CN106359389A - Preparation method of slow-release imazapyr particles - Google Patents

Preparation method of slow-release imazapyr particles Download PDF

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Publication number
CN106359389A
CN106359389A CN201610782924.0A CN201610782924A CN106359389A CN 106359389 A CN106359389 A CN 106359389A CN 201610782924 A CN201610782924 A CN 201610782924A CN 106359389 A CN106359389 A CN 106359389A
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CN
China
Prior art keywords
arsenal
preparation
weed eradication
imazapyr
smoke particle
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Pending
Application number
CN201610782924.0A
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Chinese (zh)
Inventor
张�尘
张一尘
赵健
王超
陆相瑞
孙迪圣
罗进超
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YANCHENG SOUTH CHEMICAL CO Ltd
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YANCHENG SOUTH CHEMICAL CO Ltd
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Priority to CN201610782924.0A priority Critical patent/CN106359389A/en
Publication of CN106359389A publication Critical patent/CN106359389A/en
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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
    • A01N43/50—1,3-Diazoles; Hydrogenated 1,3-diazoles
    • 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
    • A01N25/12—Powders or granules

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Dentistry (AREA)
  • Plant Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Agronomy & Crop Science (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Toxicology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention belongs to the field of pesticide, and in particular relates to a preparation method of slow-release imazapyr. The preparation method comprises the following steps: dissolving the imazapyr in the low boiling organic solvent; taking the expanded vermiculite and the zeolite, grinding into 20 to 325 meshes of mixed carrier powder; adding the mixed carrier powder into the imazapyr solution to obtain the mixture solution of the imazapyr and carrier powder; adding binder into the mixture solution of the imazapyr and carrier powder and stirring for 0.1 to 6 hours until the mixing is uniform; and then distilling the mixture solution of the imazapyr and carrier powder under the reduced pressure after being mixed with binder uniformly to obtain solid particles and imazapyr-carrier powder particles; distilling under the reduced pressure to recover organic solvent and obtain the slow-release imazapyr particles. The preparation method has the following advantages: 1, chemical and physical stability is good to avoid a lot of decomposition of the original drug; safety is good, the environmental pollution is easy to process, store and transport; 3, continuous release of imazapyr plays a sustained weed control effect.

