CN112369433A - Water-soluble bactericide and preparation method and application thereof - Google Patents
Water-soluble bactericide and preparation method and application thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N63/00—Biocides, pest repellants or attractants, or plant growth regulators containing microorganisms, viruses, microbial fungi, animals or substances produced by, or obtained from, microorganisms, viruses, microbial fungi or animals, e.g. enzymes or fermentates
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N61/00—Biocides, pest repellants or attractants, or plant growth regulators containing substances of unknown or undetermined composition, e.g. substances characterised only by the mode of action
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N65/00—Biocides, 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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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N65/00—Biocides, 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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Abstract
The invention provides a preparation method and an application method of a water-soluble bactericide, wherein the water-soluble bactericide takes a water-phase product obtained by hydrothermal reaction prepared from biomass as a raw material, and has high-efficiency inhibiting and killing effects on various harmful bacteria. In addition, the water-soluble bactericide has the advantages of wide raw materials, simple and convenient operation of the preparation method, rapidness and low cost, and is suitable for large-scale production and application.
Description
Technical Field
The present invention relates to the field of agriculture and the breeding industry. In particular, the invention relates to a water-soluble bactericide, a preparation method and application thereof.
Background
With the increasing global population and the increasing demand for food, agricultural problems, especially food safety problems, are receiving more and more attention. Pathogenic bacteria and fungi seriously affect the yield of grains and the growth of plants, and pose great threat to the grain safety of China. China is a big agricultural country, has a large population and has huge demand for food. Currently, neither the quantity nor the type of fungicide can meet the actual needs of agricultural production. For the livestock industry, pathogenic bacteria and fungi present in the farm can also affect the normal growth and fertility of livestock, etc. However, currently, the types and amounts of bactericides suitable for use in farms are small and yet to be developed.
A large amount of biological organic matters such as livestock and poultry manure, straws, microalgae, kitchen waste, sludge, water bloom, water hyacinth and the like exist in China, and the method has important significance for recycling the biological organic matters. At present, no research reports that a hydrothermal reaction product of biomass has a bactericidal effect, and the product has a high commercial value when being used as a bactericide in agricultural production and breeding industry.
Disclosure of Invention
The present invention aims to solve at least to some extent at least one of the technical problems of the prior art. Therefore, the invention provides a water-soluble bactericide, a method for preparing the water-soluble bactericide, a sterilization method and application of an aqueous phase product obtained by carrying out hydrothermal reaction on biomass in sterilization. The water-soluble bactericide takes a water-phase product obtained by the hydrothermal reaction of biomass as a raw material, and has high-efficiency inhibiting and killing effects on various harmful bacteria. In addition, the water-soluble bactericide has the advantages of wide raw materials, simple and convenient operation of the preparation method, rapidness and low cost, and is suitable for large-scale production and application.
In one aspect of the invention, a water-soluble biocide is provided. According to an embodiment of the present invention, the water-soluble bactericide includes: carrying out hydrothermal reaction on the biomass to obtain an aqueous phase product. The inventor finds that a water phase product obtained by carrying out hydrothermal reaction on biomass has high-efficiency inhibiting and killing effects on various harmful bacteria, and can be applied to agricultural production and breeding industry.
According to an embodiment of the present invention, the water-soluble bactericide may further have the following additional technical features:
according to an embodiment of the invention, the aqueous phase product comprises at least one of: bases, terpenes, ketones, glycosides, esters, phenols, aldehydes, organic acids, pyridines and organometallics. The water phase product with the composition has a good sterilization effect.
According to an embodiment of the present invention, the raw material of the biomass includes, but is not limited to, one or more of human excrement, livestock and poultry manure, straw, pulp processing wastewater, sludge, water bloom, kitchen waste, water hyacinth, and microalgae.
According to an embodiment of the invention, the aqueous phase product is obtained by: sealing the biomass and optional catalyst in a reaction kettle, adjusting the initial pressure to be 0-1 MPa, heating to 120-400 ℃, and keeping the temperature for 0-48 hours (for example, 10 minutes-10 hours) to obtain a reaction material, and collecting a water phase to obtain the water phase product.
