CN107986886B - Essential oil fertilizer and preparation method thereof - Google Patents
Essential oil fertilizer and preparation method thereof Download PDFInfo
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- CN107986886B CN107986886B CN201711491642.6A CN201711491642A CN107986886B CN 107986886 B CN107986886 B CN 107986886B CN 201711491642 A CN201711491642 A CN 201711491642A CN 107986886 B CN107986886 B CN 107986886B
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- 235000001484 Trigonella foenum graecum Nutrition 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 1
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 235000013877 carbamide Nutrition 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 230000019522 cellular metabolic process Effects 0.000 description 1
- 229940106157 cellulase Drugs 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000002124 endocrine Effects 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000005556 hormone Substances 0.000 description 1
- 229940088597 hormone Drugs 0.000 description 1
- 230000000415 inactivating effect Effects 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 235000019837 monoammonium phosphate Nutrition 0.000 description 1
- 239000006012 monoammonium phosphate Substances 0.000 description 1
- 229950006780 n-acetylglucosamine Drugs 0.000 description 1
- 239000000618 nitrogen fertilizer Substances 0.000 description 1
- 238000010606 normalization Methods 0.000 description 1
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- 210000000056 organ Anatomy 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000002686 phosphate fertilizer Substances 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
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- 235000001019 trigonella foenum-graecum Nutrition 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C9/00—Fertilisers containing urea or urea compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Pest Control & Pesticides (AREA)
- Fertilizers (AREA)
Abstract
The invention relates to an essential oil fertilizer and a preparation method thereof. The invention can effectively improve the utilization rate of the fertilizer, improve the quality of crops and achieve the purpose of increasing the yield.
Description
Technical Field
The invention relates to an essential oil fertilizer and a preparation method thereof.
Background
The essential oil can prevent infectious diseases, bacteria, viruses and mould, prevent inflammation and spasm, promote cell metabolism and cell regeneration, and make life more beautiful. Some essential oils can regulate endocrine organs, promote hormone secretion, and promote physiological and psychological activities of human body.
At present, the general utilization rate of the fertilizer is not high, the utilization rate of a nitrogen fertilizer is only about 25%, the utilization rate of a phosphate fertilizer is about 20%, and the utilization rate of potassium is about 30%. In order to realize zero growth of chemical fertilizers and pesticides, the improvement of the utilization rate of fertilizers is urgently needed.
Disclosure of Invention
The invention aims to solve the technical problem of providing an essential oil fertilizer and a preparation method thereof, and the essential oil fertilizer can effectively improve the utilization rate of the fertilizer, improve the quality of crops and achieve the purpose of increasing the yield.
In order to solve the technical problems, the invention adopts the following technical scheme:
an essential oil fertilizer, which is characterized in that: consists of fertilizer and essential oil.
Preferably, the mass ratio of the fertilizer to the essential oil is 50-99.99: 0.01-50;
the fertilizer comprises one or more than two of simple substance fertilizer, compound fertilizer, bulk blend fertilizer, organic-inorganic fertilizer, biological organic fertilizer, organic fertilizer and water-soluble fertilizer in any proportion;
the essential oil is one or more than two of essential oil stock solution, compound essential oil, essential oil-containing diluent and essential oil-containing residue in any proportion.
Adding the essential oil into the fertilizer and uniformly mixing to obtain an essential oil fertilizer;
the essential oil is prepared according to the following steps:
carrying out enzymolysis on essential oil plants by lysozyme, carrying out enzyme deactivation, extracting by liquid carbon dioxide after enzyme deactivation, and separating to obtain essential oil, wherein the separated residue is the residue containing the essential oil;
the essential oil plant is one or more than two of lavender, rose, bay, lemon, tea tree, cypress, geranium and sage in any proportion.
The essential oil plant is a fresh essential oil plant,
the fresh essential oil plant is one or two of essential oil plants which are just picked and essential oil plants which are stored in an environment of-20 to-5 ℃ just after being picked in any proportion.
The lysozyme enzymolysis further comprises water, wherein the mass ratio of the fresh essential oil plants to the lysozyme to the water is 10-50: 0.02-1: 50-90; the enzymolysis temperature is 27-55 ℃, and the enzymolysis time is 30-60 min.
The enzyme deactivation temperature is 80-120 ℃, the enzyme deactivation time is 5-20 min, and the enzyme deactivation pressure is 0-5 MPa.
