CN112320777A - Production method of 66% powdered MAP - Google Patents
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- CN112320777A CN112320777A CN202011282111.8A CN202011282111A CN112320777A CN 112320777 A CN112320777 A CN 112320777A CN 202011282111 A CN202011282111 A CN 202011282111A CN 112320777 A CN112320777 A CN 112320777A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/28—Ammonium phosphates
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/82—Compositional purity water content
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Abstract
The invention belongs to the technical field of monoammonium phosphate production, and particularly relates to a production method of 66% powdery MAP, which comprises the following steps: 1) settling; 2) performing filter pressing; 3) pre-washing and neutralizing; 4) ammoniation; 5) concentrating; 6) the method has simple steps and easy control, and can realize the production of high-concentration and high-water-solubility monoammonium phosphate products.
Description
Technical Field
The invention belongs to the technical field of monoammonium phosphate production, and particularly relates to a production method of 66% powdery MAP.
Background
The industrial monoammonium phosphate is widely applied to flame retardants, fire extinguishing agents, flame retardants for textiles, dispersants for paper making and other industries, fire-proof coatings, additives for wood products and enameling glaze agents, can also be applied to printing industry, medicine industry, feed additives and high-grade fertilizers, and can also be used as yeast nutrients, dough conditioners, leavening agents, nutrition enhancers, fermentation aids and the like in food industry.
At present, because the thermal phosphoric acid has the defects of large energy consumption and high production cost, the wet phosphoric acid is basically adopted to produce the monoammonium phosphate; the steps for producing monoammonium phosphate by using wet-process phosphoric acid as a raw material are generally as follows: the method comprises the following steps of wet-process phosphoric acid purification, ammonia neutralization, separation, concentration, crystallization and drying, wherein insoluble substances filtered in the production process are used for producing nitrogen phosphorus fertilizers or agricultural monoammonium phosphate products, so that product diversification and production process continuity are basically realized, but the following problems are specifically existed in the process of producing industrial monoammonium phosphate by wet-process phosphoric acid: 1) because the impurity content in the wet-process phosphoric acid is far higher than that of the hot-process phosphoric acid, the viscosity of the slurry is greatly changed in the ammonia neutralization process under different pH conditions, and the slurry is not beneficial to conveying and filtering; meanwhile, Fe, Ca, Mg, Al and SiO in wet-process phosphoric acid2、SO4 2-Impurities such as F and the like can generate MgNH in the ammonia neutralization process4PO4·6H2O、(FeAl)NH4(HPO4)2·0.5H2O、CaHPO4And (NH4)2SiF6And the like, thereby affecting the content of available phosphorus and water-soluble phosphorus in the product and causing the quality reduction of the product; 2) warp pre-treatmentAfter purification treatment, partial Mg still remains in the wet-process phosphoric acid2+Without removal, insoluble magnesium ammonium phosphate (MgNH) is formed during ammonia neutralization4PO4·6H2O), magnesium ammonium phosphate is more difficult to filter and separate than other products, which not only seriously affects the production operation, but also can be crystallized into the product, and is one of the reasons for the unqualified quality of the industrial grade monoammonium phosphate product.
Therefore, at present in competition for incandescence in the ammonium phosphate market, the concentration of powdery monoammonium phosphate is 55% -60% and water-soluble phosphorus accounts for 86% -90%, which no longer meets the market demand, and the improvement of the concentration and water solubility of monoammonium phosphate is the key of product upgrading, so that the research on a monoammonium phosphate product with high concentration (more than 66%) and high water solubility (more than 93% of water-soluble phosphorus and less than 6%) is of great importance.
Disclosure of Invention
The invention provides a production method of 66% powdered MAP aiming at the defects of the prior art.
