CN115517259B - Saponin-type pond cleaning agent and preparation method and application thereof - Google Patents
Saponin-type pond cleaning agent and preparation method and application thereof Download PDFInfo
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- CN115517259B CN115517259B CN202211147361.XA CN202211147361A CN115517259B CN 115517259 B CN115517259 B CN 115517259B CN 202211147361 A CN202211147361 A CN 202211147361A CN 115517259 B CN115517259 B CN 115517259B
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- saponin
- cleaning agent
- pond cleaning
- tea
- aqueous solution
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- 239000012459 cleaning agent Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 80
- 239000001397 quillaja saponaria molina bark Substances 0.000 claims abstract description 74
- 229930182490 saponin Natural products 0.000 claims abstract description 74
- 150000007949 saponins Chemical class 0.000 claims abstract description 74
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 40
- 241001122767 Theaceae Species 0.000 claims abstract description 38
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229930192760 sasanquasaponin Natural products 0.000 claims abstract description 14
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 13
- 235000018597 common camellia Nutrition 0.000 claims abstract description 9
- 239000010495 camellia oil Substances 0.000 claims abstract description 8
- 229940079593 drug Drugs 0.000 claims abstract description 6
- 239000003814 drug Substances 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims description 18
- 239000002105 nanoparticle Substances 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 14
- 239000002244 precipitate Substances 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- 239000003921 oil Substances 0.000 claims description 11
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 9
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims description 9
- ABBQHOQBGMUPJH-UHFFFAOYSA-M Sodium salicylate Chemical compound [Na+].OC1=CC=CC=C1C([O-])=O ABBQHOQBGMUPJH-UHFFFAOYSA-M 0.000 claims description 9
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 9
- ZAZSDMULJMWXBK-UHFFFAOYSA-N ethane triethoxysilane Chemical compound CC.C(C)O[SiH](OCC)OCC ZAZSDMULJMWXBK-UHFFFAOYSA-N 0.000 claims description 9
- 229960004025 sodium salicylate Drugs 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 7
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 4
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 3
- 241000209507 Camellia Species 0.000 claims 3
- 239000000463 material Substances 0.000 claims 1
- 241000238557 Decapoda Species 0.000 abstract description 20
- 241000251468 Actinopterygii Species 0.000 abstract description 15
- 244000052616 bacterial pathogen Species 0.000 abstract description 8
- 240000001548 Camellia japonica Species 0.000 abstract description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 abstract description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 6
- 239000001301 oxygen Substances 0.000 abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000005286 illumination Methods 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 3
- 230000003000 nontoxic effect Effects 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000002199 base oil Substances 0.000 abstract 1
- 230000002147 killing effect Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 244000000010 microbial pathogen Species 0.000 description 5
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 4
- 238000012851 eutrophication Methods 0.000 description 4
- 239000003446 ligand Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 241000607534 Aeromonas Species 0.000 description 3
- 241000607598 Vibrio Species 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- WQLVFSAGQJTQCK-UHFFFAOYSA-N diosgenin Natural products CC1C(C2(CCC3C4(C)CCC(O)CC4=CCC3C2C2)C)C2OC11CCC(C)CO1 WQLVFSAGQJTQCK-UHFFFAOYSA-N 0.000 description 3
- 125000003147 glycosyl group Chemical group 0.000 description 3
- 238000002329 infrared spectrum Methods 0.000 description 3
- 150000007524 organic acids Chemical class 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- NWMIYTWHUDFRPL-UHFFFAOYSA-N sapogenin Natural products COC(=O)C1(CO)C(O)CCC2(C)C1CCC3(C)C2CC=C4C5C(C)(O)C(C)CCC5(CCC34C)C(=O)O NWMIYTWHUDFRPL-UHFFFAOYSA-N 0.000 description 3
- 230000001954 sterilising effect Effects 0.000 description 3
- 238000004659 sterilization and disinfection Methods 0.000 description 3
- 231100000419 toxicity Toxicity 0.000 description 3
- 230000001988 toxicity Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 241000252230 Ctenopharyngodon idella Species 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- 235000012255 calcium oxide Nutrition 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000001965 increasing effect Effects 0.000 description 2
