CN106212449A - A kind of preparation method of plant source slow-release bactericide - Google Patents
A kind of preparation method of plant source slow-release bactericide Download PDFInfo
- Publication number
- CN106212449A CN106212449A CN201610540626.0A CN201610540626A CN106212449A CN 106212449 A CN106212449 A CN 106212449A CN 201610540626 A CN201610540626 A CN 201610540626A CN 106212449 A CN106212449 A CN 106212449A
- Authority
- CN
- China
- Prior art keywords
- plant source
- antibacterial
- walnut shell
- release
- slow
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 51
- 239000003899 bactericide agent Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 241000196324 Embryophyta Species 0.000 claims abstract description 64
- 230000001954 sterilising effect Effects 0.000 claims abstract description 47
- 241000758789 Juglans Species 0.000 claims abstract description 29
- 235000009496 Juglans regia Nutrition 0.000 claims abstract description 29
- 235000020234 walnut Nutrition 0.000 claims abstract description 29
- 229920000881 Modified starch Polymers 0.000 claims abstract description 22
- 239000004368 Modified starch Substances 0.000 claims abstract description 22
- 238000004821 distillation Methods 0.000 claims abstract description 22
- 235000019426 modified starch Nutrition 0.000 claims abstract description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000428 dust Substances 0.000 claims abstract description 16
- 239000003610 charcoal Substances 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 42
- 238000004659 sterilization and disinfection Methods 0.000 claims description 38
- 238000003756 stirring Methods 0.000 claims description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 20
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 18
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 18
- 238000000605 extraction Methods 0.000 claims description 18
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 15
- 239000006185 dispersion Substances 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 239000012530 fluid Substances 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 229920001592 potato starch Polymers 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000004530 micro-emulsion Substances 0.000 claims description 10
- 230000001804 emulsifying effect Effects 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 6
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 6
- 241000628997 Flos Species 0.000 claims description 6
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 6
- 241000366182 Melaleuca alternifolia Species 0.000 claims description 6
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 6
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 6
- 238000003763 carbonization Methods 0.000 claims description 6
- 238000004945 emulsification Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 230000010355 oscillation Effects 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 239000003643 water by type Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- JNYAEWCLZODPBN-JGWLITMVSA-N (2r,3r,4s)-2-[(1r)-1,2-dihydroxyethyl]oxolane-3,4-diol Chemical class OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O JNYAEWCLZODPBN-JGWLITMVSA-N 0.000 claims description 3
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical compound OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 claims description 2
- 210000000481 breast Anatomy 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 12
- 230000000855 fungicidal effect Effects 0.000 abstract description 7
- 239000000417 fungicide Substances 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract description 2
- 239000000284 extract Substances 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 235000015112 vegetable and seed oil Nutrition 0.000 abstract description 2
- 239000008158 vegetable oil Substances 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 26
- 235000019198 oils Nutrition 0.000 description 26
- 239000000839 emulsion Substances 0.000 description 8
- 238000010298 pulverizing process Methods 0.000 description 7
- 239000007921 spray Substances 0.000 description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 description 4
- 229920002472 Starch Polymers 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- -1 polysaccharide compounds Chemical class 0.000 description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 description 4
- 235000019698 starch Nutrition 0.000 description 4
- 239000008107 starch Substances 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 210000000582 semen Anatomy 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 244000144730 Amygdalus persica Species 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 235000006040 Prunus persica var persica Nutrition 0.000 description 1
- 241001464837 Viridiplantae Species 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000000645 desinfectant Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 241000411851 herbal medicine Species 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 239000002085 irritant Substances 0.000 description 1
- 231100000021 irritant Toxicity 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 239000003094 microcapsule Substances 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000035943 smell Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000002699 waste material Substances 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
- 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
- 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
- A01N25/26—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 in coated particulate form
-
- 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
-
- 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]
- A01N65/28—Myrtaceae [Myrtle family], e.g. teatree or clove
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Zoology (AREA)
- Agronomy & Crop Science (AREA)
- Plant Pathology (AREA)
- Environmental Sciences (AREA)
- Dentistry (AREA)
- Wood Science & Technology (AREA)
- Pest Control & Pesticides (AREA)
- Toxicology (AREA)
- Biotechnology (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Botany (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The present invention relates to the preparation method of a kind of plant source slow-release bactericide, belong to antibacterial preparation field.The method extracts vegetable oil as sterilizing source by vapor distillation, the loose structure of recycling walnut shell charcoal loads sterilizing source, it is drying to obtain antibacterial after the walnut shell carbon dust of load sterilizing source being coated with modified starch for release coated layer again, the present invention compounds the broad spectrum activity improving antibacterial with various plants, antibacterial is made to have splendid slow release effect after the load of walnut shell carbon dust is coated with by modified starch again, sterilizing time is longer, sterilizing source availability is improved, and replace chemical bactericide with botanical fungicide, avoiding antibacterial easily residual can be to human body and the problem of the harm of environment, compensate for again botanical fungicide broad spectrum activity poor, many existence releases are too fast, can not be fully utilized, cause the defect of the wasting of resources, have broad application prospects.
