Promoting growth type macroelement water-soluble fertilizer, preparation method and application thereof

Abstract

The application belongs to the technical field of new fertilizers, and particularly relates to a growth-promoting macroelement water-soluble fertilizer, a preparation method and application. The fertilizer comprises the following raw materials in parts by weight: 4-6 parts of tertiary amine synergist, 220-230 parts of potassium dihydrogen phosphate, 350-360 parts of urea, 3-5 parts of composite amino acid, 3-5 parts of sorbitol and 15-20 parts of ethylene glycol, wherein the tertiary amine synergist is N,N,N',N'-tetra(2-fluorobenzyl diamino) diphenyl ether. The application aims to innovate the macroelement water-soluble fertilizer product, prepare a new type of tertiary amine synergist, effectively improve the added value and use effect of the macroelement water-soluble fertilizer, and provide a new direction and thought for the development and use of the functional macroelement water-soluble fertilizer new technology.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of new fertilizers, and particularly relates to a growth-promoting macroelement water-soluble fertilizer, a preparation method and application, which can significantly increase the plant height, stem diameter and total net weight of corn plants, significantly promote the growth of corn, and reduce the application amount of fertilizer and the impact of fertilizer on the ecological environment during the release process. BACKGROUND

[0002] As is known to all, with the increasing global demand for food, scientific application of macroelement water-soluble fertilizer has become an indispensable way to achieve maximum agricultural productivity and food security in population growth. The wide use of macroelement water-soluble fertilizer provides a very effective and adaptable nutrient management method, which completely changes the modern agricultural method. Macroelement water-soluble fertilizer is easy to apply, can accurately control the distribution of nutrients in crops, promote the absorption of nutrients, and is suitable for various irrigation schemes, so that farmers can fertilize more conveniently, and thus has become one of the important choices for sustainable development in modern agriculture. At the same time, it can effectively reduce the negative impact on the environment and fertilizer waste. However, the existing macroelement water-soluble fertilizer products are uneven, and there are problems such as low utilization rate of compound nutrients, and unsatisfactory absorption effect of plants. There are deficiencies in the absorption and utilization rate of fertilizer by crops, and the targeting of fertilizer application for plants at different growth stages is not strong, resulting in a mismatch between fertilizer supply and plant growth demand, causing resource waste.

[0003] At present, functional macroelement water-soluble fertilizer plays an important role in promoting crop growth, improving crop stress resistance, promoting fruit coloration, and has good penetration regulation, antioxidant activity and good water retention capacity, and has been widely developed and used. Especially using tertiary amine synergist as the component required for promoting crop growth, mainly amine new fat (DA-6), which has a tertiary amine structure and obvious growth-promoting effect, but is mainly in liquid form, and needs to be further reacted with citric acid to form a salt to be added to the fertilizer. In addition, amine new fat (DA-6) has been registered as a plant growth regulator and cannot be directly added to the fertilizer for use, but can only be used alone, which greatly increases the labor cost of farmers. In addition, the existing functional macroelement water-soluble fertilizer has poor effect in promoting crop growth and increasing yield, which limits its use efficiency. SUMMARY

[0004] In order to solve the above technical problems, the present application provides a growth-promoting macroelement water-soluble fertilizer, a preparation method and application, which aims to innovate the macroelement water-soluble fertilizer product and prepare a new type of tertiary amine synergist, which can effectively improve the added value and use effect of the macroelement water-soluble fertilizer, and provide a new direction and idea for the development and use of functional macroelement water-soluble fertilizer new technology.

[0005] The application is achieved by providing a growth-promoting macroelement water-soluble fertilizer, comprising the following raw materials in parts by weight: 4-6 parts of a tertiary amine synergist, 220-230 parts of potassium dihydrogen phosphate, 350-360 parts of urea, 3-5 parts of a compound amino acid, 3-5 parts of sorbitol, and 15-20 parts of ethylene glycol.

[0006] Preferably, the tertiary amine synergist is N,N,N',N'-tetrakis(2-fluorobenzyl diamino) diphenyl ether with a molecular formula of C 40 H 32 F4N2O, belonging to a P 21 / c space group of a monoclinic crystal system, and having the following structural formula:

[0007]

[0008] Preferably, in the tertiary amine synergist, the bond length of C-F ranges from 1.36(1) to 1.37(1) The bond length of C-N ranges from 1.36(1) to 1.37(1) The bond angle of C-O-C is 112.5(3) o The bond angle of C-N-C ranges from 116.6(3) to 122.0(3) o .

