CN106973948A - A kind of matrine water emulsion of quaternary ammonium salt grafting phosphate compounding and preparation method thereof - Google Patents
A kind of matrine water emulsion of quaternary ammonium salt grafting phosphate compounding and preparation method thereof Download PDFInfo
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- CN106973948A CN106973948A CN201710182566.4A CN201710182566A CN106973948A CN 106973948 A CN106973948 A CN 106973948A CN 201710182566 A CN201710182566 A CN 201710182566A CN 106973948 A CN106973948 A CN 106973948A
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- quaternary ammonium
- ammonium salt
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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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
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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
- A01N57/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
- A01N57/10—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds
- A01N57/12—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds containing acyclic or cycloaliphatic radicals
-
- 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
- A01N65/08—Magnoliopsida [dicotyledons]
- A01N65/20—Fabaceae or Leguminosae [Pea or Legume family], e.g. pea, lentil, soybean, clover, acacia, honey locust, derris or millettia
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- 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
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Agronomy & Crop Science (AREA)
- Plant Pathology (AREA)
- Dentistry (AREA)
- Wood Science & Technology (AREA)
- Environmental Sciences (AREA)
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- Natural Medicines & Medicinal Plants (AREA)
- Pest Control & Pesticides (AREA)
- Colloid Chemistry (AREA)
Abstract
A kind of matrine water emulsion of quaternary ammonium salt grafting phosphate compounding, it is characterised in that extracted and separating matrine using ultrasonic extraction and Microwave Extraction GC-MS and chloroform extraction first；Quaternary ammonium salt is prepared under acid catalysis by Dodecyl Dimethyl Amine and epoxychloropropane again, is grafted on phosphate, the phosphate of quaternary ammonium salt grafting is obtained；Oil-in-water mode is finally taken to prepare the matrine water emulsion of quaternary ammonium salt grafting phosphate compounding.The matrine water emulsion of the quaternary ammonium salt grafting phosphate compounding of the present invention, pure plant source, safety and environmental protection kills mosquito effect good.
Description
Technical field
The invention belongs to agriculture field, and in particular to a kind of matrine water emulsion of quaternary ammonium salt grafting phosphate compounding and its
Preparation method.
Background technology
In agricultural pollution source, pollution by pesticides is the one side of most serious.It is a large amount of to use severe toxicity, the broad spectrum activity of high residue
Chemical pesticide, not only causes farmland and agricultural product Pesticides content severe overweight, but also often results in people, animal poisoning,
Threaten the life and health of people.In order to fundamentally change this situation, it is necessary to use efficient, low toxicity or nontoxic, low residual
Stay or noresidue botanical pesticide.Numerous species in plant contain the composition for killing pest and disease damage, enter after industrialization extraction,
It can be used as agricultural chemicals, i.e. botanical pesticide.Most plant pesticide low toxicities, do not destroy ecological environment, and residual is few, selectivity
By force, pest natural enemy, insect and germ are not killed plant pesticide is difficult to develop immunity to drugs, serviceable bife is long, and consumption is few, uses
Cost is low.Using plant pesticide, for promoting agricultural sustainable development, with extremely important realistic meaning.Kuh-seng is pulse family
Plant kuh-seng（Sophora flavescens Ait）Root, have heat-clearing and damp-drying drug, desinsection, the effects such as diuresis.Kuh-seng is in medicine, beast
It is of wide application in terms of medicine, agricultural chemicals, environmental sanitation medication, is a kind of rising botanical pesticide resource.
Tian Benzhi et al. exists《Prevention effect of the kuh-seng aqueous emulsion of biological pesticide 2% to cabbage caterpillar》Experimental study table in one text
Bright, 2% kuh-seng aqueous emulsion is a kind of good medicament for being used to prevent and treat brassicaceous vegetable (Chinese cabbage) insect cabbage caterpillar.The medicament has
Have good disinsection effect, do not injure natural enemy, it is free from environmental pollution the features such as, safety is grown to Chinese cabbage, and the lasting period is also longer.
