CN113717008A - Monoammonium phosphate anti-caking agent and application thereof - Google Patents
Monoammonium phosphate anti-caking agent and application thereof Download PDFInfo
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- CN113717008A CN113717008A CN202110928329.4A CN202110928329A CN113717008A CN 113717008 A CN113717008 A CN 113717008A CN 202110928329 A CN202110928329 A CN 202110928329A CN 113717008 A CN113717008 A CN 113717008A
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- monoammonium phosphate
- caking agent
- polyethylene glycol
- agent
- disulfonate
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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
- C05G3/30—Anti-agglomerating additives; Anti-solidifying additives
-
- C—CHEMISTRY; METALLURGY
- 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
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Inorganic Chemistry (AREA)
- Detergent Compositions (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses an ammonium dihydrogen phosphate anti-caking agent, and belongs to the technical field of chemical industry. The components of the composition comprise 5 to 30 percent of polyethylene glycol (400) disulfonate, 11 to 50 percent of ethylene glycol, 0.8 to 2 percent of sodium dodecyl diphenyl ether disulfonate and 10 to 80 percent of water. The monoammonium phosphate anti-caking agent by the slurry method is added into the neutralized slurry before the drying of the monoammonium phosphate and is fully mixed with the slurry, after the drying, the surface energy of the monoammonium phosphate particles can be effectively reduced, a small amount of water in the finished product can be locked, and the function of keeping the loosening of the powdery monoammonium phosphate for a long time is achieved.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a monoammonium phosphate anti-caking agent and application thereof.
Background
The monoammonium phosphate is used as a binary fertilizer containing a phosphorus element and a nitrogen element, is suitable for various soils and various crops, can be used as a seed fertilizer, a base fertilizer and an additional fertilizer, is more used as the additional fertilizer, and is also the most main basic raw material for producing a ternary compound fertilizer and a BB fertilizer. At present, powdery monoammonium phosphate has three production processes, one is a traditional method, and the method is to concentrate phosphoric acid produced by a wet method, neutralize the phosphoric acid by ammonia, and dry the neutralized monoammonium phosphate slurry to obtain a powdery monoammonium phosphate finished product. The process has higher requirement on the purity of the phosphoric acid, and is not suitable for the current situation of domestic phosphorite grade. The other method is a neutralization slurry concentration method, which is to neutralize dilute phosphoric acid by ammonia to prepare neutralized slurry, then to evaporate and concentrate the neutralized slurry, and finally to dry the neutralized slurry to obtain powdery monoammonium phosphate product. Compared with the traditional method, the monoammonium phosphate produced by the method brings more impurity types in the phosphorite, the product quality is relatively poor, and the requirement on the grade of the phosphorite is lower. And thirdly, on the basis of the second process, adding a filtering device after the diluted phosphoric acid is neutralized, removing impurities to obtain purer monoammonium phosphate clear liquid, concentrating, cooling and crystallizing, performing centrifugal separation to obtain monoammonium phosphate crystals, and finally drying to obtain finished products. In particular, the powdery monoammonium phosphate produced by the latter two processes is agglomerated due to the presence of product moisture, temperature, stacking and some impurities carried by the product itself.
Particularly, a plurality of metal cations from phosphoric acid react with monoammonium phosphate to generate a plurality of different salts or double salts, which cannot be completely removed in the purification and impurity removal process of phosphoric acid, and a very small amount of metal cations enter the finished monoammonium phosphate product and have little influence on main nutrients of the finished monoammonium phosphate product, but the impurities exist, and when a small amount of moisture exists and the environmental conditions change continuously, the moisture is evaporated and condensed repeatedly, so that the surfaces of monoammonium phosphate particles are dissolved and crystallized, crystal bridges are generated among the particles, and the particles are connected. In addition, under a certain pressure, the monoammonium phosphate product is seriously agglomerated due to the capillary adhesion effect and the like, wherein the water migration effect is also a main factor in various agglomeration factors.
Therefore, the caking is easy to generate in the storage process after the packaging, the transportation and the use by customers are not changed, and the problem is particularly obvious in the application process of mechanized and automatic equipment.
At present, various anti-caking agent products exist in the market, wherein patent document CN107746291A discloses a method for producing monoammonium phosphate anti-caking agent by a slurry method, and a caking prevention habit modifier is added before monoammonium phosphate crystals are produced, so that the crystal form of the monoammonium phosphate crystals is changed, the hygroscopicity of the monoammonium phosphate is reduced, and the caking performance of the monoammonium phosphate is improved. The medium crystal agent is mainly prepared from one or more inorganic salt mixtures, the addition amount of the medium crystal agent reaches 10% for the monoammonium phosphate product with serious caking, the addition amount is large, the quality of the product can be influenced, and the medium crystal agent is not suitable for being popularized and used. The invention patent CN109650363A discloses a full water-soluble industrial monoammonium phosphate anti-caking agent and a use method thereof, and the anti-caking agent is added to dried industrial monoammonium phosphate crystals in a spray manner by adopting a mode of combining a crystal control agent and a moisture-proof agent.
