CN103202298A - Method for manufacturing 2-chlorine-6-nitrapyrin microcapsule suspending agents - Google Patents
Method for manufacturing 2-chlorine-6-nitrapyrin microcapsule suspending agents Download PDFInfo
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- CN103202298A CN103202298A CN2013100904482A CN201310090448A CN103202298A CN 103202298 A CN103202298 A CN 103202298A CN 2013100904482 A CN2013100904482 A CN 2013100904482A CN 201310090448 A CN201310090448 A CN 201310090448A CN 103202298 A CN103202298 A CN 103202298A
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- 239000003094 microcapsule Substances 0.000 title claims abstract description 24
- 239000000375 suspending agent Substances 0.000 title claims abstract description 7
- 238000000034 method Methods 0.000 title abstract description 6
- 238000004519 manufacturing process Methods 0.000 title abstract 2
- 239000000243 solution Substances 0.000 claims abstract description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 9
- 229920001807 Urea-formaldehyde Polymers 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 230000020477 pH reduction Effects 0.000 claims abstract description 4
- DCUJJWWUNKIJPH-UHFFFAOYSA-N nitrapyrin Chemical compound ClC1=CC=CC(C(Cl)(Cl)Cl)=N1 DCUJJWWUNKIJPH-UHFFFAOYSA-N 0.000 claims description 14
- 239000000725 suspension Substances 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 11
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 claims description 8
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 6
- 239000008187 granular material Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000013530 defoamer Substances 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 150000007530 organic bases Chemical class 0.000 claims description 3
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 abstract description 3
- 208000027418 Wounds and injury Diseases 0.000 abstract description 2
- 230000006378 damage Effects 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 208000014674 injury Diseases 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 239000003960 organic solvent Substances 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract 4
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 abstract 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract 1
- 230000001276 controlling effect Effects 0.000 abstract 1
- 239000001257 hydrogen Substances 0.000 abstract 1
- 229910052739 hydrogen Inorganic materials 0.000 abstract 1
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 abstract 1
- 238000010008 shearing Methods 0.000 abstract 1
- 239000003814 drug Substances 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000000857 drug effect Effects 0.000 description 2
- 239000000618 nitrogen fertilizer Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 241000589151 Azotobacter Species 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000009931 harmful effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000000361 pesticidal effect Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
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- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention discloses a method for manufacturing 2-chlorine-6-nitrapyrin microcapsule suspending agents. The method includes dissolving a certain quantity of 2-chlorine-6-nitrapyrin in a certain quantity of toluene to obtain solution, adding a small quantity of NP (nonyl phenol)-10 emulsifying agents into the solution, uniformly stirring the solution and then adding a certain quantity of urea resin solution into the solution to obtain mixed solution; shearing the mixed solution at a high rotational speed for 40 minutes, reducing the rotational speed after materials in the mixed solution are sufficiently dispersed, and slowly adding hydrochloric acid with the concentration of 37% into the mixed solution so that a pH (potential of hydrogen) value of the mixed solution is regulated and ranges from 2.5 to 3; enabling the mixed solution to perform acidification reaction for 1 hour to form microcapsule particles; reducing the rotational speed to 200r/min within 20 minutes, controlling the temperature to range from 40 DEG C to 50 DEG C, and solidifying the microcapsule particles for 1 hour; and regulating the pH value of the microcapsule particles by 7.5-15% of sodium hydroxide aqueous solution so that the pH value ranges from 5 to 7, and adding 10-25% of NP-10 emulsifying agents into the microcapsule particles to form the microcapsule suspending agents. The method has the advantages that the products manufactured by the method are good in stability and low in environmental pollution, and contain few organic solvents, the cost is saved, and injury to operators is prevented.
Description
Technical field
The present invention relates to the pesticidal preparations processing technique field, relate in particular to a kind of preparation method of 15%-30%2-chloro-6-trichloromethyl pyridine micro-capsule suspension.
Background technology
Micro-capsule suspension refers to utilize natural or synthetic macromolecular material to form " nuclear-shell " structure small container, with the agricultural chemicals coating wherein, and is suspended in the formulations of pesticide in the water.N-serve is owing to the selection activity to azotobacter; can be used as nitrogen oxidation retarder and soil nitrogenous fertilizer protectant; when using, and one in nitrogenous fertilizer plain with urea can postpone the oxidation of ammonium ion in the soil; yet its drug effect is shorter; need repeatedly apply N-serve; medication often and dosage big relatively, thereby environment and operator are caused harmful effect.
Summary of the invention
The object of the present invention is to provide that a kind of duration of efficacy is long, toxicity is low, the preparation method of the 15%-30% N-serve micro-capsule suspension of safe ready, it can overcome the existing problem of use of existing N-serve.
