CN116812889A - Production method of amorphous potassium dihydrogen phosphate with adjustable bulk density - Google Patents

Production method of amorphous potassium dihydrogen phosphate with adjustable bulk density Download PDF

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Publication number
CN116812889A
CN116812889A CN202310858407.7A CN202310858407A CN116812889A CN 116812889 A CN116812889 A CN 116812889A CN 202310858407 A CN202310858407 A CN 202310858407A CN 116812889 A CN116812889 A CN 116812889A
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potassium dihydrogen
dihydrogen phosphate
bulk density
feed liquid
amorphous
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黄海周
王莉莉
邓燕清
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Guangxi Donglin Food And Chemical Co ltd
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Guangxi Donglin Food And Chemical Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/16Oxyacids of phosphorus; Salts thereof
    • C01B25/26Phosphates
    • C01B25/30Alkali metal phosphates
    • C01B25/308Methods for converting an alkali metal orthophosphate into another one; Purification; Decolorasing; Dehydrating; Drying
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/10Solid density

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)

Abstract

The invention discloses a production method of amorphous potassium dihydrogen phosphate with adjustable bulk density, which comprises the following steps: s1, material liquid adjustment: adding 0.1-5wt% of carboxylic acid or carboxylate into the potassium dihydrogen phosphate feed liquid, and adjusting the dry matter content of the potassium dihydrogen phosphate in the feed liquid to 10-65wt%; s2, atomizing: atomizing the feed liquid obtained in the step S1; s3, drying: and (3) carrying out hot air drying on the feed liquid atomized in the step (S2) to obtain amorphous potassium dihydrogen phosphate. The monopotassium phosphate prepared by the invention exists in an amorphous form, the specific surface area is more than 5 times of that of the common crystalline monopotassium phosphate, and the dissolution speed is high. The invention can also adjust the bulk density of amorphous potassium dihydrogen phosphate, solves the problem of dissolving speed of potassium dihydrogen phosphate, and simultaneously ensures that the product has better commodity.