Description

A kind of preparation method of spacetabs type weed eradication smoke particle
Technical field
The invention belongs to pesticide field, a kind of more particularly, to preparation method of spacetabs type weed eradication smoke particle.
Background technology
In order to improve Pesticide use safety, control the adverse effect to ecological environment for the pesticide, novel agrochemical formulations are in recent years To quickly grow.With respect to the tradition formulations of pesticide such as cream, novel agrochemical formulations have the advantage that 1) Environmental compatibility is good； 2) active component content is high, and packaging volume is little, and storing and transporting security is convenient；3) better stability of preparation, dosage form strong adaptability, it is applicable to Liquid, solid active compound.
Arsenal belongs to imidazolinone herbicide, is side chain amino acid synthetic inhibitor, is New-type wide-spectrum herbicide；This Apply after product bud and can absorb for the root of weeds, leaf rapidly, by suppressing the biosynthesiss of branched-chain amino acid and stoping weed growth, It is a kind of steriland herbicide；Applicable crops forest land, bare place.Most annual and perennial single, double cotyledons can be prevented and treated Weeds have remarkable activity of weeding to sedge weed, annual and perennial monocotyledon weed, broad leaved weed.But Arsenal There is higher water solublity (when 25 DEG C in water dissolubility 11.3g/l), easily infiltrate into deep layer in the more Zoned application of rainwater Soil, pollutes to subsoil water.
Content of the invention
The technical problem to be solved in the present invention is: provides a kind of preparation method of spacetabs type weed eradication smoke particle.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation side of spacetabs type weed eradication smoke particle Method, comprises the steps:
(1) Arsenal is dissolved in low boiling point organic solvent, is configured to the weed eradication that weed eradication smoke density is 50～250g/l Cigarette solution；
(2) Vermiculitum, zeolite and bentonite is taken uniformly to mix post-heating to 800～1000 DEG C of thermal expansion solids, powder after cooling It is broken into the mixed carrier powder of 20～325 mesh；
(3) the mixed carrier powder that step (2) obtains is added in the Arsenal solution that step (1) obtains, airtight Stir 0.1～24h in reaction vessel, obtain Arsenal-support powder mixed liquor；
(4) add binding agent in Arsenal-support powder mixed liquor that step (3) is obtained, continue stirring 0.1～6h extremely Mix homogeneously；Arsenal after mixing homogeneously with binding agent-support powder mixed liquor carries out vacuum distillation to no obvious liquid Residual, the solid content pelletize obtaining after first time vacuum distillation, obtain Arsenal-support powder granule；
(5) Arsenal-support powder granule that step (4) obtains is carried out with drying under reduced pressure removing organic solvent extremely organic molten Agent residual quantity is less than 1%wt, obtains spacetabs type weed eradication smoke particle.
Described spacetabs type weed eradication smoke particle can directly sow soil surface or inside in the form of solid particle, passes through After above-mentioned steps processing, part Arsenal is absorbed in mixed carrier powder internal voids, partly remains in mixed carrier powder Last surface；Due to Arsenal in water slightly soluble, watered for the first time or during rainwater weather, remained in mixed carrier powder surface Arsenal be dissolved in soil, spacetabs type Arsenal herbicide granule apply the initial stage discharge more amount Arsenal with rapid Remove existing weeds；Be absorbed into mixed carrier powder internal voids Arsenal be flooded profit after slowly separate out, continue all Even release Arsenal is to play lasting preventing weeding weeds effect；Meanwhile, the release Arsenal of slow low dosage decreases and goes out The poisoning to normal crop for the careless cigarette, also reduces Arsenal and enters deep soil thus the probability of polluted underground water.
Preferably, described low boiling point organic solvent include one or more of methanol, chloroform, dichloromethane or ethanol mix Bonding solvent.
Preferably, prepare Arsenal solution in described step (1) can carry out at normal temperatures or under heated condition, heating temperature Degree is not higher than the boiling point of low boiling point organic solvent.
Preferably, in described step (3) Arsenal-support powder mixed liquor preparation process can at normal temperatures or heating shape Carry out under state, heating-up temperature is not higher than the boiling point of low boiling point organic solvent.
Preferably, the weed eradication smoke density of described Arsenal solution is 60～250g/l.
Preferably, described Vermiculitum, zeolite and bentonitic mass ratio are 20:1～5:1～10.Specifically, with mass parts Meter, Vermiculitum is 20 parts, and zeolite is 1～5 part, and bentonite is 1～10 part, and because the specific surface area of different carriers is different, it is right to lead to The absorbability of Arsenal is different, and the compatibility of different carriers has using the stable release realizing Arsenal.
