CN109105367A - A kind of ethyl cinnamate aqueous emulsion and preparation method thereof - Google Patents
A kind of ethyl cinnamate aqueous emulsion and preparation method thereof Download PDFInfo
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- CN109105367A CN109105367A CN201811136668.3A CN201811136668A CN109105367A CN 109105367 A CN109105367 A CN 109105367A CN 201811136668 A CN201811136668 A CN 201811136668A CN 109105367 A CN109105367 A CN 109105367A
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- aqueous emulsion
- ethyl cinnamate
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- ethyl
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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
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/10—Aromatic or araliphatic carboxylic acids, or thio analogues thereof; Derivatives 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
- 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
- A01N25/02—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 liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
Abstract
The invention discloses a kind of ethyl cinnamate aqueous emulsions and preparation method thereof, the aqueous emulsion includes active constituent and auxiliary agent, and active constituent includes ethyl cinnamate, and auxiliary agent includes emulsifier, solvent, thickener and deionized water, wherein, emulsifier is TS-10 and NP-10P；The weight percent of each ingredient of aqueous emulsion: ethyl cinnamate is 6%~30%, solvent is 2%~50%, TS-10 is 0.2%~15%, NP-10P is 0.1~5%, thickener is 0.1%~5%, deionized water is supplemented to 100%；Ethyl cinnamate aqueous emulsion of the invention, production cost is low, and production storage safety and stability, environmental pollution is small, and prevention and treatment nematodiasis effect is good, and especially prevention and treatment pine nematode effect is fabulous.
Description
Technical field
The invention belongs to technical field of pesticide, it is related to a kind of pesticide emulsion in water and preparation method thereof, and in particular to a kind of meat
Ethyl cinnamate aqueous emulsion and preparation method thereof.
Background technique
In recent years, Bursaphelenchus xylophilus (Bursaphelenchus xylophilus) seriously threatens the production of China's agriculture and forestry.From
Between in Nanjing 20 years after being ill occur for nineteen eighty-two, huge loss is caused to China.It not only makes to national economy
At massive losses, natural landscape and ecological environment are also destroyed, China's pine forest resource composition abundant is seriously threatened.Quotient at present
Although the nematicide of product can effectively prevent nematodiasis, but toxicity is big, and nematode drug resistance is also strong, and therefore, exploitation is new
The high-efficiency low-toxicity nematicide of type becomes urgent need, and phytochemical is as natural products, is grinding for new pesticide
Study carefully hot spot.
Ethyl cinnamate belongs to Secondary metabolites, extremely wide in the distribution of nature, a large number of studies show that its
Sterilization, desinsection, anticancer, in terms of have good bioactivity, and its have to environmental hazard it is small, be easy drop
The features such as solution, makes it have boundless development and application prospect.There is researcher to isolate ethyl cinnamate from the naphthalene of mountain, and leads to
It crosses indoor toxicological test and demonstrates it to nematode with good killing effect with loose seedling water culture experiment.
Aqueous emulsion (EW) is also known as emulsifiable concentrate, is dissolved in liquid raw medicine or solid-state raw medicine not soluble in water obtained by organic solvent
Solution not soluble in water, be dispersed in water, a kind of environmentally friendly pesticidal preparations of formation, appearance is opaque white
Color emulsion.Auxiliary agent is added and by special processing technology, is distributed in water phase with making oil phase, forms stable water and milk
Agent system.Oil bead diameter is usually 0.7~20 μm, it is usually desirable to 1.5~3.5 μm.Aqueous emulsion can substantially reduce organic molten
The dosage of agent and emulsifier, it has also become generally acknowledged " environmentally protective preparation " is the substitution most economical safely effectively agent of missible oil product
One of type has the incomparable superiority of missible oil, and also therefore, it has become a new directions of pesticidal preparations development.Water at present
On the one hand the main problem that the development of emulsion faces is the physical stability for improving aqueous emulsion, is on the other hand that preparation process disappears
Time-consuming is long, time-consuming and laborious.
The present inventor carries out numerous studies and test by the recipe determination to ethyl cinnamate aqueous emulsion, has obtained best
Formula and best processing technology, and the drug effect that ethyl cinnamate aqueous emulsion prevents and treats nematodiasis, discovery are probed by pot experiment
It has significant control efficiency to Bursaphelenchus xylophilus.
Summary of the invention
The purpose of the present invention is to provide the cinnamic acids that a kind of safety and environmental protection, storage stablize, are suitble to agriculturally produce and use
Ethyl ester aqueous emulsion.
To achieve the above object, the technical scheme adopted by the invention is that:
A kind of ethyl cinnamate aqueous emulsion, the aqueous emulsion include active constituent and auxiliary agent, and the active constituent includes meat
Ethyl cinnamate, the auxiliary agent include emulsifier, solvent, thickener and deionized water, and the emulsifier is TS-10 and NP-10P.
The weight percent of each ingredient of aqueous emulsion: ethyl cinnamate is 6%~30%, solvent is 2%~50%,
TS-10 is 0.2%~15%, NP-10P is 0.1~5%, thickener is 0.1%~5%, deionized water is supplemented to 100%.