Description
Technical field
The present invention relates to the preparation method of a kind of plant source slow-release bactericide, belong to antibacterial preparation field.
Background technology
Along with progress and mankind's enhancing to ecological protection consciousness of science and technology, find new efficient, low toxicity and ring
The natural materials substituted chemistry synthesizing fungicide that the border compatibility is good is the focus of current research.Making a general survey of whole world history, plant kingdom is
The mankind provide a series of medicine, and the bacteriostasis property of plant is known from the most very early, and China uses the history of Chinese herbal medicine very
Before can tracing back to 6000.Therefore extract natural and organic ingredients from plant preparing botanical fungicide is current research
Trend, so-called botanical fungicide refers to extract from some position of the natural plants with sterilization, bacteriostatic activity effective
Composition, is isolated purification and is then passed through processing the medicament obtained.
The exploitation of existing botanical fungicide mostly concentrates in the research of single antibacterial, but the opening of single antibacterial
Sending out the waste that can cause cost, consumption is big, the longest, and single culture is mostly only played inhibitory action by single antibacterial.
Therefore, exploitation composite bactericide can not only solve the shortcoming that single antibacterial utilizes, moreover it is possible to is effectively improved inhibitory effect, strengthens
Broad spectrum antibacterial, makes pathogenic bacteria be difficult to develop immunity to drugs.
Starch is natural macromolecular compound, and low price, easy biological starch are a kind of polysaccharide compounds, is green
Plant is formed by carbon dioxide and water through photosynthesis, is mainly enriched in the organs such as the seed of plant, tuber, block, its
Yield is very abundant, degraded, it is common that be present in granular form in a large amount of plant such as Semen Maydis, rice, Semen Tritici aestivi and Semen sojae atricolor.Natural
Starch is a kind of very important energy substance, is also a kind of regenerative resource.The wall material making microcapsule of starch is because it
When highly filled, remain to show relatively low-viscosity, and there is good dissolubility, thus preferably control pesticide, antibacterial
Deng release, and there is good degradability, for making full use of of antibacterial, the protection of environment, the health of the mankind and animal
Have great significance.
Summary of the invention
The technical problem that present invention mainly solves: mostly be chloride, organic for disinfectant use in agriculture the most conventional
Iodine mixture or the chemical bactericide of phenols, also exist that acid-base value is high, corrosivity strong and the problem such as bacterial drug resistance, make for a long time
With corrosion both hands and irritant abnormal smells from the patient, the antibacterial of residual endangers environment, and botanical fungicide broad spectrum activity is poor, and exist releases more
Let slip fast, it is impossible to be fully utilized, cause the defect of the wasting of resources, it is provided that the preparation side of a kind of plant source slow-release bactericide
Method.The method is extracted vegetable oil by vapor distillation and is loaded kill as sterilizing source, the loose structure of recycling walnut shell charcoal
Bacterium source, then with modified starch for release coated layer to load sterilizing source walnut shell carbon dust be coated with after be drying to obtain sterilization
Agent, the present invention compounds the broad spectrum activity improving antibacterial with various plants, is coated with by modified starch through the load of walnut shell carbon dust again
After make antibacterial have splendid slow release effect, sterilizing time is longer, to sterilizing source availability improve, and with plant source sterilize
Agent replaces chemical bactericide, it is to avoid the problem that human body and environment can be worked the mischief by antibacterial easily residual, compensate for again plant
