CN114246182A - Pendimethalin microcapsule suspending agent and production process thereof - Google Patents
Pendimethalin microcapsule suspending agent and production process thereof Download PDFInfo
- Publication number
- CN114246182A CN114246182A CN202111680832.9A CN202111680832A CN114246182A CN 114246182 A CN114246182 A CN 114246182A CN 202111680832 A CN202111680832 A CN 202111680832A CN 114246182 A CN114246182 A CN 114246182A
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- CN
- China
- Prior art keywords
- parts
- agent
- pendimethalin
- adsorbent
- wall material
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- 239000005591 Pendimethalin Substances 0.000 title claims abstract description 93
- CHIFOSRWCNZCFN-UHFFFAOYSA-N pendimethalin Chemical compound CCC(CC)NC1=C([N+]([O-])=O)C=C(C)C(C)=C1[N+]([O-])=O CHIFOSRWCNZCFN-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 239000003094 microcapsule Substances 0.000 title claims abstract description 48
- 239000000375 suspending agent Substances 0.000 title claims abstract description 46
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 239000003463 adsorbent Substances 0.000 claims abstract description 59
- 239000012071 phase Substances 0.000 claims abstract description 36
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000000725 suspension Substances 0.000 claims abstract description 32
- 239000002245 particle Substances 0.000 claims abstract description 31
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 29
- 238000002156 mixing Methods 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 27
- 239000000839 emulsion Substances 0.000 claims abstract description 23
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 14
- 238000010008 shearing Methods 0.000 claims abstract description 12
- 125000001165 hydrophobic group Chemical group 0.000 claims abstract description 5
- 239000008346 aqueous phase Substances 0.000 claims abstract description 3
- 230000000379 polymerizing effect Effects 0.000 claims abstract description 3
- 239000010902 straw Substances 0.000 claims description 47
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 45
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 239000003795 chemical substances by application Substances 0.000 claims description 23
- 239000007788 liquid Substances 0.000 claims description 19
- 239000003921 oil Substances 0.000 claims description 19
- 239000007853 buffer solution Substances 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 17
- 239000002994 raw material Substances 0.000 claims description 17
- 239000002270 dispersing agent Substances 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 16
- 239000002562 thickening agent Substances 0.000 claims description 16
- 238000010335 hydrothermal treatment Methods 0.000 claims description 12
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 11
- 235000007164 Oryza sativa Nutrition 0.000 claims description 11
- 239000012752 auxiliary agent Substances 0.000 claims description 11
- 239000012024 dehydrating agents Substances 0.000 claims description 11
- 235000009566 rice Nutrition 0.000 claims description 11
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 239000000467 phytic acid Substances 0.000 claims description 10
- 229940068041 phytic acid Drugs 0.000 claims description 10
- 235000002949 phytic acid Nutrition 0.000 claims description 10
- 239000003755 preservative agent Substances 0.000 claims description 10
- 230000002335 preservative effect Effects 0.000 claims description 10
- 108010059892 Cellulase Proteins 0.000 claims description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 9
- 229910052782 aluminium Inorganic materials 0.000 claims description 9
- 229940106157 cellulase Drugs 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 9
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 8
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 claims description 8
- 239000001639 calcium acetate Substances 0.000 claims description 8
- 235000011092 calcium acetate Nutrition 0.000 claims description 8
- 229960005147 calcium acetate Drugs 0.000 claims description 8
- 239000003995 emulsifying agent Substances 0.000 claims description 8
- 230000001681 protective effect Effects 0.000 claims description 8
- 239000010903 husk Substances 0.000 claims description 7
- 239000004014 plasticizer Substances 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 7
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical group [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 6
- 239000000853 adhesive Substances 0.000 claims description 6
- 230000001070 adhesive effect Effects 0.000 claims description 6
- 239000001099 ammonium carbonate Substances 0.000 claims description 6
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 239000008096 xylene Substances 0.000 claims description 6
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- 239000002518 antifoaming agent Substances 0.000 claims description 5
- 239000012295 chemical reaction liquid Substances 0.000 claims description 5
- 239000013530 defoamer Substances 0.000 claims description 5
- 230000002255 enzymatic effect Effects 0.000 claims description 5
- 238000007493 shaping process Methods 0.000 claims description 5
- 229910021487 silica fume Inorganic materials 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 239000007974 sodium acetate buffer Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- 239000000413 hydrolysate Substances 0.000 claims description 3
- 239000012265 solid product Substances 0.000 claims description 3
- 108010009736 Protein Hydrolysates Proteins 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 239000004411 aluminium Substances 0.000 claims 1
- 239000011148 porous material Substances 0.000 claims 1
- 238000003973 irrigation Methods 0.000 abstract description 8
- 230000002262 irrigation Effects 0.000 abstract description 8
- 239000000575 pesticide Substances 0.000 abstract description 6
- 230000000361 pesticidal effect Effects 0.000 abstract description 5
- 238000009991 scouring Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 description 28
- 230000000052 comparative effect Effects 0.000 description 18
