CN111233556B - Urea phosphate mother liquor slow-release suspension liquid fertilizer and preparation method thereof - Google Patents
Urea phosphate mother liquor slow-release suspension liquid fertilizer and preparation method thereof Download PDFInfo
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- CN111233556B CN111233556B CN202010205157.3A CN202010205157A CN111233556B CN 111233556 B CN111233556 B CN 111233556B CN 202010205157 A CN202010205157 A CN 202010205157A CN 111233556 B CN111233556 B CN 111233556B
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
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- 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
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Abstract
The invention aims to provide a urea phosphate mother liquor slow-release suspension liquid fertilizer which is prepared from the following raw materials in parts by weight: urea phosphate mother liquor: 1000 parts of (A); pH regulator: 90-100 parts of; macronutrient-containing compound: 200-500 parts; suspending agent: 15-30 parts of a solvent; the suspending agent is one or more of xanthan gum, polyacrylamide and clay minerals; the clay mineral is one or more of montmorillonite, sepiolite, attapulgite and bentonite. The method provided by the invention can solve the problem of precipitation of the urea phosphate mother liquor with high inorganic metal ion content, and the preparation process does not generate waste water and waste residues, the generated gas is carbon dioxide, the environment is not polluted, the long-time stability of the suspended liquid fertilizer is realized, and the prepared liquid fertilizer has a slow release effect. The invention also provides a preparation method of the urea phosphate mother liquor slow-release suspension liquid fertilizer.
Description
Technical Field
The invention belongs to the technical field of liquid fertilizer production, and particularly relates to a urea phosphate mother liquor slow-release suspension liquid fertilizer and a preparation method thereof.
Background
The liquid fertilizer becomes the first choice fertilizer for the irrigation equipment due to the advantages of high dissolving speed, uniformity and the like. Due to the ready-to-use property, the fertilizer does not need to be stirred and dissolved, is very suitable for automatic fertilization, and is widely applied in irrigation technology and countries where the automatic fertilization is popularized. In the united states, liquid fertilizers account for over 38% of all fertilizers, nearly all in israel's fields use liquid fertilizers, and australia, france, germany, spain, romania, etc. are countries where liquid fertilizers are used in large quantities.
China belongs to a big agricultural country and is the first country of chemical fertilizer production and consumption in the world, but China is not a strong agricultural country, most of fertilizers used are solid fertilizers, and the produced fertilizers have a serious problem of excess capacity. Therefore, improving the utilization rate of agricultural fertilizers is a necessary requirement for improving the comprehensive agricultural production capacity. As an agricultural fertilizer production enterprise, the product structure is adjusted, and the product types are enriched to meet the different demands of different regions and different types of markets.
The suspension liquid fertilizer contains more nutrients and can contain insoluble substances, so that the requirement on fertilizer raw materials is low, the suspension liquid fertilizer has the advantages of low production cost, low investment, easiness in compounding, capability of being directly absorbed by crops, convenience in fertilization, no dust in the production and transportation process, water consumption saving and the like, and the suspension liquid fertilizer product has the characteristic of novel fertilizer development.
The urea phosphate mother liquor is a byproduct of urea phosphate production and is a binary liquid fertilizer containing N, P. Generally, the fertilizer is sold directly as an agricultural grade fertilizer, but is difficult to accept by customers due to inconvenient transportation, and the product for the agricultural grade fertilizer has low profit. Therefore, for many urea phosphate manufacturing enterprises, the urea phosphate mother liquor is a waste material, and a certain cost is consumed for treatment. However, the suspended liquid fertilizer belongs to supersaturated liquid, is in an unstable state, is greatly influenced by external force, temperature, pH value and the like, is easy to separate out crystals, and the crystals grow continuously, so that solid-liquid separation of the suspended liquid fertilizer is finally caused. Many of the liquid fertilizers in the market at present have the problem of deposition and delamination to an extent, and are more prone to deposition after long-term storage. Therefore, the urea phosphate mother liquor is difficult to prepare into liquid fertilizer, and is mostly prepared into solid fertilizer.
Disclosure of Invention
The invention aims to provide a urea phosphate mother liquor slow-release suspended liquid fertilizer and a preparation method thereof.
