CN112110762A - Water-soluble fertilizer and production process thereof - Google Patents
Water-soluble fertilizer and production process thereof Download PDFInfo
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- CN112110762A CN112110762A CN202010791963.3A CN202010791963A CN112110762A CN 112110762 A CN112110762 A CN 112110762A CN 202010791963 A CN202010791963 A CN 202010791963A CN 112110762 A CN112110762 A CN 112110762A
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
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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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- 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
- C05G3/60—Biocides or preservatives, e.g. disinfectants, pesticides or herbicides; Pest repellants or attractants
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/70—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting wettability, e.g. drying agents
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G5/00—Fertilisers characterised by their form
- C05G5/20—Liquid fertilisers
- C05G5/23—Solutions
Abstract
The invention discloses a water-soluble fertilizer and a production process thereof, and relates to the technical field of compound fertilizers. The water-soluble fertilizer comprises the following components: biochemical fulvic acid, urea, diammonium hydrogen phosphate, potassium nitrate, trace elements, modified chicoric acid, a wetting agent, a synergist and water. The preparation method comprises the following steps: heating biochemical fulvic acid, urea and water, stirring and dissolving, adding diammonium hydrogen phosphate and potassium nitrate, and continuously stirring to obtain a mixed solution A; then adding the wetting agent and the synergist into the mixed solution A, and continuously stirring to obtain a mixed solution B; then adding trace elements, and stirring to obtain a mixed solution C; and finally, dissolving the modified chicoric acid in water, adding the solution into the mixed solution C, continuously stirring and cooling to obtain the water-soluble fertilizer. The water-soluble fertilizer prepared by the invention has complete nutrient components and high crop absorption and utilization rate, and is suitable for various fertilizing modes; good stability, high water solubility and high fertilizer efficiency; can improve the crop yield and the crop quality, and has simple production process.
Description
Technical Field
The invention belongs to the technical field of compound fertilizers, and particularly relates to a water-soluble fertilizer and a production process thereof.
Background
The high-efficiency utilization of water resources and the improvement of fertilizer utilization rate are two very important aspects in high-efficiency agricultural production, and the improvement is not necessary. At present, with the aggravation of adverse factors on agricultural production and ecological environment due to the lack of water resources, the water and fertilizer integration and the vigorous development of water-saving agriculture become important ways for various countries to break through water resource constraints.
Fertilizers have become an important foundation for the development of modern agriculture as food for supplying nutrients needed by crops. The conventional compound chemical fertilizer has relatively single nutrient components, can not meet the growth requirements of crops, has low nutrient absorption rate of the crops, and only has the utilization rate of 30-40 percent, thereby causing the waste of the fertilizer; the conventional compound chemical fertilizer seriously hardens soil, damages the quality of crop products and causes a great deal of pollution to the environment. Therefore, it is necessary to find a fertilizer which can replace the conventional compound chemical fertilizer and has multi-element compound and is easily absorbed by crops. The water-soluble fertilizer is a full-nutrient compound fertilizer which can be completely and quickly dissolved in water, the nutrients are conveniently and quickly absorbed by crops, the absorption utilization rate is high, the water-soluble fertilizer can be applied to facilities such as water and fertilizer integration, and the functions of saving water and fertilizer, saving labor, increasing yield and improving quality are achieved.
Disclosure of Invention
The invention aims to provide a water-soluble fertilizer and a production process thereof, the water-soluble fertilizer has complete nutrient components and high crop absorption and utilization rate, and is suitable for various fertilization modes; and has the advantages of good stability, high water solubility and high fertilizer efficiency; can improve the crop yield and the crop quality, and has simple production process.
The technical scheme adopted by the invention for realizing the purpose is as follows:
the use of modified chicoric acid in the preparation of water-soluble fertilizers, the structural formula of the modified chicoric acid is as follows:
wherein R is amino acid potassium salt. After the amino acid potassium salt is used for modifying the chicoric acid, the chicoric acid is added into the water-soluble fertilizer, so that the bactericidal performance of the water-soluble fertilizer is improved, the infection probability of crop diseases and insect pests is reduced, the absorption of plants to magnesium can be promoted, and the generation of chlorophyll is increased; the generation of photosynthesis is facilitated, and the accumulation of carbon dioxide in the plant body is promoted, so that the yield is increased, and the product quality is improved; can also improve the stress resistance of crops.