- 230000000694 effects Effects 0.000 description 11
- 241000209094 Oryza Species 0.000 description 10
- 239000000835 fiber Substances 0.000 description 10
- 230000002035 prolonged effect Effects 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 230000000857 drug effect Effects 0.000 description 8
- 238000001179 sorption measurement Methods 0.000 description 8
- 239000001913 cellulose Substances 0.000 description 7
- 229920002678 cellulose Polymers 0.000 description 7
- 239000002689 soil Substances 0.000 description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 150000003863 ammonium salts Chemical class 0.000 description 4
- 238000010494 dissociation reaction Methods 0.000 description 4
- 230000005593 dissociations Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 3
- 230000007847 structural defect Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 239000004721 Polyphenylene oxide Substances 0.000 description 2
- 239000002775 capsule Substances 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N glycerol group Chemical group OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 229920000570 polyether Polymers 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000007226 seed germination Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000008093 supporting effect Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000000230 xanthan gum Substances 0.000 description 2
- 229920001285 xanthan gum Polymers 0.000 description 2
- 229940082509 xanthan gum Drugs 0.000 description 2
- 235000010493 xanthan gum Nutrition 0.000 description 2
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 description 1
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical group [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 230000032823 cell division Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 125000005442 diisocyanate group Chemical group 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- JGOICJFFICGNEJ-UHFFFAOYSA-M disodium;3-[dihydroxy(oxido)silyl]propanoate Chemical compound [Na+].[Na+].O[Si](O)([O-])CCC([O-])=O JGOICJFFICGNEJ-UHFFFAOYSA-M 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229940088598 enzyme Drugs 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000035558 fertility Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000002363 herbicidal effect Effects 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 230000000442 meristematic effect Effects 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- LZGUHMNOBNWABZ-UHFFFAOYSA-N n-nitro-n-phenylnitramide Chemical compound [O-][N+](=O)N([N+]([O-])=O)C1=CC=CC=C1 LZGUHMNOBNWABZ-UHFFFAOYSA-N 0.000 description 1
- PSZYNBSKGUBXEH-UHFFFAOYSA-M naphthalene-1-sulfonate Chemical compound C1=CC=C2C(S(=O)(=O)[O-])=CC=CC2=C1 PSZYNBSKGUBXEH-UHFFFAOYSA-M 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 229920000056 polyoxyethylene ether Polymers 0.000 description 1
- 229940051841 polyoxyethylene ether Drugs 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 1
- 239000004299 sodium benzoate Substances 0.000 description 1
- 235000010234 sodium benzoate Nutrition 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000004546 suspension concentrate Substances 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
- A01N33/16—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds containing nitrogen-to-oxygen bonds
- A01N33/18—Nitro compounds
-
- 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
- A01N25/02—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 liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
-
- 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
- A01N25/26—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 in coated particulate form
- A01N25/28—Microcapsules or nanocapsules
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Environmental Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Plant Pathology (AREA)
- Agronomy & Crop Science (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Toxicology (AREA)
- Dispersion Chemistry (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The application relates to the technical field of pesticide production, and particularly discloses a pendimethalin microcapsule suspending agent and a production process thereof. The microcapsule suspending agent is prepared by mixing a polymerization solution and a suspension treatment solution and then performing suspension treatment, wherein the polymerization solution is prepared by polymerizing an emulsion and a wall material, the emulsion is prepared by mixing an aqueous phase containing an adsorbent and an oil phase containing pendimethalin and then shearing and removing the adsorbent, and the adsorbent is carbon particles with surfaces grafted with a hydrophobic group and a hydrophilic group simultaneously. The pendimethalin microcapsule suspending agent reduces the possibility of scouring pendimethalin in the environment by centralized irrigation, and prolongs the pesticide effect duration of the suspending agent.
Description
Technical Field
The application relates to the technical field of pesticides, in particular to a pendimethalin microcapsule suspending agent and a production process thereof.
Background
Pendimethalin is an organic compound with a molecular formula of C13H19N3O4, and belongs to a dinitroaniline herbicide. Pendimethalin mainly inhibits meristematic cell division, does not affect weed seed germination, but acts after the sprouts, stems and roots absorb the medicament in the process of weed seed germination. In practical applications, in order to improve the action effect of pendimethalin, pesticide manufacturers usually formulate pendimethalin into a suspension for sale.
Chinese patent with publication number CN102396450B discloses a pendimethalin suspending agent, which comprises the following components in percentage by weight: 38-42% of pendimethalin, 0.1-6% of acrylic acid maleic anhydride copolymer, 0.1-6% of polyoxyethylene ether, 2-3.5% of condensed naphthalene sulfonate, 0.4-1.2% of alkyl naphthenate, 0.05-0.15% of xanthan gum, 0.01-0.5% of isooctyl alcohol, 0.3-4.0% of dimethyl silicone oil, 4.5-5.5% of ethylene glycol, 0.1% of sodium benzoate and the balance of water.