The invention provides a urea phosphate mother liquor slow-release suspension liquid fertilizer which is prepared from the following raw materials in parts by weight:
urea phosphate mother liquor: 1000 parts of (A);
pH regulator: 90-100 parts of;
macronutrient-containing compound: 200-500 parts;
suspending agent: 15-30 parts of a solvent;
the suspending agent is one or more of xanthan gum, polyacrylamide and clay minerals; the clay mineral is one or more of montmorillonite, sepiolite, attapulgite and bentonite.
Preferably, the urea phosphate mother liquor is supernatant liquor obtained after cooling and separating residual liquid after reaction of phosphoric acid and urea and crystallization separation for preparing a urea phosphate product;
the temperature of cooling separation is 10-20 ℃.
Preferably, P in the urea phosphate mother liquor2O5The mass fraction of (A) is 21-30%; the mass fraction of the N element is 7-11%; the mass fraction of the metal ions is 3-7%.
Preferably, the pH regulator is ammonium bicarbonate and/or ammonia water.
Preferably, the compound containing macroelements is one or more of urea, ammonium sulfate, ammonium polyphosphate, potassium pyrophosphate, potassium tripolyphosphate, urea ammonium nitrate solution, potassium chloride, potassium nitrate, potassium sulfate, industrial potassium dihydrogen phosphate and industrial ammonium dihydrogen phosphate.
Preferably, the suspending agent is xanthan gum, polyacrylamide and clay mineral;
the mass ratio of the xanthan gum to the polyacrylamide to the clay mineral is 10: 4-10: 1-4.
Preferably, the particle size of the clay mineral is less than 200 meshes.
Preferably, the raw materials also comprise 15-20 parts of organic fertilizer;
the organic fertilizer comprises one or more of mineralized humic acid, mineralized potassium fulvate and biochemical potassium fulvate.
The invention provides a preparation method of a urea phosphate mother liquor slow-release suspension liquid fertilizer, which comprises the following steps:
A) adding 90-100 parts of pH regulator into 1000 parts of urea phosphate mother liquor to obtain mixed mother liquor with the pH value of 3.0-7.0;
B) adding 200-500 parts by weight of a compound containing major elements into the mixed mother liquor to obtain a suspended fertilizer mother liquor;
C) adding 15-30 parts by weight of a suspending agent into the suspended fertilizer mother liquor, and dispersing and emulsifying to obtain a urea phosphate mother liquor slow-release suspended liquid fertilizer;
the suspending agent is one or more of xanthan gum, polyacrylamide and clay minerals; the clay mineral is one or more of montmorillonite, sepiolite, attapulgite and bentonite.
Preferably, the rotation speed of the dispersion emulsification in the step C) is 8000-10000 r/min;
the emulsifying time is 3-5 min.
The invention aims to provide a urea phosphate mother liquor slow-release suspension liquid fertilizer which is prepared from the following raw materials in parts by weight: urea phosphate mother liquor: 1000 parts of (A); pH regulator: 90-100 parts of a solvent; macronutrient-containing compound: 200-500 parts; suspending agent: 15-30 parts of a solvent; the suspending agent is one or more of xanthan gum, polyacrylamide and clay minerals; the clay mineral is one or more of montmorillonite, sepiolite, attapulgite and bentonite.
The preparation method of the slow-release suspension liquid fertilizer provided by the invention can realize the following beneficial effects: (1) the urea phosphate mother liquor with high inorganic metal ion content is easy to precipitate and difficult to utilize when producing liquid fertilizers or solid fertilizers, the method provided by the invention can solve the problem of precipitation of the urea phosphate mother liquor with high inorganic metal ion content, the problem of difficult treatment of acidic mother liquor generated in the urea phosphate production process is solved, waste is changed into valuable, resources are fully utilized, and economic benefits are realized; (2) waste water and waste residues are not generated in the preparation process of the suspension fertilizer, the generated gas is carbon dioxide, the environment is not polluted, more than 98% of raw materials are converted into fertilizer products, and the suspension fertilizer is green and environment-friendly; (3) the dosage of the auxiliary agent is not more than 2 percent, the characteristic of high content of inorganic metal ions in the urea phosphate mother liquor is effectively utilized, the type of the suspending agent is optimized, the long-time stability of the suspended liquid fertilizer is realized, and the slow release effect of the prepared liquid fertilizer is realized.
