CN103098813B - Preparation method of conservation tillage preemergence composite herbicide - Google Patents

Abstract

The invention relates to a preparation method of a conservation tillage preemergence composite herbicide. The method specifically consists of the following four steps: prepolymerization liquid preparation, emulsion preparation, acidification and curing. Specifically, research on composite herbicide raw material selection, emulsifying agent selection, emulsification mode selection, acidification condition selection, curing mode selection and the like are conducted to determine the optimal technological conditions. Concretely, the herbicide is a conservation tillage microencapsulated soybean field preemergence composite herbicide.

Description

Before a kind of conservation tillage seedling, use the preparation method of compound herbicide

Technical field

The present invention relates to technical field of pesticide, especially, relate to the front new herbicides preparation field of using of conservation tillage Soybean Field seedling.

Background technology

Conservation tillage is for improving agriculture work efficiency, and liberation agricultural workforce has brought into play great function.Along with the expansion of conservation tillage implement scale and the continuity of time, there is expansion rapidly in some zonal crop smotherings, and the harm of part weeds is on the rise.Conservation tillage is compared with conventional tillage; owing to having cancelled mouldboard plow, turn over and process the means of weeds; and earth's surface has stalk to cover or crop straw stubble is retained; thereby make weeds generation and harm in conservation tillage ground day by day serious, all bring certain difficulty to traditional chemical weed control, machinery or artificial weeding.Outstanding behaviours is in following several respects:

1. farmland weed increases, and grows unevenly, and weeds occurrence degree increases the weight of;

2. no-tillage farming has been protected the growing environment of farmland weed, causes rear stubble weed density large high, careless age, has increased difficulty of prevention and cure;

3. weed killer herbicide consumption increases, and has increased the weight of to a certain extent environmental;

4. there is serious conservation tillage farmland grain drop in production in weeds, and commodity reduces.

Weeds harm has now become the critical limitation factor of further expansion and stable development conservation tillage.

Soybean is the main source of vegetable protein food and feed, is also one of raw material of oil expression.The current every Annual planting area of China reaches more than 750 ten thousand hm ², account for 6.7% of the cereal crops gross area, 2.5% of gross yield.

In the long-term cultivation of conservation tillage soybean, formed complicated weed control.Common annual gramineous weed has barnyard grass, green foxtail, setaria glauca and lady's-grass, wild oat, eleusine indica etc.; Annual broadleaf weed has Siberian cocklebur, amaranth; Black nightshade, phoenix cauliflower, acalypha copperleaf, elscholtiza, water sour jujube pin, bur beggar-ticks, willow leaf thorn knotweed, pale persicaria, salsola collina, lamb's-quarters, dodder, dayflower, kitchen garden, clearvers etc.; Perennial weed has meadow pine, corn sow thistle, field thistle, reed etc.

The insecticide-applying way of soybean field herbicide is mainly to be broadcast front mixed soil and processes, broadcasts before rear seedling cauline leaf after soil treatment and seedling and process.Can according to weeds in field population, a situation arises, suit measures to local conditions, select targetedly suitable insecticide-applying way and weed killer herbicide kind.

Before broadcasting, the feature of soil treatment before rear seedling of broadcasting is: management of weeds, in germination period with before working the mischief, is prevented trouble before it happens; Early stage control weeds, can postpone or reduce intertillage number of times.The mixed soil of pre-sowing application only needs less rainfall and soil moisture; Dry early little on the impact of drug effect; The mixed soil of pre-sowing application can strengthen the control to the unearthed annual broadleaf weed of deep layer and part grassy weed; Adopt large droplet spraying, can alleviate and prevent the harm of sensitive crop around; Can execute soil drought and the evaporation of water in soil while avoiding the spring to execute the autumn.After broadcasting the front dispenser requirement dispenser of rear seedling, must keep soil moisture; Otherwise drug effect is poor, even invalid.Meanwhile, also there is other problems in dispenser before seedling, as dose and drug effect are subject to the impact of the soil texture, the content of organic matter, pH value; In sandy-soil, heavy rain can pour some weed killer herbicide at the germination position of soya seeds and poisoning occurs.

If pesticide supplying effect is undesirable before seedling, can take the mode of dispenser after seedling to remedy.The feature that after seedling, cauline leaf is processed is: be subject to the impact of soil types and humidity little; Specific aim is stronger, can be according to actual crop smothering medication.But its herbicide spectrum majority is narrower; And easily crop is around worked the mischief during medication; The weed killer herbicide using during some high temperature also can work the mischief to soybean; During dry morning, weeds slowly grow, and drug effect is bad; In addition the weeding time more late soybean the impact that is subject to of Growth and yield larger.

Therefore, when soybean weeds is carried out to chemical control, when Tanaka weeds occur with dispersing mode, should be as far as possible with soil treatment mode dispenser before seedling, and to select slightly long weed killer herbicide kind of lasting period.