Preferably, the potassium salt of amino acid is one of potassium glycinate, potassium serine, potassium alanine, potassium threonine and potassium histidine; the mass ratio of the chicoric acid to the potassium amino acid salt is 1: 1.5-1.8.
More preferably, the modified chicoric acid is prepared by the following steps:
weighing chicoric acid, 1-hydroxybenzotriazole and amino acid potassium salt (the mass ratio of the chicoric acid to the amino acid potassium salt to the 1-hydroxybenzotriazole is 1: 1.5-1.8: 0.7-0.9), dissolving the chicoric acid, the amino acid potassium salt and the amino acid potassium salt in DMF (the solid-liquid ratio of the chicoric acid to the DMF is 1: 16-18 g/mL), slowly dripping triethylamine (the volume ratio of the triethylamine to the DMF is 1: 7-8) under the condition of ice-water bath, reacting for 10-15 min, adding EDC (the mass ratio of the chicoric acid to the EDC is 1: 1-1.1), naturally heating to 23-25 ℃, and reacting for 18-20 h. Thin Layer Chromatography (TLC) was used to check if the reaction was complete. Pouring the reactant into water, respectively extracting with ethyl acetate and washing with saturated saline water, drying the organic phase with anhydrous sodium sulfate overnight, filtering, separating by silica gel column chromatography (eluent is ethyl acetate and petroleum ether with the volume ratio of 1: 2-3), distilling under reduced pressure, and drying under vacuum to obtain the modified chicoric acid.
A water-soluble fertilizer comprises the following raw material components: biochemical fulvic acid, urea, diammonium hydrogen phosphate, potassium nitrate, trace elements, the modified chicoric acid, a wetting agent, a synergist and water;
the trace elements comprise manganese ethylenediaminetetraacetate, zinc ethylenediaminetetraacetate, sodium octaborate tetrahydrate, cupric nitrate, ferrous sulfate and ammonium molybdate. The water-soluble fertilizer prepared by the invention is a multi-element water-soluble fertilizer, has complete nutrient components and high crop absorption and utilization rate, and is suitable for various fertilizing modes; the fertilizer can be directly sprayed on the leaf surfaces of crops, and all nutrient substances can directly enter the plant body from the leaf surfaces to participate in the metabolism of the crops, so that the fertilizer is prevented from being fixed by soil, and the fertilizer has better utilization rate; the wetting agent can reduce the contact angle of the water-soluble fertilizer on the leaf surface, reduce the apparent tension of the water-soluble fertilizer, and improve the wetting effect of the wetting agent on the leaf surface and the permeability of the water-soluble fertilizer, so that the effective transfer of nutrient elements is increased, and the effective utilization rate of the water-soluble fertilizer is improved; acting on the root can promote the growth of the root system of the crop and enhance the photosynthesis of the crop; the preparation method of the water-soluble fertilizer is simple, the production process conditions are easy to control, and the raw materials are sequentially added in the preparation process, so that the uniformity of the product solution is ensured, the stability is high, no precipitate is generated, and the product quality is stable.
Preferably, the raw material components include: 30-40 parts of biochemical fulvic acid, 25-30 parts of urea, 15-20 parts of diammonium hydrogen phosphate, 10-15 parts of potassium nitrate, 3-5 parts of trace elements, 1-5 parts of modified chicoric acid, 0.08-0.1 part of wetting agent, 0.5-1 part of synergist and 35-50 parts of water.
Preferably, in the trace elements, the mass ratio of manganese ethylenediaminetetraacetate, zinc ethylenediaminetetraacetate, sodium octaborate tetrahydrate, copper nitrate, ferrous sulfate and ammonium molybdate is 1-1.5: 2-2.5: 1: 0.8-1.2: 0.6-0.8: 0.7-0.9.
Preferably, the wetting agent is neoazone.
Preferably, the synergist is one of o-nitrophenol sodium, p-nitrophenol sodium and 5-nitroguaiacol sodium.
A method of preparing a water-soluble fertilizer comprising:
heating biochemical fulvic acid, urea and water, stirring and dissolving, adding diammonium hydrogen phosphate and potassium nitrate, and continuously stirring to obtain a mixed solution A;
adding a wetting agent and a synergist into the mixed solution A, and heating and stirring to obtain a mixed solution B;
adding the trace elements into the mixed solution B, and stirring to obtain a mixed solution C;
and (3) dissolving the modified chicoric acid in water, then adding the modified chicoric acid into the mixed solution C, and continuously stirring and cooling to obtain the water-soluble fertilizer.