The content of the invention
It is an object of the invention to provide a kind of matrine water emulsion of quaternary ammonium salt grafting phosphate compounding and its preparation side
Method.
To achieve these goals, present invention employs following technical scheme：
A kind of matrine water emulsion of quaternary ammonium salt grafting phosphate compounding, it is characterised in that first using ultrasonic extraction and microwave
GC-MS and chloroform extraction is extracted to extract and separating matrine；Pass through Dodecyl Dimethyl Amine and epoxy chlorine again
Propane prepares quaternary ammonium salt under acid catalysis, is grafted on phosphate, obtains the phosphate of quaternary ammonium salt grafting；Finally adopt
Oil-in-water mode is taken to prepare the matrine water emulsion of quaternary ammonium salt grafting phosphate compounding.
The matrine water emulsion of described quaternary ammonium salt grafting phosphate compounding, it is characterised in that it is by following parts by weight
Raw material is prepared from：25-30 parts of kuh-seng, 6-8 parts of anise, 5-6 parts of Gui Ye, 10-12 parts of Dodecyl Dimethyl Amine, n-butanol
30-40 parts, 6-8 parts of epoxychloropropane, 25-30 parts of ethyl acetate, 4-5 parts of diethyl maleate, 12-15 parts of phosphate aqueous solution,
80-100 parts of toluene, 5-6 parts of dibutyl succinic acid sodium sulfonate, 8-10 parts of polyvinyl alcohol, 70-75% ethanol water is appropriate, salt
Appropriate aqueous acid, appropriate chloroform, appropriate deionized water.
The matrine water emulsion of described quaternary ammonium salt grafting phosphate compounding, it is characterised in that it is by steps system
It is standby to form：
（1）Kuh-seng, anise, Gui Ye are cleaned 2-3 times with deionized water, natural air drying；Attrition grinding 50-60min, crosses 80-100
Mesh sieve, obtains granulate mixture；Granulate mixture is using 70-75% ethanol water ultrasonic extraction 2-3 times, and each ultrasound is carried
The condition taken is：Solid-liquid ratio is 7-8, and ultrasonic extraction temperature is 50-60 DEG C, and ultrasonic power is 300-400W, during ultrasonic extraction
Between 30-40min；Filtering, collects filtrate, and filtrate is reclaimed ethanol, distillation is treated by merging filtrate by 65-70 DEG C of vacuum distillation
With；
（2）Filter cake is used into aqueous hydrochloric acid solution microwave abstracting 3-4 times, the condition of each microwave abstracting is：PH is 3-4, solid-liquid ratio
For 10-11, microwave power is 500-550w, and radiated time is 20-25min, filtering, filtrate is collected, by filtrate and step（1）'s
Distillation merges, and is concentrated under reduced pressure into liquid volume and reduces 2/3；Regulation PH is 10-11, using chloroform extraction 2-3 times, every time
The condition of extraction is：The volume ratio of aqueous phase and organic phase is 3-4：1, merge organic phase, three are reclaimed by 50-60 DEG C of vacuum distillation
Chloromethanes, obtains matrine crude oil；
（3）Dodecyl Dimethyl Amine is added to deionization of 2-3 times equivalent to Dodecyl Dimethyl Amine parts by weight
In water, regulation system PH is magnetic agitation 6-8h under 6-7, normal temperature, is filtered, and is dried；Resulting product is added to n-butanol
In, magnetic agitation 20-30min, rise temperature is to 70-75 DEG C, and regulation system PH is 5-6, and epoxychloropropane is slowly added dropwise, and is added dropwise
3-4h is stirred vigorously after finishing, ethyl acetate and diethyl maleate is added, continues to be stirred vigorously 5-6h, phosphoric acid is slowly added dropwise
After the aqueous solution, completion of dropping, rise temperature is stirred at reflux 5-6h to 95-100 DEG C；
（4）By step（2）Product be added in toluene, mixing make it be completely dissolved to form oil phase, then by step（3）
Product, dibutyl succinic acid sodium sulfonate, polyvinyl alcohol be added to deionized water of 50-60 times equivalent to polyvinyl alcohol weight part
Middle dissolving forms aqueous phase；In high-shear emulsion machine, with 2500-3000r/min stir speed (S.S.), oil phase is poured slowly into aqueous phase
In, 20-30min is stirred, a kind of matrine water emulsion of quaternary ammonium salt grafting phosphate compounding is obtained.