Disclosure of Invention
The invention aims to provide an ammonium dihydrogen phosphate anti-caking agent, and the problems to be solved by the invention are as follows: in the prior art, the addition amount of the monoammonium phosphate anti-caking agent is large, or the anti-caking agent can be added uniformly only by adding new equipment, so that the corresponding anti-caking effect is achieved, and the enterprise cost is increased.
The invention discloses a monoammonium phosphate anti-blocking agent which is characterized by comprising a water locking agent, a particle surface energy reducing agent and a crystal form control agent.
The anti-caking agent is prepared by compounding a plurality of chemical substances such as a water locking agent, a particle surface energy reducer, a crystal form control agent and the like, fully exerts the synergistic effect among the components and reduces the use of the anti-caking agent.
Further, the water locking agent comprises polyethylene glycol sodium disulfonate.
Further, the molecular formula of the polyethylene glycol disulfonic acid sodium is NaSO3-O(CH2CH2O)n-SO3And (4) Na. n is about 9.
Further, the polyethylene glycol in the polyethylene glycol disulfonate is polyethylene glycol 400.
Further, the preparation method of the water locking agent comprises the following steps:
s1, adding polyethylene glycol, sulfamic acid and a catalyst into a reaction vessel;
s2, heating to 95-100 ℃, and preserving heat for 6-7 hours to obtain the product.
Further, the particle surface energy reducing agent is sodium dodecyl diphenyl ether disulfonate.
Further, the crystal form control agent is ethylene glycol, sodium polyethylene glycol disulfonate and sodium dodecyl diphenyl ether disulfonate.
Further, the weight percentages of the components are as follows: 5-30% of polyethylene glycol sodium disulfonate, 11-50% of ethylene glycol, 0.8-2% of sodium dodecyl diphenyl ether disulfonate and 10-80% of water, wherein the sum of the mass percentages of the components is 100%.
The application of the monoammonium phosphate anti-caking agent is that the addition amount of the anti-caking agent is 0.3 per mill to 5 per mill for producing 1 ton of finished products.
Further, the anti-caking agent is added into the monoammonium phosphate slurry before drying.
After the neutralization tank and before drying, the anti-caking agent is added into the slurry, so that the anti-caking agent can be fully and uniformly mixed with the material, and the uniform addition of the anti-caking agent in a finished product is further ensured. Can effectively reduce the surface energy of the monoammonium phosphate particles and lock a small amount of water in the finished product, and has the function of keeping the powdery monoammonium phosphate loose for a long time.
Further, the anti-caking agent is applied to powdery monoammonium phosphate.
The invention has the beneficial effects that:
1. the strong hydrophilicity of disulfonic acid groups in polyethylene glycol (400) disulfonic acid sodium is utilized, after the disulfonic acid groups are adsorbed on the surfaces of the monoammonium phosphate particles, water molecules can be effectively controlled to migrate along with environmental changes, so that the formation of crystal bridges among the monoammonium phosphate particles is prevented, and the added disulfonic acid groups and the added particle surface energy reducing agent and crystal form control agent have synergistic effects, so that the agglomeration of the monoammonium phosphate particles is effectively prevented;
2. the anti-caking agent can effectively and fundamentally solve the problem of caking of the powdery monoammonium phosphate product;
3. the addition amount of the anti-caking agent is greatly reduced compared with the existing anti-caking agent product, and the quality of the monoammonium phosphate product is not influenced;
4. the anti-caking agent product is added from the monoammonium phosphate slurry before drying, so that the uniform addition of the anti-caking agent product in the finished product can be fully ensured.
Detailed Description
In addition, the embodiments of the present invention and the features of the embodiments may be combined with each other without conflict.
Example 1
The embodiment of the invention provides a water locking agent, which comprises polyethylene glycol (400) sodium disulfonate.
By utilizing the strong hydrophilicity of disulfonic acid groups in polyethylene glycol (400) disulfonic acid sodium, after the disulfonic acid groups are adsorbed on the surfaces of the monoammonium phosphate particles, the migration of water molecules along with the environmental change can be effectively controlled, so that the formation of crystal bridges among the monoammonium phosphate particles is prevented, and the added disulfonic acid sodium and the added particle surface energy reducing agent, the crystal form control agent and the like have synergistic effects, so that the agglomeration of the monoammonium phosphate particles is effectively prevented.
And testing the water locking effect of the water locking agent.
