CN113929529A - Disease-resistant liquid fertilizer and preparation method thereof - Google Patents

Disease-resistant liquid fertilizer and preparation method thereof Download PDF

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Publication number
CN113929529A
CN113929529A CN202111365043.6A CN202111365043A CN113929529A CN 113929529 A CN113929529 A CN 113929529A CN 202111365043 A CN202111365043 A CN 202111365043A CN 113929529 A CN113929529 A CN 113929529A
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parts
liquid fertilizer
disease
pregelatinized starch
chitosan
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张中华
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Luohe Xinhe Biotechnology Co ltd
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Luohe Xinhe Biotechnology Co ltd
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    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05GMIXTURES 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
    • C05G3/00Mixtures of one or more fertilisers with additives not having a specially fertilising activity
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/02Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
    • A01N43/04Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
    • A01N43/14Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings
    • A01N43/16Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings with oxygen as the ring hetero atom
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
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    • AHUMAN NECESSITIES
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    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A01N65/08Magnoliopsida [dicotyledons]
    • A01N65/20Fabaceae or Leguminosae [Pea or Legume family], e.g. pea, lentil, soybean, clover, acacia, honey locust, derris or millettia
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A01N65/08Magnoliopsida [dicotyledons]
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A01N65/08Magnoliopsida [dicotyledons]
    • A01N65/32Ranunculaceae [Buttercup family], e.g. hepatica, hydrastis or goldenseal
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
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    • A01N65/46Stemonaceae [Stemona family], e.g. croomia
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    • C05G3/00Mixtures of one or more fertilisers with additives not having a specially fertilising activity
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    • C05G3/00Mixtures of one or more fertilisers with additives not having a specially fertilising activity
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    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05GMIXTURES 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
    • C05G5/00Fertilisers characterised by their form
    • C05G5/20Liquid fertilisers
    • C05G5/27Dispersions, e.g. suspensions or emulsions

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Abstract

The invention belongs to the technical field of fertilizer research, and particularly discloses a disease-resistant liquid fertilizer and a preparation method thereof. The liquid fertilizer is prepared from the following raw materials in parts by weight: 5-15 parts of radix stemonae, 5-12 parts of scutellaria baicalensis, 10-20 parts of coptis chinensis, 5-12 parts of radix sophorae flavescentis, 5-8 parts of bamboo vinegar, 5-10 parts of chitosan and 8-15 parts of pregelatinized starch. The disease-resistant liquid fertilizer provided by the invention has better slow release performance, and meanwhile, the special properties and the wrapping mode of the pregelatinized starch can accelerate the release of effective substances wrapped by the pregelatinized starch in rainy days or irrigation, and the liquid fertilizer is matched with chitosan to prevent the liquid fertilizer from being washed by rainwater and lost.

Description

Disease-resistant liquid fertilizer and preparation method thereof
Technical Field
The invention belongs to the technical field of fertilizer research, and particularly discloses a disease-resistant liquid fertilizer and a preparation method thereof.
Background
Liquid fertilizer, liquid fertilizer for short. The fertilizer is a fertilizer which has no certain shape and is in a flowing state, and comprises a clear liquid type and a suspension type. Ammonium phosphate solutions with different concentrations, which are produced by neutralizing liquid ammonia with phosphoric acid, superphosphoric acid and polyphosphoric acid, are commonly used liquid fertilizers; if other nitrogen fertilizers, potassium chloride, medium and trace elements are dissolved in a proper proportion, the multi-element liquid compound fertilizer can be produced; sometimes, a herbicide, an insecticide, a bactericide and the like can be added into the liquid fertilizer to prepare the multifunctional liquid fertilizer. The liquid fertilizer has the advantages of low production cost and convenient irrigation and fertilization.
The slow release fertilizer is also called slow release fertilizer or controlled release fertilizer. The release speed of the compounds containing nutrients in the fertilizer in soil is slow or the release speed of the nutrients can be controlled to a certain degree for the sustained absorption and utilization of crops. The slow release fertilizer can reduce the loss of fertilizer nutrients, particularly nitrogen, in soil, reduce the frequency of fertilization operation, save labor and cost, and avoid the damage to seeds or seedlings caused by excessive fertilization. Although the existing liquid fertilizer can achieve the slow release effect, the effective components are easily washed away by rainwater in rainy days, so that the loss of the effective components is caused.