Further, the weight percent of each ingredient of the aqueous emulsion: ethyl cinnamate is 10%~25%, TS-10 is
0.5%~10%, NP-10P is 0.2~3%, solvent is 2%~10%, thickener is 0.1%~4%, deionized water supplement
To 100%.
Further, the solvent is selected from one of toluene, dimethylbenzene, acetone, ethyl alcohol, DMF or a variety of.
Further, the thickener includes in XG, gum arabic, polyvinyl alcohol, bentonite, aluminium-magnesium silicate
It is one or more.
Further, the solvent is dimethylbenzene.
Further, the thickener is gum arabic.
Further, the weight percent of each ingredient of the aqueous emulsion: ethyl cinnamate 10%, TS-10 4%, NP-
10P is 1%, dimethylbenzene 5%, gum arabic 1%, deionized water are supplemented to 100%.
It is a further object of the present invention to provide a kind of preparation methods of ethyl cinnamate aqueous emulsion, comprising the following steps:
(1) ethyl cinnamate raw medicine and the solvent are weighed, being sufficiently stirred is sufficiently mixed raw medicine with solvent, and oil is made
Phase.
(2) emulsifier and thickener and deionized water are mixed in proportion, 1000~10000r/min shear 1~
10min mixes well it, and water phase is made.
(3) mulser is cut by height, is mutually slowly added to oil in water phase at 200~2000r/min, then with 1000~
10000r/min shears 20~65min and ethyl cinnamate aqueous emulsion is made.
Further, preferably, emulsifier and thickener and deionized water are mixed in proportion for the step (2),
2000~8000r/min shears 2~6min, mixes well it, water phase is made.
Further, the step (3) preferably, cuts mulser by height, will be oily mutually slow at 300~1200r/min
It is slow to be added in water phase, then shear 28~55min with 2000~9000r/min and ethyl cinnamate aqueous emulsion is made.
Another object of the present invention is to provide the purposes that the ethyl cinnamate aqueous emulsion is used to prevent and treat nematodiasis, described
Nematodiasis include but is not limited to pine nematode, Meloidogyne incognita, Ditylenchus destructor, Meloidogyne hainanensis, as
Ear beans root-knot nematode.
Compared with prior art, ethyl cinnamate aqueous emulsion of the invention has the beneficial effect that
(1) aqueous emulsion provided by the invention, effective component are ethyl cinnamate, are botanical pesticide, prevent and treat nematodiasis
With good activity, to safety of human and livestock, to environment low toxicity.
(2) aqueous emulsion in the present invention joined emulsifier TS-10 and NP-10P, and the two has ethyl cinnamate very well
Emulsifying effectiveness, oil mutually in water rapidly dispersion and it is colorless and transparent, obtain oil mutually not only well dispersed in water phase, Er Qiewen
It is qualitative, illustrate that both emulsifiers can maintain the physical stability of aqueous emulsion well.
(3) the phosphoric acid esters wedding agents NP-10P that the aqueous emulsion in the present invention joined, due to phosphoric acid ester surface-active
Agent molecule quality is larger, can effectively control the coalescence and flocculation phenomenon of aqueous emulsion, after NP-10P phosphoric acid esters wedding agents are added,
Stability is more preferable at normal temperature for aqueous emulsion.
(4) solvent all has preferable dissolubility to ethyl cinnamate, and dimethylbenzene has cheap, fusing point
It is low, the high advantage of burning point, and dissolubility is good, crystallization is not precipitated for low temperature, and using dimethylbenzene as solvent, dissolubility is good, at low cost.
(5) aqueous emulsion of the invention, production cost is low, and protection effect is good, production storage safety and stability, environmental pollution
It is small.
Detailed description of the invention
Fig. 1 is that 10% ethyl cinnamate aqueous emulsion, 1.8% abamectin aqueous emulsion and clear water handle loose seedling after loose seedling 1d
Wilting degree；
Fig. 2 is the wilting degree that clear water group handles loose seedling after loose seedling 12d；
Fig. 3 is the wilting degree that 10% ethyl cinnamate aqueous emulsion handles loose seedling after loose seedling 12d；
Fig. 4 is the wilting degree that 1.8% abamectin aqueous emulsion handles loose seedling after loose seedling 12d.
Specific embodiment
For the purposes of the present invention, technical solution and advantage are more clearly understood, present invention following specific embodiments into
Row explanation, but the present invention is limited to absolutely not these examples, and the following is only the preferred embodiment of the present invention, is used only for explaining this
Invention, it cannot be construed as a limitation to the scope of the present invention.It should be understood that thing, it is all in spirit of the invention and
Any modifications, equivalent replacements, and improvements etc. done within principle, should all be included in the protection scope of the present invention.Therefore,
The scope of protection of the patent of the present invention should be subject to the appended claims.
Unless otherwise instructed, all percentages of this specification all refer to weight percent.
(1), formulation Example
Embodiment 1:10% ethyl cinnamate aqueous emulsion
Configuration step:
(1) ethyl cinnamate raw medicine, dimethylbenzene, TS-10, NP-10P, gum arabic and deionization have been weighed according to the ratio
Water；
(2) by weighed ethyl cinnamate and dimethylbenzene, being sufficiently stirred is sufficiently mixed raw medicine with solvent, and oil is made
Phase；
(3) TS-10, NP-10P, gum arabic and deionized water are mixed in proportion, shear 3min in 3000r/min,
It is mixed well, water phase is made；
(4) mulser is cut by height, be mutually slowly added to oil in water phase at 800r/min, then sheared with 3000r/min
30min can be prepared by 10% ethyl cinnamate aqueous emulsion.