In view of the above-mentioned related technologies, the inventors believe that pendimethalin is prepared into a suspending agent in the related technologies, and although pendimethalin has a strong capability of resisting rainwater leaching, pendimethalin released by the pendimethalin suspending agent is still easy to run off under the washing condition of artificial centralized irrigation, which results in a shortened duration of the efficacy of pendimethalin.
Disclosure of Invention
In the related technology, pendimethalin is easy to run off under the scouring condition of manual centralized irrigation, so that the duration of the pesticide effect of pendimethalin is shortened. In order to improve the defect, the application provides a pendimethalin microcapsule suspending agent and a production process thereof.
In a first aspect, the application provides a pendimethalin microcapsule suspending agent, which adopts the following technical scheme:
a pendimethalin microcapsule suspending agent is prepared by mixing a polymerization liquid and a suspension treatment liquid and then performing suspension treatment on the mixture, wherein the polymerization liquid is prepared by polymerizing an emulsion and a wall material, the emulsion is prepared by mixing an aqueous phase containing an adsorbent and an oil phase containing pendimethalin and then performing shearing processing on the mixture and removing the adsorbent, and the adsorbent is carbon particles with surfaces grafted with a hydrophobic group and a hydrophilic group; the formula of the pendimethalin microcapsule suspending agent comprises the following raw materials in parts by weight: 0.35-0.55 part of protective adhesive, 1.25-1.45 parts of first dispersing agent, 2.10-2.30 parts of emulsifier, 12-16 parts of adsorbent, 0.35-0.55 part of defoamer, 31-35 parts of pendimethalin, 12.5-14.5 parts of xylene, 3.25-3.45 parts of first wall material, 3.2-3.6 parts of second wall material, 3-5 parts of second dispersing agent, 0.4-0.6 part of preservative, 0.03-0.07 part of first thickening agent, 0.3-0.7 part of non-second thickening agent, 2.0-4.0 parts of antifreezing agent and 32-36 parts of water.
Through adopting above-mentioned technical scheme, this application has changed the formula system of suspending agent, wraps up pendimethalin through the wall material, has made pendimethalin the suspending agent that exists with the capsule form, after the suspending agent of this application of using, the microcapsule plays the slow-release effect to pendimethalin to the mobility of microcapsule is worse with free pendimethalin, thereby has reduced the concentrated irrigation and has caused the possibility of erodeing to pendimethalin in the environment, has prolonged the drug effect duration of suspending agent.
In the preparation of pendimethalin microcapsule suspension formulations of the present application, emulsification occurs with the aid of an adsorbent after mixing the aqueous and oil phases. Because the surface of the adsorbent is simultaneously grafted with the hydrophilic group and the hydrophobic group, the interfacial tension between the water phase and the oil phase is reduced, so that the adsorbent can simultaneously adsorb the water phase and the oil phase, the blending between the water phase and the oil phase is promoted, and the uniformity of the emulsion is improved. By improving the uniformity of the emulsion, the probability of failure of wrapping pendimethalin by the wall material due to uneven distribution of pendimethalin is reduced, and the pesticide effect duration of the suspending agent is prolonged.
Preferably, the formula of the pendimethalin microcapsule suspending agent comprises the following raw materials in parts by weight: 0.40-0.50 part of protective adhesive, 1.30-1.40 parts of first dispersing agent, 2.15-2.25 parts of emulsifier, 13-15 parts of adsorbent, 0.40-0.50 part of defoamer, 32-34 parts of pendimethalin, 13.0-14.0 parts of xylene, 3.30-3.40 parts of first wall material, 3.3-3.5 parts of second wall material, 3.5-4.5 parts of second dispersing agent, 0.45-0.55 part of preservative, 0.04-0.06 part of first thickening agent, 0.4-0.6 part of non-second thickening agent, 2.5-3.5 parts of antifreezing agent and 33-35 parts of water.
By adopting the technical scheme, the raw material proportion of the pendimethalin microcapsule suspending agent is optimized, and the duration of the drug effect of the suspending agent is prolonged.
Preferably, the preparation method of the adsorbent comprises the following steps:
(1) drying the straws and then crushing to obtain straw powder;
(2) uniformly mixing straw powder, cellulase and a buffer solution, and standing to obtain straw enzymatic hydrolysate;
(3) uniformly mixing straw enzymatic hydrolysate, a bonding auxiliary agent, a shaping agent, citric acid, a dehydrating agent and a carbonate pore-forming agent to obtain a raw material solution, and carrying out hydrothermal treatment on a reaction solution under an oxygen-free closed condition to obtain a reaction solution; (4) and (3) carrying out solid-liquid separation on the reaction liquid, then crushing a solid product obtained by separation to obtain carbon particles, and treating the carbon particles by using a silane coupling agent to obtain the adsorbent.