Disclosure of Invention
The invention provides a disease-resistant liquid fertilizer, which has better slow release performance, and simultaneously, the special property and the wrapping mode of pregelatinized starch can accelerate the release of effective substances wrapped by the pregelatinized starch in rainy days or irrigation, and the liquid fertilizer is matched with chitosan to prevent the liquid fertilizer from being washed by rainwater and lost.
The invention provides an anti-disease liquid fertilizer which is prepared from the following raw materials in parts by weight: 5-15 parts of radix stemonae, 5-12 parts of scutellaria baicalensis, 10-20 parts of coptis chinensis, 5-12 parts of radix sophorae flavescentis, 5-8 parts of bamboo vinegar, 5-10 parts of chitosan and 8-15 parts of pregelatinized starch.
Preferably, the feed additive is prepared from the following raw materials in parts by weight: 10 parts of radix stemonae, 12 parts of scutellaria baicalensis, 18 parts of coptis chinensis, 8 parts of radix sophorae flavescentis, 8 parts of bamboo vinegar, 10 parts of chitosan and 12 parts of pregelatinized starch.
Preferably, the pregelatinized starch is derived from one or more of corn starch, tapioca starch, or potato starch.
The invention also provides a preparation method of the disease-resistant liquid fertilizer, which comprises the following steps:
weighing radix Stemonae, Scutellariae radix, Coptidis rhizoma, radix Sophorae Flavescentis, bamboo vinegar, chitosan, and pregelatinized starch in parts by weight;
mixing radix Stemonae, Scutellariae radix, Coptidis rhizoma and radix Sophorae Flavescentis, adding 50-80% ethanol solution with mass fraction of 6-10 times of the total amount of the mixture, heating and reflux extracting for 2-3 times, each for 1.0-2.0h, collecting residues, mixing extractive solutions, concentrating, and drying to obtain Chinese medicinal extract;
drying the medicine residues and then carrying out carbonization treatment to obtain biochar;
adding water which is 20-35 times of the amount of the pregelatinized starch into the pregelatinized starch, and uniformly mixing to obtain pregelatinized starch paste;
adding the crushed traditional Chinese medicine extract and the biochar into the pre-gelatinized starch paste, homogenizing for 3-5h, drying, and crushing to obtain particles;
and uniformly dispersing the particles in the mixed solution of the chitosan solution and the bamboo vinegar solution to obtain the liquid fertilizer.
Preferably, the chitosan solution is a solution prepared by mixing chitosan and acetic acid, and the mass concentration of the solution is 0.05-0.1%;
the content of organic acid in the bamboo vinegar liquid is not less than 3 percent;
the mass ratio of the chitosan solution to the bamboo vinegar solution is 1-2: 2-3.
Preferably, the mass ratio of the particulate matter to the mixed solution is 1-3: 8-15.
Preferably, the carbonization treatment is to heat the dried medicine residue to 250 ℃ under the oxygen-limited environment and maintain the temperature for 10-20 min; the temperature is continuously raised to 280-350 ℃ and maintained for 1-3 h.
Preferably, the particle size of the particles is 200-800 meshes.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the disease-resistant liquid fertilizer provided by the invention, dregs of a decoction obtained after extraction of traditional Chinese medicine raw materials are effectively utilized to be pyrolyzed to prepare the biochar, hydroxyl groups are contained on both the biochar and the pregelatinized starch chain, organic acids and other substances in the traditional Chinese medicine extract have an electron withdrawing effect due to carboxyl groups and other groups, and the biochar, the pregelatinized starch and the traditional Chinese medicine extract can be agglomerated through mutual attraction of positive and negative charges; the void structure of the biochar also enables more pregelatinized starch and traditional Chinese medicine extract to be loaded in the biochar, so that the slow release effect is achieved;
meanwhile, the pregelatinized starch has better adhesive property, and is uniformly filled on the surfaces of the biochar and the traditional Chinese medicine extract particles and in gaps formed between the biochar and the traditional Chinese medicine extract particles in the homogenizing process to form slowly-releasable agglomerates;
the agglomerates are uniformly dispersed in a mixed solution of a chitosan solution and a bamboo vinegar solution, chitosan has a film-forming property, and the loaded agglomerates can be uniformly spread on the surface of crops or the surface of soil when a liquid fertilizer is sprayed or dripped, so that the purpose of uniform and slow fertilization is achieved, and meanwhile, the loss of effective components in rainy days or irrigation can be reduced.
