CN104291291A - Production method for preparing ammonium dihydrogen phosphate byproduct special fertilizer for pumpkin - Google Patents

Production method for preparing ammonium dihydrogen phosphate byproduct special fertilizer for pumpkin Download PDF

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Publication number
CN104291291A
CN104291291A CN201410479138.4A CN201410479138A CN104291291A CN 104291291 A CN104291291 A CN 104291291A CN 201410479138 A CN201410479138 A CN 201410479138A CN 104291291 A CN104291291 A CN 104291291A
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China
Prior art keywords
pumpkin
solution
fertilizer
phosphoric acid
special fertilizer
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CN201410479138.4A
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Chinese (zh)
Inventor
陈肖虎
廖吉星
何敏
朱飞武
王丽远
彭宝林
赵伟毅
郑超
曾舒
黄芳
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Guizhou University
Guizhou Kexin Chemical and Metallurgical Co Ltd
Guiyang Sinochem Kailin Fertilizer Co Ltd
Original Assignee
Guizhou University
Guizhou Kexin Chemical and Metallurgical Co Ltd
Guiyang Sinochem Kailin Fertilizer Co Ltd
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Priority to CN201410479138.4A priority Critical patent/CN104291291A/en
Publication of CN104291291A publication Critical patent/CN104291291A/en
Pending legal-status Critical Current

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Abstract

The invention relates to the technical field of chemical engineering and particularly relates to a production method for preparing an ammonium dihydrogen phosphate byproduct special fertilizer for pumpkin. By changing factors such as temperature for preparation of ammonium dihydrogen phosphate from phosphoric acid through a wet method, the purity of the ammonium dihydrogen phosphate product is improved and meanwhile, a compound fertilizer containing N, P and K compound states can be produced, the purity of ammonium dihydrogen phosphate can be improved, the absorption rate of the produced special fertilizer for pumpkin is good, a controlled-release compound fertilizer is produced by virtue of adding formaldehyde in the filtrate, the produced special fertilizer for pumpkin can meet the nutritional needs of various periods in a growth period and thus the yield of pumpkin is greatly increased and the special fertilizer for pumpkin is an effective compound fertilizer.

Description

A kind of production method preparing primary ammonium phosphate by-product pumpkin special fertilizer
Technical field
The present invention relates to chemical technology field, particularly relate to a kind of production method preparing primary ammonium phosphate by-product pumpkin special fertilizer.
Background technology
Pumpkin pumpkin is the plant of Curcurbitaceae Cucurbita.Because the place of production is different, call is different.Have another name called wheat melon, pumpkin, pumpkin, golden wax gourd, Formosan is called golden melon, originates in Central and South America.Pumpkin has plantation all over China, and Japan is then large with Hokkaido.Tender fruity is sweet agreeable to the taste, is one of melon dish of summer and autumn.Capable of using as feed or the coarse cereals of old melon, so there is a lot of place to be also called meal melon.Be commonly used to make pumpkin pie at west pumpkin, i.e. the sweet cake of pumpkin.Pumpkin melon seeds can be cooked snacks.Pumpkin is annual draft of overgrowing, and spring is sowed, and the florescence, the fruit phase was in 7 ~ September in 5 ~ July.In order to ensure the output mistake of pumpkin, usually use the chemical mixing of N, P, K fertile used in combination with fertilizer, the preparation method (CN201310715418.6) of hut mulching plant fertilizer in pumpkin as a kind of in patent of invention, its raw material comprises fertilizer, composite fertilizer, potash fertilizer, plant ash, ground phosphate rock, carboxamide, the human and animal excreta become thoroughly decomposed, trace element, oyster shell whiting, diatomite, a kind of short material (CN201310715481.X) that fleshes up of planting for pumpkin greenhouse of patent of invention, its raw material is seaweed powder, growth hormone, xanthohumic acid, soil ulmin, ground phosphate rock, saltpetre, the pig manure become thoroughly decomposed, trace element, blood meal and lime powder, the shortcoming using chemical mixing fertilizer is N, P, the absorptivity of K element is bad, it is reported, carboxamide, the plant absorption utilization ratio of carbon ammonium is: 20% one 46%, phosphate fertilizer (two ammoniums, one ammonium, coarse whiting) plant absorption utilization ratio be: 10% one 25%, the plant absorption utilization ratio of common potash fertilizer is: 35% one 60%, life-time service can make soil aggregate be destroyed, easily cause soil compaction, soil property is hardening, thus affect the growth of farm crop, the decline of quality, cause vicious cycle.Though simultaneously fertilizer is rich in organic matter, nutrients release is slow, cause farm crop absorb slow, fertilizer efficiency is low, active balance is not reached between various available nutrient, due to the fertilizer formula not science of farm crop, cause the output of farm crop not high, quality also can not get improving.
