CN105794779A - Microcapsule suspension-type pendimetalin herbicide - Google Patents
Microcapsule suspension-type pendimetalin herbicide Download PDFInfo
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- CN105794779A CN105794779A CN201410734959.8A CN201410734959A CN105794779A CN 105794779 A CN105794779 A CN 105794779A CN 201410734959 A CN201410734959 A CN 201410734959A CN 105794779 A CN105794779 A CN 105794779A
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- pendimethalin
- microcapsule
- suspending agent
- herbicide
- microcapsule suspending
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Abstract
The present invention discloses a microcapsule suspension-type pendimetalin herbicide. The invention includes the composition and the mass fraction of the polymer material, additives, a preparation process and preparation method of the capsule suspension, the main physical and chemical indicators of the suspension and a detection and evaluation method. The microcapsule suspension-type pendimethalin herbicide has good physical and chemical properties, and can effectively control weeds in dry land crops, and play a good protection effect on crops.
Description
Technical field
The present invention relates to formulations of pesticide production field, in particular to the technology of preparing of a kind of microcapsule suspension type pendimethalin herbicide for the protection of dry field farming thing.
Background technology
Pendimethalin disappears grass or Pendimethalin also known as amine, isThe phenyl amines herbicide succeeded in developing by American Cyanamid Company.Pendimethalin is a kind of outstanding dry crop selective herbicide, can effectively prevent and kill off annual gramineae and some annual broadleaf weed, it is widely used in the weeds such as the various crop such as corn and soybean, Semen arachidis hypogaeae, Cotton Gossypii, direct-seeding dry rice, Rhizoma Solani tuber osi, Nicotiana tabacum L., vegetable, the preventing and treating barnyard grass in field, Herba Digitariae, Herba Setariae Viridis, annual bluegrass, Herba chenopodii, Herba Amaranthi tricoloris；Have good weeding selectivity and the hypotoxicity to people, animal due to pendimethalin, current pendimethalin is the big herbicide in the world the 3rd, and its sales volume is only second to steriland herbicide glyphosate, N,N'-dimethyl-.gamma..gamma.'-dipyridylium, is the selective herbicide that sales volume is maximum in the world.
Owing to pendimethalin is water insoluble, it is dissolved only in the lower boiling organic solvents such as toluene, methanol, acetone, Ketohexamethylene, therefore the many emulsifiable concentrate uses making about 20-50% with toluene, Ketohexamethylene and polyethers or anionic surfactant etc. of pendimethalin；Though pendimethalin emulsifiable concentrate can be advantageously used in dry field farming thing, but there is a large amount of organic solvent pollution air and the shorter problem of effective drug duration.Although the pendimethalin granule of about the 3-10% made with other dispensings is absent from organic solvent pollution problem, but the pendimethalin of granule materials volatilizees slowly in dry land, and herbicidal effect is not high.In order to improve the application effect of pendimethalin, the dosage form of pendimethalin has been improved by people, is made for pendimethalin microcapsule suspending agent.
Microcapsule suspending agent is the cyst material using macromolecular material as microcapsule, by Chemical Physics or physicochemical method, the active substance of pesticide is wrapped up, forms a kind of capsule with semi-permeable membrane, and they are disperseed with certain concentration, be suspended in water and remain stable for.The outstanding advantages of microcapsule suspending agent is: farm chemical ingredients slow releasing, and the longevity of residure is long, can maintain 80-120 days；Reduce contact toxicity and the poisoning of people, animal；Compare pendimethalin cream preparation reduce or eliminate organic solvent, be conducive to environmental conservation.
At present, there is pesticide producer can produce pendimethalin microcapsule suspending agent though domestic,But from the relevant report obtained, these pendimethalin microcapsule suspending agentsExist three aspects problem: one is be not completely free of aromatic hydrocarbons, organic solvent of ketone, in product still containingThe harmful substances such as toluene, dimethylbenzene, Ketohexamethylene；Two is that capsule material (capsule skin) accounts for always ratio 10-20%, and such microcapsule suspending agent lacks quick-acting；Three is that preparation cost is high, exceeds other dosage form costs 3-5 times.