[0009] The application provides a preparation method of the growth-promoting macroelement water-soluble fertilizer, comprising the following steps: weighing each raw material of the growth-promoting macroelement water-soluble fertilizer according to parts by weight, and then fully mixing and uniformly.

[0010] Preferably, in the preparation method, the preparation method of the tertiary amine synergist comprises the following steps:

[0011] 1) taking 4,4'-diamino diphenyl ether and 2-fluorobenzyl chloride as raw materials, adjusting pH to 10 in acetonitrile as a solvent, heating and refluxing at a certain temperature for a certain time, and reacting according to a certain proportion;

[0012] 2) after the reaction is completed, the product is suction filtered for a certain time;

[0013] 3) finally, drying at a certain temperature for a certain time to obtain N,N,N',N'-tetrakis(2-fluorobenzyl diamino) diphenyl ether, i.e. the tertiary amine synergist.

[0014] Preferably, in the step 1), the molar ratio of the reactants 4,4'-diamino diphenyl ether and 2-fluorobenzyl chloride is 1:4-5; the reaction temperature is 90-95°C, and the reaction time is 4-6h.

[0015] Preferably, in the step 2), the suction filtering time after the reaction is completed is 1-2h; and in the step 3), the drying temperature is 85-90°C, and the drying time is 1-2h.

[0016] The application provides a method for applying the growth-promoting macronutrient water-soluble fertilizer, and the growth-promoting macronutrient water-soluble fertilizer is applied by drip irrigation at an application amount of 3.5-4.5 kg / mu, or is applied by irrigation at an application amount of 4-8 kg / mu.

[0017] The application provides an application of the growth-promoting macronutrient water-soluble fertilizer, and the growth-promoting macronutrient water-soluble fertilizer is used when a plant needs macronutrients.

[0018] Preferably, the plant is corn.

[0019] Compared with the prior art, the application has the advantages that:

[0020] The application first adopts an organic chemical synthesis method, uses simple acetonitrile as a solvent to reflux, and prepares the growth-promoting tertiary amine synergist, no by-products are generated in the synthesis process, the preparation process is simple, the solvent acetonitrile can be recycled and reused multiple times, is green and environmentally friendly, no three wastes are generated, and the yield of the tertiary amine synergist is high. Further, the tertiary amine synergist, nitrogen, phosphorus, potassium, and compound amino acids are compounded according to a reasonable proportion, the product formula is scientific, safe and environmentally friendly, the method is simple, and the production cost is low. The growth-promoting macronutrient water-soluble fertilizer prepared by the application has the advantages of good water solubility, high product use efficiency, high economic value, and the like, and can significantly improve the net height and net weight of corn plants. In production, the production process is simple, convenient, and easy to operate, the product has high economic benefits, social benefits, and popularization value. BRIEF DESCRIPTION OF DRAWINGS

[0021] Figure 1 A single crystal structure diagram of the tertiary amine synergist N,N,N',N'-tetra(2-fluorobenzyl diamino) diphenyl ether prepared in Example 1. DETAILED DESCRIPTION

[0022] In order to make the purpose, technical scheme and advantages of the application more clear, the application will be further described in detail below with reference to the drawings and examples. It should be understood that the specific examples described herein are only used to explain the application, and are not used to limit the application.

[0023] Example 1,

[0024] (I) Preparation method of the tertiary amine synergist N,N,N',N'-tetra(2-fluorobenzyl diamino) diphenyl ether

[0025] Into a 500 mL round bottom flask, 30.00 g (149.82 mmol) of 4,4'-oxydianiline was weighed out, followed by 86.64 g (599.28 mmol) of 2-fluorobenzyl chloride, then 150 mL of acetonitrile was added, the pH was adjusted to 10, and the reaction was carried out at 90°C for 5 h. After the reaction was completed and the solution was cooled, it was filtered and dried at 85°C for 1 h to obtain 83.15 g of white powder with a yield of 98.97%. 0.10 g of the white powder was dissolved in 10 mL of a mixture of dichloromethane and methanol (1:1 by volume), and colorless block crystals were obtained by solvent evaporation for standby use. The reaction formula of the above reaction is as follows:

[0026]

[0027] (II) Determination of the crystal structure of the tertiary amine synergist N,N,N',N'-tetrakis(2-fluorobenzyl diamino) diphenyl ether:

