CN104016322A - Production method for diammonium hydrogen phosphate - Google Patents

Production method for diammonium hydrogen phosphate Download PDF

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Publication number
CN104016322A
CN104016322A CN201410213341.7A CN201410213341A CN104016322A CN 104016322 A CN104016322 A CN 104016322A CN 201410213341 A CN201410213341 A CN 201410213341A CN 104016322 A CN104016322 A CN 104016322A
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ammonium phosphate
secondary ammonium
production method
ureaphil
ammonia
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Inventor
彭宝林
廖吉星
朱飞武
韩朝应
郑超
周宾
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Guiyang Sinochem Kailin Fertilizer Co Ltd
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Guiyang Sinochem Kailin Fertilizer Co Ltd
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Abstract

The invention relates to the technical field of chemical engineering, and particularly relates to a production method for diammonium hydrogen phosphate. A diammonium hydrogen phosphate product is prepared by subjecting a high pure urea phosphate solution and ammonia to a double decomposition reaction, reacting for 20-60 min under stirring and at a temperature of 50-80 DEG C by controlling a pH value at 7.8-8.2. Physical and chemical indexes of the diammonium hydrogen phosphate product are as follows: the total nutrient content of diammonium hydrogen phosphate is higher than 74%; the content of total nitrogen is 21.02-21.20%; the content of phosphorus pentoxide is 53.0-53.52%; moisture content is 0.25-0.32%; the content of water insoluble substances is 0.087-0.096%; and the content of fluoride is 0.1-0.14%. The diammonium hydrogen phosphate product fully meets an industrial first level product standard.

Description

A kind of production method of Secondary ammonium phosphate
Technical field
The present invention relates to chemical technology field, especially a kind of production method of Secondary ammonium phosphate.
Background technology
Along with the progress of human society, industrial or agricultural has obtained the development of advancing by leaps and bounds, and safety and environmental consciousness are further improved, and PHOSPHORIC ACID TECH.GRADE hydrogen two ammoniums all have a wide range of applications at aspects such as fire-fighting, drip irrigation fertilizer, medicine and food.At present, the production of PHOSPHORIC ACID TECH.GRADE two ammoniums generally adopts thermal phosphoric acid or purifying phosphoric acid technique; With thermal phosphoric acid, produce power consumption greatly, cost is high, pollutes heavy; The foreign matter content of the diammonium phosphate product that traditional phosphoric acid by wet process ammoniation process is produced is higher, cannot use as industrial goods, and the purification process route of phosphoric acid by wet process is long, and plant construction investment is large, and cost is high; And no matter be wet phosphoric acid or thermal phosphoric acid method, all exist energy consumption large, the problem that cost is high.
As the patent No. preparation method > > that is 201210402974.3 < < acid slime co-producing diammonium phosphates the dilute phosphoric acid that to disclose to concentration be 22.0-24.0% passes into ammonia, again dilute phosphoric acid is once sent into outside circulation vaporizer, two effect interchanger and an effect interchanger, made acid slime; The strong phosphoric acid that is 35-40% to concentration passes into ammonia, makes the strong phosphoric acid that degree of neutralization is 0.4-0.7; By acid slime and strong phosphoric acid by volume for the ratio of 1:3-5 is sent into sour pump after dissolving, make phosphoric acid material pulp mixing solutions and send into again neutralizing well, in neutralizing well, send into ammonia simultaneously, carry out ammoniation-granulation reaction, in making and slip, then will in and slip send into tablets press and carry out ammoniation and granulation technique, make diammonium phosphate particle, finally this diammonium phosphate particle is carried out to drying and dehydrating, gradation sizing obtains diammonium phosphate particle; Visible, this method adopts strong phosphoric acid, and for having relatively high expectations of equipment material, operational path is long, and production cost is high.
And for example the patent No. is that the preparation method > > of a 200910244335.7 < < diammonium phosphate discloses reaction raw materials phosphoric acid (40-60%H 3pO 4) and reaction raw materials ammonia (70-90%NH 3) add in tubular reactor and carry out neutralization reaction, generate phosphor ammonium slurry; Again phosphor ammonium slurry is sprayed into tablets press, then pass into wherein ammonia, the degree of neutralization of adjusting phosphor ammonium slurry is 1.7-1.9, and carries out granulation in ammonification, generates wet solid material and tail gas generated by granulation; Be dried again, to diammonium phosphate product; Visible, the raw material ammonia amount that this method adopts is larger, and the technological process of production is long, and the concentration of its phosphoric acid is larger, and the material of equipment is had relatively high expectations, and citric acid soluble phosphorus hydrochlorate growing amount is larger, and phosphoric utilization ratio is lower, and has waste discharge, is unfavorable for environmental protection, and production cost is large.