The harm of soybean weeds is:

1, strive water, fertilizer, luminous energy with crop, occupy on the ground and underground part space, affect crop photosynthesis, disturb plant growth, reduce grain yield, affect product quality;

2, bring out and the insect pest that spreads disease;

3, increase farm production cost;

4, affect human and livestock health;

5, affect water conservancy projects

The Soybean Field chemical herbicide that has many types in prior art, for preventing and kill off different types of soybean weeds, but these weed killer herbicide existing problems have:

1, the broad-spectrum action of preventing and kill off is inadequate, and that prevents and kill off is indifferent.

2, dosage is larger, and utilization rate is lower, thereby causes residual quantity more, and this all has harm for crop, soil, people and animals.

3, prior art has the precedent of agricultural chemicals microencapsulation, but that shortcoming is envelop rate is not high, the granular degree of the micro-capsule of preparation, illiquidity, and preparation technology optimizes not.Etc..

Related art has as follows:

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CN101473816B

CN101622987B

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CN101461359B

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The different emulsifying process of < < are made the comparison > > of microencapsulation

The preparation of < < chlopyrifos microcapsule suspending agent and the optimization > > of microencapsulation condition

The preparation > > of < < ethiprole micro-capsule granula

< < interfacial polymerization is prepared agricultural chemicals microcapsules > >

The Primary Study > > of < < Studies of The Microcapsulation of Lactics

The application > > of < < microencapsulation technology in drug research

< < microbial pesticide formulation and microencapsulation technology > >

The microencapsulation technology > > of < < fine particle

" accelerator " of < < botanical biological pesticide---microencapsulation technology > >

The microencapsulation of tri-kinds of different agricultural chemicals of < < and microcapsule suspension system controlled release properties research > > thereof

< < microencapsulation of pesticide novel form > >

The present Research of < < microencapsulation of pesticide and development > >

The preparation of < < benzoyl area kind pesticide micro capsule and performance study > > thereof etc.

Summary of the invention

One object of the present invention is to provide compound herbicide before a kind of seedling that has broad-spectrum action for soybean weeds.

Another object of the present invention has been to provide the preparation method of described compound herbicide, and the method specifically comprises:

(1) pre-polymerization liquid preparation

Urea and 37% formalin are mixed according to mol ratio at 1: 2, with triethanolamine, regulate pH to 8.0, at 75 ℃ of water-bath 2h, generate urea aldehyde pre-polymerization liquid;

(2) emulsion preparation

16 weight portion mixed herbicides (thifensulfuronmethyl: prometryn=0.8: the N that 1 (weight ratio)) adds 14 weight portions, in the solvent of dinethylformamide, fully dissolve, add 1 weight portion blended emulsifier (neopelex: alkylphenol polyoxyethylene=1: 2 (weight ratios)), add again 180 weight parts waters, with ultrasonic, stir associating emulsification, condition is ultrasonic power 450w, frequency 45kHz, 75 ℃ of temperature, mixing speed is 1500r/min, and the time is 15min;

(3) acidifying

Pre-polymerization liquid and emulsion are mixed with the weight ratio of 8: 13, even with 1500r/min high-speed stirred, with ammonium chloride, slowly regulate pH to 2.0, acidifying 3h;

(4) solidify

Adopt spraying to be dried and be cured, condition is 175 ℃ of inlet temperatures, 85 ℃ of outlet temperatures, and feed rate 480L/h, obtains compound herbicide microcapsule granule.

The invention has the advantages that:

1, there is wider herbicide effect;

2, between compound herbicide composition, have synergy, herbicide effect strengthens;

3, utilized the effects such as microcapsule controlled-release, made dosage be reduced to former dosage 25%～30%, and there is more permanent herbicide effect;

4, reduced the harmful effect to crop, people and animals, soil etc.;

5, microencapsulation preparation has better particle diameter and mobility;

6, preparation technology's optimization.

Embodiment

Embodiment 1,

(1) pre-polymerization liquid preparation

Urea and 37% formalin are mixed according to mol ratio at 1: 2, with triethanolamine, regulate pH to 8.0, at 75 ℃ of water-bath 2h, generate urea aldehyde pre-polymerization liquid;

(2) emulsion preparation

16 weight portion mixed herbicides (thifensulfuronmethyl: prometryn=0.8: the N that 1 (weight ratio)) adds 14 weight portions, in the solvent of dinethylformamide, fully dissolve, add 1 weight portion blended emulsifier (neopelex: alkylphenol polyoxyethylene=1: 2 (weight ratios)), add again 180 weight parts waters, with ultrasonic, stir associating emulsification, condition is ultrasonic power 450w, frequency 45kHz, 75 ℃ of temperature, mixing speed is 1500r/min, and the time is 15min;

(3) acidifying

Pre-polymerization liquid and emulsion are mixed with the weight ratio of 8: 13, even with 1500r/min high-speed stirred, with ammonium chloride, slowly regulate pH to 2.0, acidifying 3h;

(4) solidify

Adopt spraying to be dried and be cured, condition is 175 ℃ of inlet temperatures, 85 ℃ of outlet temperatures, and feed rate 480L/h, obtains compound herbicide microcapsule granule.