Summary of the invention
In order to overcome the deficiency of domestic existing pendimethalin microcapsule suspending agent, the invention discloses a kind of newThe technology of preparing of microcapsule suspension type pendimethalin herbicide.The key feature of the technology of the present invention has 2 points, one is do not use completely such as the organic solvent such as toluene, Ketohexamethylene when preparing microcapsule, two is that the cyst wall macromolecular material of microcapsule mainly have employed the cellulose being derived from plant, and three is that determined polymerization equipment is simple to operation.Pendimethalin content reaches more than 45%, microcapsule mean diameter is 5 μm and the pendimethalin microcapsule suspending agent having good stability to adopt the technology of the present invention to prepare.
Technical scheme:
Step 1, adopt high-temperature heating method pendimethalin, plant cellulose, auxiliary agent and water are made stable heterogeneous system；
Step 2, second comonomer is dissolved in deionized water and regulate to PH for neutrality, adopt inorganic peroxide as initiator.
Step 3, will the second comonomer obtained by step 2 and be slowly added in the heterogeneous system that step 1 is obtained respectively under initiator solution stirring, carry out interface crosslinking copolyreaction heating, under nitrogen protection and suitable mixing speed.
Beneficial effect:
Adopt the technology of the present invention can obtain following four beneficial effects:
1, adopt pendimethalin microcapsule suspending agent obtained by the present invention without organic solvents such as toluene aromatic hydrocarbons, methanol, Ketohexamethylene, eliminate the pendimethalin emulsifiable concentrate being presently using and atmospheric pollution that other pendimethalin microcapsule suspending agents domestic produce because of the volatilization of organic solvent therein；
2, in the present invention, microcapsule wall material major part have employed the plant cellulose deriving from nature, and the cyst wall macromolecule generated has good biological degradability, significantly reduces the harm to environment of the non-biodegradation type macromolecular compound；
When 3, adopting the technology of the present invention to prepare pendimethalin microcapsule suspending agent, the cyst material used is few, and obtained microcapsule wall is thin, pendimethalin active matter good penetrability in capsule, and drug effect is high, and herbicidal effect is good.
4, the pendimethalin microcapsule suspending agent obtained by the technology of the present invention is adopted to have good heat stability and low temperature-melted alternation stability, and pendimethalin active matter non-crystallizable, not breaking cellular wall at a lower temperature in capsule, be conducive to using under different seasons and weather conditions.
Detailed description of the invention:
Embodiment 1:
(1) pendimethalin solid 450g and cyst material 1-carboxymethyl cellulose 7g is taken respectively, add in many mouthfuls of reaction bulbs, stirring is lower adds appropriate deionized water, it is slowly added into auxiliary agent 1 butyl 2.5g again, auxiliary agent 2 glycerol polyoxyethylene ether 2.5g, it is stirred vigorously and heats to 60-65 DEG C, obtain a uniform heterogeneous system；
(2) take cyst material 2-second comonomer acrylamide 3g, dissolve by appropriate amount of deionized water；Separately take initiator potassium persulfate 0.05g, with stand-by after deionized water dissolving；
(3) under heated and stirred, cyst material 2-second comonomer solution and initiator solution are slowly added into by (1) obtained heterogeneous system, maintain the temperature in reaction bulb between 58 ~ 68 DEG C, mixing speed is not less than 200 revs/min, synchronize to dropwise by two kinds of solution in 1 hour, terminate after being incubated 1.0 ~ 1.5 hours at 60 ~ 70 DEG C, obtain stable pendimethalin microcapsule suspending agent；
(4) from starting to drip second comonomer, constantly to inflated with nitrogen in reaction bulb until second comonomer solution and initiator solution dropwise, are incubated and terminate.
