CN112939682A - Preparation method of polyphosphate synergistic nitrophosphate fertilizer - Google Patents
Preparation method of polyphosphate synergistic nitrophosphate fertilizer Download PDFInfo
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- CN112939682A CN112939682A CN202110198168.8A CN202110198168A CN112939682A CN 112939682 A CN112939682 A CN 112939682A CN 202110198168 A CN202110198168 A CN 202110198168A CN 112939682 A CN112939682 A CN 112939682A
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B11/00—Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes
- C05B11/04—Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes using mineral acid
- C05B11/06—Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes using mineral acid using nitric acid (nitrophosphates)
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/40—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting fertiliser dosage or release rate; for affecting solubility
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/90—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting the nitrification of ammonium compounds or urea in the soil
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G5/00—Fertilisers characterised by their form
- C05G5/10—Solid or semi-solid fertilisers, e.g. powders
- C05G5/12—Granules or flakes
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Abstract
The invention is applicable to the field of nitrophosphate fertilizers, and provides a preparation method of a polyphosphate synergistic nitrophosphate fertilizer, which comprises the following steps: preparing a neutralization solution; pumping the neutralized liquid into a concentration system, and carrying out preheating, evaporation and gas-liquid separation at 135-175 ℃ to obtain concentrated slurry; introducing the concentrated slurry into a No. 1 polymerization tank, and carrying out prepolymerization at the temperature of 175-185 ℃ to obtain I-grade polymerization slurry; overflowing the I-grade polymerization slurry to a No. 2 polymerization tank when the liquid level of the I-grade polymerization slurry is full, adding medium trace elements, and carrying out repolymerization at the temperature of 180-185 ℃ to obtain II-grade polymerization slurry; and granulating, drying and screening the II-grade polymerization slurry to obtain the polyphosphate synergistic nitrophosphate fertilizer. The method solves the technical problem that the high temperature in the polymerization section is easy to overflow or even explode through two-stage polymerization reaction of prepolymerization and repolymerization, improves the effectiveness of phosphorus, has high nutrient absorption and utilization rate, has the characteristic of quick-acting and long-acting functions, and promotes the quality improvement and the yield increase of crops.
Description
Technical Field
The invention belongs to the technical field of nitrophosphate fertilizers, and particularly relates to a preparation method of a polyphosphate synergistic nitrophosphate fertilizer.
Background
The nitrophosphate fertilizer is a high-quality phosphorus compound fertilizer variety, has reasonable proportion and structure of nitrogen and phosphorus, and is suitable for most crops to N and P2O5According to the research and analysis of the Chinese plant Nutrition and Fertilizer society, the capacity of 3000 million tons of nitric phosphate fertilizer in China can replace 800 million tons of ammonium phosphate, the emission of 2000 million tons of phosphogypsum can be reduced every year, and the consumption of 400 million tons of sulfur can be reduced. However, phosphate radicals in the application process of the nitric phosphate fertilizers on the market at present are easily fixed by metal ions such as iron and calcium in soil, the migration capacity is weak, the fertilizer efficiency time is short, the nutrient utilization rate is low, the resource waste is caused, and the soil environment is likely to be damaged after long-term application.
The polyphosphate synergistic nitrophosphate fertilizer contains orthophosphate, metaphosphate and polyphosphate. Polyphosphoric acid has chelating capacity for metal ions, is not easy to be fixed, and has high phosphorus utilization rate; the polyphosphate can not be directly absorbed by plants, but is gradually hydrolyzed into orthophosphate to be utilized by the plants, and has good slow-release long-acting function; in addition, the polyphosphate has good solubility, strong mobility and high absorption and utilization rate, and can effectively solve physiological diseases of crops caused by deficiency of elements.
At present, the research on polyphosphoric acid is mostly focused on the preparation of polyphosphoric acid carriers, the application of liquid fertilizers and the like, but the application of polyphosphoric acid on nitrophosphate fertilizers is less, the polyphosphoric acid is separately added in an additive form, the cost is high, and the polyphosphoric acid is easily decomposed at high temperature in the adding process, the chelating capacity is weakened, and the effect is not ideal.
Disclosure of Invention
The invention aims to provide a preparation method of a polyphosphate synergistic nitrophosphate fertilizer, and aims to solve the problems that in the prior art, a polymerization section is easy to overflow from a tank even explode at high temperature and the phosphorus utilization rate is low.
