Growth-promoting macroelement water-soluble fertilizer as well as preparation method and application thereof

Abstract

The invention belongs to the technical field of novel fertilizers, and particularly relates to a growth promoting type macroelement water-soluble fertilizer and a preparation method and application thereof.The fertilizer is prepared from, by weight, 4-6 parts of tertiary amine synergist, 220-230 parts of monopotassium phosphate, 350-360 parts of urea, 3-5 parts of compound amino acid, 3-5 parts of sorbitol and 15-20 parts of ethylene glycol, the invention relates to N, N '-tetra (2-fluorobenzyl diamido) diphenyl ether. The invention aims at innovating a macroelement water-soluble fertilizer product to prepare the novel tertiary amine synergist, so that the additional value and the use effect of the macroelement water-soluble fertilizer can be effectively improved, and a new direction and a new idea are provided for development and use of a new functional macroelement water-soluble fertilizer technology.

Description

Technical Field

[0001] The present invention belongs to the technical field of novel fertilizers, and specifically relates to a growth-promoting macronutrient water-soluble fertilizer, a preparation method and an application thereof, which can significantly increase the plant height, stem thickness and total net weight of corn plants, significantly promote corn growth, and at the same time reduce the amount of fertilizer applied and reduce the impact of the fertilizer on the ecological environment during the release process. Background Art

[0002] As we all know, with the increasing global demand for food, the scientific application of macronutrient water-soluble fertilizers has become an indispensable way to achieve maximum agricultural productivity and ensure food security in a growing population. The widespread use of macronutrient water-soluble fertilizers provides a very effective and adaptable nutrient management method, which has completely changed contemporary agricultural methods. Macronutrient water-soluble fertilizers are easy to apply, can accurately control the distribution of nutrients in crops, promote nutrient absorption, and are suitable for various irrigation schemes, making it more convenient for farmers to fertilize. Therefore, they have 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 macronutrient water-soluble fertilizer products are uneven, with low composite nutrient utilization and unsatisfactory plant absorption effect. Fertilizers are insufficient in terms of crop absorption and utilization, and the application of fertilizers to plants at different growth stages is not targeted, resulting in a mismatch between fertilizer supply and plant growth needs, resulting in resource waste.

[0003] At present, functional macronutrient water-soluble fertilizers have also played an important role in promoting crop growth, improving crop stress resistance, and promoting fruit color change. At the same time, they also have good osmotic regulation, antioxidant activity, and good water retention capacity. They have been widely developed and used, especially using tertiary amine synergists as ingredients required to promote crop growth, mainly amine new fat (DA-6), which has a tertiary amine structure and has a significant growth-promoting effect, but is mainly in liquid form. The solid needs to be further reacted with citric acid to form a salt before it can be added to the fertilizer, and amine new fat (DA-6) has been registered as a plant growth regulator and cannot be directly added to the fertilizer for use. It can only be used alone, which greatly increases the labor cost of farmers. In addition, the existing functional macronutrient water-soluble fertilizers have poor effects in promoting crop growth and increasing yields, which limits their efficiency. Summary of the invention

[0004] In order to solve the above technical problems, the present invention provides a growth-promoting water-soluble macronutrient fertilizer and a preparation method and application thereof, aiming to innovate the products of water-soluble macronutrient fertilizers and prepare a new tertiary amine enhancer, which can effectively improve the added value and use effect of water-soluble macronutrient fertilizers, and provide new directions and ideas for the development and use of new technologies of functional water-soluble macronutrient fertilizers.

[0005] The present invention is achieved by providing a growth-promoting macronutrient water-soluble fertilizer, which 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 complex amino acids, 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-fluorobenzyldiamino)diphenyl ether, with a molecular formula of C 40 H 32 F4N2O belongs to the monoclinic P 21 / c space group, and its structural formula is as follows:

[0007]

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

[0009] The invention provides a method for preparing a growth-promoting macronutrient water-soluble fertilizer. The raw materials of the growth-promoting macronutrient water-soluble fertilizer are weighed according to weight and then fully mixed.