Visible, in prior art, longer for the technological process of production of Secondary ammonium phosphate product, energy consumption is large, and raw material availability is low, to having relatively high expectations of equipment material, can produce large quantity of exhaust gas, refuse; The demand of raw material ammonia is larger, is unfavorable for environmental protection, and production cost is larger.
Summary of the invention
In order to solve the above-mentioned technical problem existing in prior art, the invention provides a kind of method of directly utilizing production of urea phosphate PHOSPHORIC ACID TECH.GRADE hydrogen two ammoniums, the method has that operational path is short, energy consumption is low, constant product quality, raw material availability is high, by product can recycling, and cleanliness without any pollution in whole production process, without features such as " waste gas ", " waste water ", " waste residue " discharges.
Specifically be achieved by the following technical programs:
A production method for Secondary ammonium phosphate, adopts highly purified Ureaphil solution and ammonia generation replacement(metathesis)reaction, and to control pH value be 7.8-8.2, and temperature is at 50-80 ℃, and stirring reaction 20-60min prepares Secondary ammonium phosphate product.
Specifically comprise the following steps:
(1) preparation of Ureaphil solution: the Ureaphil solid that is >=97% by purity is sent in dissolving tank, adds water metering, is heated to 40-60 ℃, under agitation condition, according to stirring velocity, be that 60-80r/min stirs, after mixing, be mixed with saturated Ureaphil solution, stand-by;
(2) Secondary ammonium phosphate is synthetic: by step 1) in the saturated Ureaphil solution for preparing adopt transferpump to be transported in synthetic groove, and pass into wherein ammonia, the mol ratio of ammonia and saturated Ureaphil is (2-2.5): 1, and to control temperature be 50-80 ℃, when adjustment pH value is 7.8-8.2, according to stirring velocity, be 60-80r/min, stirring reaction 20-60min, obtains Secondary ammonium phosphate slip;
(3) Secondary ammonium phosphate slip Crystallization Separation: by step 2) obtaining adopts transferpump to proceed to crystallisation by cooling in cooling crystallizer, be cooled to≤40 ℃, Secondary ammonium phosphate crystal is proceeded to separating centrifuge separation, obtain filtrate and filter cake, filtrate is that urea slip proceeds to production of urea phosphate technique; Filter cake is Secondary ammonium phosphate product, proceeds in drying machine and is dried, and packing, obtains and meet an industrial grade Secondary ammonium phosphate product.
Described pH value is 8.
Described ammonia and the mol ratio of saturated Ureaphil are (2-2.3): 1.
The stirring velocity of described stirring is 70r/min.
Temperature when described Secondary ammonium phosphate is synthetic is controlled at 60-70 ℃.
Temperature when described Secondary ammonium phosphate is synthetic is controlled at 65 ℃.
The described stirring reaction time is 30-50min.
Described drying temperature is 85 ℃.
Described Secondary ammonium phosphate product, its physical and chemical index is that Secondary ammonium phosphate total nutrient is greater than 74%, total nitrogen 21.02-21.22%, Vanadium Pentoxide in FLAKES are 53.02-53.52%, and moisture is that 0.25-0.32%, water-insoluble are that 0.087-0.096%, fluorochemical are 0.1-0.14%.
Described Secondary ammonium phosphate product, its physical and chemical index is that Secondary ammonium phosphate total nutrient is greater than 74%, and total nitrogen 21.12%, Vanadium Pentoxide in FLAKES are 53.27%, and moisture is 0.28%, water-insoluble is 0.092%, fluorochemical is 0.13%.
Compared with prior art, technique effect of the present invention embodies as follows:
1. by highly purified Ureaphil and ammonia direct reaction, prepare Secondary ammonium phosphate, broken through the technology of phosphoric acid and ammonia react preparing phosphoric acid hydrogen two ammoniums, solved because phosphoric acid concentration difference is to equipment material requirement difference, and because of the different technical barriers of understanding the damages in various degree that bring to equipment corrosion of concentration, also avoided containing in waste liquid a large amount of phosphoric acid, the technical barrier of contaminate environment.
2. the by product producing in this law (urea slip) can be recycled as the raw materials for production of Ureaphil technique, reduces the pollution that expends and avoid environment of raw material.
