CN104310340A - Method for preparing ammonium dihydrogen phosphate and preparing special fertilizer for beet as byproduct - Google Patents
Method for preparing ammonium dihydrogen phosphate and preparing special fertilizer for beet as byproduct Download PDFInfo
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Abstract
The invention relates to the technical field of chemical industry, and especially relates to a method for preparing ammonium dihydrogen phosphate and preparing a special fertilizer for beet as a byproduct. The temperature and other coefficients of the preparation of ammonium dihydrogen phosphate from phosphoric acid through a wet process are changed, so the purity of the ammonium dihydrogen phosphate product is improved, and the N, P and K compounded fertilizer is produced. The method improves the purity of ammonium dihydrogen phosphate, and the produced special fertilizer for beet has high absorptivity, can meet the nutrition needs of beet in all stages of the growth period of beet, greatly increases the output of beet, and is an efficient compound fertilizer.
Description
Technical field
The present invention relates to chemical technology field, particularly relate to a kind of production method preparing primary ammonium phosphate by-product beet special fertilizer.
Background technology
Beet, (Beta vulgaris), You Ming Chard dish, biennial herb plant, originates in western European and Southern Coast, is transplanted to Spain from Sweden, is a main sugar source beyond tropical sugarcane.The pigment content of beet tails is very abundant, primary pigments is called beet red (Betalains), comprise red Betacyanins and the Betaxanthins of yellow, the beet tails of most kind contains the red Betacyanin of more amount, the beet tails of every 100 g contains the pigment up to 200 milligrams, is good pigment source.
Current domestic beet seed manure used is substantially all diammonium phosphate, and this is also the seed manure agriculturally generally applied.Its main component is Vanadium Pentoxide in FLAKES (P2O5) 46%, nitrogen (N) 18%.Because different crops is different to nutrient absorption law, susceptibility is different, so diammonium phosphate has used many problems on beet, such as, in diammonium phosphate, nitrogen content is higher, and beet kind bud is more weak, ammonia (NH3) often occurs in soil to burn kind of a bud phenomenon, the lighter is short of seedling disconnected ridge, and severe one big area is not emerged.
In diammonium phosphate, nitrogen content is high has promoter action to beet seedling stage growth, particularly nitrogen metabolism vigorous growth center continues part on the ground, this situation is unfavorable for that beet young root stretches to underground, so Sugarbeet Growth has occurred that root deformation is short, root head increases Sugar Content and declines.Sugar beet utilizes beet root, and above-mentioned phenomenon directly affects sugar refinery economic benefit.
Mainly concentrate on northeast, North China, the Northwest in China's beet producing region at present, these areas are all calcareous soils, because calcium in calcareous soil and water-soluble phosphorus have fixed action, make validity phosphoric acid-calcium transform the difficult octocalcium phosphate utilized by beet.Therefore, the phosphorus in diammonium phosphate in a large number fix by the calcium in soil, utilization ratio is very low is generally 10 ~ 20%.Although therefore in diammonium phosphate, content is very high, its effect is unsatisfactory, and enriches the danger that diammonium phosphate there will be again kind of bud of burning.Through the test of diammonium phosphate rate of fertilizer application for many years, enrich diammonium phosphate and do not increase production, increase sugared effect, otherwise along with diammonium phosphate consumption increases, sugar content falls progressively.
For in production primary ammonium phosphate process, the purity of primary ammonium phosphate is not high, also containing a large amount of undecomposed carboxamide, H in filtrate
2pO
4 -, HPO
4 2-, PO
4 3-deng material, investigator of the present invention is from a large amount of prior art documents and Exploration & stu dy for many years, and traditional component content of beet special fertilizer and the absorbing state of beet are studied, effectively inquire into out and produce beet special fertilizer from the filtrate of Wet-process Phosphoric Acid Production primary ammonium phosphate, the purity solving Wet-process Phosphoric Acid Production primary ammonium phosphate is not high, in filtrate, effective constituent such as cannot to utilize at the problem, the effect of the good and realizing controlled-release of the specific absorption of this special fertilizer simultaneously, at home in fertiliser production, have no report.