[0028] The above colorless block crystals were taken to a Bruker D8-ray diffractometer, and graphite monochromatized radiation was used as the diffraction light source to collect the diffraction intensity data of the single crystal. The data was reduced to obtain the structure of the tertiary amine synergist N,N,N',N'-tetrakis(2-fluorobenzyl diamino) diphenyl ether as shown in Figure 1 . The molecular formula of the compound is C 40 H 32 F4N2O, which belongs to the monoclinic P 21 / c space group. The specific single crystal data is shown in Table 1. In the compound, the bond length of C–F ranges from C–N ranges from the bond angle of C–O–C is 112.5(3) o , and the bond angle of C–N–C ranges from 116.6(3) to 122.0(3) o . The specific bond length and bond angle data are shown in Table 3.

[0029] Table 1 Crystallographic data table of the tertiary amine synergist

[0030]

[0031] Table 2 Bond length and bond angle table of the tertiary amine synergist

[0032]

[0033] (III) Preparation method of a growth-promoting macroelement water-soluble fertilizer

[0034] Accurately weigh the tertiary amine synergist N,N,N',N'-tetra(2- fluorobenzyl diamino) diphenyl ether 5 g, composite amino acid 5 g, sorbitol 5 g, ethylene glycol 15 g, potassium dihydrogen phosphate 220 g, urea 350 g, grind and mix well to obtain the growth-promoting macroelement water-soluble fertilizer.

[0035] Example 2,

[0036] Accurately weigh the tertiary amine synergist N,N,N',N'-tetra(2- fluorobenzyl diamino) diphenyl ether 4 g prepared in Example 1, composite amino acid 5 g, sorbitol 5 g, ethylene glycol 15 g, potassium dihydrogen phosphate 220 g, urea 350 g, grind and mix well to obtain the growth-promoting macroelement water-soluble fertilizer.

[0037] Example 3,

[0038] Accurately weigh the tertiary amine synergist N,N,N',N'-tetra(2- fluorobenzyl diamino) diphenyl ether 6 g prepared in Example 1, composite amino acid 5 g, sorbitol 5 g, ethylene glycol 15 g, potassium dihydrogen phosphate 220 g, urea 350 g, grind and mix well to obtain the growth-promoting macroelement water-soluble fertilizer.

[0039] Example 4,

[0040] Accurately weigh the tertiary amine synergist N,N,N',N'-tetra(2- fluorobenzyl diamino) diphenyl ether 4 g prepared in Example 1, composite amino acid 4 g, sorbitol 5 g, ethylene glycol 20 g, potassium dihydrogen phosphate 220 g, urea 350 g, grind and mix well to obtain the growth-promoting macroelement water-soluble fertilizer.

[0041] Example 5,

[0042] Accurately weigh the tertiary amine synergist N,N,N',N'-tetra(2- fluorobenzyl diamino) diphenyl ether 6 g prepared in Example 1, composite amino acid 4 g, sorbitol 4 g, ethylene glycol 20 g, potassium dihydrogen phosphate 220 g, urea 350 g, grind and mix well to obtain the growth-promoting macroelement water-soluble fertilizer.

[0043] Example 6,

[0044] Accurately weigh the tertiary amine synergist N,N,N',N'-tetra(2- fluorobenzyl diamino) diphenyl ether 5 g prepared in Example 1, composite amino acid 3 g, sorbitol 5 g, ethylene glycol 15 g, potassium dihydrogen phosphate 230 g, urea 360 g, grind and mix well to obtain the growth-promoting macroelement water-soluble fertilizer.

[0045] Example 7,

[0046] The tertiary amine synergist N,N,N',N'-tetra(2-fluorobenzyl diamino) diphenyl ether prepared in Example 1 is accurately weighed 5 g, the composite amino acid is 5 g, sorbitol is 5 g, ethylene glycol is 20 g, potassium dihydrogen phosphate is 230 g, and urea is 360 g, which are ground and uniformly stirred to obtain the growth-promoting type macronutrient water-soluble fertilizer.