Primary ammonium phosphate, is widely used in the crop of the almost all types such as all types of cash crop, grain, melon and fruit, vegetables, has remarkable increasing both production and income, the amount of changing optimizes many excellent effects such as quality.Current domestic a lot of fertilizer producer is all at production biphosphate ammonium compound fertilizer, it mainly comprises thermal phosphoric acid and phosphoric acid by wet process produces primary ammonium phosphate, and thermal phosphoric acid cost is larger, unsuitable as extensively promoting, therefore, Wet-process Phosphoric Acid Production primary ammonium phosphate product becomes main method, and the basic step of wet process phosphoric acid for preparing primary ammonium phosphate is as follows:
Reaction formula one:
CO(NH 2) 2+H 3PO 4＝CO(NH 2) 2.H 3PO 4
Reaction formula two
CO(NH 2) 2.H 3PO 4+NH 3＝NH 4·H 2PO 4+CO(NH 2) 2
After whole reaction terminates, for there is any change in carboxamide, simultaneously because carboxamide solubleness is very high, 20 DEG C time, its solubleness is 85g/100ml (refer to " phosphate fertilizer and composite fertilizer " the 20th volume the 6th phase---solubility of chemical fertilizer and Compound fertilizer production technology), simultaneously the solubility with temperature of carboxamide rising and increase, so the carboxamide contained in filtrate is after separating out by cooling crystal, also containing a large amount of undecomposed carboxamide, NH in filtrate 4 +, H 2pO 4 ~, HPO 4 2 ~, PO 4 3 ~if directly do waste water and discharge, both wasted resource, and can cause again the waste of resource, the dipotassium hydrogen phosphate product purity made is not high simultaneously.
For in Wet-process Phosphoric Acid Production primary ammonium phosphate process, the purity of primary ammonium phosphate is not high, also containing a large amount of undecomposed carboxamide, NH in filtrate 4 +, H 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 pumpkin special fertilizer and the absorbing state of pumpkin are studied, effectively inquire into out and produce pumpkin special fertilizer from the filtrate of Wet-process Phosphoric Acid Production primary ammonium phosphate, solve the problems such as effective constituent cannot utilize in the filtrate of Wet-process Phosphoric Acid Production primary ammonium phosphate, at home in fertiliser production, have no report.
For in Wet-process Phosphoric Acid 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 pumpkin special fertilizer and the absorbing state of pumpkin are studied, effectively inquire into out and produce pumpkin special fertilizer from the filtrate of Wet-process Phosphoric Acid Production primary ammonium phosphate, solve the problems such as effective constituent cannot utilize in the filtrate of Wet-process Phosphoric Acid Production primary ammonium phosphate, at home in fertiliser production, have no report.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of production method preparing primary ammonium phosphate by-product pumpkin special fertilizer, by the process production design of uniqueness, improve the purity of primary ammonium phosphate, make full use of carboxamide, H in the filtrate of wet process phosphoric acid for preparing primary ammonium phosphate simultaneously 2pO 4 ~, HPO 4 2 ~, PO 4 3 ~deng material, produce out the pumpkin special fertilizer of applicable pumpkin grows.