By adopting the technical scheme, the straw is used as a carbon source, cells in the straw are dissociated by crushing and enzymolysis, then the carbon particles are obtained by means of hydrothermal treatment, and then the carbon particles are subjected to graft modification by the silane coupling agent, so that the hydrophilic group and the hydrophobic group are grafted on the surfaces of the carbon particles to obtain the adsorbent.
In the process of hydrothermal treatment, straw fibers in the straws are damaged by crushing, so that the cellulose can permeate easily, the dissociation degree of the straw fibers is increased by the crushing treatment and the cellulose treatment together, and the adsorption performance of the adsorbent is improved. The bonding auxiliary agent bonds the residual straw part in the straw enzymolysis liquid and combines the residual straw part with the plasticizer into a carbon particle precursor. The citric acid is used for acidifying the straw fibers in the raw material liquid, so that the dissociation degree of the straw fibers is further increased, and the citric acid is reacted with a carbonate pore-forming agent, so that micro bubbles appear in the carbon particle precursor, and the porosity of the adsorbent is increased. After the straw fibers are further dissociated by the citric acid, the dehydrating agent permeates into the straw fibers, and the straw fibers are dehydrated and carbonized, so that the carbonization process of the straws is accelerated. And (3) completely carbonizing the carbon particle precursor to obtain the carbon particles.
Preferably, the adsorbent is prepared from the following raw materials in parts by weight: 100-120 parts of straw powder, 6-8 parts of cellulase, 20-40 parts of buffer solution, 6-10 parts of bonding auxiliary agent, 4-6 parts of shaping agent, 6-10 parts of citric acid, 4-8 parts of dehydrating agent and 8-12 parts of carbonate pore-forming agent.
By adopting the technical scheme, the adsorbent is prepared by taking straw powder, cellulase, buffer solution, bonding auxiliary agent, plasticizer, citric acid, dehydrating agent and carbonate pore-forming agent as raw materials and optimizing the dosage of each raw material.
Preferably, the buffer solution is an acetic acid/calcium acetate buffer solution or an acetic acid/sodium acetate buffer solution.
Through adopting above-mentioned technical scheme, acetic acid/calcium acetate buffer solution and acetic acid/sodium acetate buffer solution all can reduce the influence of PH change to cellulase activity, wherein, when electing with acetic acid/calcium acetate buffer solution, calcium acetate can decompose the production calcium carbonate in hydrothermal treatment in-process, can produce carbon dioxide after calcium carbonate reacts with citric acid, thereby microbubble content in the hydrothermal treatment system has been increased, help improving the porosity that increases the adsorbent, help improving the adsorption efficiency of adsorbent, be favorable to reducing the loss of pendimethalin, the drug effect duration of suspending agent has been prolonged.
Preferably, the dehydrating agent is phosphoric acid or phytic acid.
Through adopting above-mentioned technical scheme, phosphoric acid and phytic acid all can make straw fiber dehydration carbomorphism, the shortcoming of phytic acid is that the molecular volume is great, the diffusivity is poor, and in this application, because citric acid has promoted the dissociation of straw fiber, consequently, the poor defect of phytic acid diffusivity has been overcome, organic chain segment in the phytic acid molecule can also participate in the carbomorphism simultaneously, thereby improved the completeness of charcoal granule, help improving the adsorption efficiency of adsorbent, be favorable to reducing the loss of pendimethalin, the drug effect duration of suspending agent has been prolonged. In addition, when the buffer solution is acetic acid/calcium acetate buffer solution, phosphoric acid and phytic acid can also combine with a part of calcium ions to generate chelate precipitation, thereby providing a growth point for the formation of the carbon particle precursor, promoting the generation of carbon particles and helping to shorten the production period of the adsorbent.
Preferably, the bonding aid is selected from silica sol or aluminum sol.
By adopting the technical scheme, the silica sol and the aluminum sol can be polymerized under the heating condition, so that the straw powder is bonded. The main component of the straw powder is cellulose, the cellulose has negative charges in water, and the colloidal particles of the aluminum sol have positive charges in water, so that the aluminum sol is easily combined with the straw powder, and the bonding effect of the aluminum sol on the straw powder is better than that of the silica sol.
Preferably, the plasticizer is rice husk or silica fume.
By adopting the technical scheme, the rice hull ash and the silica fume both contain a large amount of silica components, and when the bonding auxiliary agent is silica sol or alumina sol, the rice hull ash and the silica fume both can be combined with the bonding auxiliary agent, so that the carbon particles obtained through hydrothermal treatment contain the silica components. The silicon dioxide plays a supporting role on the structure of the carbon particles, reduces the structural defects of the carbon particles and is beneficial to improving the adsorption performance of the adsorbent. The cellulose contained in the rice hulls can be carbonized in the hydrothermal treatment process, so that the structural defects in carbon particles are reduced, the adsorption performance of the adsorbent is improved, the loss of pendimethalin is reduced, and the pesticide effect duration of the suspending agent is prolonged.
