CN112390687A - Slow-release fertilizer and preparation method thereof - Google Patents
Slow-release fertilizer and preparation method thereof Download PDFInfo
- Publication number
- CN112390687A CN112390687A CN202011349886.2A CN202011349886A CN112390687A CN 112390687 A CN112390687 A CN 112390687A CN 202011349886 A CN202011349886 A CN 202011349886A CN 112390687 A CN112390687 A CN 112390687A
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- Prior art keywords
- fertilizer
- polyoxyethylene ether
- urea
- slow
- slow release
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Classifications
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C9/00—Fertilisers containing urea or urea compounds
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/40—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting fertiliser dosage or release rate; for affecting solubility
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/90—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting the nitrification of ammonium compounds or urea in the soil
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G5/00—Fertilisers characterised by their form
- C05G5/20—Liquid fertilisers
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
- Y02P60/20—Reduction of greenhouse gas [GHG] emissions in agriculture, e.g. CO2
- Y02P60/21—Dinitrogen oxide [N2O], e.g. using aquaponics, hydroponics or efficiency measures
Abstract
The invention relates to a slow release fertilizer and a preparation method thereof, which are characterized by comprising a slow release nitrogen fertilizer; the slow release nitrogen fertilizer is formed by polymerizing polyoxyethylene ether, formaldehyde and urea; the number of carbon atoms in the polyoxyethylene ether is 4-28. The fertilizer has ultralow interfacial tension, is favorable for the absorption of plants to nutrients when being applied as a foliar fertilizer, can reduce the fluidity of nitrogen, and has better slow-release effect when being applied as a base fertilizer.
Description
Technical Field
The invention relates to a slow release fertilizer and a preparation method thereof.
Background
The urea has good fluidity and is easy to run off along with water, so the utilization rate is about 20 percent, the urea formaldehyde synthesized by formaldehyde and urea can slow down the fluidity of the urea and improve the utilization rate of the urea, and the urea formaldehyde has better slow release effect, is used for rhizosphere fertilization at present and can obviously improve the utilization rate of the fertilizer.
The urea is used as the foliar fertilizer, and because the urea has larger interfacial tension, the interfacial tension needs to be reduced by means of a surfactant during use, so that the utilization rate of the urea is improved.
At present, no product which has a good slow release effect and can improve the utilization rate of a nitrogen fertilizer as rhizosphere fertilization and still can improve the utilization rate of the fertilizer without the aid of a surfactant as foliar fertilization exists.
Disclosure of Invention
The invention provides a slow release fertilizer and a preparation method thereof, which solve the technical problems that 1) rhizosphere fertilization has better slow release effect and can improve the utilization rate of a nitrogen fertilizer; 2) the foliar fertilization can still improve the utilization rate of the nitrogen fertilizer without the need of a surfactant.
In order to solve the technical problems, the invention adopts the following technical scheme:
a slow release fertilizer contains a slow release nitrogen fertilizer; the slow release nitrogen fertilizer is prepared by condensing polyoxyethylene ether, formaldehyde and urea; the number of carbon atoms in the polyoxyethylene ether is 4-28.
The slow-release nitrogen fertilizer is prepared according to the following steps:
1) preparing polyoxyethylene ether formal: mixing polyoxyethylene ether and formaldehyde, and carrying out condensation reaction to obtain polyoxyethylene ether formal;
2) preparing polyoxyethylene ether formal urea: adding urea into polyoxyethylene ether formal, and carrying out condensation reaction in an alkaline environment to obtain liquid polyoxyethylene ether formal urea; or
Adding urea into polyoxyethylene ether formal, carrying out condensation reaction in an alkaline environment, and drying to obtain polyoxyethylene ether formal urea;
the mol ratio of the polyoxyethylene ether to the formaldehyde to the urea is 1: 1-2.5: 0.5-2; the formaldehyde is provided by 30 to 45 percent of formaldehyde aqueous solution.
Preferably, the condensation reaction in the step 1) is carried out under the conditions of-0.10 to-0.05 Mpa of pressure, 75 to 120 ℃ of temperature and 40 to 120min of reaction time.
Preferably, the alkaline environment in the step 2) has a pH value of 10-14;
the condensation reaction is carried out under the conditions that the temperature is 65-100 ℃ and the reaction time is 40-120 min; the drying condition is that the drying temperature is 20-145 ℃, and the drying is carried out until the water content is lower than 2%.