Preferably, the stirring speed is 300-500 rpm; the heating temperature is 63-68 ℃.
Preferably, the water-soluble fertilizer also comprises 0.3-0.5 weight part of water-soluble limonin. The water-soluble citriodorol is added into the compound fertilizer, so that the effect of a wetting agent can be enhanced, the surface tension of the water-soluble fertilizer is reduced, the wetting effect of the water-soluble fertilizer on the surface of leaves and the permeability of the water-soluble fertilizer are improved, and the effective utilization rate of the water-soluble fertilizer is further improved; in addition, the water-soluble fertilizer prepared by adding the water-soluble limonin acts on the seeds to improve the germination rate of the seeds.
The invention also discloses application of the water-soluble fertilizer in crop fertilization.
Compared with the prior art, the invention has the following beneficial effects:
the water-soluble fertilizer prepared by the invention has complete nutrient components and high crop absorption and utilization rate, and is suitable for various fertilizing modes; the chicoric acid modified by the potassium amino acid salt is added, so that the bactericidal performance of the water-soluble fertilizer can be improved, and the infection probability of crop diseases and insect pests is reduced; and is favorable for promoting the absorption of the plants to magnesium and increasing the generation of chlorophyll; can promote photosynthesis and carbon dioxide accumulation in plant body, thereby promoting yield increase and improving product quality; can also improve the stress resistance of crops. The addition of the water-soluble limoninol can improve the wetting effect of the limoninol on the surface of the leaves and the permeability of the water-soluble fertilizer, and further improve the effective utilization rate of the water-soluble fertilizer; meanwhile, the germination rate of the seeds can be improved by acting on the seeds. The water-soluble fertilizer prepared by the invention has the advantages of simple method, easy control of production process conditions, high stability and stable product quality.
Therefore, the invention provides a water-soluble fertilizer and a production process thereof, the water-soluble fertilizer has complete nutrient components and high crop absorption and utilization rate, and is suitable for various fertilization modes; and has the advantages of good stability, high water solubility and high fertilizer efficiency; can improve the crop yield and the crop quality, and has simple production process.
Drawings
FIG. 1 is a graph showing comparison of chlorophyll contents in test example 3 of the present invention;
FIG. 2 is a graph showing the comparison between the heart rate and the yield of a bag in test example 3 of the present invention;
FIG. 3 is a schematic diagram showing the comparison of the results of quality index tests in test example 3 of the present invention;
FIG. 4 is a comparative illustration of fertilizer utilization in test example 3 of the present invention;
FIG. 5 is a schematic diagram showing the comparison of the stress resistance test results in test example 3 of the present invention;
FIG. 6 is a graph showing a comparison of a wet area and a surface tension in test example 4 of the present invention;
FIG. 7 is a graph showing the comparison of germination rates of seeds in test example 5 of the present invention.
Detailed Description
The technical solution of the present invention is further described in detail below with reference to the following detailed description and the accompanying drawings:
the chicoric acid, the potassium glycinate and the potassium alanine used in the embodiment of the invention are all purchased from the market, and the molecular weight of the chicoric acid is 474.37; the purity of the glycine potassium salt is more than or equal to 98 percent, and the purity of the alanine potassium salt is more than or equal to 98 percent.
The structural formula of the modified chicoric acid used in the embodiment 1 of the invention is as follows:
The structural formula of the modified chicoric acid used in the embodiment 2 of the invention is as follows:
Example 1:
preparation of modified chicoric acid:
weighing chicoric acid, 1-hydroxybenzotriazole and glycine potassium salt (the mass ratio of the chicoric acid to the glycine potassium salt to the 1-hydroxybenzotriazole is 1: 1.5: 0.7), dissolving the chicoric acid, the 1-hydroxybenzotriazole and the glycine potassium salt in DMF (the solid-to-liquid ratio of the chicoric acid to the DMF is 1:16g/mL), slowly dripping triethylamine (the volume ratio of the triethylamine to the DMF is 1:7) under the condition of ice-water bath, reacting for 10min, adding EDC (the mass ratio of the chicoric acid to the EDC is 1:1.1), naturally heating to 25 ℃, and reacting for 20 h. Thin Layer Chromatography (TLC) was used to check if the reaction was complete. Pouring the reactant into water, extracting with ethyl acetate and washing with saturated saline water respectively, drying the organic phase with anhydrous sodium sulfate overnight, filtering, separating with silica gel column chromatography (eluent is ethyl acetate and petroleum ether at a volume ratio of 1:2), distilling under reduced pressure, and vacuum drying to obtain modified chicoric acid.