The temperature of the liquid carbon dioxide is 15-31.26 ℃, the pressure is 5-10 MPa, the flow rate is 25-35L/h, and the extraction time is 0.5-2 h.
The method also comprises the step of adding a retention agent into the essential oil, wherein the mass ratio of the essential oil to the retention agent is 50-99.5: 0.5-50;
the retention agent is one or more than two of ethylene glycol, glycerol and isopropanol in any proportion.
The separation comprises primary separation kettle separation and secondary separation kettle separation, wherein the separation pressure of the primary separation kettle is 6-8 MPa, the separation temperature is 30-50 ℃, and the separation time is 0.5-3 h; the separation pressure of the secondary separation kettle is 4-6 MPa, the separation temperature is 25-40 ℃, and the separation time is 0.5-3 h; residue is left at the bottom after the first-stage separation kettle is separated to form a mixture.
Transferring the mixture to an oil-water separator, adding a flocculating agent into the mixture, standing for 20-150 min, wherein the mass ratio of the mixture to the flocculating agent is 99-99.99: 0.01-1, and performing oil-water separation at 30-50 ℃ to obtain lavender wax and a water treatment substance; filtering the water-treated product to obtain water and residue containing essential oil;
the flocculating agent is one or more than two of activated clay, polyaluminium chloride, sodium polyacrylate and polyacrylamide in any proportion.
The invention has the following beneficial technical effects:
1. the invention can effectively improve the utilization rate of the fertilizer, improve the quality of crops and achieve the purpose of increasing the yield.
2. The extraction of the essential oil utilizes lysozyme to break beta-1, 4 glycosidic bond between N-acetylmuramic acid and N-acetylglucosamine in cell wall, so that insoluble mucopolysaccharide of the cell wall is decomposed into soluble glycopeptide, and the content with broken cell wall escapes to facilitate extraction.
3. The essential oil extraction process adopts a low-temperature low-pressure extraction mode, effectively prevents the essential oil from being damaged by higher temperature and pressure, and is superior to supercritical extraction and subcritical extraction.
4. The addition of the retention agent can obviously prolong the service life of the essential oil.
5. The invention can obviously shorten the extraction time by lysozyme treatment.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
Adding lavender essential oil into urine, and performing spray granulation, drying, cooling and screening to obtain essential oil urea; the mass ratio of the lavender essential oil to the urine is 0.2: 99.8.
The lavender essential oil is prepared according to the following steps:
carrying out enzymolysis on freshly picked fresh lavender by lysozyme, then carrying out enzyme deactivation, extracting by liquid carbon dioxide after enzyme deactivation, and separating to obtain lavender essential oil;
the lysozyme enzymolysis further comprises water, wherein the mass ratio of the fresh lavender to the lysozyme to the water is 20:0.08: 79.92; the enzymolysis temperature is 35 ℃, and the enzymolysis time is 40 min.
The enzyme deactivation temperature is 100 ℃, the enzyme deactivation time is 10min, and the enzyme deactivation pressure is 2 MPa.
The temperature of the liquid carbon dioxide is 28 ℃, the pressure is 8MPa, the flow rate is 27L/h, and the extraction time is 0.8 h.
The method also comprises the steps of adding glycerol into the essential oil, wherein the mass ratio of the essential oil to the glycerol is 98: 2;
the separation comprises primary separation kettle separation and secondary separation kettle separation, wherein the separation pressure of the primary separation kettle is 8MPa, the separation temperature is 50 ℃, and the separation time is 1.5 h; the separation pressure of the secondary separation kettle is 5MPa, the separation temperature is 35 ℃, and the separation time is 2 h; residue is left at the bottom after the first-stage separation kettle is separated to form a mixture.
Transferring the mixture to an oil-water separator, adding activated clay into the mixture, standing for 100min, and performing oil-water separation at 35 ℃ to obtain lavender wax and water treatment product, wherein the mass ratio of the mixture to the activated clay is 99.95: 0.05; filtering the water treatment product to obtain water and residue containing essential oil.
Example 2
Adding the lavender essential oil into a fertilizer granulation roller, mixing with the fertilizer raw materials, granulating by the roller, drying, cooling and screening to obtain an essential oil compound fertilizer; the mass ratio of the essential oil to the fertilizer raw material is 2: 98; the fertilizer raw material is a mixture of urea, monoammonium phosphate and potassium chloride
The lavender essential oil is prepared according to the following steps:
thawing fresh lavender stored in the environment of-20 deg.C, performing enzymolysis with lysozyme, inactivating enzyme, extracting with liquid carbon dioxide, and separating to obtain lavender essential oil;
the lysozyme enzymolysis further comprises water, wherein the mass ratio of the fresh lavender to the lysozyme to the water is 25:0.5: 74.5; the enzymolysis temperature is 30 ℃, and the enzymolysis time is 50 min.