The present invention is achieved by the following technical programs.
A kind of production method preparing primary ammonium phosphate by-product pumpkin special fertilizer provided by the invention, is characterized in that comprising following steps:
(1) phosphoric acid adopting phosphoric acid by wet process obtained is (1.1 ~ 1.6) with carboxamide according to mol ratio: 1 mixes, and is that 5 ~ 8 DEG C/min is warming up to 160 DEG C from 90 DEG C with heat-up rate, stirring reaction 4 ~ 5h, and separation obtains intermediate;
(2) then intermediate is dissolved in phosphoric acid solution, the pH of regulator solution, 3 ~ 3.5, passes into ammonia in solution, and ammonia and intermediate are (1.1 ~ 1.4) according to mol ratio: 1, stirring reaction 2 ~ 3h, after reaction terminates, the slip of acquisition, and slip is placed in cooling crystallizer and cools to 25 ~ 30 DEG C, carry out crystallization filtration treatment, make filtrate circulation crystallization process in cooling crystallizer, the filter cake of acquisition is primary ammonium phosphate product, detects the component content in filtrate;
(3) at filtrate hydro-oxidation potassium and phosphoric acid solution, when the pH of solution is 3.3 ~ 4.0, when nitrogen component content is 16 ~ 25%, phosphorus composition content is 5 ~ 12%, potassium component content is 12 ~ 17%, formaldehyde solution is added in filtrate, temperature is risen to 65 ~ 75 DEG C,, pressure is increased to 3 ~ 4 normal atmosphere, stirring reaction 20 ~ 40min;
(4) and then in solution trace element is added, be cooled to 20 ~ 25 DEG C, separate out the Chemical Mixed Fertilizer crude product of chemical combination state, when in Chemical Mixed Fertilizer crude product chemical combination state being detected N, P, K component content non-be not 18 ~ 22%, 4 ~ 8%, 11 ~ 14% time, stop crystallization;
(5) the chemical combination state Chemical Mixed Fertilizer crude product that step (4) is separated out makes pumpkin special fertilizer through granulation and oven dry.
The concentration of described potassium hydroxide solution is 30 ~ 35%.
The concentration of described step (2) and the phosphoric acid solution of step (3) is 17 ~ 20%.
The concentration of described formaldehyde solution is 30 ~ 35%, and the mol ratio of the carboxamide contained in formaldehyde and solution is (0.5 ~ 1.5): 4.
Described trace element is Fe 2 +inner complex, H 3bO 3in one or more mixtures.
The Chemical Mixed Fertilizer of described chemical combination state contains in its composition and contains following N P and K chemical combination state structural formula: wherein, the dotted line between carbon atom and Sauerstoffatom represents to there is coordinate bond between C atom and O atom, and contains with realizing controlled-release fertile.
In the present invention, by carboxamide and phosphoric acid at 90 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, makes in solution containing a large amount of dihydrogen phosphates simultaneously; When adding potassium ion compound, dihydrogen phosphate and potassium ion react and generate primary ammonium phosphate, and in succession reach capacity; When potassium content is excessive, will reacts with the ammonium radical ion in intermediate-ion, further make intermediate-ion chelating become intermediate-ion, and with positive charge, and then when participating in other electronegative ions or compound in solution, compound salt will be formed with this ion, further enriching the nutritive ingredient in product.