2. the technical process that this law adopts is short, with short production cycle; And the equipment and the device that in whole technique, there is no high energy consumption, its power consumption is low.
The physical and chemical index of the Secondary ammonium phosphate product that 4. this law is produced meets technical grade demand completely, concrete physical and chemical index parameter can reach Secondary ammonium phosphate total nutrient and be greater than 74%, total nitrogen 21.02-21.22%, Vanadium Pentoxide in FLAKES are 53.02-53.52%, and moisture is that 0.25-0.32%, water-insoluble are that 0.087-0.096%, fluorochemical are 0.1-0.14%.
Accompanying drawing explanation
Fig. 1 is equipment flowsheet of the present invention.
1-dissolving tank 2-synthesizes groove 3-crystallizer 4-whizzer.
Embodiment
Below in conjunction with accompanying drawing and concrete embodiment, technical scheme of the present invention is done to further restriction, but claimed scope is not only confined to done description.
Noun explanation:
Ureaphil (Ureaphosphate, UP), is for No. CAS 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 that is 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, it is acid that the aqueous solution is, and starts to decompose to emit carbonic acid gas and ammonia during melting.
Principle explanation:
The present invention adopts pure Ureaphil and ammonia directly to carry out replacement(metathesis)reaction and makes Secondary ammonium phosphate product, and its production principle is as follows:
CO(NH 2) 2·H 3PO 4+2NH 3=(NH 4) 2HPO 4+CO(NH 2) 2
Ureaphil and ammonia generation replacement(metathesis)reaction, first generate primary ammonium phosphate, and along with the increasing of ammonia amount, primary ammonium phosphate continues to generate Secondary ammonium phosphate with ammonia generation replacement(metathesis)reaction, is exactly diammonium phosphate; By controlling the pH value of reaction end, obtain diammonium phosphate product, this process does not have the discharge of waste gas waste water and refuse, has the significant value of environmental protection; Meanwhile, in production process, produce urea slip, can be used as chemical fertilizers production raw material, also can proceed to production of urea phosphate technique and continue to produce Ureaphil product, make technical process reach cyclic production, reduce the consumption of raw material, reduce production costs, there is significant economic benefit.
Be illustrated in figure 1 equipment flowsheet of the present invention, raw material Ureaphil is dissolved in water in dissolving tank 1 or is diluted to the Ureaphil solution that concentration is moderate, and dissolve or dilution in control temperature and reach certain numerical value, proceeded to again in synthetic groove 2, slowly add wherein ammonia simultaneously, being uniformly mixed solution makes it that replacement(metathesis)reaction occur, and control reaction times and temperature of reaction, be adjusted to ph value of reaction one regularly simultaneously, reaction reaches terminal, mixed slurry is proceeded to and in crystallizer 3, carries out crystallisation by cooling processing, when separating out Secondary ammonium phosphate crystal completely, proceed in separating centrifuge 4, carry out centrifugal treating, obtain filtrate and filter cake, filtrate is urea slip, filter cake is Secondary ammonium phosphate, carries out dry packing and can obtain an industrial grade Secondary ammonium phosphate.
Embodiment 1
A production method for Secondary ammonium phosphate, is to adopt highly purified Ureaphil solution and ammonia generation replacement(metathesis)reaction, and to control pH value be 7.8, and temperature is at 50 ℃, and stirring reaction 20min prepares Secondary ammonium phosphate product.
Specifically comprise the following steps:
(1) preparation of Ureaphil solution: the Ureaphil solid that is 97% by purity is sent in dissolving tank, adds water metering, and being heated to temperature is 40 ℃, under agitation condition, according to stirring velocity, be that 60r/min stirs, after mixing, be mixed with saturated Ureaphil solution, stand-by;
(2) Secondary ammonium phosphate is synthetic: by step 1) in the saturated Ureaphil solution for preparing adopt transferpump to be transported in synthetic groove, and pass into wherein ammonia, the mol ratio of ammonia and saturated Ureaphil is 2:1, and to control temperature be 50 ℃, adjusting pH value is 7.8 o'clock, according to stirring velocity, be 60r/min, stirring reaction 20min, obtains Secondary ammonium phosphate slip;
(3) Secondary ammonium phosphate slip Crystallization Separation: by step 2) obtaining adopts transferpump to proceed to crystallisation by cooling in cooling crystallizer, be cooled to≤40 ℃, Secondary ammonium phosphate crystal is proceeded to separating centrifuge separation, obtain filtrate and filter cake, filtrate is that urea slip proceeds to production of urea phosphate technique; Filter cake is Secondary ammonium phosphate product, proceeds in drying machine and is dried, and in temperature, be at 85 ℃, to carry out packing after drying treatment, obtain and meet an industrial grade Secondary ammonium phosphate product.
