind of production method of PHOSPHORIC ACID TECH.GRADE dihydro coproducing ammonium Water soluble fertilizer |
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| CN104261375B (en) | 2017-04-19 |
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Address after: Xifeng County in Guizhou Province, Guiyang city town 551109 Applicant after: Guiyang Kailin Chemical Co. Ltd. Applicant after: Guizhou Ke Xinhua smelting company limited Applicant after: Guizhou University Address before: Xifeng County in Guizhou Province, Guiyang city town 551109 Applicant before: Zhonghuakai Phosphorous Chemical Fertilizer Co., Ltd., Guiyang Applicant before: Guizhou Ke Xinhua smelting company limited Applicant before: Guizhou University |
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