Detailed Description
The invention provides a urea phosphate mother liquor slow-release suspension liquid fertilizer which is prepared from the following raw materials in parts by weight:
urea phosphate mother liquor: 1000 parts of (A);
pH regulator: 90-100 parts of a solvent;
macronutrient-containing compound: 200-500 parts;
suspending agent: 15-30 parts;
the suspending agent is one or more of xanthan gum, polyacrylamide and clay minerals; the clay mineral is one or more of montmorillonite, sepiolite, attapulgite and bentonite.
In the invention, the urea phosphate mother liquor is supernatant liquor obtained after crystallization separation is carried out after phosphoric acid and urea react to prepare a urea phosphate product and the residual liquid is cooled and separated; the cooling separation temperature is preferably 10-20 ℃, and more preferably 10-15 ℃. P in the urea phosphate mother liquor2O5The mass fraction of (A) is 21-30%; the mass fraction of the N element is 7-11%. In addition, the urea phosphate mother liquor also contains metal ions such as iron, calcium, magnesium, aluminum and the like and trace organic matters, and the mass fraction of the metal ions is 3-7%.
In the present invention, the pH regulator is preferably ammonium bicarbonate and/or ammonia water, and the amount of the pH regulator is preferably 90 to 100 parts, more preferably 95 to 98 parts, and specifically, in an embodiment of the present invention, may be 90 parts or 100 parts. The pH value of the liquid fertilizer is adjusted to be within the range of 3.0-7.0 parts by using the pH value regulator so as to meet the fertilization requirement.
In the invention, the macroelement-containing compound is preferably one or more of urea, ammonium sulfate, ammonium polyphosphate (18-58-0), potassium pyrophosphate, potassium tripolyphosphate, urea ammonium nitrate solution (UAN), potassium chloride, potassium nitrate, potassium sulfate, industrial monopotassium phosphate and industrial monoammonium phosphate, and the nutrient mass concentration of the ammonium polyphosphate is N: p2O5：K2O is 18: 58: 0. Specifically, in the embodiment of the present invention, the ammonium polyphosphate may be a combination of urea, potassium pyrophosphate and ammonium tripolyphosphate, a urea ammonium nitrate solution, ammonium polyphosphate, potassium pyrophosphate and potassium chloride, or urea, tris (ammonium chloride)A combination of potassium polyphosphate and potassium chloride. The mass fraction of the macroelement-containing compound is preferably 200 to 500 parts, more preferably 300 to 400 parts, and specifically, in the embodiment of the present invention, 280 parts, 470 parts, or 200 parts.
In the invention, the suspending agent is preferably one or more of xanthan gum, polyacrylamide and clay mineral, preferably, the suspending agent is a combination of xanthan gum, polyacrylamide and clay mineral, the mass ratio of the xanthan gum, the polyacrylamide and the clay mineral is preferably 10: 4-10: 1-4, more preferably 10: 5-9: 2-3, and specifically, in the embodiment of the invention, the mass ratio may be 10: 4: 2, 10: 4 or 10: 2.
In the invention, the particle size of the clay mineral is preferably less than 200 meshes, which is beneficial to dispersion. The clay mineral is preferably one or more of montmorillonite, sepiolite, attapulgite and bentonite, and more preferably the combination of bentonite and attapulgite, or the combination of sepiolite and attapulgite. The bentonite is preferably sodium bentonite. Specifically, in the embodiment of the present invention, the suspending agent may be a suspending agent composed of xanthan gum, polyacrylamide and sodium bentonite (or sepiolite) in a mass ratio of 10: 6: 2, a suspending agent composed of xanthan gum, polyacrylamide, sodium bentonite and attapulgite in a mass ratio of 10: 4: 2, or a suspending agent composed of xanthan gum, polyacrylamide and sepiolite in a mass ratio of 10: 2.
In the invention, the raw materials preferably further comprise an organic fertilizer, and the organic fertilizer preferably comprises one or more of mineralized humic acid, mineralized potassium fulvate and biochemical potassium fulvate; the weight portion of the organic fertilizer is preferably 15-20.