The object of the present invention is achieved like this, and a kind of preparation method of N-serve micro-capsule suspension is characterized in that, comprises the steps:
1), the preparation gross weight is little colloidal suspension agent of one kilogram, get the 15%-30%2-chloro-6-trichloromethyl pyridine that accounts for gross weight, be dissolved in the 10-25% toluene that accounts for gross weight, and in solution, add the 2-4.5%NP-10 emulsifier account for gross weight, add a spot of defoamer simultaneously, after stirring, add the 18-35% urea-formaldehyde resin solution that accounts for gross weight again;
2), above-mentioned mixed solution sheared 40 minutes with high-shear homogenizer under the 3000r/min rotating speed, fully disperseed the back to reduce rotating speed, slowly adding concentration under the 800-1000r/min rotating speed in batches is 37% hydrochloric acid, in 0.5 hour pH value is transferred to 4-5; In one hour pH value is transferred to 2.5-3;
3), after pH value mixes up, acidification reaction 1 hour is wrapped up oil phase substance, forms microcapsule granule;
4), with the microcapsule granule that forms, in 20 minutes, rotating speed is dropped to 200r/min, temperature is controlled at 40-50 ℃, solidifies 1 hour;
5), regulate pH value to 5-7 with the 7.5-15% sodium hydrate aqueous solution, add the 10-25%NP-10 emulsifier, regulate viscosity in right amount, just can obtain stable micro-capsule suspension.
The making step of described urea-formaldehyde resin solution is as follows: 80 gram urea and 164 grams, 37% formalin are put into there-necked flask, back adding 2 gram organic bases stir, regulate PH to 7-9, be warming up to 50-60 ℃, stirring at low speed insulation 1 hour gets transparent thick liquid, adds 200 gram water at last, mix, be urea-formaldehyde resin solution.
The product that the present invention produces is under the storage at normal temperature condition, and good stability with an organic solvent lacks, and environmental pollution is few, and the slowly-releasing drug effect has prolonged effective drug duration, has reduced the medication number of times, has saved cost greatly, has avoided the injury to the operator.
Embodiment
Making to 15%-30%2-chloro-6-trichloromethyl pyridine micro-capsule suspension specifies as follows below:
Embodiment: be example with 20%2-chloro-6-trichloromethyl pyridine micro-capsule suspension
One, the preparation of Lauxite
80 gram urea and 164 grams, 37% formalin are put into there-necked flask, and the back that stirs adds 2 gram organic bases, regulates pH value to 7-9, be warming up to 50-60 ℃, stirring at low speed insulation 1 hour gets transparent thick liquid, add 200 gram water at last, mix, get stable urea-formaldehyde resin solution.
Two. preparing one kilogram of little colloidal suspension agent is example
The preparation gross weight is little colloidal suspension agent of one kilogram, get the 20%2-chloro-6-trichloromethyl pyridine that accounts for gross weight, be dissolved in 15% toluene that accounts for gross weight, and in solution, add the 3% NP-10 emulsifier account for gross weight, add a spot of defoamer simultaneously, after stirring, add the 25% above-mentioned urea-formaldehyde resin solution that has made that accounts for gross weight again, above-described mixed solution, under the 3000r/min rotating speed, sheared 40 minutes with high-shear homogenizer, fully disperseing the back to reduce rotating speed, is 37% hydrochloric acid adjusting pH value with concentration under the 800-1000r/min rotating speed.Hydrochloric acid solution will slowly add in batches, in 0.5 hour pH value is transferred to 4-5, continues to regulate pH value with above-mentioned hydrochloric acid solution again, and it is slower to add sour speed, in one hour pH value is transferred to 2.5-3.After pH value was adjusted to the right place, acidification reaction 1 hour was wrapped up oil phase substance, formed microcapsule granule.Reduce rotating speed again to 600r/min, and dropped to 200r/min in 20 minutes, slowly heat up, solidify, temperature is controlled at 40-50 ℃, 1 hour hardening time.Regulate pH value to 5-7 with 10% sodium hydrate aqueous solution again, add the 15%NP-10 emulsifier at last, an amount of thickener is regulated viscosity, adds one kilogram of suitable quantity of water ad pond om, just can obtain stable micro-capsule suspension.
Above-described specific embodiment; purpose of the present invention, technical scheme and beneficial effect are further described; institute is understood that; the above only is specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any modification of making, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (2)
1. the preparation method of a N-serve micro-capsule suspension is characterized in that, comprises the steps:
1), the preparation gross weight is little colloidal suspension agent of one kilogram, get the 15%-30%2-chloro-6-trichloromethyl pyridine that accounts for gross weight, be dissolved in the 10-25% toluene that accounts for gross weight, and in solution, add the 2-4.5%NP-10 emulsifier account for gross weight, add a spot of defoamer simultaneously, after stirring, add the 18-35% urea-formaldehyde resin solution that accounts for gross weight again;
2), above-mentioned mixed solution sheared 40 minutes with high-shear homogenizer under the 3000r/min rotating speed, fully disperseed the back to reduce rotating speed, slowly adding concentration under the 800-1000r/min rotating speed in batches is 37% hydrochloric acid, in 0.5 hour pH value is transferred to 4-5; In one hour pH value is transferred to 2.5-3;
3), after pH value mixes up, acidification reaction 1 hour is wrapped up oil phase substance, forms microcapsule granule;
4), with the microcapsule granule that forms, in 20 minutes, rotating speed is dropped to 200r/min, temperature is controlled at 40-50 ℃, solidifies 1 hour;
5), regulate pH value to 5-7 with the 7.5-15% sodium hydrate aqueous solution, add the 10-25%NP-10 emulsifier, regulate viscosity in right amount, just can obtain stable micro-capsule suspension.