Preferably, the condensation reaction in step 1) is carried out under a condition of pH 2-4.5 or pH 10-14.
A preparation method of a slow release fertilizer comprises the steps of adding a slow release nitrogen fertilizer into the fertilizer to obtain the slow release fertilizer; or
Mixing the slow-release nitrogen fertilizer with the fertilizer raw materials to obtain a slow-release fertilizer;
the fertilizer is one of a water-soluble fertilizer, a compound fertilizer, an organic-inorganic fertilizer, a biological organic fertilizer and an organic fertilizer;
the fertilizer raw materials are one or more of urea, ammonium sulfate, ammonium monohydrogen phosphate, diammonium phosphate, monopotassium phosphate, potassium nitrate, potassium sulfate, humic acid, bentonite and potassium chloride.
The mass ratio of the slow-release nitrogen fertilizer to the fertilizer is 0.01-100: 0-99.99.
The invention has the following beneficial technical effects:
1. according to the preparation method, raw materials are selected, reaction conditions are controlled, so that the prepared polyoxyethylene ether formal urea has good water solubility and ultralow interfacial tension, and the utilization rate of the nitrogen fertilizer can be improved on the premise of not using a surfactant for foliar fertilization.
2. This application has reduced the mobility of urea through condensing urea, can regard as slow release fertilizer to use, through the rhizosphere fertilization, can improve the utilization ratio of fertilizer.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
A slow release fertilizer contains a slow release nitrogen fertilizer; the slow release nitrogen fertilizer is formed by polymerizing polyoxyethylene ether, formaldehyde and urea; the polyoxyethylene ether is alkylphenol polyoxyethylene 4 with 23-25 carbon atoms.
The slow-release nitrogen fertilizer is prepared according to the following steps:
1) preparing polyoxyethylene ether formal: mixing polyoxyethylene ether and formaldehyde, and reacting for 60min under the conditions of-0.10 Mpa pressure, 105 ℃ temperature and pH of 2.5 to obtain polyoxyethylene ether formal;
2) preparing polyoxyethylene ether formal urea: adding urea into polyoxyethylene ether formal, and reacting for 90min under the conditions that the pH is 12 and the temperature is 80 ℃ to obtain liquid polyoxyethylene ether formal urea, wherein the obtained liquid polyoxyethylene ether formal urea is the liquid slow-release nitrogen fertilizer. Or
Spraying the obtained liquid polyoxyethylene ether formal urea at inlet temperature of 120 deg.C and outlet temperature of 60 deg.C
And (4) performing spray drying until the water content is 1.2 to obtain polyoxyethylene ether formal urea, namely the slow-release nitrogen fertilizer.
The mol ratio of the polyoxyethylene ether to the formaldehyde to the urea is 1:2.5: 1; the formaldehyde is provided by a 36% formaldehyde aqueous solution.
The liquid polyoxyethylene ether formal urea is diluted by 1000 times by water, and the interfacial tension of the product is detected by a tensiometer TX500C model drop-transfer interfacial tensiometer, and the result is 5.4 multiplied by 10-3mN/m; the urea was diluted 1000 times with water and the interfacial tension of the product was measured using a tensiometer model TX500C transdrop interfacial tensiometer, resulting in 7.5 × 10-2mN/m。
Example 2
A slow release fertilizer contains a slow release nitrogen fertilizer; the slow release nitrogen fertilizer is formed by polymerizing polyoxyethylene ether, formaldehyde and urea; the polyoxyethylene ether is AE0-7 with carbon atom number of 15-17.
The slow-release nitrogen fertilizer is prepared according to the following steps:
3) preparing polyoxyethylene ether formal: mixing polyoxyethylene ether and formaldehyde, and reacting for 80min under the conditions of-0.08 Mpa pressure, 110 ℃ temperature and pH 12 to obtain polyoxyethylene ether formal;
4) preparing polyoxyethylene ether formal urea: adding urea into polyoxyethylene ether formal, and reacting for 60min under the conditions that the pH is 12 and the temperature is 100 ℃ to obtain liquid polyoxyethylene ether formal urea, wherein the obtained liquid polyoxyethylene ether formal urea is the liquid slow-release nitrogen fertilizer. Or
And drying the obtained liquid polyoxyethylene ether formal urea under the conditions that the temperature is 60 ℃ and the pressure is-5 Kpa until the moisture is 1.5 to obtain the polyoxyethylene ether formal urea, namely the slow-release nitrogen fertilizer.