Summary of the invention
For above technical problem, the invention provides a kind of production method preparing primary ammonium phosphate by-product beet special fertilizer, by the process production design of uniqueness, improve the purity of primary ammonium phosphate, make full use of the effective constituent of wet process phosphoric acid for preparing primary ammonium phosphate simultaneously, produce out the beet special fertilizer of applicable Sugarbeet Growth.
The present invention is achieved by the following technical solutions:
A kind of production method preparing primary ammonium phosphate by-product beet special fertilizer provided by the invention, mainly comprises the following steps:
1) adopt phosphoric acid to mix with carboxamide, and be that 3 ~ 8 DEG C/min is warming up to 160 DEG C from 80 DEG C with heat-up rate, stirring reaction 4-5h, separation obtains intermediate, add in ammonia soln by intermediate again, temperature is adjusted to 50 ~ 65 DEG C, stirring reaction 2 ~ 3h, after reaction terminates, carry out crystallisation by cooling filtration treatment, Tc is 30 ~ 35 DEG C, makes filtrate circulation crystallization process in cooling crystallizer, the filter cake obtained is primary ammonium phosphate product, detects the component content in filtrate;
2) in filtrate, potassium hydroxide solution and phosphoric acid solution is added, the middle pH value of adjustment filtrate and nitrogen, phosphorus, potassium content, work as filtrate, pH value is 3.5 ~ 4, when the content of nitrogen component is 20-25%, phosphorus composition content is 4-8%, potassium component content is 10-15%, stops adding potassium hydroxide solution and phosphoric acid solution, then add formaldehyde solution in the solution, temperature rises to 50 ~ 65 DEG C, stirring reaction 2.5 ~ 4h;
3) in filtrate, the trace element such as the moderate-element such as calcium, magnesium and borax, zinc sulfate, manganous sulfate, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES is added, stirring reaction 1 ~ 1.5h;
4) by step 3) in the solution that obtains be cooled to 15 ~ 20 DEG C, carry out crystallization treatment, obtain chemical combination state composite fertilizer just finished product, described chemical combination state composite fertilizer just finished product is contained
the potassiumphosphate composite fertilizer of root.
5) first for chemical combination state composite fertilizer finished product is carried out granulation, then dry under the environment of 45 ~ 55 DEG C and make beet special fertilizer.
What phosphoric acid mixed with carboxamide is (1.2-1.5) according to mol ratio: 1.
The described intermediate added and the mol ratio of ammoniacal liquor are 1:(1.2 ~ 1.4).
The concentration of described potassium hydroxide solution is 10 ~ 15%.
The concentration of described phosphoric acid solution is 10 ~ 15%.
Described crystallization treatment is: when the content of the nitrogen component in chemical combination state composite fertilizer just finished product be 18-23%, phosphorus composition content is 3-6%, potassium component content is 8-13% time, stop crystallization.
Described chemical combination state composite fertilizer just finished product is rich in
with
realizing controlled-release fertile, wherein
with
mol ratio be 1:(2 ~ 4).
In the present invention, by carboxamide and phosphoric acid at 80 DEG C, and react be warming up to the environment of 160 DEG C with the speed of 5 DEG C/min under, generate Ureaphil, and along with the progressively rising of temperature, and then make the coordinate bond dialysis between Ureaphil and form two kinds of ion like materials, be namely exactly
with
when
ion is in phosphoric acid environment, will be close with phosphoric acid, and then carries out ionic polymerization under temperature environment when the dialysis of Ureaphil coordinate bond, makes
ion and phosphoric acid generate
intermediate-ion, make containing a large amount of dihydrogen phosphates in solution, when adding ammoniacal liquor, dihydrogen phosphate and potassium ion react and generate primary ammonium phosphate, and in succession reach capacity simultaneously; As precipitation NH
4h
2pO
4after crystal, containing a large amount of in filtrate
root, adds potassium hydroxide solution in filtrate, when potassium content is excessive, will reacts, further make intermediate-ion chelating become with the ammonium radical ion in intermediate-ion
intermediate-ion, and with positive charge, and then when participating in other electronegative ions or compound in solution, compound salt will be formed with this ion, further enriching the nutritive ingredient in product.
