CN109757478A - A kind of dicamba type missible oil and preparation method thereof - Google Patents
A kind of dicamba type missible oil and preparation method thereof Download PDFInfo
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- CN109757478A CN109757478A CN201711096023.7A CN201711096023A CN109757478A CN 109757478 A CN109757478 A CN 109757478A CN 201711096023 A CN201711096023 A CN 201711096023A CN 109757478 A CN109757478 A CN 109757478A
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- dicamba
- ester
- missible oil
- solvent
- emulsifier
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Abstract
The present invention provides a kind of dicamba type missible oil, comprising: dicamba ester, emulsifier and solvent；The dicamba ester is dicamba methyl esters, dicamba ethyl ester, dicamba butyl ester, dicamba isobutyl ester, dicamba monooctyl ester or the different monooctyl ester of dicamba.The present invention emulsifier and solvent suitable by selection, dicamba missible oil dosage form is prepared, the blank for having filled up dicamba missible oil dosage form solves the problems, such as that dicamba drug effect is poor, and drug effect is compared with aqua, it can be improved 15%~20%, penetration is improved, drift is effectively reduced, compared with aqua, anti-drift ability improves 20%~30%, is suitble to large-scale promotion application.
Description
Technical field
The present invention relates to technical field of pesticide more particularly to a kind of dicamba type missible oil and preparation method thereof.
Background technique
Dicamba (dicamba) also known as Dicamba, the chloro- O-Anisic Acid of entitled 3, the 6- bis- of Science of Chemistry belong to styrax
The herbicide of acid system is a kind of less toxic, efficient, wide spectrum herbicide, has to annual and perennial broadleaf weed and significantly prevent and kill off
Effect, and it is safer to gramineous crops such as wheat, corn, millet, rice.With the disabling of metsulfuron-methyl and chlorsulfuron preparation
With limit the use of, safety, human health and the superweed problem that glyphosate causes increasingly highlight, and dicamba is high as a tradition
Effective herbicide is noticeable, while resistance to dicamba genetically modified crops are continually developed, and dicamba welcomes new opportunity to develop.
Currently used dicamba dosage form is aqua, but aqua has drift seriously, generation phytotoxicity, the defect of drug effect difference,
Increasingly it is restricted.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is that provide a kind of dicamba type missible oil and preparation method thereof,
The dicamba missible oil drug effect with higher and penetration of preparation, are effectively reduced drift.
In order to solve the above technical problems, the present invention provides a kind of dicamba type missible oil, comprising:
Dicamba ester, emulsifier and solvent；
The dicamba ester is dicamba methyl esters, and dicamba ethyl ester, dicamba butyl ester, dicamba isobutyl ester, dicamba is pungent
Ester or the different monooctyl ester of dicamba.
The present invention is with dicamba methyl esters, dicamba ethyl ester, dicamba butyl ester, dicamba isobutyl ester, dicamba monooctyl ester or wheat
It is that raw material selects emulsifier and solvent appropriate, be finally prepared preferably using dicamba monooctyl ester as raw material that grass, which fears different monooctyl ester,
Dicamba missible oil dosage form.
Wherein, the content of dicamba ester is preferably 10wt%~70wt%, more preferable 30wt%~50wt%, in the present invention
Certain specific embodiments in, content 40wt%.
The content of the emulsifier is preferably 5wt%~20wt%, more preferable 10wt%~12wt%, in certain of the invention
In a little specific embodiments, content 10%.
The emulsifier preferably includes any one in calcium dodecyl benzene sulfonate and neopelex or two
Kind and phenethyl phenol polyoxyethylene poly-oxygen propylene aether, phenethyl phenol polyethenoxy ether, phenethyl phenol polyethenoxy ether, nonyl
Phenol brings up Polyoxyalkylene ethers, Ben-zylphenol Polyoxyethyl Ether, any one in fatty alcohol polyoxyethylene ether and castor oil polyoxyethylene ether
Or it is a variety of.More preferable calcium dodecyl benzene sulfonate and phenethyl phenol polyethenoxy ether.
It further include the solvent of surplus.