Preferably, the carbonate pore-forming agent is ammonium carbonate or sodium carbonate.
By adopting the technical scheme, the sodium carbonate and the ammonium carbonate can generate gas after reacting with the citric acid, wherein the ammonium salt remained in the carbon particles after the ammonium carbonate reacts with the citric acid. When the adsorbent made of carbon particles is used for assisting the emulsification of the water phase and the oil phase, the ammonium salt can be transferred into the emulsion, and finally the ammonium salt becomes a component of the pendimethalin microcapsule suspending agent. While the pendimethalin microcapsule suspending agent is applied, the ammonium salt can supplement nitrogen elements for the soil, so that the soil fertility is enhanced.
In a second aspect, the application provides a production process of a pendimethalin microcapsule suspending agent, and the following technical scheme is adopted.
A production process of pendimethalin microcapsule suspending agent comprises the following steps:
(1) uniformly mixing the protective adhesive, the first dispersing agent, the emulsifier, the defoaming agent, the adsorbent and water to obtain a water phase; uniformly mixing pendimethalin, xylene and a first wall material to obtain an oil phase;
(2) mixing the water phase and the oil phase, shearing the mixture of the water phase and the oil phase, and filtering to remove the adsorbent to obtain an emulsion;
(3) adding a second wall material into the emulsion, and heating and insulating the mixture of the emulsion and the second wall material to obtain a polymerization solution;
(4) and mixing the second dispersing agent, the antifreezing agent, the first thickening agent, the second thickening agent and the preservative to obtain a suspension treatment liquid, adding the suspension treatment liquid into the polymerization liquid, and shearing again to obtain the pendimethalin microcapsule suspending agent.
Through adopting above-mentioned technical scheme, this application has carried out mixed shearing to water phase and oil phase under the assistance of adsorbent, has obtained the emulsion, has made pendimethalin microcapsule suspending agent with the emulsion through polymerization processing and suspension processing again.
In summary, the present application has the following beneficial effects:
1. this application carries out the cladding with the wall material to pendimethalin, has made the microcapsule suspending agent with pendimethalin, and the capsule plays the slow release effect to pendimethalin to reduced the possibility that factors such as irrigation, precipitation led to the fact the washing to pendimethalin in the environment, prolonged the drug effect duration of suspending agent. In addition, when the microcapsule suspending agent is prepared, the adsorbent improves the uniformity of emulsion, reduces the possibility of failure in wrapping pendimethalin by wall materials due to uneven distribution of the pendimethalin, and is beneficial to prolonging the duration time of the pesticide effect of the suspending agent.
2. The preferred silica sol or alumina sol is as the bonding auxiliary agent when preparing the adsorbent in this application, and the micelle of alumina sol and the cellulose in the straw powder are opposite electric charge, consequently the combination between alumina sol and the straw powder is inseparabler for the bond effect of alumina sol to the straw powder is superior to silica sol.
3. According to the method, the water phase and the oil phase are mixed and sheared with the aid of the adsorbent to obtain the emulsion, and the emulsion is prepared into the pendimethalin microcapsule suspending agent through polymerization treatment and suspension treatment.
Detailed Description
The present application will be described in further detail with reference to examples.
The raw materials used in the preparation examples of the application can be obtained commercially, wherein the straws and the rice husks are provided by an Antui Heng renewable resources limited company in Anqing, and the straws are corn straws; the cellulase is food-grade cellulase (enzyme activity is 100000u/g) provided by Jiangsu Ruichi biological science and technology Limited company; the water content of the silica sol and the aluminum sol was 75%.
Preparation example of adsorbent
The following will explain preparation example 1 as an example.
Preparation example 1
In this preparation example, the adsorbent was prepared as follows:
(1) drying the straws at 65 ℃, and then crushing the dried straws to an average particle size of 600 mu m to obtain straw powder;
(2) uniformly mixing 100kg of straw powder, 6kg of cellulase and 20kg of buffer solution, and standing for 36 hours to obtain straw enzymatic hydrolysate; in the step, the buffer solution is acetic acid/sodium acetate buffer solution;
(3) adding 6kg of bonding auxiliary agent, 4kg of plasticizer, 6kg of citric acid, 4kg of dehydrating agent and 8kg of carbonate pore-forming agent into the straw enzymolysis liquid, uniformly mixing to obtain a raw material liquid, carrying out hydrothermal treatment on the reaction liquid at 180 ℃ under an oxygen-free closed condition, and obtaining the reaction liquid after 16 hours of treatment; in the step, the bonding auxiliary agent is silica sol, and the plasticizer is silica fume; the dehydrating agent is phosphoric acid, and the carbonate pore-forming agent is sodium carbonate;
(4) carrying out solid-liquid separation on the reaction liquid, then crushing the solid product obtained by separation to an average particle size of 840 mu m to obtain carbon particles, soaking the carbon particles for 2h by using a silane coupling agent, and drying the carbon particles to obtain an adsorbent; in the step, the silane coupling agent is a product obtained by mixing sodium carboxyethyl silanetriol and methyltriethoxysilane according to a molar ratio of 1: 1.