Meanwhile, carboxamide is in the acid situation of pH 3.5 ~ 4.0, and carboxamide can react with formaldehyde solution, generates urea aldehyde series product
or
even longer chemical chain,
can continue to react with carboxamide and formaldehyde in acid situation and generate
simultaneously
continue and carboxamide and formaldehyde reaction in acid situation, so control its reaction times at 2.5 ~ 4h, ensure in solution
with
mol ratio be 1:(2 ~ 4),
or
deng urea aldehyde series product after fertilising, under the effect of microorganism, the N, the C element that are easily absorbed by plants can be discharged, the chain length of its urea aldehyde is longer, chain needs the time of fracture longer, the time producing fertilizer efficiency can discharge after a certain time, can reach the effect of slowly-releasing generally
the release fertilizer efficiency time be 0 ~ 40 day,
the release fertilizer efficiency time be 40 ~ 80 days.
Beneficial effect of the present invention is:
Compared with prior art, there is following characteristics in the present invention:
1. in the filtrate of conventional wet lay phosphoric acid primary ammonium phosphate, be rich in carbon amide solution, the solubleness at the same temperature of carboxamide is relatively large, and isolated carboxamide crystal is rich in NH
4h
2pO
4in other crystal, entered in the filtrate after cooling precipitation carboxamide crystal also containing a large amount of carboxamide, H simultaneously
2pO
4 -, HPO
4 2-, PO
4 3-utilize Deng not operatively, the temperature of wet process phosphoric acid for preparing primary ammonium phosphate is adjusted to 80 ~ 160 DEG C by the present invention, and react from the environment of 80 DEG C to 160 DEG C with the intensification of the speed of 5 DEG C/min, the primary ammonium phosphate product purity of precipitation is not only made to reach more than 98%, after adding Strong oxdiative potassium solution in filtrate, also generate in filtrate
positively charged ion, to filtrate crystallisation separate out generate chemical combination state Chemical Mixed Fertilizer go out finished product time, ensure that chemical combination state Chemical Mixed Fertilizer goes out in finished product
intermediate-ion and dihydrogen phosphate, and coordinate bond is formed between C and O, this intermediate-ion can form multielement intermediate-ion with centering element compound chelating, and then the compound electronegative with other can be continued or ion forms inner complex, improve constituent content in double salt, and then the nutrient content that can adjust in the double salt of this ion existence, simultaneously, this inner complex can be hydrolyzed again and by crop, and then fertilizer efficiency can be provided for crop effectively for a long time, simultaneously, in conjunction with the mensuration of constituent content in the solution existed this ion, and then each constituent content during formation of adjustment double salt, dry and obtain chemical combination state double salt composite fertilizer, its specific absorption is fabulous, reduce beet planting cost and improve beet quality,
2. the carboxamide composition containing part in filtrate, adds formaldehyde solution, under acidic conditions and certain pressure intensity and temperature, generates
or
deng urea aldehyde series composite fertilizer, this beet special fertilizer can be made to reach the effect of realizing controlled-release;
3. by the constituent content in beet special fertilizer and beet the effective absorbed dose to n-p-k element carry out detection analyze, and carry out regulating to the constituent content in production process and arrange in pairs or groups, make the composite fertilizer of the chemical combination state prepared can meet the demand of crop to greatest extent, and reduce in composite heat transfer because element mismatch, the high cost caused, further avoid too much element to drop among soil, cause solidifying of composite fertilizer and contaminate environment.