The enzyme deactivation temperature is 90 ℃, and the enzyme deactivation time is 15 min.
The temperature of the liquid carbon dioxide is 25 ℃, the pressure is 9MPa, the flow rate is 30L/h, and the extraction time is 1.5 h.
Adding isopropanol into the essential oil, wherein the mass ratio of the essential oil to the isopropanol is 65: 35;
the separation comprises primary separation kettle separation and secondary separation kettle separation, wherein the separation pressure of the primary separation kettle is 6MPa, the separation temperature is 50 ℃, and the separation time is 1.5 h; the separation pressure of the secondary separation kettle is 6MPa, the separation temperature is 30 ℃, and the separation time is 2 h; residue is left at the bottom after the first-stage separation kettle is separated to form a mixture.
Transferring the mixture to an oil-water separator, adding 0.5% polyacrylamide aqueous solution into the mixture, standing for 120min, and performing oil-water separation at 45 ℃ to obtain lavender wax and water treatment product, wherein the mass ratio of the mixture to the polyacrylamide aqueous solution is 99: 1; filtering the water treatment product to obtain water and residue containing essential oil.
Example 3
Adding the lavender essential oil into the liquid water-soluble fertilizer, and uniformly mixing to obtain an essential oil liquid water-soluble fertilizer; the mass ratio of the lavender essential oil to the liquid water-soluble fertilizer is 0.4: 99.6.
The lavender essential oil is prepared according to the following steps:
carrying out enzymolysis on fresh lavender by lysozyme, then carrying out enzyme deactivation, extracting by liquid carbon dioxide after enzyme deactivation, and separating to obtain lavender essential oil;
the lysozyme enzymolysis further comprises water, wherein the mass ratio of the fresh lavender to the lysozyme to the water is 45:0.5: 54.5; the enzymolysis temperature is 42 ℃, and the enzymolysis time is 45 min.
The enzyme deactivation temperature is 120 ℃, the enzyme deactivation time is 6min, and the enzyme deactivation pressure is 3 MPa.
The temperature of the liquid carbon dioxide is 30 ℃, the pressure is 8MPa, the flow rate is 30L/h, and the extraction time is 0.9 h.
The method also comprises the step of adding a retention agent into the essential oil, wherein the mass ratio of the essential oil to the retention agent is 90: 10;
the retention agent is a composition of glycerol and isopropanol according to the mass ratio of 1: 1.
The separation comprises primary separation kettle separation and secondary separation kettle separation, wherein the separation pressure of the primary separation kettle is 7MPa, the separation temperature is 50 ℃, and the separation time is 2.5 h; the separation pressure of the secondary separation kettle is 5MPa, the separation temperature is 35 ℃, and the separation time is 2 h; residue is left at the bottom after the first-stage separation kettle is separated to form a mixture.
Transferring the mixture to an oil-water separator, adding a flocculating agent into the mixture, standing for 100min, and performing oil-water separation at 32 ℃ to obtain lavender wax and a water treatment product, wherein the mass ratio of the mixture to the flocculating agent is 99.4: 0.6; filtering the water-treated product to obtain water and residue containing essential oil;
the flocculant is a composition of activated clay and polyaluminium chloride according to the mass ratio of 1: 1.
Example 4
Adding the lavender essential oil into the bio-organic fertilizer, and performing extrusion granulation and screening to obtain an essential oil bio-organic fertilizer; the mass ratio of the lavender essential oil to the bio-organic fertilizer is 1: 99.
The lavender essential oil is prepared according to the following steps:
adding fresh lavender, water and lysozyme into a reaction kettle, wherein the mass ratio of the fresh lavender, the lysozyme to the water is 40:0.05:59.95, carrying out enzymolysis, the enzymolysis temperature is 42 ℃, the enzymolysis time is 60min, carrying out liquid carbon dioxide extraction under the conditions that the temperature is 29 ℃, the pressure is 9MPa, the flow rate is 25L/h and the extraction time is 1.2h after enzyme deactivation is carried out for 7min under the condition that the temperature is 110 ℃, and carrying out separation in a primary separation kettle and a secondary separation kettle, wherein the separation pressure of the primary separation kettle is 7MPa, the separation temperature is 45 ℃, the separation time is 2h, and residues are left at the bottom of the primary separation kettle after separation to obtain a mixture; the separation pressure of the secondary separation kettle is 4MPa, the separation temperature is 25-40 ℃, and the separation time is 3 h; the liquid discharged from the secondary separation kettle is essential oil stock solution, and the glycerol is added into the essential oil stock solution to obtain essential oil; the mass ratio of the essential oil to the glycerol is 96: 4.