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

[0011] 1) Using 4,4'-diaminodiphenyl ether and 2-fluorobenzyl chloride as raw materials, in a certain ratio, using acetonitrile as solvent, adjusting the pH value to 10, heating under reflux at a certain temperature, and reacting for a certain time;

[0012] 2) After the reaction is completed, the product is filtered for a certain period of time;

[0013] 3) Finally, drying is performed at a certain temperature for a certain period of time to obtain N,N,N',N'-tetrakis(2-fluorobenzyldiamino)diphenyl ether, i.e., a tertiary amine synergist.

[0014] Preferably, in step 1), the molar ratio of the reactants 4,4'-diaminodiphenyl 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 filtration time after the reaction is completed is 1-2 hours; in the step 3), the drying temperature is 85-90° C. and the drying time is 1-2 hours.

[0016] Provided is a method for applying a growth-promoting macronutrient water-soluble fertilizer, wherein the growth-promoting macronutrient water-soluble fertilizer is applied by drip irrigation at an application rate of 3.5-4.5 kg / mu; or by flushing at an application rate of 4-8 kg / mu.

[0017] The invention provides an application of a growth-promoting macronutrient water-soluble fertilizer, which is used when a large amount of nutrient elements are required for plant growth.

[0018] Preferably, the plant is corn.

[0019] Compared with the prior art, the advantages of the present invention are:

[0020] The present invention first adopts an organic chemical synthesis method, uses simple acetonitrile as a solvent reflux, and prepares a growth-promoting tertiary amine synergist. No by-products are generated during the synthesis process, the preparation process is simple, the solvent acetonitrile can be recycled and reused multiple times, it is green and environmentally friendly, no three wastes are generated, and the yield of the tertiary amine synergist is high. Further, tertiary amine synergists, nitrogen, phosphorus and potassium, composite amino acids, etc. are prepared in a reasonable proportion, and 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 present invention has the advantages of good water solubility, high product utilization efficiency, high economic value, etc., 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, and the product has high economic and social benefits and promotion value. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 This is a single crystal structure diagram of the tertiary amine enhancer N,N,N',N'-tetrakis(2-fluorobenzyldiamino)diphenyl ether prepared in Example 1. DETAILED DESCRIPTION

[0022] In order to make the purpose, technical solution and advantages of the present invention clearer, the present invention is further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0023] Embodiment 1,

[0024] (I) Preparation method of tertiary amine synergist N,N,N',N'-tetrakis(2-fluorobenzyldiamino)diphenyl ether

[0025] Weigh 30.00g (149.82mmol) of 4,4'-diaminodiphenyl ether and 86.64g (599.28mmol) of 2-fluorobenzyl chloride into a 500mL round-bottom flask, then add 150mL of acetonitrile, adjust the pH to 10, and react at 90℃ for 5h. After the reaction is completed, cool and filter, and dry at 85℃ for 1h to obtain 83.15g of white powder with a yield of 98.97%. Weigh 0.10g of the above white powder and dissolve it in 10mL of a mixed solution of dichloromethane and methanol (volume ratio of 1:1), and use the solvent volatilization method to obtain colorless block crystals for use. The reaction formula of the above reaction is as follows:

[0026]

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

[0028] The colorless block crystals were taken and analyzed by graphite monochromatization on a Bruker D8-ray diffractometer. Radiation is used as the diffraction light source to collect the diffraction intensity data of the single crystal. The structure of the tertiary amine synergist N,N,N',N'-tetrakis(2-fluorobenzyldiamino)diphenyl ether is obtained by reduction of the data. Figure 1 The molecular formula of this compound is C 40 H 32 F4N2O belongs to the monoclinic system P 21 / c space group. Specific single crystal data are shown in Table 1. In this compound, the C–F bond length range is The C–N bond length ranges from The bond angle of C–O–C is 112.5(3) o , the bond angle of C–N–C ranges from 116.6(3)–122.0(3) o The specific bond length and angle data are shown in Table 3.