Embodiment
Below in conjunction with specific embodiment, concrete technical scheme of the present invention is described in detail.
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 carboxamide, the ion double salt making Ureaphil form a kind of positive and negative charge to attract mutually, its mechanism structural response following expression: CO (NH
2)
2.H
3pO
4→ (H
2pO
4)
-. (H
2nCONH
3)
+
Further, under the environment that Ureaphil ion double salt exists at phosphoric acid, (H wherein
2nCONH
3)
+positive ion and phosphoric acid close, form the intermediate-ion of C → O coordinate bond, be (CO
5pN
2h
8)
+, and then make in Ureaphil intermediate containing a large amount of (H
2pO
4)
-(CO
5pN
2h
8)
+ion, when adding excessive and appropriate potassium ion, dihydrogen phosphate and potassium ion form ammonium dihydrogen phosphate crystal and are precipitated, unnecessary potassium ion and (CO
5pN
2h
8)
+ionic reaction, and displace part NH
4 +, make in solution containing (CO
5pNH
4k)
+double salt ion, and analyze by detecting and control the content of N in solution, P, K element, the chemical combination state composite fertilizer containing N, P, K element can be obtained at heat drying.
Its concrete reaction principle will carry out further instruction by following reaction structure formula and reaction mechanism:
Reaction formula one:
CO(NH
2)
2+H
3PO
4→CO(NH
2)
2.H
3PO
4
Reaction formula two:
Reaction formula three:
Wherein, the dotted line between carbon atom and Sauerstoffatom represents to there is coordinate bond between C atom and O atom.
When adding ammoniacal liquor, dihydrogen phosphate and potassium ion react and generate primary ammonium phosphate, and in succession reach capacity; As precipitation NH
4h
2pO
4after crystal, containing a large amount of in filtrate
root, adds potassium hydroxide solution in filtrate, when potassium content is excessive, will react with the ammonium radical ion in intermediate-ion.
Reaction formula four:
Wherein, the dotted line between carbon atom and Sauerstoffatom represents to there is coordinate bond between C atom and O atom.
In the present invention, carboxamide and formaldehyde are under being 3.5 ~ 4.0 alkaline case in pH value, and temperature is 50 ~ 65 DEG C can produce following reaction:
Reaction formula five
Reaction formula six
Generate urea aldehyde series product
or
even longer chemical chain,
can continue to react with carboxamide and formaldehyde in acid situation and generate
simultaneously
continue and carboxamide and formaldehyde reaction in acid situation, so control its reaction times at 2.5 ~ 4h, ensure in solution
with
mol ratio be 1:(2 ~ 4),
or
deng urea aldehyde series product after fertilising, under the effect of microorganism, the N, the C element that are easily absorbed by plants can be discharged, the chain length of its urea aldehyde is longer, chain needs the time of fracture longer, the time producing fertilizer efficiency can discharge after a certain time, can reach the effect of slowly-releasing generally
the release fertilizer efficiency time be 0 ~ 40 day,
the release fertilizer efficiency time be 40 ~ 80 days.