The solvent is environment-friendly type solvent, preferably any one in solvent naphtha, vegetable oil, soybean oil and methyl oleate
Or it is a variety of.
Preferred solvent oil 150# or solvent naphtha 200#.
The present invention also provides the preparation methods of above-mentioned dicamba type missible oil, comprising the following steps:
Dicamba ester is mixed with emulsifier and solvent, in 15~60 DEG C of 15~60min of stirring, obtains dicamba type cream
Oil.
The temperature of above-mentioned stirring is more preferably 35~45 DEG C.
In the industrial production, emulsifier and solvent are added directly into the dicamba ester being prepared, stirring can be with
Realize continuous production, and process route is simple, equipment is simple.
Compared with prior art, the present invention provides a kind of dicamba type missible oil, comprising: dicamba ester, emulsifier and molten
Agent；The dicamba ester is dicamba methyl esters, dicamba ethyl ester, dicamba butyl ester, dicamba isobutyl ester, dicamba monooctyl ester or wheat
Grass fears different monooctyl ester.The present invention emulsifier and solvent suitable by selection, are prepared dicamba missible oil dosage form, have filled up wheat straw
The blank for fearing missible oil dosage form, solves the problems, such as that dicamba drug effect is poor, drug effect can be improved 15%~20% compared with aqua, mention
High penetration, effectively reduces drift, compared with aqua, anti-drift ability improves 20%~30%, suitable to push away on a large scale
Wide application.
Detailed description of the invention
Fig. 1 is that the arrangement of testing site Caro rice spy's paper card in embodiment 9 is schemed on the spot；
Fig. 2 is droplet size distribution map in embodiment 9.
Specific embodiment
In order to further illustrate the present invention, below with reference to embodiment to dicamba type missible oil provided by the invention and its preparation
Method is described in detail.
Embodiment 1
The different monooctyl ester crude oil of the dicamba of 4.21T 95% is added to 10KL to prepare in kettle, 4.69T solvent naphtha 150# is added,
0.5T calcium dodecyl benzene sulfonate, 0.6T phenethyl phenol polyethenoxy ether, 15~25 DEG C of holding temperature, insulated and stirred 40Min is obtained
To the different monooctyl ester missible oil of 40% dicamba.
Embodiment 2
The different monooctyl ester crude oil of the dicamba of 1.053T 95% is added to 10KL to prepare in kettle, 7.947T vegetable oil is added,
0.4T calcium dodecyl benzene sulfonate, 0.6T phenethyl phenol polyethenoxy ether, 35~45 DEG C of holding temperature, insulated and stirred 35Min is obtained
To the different monooctyl ester missible oil of 10% dicamba.
Embodiment 3
The dicamba methyl esters crude oil of 7.368T 95% is added to 10KL to prepare in kettle, 1.132T solvent naphtha 200 is added,
0.7T calcium dodecyl benzene sulfonate, 0.8T castor oil polyoxyethylene ether, 35~45 DEG C of holding temperature, insulated and stirred 35Min is obtained
70% dicamba methyl esters missible oil.
Embodiment 4
By the dicamba butyl ester crude oil of 3.158T 95% be added to 10KL prepare kettle in, be added 3.842T vegetable oil and
2.0T solvent naphtha 150,0.3T calcium dodecyl benzene sulfonate, 0.7T fatty alcohol polyoxyethylene ether, 35~45 DEG C of holding temperature, heat preservation
35Min is stirred, 30% dicamba butyl ester missible oil is obtained.
Embodiment 5
By the dicamba isobutyl ester crude oil of 3.158T 95% be added to 10KL prepare kettle in, be added 2.842T vegetable oil and
3.0T solvent naphtha 150,0.4T calcium dodecyl benzene sulfonate, 0.6T fatty alcohol polyoxyethylene ether, 35~45 DEG C of holding temperature, heat preservation
35Min is stirred, 30% dicamba isobutyl emulsifiable concentrate is obtained.
Embodiment 6
The dicamba n-octyl crude oil of 4.21T 95% is added to 10KL to prepare in kettle, 4.79T solvent naphtha 150# is added,
0.3T calcium dodecyl benzene sulfonate, 0.7T phenethyl phenol polyethenoxy ether, 35~45 DEG C of holding temperature, insulated and stirred 40Min is obtained
To 40% dicamba n-octyl missible oil.