The mol ratio of the polyoxyethylene ether to the formaldehyde to the urea is 1:1.8: 0.7; the formaldehyde is provided by a 40% formaldehyde aqueous solution.
The liquid polyoxyethylene ether formal urea is diluted by 1000 times by water, and the interfacial tension of the product is detected by using a tensiometer TX500C model drop-transfer interfacial tensiometer, and the result is 6.3 multiplied by 10-3mN/m; diluting urea with water 1000 times, and detecting product with tensiometer model TX500C rotary drop interfacial tensiometerThe interfacial tension of (2) was found to be 7.5X 10-2mN/m。
Example 3
A slow release fertilizer contains a slow release nitrogen fertilizer; the slow release nitrogen fertilizer is formed by polymerizing polyoxyethylene ether, formaldehyde and urea; the polyoxyethylene ether is AE0-9 with carbon atom number of 19-21.
The slow-release nitrogen fertilizer is prepared according to the following steps:
5) preparing polyoxyethylene ether formal: mixing polyoxyethylene ether and formaldehyde, and reacting for 100min under the conditions of-0.05 Mpa pressure, 90 ℃ temperature and pH 13 to obtain polyoxyethylene ether formal;
6) preparing polyoxyethylene ether formal urea: adding urea into polyoxyethylene ether formal, and reacting for 50min under the conditions that the pH is 10 and the temperature is 100 ℃ to obtain the liquid polyoxyethylene ether formal urea. Or
And naturally airing the obtained liquid polyoxyethylene ether formal urea until the water content is 1.8 to obtain the polyoxyethylene ether formal urea.
Adding liquid polyoxyethylene ether formal urea into the liquid water-soluble fertilizer to obtain the liquid slow-release water-soluble fertilizer; the proportion of the liquid water-soluble fertilizer is 10-15-5. Or
Adding polyoxyethylene ether formal urea into the water-soluble fertilizer and uniformly mixing to obtain the slow-release water-soluble fertilizer; the proportion of the water soluble fertilizer is 10-30-10.
The mol ratio of the polyoxyethylene ether to the formaldehyde to the urea is 1:1.8: 1; the formaldehyde is provided by a 36% formaldehyde aqueous solution.
The liquid polyoxyethylene ether formal urea is diluted by 1000 times by water, and the interfacial tension of the product is detected by using a tensiometer TX500C model drop-transfer interfacial tensiometer, and the result is 7.8 multiplied by 10-3mN/m; the urea was diluted 1000 times with water and the interfacial tension of the product was measured using a tensiometer model TX500C transdrop interfacial tensiometer, resulting in 7.5 × 10-2mN/m。
Example 4
A slow release fertilizer contains a slow release nitrogen fertilizer; the slow release nitrogen fertilizer is formed by polymerizing polyoxyethylene ether, formaldehyde and urea; the polyoxyethylene ether is fatty acid polyoxyethylene methyl ether with 16-18 carbon atoms.
The slow-release nitrogen fertilizer is prepared according to the following steps:
7) preparing polyoxyethylene ether formal: mixing polyoxyethylene ether and formaldehyde, and reacting for 100min under the conditions of-0.05 Mpa pressure, 100 ℃ temperature and pH 14 to obtain polyoxyethylene ether formal;
8) preparing polyoxyethylene ether formal urea: adding urea into polyoxyethylene ether formal, and reacting for 50min at the pH of 10 and the temperature of 100 ℃ to obtain liquid polyoxyethylene ether formal urea, wherein the obtained liquid polyoxyethylene ether formal urea is the liquid slow-release nitrogen fertilizer. Or
And naturally airing the obtained liquid polyoxyethylene ether formal urea until the water content is 1.8 to obtain the polyoxyethylene ether formal urea, namely the slow-release nitrogen fertilizer.
Adding the liquid polyoxyethylene ether formal urea and the compound fertilizer raw materials into a granulation roller, and granulating, drying, screening and cooling to obtain the slow-release compound fertilizer.
Adding polyoxyethylene ether formal urea and the compound fertilizer raw materials into a granulation roller together, and granulating, drying, screening and cooling to obtain the slow-release compound fertilizer.
The mol ratio of the polyoxyethylene ether to the formaldehyde to the urea is 1:2.0: 1.2; the formaldehyde is provided by a 36% formaldehyde aqueous solution.