Preferably, described adhesive includes sodium silicate, starch, hydroxypropyl cellulose, Polyethylene Glycol or Microcrystalline Cellulose.
Preferably, the interpolation quality of described adhesive is 2%～5% that mixed carrier powder adds quality.
Preferably it is characterised in that in described step (3) addition of mixed carrier powder be the 0.4 of Arsenal quality Times～10 times.The addition of mixed carrier powder can affect to be absorbed into the ratio of the Arsenal within mixed carrier powder, The addition of mixed carrier powder is higher, and adsorbed Arsenal ratio is higher, and the ratio of free Arsenal reduces, first to applying Phase burst size can accordingly reduce.
Preferably, in described step (3), the addition of mixed carrier powder is 2 times～10 times of Arsenal quality.
Preferably, the concrete grammar of described pelletize is that the solid content obtaining after first time vacuum distillation is crossed 18～24 mesh Sieve, obtains Arsenal-support powder granule.
Preferably, preservative, such as sodium benzoate can also be added while adding binding agent in described step (4), plus Enter quality and add the 0.1%～0.5% of quality for mixed carrier powder.
The present invention compared with prior art, has the advantage that 1. chemical physical stabilities are good, it is to avoid active compound is divided in a large number Solution；2. safety is good, and environmental pollution is little to be easy to processing, storage and transport；3. it is easy to fine design, packaging, storage fee are used Low；4. apply the Arsenal of initial stage release more amount to rapidly remove existing weeds in spacetabs type weed eradication smoke particle；Absorbed Enter mixed carrier powder internal voids Arsenal be flooded profit after slowly separate out, the release Arsenal of continuous uniform is held with playing Continuous preventing weeding weeds effect；Meanwhile, the release Arsenal of slow low dosage decreases the poisoning to normal crop for the Arsenal, Reduce Arsenal and enter deep soil thus the probability of polluted underground water.
Brief description
Fig. 1 is the spacetabs type weed eradication smoke particle of embodiment 1～3 and the release profiles contrast of 25% Arsenal soluble liquid Figure.
Specific embodiment
The present invention is further illustrated in conjunction with specific embodiments, and these embodiments are intended merely to further illustrate this Bright feature and feature, rather than limiting to the claimed invention, but protection scope of the present invention is not limited to this.Following Used in embodiment, Arsenal active compound is produced by Yancheng South Chemical Co., Ltd., and purity is 98%, and remaining reagent is all selected Common technical grade reagent on market.
Embodiment 1
Take Arsenal active compound 230g, dissolved solution, in 1l methanol, is configured to the weed eradication that weed eradication smoke density is 230g/l Cigarette methanol solution；Take expanded vermiculite 400g, zeolite 100g, bentonite 200g, be ground into the mixed carrier powder of 20～100 mesh End；Mixed carrier powder is added in Arsenal methanol solution, stirs 24h in reaction vessel airtight at normal temperatures, gone out Careless cigarette mixed carrier powder mixed liquor；Sodium silicate 35g will be added in Arsenal-support powder mixed liquor, continue stirring 1h extremely mixed Close uniformly；Arsenal-support powder mixed liquor of crossing after mixing homogeneously with sodium silicate carries out vacuum distillation to no obvious liquid Residual, crosses 18-24 mesh sieve, obtains Arsenal-support powder granule；Arsenal-support powder granule carries out drying under reduced pressure removing Organic solvent is less than 1%wt to Determination of Residual Organic Solvents, obtains spacetabs type weed eradication smoke particle 969g；Wherein dissociate Arsenal 47g, Mixed carrier powder is 79.6% to the adsorption rate of Arsenal.
Embodiment 2
Take Arsenal active compound 60g, be dissolved in 1l ethanol, be configured to the Arsenal ethanol that weed eradication smoke density is 60g/l molten Liquid；Take expanded vermiculite 400g, zeolite 20g, bentonite 20g, be ground into the mixed carrier powder of 100～200 mesh；To mix Support powder adds in Arsenal ethanol solution, stirs 10h, obtain Arsenal-mixing in reaction vessel airtight at normal temperatures Support powder mixed liquor；Hydroxypropyl cellulose 10g will be added in Arsenal-support powder mixed liquor, continue stirring 6h to mixing Uniformly；Arsenal-support powder mixed liquor of crossing after mixing homogeneously with hydroxypropyl cellulose carries out first time vacuum distillation extremely No obvious liquid residue, crosses 18-24 mesh sieve, obtains Arsenal-support powder granule；Arsenal-support powder granule carries out Secondary pressure is dried and removes organic solvent to Determination of Residual Organic Solvents less than 1%wt, obtains spacetabs type weed eradication smoke particle 514g；Its In free Arsenal 20.1g, mixed carrier powder is 66.5% to the adsorption rate of Arsenal.