Source bactericide broad spectrum activity is poor, and many existence releases are too fast, it is impossible to are fully utilized, cause the defect of the wasting of resources, have wide
Application prospect.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
(1) weigh 400～500g Flos Caryophyllis, 300～400g Cortex Cinnamomi respectively to put together with 600～700g Melaleuca Alternifolia fresh braches
Enter in jet mill pulverize 20～30min, will pulverize after mixture proceed in vapor distillation device, distillation extraction 5～
Obtain distillate after 7h, then in distillate, add its volume 1～3 times of ether oscillation extractions 10～15min, at 35～40 DEG C
Distillation extraction liquid, reclaims ether and obtains plant source sterilization oil；
(2) crossing 200 mesh standard sieves after weighing 40～50g walnut shell ball mill grindings, the walnut shell powder after sieving puts into charcoal
Changing stove, at 300～400 DEG C, carbonization 2～3h obtains walnut shell carbon dust under nitrogen protection, counts by weight and weighs 80～90
Part above-mentioned plant source sterilization oil, 5～8 parts of sorbitan esters, 3～5 parts of glycerol, 1～2 part of n-butyl alcohol and 90～100 parts of distillations
Water mixes and puts in ultrasonic emulsification disperser, after ultrasonic disperse 2～3h, obtains plant source sterilization oil Microemulsions For Use；
(3) by solid-to-liquid ratio be 1:8 walnut shell carbon dust is joined above-mentioned plant source sterilization oil Microemulsions For Use in, be placed on high shear breast
In change machine, with 7000～8000r/min rotating speed cutting emulsifyings 3～4h, obtain plant source sterilization emulsified dispersed liquid, standby；
(4) three mouthfuls with agitator and condensing tube are loaded after potato starch and butyl acrylate being mixed for 3:2 in mass ratio
In flask, then in flask, add both mixture gross mass 8～10 times of deionized waters, be passed through nitrogen as protection gas, startup
Agitator adds potato starch quality 1.5～the benzoyl peroxide of 1.8% after stirring mixing 5～6min at 30～40 DEG C,
Raise bath temperature to be dried to 60～70 DEG C of stirring reactions 5～7h, obtain modified starch；
(5) it is that above-mentioned modified starch is dissolved in dimethylformamide by 1:5 by solid-to-liquid ratio, adds the poly-of the quality such as modified starch
Vinyl alcohol, insulated and stirred 15～20min at 40～50 DEG C, prepare slow release base fluid；
(6) above-mentioned standby plant source sterilization emulsified dispersed liquid is loaded in the there-necked flask with Dropping funnel and agitator,
Flask is put in the oil bath pan of 75～85 DEG C, start agitator and be stirred with 100～200r/min rotating speeds, add dispersion
Liquid quality 1～the glutaraldehyde of 2%, dropwise instill the slow release base fluid of dispersion liquid volume 1/3 during stirring, continues insulation and stirs
Filter after mixing reaction 20～30min, filtering residue is put into baking oven, at 70～80 DEG C, after heat preservation and dryness 2～3h, i.e. obtain plant source delay
Release antibacterial.
The application process of the present invention is: add clear water dilution 5～10 in the plant source slow-release bactericide present invention prepared
Times, load in agricultural watering can, be sprayed at Tanaka with the dose uniformity of every mu 8～10L, wherein sprayed once every 5～7 days, always
Spray 2～4 times altogether.After using, 3～5 days antibacterial burst sizes reach 60～after 80%, 7～9 day antibacterial release rate reach
To more than 98%, there is splendid slow release effect, and can degrade voluntarily after using, without any residual, to human body and environmentally friendly.
The invention has the beneficial effects as follows:
(1) the plant source slow-release bactericide raw material that the present invention prepares is easy to get, and preparation process is simple to operation, with low cost；
(2) the plant source slow-release bactericide that the present invention prepares has splendid slow release effect, antibacterial release in 3～5 days after using
Amount reach 60～after 80%, 7～9 day antibacterial release rate reach more than 98%；
(3) the plant source slow-release bactericide that the present invention prepares can biodegradation voluntarily, noresidue, to human body and environment without any danger
Evil.