Embodiment 2:10% ethyl cinnamate aqueous emulsion
Configuration step:
(1) ethyl cinnamate raw medicine, dimethylbenzene, TS-10, NP-10P, gum arabic and deionization have been weighed according to the ratio
Water；
(2) by weighed ethyl cinnamate and dimethylbenzene, being sufficiently stirred is sufficiently mixed raw medicine with solvent, and oil is made
Phase；
(3) TS-10, NP-10P, gum arabic and deionized water are mixed in proportion, shear 3min in 3000r/min,
It is mixed well, water phase is made；
(4) mulser is cut by height, be mutually slowly added to oil in water phase at 800r/min, then sheared with 3000r/min
30min can be prepared by 10% ethyl cinnamate aqueous emulsion.
Embodiment 3:10% ethyl cinnamate aqueous emulsion
Configuration step:
(1) ethyl cinnamate raw medicine, dimethylbenzene, TS-10, NP-10P, gum arabic and deionization have been weighed according to the ratio
Water；
(2) by weighed ethyl cinnamate and dimethylbenzene, being sufficiently stirred is sufficiently mixed raw medicine with solvent, and oil is made
Phase；
(3) TS-10, NP-10P, gum arabic and deionized water are mixed in proportion, shear 3min in 3000r/min,
It is mixed well, water phase is made；
(4) mulser is cut by height, be mutually slowly added to oil in water phase at 800r/min, then sheared with 3000r/min
30min can be prepared by 10% ethyl cinnamate aqueous emulsion.
Embodiment 4:10% ethyl cinnamate aqueous emulsion
Configuration step:
(1) ethyl cinnamate raw medicine, dimethylbenzene, TS-10, NP-10P, gum arabic and deionization have been weighed according to the ratio
Water；
(2) by weighed ethyl cinnamate and dimethylbenzene, being sufficiently stirred is sufficiently mixed raw medicine with solvent, and oil is made
Phase；
(3) TS-10, NP-10P, gum arabic and deionized water are mixed in proportion, shear 3min in 3000r/min,
It is mixed well, water phase is made；
(4) mulser is cut by height, be mutually slowly added to oil in water phase at 800r/min, then sheared with 3000r/min
30min can be prepared by 10% ethyl cinnamate aqueous emulsion.
Embodiment 5:6% ethyl cinnamate aqueous emulsion
Configuration step:
(1) ethyl cinnamate raw medicine, dimethylbenzene, TS-10, NP-10P, gum arabic and deionization have been weighed according to the ratio
Water；
(2) by weighed ethyl cinnamate and dimethylbenzene, being sufficiently stirred is sufficiently mixed raw medicine with solvent, and oil is made
Phase；
(3) TS-10, NP-10P, gum arabic and deionized water are mixed in proportion, shear 5min in 2000r/min,
It is mixed well, water phase is made；
(4) mulser is cut by height, be mutually slowly added to oil in water phase at 1100r/min, then sheared with 3800r/min
40min can be prepared by 6% ethyl cinnamate aqueous emulsion.
Embodiment 6:18% ethyl cinnamate aqueous emulsion
Configuration step:
(1) ethyl cinnamate raw medicine, toluene, TS-10, NP-10P, polyvinyl alcohol and deionized water have been weighed according to the ratio；
(2) by weighed ethyl cinnamate and toluene, being sufficiently stirred is sufficiently mixed raw medicine with solvent, and oily phase is made；
(3) TS-10, NP-10P, polyvinyl alcohol and deionized water are mixed in proportion, shears 6min in 4000r/min, makes
It is mixed well, and water phase is made；
(4) mulser is cut by height, be mutually slowly added to oil in water phase at 1000r/min, then sheared with 5000r/min
36min can be prepared by 18% ethyl cinnamate aqueous emulsion.
Embodiment 7:25% ethyl cinnamate aqueous emulsion
Configuration step:
(1) ethyl cinnamate raw medicine, DMF, TS-10, NP-10P, aluminium-magnesium silicate and deionized water have been weighed according to the ratio；
(2) by weighed ethyl cinnamate and DMF, being sufficiently stirred is sufficiently mixed raw medicine with solvent, and oily phase is made；
(3) TS-10, NP-10P, aluminium-magnesium silicate and deionized water are mixed in proportion, shears 6min in 2500r/min, makes
It is mixed well, and water phase is made；
(4) mulser is cut by height, be mutually slowly added to oil in water phase at 500r/min, then sheared with 6000r/min
45min can be prepared by 25% ethyl cinnamate aqueous emulsion.