A water-soluble fertilizer, the composition comprising: 40 parts of biochemical fulvic acid, 30 parts of urea, 15 parts of diammonium hydrogen phosphate, 15 parts of potassium nitrate, 5 parts of trace elements, 5 parts of modified chicoric acid, 0.1 part of wetting agent, 1 part of synergist and 45 parts of water; wherein, the trace elements comprise: the mass ratio of the manganese salt of ethylene diamine tetraacetic acid to the zinc salt of ethylene diamine tetraacetic acid to the sodium octaborate tetrahydrate to the copper nitrate to the ferrous sulfate to the ammonium molybdate is 1:2:1: 0.8: 0.6: 0.7; the synergist is 5-nitroguaiacol sodium.
Preparation of water-soluble fertilizer:
heating, stirring and dissolving biochemical fulvic acid, urea and water at 65 ℃ and the rotating speed of 500rpm, then adding diammonium hydrogen phosphate and potassium nitrate, and continuously stirring and dissolving to obtain a mixed solution A;
adding a wetting agent and a synergist into the mixed solution A, and heating and stirring under the condition of unchanging temperature and stirring speed to obtain a mixed solution B;
adding trace elements into the mixed solution B under the conditions of continuous heating and stirring to obtain a mixed solution C;
and (3) dissolving the modified chicoric acid in water, then adding the modified chicoric acid into the mixed solution C, continuously stirring for 2 hours, and cooling to room temperature to obtain the water-soluble fertilizer.
Example 2:
the preparation of modified chicoric acid differed from example 1 in that: the potassium salt of glycine was replaced with potassium salt of alanine.
A water-soluble fertilizer, the composition comprising: 30 parts of biochemical fulvic acid, 25 parts of urea, 18 parts of diammonium hydrogen phosphate, 15 parts of potassium nitrate, 3 parts of trace elements, 3 parts of modified chicoric acid, 0.08 part of wetting agent, 1 part of synergist and 40 parts of water; wherein, the trace elements comprise: the mass ratio of the manganese salt of ethylene diamine tetraacetic acid to the zinc salt of ethylene diamine tetraacetic acid to the sodium octaborate tetrahydrate to the copper nitrate to the ferrous sulfate to the ammonium molybdate is 1:2:1: 0.8: 0.6: 0.7; the synergist is sodium p-nitrophenolate.
The water-soluble fertilizer was prepared in the same manner as in example 1.
Example 3:
modified chicoric acid was prepared as in example 1.
A water-soluble fertilizer, the composition comprising: 35 parts of biochemical fulvic acid, 30 parts of urea, 18 parts of diammonium hydrogen phosphate, 15 parts of potassium nitrate, 4 parts of trace elements, 1 part of modified chicoric acid, 0.09 part of wetting agent, 1 part of synergist and 50 parts of water; wherein, the trace elements comprise: the mass ratio of the manganese salt of ethylene diamine tetraacetic acid to the zinc salt of ethylene diamine tetraacetic acid to the sodium octaborate tetrahydrate to the copper nitrate to the ferrous sulfate to the ammonium molybdate is 1:2:1: 0.8: 0.6: 0.7; the synergist is sodium o-nitrophenolate.
The water-soluble fertilizer was prepared in the same manner as in example 1.
Example 4:
modified chicoric acid was prepared as in example 1.
A water-soluble fertilizer, the composition comprising: 40 parts of biochemical fulvic acid, 30 parts of urea, 15 parts of diammonium hydrogen phosphate, 15 parts of potassium nitrate, 5 parts of trace elements, 5 parts of modified chicoric acid, 0.1 part of wetting agent, 1 part of synergist, 45 parts of water and 0.5 part of water-soluble cineole citrate; wherein, the trace elements comprise: the mass ratio of the manganese salt of ethylene diamine tetraacetic acid to the zinc salt of ethylene diamine tetraacetic acid to the sodium octaborate tetrahydrate to the copper nitrate to the ferrous sulfate to the ammonium molybdate is 1:2:1: 0.8: 0.6: 0.7; the synergist is 5-nitroguaiacol sodium.