Detailed description of the invention
Weigh 400～500g Flos Caryophyllis, 300～400g Cortex Cinnamomi respectively together with 600～700g Melaleuca Alternifolia fresh braches
Putting into and pulverize 20～30min in jet mill, the mixture after pulverizing proceeds in vapor distillation device, distillation extraction 5
～after 7h, obtain distillate, then in distillate, add its volume 1～3 times of ether oscillation extractions 10～15min, at 35～40 DEG C
Lower distillation extraction liquid, reclaims ether and obtains plant source sterilization oil；200 mesh are crossed after weighing 40～50g walnut shell ball mill grindings
Standard screen, the walnut shell powder after sieving puts into retort, and at 300～400 DEG C, carbonization 2～3h obtains core under nitrogen protection
Peach shell carbon dust, by weight meter weigh 80～90 parts of above-mentioned plant sources sterilization oil, 5～8 parts of sorbitan esters, 3～5 parts sweet
Oil, 1～2 part of n-butyl alcohol and 90～100 parts of distilled water mix and put in ultrasonic emulsification disperser, after ultrasonic disperse 2～3h,
To plant source sterilization oil Microemulsions For Use；It is that walnut shell carbon dust is joined in above-mentioned plant source sterilization oil Microemulsions For Use by 1:8 by solid-to-liquid ratio,
It is placed in high-shear emulsion machine, with 7000～8000r/min rotating speed cutting emulsifyings 3～4h, obtains plant source sterilization emulsifying and divide
Dissipate liquid, standby；Three with agitator and condensing tube are loaded after potato starch and butyl acrylate being mixed for 3:2 in mass ratio
In mouthful flask, then in flask, add both mixture gross mass 8～10 times of deionized waters, be passed through nitrogen as protection gas, open
Dynamic agitator adds potato starch quality 1.5～the benzoyl peroxide first of 1.8% after stirring mixing 5～6min at 30～40 DEG C
Acyl, raises bath temperature and is dried to 60～70 DEG C of stirring reactions 5～7h, obtain modified starch；It is that 1:5 is by above-mentioned by solid-to-liquid ratio
Modified starch is dissolved in dimethylformamide, adds the polyvinyl alcohol of the quality such as modified starch, is incubated and stirs at 40～50 DEG C
Mix 15～20min, prepare slow release base fluid；Above-mentioned standby plant source sterilization emulsified dispersed liquid is loaded with Dropping funnel and stirs
Mix in the there-necked flask of device, flask is put in the oil bath pan of 75～85 DEG C, start agitator and enter with 100～200r/min rotating speeds
Row stirring, adds dispersion liquid quality 1～the glutaraldehyde of 2%, dropwise instills the slow of dispersion liquid volume 1/3 during stirring
Release base fluid, filter after continuing insulated and stirred reaction 20～30min, filtering residue is put into baking oven, at 70～80 DEG C heat preservation and dryness 2～
Plant source slow-release bactericide is i.e. obtained after 3h.
Example 1
Weigh 400g Flos Caryophylli, 300g Cortex Cinnamomi respectively and put into pulverizing in jet mill together with 600g Melaleuca Alternifolia fresh braches
20min, the mixture after pulverizing proceeds to, in vapor distillation device, obtain distillate after distillation extraction 5h, then to distillate
1 times of ether oscillation extraction 10min of its volume of middle addition, distillation extraction liquid at 35 DEG C, reclaims ether and obtains plant source sterilization oil；
Crossing 200 mesh standard sieves after weighing 40g walnut shell ball mill grinding, the walnut shell powder after sieving puts into retort, at nitrogen
Under protection, at 300 DEG C, carbonization 2h obtains walnut shell carbon dust, by weight meter weigh 80 parts of above-mentioned plant sources sterilization oil, 5 parts
Sorbitan ester, 3 parts of glycerol, 1 part of n-butyl alcohol and 90 parts of distilled water mix and put in ultrasonic emulsification disperser, ultrasonic disperse
After 2h, obtain plant source sterilization oil Microemulsions For Use；By solid-to-liquid ratio be 1:8 walnut shell carbon dust is joined above-mentioned plant source sterilization oil micro-
In emulsion, it is placed in high-shear emulsion machine, with 7000r/min rotating speed cutting emulsifying 3h, obtains plant source sterilization emulsion dispersion
Liquid, standby；Three mouthfuls with agitator and condensing tube are loaded after potato starch and butyl acrylate being mixed for 3:2 in mass ratio
In flask, then in flask, add both 8 times of deionized waters of mixture gross mass, be passed through nitrogen as protection gas, startup stirring
Device adds the benzoyl peroxide of potato starch quality 1.5% after stirring mixing 5min at 30 DEG C, raise bath temperature to 60
DEG C stirring reaction 5h after be dried, obtain modified starch；It is that above-mentioned modified starch is dissolved in dimethylformamide by 1:5 by solid-to-liquid ratio
In, add the polyvinyl alcohol of the quality such as modified starch, insulated and stirred 15min at 40 DEG C, prepare slow release base fluid；By above-mentioned standby
Plant source sterilization emulsified dispersed liquid load in there-necked flask with Dropping funnel and agitator, flask is put into 75 DEG C
In oil bath pan, start agitator and be stirred with 100r/min rotating speed, add the glutaraldehyde of dispersion liquid quality 1%, in stirring
During dropwise instill the slow release base fluid of dispersion liquid volume 1/3, filter after continuing insulated and stirred reaction 20min, filtering residue put into
Baking oven, i.e. obtains plant source slow-release bactericide at 70 DEG C after heat preservation and dryness 2h.