Embodiment 8:30% ethyl cinnamate aqueous emulsion
Configuration step:
(1) weighed according to the ratio ethyl cinnamate raw medicine, ethyl alcohol, acetone, TS-10, NP-10P, gum arabic and go from
Sub- water；
(2) by weighed ethyl cinnamate, ethyl alcohol and acetone, being sufficiently stirred is sufficiently mixed raw medicine with solvent, is made
Oily phase；
(3) TS-10, NP-10P, gum arabic and deionized water are mixed in proportion, shear 3min in 5000r/min,
It is mixed well, water phase is made；
(4) mulser is cut by height, be mutually slowly added to oil in water phase at 1200r/min, then sheared with 6000r/min
50min can be prepared by 30% ethyl cinnamate aqueous emulsion.
Embodiment 9:12% ethyl cinnamate
Configuration step:
(1) ethyl cinnamate raw medicine, dimethylbenzene, TS-10, NP-10P, XG and deionized water have been weighed according to the ratio；
(2) by weighed ethyl cinnamate and dimethylbenzene, being sufficiently stirred is sufficiently mixed raw medicine with solvent, and oil is made
Phase；
(3) TS-10, NP-10P, XG and deionized water are mixed in proportion, shears 3min in 4000r/min, makes it sufficiently
It mixes, water phase is made；
(4) mulser is cut by height, be mutually slowly added to oil in water phase at 900r/min, then sheared with 6000r/min
35min can be prepared by 12% ethyl cinnamate aqueous emulsion.
Comparative example 1:10% ethyl cinnamate aqueous emulsion
Configuration step:
(1) weighed according to the ratio ethyl cinnamate raw medicine, dimethylbenzene, TS-10, peaceful cream 33, gum arabic and go from
Sub- water；
(2) by weighed ethyl cinnamate and dimethylbenzene, being sufficiently stirred is sufficiently mixed raw medicine with solvent, and oil is made
Phase；
(3) TS-10, peaceful cream 33, gum arabic and deionized water are mixed in proportion, is sheared in 3000r/min
3min mixes well it, and water phase is made；
(4) mulser is cut by height, be mutually slowly added to oil in water phase at 800r/min, then sheared with 3000r/min
30min can be prepared by 10% ethyl cinnamate aqueous emulsion.
Comparative example 2:10% ethyl cinnamate aqueous emulsion
Configuration step:
(1) weighed according to the ratio ethyl cinnamate raw medicine, dimethylbenzene, 0202C, peaceful cream 33, gum arabic and go from
Sub- water；
(2) by weighed ethyl cinnamate and dimethylbenzene, being sufficiently stirred is sufficiently mixed raw medicine with solvent, and oil is made
Phase；
(3) 0202C, peaceful cream 33, gum arabic and deionized water are mixed in proportion, is sheared in 3000r/min
3min mixes well it, and water phase is made；
(4) mulser is cut by height, be mutually slowly added to oil in water phase at 800r/min, then sheared with 3000r/min
30min can be prepared by 10% ethyl cinnamate aqueous emulsion.
Comparative example 3:10% ethyl cinnamate aqueous emulsion
Configuration step:
(1) ethyl cinnamate raw medicine, dimethylbenzene, agriculture breast 600#, trilaurin polyoxyethylene have been weighed according to the ratio
Ether, gum arabic and deionized water；
(2) by weighed ethyl cinnamate and dimethylbenzene, being sufficiently stirred is sufficiently mixed raw medicine with solvent, and oil is made
Phase；
(3) agriculture breast 600#, trilaurin polyoxyethylene ether, gum arabic and deionized water are mixed in proportion
It closes, shears 6min in 5000r/min, mix well it, water phase is made；
(4) mulser is cut by height, be mutually slowly added to oil in water phase at 900r/min, then sheared with 6000r/min
45min can be prepared by 10% ethyl cinnamate aqueous emulsion.
Comparative example 4:10% ethyl cinnamate aqueous emulsion
Configuration step:
(1) ethyl cinnamate raw medicine, dimethylbenzene, APES sulfosuccinate, mountain have been weighed according to the ratio
Pears alcohol polyoxyethylene ether, gum arabic and deionized water；
(2) by weighed ethyl cinnamate and dimethylbenzene, being sufficiently stirred is sufficiently mixed raw medicine with solvent, and oil is made
Phase；
(3) by APES sulfosuccinate, sorbitol polyoxyethylene ether, gum arabic and deionization
Water mixes in proportion, shears 6min in 5000r/min, mixes well it, water phase is made；
(4) mulser is cut by height, be mutually slowly added to oil in water phase at 600r/min, then sheared with 6000r/min
55min can be prepared by 10% ethyl cinnamate aqueous emulsion.
(2), ethyl cinnamate aqueous emulsion performance measurement
1, ethyl cinnamate aqueous emulsion physicochemical property measures
With test group: embodiment 1-4, control group: comparative example 1-4, aqueous emulsion obtained is sample respectively,
Measure ethyl cinnamate aqueous emulsion physicochemical property of the present invention.
(1) appearance: having seen whether that water and oil are precipitated, and whether observation aqueous emulsion is uniform, mobility quality.
(2) pH is measured: lg sample is weighed in 100mL beaker, 100mL water is added, is vigorously stirred 1min, stands 1min,
Measure its pH value (referring to GB/T 1601-1993).