- 208000015181 infectious disease Diseases 0.000 description 2
- 235000012054 meals Nutrition 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 231100000956 nontoxicity Toxicity 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 1
- YRIZYWQGELRKNT-UHFFFAOYSA-N 1,3,5-trichloro-1,3,5-triazinane-2,4,6-trione Chemical compound ClN1C(=O)N(Cl)C(=O)N(Cl)C1=O YRIZYWQGELRKNT-UHFFFAOYSA-N 0.000 description 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 1
- ZKQDCIXGCQPQNV-UHFFFAOYSA-N Calcium hypochlorite Chemical compound [Ca+2].Cl[O-].Cl[O-] ZKQDCIXGCQPQNV-UHFFFAOYSA-N 0.000 description 1
- 239000005892 Deltamethrin Substances 0.000 description 1
- 241000251511 Holothuroidea Species 0.000 description 1
- VQXSOUPNOZTNAI-UHFFFAOYSA-N Pyrethrin I Natural products CC(=CC1CC1C(=O)OC2CC(=O)C(=C2C)CC=C/C=C)C VQXSOUPNOZTNAI-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- IOYNQIMAUDJVEI-BMVIKAAMSA-N Tepraloxydim Chemical compound C1C(=O)C(C(=N/OC\C=C\Cl)/CC)=C(O)CC1C1CCOCC1 IOYNQIMAUDJVEI-BMVIKAAMSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 125000003172 aldehyde group Chemical group 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 229960002483 decamethrin Drugs 0.000 description 1
- OWZREIFADZCYQD-NSHGMRRFSA-N deltamethrin Chemical compound CC1(C)[C@@H](C=C(Br)Br)[C@H]1C(=O)O[C@H](C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 OWZREIFADZCYQD-NSHGMRRFSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000010813 municipal solid waste Substances 0.000 description 1
- RJMUSRYZPJIFPJ-UHFFFAOYSA-N niclosamide Chemical compound OC1=CC=C(Cl)C=C1C(=O)NC1=CC=C([N+]([O-])=O)C=C1Cl RJMUSRYZPJIFPJ-UHFFFAOYSA-N 0.000 description 1
- 229960001920 niclosamide Drugs 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- HYJYGLGUBUDSLJ-UHFFFAOYSA-N pyrethrin Natural products CCC(=O)OC1CC(=C)C2CC3OC3(C)C2C2OC(=O)C(=C)C12 HYJYGLGUBUDSLJ-UHFFFAOYSA-N 0.000 description 1
- VJFUPGQZSXIULQ-XIGJTORUSA-N pyrethrin II Chemical compound CC1(C)[C@H](/C=C(\C)C(=O)OC)[C@H]1C(=O)O[C@@H]1C(C)=C(C\C=C/C=C)C(=O)C1 VJFUPGQZSXIULQ-XIGJTORUSA-N 0.000 description 1
- 239000002516 radical scavenger Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229940080817 rotenone Drugs 0.000 description 1
- JUVIOZPCNVVQFO-UHFFFAOYSA-N rotenone Natural products O1C2=C3CC(C(C)=C)OC3=CC=C2C(=O)C2C1COC1=C2C=C(OC)C(OC)=C1 JUVIOZPCNVVQFO-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 229950009390 symclosene Drugs 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- 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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/02—Biocides, 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
- A01N43/04—Biocides, 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
- A01N43/14—Biocides, 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
- A01N43/16—Biocides, 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
-
- 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
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P15/00—Biocides for specific purposes not provided for in groups A01P1/00 - A01P13/00
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/04—Disinfection
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/023—Reactive oxygen species, singlet oxygen, OH radical
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/80—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in fisheries management
- Y02A40/81—Aquaculture, e.g. of fish
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Environmental Sciences (AREA)
- Zoology (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- General Health & Medical Sciences (AREA)
- Wood Science & Technology (AREA)
- Chemical & Material Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Toxicology (AREA)
- Dentistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Saccharide Compounds (AREA)
- Detergent Compositions (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to the technical field of fish medicines, in particular to a saponin type pond cleaning agent and a preparation method thereof. The saponin type pond cleaning agent is a nano preparation taking dendritic mesoporous silicon dioxide as a carrier and tea-oil camellia saponin and carbon nitride complex as medicines. The tea saponin pond cleaning agent has low production cost, has good stability and dispersibility in water, can release tea saponin under the illumination condition, and simultaneously catalyzes oxygen to generate oxygen free radicals and hydrogen peroxide to efficiently kill pathogenic bacteria, thereby being beneficial to the growth of shrimps and crabs; the preparation method is simple in preparation process and low in production cost, and the prepared sasanquasaponin pond cleaning agent is environment-friendly, safe, nontoxic, convenient to use and high in popularization.