2. The bamboo vinegar liquid and the chitosan solution are both acidic solutions, so that the chitosan solution can be further diluted, the phenomenon that the chitosan is not easy to apply due to the thickening effect of the chitosan is avoided, and the bamboo vinegar liquid contains various plant active substances such as plant amino acids, ketones, phenols, alkalis, polysaccharides, synthetases and the like, so that the photosynthetic rate of plants can be increased, the damage to crops caused by natural disasters such as phytotoxicity, fertilizer damage, freezing damage and the like can be relieved and repaired, and the crops can be quickly recovered to grow; it can also activate the immune system of plants, improve the disease and stress resistance of crops, and reduce the occurrence of plant diseases and insect pests.
3. The traditional Chinese medicine extract has the effect of inhibiting or killing various pathogenic bacteria causing crop diseases, and can play a better role in preventing and treating the diseases by combining the effect of the traditional Chinese medicine extract with bamboo vinegar and chitosan solution.
4. The chitosan is a substance which is not easy to dissolve in water, but can absorb water and swell, and due to the existence of the chitosan, the liquid fertilizer can be attached to the surface of crops or soil after being sprayed or drip-irrigated, and is not easy to be washed by rainwater, so that the liquid fertilizer can be applied for several hours before rain, and only the sprayed liquid fertilizer is required to be completely attached (namely, the water content of a film formed by spreading on the surfaces of the crops or soil is below 15%); in addition, the pregelatinized starch can absorb water and swell and is dissolved in cold water, so that the release of effective substances wrapped by the pregelatinized starch can be accelerated in rainy days or irrigation, and the liquid fertilizer is completely free from the influence of rainwater due to the cooperation of the pregelatinized starch and chitosan.
5. The pore structures of the biochar and the pregelatinized starch can provide attachment sites and larger space for microorganisms, and the number of the microorganisms in the soil is increased; and the biochar can improve the change of the soil microenvironment and provide a better growth environment for the deposit of microorganisms, thereby being beneficial to the growth of crops.
Detailed Description
The following detailed description is to be read in connection with specific embodiments, but it should be understood that the scope of the invention is not limited to the specific embodiments.
In the description of the present invention, reagents and starting materials are commercially available and methods for using are conventional in the art, unless otherwise specified.
Example 1
The disease-resistant liquid fertilizer is prepared from the following raw materials in parts by weight: 5 parts of radix stemonae, 5 parts of scutellaria baicalensis, 10 parts of coptis chinensis, 5 parts of radix sophorae flavescentis, 5 parts of bamboo vinegar, 5 parts of chitosan and 8 parts of pregelatinized starch.
Example 2
The disease-resistant liquid fertilizer is prepared from the following raw materials in parts by weight: 10 parts of radix stemonae, 12 parts of scutellaria baicalensis, 18 parts of coptis chinensis, 8 parts of radix sophorae flavescentis, 8 parts of bamboo vinegar, 10 parts of chitosan and 12 parts of pregelatinized starch.
Example 3
The disease-resistant liquid fertilizer is prepared from the following raw materials in parts by weight: 15 parts of radix stemonae, 12 parts of scutellaria baicalensis, 20 parts of coptis chinensis, 12 parts of radix sophorae flavescentis, 8 parts of bamboo vinegar, 10 parts of chitosan and 15 parts of pregelatinized starch.
Example 4
The disease-resistant liquid fertilizer is prepared from the following raw materials in parts by weight: 12 parts of radix stemonae, 12 parts of scutellaria baicalensis, 10 parts of coptis chinensis, 12 parts of radix sophorae flavescentis, 5 parts of bamboo vinegar, 8 parts of chitosan and 12 parts of pregelatinized starch.
Example 5
The disease-resistant liquid fertilizer is prepared from the following raw materials in parts by weight: 15 parts of radix stemonae, 5 parts of scutellaria baicalensis, 15 parts of coptis chinensis, 8 parts of radix sophorae flavescentis, 8 parts of bamboo vinegar, 8 parts of chitosan and 10 parts of pregelatinized starch.