In one aspect, the invention provides a preparation method of a polyphosphate synergistic nitrophosphate fertilizer, which comprises the following steps:
preparing a neutralization solution;
pumping the neutralized liquid into a concentration system, and carrying out preheating, evaporation and gas-liquid separation at 135-175 ℃ to obtain concentrated slurry;
introducing the concentrated slurry into a No. 1 polymerization tank, and carrying out prepolymerization at the temperature of 175-185 ℃ to obtain I-grade polymerization slurry;
overflowing the I-grade polymerization slurry to a No. 2 polymerization tank when the liquid level of the I-grade polymerization slurry is full, adding medium trace elements, and carrying out repolymerization at the temperature of 180-185 ℃ to obtain II-grade polymerization slurry;
and granulating, drying and screening the II-grade polymerization slurry to obtain the polyphosphate synergistic nitrophosphate fertilizer.
According to the preparation method of the polyphosphate synergistic nitrophosphate fertilizer, provided by the invention, through two-stage polymerization reaction of prepolymerization and repolymerization, the technical problem that a polymerization section is easy to cause groove bursting or even explosion at high temperature is solved, the operation is safer and more controllable, the product polymerization rate is high, the solubility is good, medium and trace elements are stably chelated, the phosphorus effectiveness is improved, the nutrient absorption and utilization rate is high, and the preparation method has the characteristics of quick-acting and long-acting functions, and the quality and yield of crops are promoted to be improved; in addition, the prepared polyphosphate synergistic nitrophosphate fertilizer is directly conveyed to a bulk warehouse for stockpiling without cooling and wrapping steps, and is packaged according to market demands, so that the production cost and the warehouse occupation are saved.
Drawings
FIG. 1 is a flow chart of a method for preparing a polyphosphate synergistic nitrophosphate fertilizer provided by embodiment 1 of the invention.
FIG. 2 is a flow diagram of a two-stage polymerization process according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a preparation method of a polyphosphate synergistic nitrophosphate fertilizer, which comprises the following steps:
the invention provides a method which is characterized by comprising the following steps:
s01: preparing a neutralization solution;
s02: pumping the neutralized liquid into a concentration system, and carrying out preheating, evaporation and gas-liquid separation at 135-175 ℃ to obtain concentrated slurry;
s03: introducing the concentrated slurry into a No. 1 polymerization tank, and carrying out prepolymerization at the temperature of 175-185 ℃ to obtain I-grade polymerization slurry;
s04: overflowing the I-grade polymerization slurry to a No. 2 polymerization tank when the liquid level of the I-grade polymerization slurry is full, adding medium trace elements, and carrying out repolymerization at the temperature of 180-185 ℃ to obtain II-grade polymerization slurry;
s05: and granulating, drying and screening the II-grade polymerization slurry to obtain the polyphosphate synergistic nitrophosphate fertilizer.
Specifically, the preparation of the neutralization solution in step S01 includes the steps of: (1) decomposing phosphorite with nitric acid to obtain acidolysis solution; (2) freezing and crystallizing, and filtering with calcium nitrate; (3) and (4) neutralizing the mother liquor with ammonia to obtain a neutralized solution. The neutralizing liquid contains NH4NO3、(NH4)2PO4、CaHPO4、MgHPO4、FePO4、AlPO4、CaF2And the like.
Preferably, in step S02, the concentrated slurry has a mass concentration of 80 to 97.5%.
Preferably, the amount of the concentrated slurry entering the polymerization tank No. 1 in the step S03 is 15-30 t/h, the prepolymerization time is 0.9-1.4 h, and the mass concentration of the obtained grade I polymerization slurry is 98-99%. When the concentrated slurry is introduced into the No. 1 polymerization tank, the feed extends from the top to the bottom of the tank.
Preferably, the repolymerization time in the step S04 is 0.9-1.4 h, and the mass concentration of the obtained II-grade polymerization slurry is 98.5-99.5%.
Preferably, the polymerization tail gas pipe is designed for the polymerization tank # 1 and the polymerization tank # 2 in the steps S03 and S04.