The matrine water emulsion of described quaternary ammonium salt grafting phosphate compounding, it is characterised in that described aqueous hydrochloric acid solution
Concentration be 2-3mol/L, the concentration of described phosphate aqueous solution is 0.8-1mol/L.
Using above-mentioned technical scheme, beneficial effects of the present invention are：
The present invention first crushes kuh-seng, then using ultrasonator ultrasonic extraction, utilizes cavitation effect, fuel factor and the machine of ultrasound
Tool effect is acted on, and when the ul-trasonic irradiation of big energy is in kuh-seng, kuh-seng cell membrane and organism is existed under larger pressure
Moment ruptures, and substantially reduces the extraction time of matrine, the effect of vibration of ultrasonic wave strengthens the release of intracellular matrine,
So as to improve the recovery rate of matrine.The present invention is again by the filter cake obtained after ultrasonic extraction by microwave abstracting, and microwave has
Penetrability, makes polar molecule and group produce heat with microwave high-frequency concussion, can be simultaneously rapid, equal in reactant internal and external parts
Heat evenly；Remaining matrine in filter cake is extracted, the recovery rate of matrine is further increased.The present invention is additionally added
Anistree and osmanthus leaf, aniseed essential oil and osmanthus leaf essential oil have antifeedant activity to insect, further increase the insecticidal activity of matrine.
Dodecyl Dimethyl Amine of the present invention prepares quaternary ammonium salt with epoxychloropropane under acid catalysis, then is grafted on phosphoric acid
On ester, the phosphate of quaternary ammonium salt grafting is obtained, is added in aqueous emulsion, can not only reduce system in long term storage unstable
Fixed, the phenomenon such as preparation layering, precipitation, precipitation crystallization causes the problem of bioactivity is reduced, and quaternary ammonium salt has broad-spectrum antibacterial
Function, can suppress harmful microbe growth, or even kill harmful microorganism.The quaternary ammonium salt grafting phosphate compounding of the present invention
Matrine water emulsion, pure plant source, safety and environmental protection, kill mosquito effect it is good.
Embodiment
The matrine water emulsion of the quaternary ammonium salt grafting phosphate compounding of the present embodiment, it is prepared by the raw material of following parts by weight
Form：30 parts of kuh-seng, anistree 8 parts, 6 parts of Gui Ye, 12 parts of Dodecyl Dimethyl Amine, 40 parts of n-butanol, epoxychloropropane 8
Part, 30 parts of ethyl acetate, 5 parts of diethyl maleate, 15 parts of phosphate aqueous solution, 100 parts of toluene, dibutyl succinic acid sodium sulfonate 6
Part, 10 parts of polyvinyl alcohol, appropriate 75% ethanol water, appropriate aqueous hydrochloric acid solution, appropriate chloroform, appropriate deionized water.