The method is realized by the following technical scheme:
a method for producing 66% powdered MAP, comprising the steps of:
1) and (3) settling: concentrating wet phosphoric acid to obtain concentrated phosphoric acid, and naturally settling the concentrated phosphoric acid to a temperature of less than 40 ℃;
2) and (3) filter pressing: taking the settled supernatant, performing filter pressing by using a plate-and-frame filter press, and separating filter residues;
3) pre-washing neutralization: feeding the concentrated phosphoric acid obtained by filter pressing separation into a granulator pre-washer through a concentrated phosphoric acid storage tank, adjusting the pH value of washing slurry obtained by the granulator pre-washer by controlling the addition amount of phosphoric acid in the granulator pre-washer, passing the washing slurry through a dryer washer to obtain ammonium phosphate slurry, controlling the temperature to be 60-80 ℃, the specific gravity to be 1.5-1.6 and the solid content to be 8-12%, and then carrying out filter pressing treatment on the ammonium phosphate slurry through a plate and frame filter press to separate filter residues;
4) ammoniation: feeding the ammonium phosphate slurry obtained by filter pressing into an ammoniation reactor, and carrying out neutralization reaction with gas ammonia, wherein the neutralization degree is controlled to be 0.98-1.03;
5) concentration: double-effect concentration by countercurrent feeding is adopted, and the water content of the slurry is adjusted to 25-30%;
6) and (3) drying: and (3) delivering the concentrated slurry into a nozzle of a drying tower by a high-pressure pump, carrying out countercurrent drying with 120-plus 135 ℃ hot air, overflowing from an overflow port at the bottom of the drying tower, conveying into a belt conveyor, conveying into a bulk cargo warehouse, washing tail gas generated by the drying tower with water in a washing system after gravity settling and dust removal, and emptying, wherein the washing liquid returns to the system for digestion.
The specific gravity of the settled supernatant is 1.60-1.68.
In the step 2), the concentrated phosphoric acid obtained by filter-pressing separation has the acid concentration of P2O5Calculated as 49-50%.
The granulator prewasher has the following process requirements: the specific gravity of the granulating washing liquid is 1.45-1.50, and the neutralization degree of the prewashing is less than or equal to 0.65.
The process requirement of the dryer scrubber is as follows: the specific gravity of the dry washing liquid is 1.30-1.45, and the washing neutralization degree is less than or equal to 0.3.
The granulating or drying washing liquid, P2O5The content is 39% -42%.
The pressure of the high-pressure pump is 4-8 MPa.
And (3) feeding the filter residue into a settling residue acid storage tank, mixing and stirring the filter residue obtained by filter pressing and the settling residue obtained in the step 1), and feeding the mixture into a 57% ammonium phosphate device or a slurry-method ammonium device or other ammonium phosphate devices by a pump to adjust nutrients for subsequent use.
The invention naturally settles concentrated phosphoric acid to separate out a large amount of solid precipitate (namely the settled slag), and analyzes the chemical composition of the settled slag, wherein elements from phosphorite comprise Fe, Al, F, Si, Ca, Mg, K and Na, and elements from the production process of wet-process phosphoric acid comprise phosphate radical and sulfate radical. But only 10 dissolved impurities (Fe)2+、Fe3+Al, Ca, Mg, Na, K, F, Si and SO4 2-) Plays an important role in the generated sediment, most solid phases in the sediment are acidic phosphates of iron and aluminum, most commonly (Fe, Al)3KH14(PO4)8·4H2O,(Fe,Al)3KH14(PO4)8·4H2The O compound begins to precipitate in the concentration stage and finally becomes the main component of the sediment when the phosphoric acid is 35 to 60 percent P2O5Its solubility is minimal and increases slightly with increasing temperature. When the wet-process phosphoric acid is concentrated to P2O5The content is more than 45 percent, and simultaneously, when the acid temperature is reduced to about 40 ℃, a large amount of phosphogypsum and metal compounds in the acid can be separated out, so that the application realizes the separation and removal of phosphogypsum and metal ion compound solid materials in wet-process phosphoric acid by controlling the termination temperature of sedimentation and filter pressing, which is beneficial to improving the product nutrient and water-soluble phosphorus content.