(5) in product gross mass 1000g, the mass fraction of pendimethalin solid is 45%, the mass fraction of sodium carboxymethyl cellulose and second comonomer acrylamide is 1%, and the mass fraction of auxiliary agent butyl and glycerol polyoxyethylene ether is 0.5%, and all the other are deionized water.
Detection is evaluated:
Adopting the microcapsule mean diameter that laser particle analyzer records the pendimethalin microcapsule suspending agent that said method prepares is 6 μm, adopting the freeze-thawing stability test result that FAO pesticide standard method records obtained pendimethalin microcapsule suspending agent is qualified (-10-20 DEG C, 4 cycles).
Embodiment 2:
(1) pendimethalin solid 450g and cyst material 1-carboxymethyl cellulose 10g is taken respectively, add in many mouthfuls of reaction bulbs, stirring is lower adds appropriate deionized water, it is slowly added into auxiliary agent 1 butyl 4.5g again, auxiliary agent 2 glycerol polyoxyethylene ether 4.5g, it is stirred vigorously and is heated to 60-65 DEG C, obtain a uniform heterogeneous system；
(2) take cyst material 2-second comonomer acrylamide 5g, dissolve by appropriate amount of deionized water；Separately take initiator potassium persulfate 0.1g, with stand-by after deionized water dissolving；
(3) under heated and stirred, cyst material 2-second comonomer solution and initiator solution are slowly added into by (1) obtained heterogeneous system, maintain the temperature in reaction bulb between 60 ~ 70 DEG C, mixing speed is not less than 300 revs/min, synchronize to dropwise by two kinds of solution in 1 hour, terminate after being incubated 1.0 ~ 1.5 hours at 55 ~ 65 DEG C, obtain stable pendimethalin microcapsule suspending agent；
(4) from starting to drip second comonomer, constantly to inflated with nitrogen in reaction bulb until second comonomer solution and initiator solution dropwise, are incubated and terminate.
(5) in product gross mass 1000g, the mass fraction of pendimethalin solid is 45%, the mass fraction of sodium carboxymethyl cellulose and second comonomer acrylamide is 1.5%, and the mass fraction of auxiliary agent butyl and glycerol polyoxyethylene ether is 0.9%, and all the other are deionized water.
Detection is evaluated:
Adopting the microcapsule mean diameter that laser particle analyzer records the pendimethalin microcapsule suspending agent that said method prepares is 5 μm, adopting the freeze-thawing stability test result that FAO pesticide standard method records obtained pendimethalin microcapsule suspending agent is qualified (-10-20 DEG C, 4 cycles).
Embodiment 3:
(1) pendimethalin solid 450g and cyst material 1-carboxymethyl cellulose 14g is taken respectively, add in many mouthfuls of reaction bulbs, stirring is lower adds appropriate deionized water, it is slowly added into auxiliary agent 1 dibutyl ethylene glycol ether 6g again, auxiliary agent 2 glycerol polyoxyethylene ether 6g, it is stirred vigorously and is heated to 70 DEG C, obtain a uniform heterogeneous system；
(2) take cyst material 2-second comonomer acrylamide 6g, dissolve by appropriate amount of deionized water；Separately take initiator potassium persulfate 0.15g, with stand-by after deionized water dissolving；
(3) under heated and stirred, cyst material 2-second comonomer solution and initiator solution are slowly added into by (1) obtained heterogeneous system, maintain the temperature in reaction bulb between 65 ~ 75 DEG C, mixing speed is not less than 300 revs/min, synchronize to dropwise by two kinds of solution in 1 hour, terminate after being incubated 1.0 ~ 1.5 hours at 55 ~ 65 DEG C, obtain stable pendimethalin microcapsule suspending agent；
(4) from starting to drip second comonomer, constantly to inflated with nitrogen in reaction bulb until second comonomer solution and initiator solution dropwise, are incubated and terminate.