(3) dispersibility measurement: dispersed measurement is carried out according to GB/T 32775-2016, water (hardness is added in aqueous emulsion
The ability that automatic dispersion and emulsion forms emulsion when in 342mg/L) can be divided into 4 grades, and excellent: instilling rear in water is in that cloud disperses shape
At in emulsion dispersion process without visible particle；It is good: to be dispersed with particles sink automatically but to can disperse or be sink to substantially before bottom
Comparatively fast upper it can expand dispersion behind bottom；In: part could disperse after being dispersed with particles sink automatically and need to rocking or be inverted；Difference: cannot
Automatic dispersion, is in granular form or cotton-shaped sinking, could disperse after acutely rocking.
(4) measurement of dilution stability: the sample sheared carries out lotion according to 2.4 in GB/T 1603-2001 immediately
The measurement of dilution stability.In 250mL beaker, 100mL30 DEG C of ± 2 DEG C of standard hard waters are added, draw appropriate cream with pipette
Agent sample is slowly added into hard water (by diluted concentration as defined in each product) in the case where being stirred continuously, it is made to be made into 100mL
Emulsion.After adding emulsion, continues to stir 30s with the speed of 2~3r/s, emulsion is moved to the 100mL of cleaning, drying immediately
In graduated cylinder, and graduated cylinder is placed in water bath with thermostatic control, within the scope of 30 DEG C ± 2 DEG C, stands 1h, take out, observe emulsion separation feelings
Condition then determines stability of emulsion qualification without oil slick, heavy oil and Precipitation such as in graduated cylinder.
(5) it pourability: is carried out by GB/T 31737-2015.Enough samples are mixed, are in time placed in a part therein
It in the graduated cylinder weighed (including plug), is attached at the 8/10 of graduated cylinder volume, stoppers grinding port plug, weigh, place the regular hour
(as 24 hours).Plug is opened, graduated cylinder is rotated 135 ° by stand up position, topples over 60s, then be inverted 60s, again weighing tank and plug.
The water that will be equivalent to 80% graduated cylinder volume (in (20 DEG C) graduated cylinder of falling people, stoppers grinding port plug, graduated cylinder is overturned 10 times
Afterwards, content is toppled over by aforesaid operations, third time weighs graduated cylinder and plug.
The residue W2 after residue W1 (%) and washing after toppling over is calculated by formula (2.5) and formula (2.6) respectively:
In formula:
m1The quality of-graduated cylinder, grinding port plug and sample, unit are gram (g)；
m2- topple over after, the quality of graduated cylinder, grinding port plug and residue, unit be gram (g)；
m3After-washing, the quality of graduated cylinder, grinding port plug and residue, unit is gram (g)；
m0Quality after-graduated cylinder, grinding port plug constant, unit are gram (g).
(6) it persistent foamability: is tested according to GB/T 28137-2011.25mL is had into plug graduated cylinder and adds standard hard water extremely
At 18mL graduation mark, graduated cylinder is set on balance, being weighed into sample l.0g, stiffened water is covered at away from graduated cylinder plug bottom 9cm graduation mark
Plug is turned upside down 30 times centered on graduated cylinder midpoint, each 2s.It is placed on testing stand and stands 1min, record foam volume.
(7) low-temperature stability: cold storage is carried out according in GB/T19137-2,003 2.2.Sample is placed in 100mL beaker,
It is cooled to 0 DEG C ± 2 DEG C in refrigerator, keeps 1h, is during which stirred 1 time, each 15s every 15min, whether there is or not changes for observation appearance
Change.Beaker is put back into refrigerator, continues to place 7d at 0 DEG C ± 2 DEG C, takes out beaker after 7d, restore to room temperature, test its physical property
Whether index complies with standard.
(8) it thermal stability: is carried out by " liquid preparation " in GB/T 19136-2003.Emulsifier is put into 54 DEG C of insulating boxs
Middle 30d observes its stability.Ethyl cinnamate mass fraction should be not less than ethyl cinnamate mass fraction before storing after heat storage
95%.
6%~30% ethyl cinnamate aqueous emulsion optimization of C/C composites physicochemical property standard is shown in Table 1
Embodiment 1-4 all properties measurement result is shown in Table 2:
Comparative example 1-4 all properties measurement result is shown in Table 3:
1 ethyl cinnamate aqueous emulsion optimization of C/C composites physical and chemical index of table
The ethyl cinnamate aqueous emulsion physicochemical property measurement result of 2 embodiment 1-4 of table
The ethyl cinnamate aqueous emulsion physicochemical property measurement result of 3 comparative example 1-4 of table
The standard of reference table 1, from the measurement result of table 2 it is found that the 10% ethyl cinnamate aqueous emulsion of embodiment 1-4 is physical and chemical
Performance is qualified, and stability is good；From the point of view of the result that each physicochemical property of embodiment 1-4 measures, in dispersibility measurement, implement
The good dispersion of example 1 and embodiment 4 is in embodiment 2 and embodiment 3；In pourability measurement, embodiment 1 preferably, is followed by implemented
Example 3, illustrate to be easy to pour out and it is less it is glutinous on the wall, be conducive to the effective active composition for making full use of medicament；Thermal stability
Measurement in, it is embodiment 1 again that the minimum fact of resolution ratio, which applies example 4, followed by embodiment 2, and highest is embodiment 3；It is comprehensive
Upper described, all physicochemical properties are optimal, stability most preferably embodiment 4.