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 one
A kind of production method preparing primary ammonium phosphate by-product beet special fertilizer that the present embodiment provides, mainly comprises the following steps:
1) phosphoric acid is adopted to mix with carboxamide, what phosphoric acid mixed with carboxamide is 1.2:1 according to mol ratio, and be that 3 ~ 8 DEG C/min is warming up to 160 DEG C from 80 DEG C with heat-up rate, stirring reaction 4-5h, separation obtains intermediate, again intermediate is added in ammonia soln, described intermediate and the mol ratio of ammoniacal liquor are 1:1.4, temperature is adjusted to 50 ~ 65 DEG C, stirring reaction 2 ~ 3h, after reaction terminates, carry out crystallisation by cooling filtration treatment, Tc is 30 ~ 35 DEG C, make filtrate circulation crystallization process in cooling crystallizer, the filter cake obtained is primary ammonium phosphate product, detect the component content in filtrate,
2) in filtrate, potassium hydroxide solution and phosphoric acid solution is added, the middle pH value of adjustment filtrate and nitrogen, phosphorus, potassium content, the concentration of described potassium hydroxide solution is 10%, the concentration of described phosphoric acid solution is 15%, when filtrate pH value is 3.5 ~ 4, when the content of nitrogen component is 20-25%, phosphorus composition content is 4-8%, potassium component content is 10-15%, stop adding potassium hydroxide solution and phosphoric acid solution, then formaldehyde solution is added in the solution, temperature rises to 50 ~ 65 DEG C, stirring reaction 2.5h;
3) in filtrate, the trace element such as the moderate-element such as calcium, magnesium and borax, zinc sulfate, manganous sulfate, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES is added, stirring reaction 1 ~ 1.5h;
4) by step 3) in the solution that obtains be cooled to 15 ~ 20 DEG C, carry out crystallization treatment, obtain chemical combination state composite fertilizer just finished product, when the content of the nitrogen component in chemical combination state composite fertilizer just finished product be 18%, phosphorus composition content is 6%, potassium component content is 8% time, stop crystallization.
5) first for chemical combination state composite fertilizer finished product is carried out granulation, then dry under the environment of 45 ~ 55 DEG C and make beet special fertilizer.
After testing, the purity of the primary ammonium phosphate made reaches more than 97%, containing containing in the beet special fertilizer made
the potassiumphosphate composite fertilizer of root, and contain
with
realizing controlled-release fertile, wherein
with
mol ratio be 1:2.
Embodiment two
A kind of production method preparing primary ammonium phosphate by-product beet special fertilizer that the present embodiment provides, mainly comprises the following steps:
1) phosphoric acid is adopted to mix with carboxamide, what phosphoric acid mixed with carboxamide is 1.5:1 according to mol ratio, and be that 3 ~ 8 DEG C/min is warming up to 160 DEG C from 80 DEG C with heat-up rate, stirring reaction 4-5h, separation obtains intermediate, again intermediate is added in ammonia soln, described intermediate and the mol ratio of ammoniacal liquor are 1:1.2, temperature is adjusted to 50 ~ 65 DEG C, stirring reaction 2 ~ 3h, after reaction terminates, carry out crystallisation by cooling filtration treatment, Tc is 30 ~ 35 DEG C, make filtrate circulation crystallization process in cooling crystallizer, the filter cake obtained is primary ammonium phosphate product, detect the component content in filtrate,
2) in filtrate, potassium hydroxide solution and phosphoric acid solution is added, the middle pH value of adjustment filtrate and nitrogen, phosphorus, potassium content, the concentration of described potassium hydroxide solution is 15%, the concentration of described phosphoric acid solution is 10%, when filtrate pH value is 3.5 ~ 4, when the content of nitrogen component is 20-25%, phosphorus composition content is 4-8%, potassium component content is 10-15%, stop adding potassium hydroxide solution and phosphoric acid solution, then formaldehyde solution is added in the solution, temperature rises to 50 ~ 65 DEG C, stirring reaction 4h;
3) in filtrate, the trace element such as the moderate-element such as calcium, magnesium and borax, zinc sulfate, manganous sulfate, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES is added, stirring reaction 1 ~ 1.5h;
4) by step 3) in the solution that obtains be cooled to 15 ~ 20 DEG C, carry out crystallization treatment, obtain chemical combination state composite fertilizer just finished product, when the content of the nitrogen component in chemical combination state composite fertilizer just finished product be 23%, phosphorus composition content is 3%, potassium component content is 13% time, stop crystallization.
5) first for chemical combination state composite fertilizer finished product is carried out granulation, then dry under the environment of 45 ~ 55 DEG C and make beet special fertilizer.
