CN106973990A - A kind of fumigating method for being used to prevent and treat grain entomophthora - Google Patents
A kind of fumigating method for being used to prevent and treat grain entomophthora Download PDFInfo
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- CN106973990A CN106973990A CN201610033963.0A CN201610033963A CN106973990A CN 106973990 A CN106973990 A CN 106973990A CN 201610033963 A CN201610033963 A CN 201610033963A CN 106973990 A CN106973990 A CN 106973990A
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- Prior art keywords
- substituted
- fumigant
- grain
- mould
- insect
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- 238000000034 method Methods 0.000 title claims abstract description 21
- 241001480508 Entomophthora Species 0.000 title claims abstract description 13
- 239000002316 fumigant Substances 0.000 claims abstract description 193
- 150000001875 compounds Chemical class 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 6
- 229910052731 fluorine Inorganic materials 0.000 claims description 20
- 229910052801 chlorine Inorganic materials 0.000 claims description 16
- 239000000460 chlorine Substances 0.000 claims description 16
- 229910052739 hydrogen Inorganic materials 0.000 claims description 16
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 16
- 239000001257 hydrogen Substances 0.000 claims description 14
- 125000001997 phenyl group Chemical class [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 14
- 150000002431 hydrogen Chemical class 0.000 claims description 12
- 239000011737 fluorine Substances 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000000741 silica gel Substances 0.000 claims description 10
- 229910002027 silica gel Inorganic materials 0.000 claims description 10
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 8
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 claims description 8
- 229910052794 bromium Inorganic materials 0.000 claims description 8
- 229910052736 halogen Inorganic materials 0.000 claims description 8
- 150000002367 halogens Chemical group 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 125000005073 adamantyl group Chemical group C12(CC3CC(CC(C1)C3)C2)* 0.000 claims description 7
- 239000012876 carrier material Substances 0.000 claims description 6
- 125000002947 alkylene group Chemical group 0.000 claims description 5
- 238000006467 substitution reaction Methods 0.000 claims description 5
- 125000005913 (C3-C6) cycloalkyl group Chemical group 0.000 claims description 4
- 125000006552 (C3-C8) cycloalkyl group Chemical group 0.000 claims description 4
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 4
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 4
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 4
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
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- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 abstract description 30
- 201000010099 disease Diseases 0.000 abstract description 29
- 230000007613 environmental effect Effects 0.000 abstract description 4
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- 235000010469 Glycine max Nutrition 0.000 description 48
- 241000223259 Trichoderma Species 0.000 description 38
- 238000001514 detection method Methods 0.000 description 31
- 238000012544 monitoring process Methods 0.000 description 26
- 238000012360 testing method Methods 0.000 description 25
- 244000017020 Ipomoea batatas Species 0.000 description 24
- 235000002678 Ipomoea batatas Nutrition 0.000 description 24
- 244000061456 Solanum tuberosum Species 0.000 description 24
- 235000002595 Solanum tuberosum Nutrition 0.000 description 24
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- 235000002017 Zea mays subsp mays Nutrition 0.000 description 24
- 238000004458 analytical method Methods 0.000 description 24
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- 230000000284 resting effect Effects 0.000 description 24
- 241000228212 Aspergillus Species 0.000 description 19
- 241000193830 Bacillus <bacterium> Species 0.000 description 19
- 241000194107 Bacillus megaterium Species 0.000 description 19
- 241001149956 Cladosporium herbarum Species 0.000 description 19
- 241000588724 Escherichia coli Species 0.000 description 19
- 241000589540 Pseudomonas fluorescens Species 0.000 description 19
- 241000191967 Staphylococcus aureus Species 0.000 description 19
- 241001674044 Blattodea Species 0.000 description 18