Embodiment 3
Take Arsenal active compound 105g, add in the dichloromethane of 1l, be heated to being completely dissolved when 38 DEG C, be configured to Arsenal Concentration is the Arsenal dichloromethane solution of 105g/l；Take expanded vermiculite 400g, zeolite 50g, bentonite 100g, be ground into The mixed carrier powder of 200～325 mesh；Mixed carrier powder is added in Arsenal methanol solution, airtight at normal temperatures is anti- Answer stirring 12h in container, obtain Arsenal-mixed carrier powder mixed liquor；Micro- by adding in Arsenal-support powder mixed liquor Crystalline cellulose 12g, continues stirring 5h to mix homogeneously；Arsenal-support powder after being mixed homogeneously with Microcrystalline Cellulose is mixed Close liquid and carry out vacuum distillation to no obvious liquid residue, cross 18-24 mesh sieve, obtain Arsenal-support powder granule；Arsenal- Support powder granule carries out drying under reduced pressure and removes organic solvent to Determination of Residual Organic Solvents less than 1%wt, obtains spacetabs type weed eradication Smoke particle 668g；Wherein dissociate Arsenal 32.6g, and mixed carrier powder is 69.0% to the adsorption rate of Arsenal.
Comparative example
In order to verify the sustained release performance of gained water dispersible granules in above-described embodiment, and with 25% Arsenal soluble liquid Comparison, has carried out the release experiment through upper soll layer.Experimental technique is as follows: internal diameter be in the buchner funnel of 8cm, tile 2cm Thick soil, sprays distillation water-wet soil to saturation.After 12h, the spacetabs type Arsenal of preparation in difference Example 1～3 Grain 20mg, takes 25% Arsenal soluble liquid 20mg, uniformly sows or be sprayed at soil surface respectively, subsequently distilled with 40ml Water spray, collects leachates, analyzes the herbicide active active ingredients content in leachates using efficient liquid-phase chromatography method.Spray steams Distilled water amounts to 12 times, every minor tick 1h.Calculate and add up to drench the percentage that the herbicide active active ingredients content accounts for initial application total amount Ratio is release rate (%).Draw the variation relation with spray number of times for the release rate, i.e. releasing curve diagram.
It will be noted from fig. 1 that as far as possible different carrier consumptions leads to free Arsenal content different, thus leading to difference Initial release rate after spraying twice in embodiment is widely different, but subsequent release profiles are all less compared with reference examples slope, release Put more slow and low dosage；In actual application, difference can be selected to dissociate for different Arsenal soils to be administered and go out The spacetabs type weed eradication smoke particle of careless cigarette content, applied widely.
Comparative example 2 soil eluviation is tested
By internal diameter 5cm, the glass tubing bottom of high 30cm is stoppered with the rubber stopper with sebific duct, pad one metafiltration paper, dress 1cm thickness Quartz sand, refill about 27cm thickness supplies examination soil, puts into equipped with the beaker of water, making moisture permeate up, is sufficiently humidified so as to soil Earth, earth pillar top refills the thick quartz sand of dress 1cm；Prepare four glass tubings, numbering 0～3 respectively, wherein No. 0 pipe adds 20mg 25% Arsenal soluble liquid, on the quartz sand being added on earth pillar top；It is slow that No. 1 pipe adds that 21.1mg embodiment 1 obtains Release type weed eradication smoke particle, No. 2 pipes add the spacetabs type weed eradication smoke particle that 42.8mg embodiment 2 obtains；No. 3 pipes add 31.8mg in fact Apply the spacetabs type weed eradication smoke particle that example 3 obtains；The spacetabs type weed eradication smoke particle that embodiment 1～3 obtains uniformly is sprinkling upon 1～3 respectively On the quartz sand on number pipe top；To in 0～No. 3 pipe with 30ml/h-1Speed add distillation water wash (be equivalent to rainfall 150mm/h-1), collect leachates, hplc measures, experimental result is as shown in table 1.
Table 1
Numbering Maximum Leaching Depth (cm)
0 >27
1 15.8
2 21.5
3 17.7
The soil selected in this comparative example is typical Taihu Lake rice soil, and ph is 7.1 about, and the content of organic matter is 29.1g/kg-1.In table 1, maximum Leaching Depth data combines knowable to the release experiment data of upper soll layer in Fig. 1: by this The spacetabs type weed eradication smoke particle that bright technical scheme obtains slowly can discharge Arsenal, and can effectively reduce weed eradication in soil The maximum Leaching Depth of cigarette, thus reduce the pollution to soil and groundwater for the Arsenal.
All documents that the present invention refers to all are incorporated as reference in this application, are individually drawn just as each document It is used as with reference to like that.