Preferably, in step S04, the medium trace element is one or more of magnesium oxide, zinc sulfate, manganese sulfate, boric acid, ferrous sulfate and copper sulfate, and more preferably a combination of magnesium oxide, zinc sulfate and boric acid. More preferably, the molar ratio of magnesium oxide to zinc sulfate monohydrate to boric acid is 1: 0.04: 0.07.
Preferably, the mass of the medium trace element salt is 0.1-2.0% of that of the II-grade polymerization slurry.
Preferably, the granulation mode in step S05 is at least one of biaxial granulation, drum granulation, spray granulation, high tower granulation, atomization granulation and disc granulation; the screening particle size is 2.0-4.0 mm.
TABLE 1 Key Process parameters for each section
(1) Because the polymerization slurry is an ash molten body, the content of ammonium nitrate is 60-80%, the phenomenon of overflowing can occur when the ammonium nitrate starts to decompose at 185 ℃, once the ammonium nitrate splashes on the skin, eyes and other parts, serious scald can be caused, when the temperature reaches 210 ℃ and the impurities participate, the thermal decomposition of the ammonium nitrate is obviously accelerated, explosion is easily caused, and great danger is realized (as shown in the following formula). According to the invention, two-stage polymerization reaction of prepolymerization and repolymerization is carried out, the temperature is controlled to be 175-185 ℃, and the conventional one-stage polymerization reaction needs high temperature of nearly 200 ℃, so that the safety problem that ammonium nitrate is easy to decompose and overflow or even explode in a polymerization section under the high-temperature condition is effectively solved.
Ammonium nitrate is decomposed at (200-:
NH4NO3→N2+0.5O2+2H2O+129kJ
(2) when the concentrated slurry is introduced into a No. 1 polymerization tank, feeding extends from the top of the tank to the bottom of the tank, and the feeding flow rate is controlled to be 15-30 t/h, so that the slurry is heated more uniformly, and the phenomenon of overflowing caused by overhigh local temperature is avoided; meanwhile, the slurry residence time is increased as much as possible, so that the polymerization reaction is more complete.
(3) The formation process of polyphosphoric acid is a dehydration condensation process of phosphoric acid (shown as the following formula), and polymerization tail gas pipes are designed in the polymerization tank No. 1 and the polymerization tank No. 2, so that evaporated water can be effectively taken away, and the forward reaction in the polymerization process is more thorough.
(4) The polyphosphoric acid molecule contains a large amount of-HPO3The functional group can provide a plurality of pairs of lone-pair electrons for metal ions, and medium trace elements are added to the metal ions, so that the metal ions are easier to react with Ca2+、Mg2+、Zn2+、Mn2+、Fe2+、Cu2+Forming a chelating ring or network of water-soluble polyphosphate (as shown below).
(5) Because the traditional one-stage polymerization reaction is not complete enough, the polymerization rate is low and unstable, the invention has more complete two-stage polymerization reaction, higher polymerization rate, better product solubility, lower content of water insoluble substances and easier absorption by crops after application.
(6) If polyphosphate is added, the theoretical accounting increases the cost by more than 100 yuan/ton, the production of the nitrophosphate fertilizer and the production of the polyphosphate are effectively combined, the theoretical accounting increases the cost by 20-40 yuan/ton, the production process is optimized, and the production cost is reduced.
(7) The invention can improve the effectiveness of phosphorus in the nitrophosphate fertilizer, has high nutrient absorption and utilization rate and the characteristic of quick-acting and long-acting functions, promotes the quality improvement and the yield increase of crops, widens the functional attribute of the nitrophosphate fertilizer product and improves the popularization and application value of the nitrophosphate fertilizer product.
The following detailed description of specific implementations of the present invention is provided in conjunction with specific embodiments:
example 1:
the preparation method of the polyphosphate synergistic nitrophosphate fertilizer specifically comprises the following steps:
1) preparing a neutralization solution;
2) pumping the neutralized liquid into a concentration system, and carrying out preheating, evaporation and gas-liquid separation at 175 ℃ to obtain concentrated slurry with the mass concentration of 97.5%;
3) pre-polymerization: introducing the concentrated slurry into a No. 1 polymerization tank, heating and pre-polymerizing at 180 ℃ for 1.2h under the condition that the feeding amount is 25t/h, and obtaining I-grade polymerization slurry with the mass concentration of 98.5%;
4) and (3) repolymerization: when the liquid level of the I-grade polymerization slurry is full, overflowing to a No. 2 polymerization tank, adding medium trace elements with the mass fraction of 1.88% (magnesium oxide, zinc sulfate monohydrate and boric acid with the mass ratio of 0.06: 1.7: 0.12), heating and repolymerizing at 183 ℃ for 1.2h to obtain II-grade polymerization slurry with the mass concentration of 99.3%;
5) and (3) carrying out double-shaft granulation and drying on the II-grade polymerization slurry, and screening by using a screen with the size of 2.0-4.0 mm to obtain the polyphosphate synergistic nitrophosphate fertilizer.