After testing, the purity of the primary ammonium phosphate made reaches more than 97%, containing containing in the beet special fertilizer made
the potassiumphosphate composite fertilizer of root, and contain
with
realizing controlled-release fertile, wherein
with
mol ratio be 1:3.
Embodiment three
A kind of production method preparing primary ammonium phosphate by-product beet special fertilizer that the present embodiment provides, mainly comprises the following steps:
1) phosphoric acid is adopted to mix with carboxamide, what phosphoric acid mixed with carboxamide is 1.4:1 according to mol ratio, and be that 3 ~ 8 DEG C/min is warming up to 160 DEG C from 80 DEG C with heat-up rate, stirring reaction 4-5h, separation obtains intermediate, again intermediate is added in ammonia soln, described intermediate and the mol ratio of ammoniacal liquor are 1:1.3, temperature is adjusted to 50 ~ 65 DEG C, stirring reaction 2 ~ 3h, after reaction terminates, carry out crystallisation by cooling filtration treatment, Tc is 30 ~ 35 DEG C, make filtrate circulation crystallization process in cooling crystallizer, the filter cake obtained is primary ammonium phosphate product, detect the component content in filtrate,
2) in filtrate, potassium hydroxide solution and phosphoric acid solution is added, the middle pH value of adjustment filtrate and nitrogen, phosphorus, potassium content, the concentration of described potassium hydroxide solution is 13%, the concentration of described phosphoric acid solution is 12%, when filtrate pH value is 3.5 ~ 4, when the content of nitrogen component is 20-25%, phosphorus composition content is 4-8%, potassium component content is 10-15%, stop adding potassium hydroxide solution and phosphoric acid solution, then formaldehyde solution is added in the solution, temperature rises to 50 ~ 65 DEG C, stirring reaction 3h;
3) in filtrate, the trace element such as the moderate-element such as calcium, magnesium and borax, zinc sulfate, manganous sulfate, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES is added, stirring reaction 1 ~ 1.5h;
4) by step 3) in the solution that obtains be cooled to 15 ~ 20 DEG C, carry out crystallization treatment, obtain chemical combination state composite fertilizer just finished product, when the content of the nitrogen component in chemical combination state composite fertilizer just finished product be 21%, phosphorus composition content is 5%, potassium component content is 11% time, stop crystallization.
5) first for chemical combination state composite fertilizer finished product is carried out granulation, then dry under the environment of 45 ~ 55 DEG C and make beet special fertilizer.
After testing, the purity of the primary ammonium phosphate made reaches more than 97%, containing containing in the beet special fertilizer made
the potassiumphosphate composite fertilizer of root, and contain
with
realizing controlled-release fertile, wherein
with
mol ratio be 1:4.
In order to prove the beneficial effect that the present invention reaches better, the present embodiment also provides following experimental example, specific as follows:
Experimental example one
Fertile in fertilizer with common N, P, K mixing, wherein the content of nitrogen component is 21%, phosphorus composition content is 5%, potassium component content is 11%, make nutrient solution, soilless culture is carried out to beet, cultivate after 30 days, detect the content of N, P, K composition in nutrient solution, observe its growing way, called after A1 simultaneously.
Experimental example two is to experimental example four
The beet special fertilizer be successful to embodiment tripartite method with embodiment one, as fertilizer, is made nutrient solution, is carried out soilless culture to beet, cultivate after 15 days, 30 days, 50 days, detect the content of N, P, K composition in nutrient solution respectively, observe its growing way simultaneously, respectively called after A2, A3, A4.