[0029] Table 1 Crystallographic data of tertiary amine synergist

[0030]

[0031] Table 2 Bond length and angle table of tertiary amine synergists

[0032]

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

[0034] Accurately weigh 5 g of tertiary amine enhancer N,N,N',N'-tetrakis(2-fluorobenzyldiamino)diphenyl ether, 5 g of complex amino acid, 5 g of sorbitol, 15 g of ethylene glycol, 220 g of potassium dihydrogen phosphate, and 350 g of urea, grind them and stir them thoroughly to obtain a growth-promoting macronutrient water-soluble fertilizer.

[0035] Embodiment 2,

[0036] Accurately weigh 4 g of the tertiary amine enhancer N,N,N',N'-tetrakis(2-fluorobenzyldiamino)diphenyl ether prepared in Example 1, 5 g of composite amino acid, 5 g of sorbitol, 15 g of ethylene glycol, 220 g of potassium dihydrogen phosphate, and 350 g of urea, grind them, and stir them evenly to obtain a growth-promoting macronutrient water-soluble fertilizer.

[0037] Embodiment 3,

[0038] Accurately weigh 6 g of the tertiary amine enhancer N,N,N',N'-tetrakis(2-fluorobenzyldiamino)diphenyl ether prepared in Example 1, 5 g of composite amino acid, 5 g of sorbitol, 15 g of ethylene glycol, 220 g of potassium dihydrogen phosphate, and 350 g of urea, grind them and stir them evenly to obtain a growth-promoting macronutrient water-soluble fertilizer.

[0039] Embodiment 4,

[0040] Accurately weigh 4 g of the tertiary amine enhancer N,N,N',N'-tetrakis(2-fluorobenzyldiamino)diphenyl ether prepared in Example 1, 4 g of complex amino acid, 5 g of sorbitol, 20 g of ethylene glycol, 220 g of potassium dihydrogen phosphate, and 350 g of urea, grind them and stir them evenly to obtain a growth-promoting macronutrient water-soluble fertilizer.

[0041] Embodiment 5,

[0042] Accurately weigh 6 g of the tertiary amine enhancer N,N,N',N'-tetrakis(2-fluorobenzyldiamino)diphenyl ether prepared in Example 1, 4 g of complex amino acid, 4 g of sorbitol, 20 g of ethylene glycol, 220 g of potassium dihydrogen phosphate, and 350 g of urea, grind them and stir them evenly to obtain a growth-promoting macronutrient water-soluble fertilizer.

[0043] Embodiment 6,

[0044] Accurately weigh 5 g of the tertiary amine enhancer N,N,N',N'-tetrakis(2-fluorobenzyldiamino)diphenyl ether prepared in Example 1, 3 g of composite amino acid, 5 g of sorbitol, 15 g of ethylene glycol, 230 g of potassium dihydrogen phosphate, and 360 g of urea, grind them and stir them evenly to obtain a growth-promoting macronutrient water-soluble fertilizer.

[0045] Embodiment 7,

[0046] Accurately weigh 5 g of the tertiary amine enhancer N,N,N',N'-tetrakis(2-fluorobenzyldiamino)diphenyl ether prepared in Example 1, 5 g of composite amino acid, 5 g of sorbitol, 20 g of ethylene glycol, 230 g of potassium dihydrogen phosphate, and 360 g of urea, grind them and stir them evenly to obtain a growth-promoting macronutrient water-soluble fertilizer.

[0047] Embodiment 8,

[0048] Corn seedling growth promotion test: After the corn seeds are disinfected, place them in a culture dish covered with filter paper, wet clean sterile cotton and place them on the filter paper, add 20 mL of sterile water to keep the seeds moist, and then place the culture dish in a constant temperature incubator at 28°C to ensure that the seeds can germinate normally. After the seeds germinate, select corns with the same growth potential and transplant them into the seedling tray. When the first true leaf begins to unfold, apply a 1000-fold dilution of the macronutrient water-soluble fertilizer of the samples of Examples 1-7 (the control CK group is the same as Example 1 without the addition of tert-butyl ester enhancer and other ingredients) for root irrigation. After fifteen days, observe the data such as plant height and net weight. The results are shown in Table 1.