Transferring the mixture at the bottom of the first-stage separation kettle to an oil-water separator, adding activated clay into the mixture, standing for 60min, and performing oil-water separation at 42 ℃ to obtain lavender wax and a water treatment product, wherein the mass ratio of the mixture to the activated clay is 99.5: 0.5; filtering the water treatment product to obtain water and residue containing essential oil, reusing the water to participate in enzymolysis, and using the residue for preparing the fertilizer.
Example 5
Adding the laurel essential oil into the bio-organic fertilizer, and performing extrusion granulation and screening to obtain an essential oil bio-organic fertilizer; the mass ratio of the bay laurel essential oil to the bio-organic fertilizer is 1: 99.
The bay essential oil is prepared according to the following steps:
adding fresh laurel leaves, water and lysozyme into a reaction kettle, wherein the mass ratio of the fresh laurel leaves, the lysozyme to the water is 40:0.05:59.95, carrying out enzymolysis, the enzymolysis temperature is 42 ℃, the enzymolysis time is 60min, carrying out liquid carbon dioxide extraction under the conditions of 29 ℃, 9MPa and 25L/h of flow rate after enzyme deactivation for 7min at the temperature of 110 ℃, the extraction time is 1.2h, and carrying out separation in a primary separation kettle and a secondary separation kettle, wherein the separation pressure of the primary separation kettle is 7MPa, the separation temperature is 45 ℃, the separation time is 2h, and residues are left at the bottom of the primary separation kettle after separation to obtain a mixture; the separation pressure of the secondary separation kettle is 4MPa, the separation temperature is 25-40 ℃, and the separation time is 3 h; the liquid discharged from the secondary separation kettle is essential oil stock solution, and glycerol is added into the essential oil stock solution to obtain the laurel essential oil; the mass ratio of the laurel essential oil to the glycerol is 96: 4.
Transferring the mixture at the bottom of the primary separation kettle to an oil-water separator, adding activated clay into the mixture, standing for 60min, and performing oil-water separation at 42 ℃ to obtain laurel wax and a water treatment substance, wherein the mass ratio of the mixture to the activated clay is 99.5: 0.5; filtering the water treatment product to obtain water and residue containing essential oil, reusing the water to participate in enzymolysis, and using the residue for preparing the fertilizer.
Example 6
Adding tea tree essential oil into a bio-organic fertilizer, and performing extrusion granulation and screening to obtain an essential oil bio-organic fertilizer; the mass ratio of the tea tree essential oil to the bio-organic fertilizer is 1: 99.
The tea tree essential oil is prepared according to the following steps:
adding fresh tea leaves, water and lysozyme into a reaction kettle, wherein the mass ratio of the fresh tea leaves, the lysozyme and the water is 40:0.05:59.95, carrying out enzymolysis, the enzymolysis temperature is 42 ℃, the enzymolysis time is 60min, carrying out liquid carbon dioxide extraction under the conditions of 29 ℃, 9MPa and 25L/h of flow rate after enzyme deactivation for 7min at the temperature of 110 ℃, the extraction time is 1.2h, and carrying out primary separation kettle separation and secondary separation kettle separation, wherein the separation pressure of the primary separation kettle is 7MPa, the separation temperature is 45 ℃, the separation time is 2h, and residues are left at the bottom of the primary separation kettle after separation to obtain a mixture; the separation pressure of the secondary separation kettle is 4MPa, the separation temperature is 25-40 ℃, and the separation time is 3 h; the liquid discharged from the secondary separation kettle is essential oil stock solution, and glycerol is added into the essential oil stock solution to obtain tea tree essential oil; the mass ratio of the essential oil to the glycerol is 96: 4.
Transferring the mixture at the bottom of the primary separation kettle to an oil-water separator, adding activated clay into the mixture, standing for 60min, and performing oil-water separation at 42 ℃ to obtain tea wax and water treatment substances, wherein the mass ratio of the mixture to the activated clay is 99.5: 0.5; filtering the water treatment product to obtain water and residue containing essential oil, reusing the water to participate in enzymolysis, and using the residue for preparing the fertilizer.