Preparation of water-soluble fertilizer:
heating, stirring and dissolving biochemical fulvic acid, urea and water at 65 ℃ and the rotating speed of 500rpm, then adding diammonium hydrogen phosphate and potassium nitrate, and continuously stirring and dissolving to obtain a mixed solution A;
adding a wetting agent and a synergist into the mixed solution A, and heating and stirring under the condition of unchanging temperature and stirring speed to obtain a mixed solution B;
adding trace elements into the mixed solution B under the conditions of continuous heating and stirring to obtain a mixed solution C;
and (3) dissolving the modified chicoric acid and the limonol in water, adding the solution into the mixed solution C, continuously stirring for 2 hours, and cooling to room temperature to obtain the water-soluble fertilizer.
Comparative example 1:
a water-soluble fertilizer, the composition comprising: 40 parts of biochemical fulvic acid, 30 parts of urea, 15 parts of diammonium hydrogen phosphate, 15 parts of potassium nitrate, 5 parts of trace elements, 0.1 part of wetting agent, 1 part of synergist and 45 parts of water; wherein, the trace elements comprise: the mass ratio of the manganese salt of ethylene diamine tetraacetic acid to the zinc salt of ethylene diamine tetraacetic acid to the sodium octaborate tetrahydrate to the copper nitrate to the ferrous sulfate to the ammonium molybdate is 1:2:1: 0.8: 0.6: 0.7; the synergist is 5-nitroguaiacol sodium.
The preparation method is the same as that of example 1.
Test example 1:
characterization of nuclear magnetic resonance (1H NMR)
Weighing 5 mu L of modified chicoric acid, dissolving in deuterium water to prepare a sample solution, placing the sample solution in a nuclear magnetic tube, and placing the nuclear magnetic tube in a nuclear magnetic resonance apparatus for determination. The operating conditions of the instrument are as follows: AVANCE III 400 nuclear magnetic resonance apparatus (Bruker). And analyzing the type and the amount of hydrogen in the target product through the data of the hydrogen spectrum.
The modified chicoric acid prepared in the examples 1 and 2 was subjected to nuclear magnetic hydrogen spectrum test, and the characterization results are as follows:
example 1:1H NMR(400MHz，D2O)：9.45(s，1H，OH)，9.05(s，1H，OH)，8.56(s，1H，NH)，7.18(d，J＝16.1Hz，1H，HC＝C)，7.02(s，1H，ArH)，6.88(d，J＝8.2Hz，1H，ArH)，6.70(d，J＝8.1Hz，1H，ArH)，6.37(d，J＝16.1Hz，1H，C＝CH)，4.16(q，J＝6.8Hz，2H，CH2). Indicating that the chicoric acid and the glycine potassium salt successfully react.
Example 2:1H NMR(400MHz，D2o): 9.42(s, 1H, OH), 9.10(s, 1H, OH), 8.35(d, J ═ 6.53Hz, 1H, NH), 7.31(d, J ═ 16.1Hz, 1H, HC ═ C), 6.98(s, 1H, ArH), 6.80(d, J ═ 8.2Hz, 1H, ArH), 6.67(d, J ═ 8.0Hz, 1H, ArH), 6.32(d, J ═ 16.1Hz, 1H, C ═ CH), 4.38(m, 1H, CH), 1.34(d, J ═ 7.3Hz, 3H, CH 3). Indicating that the chicoric acid and the alanine potassium salt successfully react.
Test example 2:
the performance indexes of the prepared water-soluble fertilizer are detected according to the following method, and the measurement results are shown in table 1:
pH value: detecting by using wide pH test paper, and measuring by using a pH meter;
organic matter content: according to agricultural industry standard soil detection part 6: determination of soil organic matter (NY/T1121.6-2006), namely determination by a potassium dichromate volumetric method;
n nutrient content: measuring according to national standard of determination of total nitrogen in water-alkaline potassium persulfate digestion ultraviolet spectrophotometry (GB 11894-89);
p nutrient content: measuring according to the method of national standard of determination of total phosphorus in water-ammonium molybdate spectrophotometry (GB/T11893-89);
k nutrient content: measured according to the method of flame atomic absorption spectrophotometry (GB/T11904-89) for measuring potassium and sodium in water of national standard;
the humic acid content of the water-soluble fertilizer is as follows: according to the method for measuring humic acid content of water-soluble fertilizer in agricultural industry standard (NY/T1971-2010);
content of trace elements: measuring by adopting an atomic absorption spectrometry;
lead, chromium, cadmium, arsenic, mercury content: the content of mercury, arsenic, cadmium, lead and chromium in the fertilizer is measured according to the method of measuring the content of mercury, arsenic, cadmium, lead and chromium in the fertilizer (NY/T1978-2010) in the agricultural industry standard, namely the content is measured by adopting atomic fluorescence spectrometry.