Claims (10)

1. a kind of preparation method of spacetabs type weed eradication smoke particle is it is characterised in that comprise the steps:
(1) Arsenal is dissolved in low boiling point organic solvent, is configured to the Arsenal that weed eradication smoke density is 50 ~ 250g/l molten Liquid；
(2) take Vermiculitum, zeolite and bentonite uniformly to mix post-heating to 800 ~ 1000 DEG C of thermal expansion solids, after cooling, be ground into 20 The mixed carrier powder of ~ 325 mesh；
(3) the mixed carrier powder that step (2) obtains is added in the Arsenal solution that step (1) obtains, in airtight reaction Stir 0.1 ~ 24h in container, obtain Arsenal-support powder mixed liquor；
(4) add binding agent in Arsenal-support powder mixed liquor that step (3) is obtained, continue stirring 0.1 ~ 6h to mixing Uniformly；Arsenal after mixing homogeneously with binding agent-support powder mixed liquor carries out vacuum distillation to no obvious liquid residue, The solid content pelletize obtaining after first time vacuum distillation, obtains Arsenal-support powder granule；
(5) Arsenal-support powder granule that step (4) obtains is carried out with drying under reduced pressure removing organic solvent residual to organic solvent Allowance is less than 1%wt, obtains spacetabs type weed eradication smoke particle.
2. the preparation method of spacetabs type weed eradication smoke particle as claimed in claim 1 is it is characterised in that described low boiling is organic molten Agent includes one or more of methanol, chloroform, dichloromethane or ethanol mixed solvent.
3. the preparation method of spacetabs type weed eradication smoke particle as claimed in claim 1 is it is characterised in that join in described step (1) Arsenal solution processed can be carried out at normal temperatures or under heated condition, and heating-up temperature is not higher than the boiling point of low boiling point organic solvent.
4. the preparation method of spacetabs type weed eradication smoke particle as claimed in claim 1 is it is characterised in that described Arsenal solution Weed eradication smoke density is 60 ~ 250g/l.
5. spacetabs type weed eradication smoke particle as claimed in claim 1 preparation method it is characterised in that described Vermiculitum, zeolite and Bentonitic mass ratio is 20:1 ~ 5:1 ~ 10.
6. the preparation method of spacetabs type weed eradication smoke particle as claimed in claim 1 is it is characterised in that described adhesive includes silicon Sour sodium, starch, hydroxypropyl cellulose, Polyethylene Glycol or Microcrystalline Cellulose.
7. the preparation method of spacetabs type weed eradication smoke particle as claimed in claim 6 is it is characterised in that the interpolation of described adhesive Quality is 2% ~ 5% that mixed carrier powder adds quality.
8. the preparation method of the spacetabs type weed eradication smoke particle as described in any one of claim 1 ~ 7 is it is characterised in that described step (3) in, the addition of mixed carrier powder is 0.4 times ~ 10 times of Arsenal quality.
9. the preparation method of spacetabs type weed eradication smoke particle as claimed in claim 8 is it is characterised in that mix in described step (3) The addition closing support powder is 2 times ~ 10 times of Arsenal quality.
10. spacetabs type weed eradication smoke particle as claimed in claim 1 preparation method it is characterised in that described pelletize concrete Method is that the solid content obtaining after first time vacuum distillation is crossed 18-24 mesh sieve, obtains Arsenal-support powder granule.
CN201610782924.0A 2016-08-31 2016-08-31 Preparation method of slow-release imazapyr particles Pending CN106359389A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1096411A (en) * 1993-04-28 1994-12-21 美国氰胺公司 Herbicidal extruded granular compositions
CN102461498A (en) * 2010-11-08 2012-05-23 河南好年景生物发展有限公司 Preparation method of slow-release pesticide

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1096411A (en) * 1993-04-28 1994-12-21 美国氰胺公司 Herbicidal extruded granular compositions
CN102461498A (en) * 2010-11-08 2012-05-23 河南好年景生物发展有限公司 Preparation method of slow-release pesticide

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
ADIRADIAN AND YAELG.MISHAEL: "Characterizing and Designing Polycation-Clay Nanocomposites As a Basis for Imazapyr Controlled Release Formulations", 《ENVIRONMENTAL SCIENCE & TECHNOLOGY》 *

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