Adopt technical grade standard, and the physical and chemical index of this product of sampling analysis, its result is: Secondary ammonium phosphate total nutrient is greater than 74%, and total nitrogen 21.02%, Vanadium Pentoxide in FLAKES are 53.02%, and moisture is 0.25%, water-insoluble is 0.087%, fluorochemical is 0.1%.
Embodiment 2
A production method for Secondary ammonium phosphate, is to adopt highly purified Ureaphil solution and ammonia generation replacement(metathesis)reaction, and to control pH value be 8.2, and temperature is at 80 ℃, and stirring reaction 60min prepares Secondary ammonium phosphate product.
Specifically comprise the following steps:
(1) preparation of Ureaphil solution: the Ureaphil solid that is 98% by purity is sent in dissolving tank, adds water metering, and being heated to temperature is 60 ℃, under agitation condition, according to stirring velocity, be that 80r/min stirs, after mixing, be mixed with saturated Ureaphil solution, stand-by;
(2) Secondary ammonium phosphate is synthetic: by step 1) in the saturated Ureaphil solution for preparing adopt transferpump to be transported in synthetic groove, and pass into wherein ammonia, the mol ratio of ammonia and saturated Ureaphil is 2.5:1, and to control temperature be 80 ℃, adjusting pH value is 8.2 o'clock, according to stirring velocity, be 80r/min, stirring reaction 60min, obtains Secondary ammonium phosphate slip;
(3) Secondary ammonium phosphate slip Crystallization Separation: by step 2) obtaining adopts transferpump to proceed to crystallisation by cooling in cooling crystallizer, be cooled to≤40 ℃, Secondary ammonium phosphate crystal is proceeded to separating centrifuge separating treatment, obtain filtrate and filter cake, filtrate is that urea slip proceeds to production of urea phosphate technique; Filter cake is Secondary ammonium phosphate product, proceeds in drying machine and is dried, and drying temperature is 85 ℃ of dry rear packings, obtains and meets an industrial grade Secondary ammonium phosphate product.
Adopt technical grade standard, and the physical and chemical index of this product of sampling analysis, its result is: Secondary ammonium phosphate total nutrient is greater than 74%, and total nitrogen 21.22%, Vanadium Pentoxide in FLAKES are 53.52%, and moisture is 0.32%, water-insoluble is 0.096%, fluorochemical is 0.14%.
Embodiment 3
A production method for Secondary ammonium phosphate, is to adopt highly purified Ureaphil solution and ammonia generation replacement(metathesis)reaction, and to control pH value be 8, and temperature is at 65 ℃, and stirring reaction 40min prepares Secondary ammonium phosphate product.
Specifically comprise the following steps:
(1) preparation of Ureaphil solution: the Ureaphil solid that is 99% by purity is sent in dissolving tank, adds water metering, and being heated to temperature is 50 ℃, under agitation condition, according to stirring velocity, be that 70r/min stirs, after mixing, be mixed with saturated Ureaphil solution, stand-by;
(2) Secondary ammonium phosphate is synthetic: by step 1) in the saturated Ureaphil solution for preparing adopt transferpump to be transported in synthetic groove, and pass into wherein ammonia, the mol ratio of ammonia and saturated Ureaphil is 2.3:1, and to control temperature be 65 ℃, adjusting pH value is 8 o'clock, according to stirring velocity, be 70r/min, stirring reaction 40min, obtains Secondary ammonium phosphate slip;
(3) Secondary ammonium phosphate slip Crystallization Separation: by step 2) obtaining adopts transferpump to proceed to crystallisation by cooling in cooling crystallizer, be cooled to≤40 ℃, Secondary ammonium phosphate crystal is proceeded to separating centrifuge separation, obtain filtrate and filter cake, filtrate is that urea slip proceeds to production of urea phosphate technique; Filter cake is Secondary ammonium phosphate product, proceeds in drying machine and is dried, and drying temperature is at 85 ℃, and dry rear packing, obtains and meet an industrial grade Secondary ammonium phosphate product.
Adopt technical grade standard, and the physical and chemical index of this product of sampling analysis, its result is: Secondary ammonium phosphate total nutrient is greater than 74%, and total nitrogen 21.12%, Vanadium Pentoxide in FLAKES are 53.27%, and moisture is 0.28%, water-insoluble is 0.092%, fluorochemical is 0.13%.