In a reaction kettle, biomass is subjected to hydrothermal reaction to obtain an oil phase, a water phase and residues. In the reaction process, a catalyst (for example, 0-60 wt% of Fe, Pt, Ru, Ni, Mo, etc.) may be added appropriately to further promote the reaction and improve the yield of the aqueous phase product. The hydrothermal reaction can be fully performed by adopting the heating temperature, the heating time and the heating pressure, the yield of the obtained water-phase product is high, and the water-phase product has a better sterilization effect. Further, the aqueous phase may be directly sucked or poured, or the aqueous phase may be collected by removing the oil phase and the residue by extraction (for example, with an organic solvent) and filtration. Thus, the resulting aqueous product contains at least one of: alkalies, terpenes, ketones, glycosides, esters, phenols, aldehydes, organic acids, pyridine and organic metals, and has good bactericidal effect.
According to an embodiment of the present invention, the water-soluble bactericide further includes: an adjuvant including, but not limited to, at least one of: wetting agents, penetrants, stabilizers, dispersants, and thickeners.
According to an embodiment of the present invention, the wetting agent and the penetrating agent include, but are not limited to, at least one of fatty alcohol ether, silicone polyether, alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, alkylphenol polyoxyethylene ether phosphate, phenethylphenol polyoxyethylene ether phosphate, alkyl naphthalene sulfonate, sodium laureth sulfate, disodium alkylphenol polyoxyethylene sulfosuccinate, sodium butylnaphthalene sulfonate, condensate of fatty alcohol and ethylene oxide, glycerin, dimethyl sulfoxide, tween, sulfated castor oil, sodium alkylsulfonate, sodium alkylbenzenesulfonate, and sodium alkylsulfate. The adhesion and permeation effects of the liquid preparation on the surface of the body are increased by adding the wetting agent and the penetrating agent.
According to an embodiment of the present invention, the stabilizer includes, but is not limited to, at least one of propyl gallate, alcohol compounds, dibutyl hydroxy toluene, butyl hydroxy anisole and tert-butyl p-diphenol. Therefore, the stability of the system is improved, the oxidation resistance of the effective components is ensured, and the uniform system is maintained.
According to an embodiment of the present invention, the dispersant includes, but is not limited to, at least one of alkyl sulfonate, alkyl benzene sulfonate, polycarboxylate, lignosulfonate, polycarboxylate, alkyl sulfosuccinate, dioctyl sodium sulfosuccinate, alkyl naphthalene sulfonic acid polycondensate sodium salt, and aryl phenol polyoxyethylene ether. Thereby, the components are uniformly dispersed to form a uniform system.
According to an embodiment of the present invention, the thickener includes, but is not limited to, at least one of xanthan gum, sodium methyl ester sulfonate of fatty alcohol, carboxymethyl cellulose, polyvinyl alcohol, white carbon, organic bentonite, and magnesium aluminum silicate. Thereby, the viscosity of the system is increased.
According to the embodiment of the invention, the addition amount of the auxiliary agent is 10 based on the total mass of the water-soluble bactericide-1-10-10(e.g. 10) by mass-1-10-4Mass%). Therefore, the water-soluble bactericide has a good sterilization effect and high stability, can be stored at 0-30 ℃ in the dark for 10-360 days, and has a lasting period of 3 after applicationAbout 20 days.
In another aspect of the invention, a method of preparing a water-soluble biocide is provided. According to an embodiment of the invention, the method comprises: mixing the water phase product obtained by the hydrothermal reaction of the biomass with the auxiliary agent. Therefore, the water-soluble bactericide obtained by the method provided by the embodiment of the invention has a good bactericidal effect, is easy to obtain raw materials, simple and convenient to operate, quick, low in cost and suitable for large-scale production and application.
According to an embodiment of the present invention, the water-soluble bactericide is as defined in the foregoing. It will be appreciated by those skilled in the art that the features and advantages previously described for water-soluble biocides are equally applicable to the method of preparing water-soluble biocides and will not be described in further detail herein.
In yet another aspect of the present invention, a method of sterilization is provided. According to an embodiment of the invention, the method comprises: the water-soluble bactericide as described above is applied to the object to be treated. As described above, the water-soluble bactericide according to the embodiment of the present invention has a good bactericidal effect, and therefore, it is applied (e.g., sprayed, soaked, etc.) to an object to be treated to function. Specifically, the water-soluble bactericide may be diluted as a mother liquor before application, for example, by 1 to 10 degrees, depending on the actual disease degree5Spraying by a double-spraying method, and uniformly soaking on the surface of crops; can also be diluted by 1-105Soaking seeds for 1-300 minutes; can also dilute by 1-108The fertilizer is applied by irrigating soil.