In the invention, the viscosity of the urea phosphate mother liquor slow-release suspension liquid fertilizer is 800-1900 mP.s, and preferably, the viscosity of the suspension liquid fertilizer is 1500-1900 mP.s.
The total nutrient concentration of nitrogen, phosphorus and potassium of the suspension liquid fertilizer prepared by the invention is more than 500g/L, and meets the macroelement water soluble fertilizer (NY 1107-The range is N: p2O5：K2O＝(100～200)：(200～350：(0～100)。
The invention also provides a preparation method of the urea phosphate mother liquor slow-release suspension liquid fertilizer, which comprises the following steps:
A) adding 90-100 parts of pH regulator into 1000 parts of urea phosphate mother liquor to obtain mixed mother liquor with the pH value of 3.0-7.0;
B) adding 200-500 parts by weight of a compound containing major elements into the mixed mother liquor to obtain a suspended fertilizer mother liquor;
C) adding 15-30 parts by weight of a suspending agent into the suspended fertilizer mother liquor, and dispersing and emulsifying to obtain a urea phosphate mother liquor slow-release suspended liquid fertilizer;
the suspending agent is one or more of xanthan gum, polyacrylamide and clay minerals; the clay mineral is one or more of montmorillonite, sepiolite, attapulgite and bentonite.
In the present invention, the kinds, amounts and sources of the raw materials are the same as those of the raw materials described above, and thus, the description thereof is omitted.
According to the invention, a pH regulator is added into urea phosphate mother liquor and stirred to obtain mixed mother liquor. The rotation speed of the stirring is preferably 500-1000 rpm, more preferably 600-900 rpm, most preferably 700-800 rpm, and specifically, in the embodiment of the present invention, 600 rpm may be used. The stirring time is preferably 40-50 min. The invention preferably uses a mechanical stirrer for stirring. The pH of the obtained mixed mother liquor is preferably 4.0-6.0, and more preferably 5.0-6.0.
After the mixed mother liquor is obtained, the compound containing macroelements is added into the mixed mother liquor and stirred to obtain the suspended fertilizer mother liquor.
In the invention, the rotation speed of the stirring is preferably 500-1000 rpm, more preferably 600-900 rpm, and most preferably 700-800 rpm, and specifically, in the embodiment of the invention, 600 rpm may be used. The stirring time is preferably 40-70 min, and more preferably 50-60 min. The invention preferably uses a mechanical stirrer for stirring.
After the suspension fertilizer mother liquor is obtained, the invention adds the suspending agent into the suspension fertilizer mother liquor, and carries out dispersion and emulsification to obtain the urea phosphate mother liquor slow-release suspension liquid fertilizer.
In the invention, an emulsifier is preferably adopted for the dispersion and emulsification, and the rotating speed of the emulsifier is preferably 8000-10000 r/min, more preferably 8000-9000 r/min; the time sequence of the emulsification is 3-5 min, and more preferably 3-4 min.
The invention aims to provide a urea phosphate mother liquor slow-release suspension liquid fertilizer which is prepared from the following raw materials in parts by weight: urea phosphate mother liquor: 1000 parts of (A); pH regulator: 90-100 parts of a solvent; macronutrient-containing compound: 200-500 parts; suspending agent: 15-30 parts of a solvent; the suspending agent is one or more of xanthan gum, polyacrylamide and clay minerals; the clay mineral is one or more of montmorillonite, sepiolite, attapulgite and bentonite.
The preparation method of the slow-release suspension liquid fertilizer provided by the invention can realize the following beneficial effects: (1) the urea phosphate mother liquor with high inorganic metal ion content is easy to precipitate and difficult to utilize when producing liquid fertilizers or solid fertilizers, the method provided by the invention can solve the problem of precipitation of the urea phosphate mother liquor with high inorganic metal ion content, the problem of difficult treatment of acidic mother liquor generated in the urea phosphate production process is solved, waste is changed into valuable, resources are fully utilized, and economic benefits are realized; (2) waste water and waste residues are not generated in the preparation process of the suspension fertilizer, the generated gas is carbon dioxide, the environment is not polluted, more than 98% of raw materials are converted into fertilizer products, and the suspension fertilizer is green and environment-friendly; (3) the dosage of the auxiliary agent is not more than 2 percent, the characteristic of high content of inorganic metal ions in the urea phosphate mother liquor is effectively utilized, the type of the suspending agent is optimized, the long-time stability of the suspended liquid fertilizer is realized, and the slow release effect of the prepared liquid fertilizer is realized.