- 241001177117 Lasioderma serricorne Species 0.000 description 18
- 241001124553 Lepismatidae Species 0.000 description 18
- 241000595629 Plodia interpunctella Species 0.000 description 18
- 241000318997 Rhyzopertha dominica Species 0.000 description 18
- 241000130771 Tinea pellionella Species 0.000 description 18
- HEDRZPFGACZZDS-MICDWDOJSA-N Trichloro(2H)methane Chemical compound [2H]C(Cl)(Cl)Cl HEDRZPFGACZZDS-MICDWDOJSA-N 0.000 description 18
- 238000004817 gas chromatography Methods 0.000 description 18
- 238000010813 internal standard method Methods 0.000 description 18
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 17
- 238000005070 sampling Methods 0.000 description 17
- 239000003795 chemical substances by application Substances 0.000 description 14
- 238000005160 1H NMR spectroscopy Methods 0.000 description 9
- GZUXJHMPEANEGY-UHFFFAOYSA-N bromomethane Chemical compound BrC GZUXJHMPEANEGY-UHFFFAOYSA-N 0.000 description 9
- 239000002245 particle Substances 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- 238000007689 inspection Methods 0.000 description 7
- 238000003860 storage Methods 0.000 description 7
- 229920000858 Cyclodextrin Polymers 0.000 description 6
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 6
- 231100000678 Mycotoxin Toxicity 0.000 description 6
- 239000003086 colorant Substances 0.000 description 6
- 239000002636 mycotoxin Substances 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 description 6
- 235000013305 food Nutrition 0.000 description 5
- OBTWBSRJZRCYQV-UHFFFAOYSA-N sulfuryl difluoride Chemical compound FS(F)(=O)=O OBTWBSRJZRCYQV-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 231100000614 poison Toxicity 0.000 description 4
- 239000002574 poison Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 241000228197 Aspergillus flavus Species 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- BAVONGHXFVOKBV-UHFFFAOYSA-N Carveol Chemical compound CC(=C)C1CC=C(C)C(O)C1 BAVONGHXFVOKBV-UHFFFAOYSA-N 0.000 description 2
- KRCZYMFUWVJCLI-UHFFFAOYSA-N Dihydrocarveol Chemical compound CC1CCC(C(C)=C)CC1O KRCZYMFUWVJCLI-UHFFFAOYSA-N 0.000 description 2
- 241000233866 Fungi Species 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 2
- QOSMNYMQXIVWKY-UHFFFAOYSA-N Propyl levulinate Chemical compound CCCOC(=O)CCC(C)=O QOSMNYMQXIVWKY-UHFFFAOYSA-N 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical group O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 2
- 230000036760 body temperature Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- QMVPMAAFGQKVCJ-UHFFFAOYSA-N citronellol Chemical compound OCCC(C)CCC=C(C)C QMVPMAAFGQKVCJ-UHFFFAOYSA-N 0.000 description 2
- ZYTMANIQRDEHIO-KXUCPTDWSA-N isopulegol Chemical compound C[C@@H]1CC[C@@H](C(C)=C)[C@H](O)C1 ZYTMANIQRDEHIO-KXUCPTDWSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 150000003459 sulfonic acid esters Chemical class 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- NOOLISFMXDJSKH-UTLUCORTSA-N (+)-Neomenthol Chemical compound CC(C)[C@@H]1CC[C@@H](C)C[C@@H]1O NOOLISFMXDJSKH-UTLUCORTSA-N 0.000 description 1
- BAVONGHXFVOKBV-ZJUUUORDSA-N (-)-trans-carveol Natural products CC(=C)[C@@H]1CC=C(C)[C@@H](O)C1 BAVONGHXFVOKBV-ZJUUUORDSA-N 0.000 description 1
- 239000001871 (1R,2R,5S)-5-methyl-2-prop-1-en-2-ylcyclohexan-1-ol Substances 0.000 description 1
- QMVPMAAFGQKVCJ-SNVBAGLBSA-N (R)-(+)-citronellol Natural products OCC[C@H](C)CCC=C(C)C QMVPMAAFGQKVCJ-SNVBAGLBSA-N 0.000 description 1
- JECYNCQXXKQDJN-UHFFFAOYSA-N 2-(2-methylhexan-2-yloxymethyl)oxirane Chemical compound CCCCC(C)(C)OCC1CO1 JECYNCQXXKQDJN-UHFFFAOYSA-N 0.000 description 1
- 229930195730 Aflatoxin Natural products 0.000 description 1
- XWIYFDMXXLINPU-UHFFFAOYSA-N Aflatoxin G Chemical compound O=C1OCCC2=C1C(=O)OC1=C2C(OC)=CC2=C1C1C=COC1O2 XWIYFDMXXLINPU-UHFFFAOYSA-N 0.000 description 1
- 241000228230 Aspergillus parasiticus Species 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- NOOLISFMXDJSKH-UHFFFAOYSA-N DL-menthol Natural products CC(C)C1CCC(C)CC1O NOOLISFMXDJSKH-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- 241000223194 Fusarium culmorum Species 0.000 description 1
- 241000223195 Fusarium graminearum Species 0.000 description 1
- 244000061176 Nicotiana tabacum Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- BKCAPZFNKAZZMF-UHFFFAOYSA-N O=S(C(COC1CC1)(F)F)(F)=O Chemical compound O=S(C(COC1CC1)(F)F)(F)=O BKCAPZFNKAZZMF-UHFFFAOYSA-N 0.000 description 1