Example 7
Adding the compound essential oil into the bio-organic fertilizer, and performing extrusion granulation and screening to obtain the essential oil bio-organic fertilizer; the mass ratio of the compound essential oil to the biological organic fertilizer is 1: 99.
The compound essential oil is prepared according to the following steps:
1) adding fresh lavender, water and lysozyme into a reaction kettle, wherein the mass ratio of the fresh lavender, the lysozyme to the water is 40:0.05:59.95, carrying out enzymolysis, the enzymolysis temperature is 42 ℃, the enzymolysis time is 60min, carrying out liquid carbon dioxide extraction under the conditions that the temperature is 29 ℃, the pressure is 9MPa, the flow rate is 25L/h and the extraction time is 1.2h after enzyme deactivation is carried out for 7min under the condition that the temperature is 110 ℃, and carrying out separation in a primary separation kettle and a secondary separation kettle, wherein the separation pressure of the primary separation kettle is 7MPa, the separation temperature is 45 ℃, the separation time is 2h, and residues are left at the bottom of the primary separation kettle after separation to obtain a mixture; the separation pressure of the secondary separation kettle is 4MPa, the separation temperature is 25-40 ℃, and the separation time is 3 h; the liquid discharged from the secondary separation kettle is essential oil stock solution, and the glycerol is added into the essential oil stock solution to obtain essential oil; the mass ratio of the essential oil to the glycerol is 96: 4.
Transferring the mixture at the bottom of the first-stage separation kettle to an oil-water separator, adding activated clay into the mixture, standing for 60min, and performing oil-water separation at 42 ℃ to obtain lavender wax and a water treatment product, wherein the mass ratio of the mixture to the activated clay is 99.5: 0.5; filtering the water treatment product to obtain water and residue containing essential oil, reusing the water to participate in enzymolysis, and using the residue for preparing the fertilizer.
2) Adding fresh tea leaves, water and lysozyme into a reaction kettle, wherein the mass ratio of the fresh tea leaves, the lysozyme and the water is 40:0.05:59.95, carrying out enzymolysis, the enzymolysis temperature is 42 ℃, the enzymolysis time is 60min, carrying out liquid carbon dioxide extraction under the conditions of 29 ℃, 9MPa and 25L/h of flow rate after enzyme deactivation for 7min at the temperature of 110 ℃, the extraction time is 1.2h, and carrying out primary separation kettle separation and secondary separation kettle separation, wherein the separation pressure of the primary separation kettle is 7MPa, the separation temperature is 45 ℃, the separation time is 2h, and residues are left at the bottom of the primary separation kettle after separation to obtain a mixture; the separation pressure of the secondary separation kettle is 4MPa, the separation temperature is 25-40 ℃, and the separation time is 3 h; the liquid discharged from the secondary separation kettle is essential oil stock solution, and glycerol is added into the essential oil stock solution to obtain tea tree essential oil; the mass ratio of the essential oil to the glycerol is 96: 4.
Transferring the mixture at the bottom of the primary separation kettle to an oil-water separator, adding activated clay into the mixture, standing for 60min, and performing oil-water separation at 42 ℃ to obtain tea wax and water treatment substances, wherein the mass ratio of the mixture to the activated clay is 99.5: 0.5; filtering the water treatment product to obtain water and residue containing essential oil, reusing the water to participate in enzymolysis, and using the residue for preparing the fertilizer.
Mixing the lavender essential oil prepared in the step 1) and the tea tree essential oil prepared in the step 2) according to the mass ratio of 1:1 to obtain the compound essential oil.
Example 8
Adding the residue containing the essential oil into the bio-organic fertilizer, and performing extrusion granulation and screening to obtain the essential oil bio-organic fertilizer; the mass ratio of the residue containing the essential oil to the biological organic fertilizer is 30: 70.