Example 6
The disease-resistant liquid fertilizer is prepared from the following raw materials in parts by weight: 8 parts of radix stemonae, 10 parts of scutellaria baicalensis, 18 parts of coptis chinensis, 12 parts of radix sophorae flavescentis, 6 parts of bamboo vinegar, 5 parts of chitosan and 8 parts of pregelatinized starch.
Example 7
The disease-resistant liquid fertilizer is prepared from the following raw materials in parts by weight: 15 parts of radix stemonae, 12 parts of scutellaria baicalensis, 20 parts of coptis chinensis, 12 parts of radix sophorae flavescentis, 8 parts of bamboo vinegar, 10 parts of chitosan and 15 parts of pregelatinized starch.
Example 8
The disease-resistant liquid fertilizer is prepared from the following raw materials in parts by weight: 12 parts of radix stemonae, 8 parts of scutellaria baicalensis, 12 parts of coptis chinensis, 5 parts of radix sophorae flavescentis, 8 parts of bamboo vinegar, 8 parts of chitosan and 12 parts of pregelatinized starch.
The disease-resistant liquid fertilizers provided in examples 1-8 above were all prepared as follows:
weighing radix Stemonae, Scutellariae radix, Coptidis rhizoma, radix Sophorae Flavescentis, bamboo vinegar, chitosan, and pregelatinized starch in parts by weight;
mixing radix Stemonae, Scutellariae radix, Coptidis rhizoma and radix Sophorae Flavescentis, adding 50% ethanol solution with mass fraction of 10 times of the total amount of the four materials, heating and reflux-extracting for 2 times (1.0 hr each time), collecting residues, mixing extractive solutions, concentrating, and drying to obtain Chinese medicinal extract;
drying the medicinal residue, placing into a carbonization furnace, introducing inert gas into the carbonization furnace until the oxygen content in the carbonization furnace is not more than 3%, heating to 120 deg.C, and maintaining for 20 min; continuously heating to 280 ℃, and maintaining for 3 hours for carbonization treatment to obtain biochar;
adding water which is 20 times of the amount of the pregelatinized starch into the pregelatinized starch, and uniformly mixing to obtain a pregelatinized starch paste;
adding the crushed traditional Chinese medicine extract and the biochar into the pre-gelatinized starch paste, homogenizing for 3h, drying, and crushing to obtain particles;
and uniformly dispersing the particles in a mixed solution of chitosan solution and bamboo vinegar to obtain the liquid fertilizer.
Example 9
The disease-resistant liquid fertilizer is different from the disease-resistant liquid fertilizer in the preparation method of example 1, and specifically comprises the following steps:
weighing radix Stemonae, Scutellariae radix, Coptidis rhizoma, radix Sophorae Flavescentis, bamboo vinegar, chitosan, and pregelatinized starch in parts by weight;
mixing radix Stemonae, Scutellariae radix, Coptidis rhizoma and radix Sophorae Flavescentis, adding 80% ethanol solution with mass fraction of 6 times of the total amount of the four materials, heating and reflux-extracting for 3 times, each time for 2.0 hr, collecting residues, mixing extractive solutions, concentrating, and drying to obtain Chinese medicinal extract;
drying the medicinal residue, placing into a carbonization furnace, introducing inert gas into the carbonization furnace until the oxygen content in the carbonization furnace is not more than 3%, heating to 250 deg.C, and maintaining for 10 min; continuously heating to 280 ℃, and maintaining for 3 hours to obtain biochar;
adding water which is 35 times of the amount of the pregelatinized starch into the pregelatinized starch, and uniformly mixing to obtain a pregelatinized starch paste;
adding the crushed traditional Chinese medicine extract and the biochar into the pre-gelatinized starch paste, homogenizing for 5 hours, drying, and crushing to obtain particles;
and uniformly dispersing the particles in a mixed solution of chitosan solution and bamboo vinegar to obtain the liquid fertilizer.