Description

Production method of amorphous potassium dihydrogen phosphate with adjustable bulk density
Technical Field
The invention relates to the technical field of fertilizer preparation, in particular to a production method of amorphous potassium dihydrogen phosphate with adjustable bulk density.
Background
Monopotassium phosphate is an elemental fertilizer which is very widely used in agriculture. The salt index of the fertilizer is far lower than that of high-potassium simple substance fertilizers such as potassium sulfate, potassium chloride and the like, the damage to tender leaves of crops during leaf spraying is small, and the fertilizer has extremely high safety. Is often used for foliar fertilization of commercial crops such as fruit trees, vegetables and the like. In addition, the pesticide has synergistic effect with some pesticides, so the pesticide is deeply favored by vast farmers.
Most of the commercially available potassium dihydrogen phosphate is crystalline particles or powder, and it is known from the data that the solubility in water at 20℃is 22.6g/100g of water. The solubility of the crystal is small, the specific surface area of the added crystal is small, and the dissolution speed of the crystal in water is low. Before use, the mixture is stirred vigorously for a long time to dissolve the mixture into a uniform solution, so that the solution is saturated with the user's scale.
Solubility is a physical property of a substance that cannot be altered artificially. In order to increase the dissolution rate of potassium dihydrogen phosphate, it is only possible to increase the specific surface area of the crystal. It is common practice to mechanically grind potassium dihydrogen phosphate crystals into ultra-fine powder of 200 mesh or more to increase the specific surface area. Because the particles of the target finished product are very fine, the common crushing and screening method cannot meet the requirements at all. The superfine powder with the size can be obtained by carrying out fine grinding and air separation for a plurality of times. The process has the advantages of expensive mechanical equipment, low production efficiency, high energy consumption and much higher product cost than crystalline potassium dihydrogen phosphate. The ultrafine powder obtained by mechanical grinding is crystalline in nature, but has smaller particles and a bulk density comparable to that of the crystalline product (generally greater than 1.0g/cm 3 ) And the bulk density is difficult to regulate and control, so that the commodity performance of the product is poor. Therefore, how to prepare amorphous potassium dihydrogen phosphate, which solves the problem of the dissolution rate of potassium dihydrogen phosphate and simultaneously ensures that the product has better commodity is a difficult problem in the prior potassium dihydrogen phosphate production industry.
Disclosure of Invention
The invention solves the technical problems that most of the existing commercial potassium dihydrogen phosphate is crystalline particles or powder, the solubility is small, the dissolution rate is low, the bulk density of the superfine potassium dihydrogen phosphate is difficult to regulate and control, the commodity of the product is poor, and the dissolution rate and the commodity are difficult to have.
In order to solve the problems, the invention adopts the following technical scheme:
a production method of amorphous potassium dihydrogen phosphate with adjustable bulk density comprises the following steps:
s1, material liquid adjustment: adding 0.1-5wt% of carboxylic acid or carboxylate into the potassium dihydrogen phosphate feed liquid, and adjusting the dry matter content of the potassium dihydrogen phosphate in the feed liquid to 10-65wt%;
s2, atomizing: atomizing the feed liquid obtained in the step S1;
s3, drying: and (3) carrying out hot air drying on the feed liquid atomized in the step (S2) to obtain amorphous potassium dihydrogen phosphate.
Further, the carboxylic acid is an organic matter containing a-COOH group; the carboxylate contains-COO - Organic matter of the group.
Further, the carboxylic acid is preferably one or more of acetic acid, propionic acid, oxalic acid, benzoic acid, citric acid and lactic acid; the carboxylate is preferably one or more of acetic acid, propionic acid, oxalic acid, benzoic acid, citric acid and lactic acid.
Furthermore, the atomization is realized by adopting one of high-speed centrifugal atomization, high-pressure jet atomization and high-speed airflow atomization.
In S2, the diameter of the fogdrop formed after the feed liquid is atomized is 22-112 mu m. In the present invention, the diameter of the fog drop is shown as formula d p =16.56d 0 1.52 G L -0.44 σ 0.71 μ L -0.16 (d p Refers to the diameter of fog drop, μm, d 0 Atomizer aperture, mm, G L Mass flow, g/s, sigma surface tension, 10 -5 N/cm,μ L Viscosity, mpa.s).
In the step S3, the air inlet temperature of the hot air drying is 180-400 ℃, and the air outlet temperature is 100-200 ℃.
The invention also aims at protecting the potassium dihydrogen phosphate prepared by the production method of the amorphous potassium dihydrogen phosphate with adjustable bulk density; the monopotassium phosphate is amorphous monopotassium phosphate.
The bulk density of the potassium dihydrogen phosphate obtained by the preparation method is in the range of 0.5-0.9g/cm 3