Meanwhile, the method aims to solve the problem that wet-process phosphoric acid produced by a dihydrate method contains a large amount of impurities such as Mg2+、Ca2+、Fe3+、Al3+、SO4 2-And SiF6 2These impurities, during the neutralization reaction of wet-process phosphoric acid with ammonia, give rise to complex compounds which seriously affect the viscosity of the slurry and the composition, properties and P of the ammonium phosphate product2O5The solubility and the like, a part of concentrated phosphoric acid obtained by filter pressing separation is pre-washed and neutralized, the neutralization degree is controlled to be less than or equal to 0.65, and ammonium phosphate slurry generates a certain amount of (Fe, Al) NH under the condition4(HPO4)2·0.5H2O、(Fe,Al)Mg(NH4)2(HPO4)2F3When the pH value of the complex is between 4.3 and 5.6, a magnesium-containing complex is formed and is dissolved in a neutral citrate solution, so that the washing effect is met, the ammonium phosphate slurry entering the reverse tank of the pipe is ensured to have better fluidity, and the blockage of a washing system and the reverse tank of the pipe is avoided; if the pH value of the washing slurry is more than 6, citric insoluble substances are generated, and silica gel can be formed in the neutralization process due to silicon dissolved in acid; if the pH of the washing slurry is less than 4, the yield of nitrogen elements is low, so that the total nitrogen in the monoammonium phosphate cannot meet the standard requirement.
The invention changes the pH value of the washing slurry by adjusting the addition of phosphoric acid in the pre-washing device of the granulator, combines the characteristics of the slurry, and selects and controls a proper pH value index to fully separate out metal cations so as to improve the nutrient and water-soluble phosphorus content of ammonium phosphate products.
The invention controls the ammoniation neutralization degree to be between 0.98 and 1.03, and NH of the phosphoric acid ammoniation solution3The partial pressure is small.
In order to save the steam consumption, the invention adopts a double-effect concentration process of countercurrent feeding, wherein the first effect is to realize normal-pressure concentration by using fresh steam as a heater heat source, the second effect is to realize vacuum concentration by using evaporated steam of the first effect as a heater heat source, and the vacuum degree of the second effect is generated by adding cooling water into a mixing condenser and condensing the steam of the second effect.
The invention controls the process pressure of the high-pressure pump to be 4-8MPa, so that the ammonium phosphate slurry can be atomized under high pressure in the conveying process, and is favorable for being sprayed into the drying tower.
Has the advantages that:
the method has simple steps and easy control, can realize the production of the high-concentration and high-water-solubility monoammonium phosphate product, and the obtained product has the following nutrients: the concentration is 66% (11.5% N-54.5% P)2O5-0K2O), the water content is less than 2.5 percent, and the phosphorus content of the water-soluble phosphorus is more than or equal to 95 percent.
Detailed Description
The following is a detailed description of the embodiments of the present invention, but the present invention is not limited to these embodiments, and any modifications or substitutions in the basic spirit of the embodiments are included in the scope of the present invention as claimed in the claims.