In order to further illustrate the present invention, the urea phosphate mother liquor sustained-release suspension liquid fertilizer and the preparation method thereof provided by the present invention are described in detail below with reference to the examples, but the invention should not be construed as limiting the scope of the present invention.
The urea phosphate mother liquor used in the embodiment is from waste liquor generated after urea phosphate products are produced by ChuanHeng ecological technology limited company, so that chemical waste liquor recycling is realized, and the economic benefit of enterprises is improved. P in the urea phosphate mother liquor2O5The mass percent content is about 25%, the mass percent content of N is about 11%, the content of inorganic metal ions in the urea phosphate mother liquor is high and reaches more than about 3%, wherein the inorganic metal ions comprise iron, silicon, aluminum, magnesium, trace organic matters and the like.
Example 1
S1: taking 1000 parts of urea phosphate mother liquor at room temperature, slowly adding 100 parts of ammonium bicarbonate into the urea phosphate mother liquor, and stirring by adopting a mechanical stirrer at the stirring speed of 600 revolutions per minute for 50 minutes to obtain mixed mother liquor;
s2: adding 100 parts of urea, 80 parts of potassium pyrophosphate and 100 parts of ammonium tripolyphosphate into the mixed mother liquor, and stirring for 50 minutes at the same stirring speed to obtain a suspended fertilizer mother liquor;
s3: adding 10 parts of xanthan gum, 6 parts of polyacrylamide and 2 parts of sodium bentonite into the suspension fertilizer mother liquor, and emulsifying by using an emulsifying machine, wherein the rotating speed of the emulsifying machine is 8000 revolutions per minute, and the emulsifying time is 3 minutes, so as to obtain the suspension liquid fertilizer.
Example 2
S1: taking 1000 parts of urea phosphate mother liquor at room temperature, slowly adding 100 parts of ammonium bicarbonate into the urea phosphate mother liquor, and stirring by adopting a mechanical stirrer at the stirring speed of 600 revolutions per minute for 50 minutes to obtain mixed mother liquor;
s2: adding 200 parts of UAN, 150 parts of ammonium polyphosphate, 100 parts of potassium pyrophosphate and 20 parts of potassium chloride into the mixed mother liquor, and stirring for 50 minutes at the same stirring speed to obtain a suspended fertilizer mother liquor;
s3: adding 15 parts of potassium fulvate, 10 parts of xanthan gum, 4 parts of polyacrylamide, 2 parts of sodium bentonite and 2 parts of attapulgite into the suspension fertilizer mother liquor, and emulsifying by using an emulsifying machine at the rotating speed of 8000 revolutions per minute for 3 minutes to obtain the suspension liquid fertilizer.
Example 3
S1: taking 1000 parts of urea phosphate mother liquor at room temperature, slowly adding 90 parts of ammonia water into the urea phosphate mother liquor, and stirring by using a mechanical stirrer at the stirring speed of 600 revolutions per minute for 50 minutes to obtain mixed mother liquor;
s2: adding 100 parts of urea, 80 parts of potassium tripolyphosphate and 20 parts of potassium chloride into the mixed mother liquor, and stirring for 50 minutes at the same stirring speed to obtain a suspension fertilizer mother liquor;
s3: adding 20 parts of potassium fulvate, 10 parts of xanthan gum, 10 parts of polyacrylamide and 2 parts of sepiolite into the suspension fertilizer mother liquor, and emulsifying by using an emulsifying machine at the rotating speed of 8000 revolutions per minute for 3 minutes to obtain the suspension liquid fertilizer.
Example 4
The preparation method is the same as that of example 2, and the preparation raw materials are different from example 2 only in that 2 parts of sodium bentonite in step S3 are replaced by 2 parts of sepiolite, and the other raw materials are the same as those in example 3.