The lavender essential oil-containing residue is prepared according to the following steps:
adding fresh lavender, water and lysozyme into a reaction kettle, wherein the mass ratio of the fresh lavender, the lysozyme to the water is 40:0.05:59.95, carrying out enzymolysis, the enzymolysis temperature is 42 ℃, the enzymolysis time is 60min, carrying out liquid carbon dioxide extraction under the conditions that the temperature is 29 ℃, the pressure is 9MPa, the flow rate is 25L/h and the extraction time is 1.2h after enzyme deactivation is carried out for 7min under the condition that the temperature is 110 ℃, and carrying out separation in a primary separation kettle and a secondary separation kettle, wherein the separation pressure of the primary separation kettle is 7MPa, the separation temperature is 45 ℃, the separation time is 2h, and residues are left at the bottom of the primary separation kettle after separation to obtain a mixture; the separation pressure of the secondary separation kettle is 4MPa, the separation temperature is 25-40 ℃, and the separation time is 3 h; the liquid discharged from the secondary separation kettle is essential oil stock solution, and the glycerol is added into the essential oil stock solution to obtain essential oil; the mass ratio of the essential oil to the glycerol is 96: 4.
Transferring the mixture at the bottom of the first-stage separation kettle to an oil-water separator, adding activated clay into the mixture, standing for 60min, and performing oil-water separation at 42 ℃ to obtain lavender wax and a water treatment product, wherein the mass ratio of the mixture to the activated clay is 99.5: 0.5; filtering the water treatment product to obtain water and residue containing essential oil.
The beneficial effects of the present invention are further illustrated below in conjunction with experimental data:
experiment-essential oil detection
1. Experimental materials
1, materials and methods:
1.1 test site: an oil production enterprise Yili Xinjiang.
1.2 test materials: effects were compared with lavender essential oils prepared in examples 1 to 4, comparative example 1 (except that the extraction method was supercritical carbon dioxide extraction, the other preparation methods were the same as in example 1), comparative example 2 (except that lysozyme treatment was performed, but the extraction method was supercritical carbon dioxide extraction, the other preparation methods were the same as in example 1), comparative example 4 (except that lysozyme treatment was not performed, the other preparation methods were the same as in example 1), and comparative example 5 (except that lysozyme was replaced with a composition comprising cellulase AE80 and xylanase at a mass ratio of 1:3, the other preparation methods were the same as in example 1).
1.3, detection: relative total content and essential oil volatility of linalool, linalyl acetate and lavender acetate.
1.4 detection method: detecting the relative total content and the volatility of linalool, linalyl acetate and lavender acetate in the crude oil by adopting a Thermo Focus DSQ chromatograph-mass spectrometer, wherein the detection method of the relative total content comprises the following steps:
a chromatographic column: VF-5ms quartz capillary chromatography column (30 m.times.0.25 mm. times.0.25 μm, Varian) column temperature: 60 ℃ (keeping for 2 min) to 300 ℃ (heating rate: 20 ℃/min, keeping for 5 min) injection port temperature: transmission line temperature of 250 ℃: ion source temperature of 250 ℃: 250 ℃ carrier gas (flow): he (1.0mL/min, >99.999%) sample size: 1.0 μ L split ratio: 250:1 mass spectrometer detector: EI source, 70eV mass range: 41-350 amu search spectral library: the relative content of NIST library is calculated by an area normalization method, and the measurement result is shown in table 1;
measurement of volatility of essential oil Lavender essential oil prepared in the same weight as in examples 1 to 4 and comparative example 3 (except that no retention agent was added, the other preparation methods were the same as in example 1) was placed in an open bottle of 5cm by 5cm, left open at 25 ℃ for 48 hours, and the total content of linalool, linalyl acetate and lavender acetate was measured by using a Thermo Focus DSQ chromatograph-mass spectrometer, and the measurement results are shown in Table 2.
The experiment was conducted in a consistent manner except for the different treatments used in the experiment.
2 results and analysis
2.1 the relative total content of linalool, linalyl acetate and lavender acetate in the crude oil is shown in Table 1
TABLE 1
| Total content (%) | |
| Example 1 | 76.3 |
| Example 2 | 75.3 |
| Example 3 | 75.8 |
| Example 4 | 75.6 |
| Comparative example 1 | 72.7 |
| Comparative example 2 | 70.8 |
| Comparative example 4 | 15.6 |
| Comparative example 5 | 62.3 |
2.2 after standing for 48h, the remaining total content of linalool, linalyl acetate and lavender acetate is shown in Table 2
TABLE 2
| Total content (%) | |
| Example 1 | 18.4 |
| Example 2 | 8.2 |
| Example 3 | 16.8 |
| Examples4 | 20.6 |
| Comparison 3 | 3.1 |
As can be seen from table 1, the lavender essential oil extracted by lysozyme and liquid carbon dioxide and prepared by the invention has higher essential oil content than the lavender essential oil extracted by supercritical carbon dioxide and prepared by comparison 1, and is also higher than the lavender essential oil prepared by lysozyme treatment and then supercritical treatment and prepared by comparison 2, the content of the essential oil in comparison 1 is higher than that in comparison 2, and the decomposition of the essential oil caused by higher temperature and pressure is likely to be testified; as can be seen from comparison of the lavender essential oils prepared in example 1 and comparative example 4, the extraction rate of the essential oil is much lower than that of example 1 in comparative example 4 without lysozyme treatment; as can be seen from comparison of comparative example 5 with example 1, the effect of the treatment with lysozyme was better than that with the other enzymes.