The standard of reference table 1, contrast table 2, from the measurement result of table 3 it is found that the 10% ethyl cinnamate water of comparative example 1-4
Emulsion physicochemical property, comparative example 1-2 is qualified, and the dispersibility of comparative example 3 and comparison 4 is middle rank, and emulsifier part disperses automatically
It could disperse after having particles sink that need to rock or be inverted；The dilution stability (100 times) of comparative example 4 is unqualified to be had under oil droplet shape
Heavy, the thermal stability of comparative example 3 has layering to occur, resolution ratio highest, the resolution ratio of thermal stability determination, and comparative example 1-4 is high
In embodiment 1-4；In conclusion the physicochemical property and stability of comparative example 1-2 is better than comparative example 3-4, still in comparative example
The physicochemical property and stability of comparative example 1-4 is poorer than embodiment 1-4.
To sum up, 4 physicochemical property of embodiment and stability are preferably optimal, illustrate that embodiment 4 is optimization formula, and TS-
10 compare other conventional emulsifiers with NP-10P emulsifier, good to the emulsifying effectiveness of ethyl cinnamate aqueous emulsion, are conducive to cortex cinnamomi
The stability of acetoacetic ester aqueous emulsion.
2, virulence test of the ethyl cinnamate water and milk to Bursaphelenchus xylophilus
Bursaphelenchus xylophilus cytotoxicity is measured using dipping bioassay.The cinnamic acid second of embodiment 4-7 is weighed respectively
Ester aqueous emulsion sample 0.1g is sufficiently stirred after 5mL acetone is added and is completely dissolved in sample in acetone, then is settled to sterile water
100mL, be made into concentration be 1000mg/L mother liquor, content of acetone be 5% (V/V), then respectively compound concentration be 5mg/L,
2mL medical fluid is added in the culture dish that diameter is 3cm, then passes through shifting by the solution of 10mg/L, 20mg/L, 40mg/L, 80mg/L
Liquid rifle draws 40~60 2 age nematodes under stereoscope, and is added in the culture dish equipped with medical fluid, the perfect number under stereoscope
Outlet borer population simultaneously records, and is not necessarily to feeding；Each processing sets 3 repetitions.It is control (CK) with clear water (containing 5% acetone), with cortex cinnamomi
Acetoacetic ester raw medicine and the former medicine of AVM are positive control.After processing for 24 hours, nematode survival number is checked with stereomicroscope.It is logical
It crosses formula (2.7) and calculates the death rate, carry out virulence regression equation, correlation coefficient r and LC with data processing software SPSS50Meter
It calculates.By comparing LC50, compare raw medicine and aqueous emulsion to the cytotoxicity of nematode.The processing of data uses Excel software, virulence
Regression equation calculation uses SPSS software, and test result is shown in Table 4.
Virulence test of the 4 ethyl cinnamate water and milk of table to Bursaphelenchus xylophilus
By the virulence test result of table 4 it is found that the LC of ethyl cinnamate raw medicine50For 32.25 μ g/mL, and manufactured 10%
Ethyl cinnamate aqueous emulsion LC50For 25.40 μ g/mL, 6% ethyl cinnamate aqueous emulsion LC50It is 28.57,18% ethyl cinnamate
Aqueous emulsion LC50It is 25.16,25% ethyl cinnamate aqueous emulsion LC50It is 24.53, the results showed that, ethyl cinnamate water and milk is made
Opposite raw medicine is more preferable to the cytotoxicity of Bursaphelenchus xylophilus after agent, and the content of aqueous emulsion effective component ethyl cinnamate is higher, right
The cytotoxicity of Bursaphelenchus xylophilus is better.
3, pot experiment of the ethyl cinnamate water and milk to Bursaphelenchus xylophilus
(1) for trying nematode
The Bursaphelenchus xylophilus sterilized is seeded in the culture medium for covering with a mao spore (Pestalotia sp.), in constant temperature incubation
7d is cultivated in case, until culture medium color all becomes brown, then nematode covers with plate, and nematode is placed in 4 DEG C of preservations.It uses
When, with sterile water washing plate for several times, 2 arrive 3mL every time, collect flushing liquor and be put into culture medium, each plate it is flushable go out about
5000 nematodes.
(2) Song Miao acquisition and culture
The healthy black pine (Pinus thunbergii Parl) of purchase height about 80cm or so, plantation are 20cm in diameter
In plastic tub, and with laterite culture.
(3) Song Miao is inoculated with
A side shoot for choosing loose seedling, is splayed at from loose seedling major branch about 5cm with scalpel and cuts off pine branch, cuts breaking part
Up, and in wound pine branch is snarled with preservative film, puts on the plastic tube of length about 8cm, tighten plastic tube and pine with cord
Scion grafting mouth, after snarl close joint interface with preservative film again, from nozzle be inoculated with nematode, 1000 Bursaphelenchus xylophiluses of every scion grafting kind.Again with wet
The absorbent cotton of profit clogs nozzle, in order to make nematode more successfully infect pine branch, needs periodically to soak absorbent cotton, to maintain latex
Humidity in managing.