Embodiment 4
A production method for Secondary ammonium phosphate, is to adopt highly purified Ureaphil solution and ammonia generation replacement(metathesis)reaction, and to control pH value be 7.9, and temperature is at 60 ℃, and stirring reaction 30min prepares Secondary ammonium phosphate product.
Specifically comprise the following steps:
(1) preparation of Ureaphil solution: the Ureaphil solid that is 98% by purity is sent in dissolving tank, adds water metering, and being heated to temperature is 45 ℃, under agitation condition, according to stirring velocity, be that 65r/min stirs, after mixing, be mixed with saturated Ureaphil solution, stand-by;
(2) Secondary ammonium phosphate is synthetic: by step 1) in the saturated Ureaphil solution for preparing adopt transferpump to be transported in synthetic groove, and pass into wherein ammonia, the mol ratio of ammonia and saturated Ureaphil is 2.2:1, and to control temperature be 60 ℃, adjusting pH value is 7.9 o'clock, according to stirring velocity, be 65r/min, stirring reaction 30min, obtains Secondary ammonium phosphate slip;
(3) Secondary ammonium phosphate slip Crystallization Separation: by step 2) obtaining adopts transferpump to proceed to crystallisation by cooling in cooling crystallizer, be cooled to≤40 ℃, Secondary ammonium phosphate crystal is proceeded to separating centrifuge separating treatment, obtain filtrate and filter cake, filtrate is that urea slip proceeds to production of urea phosphate technique; Filter cake is Secondary ammonium phosphate product, proceeds in drying machine and is dried, and drying temperature is dry rear packing at 85 ℃, obtains and meets an industrial grade Secondary ammonium phosphate product.
Adopt technical grade standard, and the physical and chemical index of this product of sampling analysis, its result is: Secondary ammonium phosphate total nutrient is greater than 74%, and total nitrogen 21.20%, Vanadium Pentoxide in FLAKES are 53.32%, and moisture is 0.28%, water-insoluble is 0.095%, fluorochemical is 0.12%.
Embodiment 5
A production method for Secondary ammonium phosphate, is to adopt highly purified Ureaphil solution and ammonia generation replacement(metathesis)reaction, and to control pH value be 8.1, and temperature is at 70 ℃, and stirring reaction 50min prepares Secondary ammonium phosphate product.
Specifically comprise the following steps:
(1) preparation of Ureaphil solution: the Ureaphil solid that is 98% by purity is sent in dissolving tank, adds water metering, is heated to stabilize to 55 ℃, under agitation condition, according to stirring velocity, be that 75r/min stirs, after mixing, be mixed with saturated Ureaphil solution, stand-by;
(2) Secondary ammonium phosphate is synthetic: by step 1) in the saturated Ureaphil solution for preparing adopt transferpump to be transported in synthetic groove, and pass into wherein ammonia, the mol ratio of ammonia and saturated Ureaphil is 2.1:1, and to control temperature be 70 ℃, adjusting pH value is 8.1 o'clock, according to stirring velocity, be 75r/min, stirring reaction 50min, obtains Secondary ammonium phosphate slip;
(3) Secondary ammonium phosphate slip Crystallization Separation: by step 2) obtaining adopts transferpump to proceed to crystallisation by cooling in cooling crystallizer, be cooled to≤40 ℃, Secondary ammonium phosphate crystal is proceeded to separating centrifuge separation, obtain filtrate and filter cake, filtrate is that urea slip proceeds to production of urea phosphate technique; Filter cake is Secondary ammonium phosphate product, proceed in drying machine dry, drying temperature be 85 ℃ dry after, packing, obtains and meets an industrial grade Secondary ammonium phosphate product.
Adopt technical grade standard, and the physical and chemical index of this product of sampling analysis, its result is: Secondary ammonium phosphate total nutrient is greater than 74%, and total nitrogen 21.18%, Vanadium Pentoxide in FLAKES are 53.42%, and moisture is 0.29%, water-insoluble is 0.089%, fluorochemical is 0.11%.
Embodiment 6
A production method for Secondary ammonium phosphate, is to adopt highly purified Ureaphil solution and ammonia generation replacement(metathesis)reaction, and to control pH value be 8, and temperature is at 63 ℃, and stirring reaction 42min prepares Secondary ammonium phosphate product.