Example 10
A disease-resistant liquid fertilizer, which is different from the liquid fertilizer prepared in example 9 in that the preparation method comprises the following specific steps:
weighing radix Stemonae, Scutellariae radix, Coptidis rhizoma, radix Sophorae Flavescentis, bamboo vinegar, chitosan, and pregelatinized starch in parts by weight;
mixing radix Stemonae, Scutellariae radix, Coptidis rhizoma and radix Sophorae Flavescentis, adding 60% ethanol solution with mass fraction of 8 times of the total amount of the four materials, heating and reflux-extracting for 2 times, each time for 1.0 hr, collecting residues, mixing extractive solutions, concentrating, and drying to obtain Chinese medicinal extract;
drying the medicinal residue, placing into a carbonization furnace, introducing inert gas into the carbonization furnace until the oxygen content in the carbonization furnace is not more than 3%, heating to 200 deg.C, and maintaining for 15 min; continuously heating to 300 ℃, and maintaining for 2 hours to obtain biochar;
adding water which is 25 times of the amount of the pregelatinized starch into the pregelatinized starch, and uniformly mixing to obtain a pregelatinized starch paste;
adding the crushed traditional Chinese medicine extract and the biochar into the pre-gelatinized starch paste, homogenizing for 5 hours, drying, and crushing to obtain particles;
and uniformly dispersing the particles in a mixed solution of chitosan solution and bamboo vinegar to obtain the liquid fertilizer.
Comparative example 1
A disease-resistant liquid fertilizer, which is different from example 1 in that: no pregelatinized starch was added.
Comparative example 2
A disease-resistant liquid fertilizer, which is different from example 1 in that: no biochar was added.
Comparative example 3
A disease-resistant liquid fertilizer, which is different from example 1 in that: no chitosan was added.
Comparative example 4
A disease-resistant liquid fertilizer, which is different from example 1 in that: bamboo vinegar was not added.
Comparative example 5
A disease-resistant liquid fertilizer, which is different from example 1 in that: the traditional Chinese medicine extract is replaced by a special granular fertilizer slow-release fertilizer (brand name growth magic) for the commercial Lei Li Hai organic fertilizer universal type flower, vegetable and plant.
Experimental example 1
Description of the Slow Release Properties of the liquid Fertilizer
1. Method of producing a composite material
20g of liquid fertilizer is weighed, 20 times of water is added to soak the fertilizer at a constant temperature of 25 ℃, and the initial dissolution rate and the dissolution rate of 2 to 7 days are respectively measured. Wherein the initial dissolution rate is calculated according to formula (1):
initial dissolution rate of 24 h/content of the extract in the sample (1)
The dissolved substances are several antibacterial and insecticidal effective components in the liquid fertilizer, namely baicalin and berberine hydrochloride.
The content determination of baicalin refers to a method for determining the content of baicalin in a finished prescription preparation recorded in the first part of Chinese pharmacopoeia, which adopts a high performance liquid chromatography, and comprises the following specific steps:
octadecylsilane chemically bonded silica is used as a filler in chromatographic conditions and system applicability tests; methanol-water-phosphoric acid (50:50:0.3) is used as a mobile phase; the detection wavelength was 276 nm. The number of theoretical plates is not less than 1000 calculated according to baicalin peak.
Preparation of reference solution A proper amount of baicalin reference substance is precisely weighed, and added with 70% ethanol to obtain a solution containing 25 μ g of baicalin per 1 ml.
Precisely measuring 2ml of the product to be tested, placing into a 10ml measuring flask, adding 70% ethanol, shaking, diluting with 70% ethanol to scale, shaking, standing, filtering, and collecting the filtrate.
The determination method comprises precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into liquid chromatograph, and determining.
The content of berberine hydrochloride is determined by referring to a method for determining the content of baicalin in a finished prescription preparation recorded in Chinese pharmacopoeia, namely by adopting a high performance liquid chromatography, and the specific method comprises the following steps:
octadecylsilane chemically bonded silica is used as a filler in chromatographic conditions and system applicability tests; acetonitrile-0.033 mol/L potassium dihydrogen phosphate solution (35: 65) is used as a mobile phase; the detection wavelength was 345 nm. The number of theoretical plates is not less than 4000 calculated according to berberine hydrochloride peak.
Preparation of reference substance solution taking appropriate amount of berberine hydrochloride reference substance, precisely weighing, and adding methanol to obtain solution containing 25 μ g per 1 ml.