As can be seen from Table 2, the invention added with the retention agent can obviously delay the volatilization of the essential oil and prolong the service life.
Experiment two fertilizer efficiency experiment
1. Experimental materials
1, materials and methods:
1.1 test site: the Lin-Yiluo village is in the Manzhuang official village.
1.2 test materials: a fertilizer effect test was conducted on a common compound fertilizer (except that no essential oil was added, the other preparation methods were the same as in example 1), comparative example 6 (except that the added essential oil was laurel essential oil prepared in example 5, the other preparation methods were the same as in example 1), comparative example 7 (except that the added essential oil was tea tree essential oil prepared in example 6, the other preparation methods were the same as in example 1), comparative example 8 (except that the added essential oil was compound essential oil prepared in example 7, the other preparation methods were the same as in example 1), and each 160kg of the compound fertilizer of example 1; the rice is Yu-Zhi-5, 25 kg.
The experiment is consistent in other management except for different experimental treatments.
1.3 experimental design: the same field as the first crop of 10 mu is selected, and divided into 5 groups and 2 groups. Ordinary compound fertilizers (except that no essential oil is added, the other preparation methods are the same as those in example 1), comparison 6 (except that the added essential oil is the laurel essential oil prepared in example 5, the other preparation methods are the same as those in example 1), comparison 7 (except that the added essential oil is the tea tree essential oil prepared in example 6, the other preparation methods are the same as those in example 1), comparison 8 (except that the added essential oil is the compound essential oil prepared in example 7, the other preparation methods are the same as those in example 1) and example 1 are respectively applied to plowed soil, 40kg of treatment fertilizers are applied to each mu on average, mechanical sowing is adopted, 5kg of rice seeds are sowed to each mu, the width of the fenugreek leaves of the rice, the content of chlorophyll a and b and the yield after harvesting are measured.
The experiment is consistent in other management except that the fertilizer is adopted for different treatments.
2 results and analysis
The average sword leaf width and chlorophyll a and b contents of rice are shown in Table 1
TABLE 1 average Sword leaf Width of Rice, chlorophyll a, b content
| Ordinary fertilizer | Example 1 | Comparative example 6 | Comparative example 7 | Comparative example 8 | |
| Average blade width (cm) of sword leaf | 2.05 | 2.16 | 2.12 | 2.13 | 2.14 |
| Average chlorophyll a content (mg/g) | 0.38 | 0.50 | 0.47 | 0.47 | 0.49 |
| Average chlorophyll b content (mg/g) | 0.13 | 0.14 | 0.14 | 0.13 | 0.14 |
| Chlorophyll a content/chlorophyll b content | 2.92 | 3.57 | 3.36 | 3.62 | 3.5 |
It can be seen from table 1 that under the same conditions, the present invention can significantly increase the width of rice leaves, increase the chlorophyll a content and the ratio of chlorophyll a content/chlorophyll b content, and increase rice photosynthesis.
The rice yields are shown in Table 2
TABLE 2 Rice yield in each treatment
| Yield 1 (kg) | Yield 2 (kg) | Average yield (kg) | Yield increase (%) | |
| Ordinary fertilizer | 441.5 | 444.8 | 443.15 | |
| Example 1 | 483.6 | 479.4 | 481.5 | 8.65 |
| Comparative example 6 | 458.3 | 460.5 | 459.4 | 3.67 |
| Comparative example 7 | 463.4 | 459.8 | 461.6 | 4.16 |
| Comparative example 8 | 476.5 | 479.4 | 477.95 | 7.85 |
It can be seen from table 2 that under the same conditions, the present invention can significantly increase crop yield, with example 1 increasing up to 8.65%.