Specifically comprise the following steps:
(1) preparation of Ureaphil solution: the Ureaphil solid that is 98% by purity is sent in dissolving tank, adds water metering, is heated to 58 ℃ of temperature, under agitation condition, according to stirring velocity, be that 66r/min stirs, after mixing, be mixed with saturated Ureaphil solution, stand-by;
(2) Secondary ammonium phosphate is synthetic: by step 1) in the saturated Ureaphil solution for preparing adopt transferpump to be transported in synthetic groove, and pass into wherein ammonia, the mol ratio of ammonia and saturated Ureaphil is 2.4:1, and to control temperature be 63 ℃, adjusting pH value is 8 o'clock, according to stirring velocity, be 66r/min, stirring reaction 42min, obtains Secondary ammonium phosphate slip;
(3) Secondary ammonium phosphate slip Crystallization Separation: by step 2) obtaining adopts transferpump to proceed to crystallisation by cooling in cooling crystallizer, be cooled to≤40 ℃, Secondary ammonium phosphate crystal is proceeded to separating centrifuge separation, obtain filtrate and filter cake, filtrate is that urea slip proceeds to production of urea phosphate technique; Filter cake is Secondary ammonium phosphate product, proceeds in drying machine and is dried, and drying temperature is 85 ℃ of dry rear packings, obtains and meets an industrial grade Secondary ammonium phosphate product.
Adopt technical grade standard, and the physical and chemical index of this product of sampling analysis, its result is: Secondary ammonium phosphate total nutrient is greater than 74%, and total nitrogen 21.08%, Vanadium Pentoxide in FLAKES are 53.22%, and moisture is 0.27%, water-insoluble is 0.093%, fluorochemical is 0.11%.
Embodiment 7
A production method for Secondary ammonium phosphate, is to adopt highly purified Ureaphil solution and ammonia generation replacement(metathesis)reaction, and to control pH value be 8.1, and temperature is at 59 ℃, and stirring reaction 53min prepares Secondary ammonium phosphate product.
Specifically comprise the following steps:
(1) preparation of Ureaphil solution: the Ureaphil solid that is 97% by purity is sent in dissolving tank, adds water metering, and being heated to temperature is 52 ℃, under agitation condition, according to stirring velocity, be that 77r/min stirs, after mixing, be mixed with saturated Ureaphil solution, stand-by;
(2) Secondary ammonium phosphate is synthetic: by step 1) in the saturated Ureaphil solution for preparing adopt transferpump to be transported in synthetic groove, and pass into wherein ammonia, the mol ratio of ammonia and saturated Ureaphil is 2.2:1, and to control temperature be 59 ℃, adjusting pH value is 8.1 o'clock, according to stirring velocity, be 76r/min, stirring reaction 53min, obtains Secondary ammonium phosphate slip;
(3) Secondary ammonium phosphate slip Crystallization Separation: by step 2) obtaining adopts transferpump to proceed to crystallisation by cooling in cooling crystallizer, be cooled to≤40 ℃, Secondary ammonium phosphate crystal is proceeded to separating centrifuge separation, obtain filtrate and filter cake, filtrate is that urea slip proceeds to production of urea phosphate technique; Filter cake is Secondary ammonium phosphate product, proceeds in drying machine and is dried, and drying temperature is 85 ℃ of dry rear packings, obtains and meets an industrial grade Secondary ammonium phosphate product.
Adopt technical grade standard, and the physical and chemical index of this product of sampling analysis, its result is: Secondary ammonium phosphate total nutrient is greater than 74%, and total nitrogen 21.15%, Vanadium Pentoxide in FLAKES are 53.12%, and moisture is 0.31%, water-insoluble is 0.095%, fluorochemical is 0.12%.
At this, it is important to point out: above embodiment only limits to understand technical scheme of the present invention is further elaborated; and can not be interpreted as technical scheme of the present invention is done to further restriction; those skilled in the art is in the scope of above-described embodiment and technical scheme of the present invention; that makes does not have outstanding substantive distinguishing features and significant progressive improvement with the present invention, still belongs to protection category of the present invention.

Claims (10)

1. a production method for Secondary ammonium phosphate, is characterized in that: adopt highly purified Ureaphil solution and ammonia generation replacement(metathesis)reaction, control pH value is 7.8-8.2, and temperature is at 50-80 ℃, and stirring reaction 20-60min, prepares Secondary ammonium phosphate product.