The application process of the present invention is: adds clear water in the plant source slow-release bactericide present invention prepared and dilutes 5 times, dress
Enter in agricultural watering can, spray Tanaka with the dose uniformity of every mu of 8L, wherein sprayed once every 5 days, altogether spray 2 times,.
After using, within 3 days, antibacterial burst size reaches 60%, and after 7 days, antibacterial release rate reaches 98.5%, has splendid slow release effect,
And can degrade voluntarily after using, without any residual, to human body and environmentally friendly.
Example 2
Weigh 450g Flos Caryophylli, 350g Cortex Cinnamomi respectively and put into pulverizing in jet mill together with 650g Melaleuca Alternifolia fresh braches
25min, the mixture after pulverizing proceeds to, in vapor distillation device, obtain distillate after distillation extraction 6h, then to distillate
2 times of ether oscillation extraction 13min of its volume of middle addition, distillation extraction liquid at 38 DEG C, reclaims ether and obtains plant source sterilization oil；
Crossing 200 mesh standard sieves after weighing 45g walnut shell ball mill grinding, the walnut shell powder after sieving puts into retort, at nitrogen
Under protection, at 350 DEG C, carbonization 2h obtains walnut shell carbon dust, by weight meter weigh 85 parts of above-mentioned plant sources sterilization oil, 7 parts
Sorbitan ester, 4 parts of glycerol, 1 part of n-butyl alcohol and 95 parts of distilled water mix and put in ultrasonic emulsification disperser, ultrasonic disperse
After 2h, obtain plant source sterilization oil Microemulsions For Use；By solid-to-liquid ratio be 1:8 walnut shell carbon dust is joined above-mentioned plant source sterilization oil micro-
In emulsion, it is placed in high-shear emulsion machine, with 7500r/min rotating speed cutting emulsifying 3h, obtains plant source sterilization emulsion dispersion
Liquid, standby；Three mouthfuls with agitator and condensing tube are loaded after potato starch and butyl acrylate being mixed for 3:2 in mass ratio
In flask, then in flask, add both 9 times of deionized waters of mixture gross mass, be passed through nitrogen as protection gas, startup stirring
Device adds the benzoyl peroxide of potato starch quality 1.7% after stirring mixing 6min at 35 DEG C, raise bath temperature to 65
DEG C stirring reaction 6h after be dried, obtain modified starch；It is that above-mentioned modified starch is dissolved in dimethylformamide by 1:5 by solid-to-liquid ratio
In, add the polyvinyl alcohol of the quality such as modified starch, insulated and stirred 18min at 45 DEG C, prepare slow release base fluid；By above-mentioned standby
Plant source sterilization emulsified dispersed liquid load in there-necked flask with Dropping funnel and agitator, flask is put into 80 DEG C
In oil bath pan, start agitator and be stirred with 150r/min rotating speed, add the glutaraldehyde of dispersion liquid quality 1%, in stirring
During dropwise instill the slow release base fluid of dispersion liquid volume 1/3, filter after continuing insulated and stirred reaction 25min, filtering residue put into
Baking oven, i.e. obtains plant source slow-release bactericide at 75 DEG C after heat preservation and dryness 2h.
The application process of the present invention is: adds clear water in the plant source slow-release bactericide present invention prepared and dilutes 8 times, dress
Enter in agricultural watering can, spray Tanaka with the dose uniformity of every mu of 9L, wherein sprayed once every 6 days, altogether spray 3 times,.
After using, within 4 days, antibacterial burst size reaches 70%, and after 8 days, antibacterial release rate reaches 99%, has splendid slow release effect, and
Can degrade voluntarily after using, without any residual, to human body and environmentally friendly.