[0049] Table 1 Statistics of corn growth promotion test results at different concentrations

[0050] Different treatment 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: From Table 1, it can be seen that compared with the blank control, the average plant height, average stem thickness and total net weight data of corn plants, the macronutrient water-soluble fertilizers with tertiary amine synergists significantly increased the plant height, stem thickness and total net weight of corn plants. The growth-promoting macronutrient water-soluble fertilizer prepared in Example 1 was compared with the control CK data, and its average plant height, stem thickness and total net weight of corn plants were significantly better than other treatments. The average plant height of corn plants in the seedling stage increased by 15.9%, the average stem thickness increased by 14.3%, and the total net weight increased by 33.7%. Therefore, it can be concluded that the growth-promoting macronutrient water-soluble fertilizer of the present invention can be widely promoted and used. Considering the cost comprehensively, it is used by drip irrigation: 3.5-4.5 kg / mu; by flushing: 4-8 kg / mu.

Claims

1. A growth-promoting macronutrient water-soluble fertilizer, characterized in that: By weight, it includes the following raw materials: 4–6 parts of tertiary amine enhancer, 220–230 parts of potassium dihydrogen phosphate, 350–360 parts of urea, 3–5 parts of complex amino acids, 3–5 parts of sorbitol and 15–20 parts of ethylene glycol.

2. The growth-promoting macronutrient water-soluble fertilizer according to claim 1, characterized in that: The tertiary amine synergist is N,N,N',N'-tetrakis(2-fluorobenzyldiamino)diphenyl ether, with a molecular formula of C 40 H 32 F4N2O belongs to the monoclinic P 21 / c space group, and its structural formula is as follows:

3. The growth-promoting macronutrient water-soluble fertilizer according to claim 2, characterized in that: In the tertiary amine synergist, the C–F bond length range is The C–N bond length ranges from The bond angle of C–O–C is 112.5(3) o , the bond angle of C–N–C ranges from 116.6(3)–122.0(3) o .

4. A method for preparing a growth-promoting macronutrient water-soluble fertilizer, characterized in that: The various raw materials of the growth-promoting macronutrient water-soluble fertilizer described in claim 1 are weighed according to weight and then mixed thoroughly.

5. The method for preparing the growth-promoting macronutrient water-soluble fertilizer according to claim 4, characterized in that: The preparation method of the tertiary amine synergist comprises the following steps: 1) Using 4,4'-diaminodiphenyl ether and 2-fluorobenzyl chloride as raw materials, in a certain ratio, using acetonitrile as solvent, adjusting the pH value to 10, heating under reflux at a certain temperature, and reacting for a certain time; 2) After the reaction is completed, the product is filtered for a certain period of time; 3) Finally, drying is performed at a certain temperature for a certain period of time to obtain N,N,N',N'-tetrakis(2-fluorobenzyldiamino)diphenyl ether, i.e., a tertiary amine synergist.

6. The method for preparing the growth-promoting macronutrient water-soluble fertilizer according to claim 5, characterized in that: In the step 1), the molar ratio of the reactants 4,4'-diaminodiphenyl ether and 2-fluorobenzyl chloride is 1:4-5; the reaction temperature is 90-95° C., and the reaction time is 4-6 hours.

7. The method for preparing the growth-promoting macronutrient water-soluble fertilizer according to claim 5, characterized in that: In the step 2), the filtration time after the reaction is completed is 1-2 hours; in the step 3), the drying temperature is 85-90° C. and the drying time is 1-2 hours.

8. A method for applying a growth-promoting macronutrient water-soluble fertilizer, characterized in that: The growth-promoting macronutrient water-soluble fertilizer of claim 1 is applied by drip irrigation at an application rate of 3.5-4.5 kg / mu; or by flushing at an application rate of 4-8 kg / mu.

9. Application of a growth-promoting macronutrient water-soluble fertilizer, characterized in that: Used when plants need large amounts of nutrients to grow.

10. The use of the growth-promoting macronutrient water-soluble fertilizer according to claim 9, characterized in that: The plant is corn.

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