2. the preparation method of a kind of N-serve micro-capsule suspension according to claim 1, it is characterized in that, the making step of described urea-formaldehyde resin solution is as follows: 80 gram urea and 164 grams, 37% formalin are put into there-necked flask, and the back that stirs adds 2 gram organic bases, regulates PH to 7-9, be warming up to 50-60 ℃, stirring at low speed insulation 1 hour gets transparent thick liquid, adds 200 gram water at last, mix, be urea-formaldehyde resin solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013100904482A CN103202298A (en) | 2013-03-21 | 2013-03-21 | Method for manufacturing 2-chlorine-6-nitrapyrin microcapsule suspending agents |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013100904482A CN103202298A (en) | 2013-03-21 | 2013-03-21 | Method for manufacturing 2-chlorine-6-nitrapyrin microcapsule suspending agents |
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| Publication Number | Publication Date |
|---|---|
| CN103202298A true CN103202298A (en) | 2013-07-17 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2013100904482A Pending CN103202298A (en) | 2013-03-21 | 2013-03-21 | Method for manufacturing 2-chlorine-6-nitrapyrin microcapsule suspending agents |
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| Country | Link |
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| CN (1) | CN103202298A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104276907A (en) * | 2014-10-28 | 2015-01-14 | 浙江奥复托化工有限公司 | Environment-friendly type controlled-release nitrogen fertilizer preparation and preparation method thereof |
| CN106458783A (en) * | 2014-05-02 | 2017-02-22 | 美国陶氏益农公司 | Microencapsulated nitrification inhibitor composition |
| CN107285968A (en) * | 2017-07-25 | 2017-10-24 | 张忠庆 | Delay microcapsules suspension formulation of control-release function and its preparation method and application with nitrogenous fertilizer |
| CN110602948A (en) * | 2017-03-17 | 2019-12-20 | 美国陶氏益农公司 | Microencapsulated nitrification inhibitor compositions |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090227458A1 (en) * | 2007-01-22 | 2009-09-10 | Dow Agrosciences Llc | Enhanced nitrification inhibitor composition |
| CN102187871A (en) * | 2010-11-22 | 2011-09-21 | 南通联农农药制剂研究开发有限公司 | Thiacloprid microcapsule preparation and preparation method thereof |
| CN102239831A (en) * | 2011-05-03 | 2011-11-16 | 谭晓辉 | Lythidathion microcapsule suspending agent and preparation method |
| WO2011156048A1 (en) * | 2010-06-07 | 2011-12-15 | Dow Agrosciences Llc | Microcapsule suspensions including high levels of agriculturally active ingredients |
-
2013
- 2013-03-21 CN CN2013100904482A patent/CN103202298A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090227458A1 (en) * | 2007-01-22 | 2009-09-10 | Dow Agrosciences Llc | Enhanced nitrification inhibitor composition |
| WO2011156048A1 (en) * | 2010-06-07 | 2011-12-15 | Dow Agrosciences Llc | Microcapsule suspensions including high levels of agriculturally active ingredients |
| CN102187871A (en) * | 2010-11-22 | 2011-09-21 | 南通联农农药制剂研究开发有限公司 | Thiacloprid microcapsule preparation and preparation method thereof |
| CN102239831A (en) * | 2011-05-03 | 2011-11-16 | 谭晓辉 | Lythidathion microcapsule suspending agent and preparation method |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106458783A (en) * | 2014-05-02 | 2017-02-22 | 美国陶氏益农公司 | Microencapsulated nitrification inhibitor composition |
| JP2017518249A (en) * | 2014-05-02 | 2017-07-06 | ダウ アグロサイエンシィズ エルエルシー | Microencapsulated nitrification inhibitor composition |
| CN104276907A (en) * | 2014-10-28 | 2015-01-14 | 浙江奥复托化工有限公司 | Environment-friendly type controlled-release nitrogen fertilizer preparation and preparation method thereof |
| CN110602948A (en) * | 2017-03-17 | 2019-12-20 | 美国陶氏益农公司 | Microencapsulated nitrification inhibitor compositions |
| CN110602948B (en) * | 2017-03-17 | 2022-04-01 | 美国陶氏益农公司 | Microencapsulated nitrification inhibitor compositions |
| CN107285968A (en) * | 2017-07-25 | 2017-10-24 | 张忠庆 | Delay microcapsules suspension formulation of control-release function and its preparation method and application with nitrogenous fertilizer |
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Application publication date: 20130717 |