The matrine water emulsion of the quaternary ammonium salt grafting phosphate compounding of the present embodiment, it is prepared from by the steps：
（1）Kuh-seng, anise, Gui Ye are cleaned into 3 times, natural air drying with deionized water；Attrition grinding 60min, crosses 100 mesh sieves, obtains
To granulate mixture；Granulate mixture is using 75% ethanol water ultrasonic extraction 2-3 times, and the condition of each ultrasonic extraction is：
Solid-liquid ratio is 7, and ultrasonic extraction temperature is 60 DEG C, and ultrasonic power is 400W, ultrasonic extraction time 30min；Filtering, collects filter
Filtrate is reclaimed ethanol, distillation is stand-by by liquid, merging filtrate by 70 DEG C of vacuum distillations；
（2）Filter cake is used into aqueous hydrochloric acid solution microwave abstracting 4 times, the condition of each microwave abstracting is：PH is 3, and solid-liquid ratio is 10,
Microwave power is 550w, and radiated time is 25min, filtering, filtrate is collected, by filtrate and step（1）Distillation merge, decompression
It is concentrated into liquid volume and reduces 2/3；It is 11 to adjust PH, and using chloroform extraction 3 times, the condition extracted every time is：Aqueous phase with
The volume ratio of organic phase is 4：1, merge organic phase, reclaim chloroform by 60 DEG C of vacuum distillations, obtain matrine crude oil；
（3）Dodecyl Dimethyl Amine is added to deionized water of 3 times equivalent to Dodecyl Dimethyl Amine parts by weight
In, regulation system PH is magnetic agitation 8h under 6, normal temperature, is filtered, and is dried；Resulting product is added in n-butanol, magnetic force
30min is stirred, rise temperature is to 75 DEG C, and regulation system PH is 5, is stirred vigorously after epoxychloropropane, completion of dropping is slowly added dropwise
4h, adds ethyl acetate and diethyl maleate, continues to be stirred vigorously 6h, is slowly added dropwise after phosphate aqueous solution, completion of dropping,
Rise temperature is stirred at reflux 6h to 100 DEG C；
（4）By step（2）Product be added in toluene, mixing make it be completely dissolved to form oil phase, then by step（3）
Product, dibutyl succinic acid sodium sulfonate, polyvinyl alcohol be added in deionized water of 60 times equivalent to polyvinyl alcohol weight part
Dissolving forms aqueous phase；In high-shear emulsion machine, with 3000r/min stir speed (S.S.), oil phase is poured slowly into aqueous phase, stirred
30min, obtains a kind of matrine water emulsion of quaternary ammonium salt grafting phosphate compounding.
The concentration of the aqueous hydrochloric acid solution of the present embodiment is 3mol/L, and the concentration of phosphate aqueous solution is 1mol/L.
Claims (4)
1. a kind of matrine water emulsion of quaternary ammonium salt grafting phosphate compounding, it is characterised in that first using ultrasonic extraction with it is micro-
Ripple extracts GC-MS and chloroform extraction to extract and separating matrine；Pass through Dodecyl Dimethyl Amine and epoxy again
Chloropropane prepares quaternary ammonium salt under acid catalysis, is grafted on phosphate, obtains the phosphate of quaternary ammonium salt grafting；Finally
Oil-in-water mode is taken to prepare the matrine water emulsion of quaternary ammonium salt grafting phosphate compounding.
2. according to claims 1 quaternary ammonium salt grafting phosphate compounding matrine water emulsion, it is characterised in that its by
The raw material of following parts by weight is prepared from：25-30 parts of kuh-seng, 6-8 parts of anise, 5-6 parts of Gui Ye, Dodecyl Dimethyl Amine
10-12 parts, 30-40 parts of n-butanol, 6-8 parts of epoxychloropropane, 25-30 parts of ethyl acetate, 4-5 parts of diethyl maleate, phosphoric acid
12-15 parts of the aqueous solution, 80-100 parts of toluene, 5-6 parts of dibutyl succinic acid sodium sulfonate, 8-10 parts of polyvinyl alcohol, 70-75% second
Appropriate alcohol solution, appropriate aqueous hydrochloric acid solution, appropriate chloroform, appropriate deionized water.