Table 1 example 1 determination of contents of respective indexes of water-soluble fertilizer
| Index (I) | Detecting the content | Index (I) | Detecting the content |
| Total nitrogen (g/L) | 10.72 | Boron (mg/L) | ＜2.5 |
| Phosphorus (in P)2O5Meter) (g/L) | 98.6 | Lead (mg/kg) | ＜2.5 |
| Potassium (in K)2O meter) (g/L) | 118.6 | Cadmium (mg/kg) | ＜0.25 |
| Calcium (mg/L) | 863 | Chromium (mg/kg) | ＜1.0 |
| Magnesium (mg/L) | 803 | Arsenic (mg/kg) | ＜0.050 |
| Iron (mg/L) | 38.1 | Mercury (mg/kg) | ＜0.005 |
| Manganese (mg/L) | 7.3 | Water insoluble substance (g/L) | ＜0.005 |
| Copper (mg/L) | ＜2.5 | Organic matter (g/L) | 15.2 |
| Zinc (mg/L) | 33.4 | pH value | 6.0 |
| Molybdenum (mg/L) | 32.1 | Humic acid (g/L) | 52.1 |
The water-soluble fertilizer prepared in the embodiment 1 of the invention has the following physical and chemical properties: macroelement (in N, P)2O5、K2Calculated by O) is 227.4g/L, and the nutrient content ratio is N: p2O5：K2O1: 9.19: 11.06; pH 6.0; the content of humic acid is 52.1 g/L; the water-soluble fertilizer prepared by the embodiment of the invention meets the requirements of agricultural industry standard water-soluble fertilizer containing humic acid (NY 1106-2010).
Test example 3:
determination of the Effect on plants
Basic physicochemical properties of the tested soil: the pH value is 6.2, the organic matter is 23.4g/kg, the alkaline hydrolysis nitrogen is 107.9mg/kg, the quick-acting phosphorus is 28.3mg/kg, and the quick-acting potassium is 168.3 mg/kg.
The tested Chinese cabbage variety is green hybrid No. 3, and the seedling raising time is 20 days. Transplanting one strain every 0.5m, and watering once every 15 days from the transplanting day.
Three processes are set: t0 (no fertilizer application), T1 (water-soluble fertilizer root application), T2 (water-soluble fertilizer foliar spray); spraying and root irrigation are carried out on the water-soluble fertilizer stock solution for three times, and the water-soluble fertilizer stock solution is diluted by 1000 times with water when being used at the seedling stage, the lotus socket stage and before balling.
Each treatment was set up in triplicate, randomized block arrangement, and each treatment cell was 25m in area 2100 Chinese cabbages are transplanted in each cell.
Sampling and measuring:
measuring chlorophyll content of leaf with SPAD instrument at early stage of heading Chinese cabbage; the yield is calculated according to the cell during harvesting, and the overground part of the yield is taken to measure the average fresh weight of a single plant; the leaf without core of Chinese cabbage is removed, the core weight, the core circumference and the core height of each plant are measured, and the core rate and the yield are calculated (the core rate is the core fresh weight of each plant/the fresh weight of each plant, and the yield is the core fresh weight of each plant × 100 × 10000/25).
Taking fresh cabbage leaf with core, shearing, mixing, and measuring vitamin C (measured by 2, 6-dichloroindophenol method) and nitrate (measured by salicylic acid-sulfuric acid colorimetric method). Weighing Chinese cabbage leaf, deactivating enzyme at 105 deg.C for 30min, oven drying at 75 deg.C, and determining nitrogen, phosphorus and potassium content (by adopting H)2SO4-H2O2Combined digestion method), calculating fertilizer utilization:
fertilizer utilization ratio (%) - (the accumulation amount of nutrients in plants treated by fertilization-the accumulation amount of nutrients in plants not treated by fertilization)/nutrient input amount x 100
In the early stage of heading Chinese cabbage, collecting the normal growth leaf of Chinese cabbage, cleaning with gauze, treating in a thermostat at about 50 deg.C for 30min, and treating under stress. Washing the treated group leaves and the control group leaves with deionized water for 2 times, then completely absorbing surface moisture by clean filter paper, weighing 2g, cutting into small sections with the length of about 1cm, placing the small sections into a beaker (the size is enough to hold an electrode), pressing the small sections by a glass rod, accurately adding 20mL of distilled water into the beaker, and immersing the leaves. Placing it in a vacuum drier, and evacuating the air in the intercellular spaces with an air extractor; the air is again slowly released and the water is forced into the tissue to sink the blades. Taking out the small beaker after the air pumping, placing the small beaker on an experiment table for standing for 20min, then slightly stirring the blades by using a glass rod, and measuring the conductance value of C by using a conductivity meter at the constant temperature of 20-25 DEG C1(ii) a Measuring conductivity, placing in 100 deg.C boiling water bath for 15min to kill plant tissue, taking out, cooling to 25 deg.C, measuring boiling conductivity to C2. The calculated injury (%) is:
Lt＝C1/C2×100％
the experimental data were analyzed using the software SPASS 13.0.