Example 2:
on the basis of the embodiment 1, the temperature of evaporation and concentration in the step 2) is changed to 165 ℃, and the polyphosphate synergistic nitrophosphate fertilizer is prepared.
Example 3:
on the basis of example 1, the feeding amount of the concentrated slurry in the step 3) to the polymerization tank No. 1 is changed to be 29t/h, so that the polyphosphate phosphate enhanced nitrophosphate fertilizer is prepared.
Example 4:
on the basis of the example 1, the temperature of the prepolymerization reaction in the step 3) is changed to 175 ℃, and the polyphosphate phosphate synergistic nitrophosphate fertilizer is prepared.
Example 5:
on the basis of example 1, the time of the prepolymerization reaction in the step 3) is changed to 0.95h, so that the polyphosphate phosphate synergistic nitrophosphate fertilizer is prepared.
Example 6:
on the basis of the embodiment 1, the temperature of the repolymerization reaction in the step 4) is changed to 180 ℃, and the polyphosphate synergistic nitrophosphate fertilizer is prepared.
Example 7:
on the basis of the example 1, the time of repolymerization reaction in the step 4) is changed to 1.1h, and the polyphosphate phosphate synergistic nitrophosphate fertilizer is prepared.
Example 8:
on the basis of the embodiment 1, the addition amount of the trace elements in the step 4) is changed to 0.9% (the mass ratio of magnesium oxide, zinc sulfate monohydrate and boric acid is 0.03: 0.8: 0.06), and the polyphosphate phosphate synergistic nitrophosphate fertilizer is prepared.
The specific process parameters for each section of examples 1-8 are combined and shown in Table 2.
TABLE 2 detailed process parameters of each section of different examples
Comparative example 1:
different from the embodiment 1, the temperature of the evaporation concentration in the step 2) is changed to 125 ℃ in the comparative example 1, and the finished product of the nitrophosphate fertilizer is prepared.
Comparative example 2:
different from the example 1, the comparative example 2 adopts a one-stage prepolymerization reaction, only the polymerization tank No. 1 is opened, and the polymerization tank No. 2 is closed, so that the finished product of the nitrophosphate fertilizer is prepared.
Comparative example 3:
different from the embodiment 1, in the comparative example 3, the temperature of the prepolymerization in the step 3) is changed to 162 ℃, and the reaction time is changed to 0.8h, so that the finished product of the nitrophosphate fertilizer is prepared.
Comparative example 4:
different from the embodiment 1, the comparative example 4 changes the temperature of the repolymerization reaction in the step 4) to 165 ℃ and the reaction time to 0.8h, and a finished product of the nitrophosphate fertilizer is prepared.
Comparative example 5:
different from the embodiment 1, the comparison example 5 changes the adding amount of the trace element salt in the step 4) to 0, and the finished product of the nitrophosphate fertilizer is prepared.
The samples of examples 1 to 8 and comparative examples 1 to 5 were subjected to the composition detection analysis, and the results thereof are shown in Table 3:
TABLE 3 indexes of detection of samples of examples and comparative examples
As can be seen from Table 3, the polymerization rate of the nitrophosphate fertilizer is about 15%, compared with the comparative example, the content of water-insoluble substances is lower than 1%, and the solubility is better.
The beneficial effects of the invention are further illustrated below in conjunction with field test data:
the field test is detailed as follows:
test work: shanghai Qing tea
Test site: guangdong Huizhou red loam
Test time: 2019.10-2019.12
Fertilizer to be tested: polyphosphate synergized nitrophosphate fertilizers (examples 1-8), nitrophosphate fertilizers (comparative examples 1-5).