Example 3
Weigh 500g Flos Caryophylli, 400g Cortex Cinnamomi respectively and put into pulverizing in jet mill together with 700g Melaleuca Alternifolia fresh braches
30min, the mixture after pulverizing proceeds to, in vapor distillation device, obtain distillate after distillation extraction 7h, then to distillate
3 times of ether oscillation extraction 15min of its volume of middle addition, distillation extraction liquid at 40 DEG C, reclaims ether and obtains plant source sterilization oil；
Crossing 200 mesh standard sieves after weighing 50g walnut shell ball mill grinding, the walnut shell powder after sieving puts into retort, at nitrogen
Under protection, at 400 DEG C, carbonization 3h obtains walnut shell carbon dust, by weight meter weigh 90 parts of above-mentioned plant sources sterilization oil, 8 parts
Sorbitan ester, 5 parts of glycerol, 2 parts of n-butyl alcohol and 100 parts of distilled water mix and put in ultrasonic emulsification disperser, ultrasonic point
After dissipating 3h, obtain plant source sterilization oil Microemulsions For Use；It is that walnut shell carbon dust is joined above-mentioned plant source sterilization oil by 1:8 by solid-to-liquid ratio
In microemulsion, it is placed in high-shear emulsion machine, with 8000r/min rotating speed cutting emulsifying 4h, obtains plant source sterilization emulsifying and divide
Dissipate liquid, standby；Three with agitator and condensing tube are loaded after potato starch and butyl acrylate being mixed for 3:2 in mass ratio
In mouthful flask, then adding both 10 times of deionized waters of mixture gross mass in flask, be passed through nitrogen as protection gas, startup is stirred
Mix the benzoyl peroxide adding potato starch quality 1.8% after device stirs mixing 6min at 40 DEG C, raise bath temperature extremely
It is dried after 70 DEG C of stirring reaction 7h, obtains modified starch；It is that above-mentioned modified starch is dissolved in dimethylformamide by 1:5 by solid-to-liquid ratio
In, add the polyvinyl alcohol of the quality such as modified starch, insulated and stirred 20min at 50 DEG C, prepare slow release base fluid；By above-mentioned standby
Plant source sterilization emulsified dispersed liquid load in there-necked flask with Dropping funnel and agitator, flask is put into 85 DEG C
In oil bath pan, start agitator and be stirred with 200r/min rotating speed, add the glutaraldehyde of dispersion liquid quality 2%, in stirring
During dropwise instill the slow release base fluid of dispersion liquid volume 1/3, filter after continuing insulated and stirred reaction 30min, filtering residue put into
Baking oven, i.e. obtains plant source slow-release bactericide at 80 DEG C after heat preservation and dryness 3h.
The application process of the present invention is: adds clear water in the plant source slow-release bactericide present invention prepared and dilutes 10 times,
Load in agricultural watering can, spray Tanaka with the dose uniformity of every mu of 10L, wherein sprayed once every 7 days, altogether sprinkling 4 times, i.e.
Can.After using, within 5 days, antibacterial burst size reaches 80%, and after 9 days, antibacterial release rate reaches 99.5%, has splendid slow release
Effect, and can degrading voluntarily after using, without any residual, to human body and environmentally friendly.
Claims (1)
1. the preparation method of a plant source slow-release bactericide, it is characterised in that concrete preparation process is:
(1) weigh 400～500g Flos Caryophyllis, 300～400g Cortex Cinnamomi respectively to put together with 600～700g Melaleuca Alternifolia fresh braches
Enter in jet mill pulverize 20～30min, will pulverize after mixture proceed in vapor distillation device, distillation extraction 5～
Obtain distillate after 7h, then in distillate, add its volume 1～3 times of ether oscillation extractions 10～15min, at 35～40 DEG C
Distillation extraction liquid, reclaims ether and obtains plant source sterilization oil；
(2) crossing 200 mesh standard sieves after weighing 40～50g walnut shell ball mill grindings, the walnut shell powder after sieving puts into charcoal
Changing stove, at 300～400 DEG C, carbonization 2～3h obtains walnut shell carbon dust under nitrogen protection, counts by weight and weighs 80～90
Part above-mentioned plant source sterilization oil, 5～8 parts of sorbitan esters, 3～5 parts of glycerol, 1～2 part of n-butyl alcohol and 90～100 parts of distillations