The liquid polyoxyethylene ether formal urea is diluted by 1000 times by water, and the interfacial tension of the product is detected by using a tensiometer TX500C model drop-transfer interfacial tensiometer, and the result is 6.9 multiplied by 10-3mN/m; the urea was diluted 1000 times with water and the interfacial tension of the product was measured using a tensiometer model TX500C transdrop interfacial tensiometer, resulting in 7.5 × 10-2mN/m。
Example 5
A slow release fertilizer contains a slow release nitrogen fertilizer; the slow release nitrogen fertilizer is formed by polymerizing polyoxyethylene ether, formaldehyde and urea; the polyoxyethylene ether is AE0-12 with the carbon number of 24-26.
And mixing the slow-release nitrogen fertilizer, the large-particle urea, the granular diammonium phosphate and the granular potassium chloride according to a mass ratio of 8:20:30:42 to obtain the slow-release mixed fertilizer.
The beneficial effects of the present invention are further illustrated below in conjunction with experimental data:
experiment one
Test material
1, materials and methods:
1.1 test site: sandeng (cigarette table) agricultural science and technology limited.
1.2 test detection: chlorophyll relative content (SPAD).
1.3 test materials: urea and treatment 1 (composition of urea and polyoxyethylene ether formal urea prepared in example 2 of the present application in a mass ratio of 95: 5).
1.4 Experimental implementation: two acres of adjacent tomato fields are taken, tomatoes are simultaneously sowed, and when the tomatoes grow for 45 days, the tomatoes are simultaneously treated in a way that urea and treatment 1 (a composition prepared from the urea and polyoxyethylene ether formal urea prepared in the embodiment 2 of the application according to a mass ratio of 95: 5) are diluted by 1000 times and sprayed on the leaves of the tomatoes in a leaf surface spraying way, wherein the treatment rate is 1 acre per treatment, and the using amount of the treatment solution is 20 kg/acre.
1.5 detection method: before treatment, respectively randomly picking 30 leaves from two acres of fields to be treated, detecting the relative content of the green leaves by adopting a SPAD502 chlorophyll content tester, and averaging; after 72h of treatment, 30 leaves are randomly picked from each treatment, a SPAD502 chlorophyll content tester is adopted to detect the relative content of green leaves, and an average value is taken.
The method is consistent except that the treatment is different.
2 results and analysis
The relative chlorophyll content (SPAD) is shown in Table 1
TABLE 1
| Relative chlorophyll content (SPAD) before treatment | Treating for 72h chlorophyll relative content (SPAD) | |
| Urea | 33.8 | 38.7 |
| Process 1 | 33.6 | 45.6 |
The molecular formula of the leaf green a is C55H72O5N4Mg, the molecular formula of leaf green b is C55H70O6N4Mg, namely, the plant leaves absorb nitrogen fertilizer and are partially converted into chlorophyll, as can be seen from the data in Table 1, the addition of treatment 1 (the composition of urea and polyoxyethylene ether formal urea prepared in the example 2 of the present application according to the mass ratio of 95: 5) can obviously improve the content of chlorophyll in the leaves, and the treatment 1 (the composition of urea and polyoxyethylene ether formal urea prepared in the example 2 of the present application according to the mass ratio of 95: 5) can obviously improve the utilization rate of nitrogen compared with urea. The method does not use an auxiliary agent as a foliar fertilizer, and can improve the utilization rate of nitrogen.
Experiment two
Test material
1, materials and methods:
1.1 test site: sandeng (cigarette table) agricultural science and technology limited.
1.2 test detection: initial nutrient release rate (%), nutrient release period (day), and 28-day cumulative nutrient release rate (%), converted by detecting nitrogen content.
1.3 test materials: the polyoxyethylene ether formal urea prepared in example 2.
1.4 Experimental implementation: the polyoxyethylene ether formal urea prepared in example 2 was tested for initial nutrient release rate (%), nutrient release period (days) and 28-day cumulative nutrient release rate (%) as specified in GB/T23348-2009 slow release fertilizer.
1.5 detection standard: GB/T23348-2009 slow-release fertilizer.
The method is consistent with other management methods except different processing.
2 results and analysis
The initial nutrient release rate (%), the nutrient release period (day), and the 28-day cumulative nutrient release rate (%) are shown in Table 2.
TABLE 2
| Test treatment | Example 2 |
| Initial nutrient release rate (%) | 6 |
| Nutrient release period (Tian) | 84 |
| Cumulative nutrient release rate (%). in 28 days | 58 |
As can be seen from Table 2, the polyoxyethylene ether formal urea prepared by the method can meet the requirements of GB/T23348-.