Planting Shanghai Qing by cell test, setting 13 treatments, repeating each treatment 3 times, and setting 39 cells with cell area of 1.2m × 5m ═ 6m2The row spacing is 15cm multiplied by 10cm, each hole is 3-5 plants, the fertilizing amount of each treatment is as follows, the fertilizing mode is uniform spreading, and the field management of other districts is consistent.
TABLE 4 Experimental treatments for fertilization details
The test effect is as follows:
TABLE 5 Effect of treatments on the yield of Shanghai green
As can be seen from Table 5, the respective treatment yields were example 1, example 2, example 3, example 6, example 4, example 5, example 7, example 8, comparative example 1, comparative example 5, comparative example 3, comparative example 4, and comparative example 2 in this order from high to low.
Among 8 examples, example 1 had the highest yield and was significantly different from the other treatments; the yield difference of the examples 2 to 7 is small, while the yield of the example 8 is obviously reduced, which shows that the yield increasing effect is better when the addition amount of the medium trace element is 1.88%.
The yield difference of the embodiments 1 to 8 is obvious compared with the comparative examples 1 to 5, which shows that the polyphosphate synergistic nitrophosphate fertilizer prepared by the method has a better effect of improving the yield of Shanghai Qing.
TABLE 6 influence of the treatments on the quality index of Shanghai Qing
As can be seen from table 6, the soluble sugar and soluble protein content of shanghai green of example 1 were highest in all treatments; the yield difference of the examples 2 to 7 is small, and the two quality indexes of the example 8 are obviously reduced, which shows that the quality index of the Shanghai Qing has better synergistic effect when the addition amount of the medium trace element is 1.88%.
The content of soluble sugar and soluble protein in the embodiments 1 to 8 is higher than that in the comparative examples 1 to 5, which shows that the polyphosphate synergistic nitrophosphate fertilizer prepared by the method can better improve the quality of Shanghai Qing.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (9)
1. A preparation method of a polyphosphate synergistic nitrophosphate fertilizer is characterized by comprising the following steps:
preparing a neutralization solution;
pumping the neutralized liquid into a concentration system, and carrying out preheating, evaporation and gas-liquid separation at 135-175 ℃ to obtain concentrated slurry;
introducing the concentrated slurry into a No. 1 polymerization tank, and carrying out prepolymerization at the temperature of 175-185 ℃ to obtain I-grade polymerization slurry;
overflowing the I-grade polymerization slurry to a No. 2 polymerization tank when the liquid level of the I-grade polymerization slurry is full, adding medium trace elements, and carrying out repolymerization at the temperature of 180-185 ℃ to obtain II-grade polymerization slurry;
and granulating, drying and screening the II-grade polymerization slurry to obtain the polyphosphate synergistic nitrophosphate fertilizer.
2. The method of claim 1, wherein the preparation of the neutralization solution comprises the steps of: (1) decomposing phosphorite with nitric acid to obtain acidolysis solution; (2) freezing and crystallizing, and filtering with calcium nitrate; (3) and (4) neutralizing the mother liquor with ammonia to obtain a neutralized solution.
3. The method according to claim 1, wherein the concentrated slurry has a mass concentration of 80 to 97.5%.
4. The preparation method according to claim 1, wherein the concentrated slurry is introduced into a No. 1 polymerization tank at a rate of 15-30 t/h, and the feed extends from the top to the bottom of the tank; the prepolymerization reaction time is 0.9-1.4 h, and the mass concentration of the obtained I-grade polymerization slurry is 98-99%.
5. The preparation method according to claim 1, wherein the repolymerization time is 0.9-1.4 h, and the mass concentration of the obtained II-grade polymerization slurry is 98.5-99.5%.
6. The method of claim 1, wherein the medium trace element is a combination of one or more of magnesium oxide, zinc sulfate, manganese sulfate, boric acid, ferrous sulfate, and copper sulfate.
7. The method according to claim 1, wherein the medium trace element accounts for 0.1-2.0% of the mass of the II-grade polymer slurry.
8. The method according to claim 1, wherein the granulation method is at least one of biaxial granulation, drum granulation, spray granulation, high tower granulation, atomization granulation, and disk granulation.
9. The method according to claim 8, wherein the slurry-spraying granulation is carried out by using a device integrating granulation, polishing, drying and conveying.
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Application publication date: 20210611 |