The above tests were carried out for example 1, example 2, example 3, example 4, comparative example 1.
1. Measurement of chlorophyll content
The results are shown in FIG. 1. From the analysis in the figure, it can be seen that the samples prepared in example 1 and experimental example 2 can promote the increase of chlorophyll content in crops, which is obviously higher than that of comparative example 1. The modified chicoric acid can improve the chlorophyll content in crops, and the effect of the example 1 is equivalent to that of the example 2.
2. Bag heart rate and yield determination
The results are shown in FIG. 2. As can be seen from the figure, the water-soluble fertilizer prepared in this example was applied to improve the crop yield and the yield significantly as compared to the case of the non-fertilization treatment, and was better than the comparative example. The water-soluble fertilizer prepared by adding the modified chicoric acid can improve the crop yield.
3. Quality index measurement
The results are shown in FIG. 3. From the analysis in the figure, the Vc and nitrate contents of the sample prepared in the example 1 of the invention are obviously higher than those of the sample prepared in the comparative example 1 after being applied to crops, and the addition of the modified chicoric acid is favorable for improving the quality of the crops. The effect of example 1 is slightly better than that of examples 2 to 3.
4. Determination of fertilizer utilization
The results are shown in FIG. 4. As can be seen from the figure, the utilization rate of the fertilizer by the foliar fertilization mode crops is slightly higher than that by the root fertilization. After the sample prepared in the example 1 is applied to crops, the fertilizer utilization rate is obviously higher than that of the comparative example 1, and the water-soluble fertilizer prepared by adding the modified chicoric acid can promote the absorption and utilization of the fertilizer by the crops.
5. Stress resistance determination
The results are shown in FIG. 5. From the analysis of the figure, it is clear that the application of the fertilizer can reduce the crop injury rate obviously compared with the control group. After the water-soluble fertilizer prepared in example 1 is applied to crops, the injury rate of the crops is obviously reduced and is lower than that of comparative example 1. The addition of the modified chicoric acid has an effect of enhancing the stress resistance of crops.
Test example 4:
1. wetted area
Picking fresh Ligustrum lucidum leaves growing uniformly on the same position, washing the front and back surfaces of the leaves with clear water, and naturally drying the leaves in the shade. The leaves cleaned and air-dried on the surface are fixed on a glass plate by a double-sided adhesive tape, 50 mu L of spray liquid diluted by water-soluble fertilizer stock solution is slowly dripped by a microsyringe from the height of 1cm away from the leaves at the same speed in sequence, the wetting area is measured after the spraying liquid is wetted and balanced, and the wetting area is calculated (the room temperature is 25 ℃).
2. Surface tension measurement
And (3) measuring the surface tension of the solution diluted by the water-soluble fertilizer stock solution by using a maximum bubble pressure method. And (3) putting a sample to be detected into the sample tube, keeping the depth of the capillary tube inserted into the liquid to be 0, then closing the pressure relief switch, turning off the liquid drop switch to enable the liquid to flow down, controlling the bubbling speed in the sample tube to be about 6 s/time through the water flow speed, enabling the sample tube to be a single bubble to be blown out, and reading the maximum pressure when the bubble is blown out through a micro differential pressure meter to obtain the maximum bubble pressure delta p. The surface tension of the solution was then calculated by the laplace equation:
△p＝2γ/r
wherein r is the capillary radius, determined from the surface tension of the known clean water at room temperature of 25 ℃.
The results of the above two tests on the samples obtained in example 1 and example 4 are shown in fig. 6. As can be seen from the figure, the wetting area of the sample prepared in example 4 is obviously higher than that of example 1, and the surface tension is lower than that of example 1, which shows that the water-soluble limoninol can enhance the effect of the wetting agent, is beneficial to the crops to absorb the nutrient components in the fertilizer, promotes the growth of the crops and improves the quality.