Meanwhile, 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 continuing and carboxamide and formaldehyde reaction in acid situation, in the present invention, improving speed of response by increasing pressure. 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, and the present invention exists following characteristics:
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 KH 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 90 ~ 160 DEG C by the present invention, and react from the environment of 90 DEG C to 160 DEG C with the intensification of the speed of 5 ~ 8 DEG C/min, not only make the primary ammonium phosphate product purity of precipitation reach more than 98%, 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, and by avoiding adding of chlorine element, while making the quality product of chemical combination state double salt composite fertilizer can meet the requirement of pumpkin nutrient composition, avoid the infringement that fertilizer brings pumpkin, reduce pumpkin planting cost and improve pumpkin output,
2. the carboxamide composition containing part in filtrate, adds formaldehyde solution, under acidic conditions and certain pressure intensity and temperature, generates with deng urea aldehyde series composite fertilizer, this pumpkin special fertilizer can be made to reach the effect of realizing controlled-release;
3. by the constituent content in pumpkin special fertilizer and pumpkin 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)-and (CO 5pN 2h 8) +ion, when adding ammonia in solution, ammonia can generate NH with acid-respons 4 +, by decrease temperature crystalline, generate NH4H 2pO 4, when adding excessive and appropriate potassium ion in filtrate, 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, can produce and react:
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 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
The present embodiment provides a kind of production method preparing primary ammonium phosphate by-product pumpkin special fertilizer, comprises following steps:
(1) phosphoric acid solution adopting phosphoric acid by wet process obtained is that 1.1:1 mixes with carboxamide according to mol ratio, and is that 5min is warming up to 160 DEG C from 90 DEG C with heat-up rate, stirring reaction 5h, and separation obtains intermediate;
(2) be then dissolved in phosphoric acid solution by intermediate, the concentration of this phosphoric acid solution is 17%, and the pH of regulator solution is 3, ammonia is passed into again in solution, ammonia and intermediate are 1.1:1 according to mol ratio, stirring reaction 3h, after reaction terminates, the slip obtained, and slip is placed in cooling crystallizer and cools to 25 DEG C, carry out crystallization filtration treatment, make filtrate circulation crystallization process in cooling crystallizer, the filter cake obtained is primary ammonium phosphate product, detects the component content in filtrate;
(3) at filtrate hydro-oxidation potassium and phosphoric acid, concentration is respectively 30%, 17%, when the pH of solution is 4.0, when nitrogen component content is 16%, phosphorus composition content is 5%, potassium component content is 12%, in filtrate, add formaldehyde solution, concentration is 30%, and the mol ratio of the carboxamide contained in formaldehyde and solution is 0.5:4, temperature is risen to 75 DEG C, pressure is increased to 4 normal atmosphere, stirring reaction 20min;
And then Fe is added in solution 2 +inner complex, H 3bO 3deng trace element, be cooled to 20 DEG C, separate out the Chemical Mixed Fertilizer crude product of chemical combination state, make pumpkin special fertilizer through granulation and oven dry.
After testing, the purity of the biphosphate ammonium product using the method to make is more than 98%, and N, P, K component content of the pumpkin special fertilizer made is non-is not 18%, 4%, 11%.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, and contains with realizing controlled-release fertile.
Embodiment two
The present embodiment provides a kind of production method preparing primary ammonium phosphate by-product pumpkin special fertilizer, comprises following steps:
(1) phosphoric acid solution adopting phosphoric acid by wet process obtained is that 1.6:1 mixes with carboxamide according to mol ratio, and is that 8 DEG C/min is warming up to 160 DEG C from 90 DEG C with heat-up rate, stirring reaction 4h, and separation obtains intermediate;
(2) be then dissolved in phosphoric acid solution by intermediate, the concentration of this phosphoric acid solution is 20%, and the pH of regulator solution is 3.5, ammonia is passed into again in solution, ammonia and intermediate are 1.4:1 according to mol ratio, stirring reaction 2h, after reaction terminates, the slip obtained, and slip is placed in cooling crystallizer and cools to 30 DEG C, carry out crystallization filtration treatment, make filtrate circulation crystallization process in cooling crystallizer, the filter cake obtained is primary ammonium phosphate product, detects the component content in filtrate;
(3) at filtrate hydro-oxidation potassium and phosphoric acid, concentration is respectively 35%, 20%, when the pH of solution is 3.3, when nitrogen component content is 25%, phosphorus composition content is 12%, potassium component content is 17%, in filtrate, add formaldehyde solution, concentration is 35%, and the mol ratio of the carboxamide contained in formaldehyde and solution is 1.5:4, temperature is risen to 65 DEG C, pressure is increased to 3 normal atmosphere, stirring reaction 40min;
And then Fe is added in solution 2 +inner complex, H 3bO 3deng trace element, be cooled to 20 ~ 25 DEG C, separate out the Chemical Mixed Fertilizer crude product of chemical combination state, make pumpkin special fertilizer through granulation and oven dry.