Embodiment 7
By the dicamba ethyl ester crude oil of 4.21T 95% be added to 10KL prepare kettle in, be added 1.79T solvent naphtha 150# and
3T vegetable oil, 0.3T calcium dodecyl benzene sulfonate, 0.7T phenethyl phenol polyethenoxy ether and 0.1T phenethyl phenol polyoxyethylene
Polyethenoxy ether, obtains 40% dicamba ethyl ester missible oil by 35~45 DEG C of holding temperature, insulated and stirred 40Min.
8 pharmacodynamic test of embodiment:
1. experimental condition
1.1 for studying object as corn, and kind is safe No. 14 beautiful.
Purslane (Portulaca oleracea L.), acalypha copperleaf (Acalypha australis L.) etc. are annual wealthy
Leaf weeds.
1.2 be experimental field Shajiang black soil, PH 7.2, the content of organic matter 1.5%.It sows, plants on July 31st, 2016
Training density is 4000 plants/acre.
1.3 unused herbicides.
2 test medicines
Respectively by the different monooctyl ester EC of 40% dicamba prepared in the above embodiments, the different monooctyl ester EC of 10% dicamba, 40% wheat straw
Fear the dicamba butyl ester of n-octyl EC, 30% dicamba isobutyl ester EC, 30% EC, 70% dicamba methyl esters EC, 40% dicamba second
Ester EC.
2.1 comparison medicament
480g/L dicamba dimethylamine salt SL, Shandong Weifang Rainbow Chemical Co., Ltd..
2.2 reagent agent experimental designs
1 dicamba esters EC Control Weeds in Maize Field field control effectiveness test of table designs table
2.3 plot areas and repetition
Plot area: 20 square metres
Number of repetition: 2 repetitions
2.4 application method
2.4.1 application method
Summer jade seedling stage cauline leaf sprinkling.
2.4.2 spraying equipment
Singapore's benefit agriculture HD400 type knapsack sprayer
2.4.3 spraying time and number
Spraying time is on August 23rd, 2016.The time of infertility Shi Yici herbicide.
2.4.4 usage amount
600 liter/hectare of spouting liquid
2.4 prevention and treatment disease pests and non-target weeds medicament data
Without spraying other pesticides in experimental period.
3 investigation, record and measurement method
3.1 meteorological and field management data
3.1.1 meteorological data
It is August 23 days, fine, 23-30 DEG C of temperature, relative humidity 84-94%, 3-4 grades of south wind.
3.1.2 field management data
Generally conventional management.Without irrigation.
3.2 weedy rices
3.2.1 control time and number
The time of infertility is investigated 5 times altogether.I.e. handle after 15 days, 30 days, 45 days and harvest before.It is range estimation before harvest.
3.2.2 investigation method
Strain preventive effect is investigated using four point samplings.Every 0.25 square metre of investigation area.It combines within the 60th day after medicine and adjusts
Look into the fresh weight of weeds.And the investigation of weeds radix uses 9 point sampling of W type, radix table is as shown in table 2.
2 Control Weeds in Maize Field field control effectiveness test radix table of table
| Purslane | Acalypha copperleaf | Other broadleaf weeds | Sum | |
| Strain number/square metre | 18.8 | 2.1 | 0.6 | 21.4 |
| Proportion (%) | 87.6 | 9.8 | 2.6 | - |
3.2.3 drug effect calculation method
Strain number preventive effect=(blank area strain number-treatment region strain number)/blank area strain number × 100
Fresh weight preventive effect=(blank area fresh weight-treatment region fresh weight)/blank area fresh weight × 100
The investigation of 3.3 crops
3.3.1 control time and number
It is observed continuously after medicine 15 days.30 days, 45 days and harvest time are observed 3 times again after medicine.
3.3.2 investigation method
Using visual observations, symptom of chemical damage and severity are recorded.As a result, it has been found that not occurring jade in all processing
The phenomenon that rice is by phytotoxicity.
3.4 influence other biological
Nothing.