- ZMSRCMWBEGLBAI-UHFFFAOYSA-N O=S(C1(F)F)(OC1(F)F)=O Chemical compound O=S(C1(F)F)(OC1(F)F)=O ZMSRCMWBEGLBAI-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 206010035664 Pneumonia Diseases 0.000 description 1
- 208000005374 Poisoning Diseases 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- 230000007059 acute toxicity Effects 0.000 description 1
- 231100000403 acute toxicity Toxicity 0.000 description 1
- 239000005409 aflatoxin Substances 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 208000006673 asthma Diseases 0.000 description 1
- JGQFVRIQXUFPAH-UHFFFAOYSA-N beta-citronellol Natural products OCCC(C)CCCC(C)=C JGQFVRIQXUFPAH-UHFFFAOYSA-N 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 229930007646 carveol Natural products 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 235000000484 citronellol Nutrition 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- KTHXBEHDVMTNOH-UHFFFAOYSA-N cyclobutanol Chemical compound OC1CCC1 KTHXBEHDVMTNOH-UHFFFAOYSA-N 0.000 description 1
- XCIXKGXIYUWCLL-UHFFFAOYSA-N cyclopentanol Chemical compound OC1CCCC1 XCIXKGXIYUWCLL-UHFFFAOYSA-N 0.000 description 1
- 239000000645 desinfectant Substances 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 229930007024 dihydrocarveol Natural products 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000002158 endotoxin Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000021393 food security Nutrition 0.000 description 1
- 238000003958 fumigation Methods 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 210000002216 heart Anatomy 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 230000000266 injurious effect Effects 0.000 description 1
- 229940095045 isopulegol Drugs 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 201000007270 liver cancer Diseases 0.000 description 1
- 208000014018 liver neoplasm Diseases 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229940041616 menthol Drugs 0.000 description 1
- 229940102396 methyl bromide Drugs 0.000 description 1
- 239000003471 mutagenic agent Substances 0.000 description 1
- 231100000707 mutagenic chemical Toxicity 0.000 description 1
- ZYTMANIQRDEHIO-UHFFFAOYSA-N neo-Isopulegol Natural products CC1CCC(C(C)=C)C(O)C1 ZYTMANIQRDEHIO-UHFFFAOYSA-N 0.000 description 1
- 210000000653 nervous system Anatomy 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- NNFCIKHAZHQZJG-UHFFFAOYSA-N potassium cyanide Chemical compound [K+].N#[C-] NNFCIKHAZHQZJG-UHFFFAOYSA-N 0.000 description 1
- 230000003389 potentiating effect Effects 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 208000005069 pulmonary fibrosis Diseases 0.000 description 1
- 230000028327 secretion Effects 0.000 description 1
- 230000007226 seed germination Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000007619 statistical method Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 230000004936 stimulating effect Effects 0.000 description 1
- -1 sulfonyl Fluorine Chemical compound 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 230000001960 triggered effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23B—PRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
- A23B9/00—Preservation of edible seeds, e.g. cereals
- A23B9/16—Preserving with chemicals
- A23B9/18—Preserving with chemicals in the form of gases, e.g. fumigation; Compositions or apparatus therefor
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C309/00—Sulfonic acids; Halides, esters, or anhydrides thereof
- C07C309/78—Halides of sulfonic acids
- C07C309/79—Halides of sulfonic acids having halosulfonyl groups bound to acyclic carbon atoms
- C07C309/84—Halides of sulfonic acids having halosulfonyl groups bound to acyclic carbon atoms of a carbon skeleton substituted by carboxyl groups
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2200/00—Function of food ingredients
- A23V2200/10—Preserving against microbes
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2300/00—Processes
- A23V2300/30—Ion-exchange
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a kind of fumigating method for being used to prevent and treat grain entomophthora, it includes following operation：Under room temperature to 40 DEG C of environment, fumigant is placed on to lower section or/and the surrounding of grain heap；The fumigant is with formula I：Or formula II：
Description
Technical field
The present invention is to be related to a kind of fumigating method for being used to prevent and treat grain entomophthora, belongs to grain Techniques of preserving field.