Example 5
The preparation method is the same as that of example 2, and the preparation raw materials are different from example 2 only in that 10 parts of xanthan gum and 4 parts of polyacrylamide are used as the suspending agent in step S3, sodium bentonite and attapulgite are not included in the suspending agent, and other raw materials are the same as those in example 2.
Example 6
The preparation method is the same as that of example 2, and the preparation raw materials are different from example 2 only in that 2 parts of sodium bentonite and 2 parts of attapulgite are used as the suspending agent in step S3, xanthan gum and polyacrylamide are not included in the suspending agent, and other raw materials are the same as those in example 2.
Example 7
The preparation method is the same as that of example 3, and the preparation raw materials are different from example 3 only in that 2 parts of sepiolite is used as the suspending agent in step S3, xanthan gum and polyacrylamide are not included in the suspending agent, and other raw materials are the same as those in example 3.
Comparative example 1
The preparation method is the same as that of example 3, and the preparation raw materials are different from example 3 only in that step S3 does not contain xanthan gum, polyacrylamide and sepiolite, and other raw materials are the same as those of example 3.
Detection of stability of suspended liquid fertilizer
The test method comprises the following steps: the prepared suspension liquid fertilizer is stored in a freezer at the temperature of-5 ℃, taken out on the 0 th day, the 7 th day, the 14 th day, the 30 th day, the 60 th day and the 90 th day according to the time in the table 2, whether the suspension liquid fertilizer has layering and crystal precipitation conditions or not is observed, the quality of the suspension liquid fertilizer is judged according to the layering conditions and the crystal precipitation amount, and the stability of the suspension liquid fertilizer in temperature and time is examined. The results are shown in tables 1 and 2.
TABLE 1 analysis of suspended liquid fertilizer
Note:
1) n sum of K2O adopts the determination of the total nitrogen, phosphorus and potassium contents of the water-soluble fertilizer (1977-;
2)P2O5total adoption of the ammonium polyphosphate of Fertilizer grade (Q/CHHG 10-2018)
TABLE 2 percentage of precipitation of suspended liquid fertilizer
Note: "- - -' indicates that the suspended liquid fertilizer has no precipitation and layering phenomenon;
the precipitation amount (%). the precipitation mass after drying/the total mass of the liquid fertilizer is 100%
Because the urea phosphate mother liquor used in the invention has a high metal ion content, as in examples 1 and 2, when a large amount of nitrogen fertilizer, potassium fertilizer and phosphate fertilizer is added into the mixed liquor of the urea phosphate mother liquor and ammonium bicarbonate or ammonia water, a trace precipitation phenomenon occurs, especially in the preparation methods described in examples 2 and 4, because the addition amounts of UAN, potassium polyphosphate and potassium polyphosphate are larger, the addition amount of the raw material containing the major elements is about 1/2 of the mass of the urea phosphate mother liquor, and the precipitation phenomenon occurs shortly after the addition of the raw material containing the major elements, but a uniformly dispersed and stable suspension liquid fertilizer is formed after the addition of the suspending agent for emulsification. As shown in the above table, the precipitation and delamination phenomena were not observed even after the samples of example 1, example 2 and example 3 were left for 90 days at room temperature. Example 4 compared to example 2, the suspended liquid fertilizer was stable at day 90 after optimization of the suspending agent.
In example 5, only xanthan gum and polyacrylamide are selected as the suspending agent on the basis of example 2, and in example 6, only bentonite and attapulgite are selected as the suspending agent on the basis of example 2, and it can be seen from stability data that the effect of only clay mineral is the worst, and the analysis reason may be that the content of inorganic metal ions in the urea phosphate mother liquor used in the invention is high, the clay mineral also belongs to inorganic substances, and the layering phenomenon occurs rapidly when the inorganic metal ions and the inorganic clay meet and adsorb to rapidly cohere, so that the stability of the suspended liquid fertilizer is poor.
The effect data of example 7 also demonstrate the inference that precipitation occurs at day 14 and demixing occurs as precipitation increases when compared to example 3 when only sepiolite is included in the suspended fertilizer and no xanthan and polyacrylamide are included.