Compared with the prior art, the invention has the following beneficial effects: potassium dihydrogen phosphate crystal belongs to tetragonal system, and the traditional production mainly comprises gradually saturating solute by evaporating water, forming small amount of potassium dihydrogen phosphate crystal nucleus in solution, and driving force for crystallizationUnder the action of the crystal grains with complete appearance are gradually formed. And (3) centrifugally separating mother liquor, and drying by airflow to obtain a crystal potassium dihydrogen phosphate product. Potassium dihydrogen phosphate crystals need to undergo both nucleation and crystal growth processes. The supersaturation degree of the feed liquid is reduced by controlling the dry matter content of the monopotassium phosphate in the feed liquid, so that the formation of crystal nuclei can be inhibited, and the crystals lack the necessary conditions for generation; in addition, the feed liquid is atomized into tiny fog drops with large specific surface area, and each tiny fog drop only contains trace potassium dihydrogen phosphate dry matter and moisture, so that the moisture in the fog drops is instantaneously evaporated through hot air flow, and the dry matter grows into amorphous potassium dihydrogen phosphate without enough time. On the other hand, a small amount of carboxylic acid or carboxylate is mixed into the potassium dihydrogen phosphate feed liquid, the carboxylic acid or carboxylate which is uniformly dispersed in the feed liquid can exist stably at normal temperature, in the high-temperature drying process, the carboxylic acid or carboxylate is heated and decomposed in situ to generate carbon dioxide, and carbon dioxide molecules are wrapped in the dried material to form tiny holes, so that the material becomes bulked, the bulk density of the material is reduced, and the commodity of the product is improved. Therefore, the invention can adjust the content of carboxylic acid or carboxylate in a certain range, and can adjust and control the bulk density of amorphous potassium dihydrogen phosphate to be 0.5-0.9g/cm 3 . The monopotassium phosphate prepared by the invention exists in an amorphous form, the specific surface area is more than 5 times of that of the common crystalline monopotassium phosphate (the result of comparison with the dissolution rate), and the dissolution rate is high; the invention can also adjust the bulk density of amorphous potassium dihydrogen phosphate, solves the problem of dissolving speed of potassium dihydrogen phosphate, and simultaneously ensures that the product has better commodity.
Detailed Description
The invention is further illustrated by the following examples and experiments.
Example 1
A production method of amorphous potassium dihydrogen phosphate with adjustable bulk density comprises the following steps:
s1, material liquid adjustment: adding 0.1wt% of acetic acid into the potassium dihydrogen phosphate feed liquid, and adjusting the dry matter content of the potassium dihydrogen phosphate in the feed liquid to 10wt%;
s2, atomizing: atomizing the feed liquid obtained in the step S1 into mist drops with the diameter of 22 mu m by adopting high-speed centrifugal atomization;
s3, drying: and (3) carrying out hot air drying on the feed liquid atomized in the step S2 under the condition that the air inlet temperature is 180 ℃ and the air outlet temperature is 100 ℃ to obtain amorphous potassium dihydrogen phosphate.
Example 2
A production method of amorphous potassium dihydrogen phosphate with adjustable bulk density comprises the following steps:
s1, material liquid adjustment: adding 5wt% of propionic acid into the monopotassium phosphate feed liquid, and adjusting the dry matter content of the monopotassium phosphate in the feed liquid to 65wt%;
s2, atomizing: atomizing the feed liquid obtained in the step S1 into mist drops with the diameter of 112 mu m by adopting high-pressure jet atomization;
s3, drying: and (3) carrying out hot air drying on the feed liquid atomized in the step S2 under the condition that the air inlet temperature is 400 ℃ and the air outlet temperature is 200 ℃ to obtain amorphous potassium dihydrogen phosphate.
Example 3
A production method of amorphous potassium dihydrogen phosphate with adjustable bulk density comprises the following steps:
s1, material liquid adjustment: adding 3wt% of potassium acetate into the potassium dihydrogen phosphate feed liquid, and adjusting the dry matter content of the potassium dihydrogen phosphate in the feed liquid to 30wt%;
s2, atomizing: atomizing the feed liquid obtained in the step S1 into mist drops with the diameter of 110 mu m by adopting high-speed airflow atomization;
s3, drying: and (3) carrying out hot air drying on the feed liquid atomized in the step S2 under the condition that the air inlet temperature is 200 ℃ and the air outlet temperature is 150 ℃ to obtain amorphous potassium dihydrogen phosphate.
Example 4
A production method of amorphous potassium dihydrogen phosphate with adjustable bulk density comprises the following steps:
s1, material liquid adjustment: adding 1wt% of citric acid into the potassium dihydrogen phosphate feed liquid, and adjusting the dry matter content of the potassium dihydrogen phosphate in the feed liquid to 45wt%;
s2, atomizing: atomizing the feed liquid obtained in the step S1 into mist drops with the diameter of 80 mu m by adopting high-pressure jet atomization;
s3, drying: and (3) carrying out hot air drying on the feed liquid atomized in the step S2 under the condition that the air inlet temperature is 300 ℃ and the air outlet temperature is 120 ℃ to obtain amorphous potassium dihydrogen phosphate.
Example 5
A production method of amorphous potassium dihydrogen phosphate with adjustable bulk density comprises the following steps:
s1, material liquid adjustment: adding 0.5wt% of benzoic acid into the potassium dihydrogen phosphate feed liquid, and adjusting the dry matter content of the potassium dihydrogen phosphate in the feed liquid to 20wt%;
s2, atomizing: atomizing the feed liquid obtained in the step S1 into mist drops with the diameter of 30 mu m by adopting high-speed centrifugal atomization;