Description
Technical Field
The invention relates to the technical field of fish medicines, in particular to a saponin type pond cleaning agent and a preparation method and application thereof.
Background
The shrimp and crab are subjected to pond cleaning treatment before or after a cultivation period, so that the purpose is to eliminate wild fish, and the problems of organization, reduction, acidification and poisoning of the pond are solved, so that the normal growth and safety of the shrimp and crab are protected. The quick lime, tea meal, bleaching powder, pyrethrin, niclosamide and other medicines are often selected for disinfection, but excessive use of the quick lime easily causes too high pH of water, excessive alkalization of the pond bottom, influences the growth of shrimps, crabs and sea cucumbers, has too short or residual action time of other chemical reagents, has poor sterilization effect, and does not have the effect of improving the pond environment. The tea seed cake can effectively kill the miscellaneous fishes, is favorable for the growth of plankton in the pond, and is favorable for the cultivation of the shrimps and crabs, but the tea seed cake is residues after oil extraction of camellia seeds, has complex composition, can promote eutrophication of the pond by using, and causes the propagation of pathogenic microorganisms, thereby causing the death caused by pathogenic bacteria infection of the shrimps and crabs.
The Chinese patent publication No. CN1977618 discloses a method for preparing tea saponin pond cleaning agent by taking tea seed cake as raw material, mixing and drying tea seed cake extract, soluble starch, salt and calcium hydroxide to prepare the tea saponin pond cleaning agent; the Chinese patent with publication No. CN114097789A discloses a method for preparing a compound tea saponin pond cleaning agent by taking tea seed cake as a raw material, and the compound tea saponin pond cleaning agent is prepared by mixing and drying tea seed cake water extract, rotenone, trichloroisocyanuric acid and deltamethrin. The tea seed meal is extracted to extract tea saponin, so that the content of the tea saponin serving as an effective component is increased, and a good effect of killing the trash fish is obtained, but the killing effect of microorganisms in the water body is not effectively studied, and the death of shrimps and crabs caused by the infection of pathogenic microorganisms in the water body is caused by the propagation of pathogenic microorganisms.
Disclosure of Invention
Based on the above, the invention aims to provide a novel saponin type pond cleaning agent, which solves the problem that the saponin type pond cleaning agent in the prior art cannot effectively kill pathogenic microorganisms in water body to influence the normal growth of shrimps and crabs. The invention also provides a preparation method of the saponin type pond cleaning agent, which has the advantages of simple preparation process and low production cost, and the obtained saponin type pond cleaning agent has good stability and dispersibility in water, is convenient to apply, and has the effects of killing wild fish and pathogenic microorganisms with high efficiency; is environment-friendly, safe and nontoxic, does not cause eutrophication of water body, and realizes better pond cleaning effect.
In order to solve the technical problems of the invention, the invention adopts the following technical scheme:
the first aim of the invention is to provide a saponin type pond cleaning agent, which is a nano preparation taking dendritic mesoporous silica nano particles as a carrier and taking tea-oil camellia saponin and carbon nitride coordination compound as medicines. The tea-oil saponin and the carbon nitride are coordinated to form a novel saponin type pond cleaning agent.
Further, the oil tea saponin contains more than 90% of saponin.