All wt part all in " kilogram ".

The contrast of embodiment 2, weed killer herbicide control efficiency

With weed killer herbicide of the present invention, carry out effect experiment contrast with using separately thifensulfuronmethyl, Prometryn weedicide agent, the actual drug consumption of weed killer herbicide of the present invention is to use separately 30% of weed killer herbicide consumption, the results are shown in Table 1:

Table 1, weed killer herbicide of the present invention and the independent Contrast on effect that uses weed killer herbicide

Note :-: invalid; +: effectively; ++: effect is better; +++: effective; ++++: effect is very good.

The comparative trial of embodiment 3, different emulsifiers

With the independent use of compound emulsifying agent of the present invention and other emulsifier, carry out emulsifying effectiveness comparative trial, the results are shown in Table 2:

Table 2, the impact of different emulsification on emulsifying effectiveness

Result shows, the use of emulsifier can have influence on the particle diameter of final emulsification, and the present invention, according to the difference of compound material, has creatively used compound emulsifying agent, obtains best emulsifying effectiveness.

The comparative trial of embodiment 4, ultrasonic-stirring associating emulsification

With ultrasonic-stirring associating emulsification of the present invention and the stirring of independent different rotating speeds, independent ultrasonic emulsification, carry out emulsifying effectiveness comparative trial, the results are shown in Table 3:

Table 3, the impact of different emulsification method on emulsifying effectiveness

Result shows, ultrasonic-stirring is combined to be emulsified under the experiment condition that guarantees relatively placidity and is had better dispersity and emulsifying effectiveness, simultaneously, separately there is related experiment to show, when the time of associating emulsification of the present invention, increase, or experiment condition is strengthened rear emulsifying effectiveness and is but declined to some extent, this may be during due to ultrasonic emulsification, after experiment condition is violent, the inner droplet existing of emulsion collides mutually, in collision process, between droplet, there is merged and possibility that be crashed to pieces, therefore the definite experiment condition of the present invention is the experiment condition that has most that forms optimum emulsification effect.

The comparative trial of embodiment 5, different curing methods

With spraying dry solidification method of the present invention and traditional intensification solidification method, carry out comparative trial, the results are shown in Table 4:

Result shows, it is fast that spray-dired solidification method has encystation speed, processing step is simple, the feature of microcapsule granule good fluidity, simultaneously, because spraying dry solidification method is prepared the impact that micro-capsule is subject to many factors, as the temperature of the concentration of the viscosity of mixed liquor, the uniformity, core and wall material, ratio, spraying, inlet amount etc., the present invention determines that process conditions are all definite optimum process conditions under the considering of these influence factors.

In addition, the present invention has also studied the impact of acidulated condition for microcapsule diameter, be mainly research be acidifying pH, souring temperature, the impact of acidificatoin time on particle diameter, finally determined acidulated condition.

Claims (2)

1. before conservation tillage seedling, use a preparation method for compound herbicide, it is characterized in that comprising step:

(1) pre-polymerization liquid preparation

Urea and 37% formalin are mixed according to mol ratio at 1: 2, with triethanolamine, regulate pH to 8.0, at 75 ℃ of water-bath 2h, generate urea aldehyde pre-polymerization liquid;

(2) emulsion preparation

16 weight portion mixed herbicides add the N of 14 weight portions, in the solvent of dinethylformamide, fully dissolve, add 1 weight portion blended emulsifier, add again 180 weight parts waters, with ultrasonic, stir associating emulsification, condition is ultrasonic power 450w, frequency 45kHz, 75 ℃ of temperature, mixing speed is 1500r/min, and the time is 15min, wherein, mixed herbicide is thifensulfuronmethyl: prometryn=0.8: 1 (weight ratio) mixes, and blended emulsifier is neopelex: alkylphenol polyoxyethylene=1: 2 (weight ratio) mixes;

(3) acidifying

Pre-polymerization liquid and emulsion are mixed with the weight ratio of 8: 13, even with 1500r/min high-speed stirred, with ammonium chloride, slowly regulate pH to 2.0, acidifying 3h;

(4) solidify

Adopt spraying to be dried and be cured, condition is 175 ℃ of inlet temperatures, 85 ℃ of outlet temperatures, and feed rate 480L/h, obtains compound herbicide microcapsule granule.

2. the weed killer herbicide of being prepared by method claimed in claim 1.