Preparing a sample solution, precisely measuring 2mL of the sample solution, placing the sample solution in a conical flask with a plug, precisely adding 10mL of a hydrochloric acid-methanol (1: 100) mixed solution, weighing, heating in a 50 ℃ water bath for 15min, taking out, cooling, carrying out ultrasonic treatment (power 250W and frequency 33kHz) for 30min, cooling, weighing again, supplementing the lost weight with methanol, shaking up, filtering, precisely taking 2mL of a subsequent filtrate, volatilizing the solvent at low temperature, dissolving residues with a proper amount of methanol, adding the residues onto an alkaline alumina column (100-200 meshes, 8g and inner diameter of 1cm), eluting with 35mL of methanol, collecting the eluate, evaporating to dryness, adding methanol to dissolve the residues, transferring the residues into a 10mL measuring flask, adding methanol to dilute to scale, and shaking to obtain the test sample.
The determination method comprises precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into liquid chromatograph, and determining.
2. Results
The results are shown in tables 1-2.
TABLE 1 change in the dissolution rate of baicalin (%)
Grouping Initial stage 2d 3d 4d 5d 6d 7d
Example 1 1.22 2.31 3.54 5.32 7.34 9.13 12.46
Example 2 1.23 2.33 3.56 6.01 7.76 9.46 12.97
Example 3 1.21 2.29 3.49 5.56 7.89 8.94 13.01
Example 4 1.19 2.28 3.29 5.76 7.92 8.59 13.34
Example 5 1.25 2.36 3.67 5.23 8.03 8.98 12.66
Example 6 1.17 2.27 3.39 5.84 7.37 9.43 12.87
Example 7 1.24 2.34 3.78 6.14 7.83 8.61 13.38
Example 8 1.15 2.29 3.54 5.97 7.24 9.43 12.76
Example 9 1.22 2.32 3.68 5.94 7.63 8.23 13.55
Example 10 1.18 2.30 3.87 5.22 7.91 9.13 12.89
Comparative example 1 3.34 5.19 8.23 13.67 20.45 27.49 36.69
Comparative example 2 2.56 4.24 6.42 11.23 16.72 21.34 28.47
Comparative example 3 1.26 2.35 5.01 10.02 15.03 19.76 23.34
Comparative example 4 2.87 4.56 7.13 11.98 17.78 21.49 24.46
Comparative example 5 1.23 2.34 5.67 9.85 15.14 18.85 25.37
TABLE 2 change in dissolution rate (%) of berberine hydrochloride in each example and comparative example
Figure BDA0003360325010000101
Figure BDA0003360325010000111
As can be seen from tables 1-2, the dissolution rates of the antibacterial and bactericidal active ingredients baicalin and berberine hydrochloride of the liquid fertilizer provided by the application are slowly increased along with the increase of the soaking time, and are only 12.46% -14.83% at the 7 th day of soaking, which indicates that the liquid fertilizer provided by the invention has better slow release performance, can be slowly released even after being soaked in water for a long time, and reduces the loss of the active ingredients of the fertilizer.
Experimental example 2
The disease resistance effect of the liquid fertilizer provided in example 1 will be described by taking the liquid fertilizer as an example.
Selecting test areas with basically the same corn growth conditions, randomly dividing the test areas into 6 areas, dividing each area into 3 cells, wherein each cell is randomly arranged and comprises 50 corns. Wherein, the fertilizers provided by the embodiment 1 and the comparative examples 1 to 4 are respectively applied to 5 areas, and are respectively diluted by 800 times with clear water and then sprayed; the rest 1 area was applied with Taibaofeng microbial inoculum (produced by Schlemongtai Biotechnology Co., Ltd.), hole application, application amount of 40 g/strain, as an observation group. Each cell is 3 groups of repeated tests of each cell, the disease incidence rate of each cell is counted after 1 month, and the average value of 3 cells in the same cell is taken as the disease incidence rate of each cell. The results are shown in Table 3.
Table 3 statistics of disease incidence (%) -for each group of example 1, comparative examples 1 to 4 and observation group
Figure BDA0003360325010000112
Figure BDA0003360325010000121
Tomato was used as the subject in the same manner, and the disease incidence was counted after 1 month, and the results are shown in table 4.