Water mixes and puts in ultrasonic emulsification disperser, after ultrasonic disperse 2～3h, obtains plant source sterilization oil Microemulsions For Use；
(3) by solid-to-liquid ratio be 1:8 walnut shell carbon dust is joined above-mentioned plant source sterilization oil Microemulsions For Use in, be placed on high shear breast
In change machine, with 7000～8000r/min rotating speed cutting emulsifyings 3～4h, obtain plant source sterilization emulsified dispersed liquid, standby；
(4) three mouthfuls with agitator and condensing tube are loaded after potato starch and butyl acrylate being mixed for 3:2 in mass ratio
In flask, then in flask, add both mixture gross mass 8～10 times of deionized waters, be passed through nitrogen as protection gas, startup
Agitator adds potato starch quality 1.5～the benzoyl peroxide of 1.8% after stirring mixing 5～6min at 30～40 DEG C,
Raise bath temperature to be dried to 60～70 DEG C of stirring reactions 5～7h, obtain modified starch；
(5) it is that above-mentioned modified starch is dissolved in dimethylformamide by 1:5 by solid-to-liquid ratio, adds the poly-of the quality such as modified starch
Vinyl alcohol, insulated and stirred 15～20min at 40～50 DEG C, prepare slow release base fluid；
(6) above-mentioned standby plant source sterilization emulsified dispersed liquid is loaded in the there-necked flask with Dropping funnel and agitator,
Flask is put in the oil bath pan of 75～85 DEG C, start agitator and be stirred with 100～200r/min rotating speeds, add dispersion
Liquid quality 1～the glutaraldehyde of 2%, dropwise instill the slow release base fluid of dispersion liquid volume 1/3 during stirring, continues insulation and stirs
Filter after mixing reaction 20～30min, filtering residue is put into baking oven, at 70～80 DEG C, after heat preservation and dryness 2～3h, i.e. obtain plant source delay
Release antibacterial.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610540626.0A CN106212449A (en) | 2016-07-11 | 2016-07-11 | A kind of preparation method of plant source slow-release bactericide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610540626.0A CN106212449A (en) | 2016-07-11 | 2016-07-11 | A kind of preparation method of plant source slow-release bactericide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106212449A true CN106212449A (en) | 2016-12-14 |
Family
ID=57518980
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610540626.0A Pending CN106212449A (en) | 2016-07-11 | 2016-07-11 | A kind of preparation method of plant source slow-release bactericide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106212449A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111602668A (en) * | 2020-03-25 | 2020-09-01 | 福建省农业科学院茶叶研究所 | Green herbicide and use method thereof |
| CN112535173A (en) * | 2020-12-02 | 2021-03-23 | 武汉庆发禾盛农业发展有限公司 | Vegetable seed sterilization and activation treatment agent and preparation method thereof |
| CN113796382A (en) * | 2021-10-23 | 2021-12-17 | 济南天邦化工有限公司 | Granular slow-release bactericide and production process thereof |
| CN113913096A (en) * | 2021-09-24 | 2022-01-11 | 四川汇园宝新材料科技有限公司 | Antiviral coating and preparation method thereof |
| CN116391604A (en) * | 2023-03-30 | 2023-07-07 | 凯盛浩丰农业有限公司 | Soilless cultivation technology for watermelons |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101062878A (en) * | 2006-04-30 | 2007-10-31 | 中国科学院过程工程研究所 | Degradable natural organic matter bundled slow-releasing fertilizer and preparation method and usage thereof |
| CN101445408A (en) * | 2008-11-24 | 2009-06-03 | 天津农学院 | Botanical material coated fertilizer with bactericidal and sustained-release functions |
| CN103979534A (en) * | 2014-05-14 | 2014-08-13 | 石家庄金太阳生物有机肥有限公司 | Active carbon preparing method by adopting walnut shell as raw material and application of the active carbon |
| CN104803746A (en) * | 2015-04-13 | 2015-07-29 | 安徽天叶肥料有限公司 | Carbon-based slow release fertilizer with high phosphorus content and preparation method of fertilizer |
| CN105037015A (en) * | 2015-09-11 | 2015-11-11 | 江苏锦宇环境工程有限公司 | Preparing method for slow-release fertilizer based on nutshell biomass carbon |
| CN105565978A (en) * | 2015-12-23 | 2016-05-11 | 成都新柯力化工科技有限公司 | Polymeric carbon micro-sphere fertilizer sustained-release synergist and method for preparing same |
| CN105694320A (en) * | 2016-03-22 | 2016-06-22 | 华南农业大学 | Plant source extract anti-bacterial preservative film, and preparation method and application thereof |
-
2016