The stability results of example 2 and example 4 demonstrate that the time stability of the prepared suspension liquid fertilizer is better when the suspending agent only comprises xanthan gum, polyacrylamide and clay mineral, which indicates that when the liquid fertilizer is produced by using urea phosphate mother liquor with high inorganic metal ion content as the raw material, the effect of simultaneously selecting organic high molecular material and inorganic clay as the suspending agent is better, wherein the inorganic clay is preferably the combination of sepiolite and attapulgite.
Suspended liquid fertilizer release rate tracking
Purpose of the experiment: the time stability of the suspension liquid fertilizer prepared by the invention at the temperature of-5 ℃ is detected.
The experimental method comprises the following steps: according to the time shown in the table 3, the phosphorus in the suspension liquid fertilizer is taken out and analyzed on the 0 th day, the 7 th day, the 14 th day, the 30 th day, the 60 th day and the 90 th day respectively, and the process of hydrolyzing the polymerized phosphorus into orthophosphate and the process of slowly releasing the suspension liquid fertilizer are carried out. The results are shown in Table 3.
Table 3 example liquid fertilizer polymerization rate as a function of time
| Examples | Day 0 | Day 7 | Day 14 | Day 30 | Day 60 | Day 90 |
| Example 1 | 26.95 | 26.34 | 26.01 | 25.45 | 20.15 | 10.76 |
| Example 2 | 25.37 | 24.29 | 23.98 | 21.12 | 17.87 | 8.76 |
| Example 3 | 12.46 | 12.72 | 12.03 | 11.34 | 9.23 | 4.87 |
| Example 4 | 26.41 | 26.06 | 22.56 | 17.45 | 14.67 | 9.54 |
| Example 5 | 25.87 | 23.56 | 22.82 | 17.46 | 13.34 | 7.31 |
| Example 6 | 26.01 | 24.45 | 23.76 | 18.18 | 14.98 | 8.54 |
| Example 7 | 12.76 | 11.65 | 10.76 | 8.65 | 5.01 | 3.26 |
| Comparative example 1 | 12.26 | - | - | - | - | - |
Note: 1. comparative example 1 no slow release effect was observed because of severe delamination;
2. the polymerization rate test method is carried out according to the method in Q/CHHG 10-2018 & lt & ltammonium polyphosphate of fertilizer grade ].
As can be seen from table 3, the polymerization rates of the suspended liquid fertilizers of examples 1 to 6 showed a gradually decreasing trend with time. The change is caused by slow hydrolysis of polymeric phosphorus, and the process of hydrolyzing polymeric phosphorus into orthophosphate is the process of slowly releasing phosphorus in the liquid fertilizer. Therefore, the six suspension type liquid fertilizers of examples 1 to 6 all have slow release effect, because the precipitates of examples 4, 5 and 6 are more, a few layering phenomena occur, and the suspension effect is not ideal. In the hydrolysis process, the medium and trace nutrients (iron, silicon, aluminum and magnesium) in the mother liquor are released so as to be slowly released.
The suspending agent containing organic polymer materials and inorganic clay in the liquid fertilizer has better slow release effect because: this application is inorganic metal ion content is higher in the urea phosphate mother liquor, and inorganic clay can adsorb inorganic metal ion, and organic macromolecular material increases liquid fertilizer viscosity, and complex and adhesion are on inorganic clay surface simultaneously, so inorganic clay, organic macromolecular material, organic macromolecular fertilizer bed layer package and formation can stabilize the tiny granular structure of suspension, just can appear releasing the nutrient effect in microelement and the auxiliary agent in the mother liquor slowly along with the extension of time.
The sepiolite is fibrous hydrous magnesium silicate, is shaped like a clod, a peel or a nodule, is in the shape of anisometric needle and is aggregated into a fiber shape, and the surface hydroxyl can be quickly swelled and dispersed when meeting water or polar solution to form a network in which monomer fibers or smaller fiber bundles are irregularly dispersed and mutually restricted, and has increased specific surface energy and strong adsorbability.