According to an embodiment of the present invention, the object to be treated includes, but is not limited to, at least one of the following: field crops, vegetable crops, fruits, ornamental crops and farm environments. Thereby, the harmful bacteria on the substance can be effectively killed.
According to embodiments of the invention, the field crop includes, but is not limited to, at least one of: corn, wheat and tobacco; the vegetable crops include, but are not limited to, at least one of the following: tomatoes, cucumbers, cabbages and peppers; the fruit includes, but is not limited to, at least one of the following: apples, pears and grapes; the ornamental crops include, but are not limited to, at least one of the following: rose, peony and peony. Thereby, the harmful bacteria on the surface of the plant can be effectively killed.
According to an embodiment of the invention, the farm environment includes, but is not limited to, at least one of: equipment, site, feeding materials and waste. Therefore, pathogenic bacteria on all substances except the bodies of the livestock in the farm can be effectively killed.
In a further aspect of the invention, the invention proposes the use of an aqueous phase product obtained by hydrothermal reaction of biomass for sterilization. The water phase product has better sterilization effect, is easy to obtain and has better application prospect.
According to an embodiment of the invention, the aqueous phase product is provided in the form of the water-soluble biocide described above. Since the water-soluble bactericide as described above contains an aqueous product, the aqueous product can be provided from the water-soluble bactericide.
According to an embodiment of the invention, the bacteria include, but are not limited to, at least one of the following: cercospora keratolytica, Rhizoctonia solani, Fusarium graminearum, Verticillium dahliae and mosaic virus. The water phase product obtained by the biomass hydrothermal reaction has better inhibition effect on the thalli.
According to an embodiment of the invention, the aqueous phase product is used for preventing or treating downy mildew, ring spot, anthracnose, ulcer disease, wildfire disease, scab, soft rot, black rot and/or bacterial wilt of plant infection.
According to an embodiment of the invention, the aqueous phase product is used for killing staphylococcus aureus, escherichia coli, streptococcus and/or klebsiella in livestock and poultry farms, preventing or treating foot-and-mouth disease, infectious rhinotracheitis, recessive mastitis and/or parasitic diseases.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 shows a GC-MS mass spectrum of an aqueous phase product from hydrothermal reaction of biomass according to one embodiment of the present invention.
Detailed Description
The scheme of the invention will be explained with reference to the examples. It will be appreciated by those skilled in the art that the following examples are illustrative of the invention only and should not be taken as limiting the scope of the invention. The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1
(1) Weighing a certain amount of livestock and poultry manure, and adding the livestock and poultry manure into a high-temperature high-pressure reaction kettle. Nitrogen was introduced and the initial pressure was adjusted to 0.5 MPa. The raw material was heated to 320 ℃ and the residence time was 20 min. Stopping heating the reaction kettle, opening the reaction kettle gas releasing device when the temperature is reduced to the room temperature until the pressure in the reaction kettle is reduced to the atmospheric pressure, and opening the reaction kettle. The water and oily substance were separated using a separatory funnel. The aqueous phase and the residue were separated by a filtration apparatus to obtain an aqueous phase.
GC-MS detection is carried out on the water phase, the obtained mass spectrogram is shown in figure 1, and the water phase is analyzed to find that the water phase contains alkalis, terpenes, ketones, glycosides, esters, phenols, aldehydes, organic acids, pyridine and organic metals.
(2) Adding fatty alcohol ether as wetting agent and penetrant, adding methanol as stabilizer at a ratio of 10-3％。
(3) The composition is diluted by 1000 times by adding water, is uniformly sprayed on diseased wheat, has the killing effect on fusarium graminearum of more than 70 percent, can be stored for 360 days in a dark place at 0-30 ℃, and has the lasting period of 15 days.
Example 2
(1) Weighing a proper amount of fresh algal bloom (the solid content is 12 percent), and adding the fresh algal bloom into a high-temperature high-pressure reaction kettle. Nitrogen was introduced and the initial pressure was adjusted to 0.5 MPa. The raw materials were heated to 200 ℃ and the residence time was 360 min. Stopping heating the reaction kettle, opening the reaction kettle gas releasing device when the temperature is reduced to the room temperature until the pressure in the reaction kettle is reduced to the atmospheric pressure, and opening the reaction kettle. The aqueous phase and the solid residue were separated by a filtration apparatus to obtain an aqueous phase. The water phase contains alkalis, terpenoids, ketones, glycosides, esters, phenols, aldehydes, organic acids, pyridine and organic metals.