Background technology
At present, the annual grain loss wastage of China is about as much as granary province of China first at 100,000,000,000 jin or so ---
Heilongjiang Province's grain yield of 1 year.According to measuring and calculating, China's grain postpartum such as only stores, transported, processing at the intermediate links loss wave
Take total amount up to 70,000,000,000 jin or so, only grain storage link loses about 40,000,000,000 jin wherein in intermediate links.China's annual postpartum it is mould fall
Grain loss should not be underestimated, the serious threat that fungi and endotoxin contamination are caused to China's grain security.According to Scientia Agricultura Sinica
Processing of farm products research institute of institute researcher Liu Yang is introduced：" China puts into the increases in grain production that all one's effort that exceeds 100 billion strives for 1% every year,
But the grain post-harvest loss caused by going mouldy is up to 21,000,000 tons every year, accounts for the 4.2% of national total output of grain, that causes is straight
It is about 180 hundred million to 240 hundred million yuan to connect economic loss.”
In addition, mycotoxin pollution is also serious to restrict China's Foreign Trade.In recent years, the peace that mycotoxin contaminated food products is caused
Total event takes place frequently, not only serious to threaten China's human and livestock health, while also restricting agricultural products in China foreign trade.From 2002~2011
It is close on 10 Nian Zhong China's exports European Union and eats discovery after agricultural product relevant contravention statistical analysis：Remained in heavy metal, agricultural and veterinary chemicals etc.
In the factor of numerous restriction China's Foreign Trades, exceeded mycotoxin is topmost reason, the fault triggered by mycotoxin
Event is up to 28.6%.It is reported that, mycotoxin is abiogenous most dangerous food contaminant, and the poison of aflatoxin
Property be 10 times of potassium cyanide, 68 times of arsenic, be to trigger one of main inducement of liver cancer.Mycotoxin is mainly in production
Produced afterwards during foodstuff preservation, during China's foodstuff preservation, mould is with aspergillus flavus, Asia sickle-like bacteria, cereal sickle
Based on knife bacterium；In American-European countries, except mould is in addition to aspergillus flavus, Fusarium graminearum, also aspergillus parasiticus, fusarium culmorum.
Meanwhile, it is short with American-European countries grain storage storage phase, originate single, the features such as quantity is small is compared, and China's grain storage feature is mainly showed
It is big for content of molds height, storage phase length, wide material sources, miscellaneous, quantity wide in variety.In addition, in silo and transportation by
Insect pest and the grain that loses also should not be underestimated, after the killed food of damaging by worms of grain, broken grain increases, percentage of seedgermination reduction；In addition,
Insect spinning can also make grain lump.And frass, worm corpse and the smelly liquid for the insect secretion having then pollute grain, or even produce poison
Element, causes grain heating to be gone mouldy.Common Grainhouse injurious insect have curculionid class, lesser grain borer, casemaking clothes moth, silverfish, gelechiid, lasioderma serricorne,
Cockroach and Indian meal moth etc..At present, most of grain depots bury square with inserting tube method fumigant insect killing etc. using grain face dispenser, cloth bag
Formula, fumigant used is mainly hydrogen phosphide, oxirane, bromomethane and vikane, with people's environmental protection and awareness of safety
Improve, the limitation of above fumigant is progressively embodied, such as：Hydrogen phosphide is causing toxicity by force, infringement lung, the heart, liver, kidney, in
Pivot nervous system and bone, over-exposure cause asthma, pneumonia or pulmonary fibrosis disease, and easily spontaneous combustion etc. it is dangerous because
Element；The mutagens and explosivity of oxirane；Bromomethane is produced to the destructive and direct of ozone of atmospheric advection layer to the mankind
It is raw to poison the highest attention for having caused people.Since after 1997 the 9th time " Montreal Protocol Meeting of States Parties ",
Developed country has arranged the phased out use bromomethane disinfectant from 2005, and China is also formally signed in April, 2003
Affix one's name to《Montreal Protocol》Copenhagen amendment, promise will exist in stopping methyl bromide before 1 day January in 2015 comprehensively
Use in the industries such as agricultural, storage, tobacco.Certainly, this promise will also be performed in grain sterilization；Vikane is normal
It is a kind of colourless, poisonous under normal temperature and pressure, has strong and stimulating gas, acute toxicity major determinant central nervous system causes frightened
Faint；In addition, can also be deposited in skeleton, it is dangerous with progressive poisoning.Current research finds chemical fumigant sulfonyl
Fluorine, a kind of potent greenhouse gases can be turned into by being dispersed into after air, and one kilogram of vikane is discharged into the effect in air to global warming
Fruit is 4800 times of one kilogram of carbon dioxide；Although only existing minimal amount of vikane in present air, about 1.5 part per trillions,
In i.e. every 1,000,000 air molecules, only 1.5 are vikanes, but it is being increased with annual 5% speed, is not used as
The substitute of bromomethane, the application of vikane and the atmospheric warming effect that causes should cause enough attention！
In summary, solve grain and go mouldy problem as the great demand for ensureing national food security, explore and be adapted to China's grain
Effective preventing control method of entomophthora has turned into the current research topic for being badly in need of solving in food storage.