The second object of the invention is to provide a preparation method of a saponin pond cleaning agent, which comprises the following steps:
s1, adding triethanolamine into a sodium salicylate aqueous solution with the mass fraction of 1-3% to adjust the pH value to 6-8, slowly adding a cetyl trimethyl ammonium bromide aqueous solution with the mass fraction of 3-6%, uniformly mixing, slowly adding tetraethoxysilane and 1, 2-bis (triethoxysilane) -ethane, reacting for a certain time at room temperature, centrifuging, and collecting precipitate to obtain dendritic mesoporous silica nanoparticles;
s2, uniformly mixing the dendritic mesoporous silica nano particles obtained in the step S1 with cyanamide, and reacting for a period of time under a heating condition to obtain carbon nitride-loaded silica;
s3, dissolving the sasanqua saponin in an organic solvent to obtain a sasanqua saponin solution with the mass fraction of 5-10%, then adding the silicon dioxide loaded with carbon nitride obtained in the S2, stirring at room temperature for reacting for a period of time, centrifuging, and collecting the precipitate to obtain the saponin type pond cleaning agent.
The technical principle of the invention is as follows: the oil tea saponin consists of sapogenin, glycosyl and organic acid ligand, wherein the sapogenin structure contains aldehyde group, the glycosyl ligand and the organic acid ligand contain carboxyl; the carbonyl group can accept electrons, and the nitrogen in the carbon nitride has a lone pair of electrons, so that the two can form a coordination bond. According to the invention, the dendritic mesoporous silica nano particles are prepared, then carbon nitride is dispersed and fixed therein, and finally, the sapogenin, glycosyl and organic acid ligand of the camellia saponin are all fixed on the dendritic mesoporous silica through coordination by coordination through coordination of the camellia saponin and the carbon nitride, so that the dendritic mesoporous silica nano particles are not easy to degrade in water, and the stability of the dendritic mesoporous silica nano particles in water is maintained. Under the illumination condition, carbon nitride breaks coordination bonds due to photon absorption to release tea saponin, oxygen is catalyzed to generate oxygen free radicals and hydrogen peroxide to kill pathogenic bacteria effectively, and tea saponin can kill wild fish without causing eutrophication of water body and can stimulate shrimp and crab growth.
In the step S1, the volume ratio of the cetyltrimethylammonium bromide aqueous solution to the sodium salicylate aqueous solution is 1-3:1.
In S1, the addition amount of tetraethoxysilane and 1, 2-bis (triethoxysilane) -ethane is 2-5% of the total mass of the mixture.
In S1, the reaction time is 16-36 h, and the centrifugation condition is 3000-5000 rpm, and 20-40 min.
Further, in S2, the mass ratio of the dendritic mesoporous silica to the cyanamide is 1:0.1-0.5; the heating reaction conditions are as follows: heating to 500-600 ℃ at a heating rate of 3-6 ℃ per minute for 3-6 h.
In S3, the organic solvent is any one of n-butanol, acetone, and ethanol.
Further, in S3, the mass ratio of the silicon dioxide loaded with silicon nitride to the tea-oil camellia saponin is 5-10:1; the stirring reaction condition is 500-2000 rpm, the reaction time is 3-6 h, the centrifugation condition is 3000-5000 rpm, and the reaction time is 20-40 min.
The third object of the present invention is to provide an application of the above-mentioned saponin-type pond cleaning agent in the pond cleaning, which is characterized in that the saponin-type pond cleaning agent is diluted with water and then added in an amount of 1-5 mg/m 3 Is sprayed into the fishpond.
Compared with the prior art, the invention has the following beneficial effects:
1. the novel oil tea saponin pond cleaning agent is simple in preparation process, low in production cost, good in stability and dispersibility in water, convenient to use and high in popularization.
2. The tea saponin pond cleaning agent prepared by the invention can release tea saponin under illumination condition, and simultaneously catalyze oxygen to generate oxygen free radicals and hydrogen peroxide to efficiently kill pathogenic bacteria, while the tea saponin can kill wild fish, does not cause eutrophication of water body and can stimulate shrimp and crab growth.
3. The oil tea saponin pond cleaning agent prepared by the invention is environment-friendly, safe and nontoxic.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is an electron microscope image of the saponin pond cleaning agent of the present invention;
FIG. 2 is an infrared spectrum of the saponin-type pond cleaning agent, carbon nitride-loaded silicon dioxide, tea saponin and carbon nitride of the present invention.
Detailed Description
In order to make the purposes, technical solutions and some points of the embodiments of the present invention more clear, the technical solutions of the present invention will be clearly and completely described below with reference to the drawings and the specific embodiments of the present invention.