100 g of monoammonium phosphate with the moisture content of 2.5 percent is respectively taken as a control group, a water locking agent with the weight of 2 thousandth of the weight of the monoammonium phosphate and other similar substances and blanks are respectively added as the control group, the metered additives are dissolved in 2 percent of water and then are uniformly mixed with the monoammonium phosphate, the mixture is placed in an oven, and the mixture is kept at the constant temperature of 50 +/-1 ℃ for a plurality of times to measure the weight change of the monoammonium phosphate.
The water locking test data are only partial test data, but are not limited to the water locking effect expressed by the test data.
Monoammonium phosphate with 2% water added was tested at 2 hours, 4 hours, 6 hours, 10 hours for a weight loss of 1.5 grams, 2.5 grams, 3.0 grams, 3.2 grams, respectively.
The monoammonium phosphate with added glycerol was tested at 2 hours, 4 hours, 6 hours, and 10 hours to reduce the weight by 1.3 grams, 2.0 grams, 2.4 grams, and 2.6 grams, respectively.
The monoammonium phosphate with added polyethylene glycol (400) was tested at 2 hours, 4 hours, 6 hours, and 10 hours for a weight loss of 1.4 grams, 2.3 grams, 2.9 grams, and 3.1 grams, respectively.
The monoammonium phosphate with added polyethylene glycol (400) disulfonate was tested at 2 hours, 4 hours, 6 hours, and 10 hours for a weight loss of 1.0 grams, 1.5 grams, 1.8 grams, and 1.9 grams, respectively.
As can be seen from the above test methods, the weight reduction of the monoammonium phosphate added with the polyethylene glycol (400) disulfonic acid sodium is minimal, and the water locking effect is good.
Example 2
The embodiment of the invention provides a preparation method of a water locking agent. Adding polyethylene glycol (400) into a reaction kettle, adding metered sulfamic acid and a proper amount of catalyst (such as urea), slowly stirring to be basically uniform, regulating the stirring speed of the reaction kettle to be more than 60r/min, heating to 95-100 ℃, preserving heat for 6-7h, and neutralizing with sodium hydroxide to obtain the polyethylene glycol (400) sodium disulfonate.
Example 3
This example is a powdery monoammonium phosphate anticaking agent containing the following components (by mass%):
polyethylene glycol (400) disulfonic acid sodium salt: 10 percent;
ethylene glycol: 14 percent;
sodium dodecyl diphenyl ether disulfonate: 2.0 percent;
water: 74 percent;
accurately weighing the components according to the proportion, adding the components into a mixing tank with a stirring device, and stirring for 30 minutes to uniformly mix.
Example 4
This example is a powdery monoammonium phosphate anticaking agent containing the following components (by mass%):
polyethylene glycol (400) disulfonic acid sodium salt: 20 percent;
ethylene glycol: 24 percent;
sodium dodecyl diphenyl ether disulfonate: 2.0 percent;
water: 54 percent;
accurately weighing the components according to the proportion, adding the components into a mixing tank with a stirring device, and stirring for 30 minutes to uniformly mix.
Example 5
This example is a powdery monoammonium phosphate anticaking agent containing the following components (by mass%):
polyethylene glycol (400) disulfonic acid sodium salt: 8 percent;
ethylene glycol: 34 percent;
sodium dodecyl diphenyl ether disulfonate: 2.0 percent;
water: 56 percent;
accurately weighing the components according to the proportion, adding the components into a mixing tank with a stirring device, and stirring for 30 minutes to uniformly mix.
Example 6
This example is a powdery monoammonium phosphate anticaking agent containing the following components (by mass%):
polyethylene glycol (400) disulfonic acid sodium salt: 10 percent;
ethylene glycol: 40 percent;
sodium dodecyl diphenyl ether disulfonate: 1.0 percent;
water: 49 percent;
accurately weighing the components according to the proportion, adding the components into a mixing tank with a stirring device, and stirring for 30 minutes to uniformly mix.
Example 7
This example is a powdery monoammonium phosphate anticaking agent containing the following components (by mass%):
polyethylene glycol (400) disulfonic acid sodium salt: 15 percent;
ethylene glycol: 45 percent;
sodium dodecyl diphenyl ether disulfonate: 1.0 percent;
water: 39 percent;
accurately weighing the components according to the proportion, adding the components into a mixing tank with a stirring device, and stirring for 30 minutes to uniformly mix.
Example 8
This example is a powdery monoammonium phosphate anticaking agent containing the following components (by mass%):
polyethylene glycol (400) disulfonic acid sodium salt: 30 percent;
ethylene glycol: 15 percent;
sodium dodecyl diphenyl ether disulfonate: 2.0 percent;
water: 56 percent;
accurately weighing the components according to the proportion, adding the components into a mixing tank with a stirring device, and stirring for 30 minutes to uniformly mix.
Comparative example 1
This embodiment is a comparative example of the present invention, which is based on example 4 and is modified by adding sodium polyethylene glycol (400) disulfonate to the monoammonium phosphate anticaking agent component, replacing it with sodium lauryl sulfate, and using the same amount and production process for the rest of the components.