s3, drying: and (3) carrying out hot air drying on the feed liquid atomized in the step S2 under the condition that the air inlet temperature is 220 ℃ and the air outlet temperature is 180 ℃ to obtain amorphous potassium dihydrogen phosphate.
Example 6
A production method of amorphous potassium dihydrogen phosphate with adjustable bulk density comprises the following steps:
s1, material liquid adjustment: adding 4wt% of potassium oxalate into the potassium dihydrogen phosphate feed liquid, and adjusting the dry matter content of the potassium dihydrogen phosphate in the feed liquid to 25wt%;
s2, atomizing: atomizing the feed liquid obtained in the step S1 into mist drops with the diameter of 50 mu m by adopting high-speed airflow atomization;
s3, drying: and (3) carrying out hot air drying on the feed liquid atomized in the step S2 under the condition that the air inlet temperature is 400 ℃ and the air outlet temperature is 200 ℃ to obtain amorphous potassium dihydrogen phosphate.
Example 7
A production method of amorphous potassium dihydrogen phosphate with adjustable bulk density comprises the following steps:
s1, material liquid adjustment: adding 0.2wt% of lactic acid into the potassium dihydrogen phosphate feed liquid, and adjusting the dry matter content of the potassium dihydrogen phosphate in the feed liquid to 60wt%;
s2, atomizing: atomizing the feed liquid obtained in the step S1 into mist drops with the diameter of 40 mu m by adopting high-speed centrifugal atomization;
s3, drying: and (3) carrying out hot air drying on the feed liquid atomized in the step S2 under the condition that the air inlet temperature is 300 ℃ and the air outlet temperature is 100 ℃ to obtain amorphous potassium dihydrogen phosphate.
Control group 1
The preparation method of the monopotassium phosphate in the control group comprises the following steps:
s1, material liquid adjustment: adjusting the dry matter content of the monopotassium phosphate to 50 weight percent, and heating to dissolve the monopotassium phosphate into a uniform solution;
s2, cooling and crystallizing: naturally cooling the solution obtained in the step S1 to normal temperature under stirring to obtain a feed liquid containing crystalline potassium dihydrogen phosphate;
s3, solid-liquid separation: filtering and separating mother liquor from the feed liquid containing the crystal potassium dihydrogen phosphate obtained in the step S2 to obtain a crystal potassium dihydrogen phosphate wet material;
s4, drying: and (3) carrying out hot air drying on the crystalline potassium dihydrogen phosphate wet material obtained in the step (S3) under the condition that the air inlet temperature is 180 ℃ and the air outlet temperature is 100 ℃ to obtain crystalline potassium dihydrogen phosphate.
Control group 2:
the production process of amorphous potassium dihydrogen phosphate includes the following steps:
s1, material liquid adjustment: adjusting the dry matter content of potassium dihydrogen phosphate to 10wt%;
s2, atomizing: atomizing the feed liquid obtained in the step S1 into mist drops with the diameter of 22 mu m by adopting high-speed centrifugal atomization;
s3, drying: and (3) carrying out hot air drying on the feed liquid atomized in the step S2 under the condition that the air inlet temperature is 180 ℃ and the air outlet temperature is 100 ℃ to obtain amorphous potassium dihydrogen phosphate.
The results of comparing the indices of potassium dihydrogen phosphate obtained in examples 1 to 7 and control groups 1 to 2 are shown in table 1:
TABLE 1
Note that: ) The phosphorus pentoxide and potassium oxide contents of the monopotassium phosphate are tested according to HG/T2321-2016 standard, and the results are the average value of multiple groups of parallel tests. The dissolution rate was measured by dissolving 10g of the sample in 100g of distilled water at the same temperature with a magnetic stirrer at the same stirring rate, and the measurement result was the average value of a plurality of sets of parallel tests.
As is clear from Table 1, the product forms of examples 1 to 7 are amorphous, the dissolution rate is less than 1min, and as is clear from examples 1 to 7, the product form of the present invention is changed and the dissolution rate is greatly increased compared with the potassium dihydrogen phosphate produced by the conventional process, and as is clear from examples 1 to 7, the bulk density of the control group 2 is higher than that of examples 1 to 7 and the dissolution rate is also lower than that of examples 1 to 7, which means that the bulk density of the potassium dihydrogen phosphate can be adjusted by the carboxylic acid or carboxylate, and the dissolution rate of the potassium dihydrogen phosphate is also affected to some extent. The invention reduces the supersaturation degree of the feed liquid by adjusting and controlling the dry matter content of the potassium dihydrogen phosphate in the feed liquid, can inhibit the formation of crystal nucleus, and makes crystals lack the necessary condition for generation. The invention also mixes a small amount of carboxylic acid or carboxylate into the monopotassium phosphate feed liquid, and utilizes the principle that the carboxylic acid or carboxylate is decomposed by heating at high temperature to generate carbon dioxide, so that the materials become bulked in the high-temperature drying process, the bulk density of the materials is reduced, and the commodity of the product is improved. The invention has outstanding technical effects.
The foregoing description is directed to the preferred embodiments of the present invention, but the embodiments are not intended to limit the scope of the invention, and all equivalent changes or modifications made under the technical spirit of the present invention should be construed to fall within the scope of the present invention.