The content of the invention
In view of the above-mentioned problems existing in the prior art and demand, it is an object of the invention to provide a kind of environmental protection, safely and effectively
Be used for prevent and treat the fumigating method of grain entomophthora.
For achieving the above object, the present invention is adopted the following technical scheme that：
A kind of fumigating method for being used to prevent and treat grain entomophthora, including following operation：Under room temperature to 40 DEG C of environment, by fumigant
It is placed on lower section or/and the surrounding of grain heap；The fumigant is with formula I：Or formula II：
The compound of shown chemical constitution, wherein, in the formula I：X is halogen or hydroxyl；Y1And Y2It is each independently selected from H
Or F；R1For R3Substituted C1-C10Alkyl, R3Substituted C2-C10Alkylene, R3Substituted phenyl, R3Substitution
Benzyl, R3Substituted C3-C8Cycloalkyl, R3Substituted C3-C8Cycloalkenyl group or R3Substituted adamantyl；The R3
Selected from hydrogen, hydroxyl, halogen, C1-C3Alkyl, C2-C3At least one of alkylene；In the formula II：X is halogen
Element or hydroxyl；R2For R3Substituted C1-C4Alkyl, R3Substituted C2-C4Alkylene, R3Substituted phenyl, R3Substitution
Benzyl, R3Substituted C3-C8Cycloalkyl, R3Substituted C3-C8Cycloalkenyl group or R3Substituted adamantyl；It is described
R3Selected from hydrogen, hydroxyl, halogen, C1-C3Alkyl, C2-C3At least one of alkylene.
Preferably, in the formula I：X is F, Cl, Br or OH；Y1And Y2It is simultaneously F or Y1、Y2
One of them is F；R1For R3Substituted C1-C10Alkyl, R3Substituted C2-C10Alkylene, R3Substituted phenyl,
R3Substituted benzyl, R3Substituted C3-C6Cycloalkyl, R3Substituted C3-C6Cycloalkenyl group or R3Substituted adamantyl；
The R3Selected from least one of hydrogen, hydroxyl, fluorine, chlorine, bromine, methyl, ethyl, isopropyl, pi-allyl.
As further preferred scheme, in the formula I：X is F or Cl；Y1And Y2It is simultaneously F；R1For R3Substitution
C1-C4Alkyl, R3Substituted C2-C4Alkylene, R3Substituted phenyl or R3Substituted C3-C6Cycloalkyl；It is described
R3Selected from least one of hydrogen, hydroxyl, fluorine, chlorine.
As still more preferably scheme, in the formula I：X is F；Y1And Y2It is simultaneously F；R1For C1-C4Alkane
Base, C2-C4Alkylene, phenyl or C3-C7Cycloalkyl is (i.e.：R3For hydrogen).
Preferably, in the formula II：X is F, Cl, Br or OH；R2For R3Substituted C1-C4Alkyl,
R3Substituted C2-C4Alkylene, R3Substituted phenyl, R3Substituted benzyl, R3Substituted C3-C7Cycloalkyl, R3Substitution
C3-C7Cycloalkenyl group or R3Substituted adamantyl；The R3Selected from hydrogen, hydroxyl, fluorine, chlorine, bromine, methyl, ethyl,
At least one of isopropyl, pi-allyl.