Example 1
A method for producing 66% powdered MAP, comprising the steps of:
1) and (3) settling: concentrating wet phosphoric acid to obtain concentrated phosphoric acid, and naturally settling the concentrated phosphoric acid to a temperature of less than 40 ℃;
2) and (3) filter pressing: taking the settled supernatant, performing filter pressing by using a plate-and-frame filter press, and separating filter residues;
3) pre-washing neutralization: feeding the concentrated phosphoric acid obtained by filter pressing separation into a granulator pre-washer through a concentrated phosphoric acid storage tank, adjusting the pH value of washing slurry obtained by the granulator pre-washer by controlling the addition amount of phosphoric acid in the granulator pre-washer, passing the washing slurry through a dryer washer to obtain ammonium phosphate slurry, controlling the temperature to be 80 ℃, the specific gravity to be 1.6 and the solid content to be 12%, and then carrying out filter pressing treatment on the ammonium phosphate slurry through a plate and frame filter press to separate filter residues;
4) ammoniation: feeding the ammonium phosphate slurry obtained by filter pressing into an ammoniation reactor, and carrying out neutralization reaction with gas ammonia, wherein the neutralization degree is controlled to be 1.03;
5) concentration: double-effect concentration is carried out by adopting counter-current feeding, and the water content of the slurry is adjusted to 30%;
6) and (3) drying: sending the concentrated slurry into a nozzle of a drying tower by a high-pressure pump, carrying out countercurrent drying with hot air at 135 ℃, overflowing from an overflow port at the bottom of the drying tower, conveying the overflow into a belt conveyor to a bulk cargo warehouse, carrying out gravity settling dust removal on tail gas generated by the drying tower, then sending the tail gas into a washing system to be washed by water, and then emptying, and returning the washing liquid to a system for digestion;
the specific gravity of the settled supernatant is 1.68;
in the step 2), the concentrated phosphoric acid obtained by filter-pressing separation has the acid concentration of P2O5Calculated as 50%;
the granulator prewasher has the following process requirements: the specific gravity of the granulation washing liquid is as follows; 1.50, the degree of neutralization in prewashing is 0.65;
the process requirement of the dryer scrubber is as follows: the specific gravity of the dry washing liquid is 1.45, and the washing neutralization degree is 0.3;
the granulating or drying washing liquid, P2O5The content is 42%;
the pressure of the high-pressure pump is 8 MPa;
and (3) feeding the filter residue into a settling residue acid storage tank, mixing and stirring the filter residue obtained by filter pressing and the settling residue obtained in the step 1), and feeding the mixture into a 57% ammonium phosphate device or a slurry-method ammonium device or other ammonium phosphate devices by a pump to adjust nutrients for subsequent use.
Example 2
A method for producing 66% powdered MAP, comprising the steps of:
1) and (3) settling: concentrating wet phosphoric acid to obtain concentrated phosphoric acid, and naturally settling the concentrated phosphoric acid to a temperature of less than 40 ℃;
2) and (3) filter pressing: taking the settled supernatant, performing filter pressing by using a plate-and-frame filter press, and separating filter residues;
3) pre-washing neutralization: feeding the concentrated phosphoric acid obtained by filter pressing separation into a granulator pre-washer through a concentrated phosphoric acid storage tank, adjusting the pH value of washing slurry obtained by the granulator pre-washer by controlling the addition amount of phosphoric acid in the granulator pre-washer, passing the washing slurry through a dryer washer to obtain ammonium phosphate slurry, controlling the temperature to be 60 ℃, the specific gravity to be 1.5 and the solid content to be 8%, and then carrying out filter pressing treatment on the ammonium phosphate slurry through a plate and frame filter press to separate filter residues;
4) ammoniation: feeding the ammonium phosphate slurry obtained by filter pressing into an ammoniation reactor, and carrying out neutralization reaction with gas ammonia, wherein the neutralization degree is controlled to be 0.98;
5) concentration: double-effect concentration is carried out by adopting counter-current feeding, and the water content of the slurry is adjusted to 25%;
6) and (3) drying: sending the concentrated slurry into a nozzle of a drying tower by a high-pressure pump, carrying out countercurrent drying with hot air at 120 ℃, overflowing from an overflow port at the bottom of the drying tower, conveying to a bulk cargo warehouse by a belt conveyor, washing tail gas generated by the drying tower with water in a washing system after gravity settling and dust removal, and emptying, wherein the washing liquid returns to the system for digestion;
the specific gravity of the settled supernatant is 1.60;
in the step 2), the concentrated phosphoric acid obtained by filter-pressing separation has the acid concentration of P2O5Calculated as 49 percent;
the granulator prewasher has the following process requirements: the specific gravity of the granulation washing liquid is 1.45, and the neutralization degree of the pre-washing is 0.45;
the process requirement of the dryer scrubber is as follows: the specific gravity of the dry washing liquid is 1.30, and the washing neutralization degree is 0.1;
the granulating or drying washing liquid, P2O5The content is 39%;
the pressure of the high-pressure pump is 4 MPa.