(2) Adding fatty alcohol ether as wetting agent and penetrant, adding methanol as stabilizer at a ratio of 10-2％。
(3) Diluting 1000 times with water, irrigating Chinese cabbage vegetable field, and keeping away from light at 0-30 deg.C for 360 days with a lasting period of 15 days, wherein the effect of killing soft rot bacteria is above 70%.
Example 3
(1) Weighing a proper amount of fresh sludge (the solid content is 40 percent), and adding the fresh sludge into a high-temperature high-pressure reaction kettle. Nitrogen was introduced and the initial pressure was adjusted to 0.5 MPa. The raw materials were heated to 250 ℃ and the residence time was 480 min. Stopping heating the reaction kettle, opening the condensed water of the reaction kettle to cool the reaction kettle, opening the air bleeder of the reaction kettle when the temperature is reduced to the room temperature until the air pressure in the reaction kettle is reduced to the atmospheric pressure, and opening the reaction kettle. The aqueous phase and the solid residue were separated by a filtration apparatus to obtain an aqueous phase. The water phase contains alkalis, terpenoids, ketones, glycosides, esters, phenols, aldehydes, organic acids, pyridine and organic metals.
(2) Adding fatty alcohol ether as wetting agent and penetrant, adding methanol as stabilizer at a ratio of 10-3％。
(3) Adding water to dilute 100 times, soaking seeds for 10min, wherein the killing effect on ralstonia solanacearum reaches more than 70%, the ralstonia solanacearum can be stored for 360 days at 0-30 ℃ in the dark, and the lasting period is 15 days.
Example 4
(1) Weighing a proper amount of human excrement (the solid content is 15 percent) and adding the human excrement into a high-temperature high-pressure reaction kettle. Nitrogen was introduced and the initial pressure was adjusted to 0.5 MPa. The raw material was heated to 340 ℃ and the residence time was 30 min. Stopping heating the reaction kettle, opening the reaction kettle gas releasing device when the temperature is reduced to the room temperature until the pressure in the reaction kettle is reduced to the atmospheric pressure, and opening the reaction kettle. The water and oily material were separated using a separatory funnel and acetone. The aqueous phase and the residue were separated by a filtration apparatus to obtain an aqueous phase. The water phase contains alkalis, terpenoids, ketones, glycosides, esters, phenols, aldehydes, organic acids, pyridine and organic metals.
(2) Adding fatty alcohol ether as wetting agent and penetrant, adding methanol as stabilizer at a ratio of 10-3％。
(3) The water is added for dilution by 1000 times, and the apple tree is sprayed, the effect of killing anthracnose germs reaches more than 70 percent, the apple tree can be stored for 360 days at 0-30 ℃ in the dark, and the lasting period is 15 days.
Example 5
(1) Weighing a certain amount of livestock and poultry manure, and adding the livestock and poultry manure into a high-temperature high-pressure reaction kettle. Nitrogen was introduced and the initial pressure was adjusted to 0.5 MPa. The raw material was heated to 320 ℃ and the residence time was 20 min. Stopping heating the reaction kettle, opening the reaction kettle gas releasing device when the temperature is reduced to the room temperature until the pressure in the reaction kettle is reduced to the atmospheric pressure, and opening the reaction kettle. The water and oily substance were separated using a separatory funnel. The aqueous phase and the residue were separated by a filtration apparatus to obtain an aqueous phase.
GC-MS detection is carried out on the water phase, the obtained mass spectrogram is shown in figure 1, and the water phase is analyzed to find that the water phase contains alkalis, terpenes, ketones, glycosides, esters, phenols, aldehydes, organic acids, pyridine and organic metals.
(2) Diluting the water phase product by 10 times, performing a spraying test in a pig farm, and sampling and counting by a microscope after spraying for 6 hours. Test results show that the killing rate of the bactericide to staphylococcus aureus reaches more than 80 percent; the killing rate to colibacillus can reach above 70%.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. A water-soluble biocide, comprising: carrying out hydrothermal reaction on the biomass to obtain an aqueous phase product.