As further preferred scheme, in the formula II：X is F or Cl；R2For R3Substituted C1-C4Alkyl,
R3Substituted C2-C4Alkylene, R3Substituted C3-C7Cycloalkyl or R3Substituted phenyl；The R3Selected from hydrogen, hydroxyl,
At least one of fluorine, chlorine.
As still more preferably scheme, in the formula II：X is F；R2For C1-C4Alkyl, C2-C4Alkylene or
Phenyl is (i.e.：R3For hydrogen).
Specifically, fumigant of the invention includes but is not limited to the compound with following chemical structural formulas：
(being abbreviated as fumigant 1),(being abbreviated as fumigant 2),
(being abbreviated as fumigant 3),(being abbreviated as fumigant 4),
(being abbreviated as fumigant 5),(being abbreviated as fumigant 6),
(being abbreviated as fumigant 7),(being abbreviated as fumigant 8),
(being abbreviated as fumigant 9),(being abbreviated as fumigant 10),
(being abbreviated as fumigant 11),(being abbreviated as fumigant 12),
(being abbreviated as fumigant 13),(being abbreviated as fumigant 14),
(being abbreviated as fumigant 15),(being abbreviated as fumigant 16),
(being abbreviated as fumigant 17),(being abbreviated as fumigant 18),
(being abbreviated as fumigant 19),(being abbreviated as fumigant 20),
(being abbreviated as fumigant 21),(being abbreviated as fumigant 22),
(being abbreviated as fumigant 23)；
(being abbreviated as fumigant 24),(being abbreviated as fumigant 25),
(being abbreviated as fumigant 26),(being abbreviated as fumigant 27),
(being abbreviated as fumigant 28),(being abbreviated as fumigant 29),
(being abbreviated as fumigant 30),(being abbreviated as fumigant 31),
(being abbreviated as fumigant 32),(being abbreviated as fumigant 33),
(being abbreviated as fumigant 33),(being abbreviated as fumigant 35),
(being abbreviated as fumigant 36),(being abbreviated as fumigant 37),
(being abbreviated as fumigant 38),(being abbreviated as fumigant 39),
(being abbreviated as fumigant 40),(being abbreviated as fumigant 41),
(being abbreviated as fumigant 42),(being abbreviated as fumigant 43),
(being abbreviated as fumigant 44),(being abbreviated as fumigant 45),
(being abbreviated as fumigant 46),(being abbreviated as fumigant 47),
(being abbreviated as fumigant 48),(being abbreviated as fumigant 49),
(being abbreviated as fumigant 50),(being abbreviated as fumigant 51),
(being abbreviated as fumigant 52),(being abbreviated as fumigant 53),
(being abbreviated as fumigant 54).
Preferably, at room temperature, the lower section for grain heap fumigant being placed in closed environment or/and surrounding.
Preferably, the fumigant is supported on the carrier material with suction-operated, described carrier material bag
Include but be not limited to filter paper, silica gel, filter membrane, cotton, sponge or cloth etc..
Preferably, by the carrier material for being loaded with fumigant be placed on to external diffusion mouth or mesh face it is hollow
In device, described hollow devices include but is not limited to case structure, box structure, cage construction or sack etc..
As further preferred scheme, the hollow devices have fan and speed-regulating function.
As further preferred scheme, the hollow devices have self-heating and temperature adjustment function.
Compared with prior art, the present invention has the advantages that：
The present invention is not only realized to the common worm of grain by being used as fumigant from the compound with formula I or II structure
The safe and effective preventing and treating of mildew evil, and it is minimum to the pollution of environment, there is no fumigant residue problem, with environmental protection
Advantage；Especially, present invention can be implemented in plurality of cereals and various grain entomophthora diseases are carried out once under same stifling environment
Property processing, and the grain after suffocating treatment of the present invention, can be placed under silo environment or traffic condition at least half a year with
On no longer demutation entomophthora disease；In addition, the inventive method also have it is simple to operate, cost is low, applicable grain variety and worm
The advantages of mildew evil scope is wide, has important value and far reaching significance to permanent preserve of safety of grain.
Embodiment
Technical scheme is described in further details below by embodiment.