Example 1:
s1, adding triethanolamine into 1L of sodium salicylate aqueous solution with the mass fraction of 1%, regulating the pH value to 6, slowly adding 1L of cetyl trimethyl ammonium bromide aqueous solution with the mass fraction of 3%, uniformly mixing, slowly adding tetraethoxysilane with the total mass of 5% of the mixture and 1, 2-bis (triethoxysilane) -ethane, reacting for 16 hours at room temperature, centrifuging at 3000rpm for 40 minutes, and collecting precipitate to obtain 186g dendritic mesoporous silica nanoparticles.
S2, uniformly mixing 100g of dendritic mesoporous silica nano particles with 10g of cyanamide, and heating to 500 ℃ at a temperature rising rate of 3 ℃ per minute for reaction for 6 hours to obtain 105g of carbon nitride-loaded silica.
S3, dissolving the sasanqua saponin in an n-butanol solution to obtain 100mL of sasanqua saponin solution with the mass fraction of 5%, adding 25g of silicon dioxide loaded with carbon nitride, stirring at 2000rpm at room temperature for reaction for 3 hours, centrifuging at 5000rpm for 20 minutes, and collecting precipitate to obtain 28g of saponin type pond cleaning agent.
Example 2:
s1, adding triethanolamine into 1L of sodium salicylate aqueous solution with the mass fraction of 3%, regulating the pH value to 8, slowly adding 3L of cetyltrimethylammonium bromide aqueous solution with the mass fraction of 6%, uniformly mixing, slowly adding tetraethoxysilane with the total mass of 2% of the mixture and 1, 2-bis (triethoxysilane) -ethane, reacting at room temperature for 36 hours, centrifuging at 5000rpm for 20 minutes, and collecting precipitate to obtain 152g of dendritic mesoporous silica nanoparticles.
S2, uniformly mixing 100g of dendritic mesoporous silica nano particles with 50g of cyanamide, and heating to 600 ℃ at a heating rate of 6 ℃ per minute for reaction for 3 hours to obtain 141g of carbon nitride-loaded silica.
S3, dissolving the sasanqua saponin in an acetone solution to obtain 100mL of a sasanqua saponin solution with the mass fraction of 10%, adding 100g of silicon dioxide loaded with carbon nitride, stirring at 500rpm at room temperature for reaction for 6 hours, centrifuging at 3000rpm for 40 minutes, and collecting precipitate to obtain 106g of saponin type pond cleaning agent.
Example 3:
s1, adding triethanolamine into 1L of sodium salicylate aqueous solution with the mass fraction of 2%, regulating the pH value to 7, slowly adding 2L of cetyltrimethylammonium bromide aqueous solution with the mass fraction of 5%, uniformly mixing, slowly adding tetraethoxysilane with the total mass of 4% of the mixture and 1, 2-bis (triethoxysilane) -ethane, reacting for 24 hours at room temperature, centrifuging at 4000rpm for 30 minutes, and collecting precipitate to obtain 226g of dendritic mesoporous silica nanoparticles.
S2, uniformly mixing 100g of dendritic mesoporous silica nano particles with 30g of cyanamide, and heating to 550 ℃ at a temperature rising rate of 5 ℃ per minute for reaction for 5 hours to obtain 122g of carbon nitride-loaded silica.
S3, dissolving the sasanqua saponin in an ethanol solution to obtain 100mL of an 8% sasanqua saponin solution, adding 60g of silicon dioxide loaded with carbon nitride, stirring at 1000rpm at room temperature for reaction for 5 hours, centrifuging at 4000rpm for 30 minutes, and collecting precipitate to obtain 63g of saponin type pond cleaning agent.
Test example 1: structural analysis of the saponin-type pond scavenger prepared in example 1
The method comprises the following steps: the saponin type pond cleaning agent prepared in the example 1 is taken to be a proper amount for JEM-2100 transmission electron microscope observation of morphology; and taking a proper amount of the saponin type pond cleaning agent prepared in the embodiment 1, silicon dioxide loaded with carbon nitride, and raw material sasanqua saponin and carbon nitride KBr tablets, scanning by using a Bruker EQUINOX 55 infrared spectrometer, and carrying out infrared spectrum analysis, wherein the results are shown in figures 1-2.