As shown in Table 1, the production examples 1 to 5 were different in the raw material ratio of the adsorbent.
Preparation example 6
The difference between the preparation example and the preparation example 3 is that the buffer solution is acetic acid/calcium acetate buffer solution.
Preparation example 7
The difference between the preparation example and the preparation example 6 is that phytic acid is used as the dehydrating agent.
Preparation example 8
The difference between the preparation example and the preparation example 7 is that the bonding aid is alumina sol.
Preparation example 9
The difference between the preparation example and the preparation example 8 is that rice hulls are used as the shaping agent.
Preparation example 10
The difference between the preparation example and the preparation example 9 is that ammonium carbonate is used as the carbonate pore-forming agent.
Examples
The raw materials used in the examples of the present application are all commercially available, wherein the polyether defoamer is provided by Jinan Ruiyuan chemical Co., Ltd, the preservative ZN10 is provided by Jinan Zhongsheng chemical Co., Ltd, and the SP-7205, SP-7290, SP-7123, SP-7311 and SP-7450 are provided by Jiangsu Opting chemical science and technology Co., Ltd.
Examples 1 to 5
The following description will be given by taking example 1 as an example.
Example 1
The pendimethalin microcapsule suspension of example 1 was prepared as follows:
(1) uniformly mixing 0.35kg of protective glue, 1.25kg of first dispersing agent, 2.10kg of emulsifier, 0.35kg of defoaming agent, 12kg of adsorbent and 32kg of water to obtain a water phase, and keeping the temperature at 30 ℃ for later use; uniformly mixing 31kg of pendimethalin, 12.5kg of dimethylbenzene and 3.25kg of first wall material to obtain an oil phase, and keeping the temperature at 55 ℃ for later use; in the step, the protective glue is SP-7205, the first dispersing agent is SP-7290, the emulsifier is SP-7123, the defoaming agent is a polyether defoaming agent, the adsorbent is the adsorbent of preparation example 1, and the first wall material is diisocyanate;
(2) mixing the water phase and the oil phase, shearing the mixture of the water phase and the oil phase at a shearing rate of 10000r/min for 3min, and then filtering to remove the adsorbent to obtain an emulsion;
(3) adding 3.2kg of second wall material in total into the emulsion in four batches within 30min, heating the mixture of the emulsion and the second wall material to 60 ℃, and preserving heat for 5h to obtain a polymerization solution; in the step, the second wall material is SP-7311;
(4) mixing 3.0kg of second dispersing agent, 2.0kg of antifreezing agent, 0.03kg of first thickening agent, 0.3kg of second thickening agent and 0.4kg of preservative to obtain suspension treatment liquid, adding the suspension treatment liquid into polymerization liquid, and shearing at the shearing rate of 10000r/min for 3min to obtain pendimethalin microcapsule suspending agent; in the step, the second dispersing agent is SP-7450, the preservative is pesticide preservative ZN10, the antifreezing agent is glycerin, the first thickening agent is xanthan gum, and the second thickening agent is magnesium aluminum silicate.
As shown in Table 2, examples 1 to 5 differ mainly in the ratio of raw materials.
TABLE 2
Example 6
This example is different from example 5 in that the production example of the adsorbent is production example 2.
As shown in Table 3, example 3 is different from examples 5 to 14 in the preparation examples of the adsorbents.
TABLE 3
Comparative example
Comparative example 1
Refer to pendimethalin suspension prepared in example 1 of chinese patent publication No. CN 102396450B.
Comparative example 2
This comparative example differs from example 3 in that no adsorbent was used in the preparation of pendimethalin microcapsule suspension.
Comparative example 3
This comparative example differs from example 3 in that activated carbon was used as the adsorbent in the preparation of pendimethalin microcapsule suspension.
Performance detection test method
The pesticide mobility test is carried out according to the 'chemical pesticide environmental safety evaluation test criterion' (GB/T31270.5-2014), and the rainfall standard in the original test method is only improved to 800mm/48h from 200mm/48h during the test so as to simulate the condition of centralized irrigation. During detection, mixed soil formed by mixing Suzhou yellow brown soil and Changsha red soil according to the weight ratio of 4:6 is adopted to test the mobility grade (R) of pendimethalin in soilf) The test results are shown in Table 4.