Claims (7)
1. A slow release fertilizer is characterized by containing a slow release nitrogen fertilizer; the slow release nitrogen fertilizer is prepared by condensing polyoxyethylene ether, formaldehyde and urea; the number of carbon atoms in the polyoxyethylene ether is 4-28.
2. The slow release fertilizer of claim 1, wherein the slow release nitrogen fertilizer is produced by the steps of:
1) preparing polyoxyethylene ether formal: mixing polyoxyethylene ether and formaldehyde, and carrying out condensation reaction to obtain polyoxyethylene ether formal;
2) preparing polyoxyethylene ether formal urea: adding urea into polyoxyethylene ether formal, and carrying out condensation reaction in an alkaline environment to obtain liquid polyoxyethylene ether formal urea; or
Adding urea into polyoxyethylene ether formal, carrying out condensation reaction in an alkaline environment, and drying to obtain polyoxyethylene ether formal urea;
the mol ratio of the polyoxyethylene ether to the formaldehyde to the urea is 1: 1-2.5: 0.5-2; the formaldehyde is provided by 30 to 45 percent of formaldehyde aqueous solution.
3. The slow release fertilizer of claim 2, wherein the condensation reaction in step 1) is carried out under a pressure of-0.10 to-0.05 MPa, at a temperature of 75 to 120 ℃ and for a reaction time of 40 to 120 min.
4. The slow release fertilizer of claim 3, wherein the alkaline environment in step 2) is a pH of 10 to 14;
the condensation reaction is carried out under the conditions that the temperature is 65-100 ℃ and the reaction time is 40-120 min; the drying temperature is 20-145 ℃, and the drying is carried out until the water content is lower than 2%.
5. The slow release fertilizer according to any one of claims 2, 3 and 4, wherein the condensation reaction in step 1) is carried out under a condition of pH 2 to 4.5 or pH 10 to 14.
6. A preparation method of a slow release fertilizer is characterized in that a slow release nitrogen fertilizer is added into the fertilizer to obtain the slow release fertilizer; or
Mixing the slow-release nitrogen fertilizer with the fertilizer raw materials to obtain a slow-release fertilizer;
the fertilizer is one of a water-soluble fertilizer, a compound fertilizer, an organic-inorganic fertilizer, a biological organic fertilizer and an organic fertilizer;
the fertilizer raw materials are one or more of urea, ammonium sulfate, ammonium monohydrogen phosphate, diammonium phosphate, monopotassium phosphate, potassium nitrate, potassium sulfate, humic acid, bentonite and potassium chloride.
7. The method for preparing a slow-release fertilizer according to claim 6, wherein the mass ratio of the slow-release nitrogen fertilizer to the fertilizer is 0.01-100: 0-99.99.
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| CN202011349886.2A CN112390687A (en) | 2020-11-26 | 2020-11-26 | Slow-release fertilizer and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030154754A1 (en) * | 2001-08-30 | 2003-08-21 | Giancarlo Costa | Method for making nitrogenous and complex fertilizers in highly homogenized spherical granule form starting from urea formaldehyde liquid resins and the fertilizer made thereby |
| CN104892150A (en) * | 2015-05-27 | 2015-09-09 | 山东农业大学 | Instant slow-release nitrogen fertilizer and preparation method thereof |
| CN110342992A (en) * | 2019-06-28 | 2019-10-18 | 深圳诺普信农化股份有限公司 | The preparation method of urea-formaldehyde fertilizer water slurry |
-
2020
- 2020-11-26 CN CN202011349886.2A patent/CN112390687A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030154754A1 (en) * | 2001-08-30 | 2003-08-21 | Giancarlo Costa | Method for making nitrogenous and complex fertilizers in highly homogenized spherical granule form starting from urea formaldehyde liquid resins and the fertilizer made thereby |
| CN104892150A (en) * | 2015-05-27 | 2015-09-09 | 山东农业大学 | Instant slow-release nitrogen fertilizer and preparation method thereof |
| CN110342992A (en) * | 2019-06-28 | 2019-10-18 | 深圳诺普信农化股份有限公司 | The preparation method of urea-formaldehyde fertilizer water slurry |
Non-Patent Citations (1)
| Title |
|---|
| 殷宗泰编: "《精细化工概论》", 31 October 1985, 化学工业出版社 * |
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Application publication date: 20210223 |