(5) in product gross mass 1000g, the mass fraction of pendimethalin solid is 45%, the mass fraction of sodium carboxymethyl cellulose and second comonomer acrylamide is 2%, and the mass fraction of auxiliary agent butyl and glycerol polyoxyethylene ether is 1.2%, and all the other are deionized water.
Detection is evaluated:
Adopting the microcapsule mean diameter that laser particle analyzer records the pendimethalin microcapsule suspending agent that said method prepares is 5 μm, adopting the freeze-thawing stability test result that FAO pesticide standard method records obtained pendimethalin microcapsule suspending agent is qualified (-10-20 DEG C, 4 cycles).
Claims (5)
1. a microcapsule suspension type pendimethalin herbicide technology of preparing, it is characterised in that this technology includes the composition of cyst wall macromolecular material and mass fraction, auxiliary agent composition and mass fraction, pendimethalin microcapsule suspending agent preparation technology flow chart and preparation method, the main physical and chemical index of microcapsule suspending agent and detection method.
2. according to claim 1, described cyst wall macromolecular material composition includes the compound monomer in a kind of material being derived from plant and 1-2 kind molecular structure containing unsaturated double-bond, and the carbon number in every kind of compound monomer containing unsaturated double-bond is 3-10.
3. according to claim 2, described in be derived from the material of plant and the quality containing unsaturated double-bond compound monomer accounts for the 0.1-3.0% of product gross mass.
4., according to claim 1, described auxiliary agent is polyol fat ether and the polyhydric alcohol polyoxyethylene ether that boiling point is higher than 120 DEG C.
5. according to claim 1, the main physical and chemical index of described pendimethalin microcapsule suspending agent is: microcapsule mean diameter, and it is laser particle analyzer method that evaluation methodology is commented in detection；Freeze-thawing stability, inspection assessment method is the method in the pesticide standard of FAO's FAO defined.
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| CN201410734959.8A CN105794779B (en) | 2014-12-08 | 2014-12-08 | A kind of microcapsule suspension type pendimethalin herbicide |
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| CN201410734959.8A CN105794779B (en) | 2014-12-08 | 2014-12-08 | A kind of microcapsule suspension type pendimethalin herbicide |
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| CN105794779A true CN105794779A (en) | 2016-07-27 |
| CN105794779B CN105794779B (en) | 2018-07-10 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1464385A1 (en) * | 2003-04-04 | 2004-10-06 | Cognis Iberia, S.L. | Microcapsules (XVIII) |
| CN102100229A (en) * | 2009-12-16 | 2011-06-22 | 联合国南通农药剂型开发中心 | Pesticide micro-capsule granules and preparation method thereof |
| CN102696594A (en) * | 2012-06-28 | 2012-10-03 | 上海沪联生物药业（夏邑）有限公司 | Pendimethalin micro-capsule suspending agent and preparation method thereof |
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2014
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1464385A1 (en) * | 2003-04-04 | 2004-10-06 | Cognis Iberia, S.L. | Microcapsules (XVIII) |
| CN102100229A (en) * | 2009-12-16 | 2011-06-22 | 联合国南通农药剂型开发中心 | Pesticide micro-capsule granules and preparation method thereof |
| CN102696594A (en) * | 2012-06-28 | 2012-10-03 | 上海沪联生物药业（夏邑）有限公司 | Pendimethalin micro-capsule suspending agent and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 徐浩龙: "羧甲基纤维素接枝丙烯酸/丙烯酰胺缓释肥包膜材料的制备、性能及应用", 《化学与生物工程》 * |
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| CN105794779B (en) | 2018-07-10 |
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Denomination of invention: Microcapsule suspension-type pendimetalin herbicide Effective date of registration: 20181121 Granted publication date: 20180710 Pledgee: Bank of China Limited by Share Ltd Nanjing City South Branch Pledgor: Nanjing Gaozheng Agrochemical Co., Ltd. Registration number: 2018320000323 |