Comparative example 2
This embodiment is a comparative example of the present invention, which is based on example 4 and is modified by adding no sodium polyethylene glycol (400) disulfonate to the monoammonium phosphate anticaking agent component, replacing it with dodecylbenzene sulfonic acid, and the rest of the components, the amounts and the production processes are the same.
Comparative example 3
This embodiment is a comparative example of the present invention, which is based on example 4 and is modified by adding sodium polyethylene glycol (400) disulfonate to the monoammonium phosphate anticaking agent component, replacing it with sodium polyacrylate, and using the same amount and production process for the rest of the components.
Comparative example 4
This embodiment is a comparative example of the present invention, which is based on example 4 and is modified by adding no sodium polyethylene glycol (400) disulfonate to the monoammonium phosphate anticaking agent component, replacing it with polyacrylamide, and the rest components, the amounts and the production processes are the same.
Comparative example 5
This embodiment is a comparative example of the present invention, which is based on example 4 and is modified by adding no sodium polyethylene glycol (400) disulfonate to the monoammonium phosphate anticaking agent component, replacing with glycerin, and the rest components, the amounts and the production process are the same.
Comparative example 6
This embodiment is a comparative example of the present invention, which is based on example 4 and is modified by adding no sodium polyethylene glycol (400) disulfonate to the monoammonium phosphate anticaking agent component, replacing with sodium polyphosphate, and the rest components, the amounts and the production process are the same.
Detection of
Spraying the monoammonium phosphate anti-caking agent in each embodiment and comparative example on the surface of a test fertilizer according to a certain addition amount, forming the anti-caking agent into a cylinder with the diameter of 50 multiplied by 40mm under the pressure of 2MPa, and then placing the cylinder in a test box with the temperature of 60 ℃ for 12 hours under the pressure; and then the sample is placed in an environment with the relative humidity of 60% and the temperature of 40 ℃ for 12 hours under the pressure, the cycle is carried out for three times to obtain a sample, and then the crushing pressure of the sample is tested, and the unit is as follows: and N is added. Blank group is without adding anti-caking agent.
Test result table
As can be seen from the above table, the effect of adding the monoammonium phosphate anti-caking agent is obviously better than that of the comparative example and the blank group.
The invention is not limited to the above alternative embodiments, and any other various forms of products can be obtained by anyone in the light of the present invention, but any changes in shape or structure thereof, which fall within the scope of the present invention as defined in the claims, fall within the scope of the present invention.
Claims (10)
1. An ammonium dihydrogen phosphate anti-caking agent is characterized by comprising a water locking agent, a particle surface energy reducing agent and a crystal form control agent.
2. The monoammonium phosphate anti-caking agent according to claim 1, wherein the water-locking agent comprises sodium polyethylene glycol disulfonate.
3. The monoammonium phosphate anti-caking of claim 2The agent is characterized in that the molecular formula of the polyethylene glycol disulfonic acid sodium is NaSO3-O(CH2CH2O)n-SO3Na。
4. The monoammonium phosphate anti-caking agent according to claim 2, wherein the polyethylene glycol in the polyethylene glycol disulfonate is polyethylene glycol 400.
5. The monoammonium phosphate anti-caking agent according to claim 2, wherein the preparation method of the water-locking agent comprises the following steps:
s1, adding polyethylene glycol, sulfamic acid and a catalyst into a reaction vessel;
s2, heating to 95-100 ℃, and preserving heat for 6-7 hours to obtain the product.
6. The monoammonium phosphate anti-caking agent according to claim 1, wherein the particle surface energy reducing agent is sodium dodecyldiphenyl ether disulfonate.
7. The monoammonium phosphate anti-caking agent according to claim 1, wherein the crystal form control agent is ethylene glycol, sodium polyethylene glycol disulfonate and dodecyl diphenyl ether disulfonate.
8. The monoammonium phosphate anti-caking agent according to claim 1, which comprises 5 to 30 mass percent of sodium polyethylene glycol (400) disulfonate, 11 to 50 mass percent of ethylene glycol, 0.8 to 2 mass percent of sodium dodecyl diphenyl ether disulfonate and 10 to 80 mass percent of water, wherein the sum of the mass percent of the components is 100 percent.
9. Use of a mono-ammonium phosphate anti-caking agent, characterized in that the anti-caking agent according to any one of claims 1 to 8 is added in an amount of 0.3 to 5 per thousand.
10. The use of a mono-ammonium phosphate anti-caking agent according to claim 9, wherein the anti-caking agent is added directly to the mono-ammonium phosphate slurry.
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| 邵建华: "由氨基磺酸为磺化剂合成聚氧乙烯硫酸钠", 《化学世界》 * |
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