- 2016-07-11 CN CN201610540626.0A patent/CN106212449A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101062878A (en) * | 2006-04-30 | 2007-10-31 | 中国科学院过程工程研究所 | Degradable natural organic matter bundled slow-releasing fertilizer and preparation method and usage thereof |
| CN101445408A (en) * | 2008-11-24 | 2009-06-03 | 天津农学院 | Botanical material coated fertilizer with bactericidal and sustained-release functions |
| CN103979534A (en) * | 2014-05-14 | 2014-08-13 | 石家庄金太阳生物有机肥有限公司 | Active carbon preparing method by adopting walnut shell as raw material and application of the active carbon |
| CN104803746A (en) * | 2015-04-13 | 2015-07-29 | 安徽天叶肥料有限公司 | Carbon-based slow release fertilizer with high phosphorus content and preparation method of fertilizer |
| CN105037015A (en) * | 2015-09-11 | 2015-11-11 | 江苏锦宇环境工程有限公司 | Preparing method for slow-release fertilizer based on nutshell biomass carbon |
| CN105565978A (en) * | 2015-12-23 | 2016-05-11 | 成都新柯力化工科技有限公司 | Polymeric carbon micro-sphere fertilizer sustained-release synergist and method for preparing same |
| CN105694320A (en) * | 2016-03-22 | 2016-06-22 | 华南农业大学 | Plant source extract anti-bacterial preservative film, and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 高兆银 等: "中草药提取物对2 种杧果采后病原菌的抑菌活性", 《热带作物学报》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111602668A (en) * | 2020-03-25 | 2020-09-01 | 福建省农业科学院茶叶研究所 | Green herbicide and use method thereof |
| CN112535173A (en) * | 2020-12-02 | 2021-03-23 | 武汉庆发禾盛农业发展有限公司 | Vegetable seed sterilization and activation treatment agent and preparation method thereof |
| CN113913096A (en) * | 2021-09-24 | 2022-01-11 | 四川汇园宝新材料科技有限公司 | Antiviral coating and preparation method thereof |
| CN113796382A (en) * | 2021-10-23 | 2021-12-17 | 济南天邦化工有限公司 | Granular slow-release bactericide and production process thereof |
| CN116391604A (en) * | 2023-03-30 | 2023-07-07 | 凯盛浩丰农业有限公司 | Soilless cultivation technology for watermelons |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106212449A (en) | A kind of preparation method of plant source slow-release bactericide | |
| CN102976846B (en) | A kind of compound botanical seed coat agent and preparation method thereof | |
| CN103262847B (en) | Biogenic pesticide containing xanthoxylin and abamectin and preparation method thereof | |
| CN105713414A (en) | Insectproof bacteriostatic wood-plastic floor and preparation method thereof | |
| CN102669133A (en) | Seed coating agent for preventing ginger wilt | |
| CN105396165A (en) | Preparation method for environmentally-friendly biomass deodorant | |
| CN102674916A (en) | Bio-organic fertilizer | |
| CN102726459A (en) | Swainsonia salsula Taub. acaricide and its preparation method | |
| CN105087016B (en) | Soil conditioner rich in ocean substance | |
| CN107568256A (en) | The preparation method of one vegetative insecticide | |
| CN106008087A (en) | Microorganism bacterium fertilizer and preparation method thereof | |
| CN104151019A (en) | Vegetable organic fertilizer and preparation method thereof | |
| CN104430574A (en) | Preparation process of compound plant source seed-coating agent | |
| CN107156207A (en) | A kind of vegetable source natural insecticide and preparation method thereof | |
| CN106818946A (en) | Vegetable insecticide and preparation method thereof | |
| CN105994416A (en) | Novel pesticide and production technology thereof | |
| CN106492255A (en) | A kind of preparation method of composite type natural plant deodorizer | |
| CN102805089B (en) | Insect and mite killing composition containing Cyflumetofen and emamectin benzoate | |
| CN101543221A (en) | Sterilizing composite compounded by mancozeb and tea saponin and application thereof | |
| CN108101689A (en) | Activated sludge organic biofertilizer and preparation method thereof | |
| CN106699445A (en) | Organic soil modifier and preparation method thereof | |
| CN103503876B (en) | A kind of brominated worm Benzoylamide and the Pesticidal combination of neires toxin | |
| KR101834749B1 (en) | Manufacturing Method of Animal Feed Additives Comprising Artemisia Capillaris, Houttuynia Cordata, and Perilla Frutescens | |
| CN102125060A (en) | Water dispersible granules for trichoderma and pseudomonas fluorescens bacteria and preparation method thereof | |
| CN107827577A (en) | A kind of salvia plebeia extract prevents the film forming agent of soil-borne disease insect pest |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20161214 |