3. according to claims 1 quaternary ammonium salt grafting phosphate compounding matrine water emulsion, it is characterised in that its by
The steps is prepared from：
（1）Kuh-seng, anise, Gui Ye are cleaned 2-3 times with deionized water, natural air drying；Attrition grinding 50-60min, crosses 80-100
Mesh sieve, obtains granulate mixture；Granulate mixture is using 70-75% ethanol water ultrasonic extraction 2-3 times, and each ultrasound is carried
The condition taken is：Solid-liquid ratio is 7-8, and ultrasonic extraction temperature is 50-60 DEG C, and ultrasonic power is 300-400W, during ultrasonic extraction
Between 30-40min；Filtering, collects filtrate, and filtrate is reclaimed ethanol, distillation is treated by merging filtrate by 65-70 DEG C of vacuum distillation
With；
（2）Filter cake is used into aqueous hydrochloric acid solution microwave abstracting 3-4 times, the condition of each microwave abstracting is：PH is 3-4, solid-liquid ratio
For 10-11, microwave power is 500-550w, and radiated time is 20-25min, filtering, filtrate is collected, by filtrate and step（1）'s
Distillation merges, and is concentrated under reduced pressure into liquid volume and reduces 2/3；Regulation PH is 10-11, using chloroform extraction 2-3 times, every time
The condition of extraction is：The volume ratio of aqueous phase and organic phase is 3-4：1, merge organic phase, three are reclaimed by 50-60 DEG C of vacuum distillation
Chloromethanes, obtains matrine crude oil；
（3）Dodecyl Dimethyl Amine is added to deionization of 2-3 times equivalent to Dodecyl Dimethyl Amine parts by weight
In water, regulation system PH is magnetic agitation 6-8h under 6-7, normal temperature, is filtered, and is dried；Resulting product is added to n-butanol
In, magnetic agitation 20-30min, rise temperature is to 70-75 DEG C, and regulation system PH is 5-6, and epoxychloropropane is slowly added dropwise, and is added dropwise
3-4h is stirred vigorously after finishing, ethyl acetate and diethyl maleate is added, continues to be stirred vigorously 5-6h, phosphoric acid is slowly added dropwise
After the aqueous solution, completion of dropping, rise temperature is stirred at reflux 5-6h to 95-100 DEG C；
（4）By step（2）Product be added in toluene, mixing make it be completely dissolved to form oil phase, then by step（3）
Product, dibutyl succinic acid sodium sulfonate, polyvinyl alcohol be added to deionized water of 50-60 times equivalent to polyvinyl alcohol weight part
Middle dissolving forms aqueous phase；In high-shear emulsion machine, with 2500-3000r/min stir speed (S.S.), oil phase is poured slowly into aqueous phase
In, 20-30min is stirred, a kind of matrine water emulsion of quaternary ammonium salt grafting phosphate compounding is obtained.
4. the matrine water emulsion of the quaternary ammonium salt grafting phosphate compounding according to claims 2,3, it is characterised in that institute
The concentration for the aqueous hydrochloric acid solution stated is 2-3mol/L, and the concentration of described phosphate aqueous solution is 0.8-1mol/L.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114287451A (en) * | 2021-12-31 | 2022-04-08 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of natural plant modified antibacterial liquid and product thereof |
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| CN104488998A (en) * | 2014-11-28 | 2015-04-08 | 馥稷生物科技发展（上海）有限公司 | Synergistic compound hicide caphidicide containing sophocarpidine and preparation method of synergistic compound hicide caphidicide |
| CN105968133A (en) * | 2016-05-18 | 2016-09-28 | 大连和田科技有限公司 | Preparation method of phosphate quaternary ammonium salt bactericide |
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2017
- 2017-03-24 CN CN201710182566.4A patent/CN106973948A/en active Pending
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| CN1422531A (en) * | 2002-12-17 | 2003-06-11 | 吕世禄 | 0.36% kuh-seng lye emulsion farm chemical and production method thereof |
| CN104488998A (en) * | 2014-11-28 | 2015-04-08 | 馥稷生物科技发展（上海）有限公司 | Synergistic compound hicide caphidicide containing sophocarpidine and preparation method of synergistic compound hicide caphidicide |
| CN105968133A (en) * | 2016-05-18 | 2016-09-28 | 大连和田科技有限公司 | Preparation method of phosphate quaternary ammonium salt bactericide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114287451A (en) * | 2021-12-31 | 2022-04-08 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of natural plant modified antibacterial liquid and product thereof |
| CN114287451B (en) * | 2021-12-31 | 2022-12-27 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of natural plant modified antibacterial liquid and product thereof |
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