Pot experiment is carried out with the 10% ethyl cinnamate aqueous emulsion of embodiment 4-7.Every processing sets 3 repetitions.In loose seedling
After inoculation nematode 24 hours, compound concentration is the 10% ethyl cinnamate aqueous emulsion of 250 μ g/mL, is then packed into medical fluid and sprays
Bottle, after being uniformly sprayed on inoculation nematode 24 hours in the loose seedling of examination health." CK+ worm " control (CK is clear water) and sun are set respectively
Property control (abamectin solution).
(4) symptom is observed
7d and 15d respectively observes primary loose seedling external symptom after inoculation, then carries out the calculating of loose seedling severity Scaling and index,
Severity Scaling is as follows:
0 grade: needle is green, and loose seedling is normal；
1 grade: Song Miao upper 1/4 or less needle jaundice；
2 grades: Song Miao upper 1/4~3/4 needle jaundice；
3 grades: Song Miao upper 3/4 or more needle jaundice, 1/2 or less needle are withered；
4 grades: Song Miao upper 1/2 or more needle is withered, and Song Miao is dying or dead.
Disease-sensitive index is calculated by formula (2.8).And the disease severity respectively handled.
Wherein: XiFor the loose seedling number of each sick grade, aiFor each sick grade, amaxFor highest disease grade (being herein 4 grades).
(5) loose seedling resin flux measures fixed
9d after inoculation digs an about 0.25cm in loose seedling major branch lower part with scalpel2Xylem is seen in duck eye, hole deeply, after for 24 hours
Observe each loose seedling resin flux amount.
Resin flux amount grade scale is shown in:
1 grade: rosin is flowed down from aperture, and there are many discharge；
2 grades: rosin flows out aperture, but is less than level-one；
3 grades: rosin is only accumulated in aperture lower edge；
4 grades: rosin is exuded on circular hole wall；
5 grades: without resin on hole wall.
(6) test result is shown in Table 5, table 6 and attached drawing 1-4
Influence of the 5 10% ethyl cinnamate aqueous emulsion of table to pine nematode disease index
As shown in Table 5,10% ethyl cinnamate aqueous emulsion can effectively prevent pine nematode, water planting potting pine in process chamber
After seedling 7d, the loose seedling disease index of 10% ethyl cinnamate aqueous emulsion processing group is 0.08, the processing of 6% ethyl cinnamate aqueous emulsion
The loose seedling disease index of group is 0.11, and the loose seedling disease index of 18% ethyl cinnamate aqueous emulsion processing group is 0.09,25% meat
The loose seedling disease index of ethyl cinnamate aqueous emulsion processing group is 0.07, and avermectin processing group disease index is 0.04, and is compareed
The disease index of group (CK) is 0.28, and control group needle starts to turn yellow.In process chamber after water planting potting pine seedling 15d, 10% cortex cinnamomi
The loose seedling disease index of acetoacetic ester aqueous emulsion processing group is 0.22, and the loose seedling diseases feelings of 6% ethyl cinnamate aqueous emulsion processing group refer to
Number is 0.31, and the loose seedling disease index of 18% ethyl cinnamate aqueous emulsion processing group is 0.25,25% ethyl cinnamate aqueous emulsion
The loose seedling disease index of processing group is 0.19, and avermectin processing group disease index is 0.09, and control group disease index is 0.54,
Know that control group aggravation, loose seedling Huang needle increase at this time, part branch starts to wither, and 10% ethyl cinnamate aqueous emulsion
Then change less with 1.8% abamectin aqueous emulsion processing group, ethyl cinnamate aqueous emulsion is made, Bursaphelenchus xylophilus is prevented later
Effect is slightly less than 1.8% abamectin aqueous emulsion, and the content of aqueous emulsion effective component ethyl cinnamate is higher, prevents Bursaphelenchus xylophilus
Effect is better.
6 10% ethyl cinnamate aqueous emulsion of table is on the other influence of pine nematode potting pine seedling resin flux magnitude
After Song Miao is infected, because of the infringement of nematode, loose seedling resin flux amount can be reduced slowly until last stop secretion tree
Rouge, loose seedling resin flux magnitude is not higher, and resin flux amount is fewer, then pine nematode is more serious.As can be seen from Table 6,15d after inoculation,
10% ethyl cinnamate aqueous emulsion, 1.8% abamectin aqueous emulsion and CK group do not stop flowing ester.Wherein 10% cinnamic acid second
Loose seedling resin flux magnitude is not no more than 3 after ester aqueous emulsion and the processing of 1.8% abamectin aqueous emulsion, respectively 3.00 ± 0.00 Hes
2.33 ± 0.33, illustrate that 10% ethyl cinnamate aqueous emulsion handles Song Miaohou, nematodiasis can be effectively prevented, enable loose seedling just
It is frequently grown.
Fig. 1 is that 10% ethyl cinnamate aqueous emulsion, 1.8% abamectin aqueous emulsion and clear water handle loose seedling after loose seedling 1d
Wilting degree, it will be seen from figure 1 that the loose seedling Huang needle no significant difference of each potting；Fig. 2 is that clear water handles pine after loose seedling 12d
The wilting degree of seedling, as can be seen from Figure 2, the loose seedling Huang needle no significant difference between each potting, but opposite Fig. 1 Huang needle is on the high side；Fig. 3
The wilting degree of loose seedling after loose seedling 12d is handled for 10% ethyl cinnamate aqueous emulsion, as can be seen from Figure 3 the Song Miaohuang between each potting
Needle no significant difference, but opposite Fig. 2 Huang needle is on the low side；Fig. 4 is that 1.8% abamectin aqueous emulsion handles loose seedling after loose seedling 12d
Wilting degree, the loose seedling Huang needle no significant difference between each potting as seen from Figure 4, but opposite Fig. 2 Huang needle is on the low side.