Claims (8)

1. A production method of amorphous potassium dihydrogen phosphate with adjustable bulk density is characterized in that: the method comprises the following steps:
s1, material liquid adjustment: adding 0.1-5wt% of carboxylic acid or carboxylate into the potassium dihydrogen phosphate feed liquid, and adjusting the dry matter content of the potassium dihydrogen phosphate in the feed liquid to 10-65wt%;
s2, atomizing: atomizing the feed liquid obtained in the step S1;
s3, drying: and (3) carrying out hot air drying on the feed liquid atomized in the step (S2) to obtain amorphous potassium dihydrogen phosphate.
2. The method for producing amorphous potassium dihydrogen phosphate with adjustable bulk density as described in claim 1, wherein said carboxylic acid is an organic substance containing-COOH group; the carboxylate contains-COO - Organic matter of the group.
3. The method for producing amorphous potassium dihydrogen phosphate with adjustable bulk density as in claim 2, wherein the carboxylic acid is one or more of acetic acid, propionic acid, oxalic acid, benzoic acid, citric acid, and lactic acid; the carboxylate is one or more of acetic acid, propionic acid, oxalic acid, benzoic acid, citric acid and lactic acid.
4. The method for producing amorphous potassium dihydrogen phosphate with adjustable bulk density as described in claim 1, wherein said atomizing is performed by one of high-speed centrifugal atomization, high-pressure jet atomization and high-speed air stream atomization.
5. The method for producing amorphous potassium dihydrogen phosphate with adjustable bulk density as described in claim 1, wherein in S2, the diameter of droplets formed after atomization of the feed liquid is 22-112 μm.
6. The method for producing amorphous potassium dihydrogen phosphate with adjustable bulk density as described in claim 1, wherein in S3, the air inlet temperature of said hot air drying is 180-400 ℃, and the air outlet temperature is 100-200 ℃.
7. A potassium dihydrogen phosphate prepared by the method for producing an amorphous potassium dihydrogen phosphate having an adjustable bulk density as described in any one of claims 1 to 6; the monopotassium phosphate is amorphous monopotassium phosphate.
8. The potassium dihydrogen phosphate as set forth in claim 7 having a bulk density in the range of 0.5 to 0.9g/cm 3
CN202310858407.7A 2023-07-13 2023-07-13 Production method of amorphous potassium dihydrogen phosphate with adjustable bulk density Pending CN116812889A (en)

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