Results: the electron microscope image of the saponin type pond cleaning agent shown in the figure 1 shows that dendritic mesoporous silicon dioxide is well dispersed, carbon nitride and oil tea saponin particles are loaded in dendritic mesopores, and the distribution is uniform, so that the saponin type pond cleaning agent can be well dispersed in water.
As can be seen from the infrared spectrum of FIG. 2, the carbon nitride is shown at 809cm -1 Has a characteristic triazine vibration peak of 1200-1700 cm -1 The nearby peaks are caused by stretching vibrations of the C-N heterocycle; the tea saponin is 1716cm -1 And 1635cm -1 The carbonyl characteristic absorption peaks are located, and the absorption peaks of the saponin type pond cleaning agents C=C and C=N are obviously enhanced and are shifted, so that the tea-oil saponin and the carbon nitride form coordination combination to generate a new compound.
Test example 2: the killing effect of the saponin pond cleaning agent prepared in the example 1 on the wild fish and pathogenic bacteria is measured
The method comprises the following steps: 20 crucian, grass carp, base shrimp and river crab are purchased from farmer market, the length of the crucian body is 10-15 cm, the length of the grass carp body is 10-20 cm, the length of the base shrimp body is 3-6 cm and the length of the river crab is 20-30 g. Subpackaging in 4 experimental aquariums with the size of 120cm×60cm for river crab culture test field. Testing initial concentration of Vibrio and Aeromonas, the saponin type pond cleaning agent of example 1 was added at 1, 3 and 5mg/m 3 The amounts are respectively added into an experimental aquarium, oil tea saponin is used as a control 1, carbon nitride is used as a control 2, the experimental aquarium is irradiated for 2 hours under sunlight, toxic reactions of fish, shrimp and crab are observed after 12 hours, 24 hours and 48 hours respectively, the concentration of vibrio and aeromonas is tested, and the sterilization rate is calculated, and the results are shown in tables 1-2.
TABLE 1 cumulative mortality of fish with saponin-type pond cleaning agent (%)
Results: the saponin type pond cleaning agent prepared in the embodiment 1 of the invention has no toxicity to prawn and crab, no death occurs, but has obvious killing effect to fish, and as can be seen from the table 1, the carbon nitride of the control 2 has no toxicity to fish, the oil tea saponin of the control 1 has certain toxicity to fish, but the toxicity of the complex of the two (the saponin type pond cleaning agent) to fish is obviously enhanced compared with that of the oil tea saponin of the control 1, so that the carbon nitride and the oil tea saponin have synergistic toxicity increasing effect.
TABLE 2 sterilizing rate of saponin type pond cleaning agent for pathogenic bacteria (%)
Results: from Table 2, it can be seen that although carbon nitride and tea saponin have a certain killing effect on vibrio and aeromonas, the bactericidal activity of the complex of tea saponin (saponin type pond cleaner) on pathogenic bacteria is obviously higher than that of the complex of tea saponin type pond cleaner) on pathogenic bacteria, which indicates that the complex has stronger bactericidal activity and synergistic effect when the complex of tea saponin type pond cleaner and the complex of tea saponin type pond cleaner are matched.
While the preferred embodiments of the present patent have been described in detail, the present patent is not limited to the above embodiments, and other various modifications and variations may be made within the knowledge of those skilled in the art. It is not necessary here nor is it exhaustive of all embodiments. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the invention are desired to be protected by the following claims.