Test example 5:
influence on seed germination rate
The test seeds are rice seeds. Two treatments were performed: h1 (soaking seeds in clear water), H2 (soaking seeds by 4000 times of dilution of water-soluble fertilizer stock solution); one petri dish, 100 rice seeds and a quantitative amount of quartz sand were used for each treatment. During the test, a certain amount of quartz sand is flatly paved at the bottom of a culture dish, the quartz sand is wetted by deionized water, the rice seeds soaked by the fertilizer liquid are evenly flatly paved on the quartz sand, and the quartz sand is subjected to backlight treatment and cultured in a 25 ℃ culture box for 12 hours; the number of germinated seeds was measured at 3 days, 5 days, and 7 days, respectively. And (3) statistically calculating the germination rates of the seeds under different treatments:
the germination rate (%) is 7 days, the germination number of the seeds is 100
The above tests were carried out for examples 1 and 4, and the results are shown in FIG. 7. As can be seen from the figure, the germination rate of the seeds after the seeds are soaked by the fertilizer is obviously improved compared with the control group. And the germination rate of the seeds after the sample prepared in the example 4 is soaked is better than that of the sample prepared in the example 1, which shows that the addition of the water-soluble limonin can improve the germination rate of the seeds.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. Use of modified chicoric acid in the preparation of a water-soluble fertilizer, the modified chicoric acid having the following structural formula:
wherein R is amino acid potassium salt.
2. Use of modified chicoric acid in the preparation of water-soluble fertilizers according to claim 1, characterized in that: the potassium amino acid salt is one of potassium glycinate, potassium serine salt, potassium alanine salt, potassium threonine salt and potassium histidine salt; the mass ratio of the chicoric acid to the potassium amino acid salt is 1: 1.5-1.8.
3. A water-soluble fertilizer comprises the following raw material components: biochemical fulvic acid, urea, diammonium hydrogen phosphate, potassium nitrate, trace elements, modified chicoric acid as claimed in claim 1, a wetting agent, a synergist and water;
the trace elements consist of manganese ethylenediaminetetraacetate, zinc ethylenediaminetetraacetate, sodium octaborate tetrahydrate, cupric nitrate, ferrous sulfate and ammonium molybdate.
4. A water-soluble fertilizer according to claim 3, wherein: the raw material components comprise: 30-40 parts of biochemical fulvic acid, 25-30 parts of urea, 15-20 parts of diammonium hydrogen phosphate, 10-15 parts of potassium nitrate, 3-5 parts of trace elements, 1-5 parts of modified chicoric acid, 0.08-0.1 part of wetting agent, 0.5-1 part of synergist and 35-50 parts of water.
5. A water-soluble fertilizer according to claim 3 or 4, characterized in that: in the trace elements, the mass ratio of manganese ethylenediaminetetraacetate, zinc ethylenediaminetetraacetate, sodium octaborate tetrahydrate, copper nitrate, ferrous sulfate and ammonium molybdate is 1-1.5: 2-2.5: 1: 0.8-1.2: 0.6-0.8: 0.7-0.9.
6. A water-soluble fertilizer according to claim 3 or 4, characterized in that: the wetting agent is neoazone.
7. A water-soluble fertilizer according to claim 3 or 4, characterized in that: the synergist is one of o-nitrophenol sodium, p-nitrophenol sodium and 5-nitroguaiacol sodium.
8. A method of producing a water-soluble fertilizer as claimed in any one of claims 3 to 7, comprising:
heating, stirring and dissolving the biochemical fulvic acid, the urea and the water, adding the diammonium hydrogen phosphate and the potassium nitrate, and continuously stirring to obtain a mixed solution A;
adding the wetting agent and the synergist into the mixed solution A, and heating and stirring to obtain a mixed solution B;
adding the trace elements into the mixed solution B, and stirring to obtain a mixed solution C;
and (3) dissolving the modified chicoric acid in water, then adding the solution into the mixed solution C, and continuously stirring and cooling to obtain the water-soluble fertilizer.
9. The method for preparing a water-soluble fertilizer according to claim 8, wherein: the stirring speed is 300-500 rpm; the heating temperature is 63-68 ℃.
10. Use of a water-soluble fertilizer according to any one of claims 3 to 7 for fertilizing a crop.
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