After testing, the purity of the biphosphate ammonium product using the method to make is more than 98%, and N, P, K component content of the pumpkin special fertilizer made is non-is not 22%, 8%, 14%.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, and contains with realizing controlled-release fertile.
Embodiment three
The present embodiment provides a kind of production method preparing primary ammonium phosphate by-product pumpkin special fertilizer, comprises following steps:
(1) phosphoric acid solution adopting phosphoric acid by wet process obtained is that 1.4:1 mixes with carboxamide according to mol ratio, and is that 7 DEG C/min is warming up to 160 DEG C from 90 DEG C with heat-up rate, stirring reaction 4.5h, and separation obtains intermediate;
(2) be then dissolved in phosphoric acid solution by intermediate, the concentration of this phosphoric acid solution is 19%, and the pH of regulator solution is 3.2, ammonia is passed into again in solution, ammonia and intermediate are 1.25:1 according to mol ratio, stirring reaction 2.5h, after reaction terminates, the slip obtained, and slip is placed in cooling crystallizer and cools to 27 DEG C, carry out crystallization filtration treatment, make filtrate circulation crystallization process in cooling crystallizer, the filter cake obtained is primary ammonium phosphate product, detects the component content in filtrate;
(3) at filtrate hydro-oxidation potassium and phosphoric acid, concentration is respectively 32%, 18%, when the pH of solution is 3.7, when nitrogen component content is 22%, phosphorus composition content is 7%, potassium component content is 15%, in filtrate, add formaldehyde solution, concentration is 38%, and the mol ratio of the carboxamide contained in formaldehyde and solution is 1:4, temperature is risen to 70 DEG C, pressure is increased to 3.5 normal atmosphere, stirring reaction 30min;
And then Fe is added in solution 2 +inner complex, H 3bO 3deng trace element, be cooled to 20 ~ 25 DEG C, separate out the Chemical Mixed Fertilizer crude product of chemical combination state, make pumpkin special fertilizer through granulation and oven dry.
After testing, the purity of the biphosphate ammonium product using the method to make is more than 98%, and N, P, K component content of the pumpkin special fertilizer made is non-is not 20%, 6%, 12.5%.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, and contains with realizing controlled-release fertile.
In order to well prove the beneficial effect of patent of the present invention, the present invention also provides following experimental example:
Experimental group 1 ~ 3
Using above-described embodiment make pumpkin special fertilizer as fertilizer respectively the direct pumpkin to result apply fertilizer, with make nutrient solution pumpkin seedling cultivated, the output of statistics pumpkin, after Solution culture method 30, detect N, P, K component content wherein, and the growing way situation of pumpkin seedling.
Control group 1 ~ 3
Fertile in fertilizer using common N, P, K mixing, N, P, K component content wherein in this mixing fertilizer is identical to N, P, K component content in embodiment three respectively at embodiment one, the direct pumpkin to result applies fertilizer respectively, with make nutrient solution pumpkin seedling cultivated, the output of statistics pumpkin, after Solution culture method 30, detect N, P, K component content wherein, and the growing way situation of pumpkin seedling.
By being the contrast of experimental group and control group, high 600 ~ 800kg/ the mu of output of the yield increased group of experimental group, in seedling is cultivated, seedling length 20 ~ the 30cm higher than control group of experimental group, N, P, K residual condition in the nutritive medium simultaneously in experimental group is 67%, 56%, 44% of control group respectively.