The concentration of the nutrient solution in above experimental example is suitable for, and be prior art, this experimental example seldom elaborates, above experimental example with 20 strain beets for detected result is as table 1, table 2 and table 3:
Table 1: the content cultivating N, P, K composition after 15 days
Table 2: the content cultivating N, P, K composition after 30 days
Table 3: the content cultivating N, P, K composition after 50 days
As can be seen from table 1 ~ 3, compared with the beet special fertilizer produced with common composite fertilizer and the present invention, when cultivating detection in the 15th day, its N, P, the absorbing state difference of K is little, but when detecting by the 30th day, N in the beet special fertilizer solution that the present invention produces, P, the content of K is starkly lower than common special fertilizer, when detecting by the 50th day, N in common composite fertilizer's nutrient solution, P, K component residue has 60 ~ 80% not absorb, and the N in the nutrient solution of the beet special fertilizer that the present invention produces, P, K composition only remains 30 ~ 40% and is not absorbed, illustrate that the beet special fertilizer that the present invention produces has the good feature of specific absorption.
Claims (7)
1. prepare a production method for primary ammonium phosphate by-product beet special fertilizer, mainly comprise the following steps:
1) adopt phosphoric acid to mix with carboxamide, and be that 3 ~ 8 DEG C/min is warming up to 160 DEG C from 80 DEG C with heat-up rate, stirring reaction 4-5h, separation obtains intermediate, add in ammonia soln by intermediate again, temperature is adjusted to 50 ~ 65 DEG C, stirring reaction 2 ~ 3h, after reaction terminates, carry out crystallisation by cooling filtration treatment, Tc is 30 ~ 35 DEG C, makes filtrate circulation crystallization process in cooling crystallizer, the filter cake obtained is primary ammonium phosphate product, detects the component content in filtrate;
2) in filtrate, potassium hydroxide solution and phosphoric acid solution is added, the middle pH value of adjustment filtrate and nitrogen, phosphorus, potassium content, work as filtrate, pH value is 3.5 ~ 4, when the content of nitrogen component is 20-25%, phosphorus composition content is 4-8%, potassium component content is 10-15%, stops adding potassium hydroxide solution and phosphoric acid solution, then add formaldehyde solution in the solution, temperature rises to 50 ~ 65 DEG C, stirring reaction 2.5 ~ 4h;
3) in filtrate, the trace element such as the moderate-element such as calcium, magnesium and borax, zinc sulfate, manganous sulfate, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES is added, stirring reaction 1 ~ 1.5h;
4) by step 3) in the solution that obtains be cooled to 15 ~ 20 DEG C, carry out crystallization treatment, obtain chemical combination state composite fertilizer just finished product, described chemical combination state composite fertilizer just finished product is contained
the potassiumphosphate composite fertilizer of root.
5) first for chemical combination state composite fertilizer finished product is carried out granulation, then dry under the environment of 45 ~ 55 DEG C and make beet special fertilizer.
2. a kind of production method preparing primary ammonium phosphate by-product beet special fertilizer as claimed in claim 1, is characterized in that: what phosphoric acid mixed with carboxamide is (1.2-1.5) according to mol ratio: 1.
3. a kind of production method preparing primary ammonium phosphate by-product beet special fertilizer as claimed in claim 1, is characterized in that: the described intermediate added and the mol ratio of ammoniacal liquor are 1:(1.2 ~ 1.4).
4. a kind of production method preparing primary ammonium phosphate by-product beet special fertilizer as claimed in claim 1, is characterized in that: the concentration of described potassium hydroxide solution is 10 ~ 15%.
5. a kind of production method preparing primary ammonium phosphate by-product beet special fertilizer as claimed in claim 1, is characterized in that: the concentration of described phosphoric acid solution is 10 ~ 15%.
6. a kind of production method preparing primary ammonium phosphate by-product beet special fertilizer as claimed in claim 1, it is characterized in that: described crystallization treatment is: when the content of the nitrogen component in chemical combination state composite fertilizer just finished product be 18-23%, phosphorus composition content is 3-6%, potassium component content is 8-13% time, stop crystallization.
7. a kind of production method preparing primary ammonium phosphate by-product beet special fertilizer as claimed in claim 6, is characterized in that: described chemical combination state composite fertilizer just finished product is rich in
with
realizing controlled-release fertile, wherein
with
mol ratio be 1:(2 ~ 4).
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