[0047] Example 8,

[0048] Corn seedling growth promotion test: after the corn seeds are disinfected, they are placed in a culture dish lined with filter paper, clean sterile cotton is moistened and placed on the filter paper, 20 mL of sterile water is added to keep the seeds moist, and then the culture dish is placed in a constant temperature incubator at 28°C to ensure normal seed germination. After the seeds germinate, corns with the same growth potential are transplanted into a seedling tray. When the first true leaf unfolds, the sample diluted 1000 times in Example 1-7 macronutrient water-soluble fertilizer (the control CK group is the same as Example 1 without adding tertiary amine synergist) is used for root irrigation. After fifteen days, the plant height, net weight and other data are observed, and the results are shown in Table 1.

[0049] Table 1: Data statistics of corn growth promotion test results at different concentrations

[0050] Different treatments Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 CK Average plant height (cm) 44.78 43.85 43.90 43.21 43.96 43.89 44.86 38.62 Average stem diameter (mm) 3.68 3.54 3.65 3.23 3.32 3.28 3.59 3.22 Total net weight (g) 23.31 23.05 22.93 22.88 23.22 22.98 23.27 17.43

[0051] Experimental result analysis: As can be seen from Table 1, compared with the blank control, the average plant height, average stem diameter and total net weight data of the corn plants, the addition of tertiary amine synergist macronutrient water-soluble fertilizer significantly increased the plant height, stem diameter and total net weight of the corn plants. The growth-promoting type macronutrient water-soluble fertilizer prepared in Example 1 is significantly better than the control CK in terms of average plant height, stem diameter and total net weight of corn plants. The average plant height of corn plants is increased by 15.9%, the average stem diameter is increased by 14.3%, and the total net weight is increased by 33.7%. Therefore, it can be concluded that the growth-promoting type macronutrient water-soluble fertilizer of the present application can be widely used. Considering the cost, it can be used by drip irrigation at 3.5-4.5 kg / acre, and by flushing at 4-8 kg / acre.

Claims

1. A growth-promoting macronutrient water-soluble fertilizer, characterized by, By weight parts, including the following raw materials: tertiary amine synergist 4-6 parts, potassium dihydrogen phosphate 220-230 parts, urea 350-360 parts, complex amino acids 3-5 parts, sorbitol 3-5 parts and ethylene glycol 15-20 parts; The tertiary amine synergist is N , N , N ', N - tetra(2-fluorobenzyl diamino)diphenyl ether, molecular formula C 40 H 32 F4N2O, belongs to monoclinic system P 21 / c space group, the structural formula is as follows: ； The bond lengths of C-F range from 1.357(5) to 1.376(4) A, the bond lengths of C-N range from 1.390(4) to 1.455(4) A, the bond angle of C-O-C is 112.5(3) o , the bond angles of C-N-C range from 116.6(3) to 122.0(3) o .

2. A method for preparing a growth-promoting macroelement water-soluble fertilizer, characterized by, The various raw materials of the growth-promoting macroelement water-soluble fertilizer described in claim 1 are weighed according to weight parts, and then fully mixed and uniformly mixed.

3. The method of claim 2, wherein the method is characterized by, The preparation method of the tertiary amine synergist comprises the following steps: 1) 4, 4'-diamino diphenyl ether and 2-fluorobenzyl chloride are used as raw materials, acetonitrile is used as a solvent, the pH value is adjusted to 10, heated to reflux at a certain temperature for a certain time; 2) After the reaction is completed, the product is filtered for a certain time; 3) Finally, dry at a certain temperature for a certain time, to obtain N , N , N ', N '- Tetra (2-fluorobenzyl diamino) diphenyl ether, namely tertiary amine synergist.

4. The method of claim 3, wherein the method is characterized by, In step 1), the molar ratio of the reactants 4, 4'-diamino diphenyl ether and 2-fluorobenzyl chloride is 1:4-5; the reaction temperature is 90-95℃, and the reaction time is 4-6 h.

5. The method of claim 3, wherein the method is characterized by, In step 2), the filtering time after the reaction is completed is 1-2 h; in step 3), the drying temperature is 85-90℃, and the drying time is 1-2 h.

6. A method of applying a growth-promoting macronutrient water-soluble fertilizer, characterized by, The growth-promoting macroelement water-soluble fertilizer described in claim 1 is applied by drip irrigation, and the application amount is 3.5-4.5 kg / mu; or applied by flushing, and the application amount is 4-8 kg / mu.

7. Use of the growth-promoting macro-element water-soluble fertilizer according to claim 1, characterized in that, It is used when plants need a large amount of nutrients.

8. The use of the growth-promoting macroelement water-soluble fertilizer according to claim 7, characterized in that, The plant is corn.

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