2. the production method of Secondary ammonium phosphate as claimed in claim 1, is characterized in that following steps:
(1) preparation of Ureaphil solution: the Ureaphil solid that is >=98% by purity is sent in dissolving tank, adds water metering, is heated to 40-60 ℃, under agitation condition, according to stirring velocity, be 60-80r/min, after mixing, be mixed with saturated Ureaphil solution, stand-by;
(2) Secondary ammonium phosphate is synthetic: by step 1) in the saturated Ureaphil solution for preparing adopt transferpump to be transported in synthetic groove, and pass into wherein ammonia, the mol ratio of ammonia and saturated Ureaphil is (2-2.5): 1, and to control temperature be 50-80 ℃, when adjustment pH value is 7.8-8.2, according to stirring velocity, be 60-80r/min, stirring reaction 20-60min, obtains Secondary ammonium phosphate slip;
(3) Secondary ammonium phosphate slip Crystallization Separation: by step 2) obtaining adopts transferpump to proceed to crystallisation by cooling in cooling crystallizer, be cooled to≤40 ℃, Secondary ammonium phosphate crystal is proceeded to separating centrifuge separating treatment, obtain filtrate and filter cake, filtrate is that urea slip proceeds to production of urea phosphate technique; Filter cake is Secondary ammonium phosphate product, proceeds in drying machine and is dried, and packing, obtains and meet an industrial grade Secondary ammonium phosphate product.
3. the production method of Secondary ammonium phosphate as claimed in claim 1 or 2, is characterized in that: described pH value is 8.
4. the production method of Secondary ammonium phosphate as claimed in claim 1 or 2, is characterized in that: described ammonia and the mol ratio of saturated Ureaphil are (2-2.3): 1.
5. the production method of Secondary ammonium phosphate as claimed in claim 1 or 2, is characterized in that: described stirring velocity is 70r/min.
6. the production method of Secondary ammonium phosphate as claimed in claim 2, is characterized in that: temperature when described Secondary ammonium phosphate is synthetic is controlled at 60-70 ℃.
7. the production method of Secondary ammonium phosphate as claimed in claim 2, is characterized in that: temperature when described Secondary ammonium phosphate is synthetic is controlled at 65 ℃.
8. the production method of Secondary ammonium phosphate as claimed in claim 1 or 2, is characterized in that: the described stirring reaction time is 30-50min.
9. the production method of Secondary ammonium phosphate as claimed in claim 2, is characterized in that: described drying temperature is 85 ℃.
10. the production method of Secondary ammonium phosphate as claimed in claim 1 or 2, it is characterized in that: described Secondary ammonium phosphate product, its physical and chemical index is that Secondary ammonium phosphate total nutrient is greater than 74%, total nitrogen 21.02-21.22%, Vanadium Pentoxide in FLAKES are 53.02-53.52%, and moisture is that 0.25-0.32%, water-insoluble are that 0.087-0.096%, fluorochemical are 0.1-0.14%.
CN201410213341.7A 2014-05-20 2014-05-20 Production method for diammonium hydrogen phosphate Pending CN104016322A (en)

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CN104291286A (en) * 2014-09-19 2015-01-21 贵阳中化开磷化肥有限公司 Production for preparing special fertilizer for peas from diammonium hydrogen phosphate byproduct
CN104310330A (en) * 2014-09-19 2015-01-28 贵州大学 Method for preparing ammonium dihydrogen phosphate and preparing special composite fertilizer for orange trees as byproduct
CN104310334A (en) * 2014-09-19 2015-01-28 贵州大学 Method for preparing ammonium dihydrogen phosphate and preparing special composite fertilizer for Artemisia carvifolia as byproduct
CN104326449A (en) * 2014-09-19 2015-02-04 贵州大学 Method for preparing ammonium dihydrogen phosphate and by-product special compound fertilizer for eggplant
CN104326452A (en) * 2014-09-19 2015-02-04 贵州大学 Method for preparing ammonium dihydrogen phosphate and by-product special compound fertilizer for pineapple
CN104401953A (en) * 2014-11-21 2015-03-11 贵阳中化开磷化肥有限公司 Di-ammonium phosphate produced by wet process phosphoric acid and production method of di-ammonium phosphate
CN110371939A (en) * 2019-07-26 2019-10-25 武汉科技大学 A kind of preparation method of the Diammonium phosphate (DAP) based on phosphoric acid raffinate