TABLE 4
| Sample(s) | Rf | Sample(s) | Rf |
| Example 1 | 0.37 | Example 10 | 0.31 |
| Example 2 | 0.36 | Example 11 | 0.29 |
| Example 3 | 0.35 | Example 12 | 0.28 |
| Example 4 | 0.36 | Example 13 | 0.26 |
| Example 5 | 0.36 | Example 14 | 0.26 |
| Example 6 | 0.34 | Comparative example 1 | 0.57 |
| Example 7 | 0.33 | Comparative example 2 | 0.44 |
| Example 8 | 0.34 | Comparative example 3 | 0.45 |
| Example 9 | 0.34 | / | / |
As can be seen by combining examples 1-5 with comparative example 1 and combining Table 4, the mobility grades measured by examples 1-5 are all lower than that of comparative example 1, which shows that under the condition of concentrated irrigation, the microcapsule of the present application has a slow release effect on pendimethalin, and the mobility of the microcapsule is poorer than that of free pendimethalin, so that the possibility of pendimethalin loss in soil caused by concentrated irrigation is reduced, and the duration of the efficacy of the suspending agent is prolonged.
As can be seen by combining example 3 and comparative examples 1-2 with table 4, the mobility grade measured in example 3 is lower than that of comparative example 1 and comparative example 2, which illustrates that preparing microcapsules helps to reduce the run-off of pendimethalin, but under the condition of no added adsorbent, pendimethalin is unevenly distributed, which results in a part of the wall material failing to wrap pendimethalin, so that the content of free pendimethalin in the pendimethalin microcapsule suspension is increased, and thus the mobility grade measured in example 3 is lower than that of comparative example 2.
As can be seen by combining example 3 and comparative example 3 and table 4, the mobility grade measured in example 3 is lower than that in comparative example 3, which illustrates that when ordinary activated carbon is used as an adsorbent, the activated carbon is difficult to adsorb both the water phase and the oil phase, resulting in uneven distribution of pendimethalin, and also has an influence on the anti-leaching performance of the pendimethalin microcapsule suspension, so that the mobility grade measured in example 3 is lower than that in comparative example 3.
As can be seen by combining example 3 with examples 6-9 and by combining Table 4, the mobility grade measured in example 7 was lower in example 3 and examples 6-9, indicating that the adsorbents made according to the formulation system of preparation 3 are most advantageous in extending the duration of efficacy of the suspending agent in preparations 1-5.
It can be seen from the combination of example 7 and example 10 and the combination of table 4 that the mobility grade measured in example 10 is lower than that in example 7, which indicates that carbon dioxide is generated after calcium carbonate generated by decomposition of calcium acetate during hydrothermal treatment reacts with citric acid, and the carbon dioxide increases the content of microbubbles in the hydrothermal treatment system, thereby improving the adsorption effect of the adsorbent, reducing the loss of pendimethalin and prolonging the duration of the drug effect of the suspending agent.
It can be seen from the combination of example 10 and example 11 and the combination of table 4 that the mobility grade measured in example 11 is lower than that in example 10, which indicates that the citric acid promotes the dissociation of the straw fiber, so that the defect of poor phytic acid diffusivity is overcome, and meanwhile, the organic chain segment in the phytic acid molecule participates in carbonization, so that the integrity of the carbon particles is improved, the adsorption effect of the adsorbent is improved, the loss of pendimethalin is reduced, and the duration of the drug effect of the suspending agent is prolonged.
It can be seen from the combination of example 11 and example 12 and table 4 that the mobility grade measured in example 12 is lower than that in example 11, which indicates that when the bonding aid is aluminum sol, the bonding degree of the aluminum sol and the straw powder is better, so that the coating effect of the microcapsules on pendimethalin is improved, and the loss possibility of pendimethalin is reduced.
It can be seen from the combination of example 13 and example 12 and the combination of table 4 that the mobility grade measured in example 13 is lower than that in example 12, which shows that when the plasticizer is rice husk, silica in the rice husk has a supporting effect on the structure of the carbon particles, and simultaneously cellulose in the rice husk can be carbonized in the hydrothermal treatment process, so that the structural defects in the carbon particles are reduced, and therefore, the rice husk is more favorable for improving the adsorption performance of the adsorbent, reducing the loss of pendimethalin, and prolonging the duration of the drug effect of the suspending agent.