And (3) feeding the filter residue into a settling residue acid storage tank, mixing and stirring the filter residue obtained by filter pressing and the settling residue obtained in the step 1), and feeding the mixture into a 57% ammonium phosphate device or a slurry-method ammonium device or other ammonium phosphate devices by a pump to adjust nutrients for subsequent use.
Example 3
A method for producing 66% powdered MAP, comprising the steps of:
1) and (3) settling: concentrating wet phosphoric acid to obtain concentrated phosphoric acid, and naturally settling the concentrated phosphoric acid to a temperature of less than 40 ℃;
2) and (3) filter pressing: taking the settled supernatant, performing filter pressing by using a plate-and-frame filter press, and separating filter residues;
3) pre-washing neutralization: feeding the concentrated phosphoric acid obtained by filter pressing separation into a granulator pre-washer through a concentrated phosphoric acid storage tank, adjusting the pH value of washing slurry obtained by the granulator pre-washer by controlling the addition amount of phosphoric acid in the granulator pre-washer, passing the washing slurry through a dryer washer to obtain ammonium phosphate slurry, controlling the temperature to be 70 ℃, the specific gravity to be 1.55 and the solid content to be 10%, and then carrying out filter pressing treatment on the ammonium phosphate slurry through a plate and frame filter press to separate filter residues;
4) ammoniation: feeding the ammonium phosphate slurry obtained by filter pressing into an ammoniation reactor, and carrying out neutralization reaction with gas ammonia, wherein the neutralization degree is controlled to be 1.0;
5) concentration: double-effect concentration is carried out by adopting counter-current feeding, and the water content of the slurry is adjusted to 28%;
6) and (3) drying: sending the concentrated slurry into a nozzle of a drying tower by a high-pressure pump, carrying out countercurrent drying with hot air at 128 ℃, overflowing from an overflow port at the bottom of the drying tower, conveying to a bulk cargo warehouse by a belt conveyor, washing tail gas generated by the drying tower with water in a washing system after gravity settling and dust removal, and emptying, wherein the washing liquid returns to the system for digestion;
the specific gravity of the settled supernatant is 1.65;
in the step 2), the concentrated phosphoric acid obtained by filter-pressing separation has the acid concentration of P2O5Calculated as 49.5%;
the granulator prewasher has the following process requirements: the specific gravity of the granulation washing liquid is 1.48, and the neutralization degree of the pre-washing is 0.60;
the process requirement of the dryer scrubber is as follows: the specific gravity of the dry washing liquid is 1.40, and the washing neutralization degree is 0.2;
the granulating or drying washing liquid, P2O5The content is 40 percent;
the pressure of the high-pressure pump is 5 MPa;
and (3) feeding the filter residue into a settling residue acid storage tank, mixing and stirring the filter residue obtained by filter pressing and the settling residue obtained in the step 1), and feeding the mixture into a 57% ammonium phosphate device or a slurry-method ammonium device or other ammonium phosphate devices by a pump to adjust nutrients for subsequent use.