2. The water-soluble bactericide as claimed in claim 1, wherein said aqueous product contains at least one of:
bases, terpenes, ketones, glycosides, esters, phenols, aldehydes, organic acids, pyridines and organometallics;
optionally, the raw material of the biomass includes, but is not limited to, one or more of human feces, livestock and poultry manure, straw, pulp processing wastewater, sludge, water bloom, kitchen waste, water hyacinth, and microalgae.
3. The water-soluble bactericide as claimed in claim 1, wherein said aqueous product is obtained by:
sealing the biomass and optional catalyst in a reaction kettle, adjusting the initial pressure to be 0-1 MPa, heating to 120-400 ℃, and keeping the time for 0-48 hours to obtain a reaction material, and collecting a water phase to obtain the water phase product.
4. The water-soluble bactericide as claimed in claim 1, further comprising: an adjuvant including, but not limited to, at least one of: wetting agents, penetrants, stabilizers, dispersants, and thickeners;
optionally, the wetting and penetrating agents include, but are not limited to, at least one of fatty alcohol ethers, silicone polyethers, alkylphenol polyoxyethylene ether formaldehyde condensate sulfates, alkylphenol polyoxyethylene ether phosphates, phenethylphenol polyoxyethylene ether phosphates, alkylnaphthalene sulfonates, sodium laureth sulfate, disodium alkylphenol polyoxyethylene sulfosuccinates, sodium butylnaphthalene sulfonate, condensates of fatty alcohols with ethylene oxide, glycerol, dimethyl sulfoxide, tweens, sulfated castor oil, sodium alkylsulfonates, sodium alkylbenzenesulfonates, and sodium alkylsulfates;
the stabilizer includes, but is not limited to, at least one of propyl gallate, alcohol compounds, dibutyl hydroxy toluene, butyl hydroxy anisole and tert-butyl p-diphenol;
the dispersant includes, but is not limited to, at least one of alkyl sulfonate, alkyl benzene sulfonate, polycarboxylate, lignosulfonate, polycarboxylate, alkyl sulfosuccinate, dioctyl sodium sulfosuccinate, alkyl naphthalene sulfonic acid polycondensate sodium salt, and aryl phenol polyoxyethylene ether;
the thickener includes, but is not limited to, at least one of xanthan gum, sodium methyl fatty alcohol sulfonate, carboxymethyl cellulose, polyvinyl alcohol, white carbon black, organic bentonite and magnesium aluminum silicate;
optionally, the addition amount of the auxiliary agent is 10 based on the total mass of the water-soluble bactericide-1-10-10Mass percent;
optionally, the water-soluble bactericide can be stored at 0-30 ℃ in the dark for 10-360 days, and the lasting period after application is 3-20 days.
5. A method of preparing a water-soluble biocide, comprising: mixing the water phase product obtained by the hydrothermal reaction of the biomass with the auxiliary agent.
6. The method according to claim 5, wherein the water-soluble bactericide is as defined in any one of claims 1 to 4.
7. A method of sterilization, comprising:
a water-soluble bactericide as claimed in any one of claims 1 to 4, which is applied to an object to be treated.
8. The method of claim 7, wherein the treatment includes, but is not limited to, at least one of: field crops, vegetable crops, fruits, ornamental crops and farm environments;
optionally, the field crop includes, but is not limited to, at least one of: corn, wheat and tobacco;
the vegetable crops include, but are not limited to, at least one of the following: tomatoes, cucumbers, cabbages and peppers;
the fruit includes, but is not limited to, at least one of the following: apples, pears and grapes;
the ornamental crops include, but are not limited to, at least one of the following: rose, peony and peony;
the farm environment includes, but is not limited to, at least one of: equipment, site, feeding materials and waste.
9. Use of an aqueous phase product obtained by hydrothermal reaction of biomass for sterilization.
10. Use according to claim 9, wherein the aqueous phase product is provided in the form of a water-soluble bactericide according to any one of claims 1 to 4;
optionally, the bacteria include, but are not limited to, at least one of the following: keratomyces, rhizoctonia solani, fusarium graminearum, verticillium dahliae, and mosaic virus;
optionally, the aqueous phase product is used for preventing or treating downy mildew, ring spot, anthracnose, ulcer, wildfire, scab, soft rot, black rot and/or bacterial wilt of plant infection;
optionally, the water phase product is used for killing staphylococcus aureus, escherichia coli, streptococcus and/or klebsiella in livestock and poultry farms, and preventing or treating foot-and-mouth disease, infectious rhinotracheitis, recessive mastitis and/or parasitic diseases.
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