As can be seen by combining example 14, example 13 and table 4, the mobility grade measured in example 14 is close to that of example 13, indicating that replacement of sodium carbonate with ammonium carbonate does not adversely affect the duration of efficacy of the suspension concentrate.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. A pendimethalin microcapsule suspending agent is characterized in that the microcapsule suspending agent is prepared by mixing a polymerization solution and a suspension treatment solution and then performing suspension treatment, the polymerization solution is prepared by polymerizing an emulsion and a wall material, the emulsion is prepared by mixing an aqueous phase containing an adsorbent and an oil phase containing pendimethalin and then performing shearing processing and removing the adsorbent, and the adsorbent is carbon particles with surfaces grafted with a hydrophobic group and a hydrophilic group simultaneously; the formula of the pendimethalin microcapsule suspending agent comprises the following raw materials in parts by weight: 0.35-0.55 part of protective adhesive, 1.25-1.45 parts of first dispersing agent, 2.10-2.30 parts of emulsifier, 12-16 parts of adsorbent, 0.35-0.55 part of defoamer, 31-35 parts of pendimethalin, 12.5-14.5 parts of xylene, 3.25-3.45 parts of first wall material, 3.2-3.6 parts of second wall material, 3-5 parts of second dispersing agent, 0.4-0.6 part of preservative, 0.03-0.07 part of first thickening agent, 0.3-0.7 part of non-second thickening agent, 2.0-4.0 parts of antifreezing agent and 32-36 parts of water.
2. The pendimethalin microcapsule suspension as claimed in claim 1, wherein the pendimethalin microcapsule suspension comprises the following raw materials in parts by weight: 0.40-0.50 part of protective adhesive, 1.30-1.40 parts of first dispersing agent, 2.15-2.25 parts of emulsifier, 13-15 parts of adsorbent, 0.40-0.50 part of defoamer, 32-34 parts of pendimethalin, 13.0-14.0 parts of xylene, 3.30-3.40 parts of first wall material, 3.3-3.5 parts of second wall material, 3.5-4.5 parts of second dispersing agent, 0.45-0.55 part of preservative, 0.04-0.06 part of first thickening agent, 0.4-0.6 part of non-second thickening agent, 2.5-3.5 parts of antifreezing agent and 33-35 parts of water.
3. A pendimethalin microcapsule suspension according to claim 1, wherein the adsorbent is prepared by a process comprising the steps of:
(1) drying the straws and then crushing to obtain straw powder;
(2) uniformly mixing straw powder, cellulase and a buffer solution, and standing to obtain straw enzymatic hydrolysate;
(3) uniformly mixing straw enzymatic hydrolysate, a bonding auxiliary agent, a shaping agent, citric acid, a dehydrating agent and a carbonate pore-forming agent to obtain a raw material solution, and carrying out hydrothermal treatment on a reaction solution under an oxygen-free closed condition to obtain a reaction solution;
(4) and (3) carrying out solid-liquid separation on the reaction liquid, then crushing a solid product obtained by separation to obtain carbon particles, and treating the carbon particles by using a silane coupling agent to obtain the adsorbent.
4. A pendimethalin microcapsule suspension according to claim 3, wherein the adsorbent is prepared from the following raw materials in parts by weight: 100-120 parts of straw powder, 6-8 parts of cellulase, 20-40 parts of buffer solution, 6-10 parts of bonding auxiliary agent, 4-6 parts of shaping agent, 6-10 parts of citric acid, 4-8 parts of dehydrating agent and 8-12 parts of carbonate pore-forming agent.
5. A pendimethalin microcapsule suspension according to claim 4, wherein the buffer solution is an acetic acid/calcium acetate buffer solution or an acetic acid/sodium acetate buffer solution.
6. A pendimethalin microcapsule suspension according to claim 5, wherein the dehydrating agent is phosphoric acid or phytic acid.
7. A pendimethalin microcapsule suspension according to claim 4, wherein the binding aid is selected from silica sol or aluminium sol.
8. A pendimethalin microcapsule suspension according to claim 7, wherein the plasticizer is rice husk or silica fume.
9. A pendimethalin microcapsule suspension as claimed in claim 4, wherein the carbonate pore former is selected from ammonium carbonate or sodium carbonate.
10. A process for the production of a pendimethalin microcapsule suspension according to any of claims 1-9, comprising the steps of:
(1) uniformly mixing the protective adhesive, the first dispersing agent, the emulsifier, the defoaming agent, the adsorbent and water to obtain a water phase; uniformly mixing pendimethalin, xylene and a first wall material to obtain an oil phase;
(2) mixing the water phase and the oil phase, shearing the mixture of the water phase and the oil phase, and filtering to remove the adsorbent to obtain an emulsion;
(3) adding a second wall material into the emulsion, and heating and insulating the mixture of the emulsion and the second wall material to obtain a polymerization solution;
(4) and mixing the second dispersing agent, the antifreezing agent, the first thickening agent, the second thickening agent and the preservative to obtain a suspension treatment liquid, adding the suspension treatment liquid into the polymerization liquid, and shearing again to obtain the pendimethalin microcapsule suspending agent.
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| CN107980770A (en) * | 2017-11-20 | 2018-05-04 | 联合国南通农药剂型开发中心（江苏省农药新剂型及新助剂工程技术研究中心、南通精细化工生产力促进中心） | A kind of microcapsule suspending agent of propargite and its preparation method and application |
| CN109497061A (en) * | 2018-12-21 | 2019-03-22 | 江苏精禾界面科技有限公司 | A kind of pendimethalin microcapsule suspending agent and preparation method thereof |
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