CN115092899A (en) * 2022-06-27 2022-09-23 佛山市德方纳米科技有限公司 Preparation method of diammonium hydrogen phosphate and battery positive electrode material

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GB1191635A (en) * 1966-07-27 1970-05-13 Marchon Products Ltd Improvements in the manufacture of Orthophosphates
DE1767676A1 (en) * 1968-06-04 1971-09-23 Kalk Chemische Fabrik Gmbh Process for the production of low-fluorine phosphates
CN101519197A (en) * 2009-04-08 2009-09-02 四川川恒化工股份有限公司 Method for producing type I ammonium polyphosphate with high degree of polymerization

Cited By (23)

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CN104326452A (en) * 2014-09-19 2015-02-04 贵州大学 Method for preparing ammonium dihydrogen phosphate and by-product special compound fertilizer for pineapple
CN104291286B (en) * 2014-09-19 2016-08-17 贵州开磷集团股份有限公司 A kind of production method preparing diammonium phosphate by-product Semen Pisi sativi special fertilizer
CN104229765A (en) * 2014-09-19 2014-12-24 贵阳中化开磷化肥有限公司 Production method for preparing ammonium phosphate byproduct used as special fertilizer for red peonies
CN104261376A (en) * 2014-09-19 2015-01-07 贵阳中化开磷化肥有限公司 Preparation method of special compound fertilizer for haricot
CN104276550A (en) * 2014-09-19 2015-01-14 贵阳中化开磷化肥有限公司 Production method for preparing special fertilizer for dasheen from diammonium hydrogen phosphate by-products
CN104276551A (en) * 2014-09-19 2015-01-14 贵阳中化开磷化肥有限公司 Production method for preparing diammonium hydrogen phosphate and byproduct special fertilizer for oats
CN104291286A (en) * 2014-09-19 2015-01-21 贵阳中化开磷化肥有限公司 Production for preparing special fertilizer for peas from diammonium hydrogen phosphate byproduct
CN104310330A (en) * 2014-09-19 2015-01-28 贵州大学 Method for preparing ammonium dihydrogen phosphate and preparing special composite fertilizer for orange trees as byproduct
CN104310334A (en) * 2014-09-19 2015-01-28 贵州大学 Method for preparing ammonium dihydrogen phosphate and preparing special composite fertilizer for Artemisia carvifolia as byproduct
CN104261937B (en) * 2014-09-19 2016-01-06 贵州开磷集团股份有限公司 A kind of production method preparing primary ammonium phosphate by-product Chinese yam special fertilizer
CN104261937A (en) * 2014-09-19 2015-01-07 贵阳中化开磷化肥有限公司 Production method for preparing ammonium dihydrogen phosphate and byproduct special fertilizer for Chinese yam
CN104310334B (en) * 2014-09-19 2017-02-08 贵州大学 Method for preparing ammonium dihydrogen phosphate and preparing special composite fertilizer for Artemisia carvifolia as byproduct
CN104326449A (en) * 2014-09-19 2015-02-04 贵州大学 Method for preparing ammonium dihydrogen phosphate and by-product special compound fertilizer for eggplant
CN104276551B (en) * 2014-09-19 2016-03-09 贵州开磷集团股份有限公司 A kind of production method preparing Secondary ammonium phosphate by-product oat special fertilizer
CN104250001B (en) * 2014-09-19 2016-03-16 贵州开磷集团股份有限公司 A kind of production method preparing potassium primary phosphate by-product fertilizer special for tobacco
CN104261376B (en) * 2014-09-19 2016-04-27 贵州开磷集团股份有限公司 A kind of preparation method of French beans composite fertilizer special
CN104250001A (en) * 2014-09-19 2014-12-31 贵阳中化开磷化肥有限公司 Production method of special tobacco fertilizer serving as byproduct of preparation of monopotassium phosphate
CN104276550B (en) * 2014-09-19 2016-08-17 贵州开磷集团股份有限公司 A kind of production method preparing diammonium phosphate by-product Fructus Colocasiae Esculentae special fertilizer
CN104229765B (en) * 2014-09-19 2016-08-24 贵州开磷集团股份有限公司 A kind of production method preparing ammonium phosphate by-product Radix Paeoniae Rubra special fertilizer
CN104401953A (en) * 2014-11-21 2015-03-11 贵阳中化开磷化肥有限公司 Di-ammonium phosphate produced by wet process phosphoric acid and production method of di-ammonium phosphate
CN110371939A (en) * 2019-07-26 2019-10-25 武汉科技大学 A kind of preparation method of the Diammonium phosphate (DAP) based on phosphoric acid raffinate
CN110371939B (en) * 2019-07-26 2022-08-16 武汉科技大学 Preparation method of diammonium phosphate based on phosphoric acid extraction spent acid
CN115092899A (en) * 2022-06-27 2022-09-23 佛山市德方纳米科技有限公司 Preparation method of diammonium hydrogen phosphate and battery positive electrode material

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