Claims (6)

1. prepare a production method for primary ammonium phosphate by-product pumpkin special fertilizer, it is characterized in that comprising following steps:
(1) phosphoric acid adopting phosphoric acid by wet process obtained is (1.1 ~ 1.6) with carboxamide according to mol ratio: 1 mixes, and is that 5 ~ 8 DEG C/min is warming up to 160 DEG C from 90 DEG C with heat-up rate, stirring reaction 4 ~ 5h, and separation obtains intermediate;
(2) then intermediate is dissolved in phosphoric acid solution, the pH of regulator solution, 3 ~ 3.5, passes into ammonia in solution, and ammonia and intermediate are (1.1 ~ 1.4) according to mol ratio: 1, stirring reaction 2 ~ 3h, after reaction terminates, the slip of acquisition, and slip is placed in cooling crystallizer and cools to 25 ~ 30 DEG C, carry out crystallization filtration treatment, make filtrate circulation crystallization process in cooling crystallizer, the filter cake of acquisition is primary ammonium phosphate product, detects the component content in filtrate;
(3) at filtrate hydro-oxidation potassium and phosphoric acid solution, when the pH of solution is 3.3 ~ 4.0, when nitrogen component content is 16 ~ 25%, phosphorus composition content is 5 ~ 12%, potassium component content is 12 ~ 17%, formaldehyde solution is added in filtrate, temperature is risen to 65 ~ 75 DEG C, pressure is increased to 3 ~ 4 normal atmosphere, stirring reaction 20 ~ 40min;
(4) and then in solution trace element is added, be cooled to 20 ~ 25 DEG C, separate out the Chemical Mixed Fertilizer crude product of chemical combination state, when in Chemical Mixed Fertilizer crude product chemical combination state being detected N, P, K component content non-be not 18 ~ 22%, 4 ~ 8%, 11 ~ 14% time, stop crystallization;
(5) the chemical combination state Chemical Mixed Fertilizer crude product that step (4) is separated out makes pumpkin special fertilizer through granulation and oven dry.
2. prepare the production method of primary ammonium phosphate by-product pumpkin special fertilizer as claimed in claim 1, it is characterized in that: the concentration of described potassium hydroxide solution is 30 ~ 35%.
3. prepare the production method of primary ammonium phosphate by-product pumpkin special fertilizer as claimed in claim 1, it is characterized in that: the concentration of described step (2) and the phosphoric acid solution of step (3) is 17 ~ 20%.
4. prepare the production method of primary ammonium phosphate by-product pumpkin special fertilizer as claimed in claim 1, it is characterized in that: the concentration of described formaldehyde solution is 30 ~ 35%, and the mol ratio of the carboxamide contained in formaldehyde and solution is (0.5 ~ 1.5): 4.
5. prepare the production method of primary ammonium phosphate by-product pumpkin special fertilizer as claimed in claim 1, it is characterized in that: described trace element is Fe 2 +inner complex, H 3bO 3in one or more mixtures.
6. prepare the production method of primary ammonium phosphate by-product pumpkin special fertilizer as claimed in claim 1, it is characterized in that: the Chemical Mixed Fertilizer of described chemical combination state contains in its composition and contains following N P and K chemical combination state structural formula: wherein, the dotted line between carbon atom and Sauerstoffatom represents to there is coordinate bond between C atom and O atom, and contains with realizing controlled-release fertile.
CN201410479138.4A 2014-09-19 2014-09-19 Production method for preparing ammonium dihydrogen phosphate byproduct special fertilizer for pumpkin Pending CN104291291A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1343186A (en) * 1999-03-18 2002-04-03 Oms投资公司 Processes for preparing granular composite fertilizer compositions and products produced thereby
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

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1343186A (en) * 1999-03-18 2002-04-03 Oms投资公司 Processes for preparing granular composite fertilizer compositions and products produced thereby
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

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