Wherein, the nutrients of the monoammonium phosphate products of examples 1-3 are shown in Table 1;
TABLE 1
Item | Concentration of | Components | Water soluble phosphorus content | Moisture content |
Example 1 | 66% | 11.5%N-54.5%P2O5-0K2O | 96.4% | 2.4% |
Example 2 | 66% | 11.5%N-54.5%P2O5-0K2O | 95.7% | 2.0% |
Example 3 | 66% | 11.5%N-54.5%P2O5-0K2O | 96.6% | 2.1% |
Claims (9)
1. A method for producing 66% powdered MAP, comprising the steps of:
1) and (3) settling: concentrating wet phosphoric acid to obtain concentrated phosphoric acid, and naturally settling the concentrated phosphoric acid to a temperature of less than 40 ℃;
2) and (3) filter pressing: taking the settled supernatant, performing filter pressing by using a plate-and-frame filter press, and separating filter residues;
3) pre-washing neutralization: feeding the concentrated phosphoric acid obtained by filter pressing separation into a granulator pre-washer through a concentrated phosphoric acid storage tank, adjusting the pH value of washing slurry obtained by the granulator pre-washer by controlling the addition amount of phosphoric acid in the granulator pre-washer, passing the washing slurry through a dryer washer to obtain ammonium phosphate slurry, controlling the temperature to be 60-80 ℃, the specific gravity to be 1.5-1.6 and the solid content to be 8-12%, and then carrying out filter pressing treatment on the ammonium phosphate slurry through a plate and frame filter press to separate filter residues;
4) ammoniation: feeding the ammonium phosphate slurry obtained by filter pressing into an ammoniation reactor, and carrying out neutralization reaction with gas ammonia, wherein the neutralization degree is controlled to be 0.98-1.03;
5) concentration: double-effect concentration by countercurrent feeding is adopted, and the water content of the slurry is adjusted to 25-30%;
6) and (3) drying: and (3) delivering the concentrated slurry into a nozzle of a drying tower by a high-pressure pump, carrying out countercurrent drying with 120-plus 135 ℃ hot air, overflowing from an overflow port at the bottom of the drying tower, conveying into a belt conveyor, conveying into a bulk cargo warehouse, washing tail gas generated by the drying tower with water in a washing system after gravity settling and dust removal, and emptying, wherein the washing liquid returns to the system for digestion.
2. The method of producing 66% powdered MAP according to claim 1 wherein the settled supernatant has a specific gravity of 1.60 to 1.68.
3. The process for producing 66% powdered MAP according to claim 1 wherein in step 2), the concentrated phosphoric acid obtained by pressure filtration separation has an acid concentration of P2O5Calculated as 49-50%.
4. The method of producing 66% powdered MAP as claimed in claim 1, wherein the granulator prewasher has the process requirements: the specific gravity of the granulating washing liquid is 1.45-1.50, and the neutralization degree of the prewashing is less than or equal to 0.65.
5. The method of claim 1 for producing 66% powdered MAP, wherein the desiccant scrubber has process requirements: the specific gravity of the dry washing liquid is 1.30-1.45, and the washing neutralization degree is less than or equal to 0.3.
6. Process for the production of 66% powdered MAP according to claim 1 wherein the granulation wash or the drying wash, P, is2O5The content is 39% -42%.
7. The method of producing 66% powdered MAP as claimed in claim 1 wherein the high pressure pump is at a pressure of 4 to 8 MPa.
8. The method of claim 1 for producing 66% powdered MAP wherein the countercurrent feed double effect concentration is achieved by atmospheric concentration using live steam as the heater heat source and by vacuum concentration using evaporative steam as the heater heat source.
9. The method of claim 8 wherein the 66% powdered MAP is produced by condensing a secondary effect of steam by adding cooling water to the mixing condenser.
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CN113501509A (en) * | 2021-08-19 | 2021-10-15 | 云南云天化红磷化工有限公司 | System and method for preparing 66% powdery monoammonium phosphate by one-step method |
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CN104229764A (en) * | 2014-09-01 | 2014-12-24 | 云南云天化国际化工有限公司 | Method for continuously producing water-soluble monoammonium phosphate by using wet-process phosphoric acid |
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CN104229764A (en) * | 2014-09-01 | 2014-12-24 | 云南云天化国际化工有限公司 | Method for continuously producing water-soluble monoammonium phosphate by using wet-process phosphoric acid |
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CN113501509A (en) * | 2021-08-19 | 2021-10-15 | 云南云天化红磷化工有限公司 | System and method for preparing 66% powdery monoammonium phosphate by one-step method |
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