Whole result shows that 10% ethyl cinnamate aqueous emulsion can effectively prevent pine nematode, and preventive effect is obvious.
Based on the above description of the preferred embodiments of the present invention, through the above description, related personnel completely can be with
Without departing from the scope of the technological thought of the present invention', various changes and amendments are carried out.The technical scope of this invention
It is not limited to the contents of the specification, it is necessary to determine the technical scope according to the scope of the claims.
Claims (10)
1. a kind of ethyl cinnamate aqueous emulsion, which is characterized in that the aqueous emulsion includes active constituent and auxiliary agent, the activity at
Point include ethyl cinnamate, the auxiliary agent includes emulsifier, solvent, thickener and deionized water, the emulsifier be TS-10 and
NP-10P；
The weight percent of each ingredient of aqueous emulsion: ethyl cinnamate is 6%~30%, solvent is 2%~50%, TS-10
For 0.2%~15%, NP-10P be 0.1~5%, thickener is 0.1%~5%, deionized water is supplemented to 100%.
2. a kind of ethyl cinnamate aqueous emulsion according to claim 1, it is characterised in that: the weight of each ingredient of aqueous emulsion
Measure percentage: ethyl cinnamate is 10%~25%, TS-10 is 0.5%~10%, NP-10P is 0.2~3%, solvent 2%
~10%, thickener is that 0.1%~4%, deionized water is supplemented to 100%.
3. a kind of ethyl cinnamate aqueous emulsion according to claim 1, it is characterised in that: the solvent is selected from toluene, two
One of toluene, acetone, ethyl alcohol, DMF or a variety of；The thickener includes selected from XG, gum arabic, polyvinyl alcohol, swollen
One of profit soil, aluminium-magnesium silicate are a variety of.
4. a kind of ethyl cinnamate aqueous emulsion according to claim 4 and preparation method thereof, it is characterised in that: the solvent
For dimethylbenzene；The thickener is gum arabic.
5. a kind of ethyl cinnamate aqueous emulsion according to claim 1, it is characterised in that: the weight of each ingredient of aqueous emulsion
Measure percentage: ethyl cinnamate 10%, TS-10 4%, NP-10P 1%, dimethylbenzene 5%, gum arabic 1%,
Deionized water is supplemented to 100%.
6. ethyl cinnamate aqueous emulsion described in -5 any claims is used to prevent and treat the use of nematodiasis according to claim 1
On the way.
7. purposes according to claim 6, it is characterised in that: the nematodiasis includes pine nematode, Root Knot
Nematode, Ditylenchus destructor, Meloidogyne hainanensis, Meloidogyne enterolobii.
8. a kind of preparation method of ethyl cinnamate aqueous emulsion as claimed in any one of claims 1-5, feature
It is, comprising the following steps:
(1) ethyl cinnamate raw medicine and the solvent are weighed, being sufficiently stirred is sufficiently mixed raw medicine with solvent, and oily phase is made.
(2) emulsifier and thickener and deionized water are mixed in proportion, shears 1~10min in 1000~10000r/min, makes
It is mixed well, and water phase is made.
(3) mulser is cut by height, is mutually slowly added to oil in water phase at 200~2000r/min, then with 1000~
10000r/min shears 20~65min and ethyl cinnamate aqueous emulsion is made.
9. the preparation method of ethyl cinnamate aqueous emulsion according to claim 8, which is characterized in that in the step (2),
Emulsifier and thickener and deionized water are mixed in proportion, 2~6min is sheared in 2000~8000r/min, keeps it sufficiently mixed
It is even, water phase is made.
10. the preparation method of ethyl cinnamate aqueous emulsion according to claim 9, which is characterized in that the step (3)
In, mulser is cut by height, is mutually slowly added to oil in water phase at 300~1200r/min, then with 2000~9000r/min
It shears 28~55min and ethyl cinnamate aqueous emulsion is made.
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| CN1149417A (en) * | 1995-09-12 | 1997-05-14 | 韩国科学技术研究院 | Cultivating method for bean sprouts and mung bean sprouts |
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2018
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|---|---|---|---|---|
| US5180586A (en) * | 1989-10-19 | 1993-01-19 | Takasago International Corporation | Acaricidal composition |
| CN1149417A (en) * | 1995-09-12 | 1997-05-14 | 韩国科学技术研究院 | Cultivating method for bean sprouts and mung bean sprouts |
| CN1350782A (en) * | 2000-10-27 | 2002-05-29 | 孙国兴 | Efficient killing attractant for imaginal ballworm and its special device |
| KR20090102136A (en) * | 2008-03-25 | 2009-09-30 | 주식회사 내츄로바이오텍 | Compositions for controlling nematodes and eggs comprising plant extracts as effective components |
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