Table 4 statistics of disease incidence (%) -for each group of example 1, comparative examples 1 to 4 and observation group
Grouping Disease incidence (%)
Example 1 4.00
Comparative example 1 3.33
Comparative example 2 4.67
Comparative example 3 8.00
Comparative example 4 9.33
Observation group 4.67
As can be seen from tables 3 to 4, the disease resistance effect of the liquid fertilizer of the group of example 1 is superior to that of the existing disease resistance fertilizer, suggesting that the liquid fertilizer provided by the present invention has a better disease resistance effect; meanwhile, the disease resistance effect of the liquid fertilizer in the group 1 is better than that of each proportional group, which suggests that the raw materials of the liquid fertilizer provided by the invention have a synergistic effect.
The above disclosure is only for a few specific embodiments of the present invention, however, the present invention is not limited to the above embodiments, and any variations that can be made by those skilled in the art are intended to fall within the scope of the present invention.

Claims (8)

1. The disease-resistant liquid fertilizer is characterized by being prepared from the following raw materials in parts by weight: 5-15 parts of radix stemonae, 5-12 parts of scutellaria baicalensis, 10-20 parts of coptis chinensis, 5-12 parts of radix sophorae flavescentis, 5-8 parts of bamboo vinegar, 5-10 parts of chitosan and 8-15 parts of pregelatinized starch.
2. The disease-resistant liquid fertilizer as claimed in claim 1, which is prepared from the following raw materials in parts by weight: 10 parts of radix stemonae, 12 parts of scutellaria baicalensis, 18 parts of coptis chinensis, 8 parts of radix sophorae flavescentis, 8 parts of bamboo vinegar, 10 parts of chitosan and 12 parts of pregelatinized starch.
3. The disease-resistant liquid fertilizer as claimed in claim 1 or 2, wherein the pregelatinized starch is derived from one or a mixture of corn starch, tapioca starch, or potato starch.
4. The method for preparing the disease-resistant liquid fertilizer as claimed in claim 1 or 2, comprising the steps of:
weighing radix Stemonae, Scutellariae radix, Coptidis rhizoma, radix Sophorae Flavescentis, bamboo vinegar, chitosan, and pregelatinized starch in parts by weight;
mixing radix Stemonae, Scutellariae radix, Coptidis rhizoma and radix Sophorae Flavescentis, adding 50-80% ethanol solution with mass fraction of 6-10 times of the total amount of the mixture, reflux extracting for 2-3 times (1.0-2.0 hr for each time), collecting residues, mixing extractive solutions, concentrating, and drying to obtain Chinese medicinal extract;
drying the medicine residues and then carrying out carbonization treatment to obtain biochar;
adding water which is 20-35 times of the amount of the pregelatinized starch into the pregelatinized starch, and uniformly mixing to obtain pregelatinized starch paste;
adding the crushed traditional Chinese medicine extract and the biochar into the pre-gelatinized starch paste, homogenizing for 3-5h, drying, and crushing to obtain particles;
and uniformly dispersing the particles in the mixed solution of the chitosan solution and the bamboo vinegar solution to obtain the liquid fertilizer.
5. The method for producing a disease-resistant liquid fertilizer as claimed in claim 4,
the chitosan solution is prepared by mixing the chitosan and acetic acid, and the mass concentration of the solution is 0.05-0.1%;
the content of organic acid in the bamboo vinegar liquid is not less than 3 percent;
the mass ratio of the chitosan solution to the bamboo vinegar solution is 1-2: 2-3.
6. The method for preparing the disease-resistant liquid fertilizer as claimed in claim 5, wherein the mass ratio of the particulate matter to the mixed solution is 1-3: 8-15.
7. The method for preparing the disease-resistant liquid fertilizer as claimed in claim 4, wherein the carbonization treatment is carried out by heating the dried medicine residue to 250 ℃ under an oxygen-limited environment, and maintaining the temperature for 10-20 min; the temperature is continuously raised to 280-350 ℃ and maintained for 1-3 h.
8. The method for preparing the disease-resistant liquid fertilizer as recited in claim 4, wherein the particle size of the particles is 200-800 mesh.
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