The water-soluble polymer is a polymer with huge molecular weight, when a small amount of polymer is dissolved in water, molecular chains are mutually entangled, the phase change increases the length of the molecular chains, so that the solution is thickened, the sedimentation rate of insoluble particles is reduced, groups on the molecular chains have complexation and adsorption with metal ions and the insoluble particles, the ions and the insoluble particles are fixed, and the free states of the ions and the insoluble particles in a liquid phase are reduced. As a result, the sedimentation rate of the suspension liquid is greatly prolonged, and the use of the liquid fertilizer and the total nutrient are not influenced and reduced in the period of validity of the suspension fertilizer. Therefore, the sepiolite and the water-soluble polymer have good adsorption capacity, can adsorb inorganic metal ions in urea phosphate mother liquor, finally form suspended particles which can exist stably in the liquid fertilizer, are not easy to settle, and can show a certain slow release effect.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. A urea phosphate mother liquor slow-release suspension liquid fertilizer is prepared from the following raw materials in parts by weight:
urea phosphate mother liquor: 1000 parts of (A);
pH regulator: 90-100 parts of a solvent;
macronutrient-containing compound: 200-500 parts;
suspending agent: 15-30 parts of a solvent;
the suspending agent is xanthan gum, polyacrylamide and clay mineral; the clay mineral is one or more of montmorillonite, sepiolite, attapulgite and bentonite; the mass ratio of the xanthan gum to the polyacrylamide to the clay mineral is 10: (4-10): (1-4);
the compound containing macroelements is one or more of urea, ammonium sulfate, ammonium polyphosphate, potassium pyrophosphate, potassium tripolyphosphate, urea ammonium nitrate solution, potassium chloride, potassium nitrate, potassium sulfate, industrial monopotassium phosphate and industrial monoammonium phosphate.
2. The urea phosphate mother liquor slow-release suspension liquid fertilizer as claimed in claim 1, wherein the urea phosphate mother liquor is a supernatant of a residual liquid obtained after crystallization separation for preparing a urea phosphate product after reaction of phosphoric acid and urea;
the temperature of cooling separation is 10-20 ℃.
3. The urea phosphate mother liquor slow release suspended liquid fertilizer of claim 1, wherein P in the urea phosphate mother liquor2O5The mass fraction of (A) is 21-30%; the mass fraction of the N element is 7-11%; the mass fraction of the metal ions is 3-7%.
4. The urea phosphate mother liquor slow-release suspension liquid fertilizer according to claim 1, wherein the pH regulator is ammonium bicarbonate and/or ammonia water.
5. The urea phosphate mother liquor slow-release suspension liquid fertilizer as claimed in claim 1, wherein the clay mineral has a particle size of < 200 mesh.
6. The urea phosphate mother liquor slow-release suspension liquid fertilizer as claimed in any one of claims 1 to 5, characterized in that the raw materials further comprise 15 to 20 parts of organic fertilizer;
the organic fertilizer comprises one or more of mineralized humic acid, mineralized potassium fulvate and biochemical potassium fulvate.
7. The preparation method of the urea phosphate mother liquor slow-release suspension liquid fertilizer as claimed in claim 1, comprising the following steps:
A) adding 90-100 parts of pH regulator into 1000 parts of urea phosphate mother liquor to obtain mixed mother liquor with the pH value of 3.0-7.0;
B) adding 200-500 parts by weight of a compound containing major elements into the mixed mother liquor to obtain a suspended fertilizer mother liquor;
C) adding 15-30 parts by weight of a suspending agent into the suspended fertilizer mother liquor, and dispersing and emulsifying to obtain a urea phosphate mother liquor slow-release suspended liquid fertilizer;
the suspending agent is one or more of xanthan gum, polyacrylamide and clay minerals; the clay mineral is one or more of montmorillonite, sepiolite, attapulgite and bentonite.
8. The method according to claim 7, wherein the rotation speed of the dispersion emulsification in the step C) is 8000-10000 rpm;
the emulsifying time is 3-5 min.
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| US4456463A (en) * | 1982-10-15 | 1984-06-26 | Stoller Enterprises, Inc. | Ammonia stabilized high analysis liquid fertilizers |
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| CN104291288B (en) * | 2014-09-19 | 2017-02-15 | 贵州大学 | Method for preparing monoammonium phosphate and co-producing special compound fertilizer for potatoes |
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| CN107652038A (en) * | 2017-10-11 | 2018-02-02 | 金正大生态工程集团股份有限公司 | A kind of method that sulphur urea phosphate fertilizer is produced using urea phosphate mother liquor |
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