Claims (4)
1. The saponin type pond cleaning agent is characterized by taking dendritic mesoporous silica nano particles as a carrier and taking tea-oil camellia saponin and carbon nitride coordination compounds as nano preparations of medicines;
the preparation method of the saponin type pond cleaning agent comprises the following steps:
s1, adding triethanolamine into a sodium salicylate aqueous solution with the mass fraction of 1-3% to adjust the pH value to 6-8, slowly adding a cetyl trimethyl ammonium bromide aqueous solution with the mass fraction of 3-6%, uniformly mixing, slowly adding tetraethoxysilane and 1, 2-bis (triethoxysilane) -ethane, reacting for a certain time at room temperature, centrifuging, and collecting precipitate to obtain dendritic mesoporous silica nanoparticles;
s2, uniformly mixing the dendritic mesoporous silica nano particles obtained in the step S1 with cyanamide, and reacting for a period of time under a heating condition to obtain carbon nitride-loaded silica;
s3, dissolving the sasanqua saponin in an organic solvent to obtain a sasanqua saponin solution with the mass fraction of 5-10%, then adding the carbon nitride-loaded silicon dioxide obtained in the S2, stirring at room temperature for reacting for a period of time, centrifuging, and collecting the precipitate to obtain a saponin type pond cleaning agent;
in the S1, the volume ratio of the hexadecyl trimethyl ammonium bromide aqueous solution to the sodium salicylate aqueous solution is 1-3:1;
in S1, the addition amount of tetraethoxysilane and 1, 2-bis (triethoxysilane) -ethane is 2-5% of the total mass of the mixture;
in the S1, the reaction time is 16-36 h, and the centrifugation condition is 3000-5000 rpm for 20-40 min;
s2, the mass ratio of the dendritic mesoporous silica to the cyanamide is 1:0.1-0.5; the heating reaction conditions are as follows: heating to 500-600 ℃ at a heating rate of 3-6 ℃ per minute for reaction for 3-6 hours;
s3, the organic solvent is any one of n-butanol, acetone and ethanol;
s3, the mass ratio of the silicon dioxide loaded with silicon nitride to the tea-oil camellia saponin is 5-10:1; the stirring reaction condition is 500-2000 rpm, the reaction time is 3-6 h, and the centrifugation condition is 3000-5000 rpm for 20-40 min.
2. The saponin pond cleaning agent according to claim 1, wherein the oil tea saponin contains more than 90% of saponin.
3. The method for preparing a saponin pond cleaning agent according to claim 1 or 2, comprising the steps of:
s1, adding triethanolamine into a sodium salicylate aqueous solution with the mass fraction of 1-3% to adjust the pH value to 6-8, slowly adding a cetyl trimethyl ammonium bromide aqueous solution with the mass fraction of 3-6%, uniformly mixing, slowly adding tetraethoxysilane and 1, 2-bis (triethoxysilane) -ethane, reacting for a certain time at room temperature, centrifuging, and collecting precipitate to obtain dendritic mesoporous silica nanoparticles;
s2, uniformly mixing the dendritic mesoporous silica nano particles obtained in the step S1 with cyanamide, and reacting for a period of time under a heating condition to obtain carbon nitride-loaded silica;
s3, dissolving the sasanqua saponin in an organic solvent to obtain a sasanqua saponin solution with the mass fraction of 5-10%, then adding the carbon nitride-loaded silicon dioxide obtained in the S2, stirring at room temperature for reacting for a period of time, centrifuging, and collecting the precipitate to obtain a saponin type pond cleaning agent;
in the S1, the volume ratio of the hexadecyl trimethyl ammonium bromide aqueous solution to the sodium salicylate aqueous solution is 1-3:1;
in S1, the addition amount of tetraethoxysilane and 1, 2-bis (triethoxysilane) -ethane is 2-5% of the total mass of the mixture;
in the S1, the reaction time is 16-36 h, and the centrifugation condition is 3000-5000 rpm for 20-40 min;
s2, the mass ratio of the dendritic mesoporous silica to the cyanamide is 1:0.1-0.5; the heating reaction conditions are as follows: heating to 500-600 ℃ at a heating rate of 3-6 ℃ per minute for reaction for 3-6 hours;
s3, the organic solvent is any one of n-butanol, acetone and ethanol;
s3, the mass ratio of the silicon dioxide loaded with silicon nitride to the tea-oil camellia saponin is 5-10:1; the stirring reaction condition is 500-2000 rpm, the reaction time is 3-6 h, and the centrifugation condition is 3000-5000 rpm for 20-40 min.
4. Use of the saponin-type pond cleaning agent according to claim 1 or 2 in pond cleaning, wherein the saponin-type pond cleaning agent is diluted with water and then mixed with water according to a ratio of 1-5 mg/m 3 Is sprayed on the fishpondIs prepared from the above materials.
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