4 results and analysis
3 dicamba esters EC of table prevents and kill off corn field purslane field control effectiveness test effect
The above results summarize, and experiment 1-7 is the drug effect of dicamba esters product, and 8 be dicamba dimethylamine aqua drug effect,
7 days preventive effects compare average phase difference 16%, and 15 days preventive effects compare average phase difference 16.8%, 30 days differences 17.3%, 45 days phases
Poor 16.4%, and best with No. 1 drug effect in esters, the different monooctyl ester missible oil of 40% dicamba.From the point of view of drug effect, attachment penetration increases
Qiang Liao.
The experiment of 9 anti-drift of embodiment:
Test medicine: 40% dicamba different monooctyl ester EC, 70% dicamba methyl esters EC, 41% dicamba dimethylamine SL
It is tested by EC120-B helicopter
Test place: Hebei province's Xingtai City
When test, 27 DEG C of temperature, it is classified 2 grades
Test site deployment scenarios are as shown in Figure 1.
Test method: mist droplet particle size method
Droplet size is distributed as shown in Fig. 2, from left to right successively are as follows: the different monooctyl ester EC of 40% dicamba, 70% dicamba first
Ester EC, 41% dicamba dimethylamine SL.
By droplet size and distribution, it can be concluded that, the mist droplet particle size of dicamba esters EC is larger, densely distributed, is not easy
Drift, and substantially without droplet on the paper card of SL, drift is more serious.It can be seen that dicamba esters EC provided by the invention
Anti-drift effect, which has, to be obviously improved.
Note: above-mentioned 41% dicamba dimethylamine salt SL is prepared in accordance with the following methods:
3.683T soft water is added to 10KL to prepare in kettle, adds the dicamba raw medicine of 4.167T 96%, is added dropwise 40%
Dimethylamine 2.15T, is added dropwise, and is warming up to 70-80 DEG C, keeps the temperature 60-70Min, controls PH=7.0-9.0, and heat preservation terminates, and passes through
Physics filters pressing handles to obtain 41% dicamba dimethylamine aqua.
By above-described embodiment and comparative example it is found that dicamba missible oil prepared by the present invention has higher drug effect and infiltration
Power, while the problem of drifting about, is greatly improved.
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.It should be pointed out that pair
For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out
Some improvements and modifications, these improvements and modifications also fall within the scope of protection of the claims of the present invention.
Claims (8)
1. a kind of dicamba type missible oil characterized by comprising
Dicamba ester, emulsifier and solvent；
The dicamba ester be dicamba methyl esters, dicamba ethyl ester, dicamba butyl ester, dicamba isobutyl ester, dicamba monooctyl ester or
The different monooctyl ester of dicamba.
2. dicamba type missible oil according to claim 1 characterized by comprising
Dicamba ester 10wt%~70wt%；
Emulsifier 5wt%~20wt%；
The solvent of surplus.
3. dicamba type missible oil according to claim 1, which is characterized in that the dicamba ester content be 30wt%~
50wt%.
4. dicamba type missible oil according to claim 1, which is characterized in that the emulsifier content be 10wt%~
12wt%.
5. dicamba type missible oil according to claim 1, which is characterized in that the emulsifier includes dodecyl benzene sulfonic acid
Any one in calcium and neopelex or two kinds and phenethyl phenol polyoxyethylene poly-oxygen propylene aether, phenethyl
Phenol polyethenoxy ether, phenethyl phenol polyethenoxy ether, nonyl phenol bring up Polyoxyalkylene ethers, Ben-zylphenol Polyoxyethyl Ether, fatty alcohol polyoxy
Any one or more in vinethene and castor oil polyoxyethylene ether.
6. dicamba type missible oil according to claim 1, which is characterized in that the solvent is solvent naphtha, vegetable oil, soybean
Oil and any one or more in methyl oleate.
7. dicamba type missible oil according to claim 6, which is characterized in that the solvent naphtha is solvent naphtha 150# or solvent
Oily 200#.
8. the preparation method of the described in any item dicamba type missible oil of claim 1~7, which comprises the following steps:
Dicamba ester is mixed with emulsifier and solvent, in 15~60 DEG C of 15~60min of stirring, obtains dicamba type missible oil.
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