Claims (8)
1. An essential oil fertilizer, which is characterized in that: consists of fertilizer and essential oil;
adding the essential oil into the fertilizer and uniformly mixing to obtain an essential oil fertilizer;
the essential oil is prepared according to the following steps:
carrying out enzymolysis on essential oil plants by lysozyme, carrying out enzyme deactivation, extracting by liquid carbon dioxide after enzyme deactivation, and separating to obtain essential oil, wherein the separated residue is the residue containing the essential oil;
the essential oil plant is one or more than two of fresh lavender, fresh laurel and fresh tea tree in any proportion;
the essential oil plant is a fresh essential oil plant;
the temperature of the liquid carbon dioxide is 25-30 ℃, the pressure is 8-10 Mpa, the flow rate is 25-35L/h, and the extraction time is 0.5-2 h;
the mass ratio of the fertilizer to the essential oil is 50-99.99: 0.01-50;
the lysozyme enzymolysis further comprises water, wherein the mass ratio of the fresh essential oil plants to the lysozyme to the water is 10-50: 0.02-1: 50-90; the enzymolysis temperature is 27-55 ℃, and the enzymolysis time is 30-60 min.
2. The essential oil fertilizer as claimed in claim 1, wherein the mass ratio of the fertilizer to the essential oil is 50-99.99: 0.01-50;
the fertilizer comprises one or more than two of simple substance fertilizer, compound fertilizer, bulk blend fertilizer, organic-inorganic fertilizer, biological organic fertilizer, organic fertilizer and water-soluble fertilizer in any proportion;
the essential oil is one or more than two of essential oil stock solution, compound essential oil and essential oil-containing diluent in any proportion.
3. The preparation method of the essential oil fertilizer is characterized by comprising the following steps of: adding the essential oil into the fertilizer and uniformly mixing to obtain an essential oil fertilizer;
the essential oil is prepared according to the following steps:
carrying out enzymolysis on essential oil plants by lysozyme, carrying out enzyme deactivation, extracting by liquid carbon dioxide after enzyme deactivation, and separating to obtain essential oil, wherein the separated residue is the residue containing the essential oil;
the essential oil plant is one or more than two of fresh lavender, fresh laurel and fresh tea tree in any proportion;
the essential oil plant is a fresh essential oil plant;
the temperature of the liquid carbon dioxide is 25-30 ℃, the pressure is 8-10 Mpa, the flow rate is 25-35L/h, and the extraction time is 0.5-2 h;
the mass ratio of the fertilizer to the essential oil is 50-99.99: 0.01-50;
the lysozyme enzymolysis further comprises water, wherein the mass ratio of the fresh essential oil plants to the lysozyme to the water is 10-50: 0.02-1: 50-90; the enzymolysis temperature is 27-55 ℃, and the enzymolysis time is 30-60 min.
4. The method for producing an essential oil fertilizer as claimed in claim 3, wherein the essential oil plant is a fresh essential oil plant,
the fresh essential oil plant is one or two of essential oil plants which are just picked and essential oil plants which are stored in an environment of-20 to-5 ℃ just after being picked in any proportion.
5. The method for producing an essential oil fertilizer as set forth in claim 3, characterized in that: the enzyme deactivation temperature is 80-120 ℃, the enzyme deactivation time is 5-20 min, and the enzyme deactivation pressure is 0-5 MPa.
6. The method for producing an essential oil fertilizer as set forth in claim 3, characterized in that: the method also comprises the step of adding a retention agent into the essential oil, wherein the mass ratio of the essential oil to the retention agent is 50-99.5: 0.5-50;
the retention agent is one or more than two of ethylene glycol, glycerol and isopropanol in any proportion.
7. The method for producing an essential oil fertilizer as set forth in claim 3, characterized in that: the separation comprises primary separation kettle separation and secondary separation kettle separation, wherein the separation pressure of the primary separation kettle is 6-8 MPa, the separation temperature is 30-50 ℃, and the separation time is 0.5-3 h; the separation pressure of the secondary separation kettle is 4-6 MPa, the separation temperature is 25-40 ℃, and the separation time is 0.5-3 h; residue is left at the bottom after the first-stage separation kettle is separated to form a mixture.
8. The method for producing an essential oil fertilizer as claimed in claim 7, characterized in that: transferring the mixture to an oil-water separator, adding a flocculating agent into the mixture, standing for 20-150 min, wherein the mass ratio of the mixture to the flocculating agent is 99-99.99: 0.01-1, and performing oil-water separation at 30-50 ℃ to obtain lavender wax and a water treatment substance; filtering the water-treated product to obtain water and residue containing essential oil;
the flocculating agent is one or more than two of activated clay, polyaluminium chloride, sodium polyacrylate and polyacrylamide in any proportion.
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