Embodiment 1：The preparation of fumigant
1st, the preparation of fumigant 15 (fluoro- 2- (sulphonyl is fluorine-based) the acetic acid ring propyl ester of 2,2- bis-)：
Take ring propyl alcohol (58mg) to add dichloromethane (10mL), perfluorinated sulfonic acid ester (1mL) be added dropwise under ice-water bath cooling,
Drop finishes, and is warmed to room temperature naturally, after reaction completely, adds water and reaction is quenched, extracted with dichloromethane (100mL × 2), washes
Solvent is evaporated off in (10mL × 2), saturated common salt washing (10mL × 2), anhydrous sodium sulfate drying, pressurization, obtains crude product and smokes
Steam agent 15 (2,2- bis- fluoro- 2- (sulphonyl is fluorine-based) acetic acid ring propyl ester), molar yield 90%；1HNMR(CDCl3)δ(ppm)2.70
(m,1H),0.60(m,2H),0.35(m,2H).LR-ESI:[M+H]+218.99。
2nd, the preparation of fumigant 16,17,18,19,20,21,22,23：
The preparation method of fumigant 15 in reference 1, respectively by cyclobutanol, cyclopentanol, menthol, isopulegol, dihydro
Carveol, carveol, citronellol, lemon alcohol and perfluorinated sulfonic acid ester are reacted, so as to which corresponding fumigant is made：
(16)；1HNMR(CDCl3)δ(ppm)4.23(m,1H),2.30(m,2H),1.91-2.08(m,
4H).LR-ESI:[M+H]+233.0；
(17)；1HNMR(CDCl3)δ(ppm)4.12(m,1H),1.92(m,2H),1.46-1.63(m,
6H).LR-ESI:[M+H]+247.02；
(18)；1HNMR(CDCl3)δ(ppm)4.03(m,1H),1.85-1.98(m,2H),
(d, J=6.0Hz, the 6H) .LR-ESI of 1.50-1.62 (m, 5H), 1.20-1.29 (m, 2H), 0.97 (d, J=5.6Hz, 3H), 0.89:
[M+H]+317.10；
(19)；1HNMR(CDCl3)δ(ppm)5.10(s,1H),4.90(s,1H),4.04(m,1H),
(d, J=5.6Hz, the 3H) of 2.65 (m, 1H), 1.90 (s, 3H), 1.55-1.69 (m, 5H), 1.25-1.35 (m, 2H), 0.95
LR-ESI:[M]+314.08；
(20)；1HNMR(CDCl3)δ(ppm)5.11(s,1H),4.87(s,1H),4.08(m,1H),
2.20 (m, 1H), 2.10 (m, 1H), 1.88 (s, 3H), 1.56-1.72 (m, 4H), 1.22-1.34 (m, 2H), 0.94 (d, J=5.6
Hz,3H).LR-ESI:[M]+314.08；
(21)；1HNMR(CDCl3)δ(ppm)5.32(m,1H),5.15(s,1H),4.93(s,1H),
4.32(m,1H),2.30(m,1H),1.75-1.90(m,4H),1.86(s,3H),1.82(s,3H).LR-ESI:[M+1]+
313.06；
(22)；1HNMR(CDCl3)δ(ppm)5.22(s,1H),4.07(m,2H),2.01
(m, 2H), 1.85 (s, 3H), 1.73 (s, 3H), 1.50-1.61 (m, 5H), 0.98 (d, J=6.0Hz, 3H) .LR-ESI:[M+1]+
317.10；
(23)；1HNMR(CDCl3)δ(ppm)5.38(m,1H),5.22(m,1H),
4.45(m,2H),2.10(m,2H),2.04(m,2H),1.90(s,3H),1.88(s,3H),1.80(s,3H).LR-ESI:
[M+1]+315.08。
3rd, the preparation of remaining fumigant：
Because remaining fumigant is known compound, it can be prepared according to respective disclosed preparation method.
Embodiment 2：Grain fumigating is tested
Grain variety：Corn, paddy, wheat, soybean, soya bean, broad bean, potato, sweet potato etc.
Disease：Aspergillus, mould, trichoderma, cladosporium herbarum, head mold, trichoderma, staphylococcus aureus, Escherichia coli,
Bacillus megaterium, hay bacillus and pseudomonas fluorescens etc.
Fumigant：Fumigant 24 (No. CAS：677-25-8)
First fumigant is directly placed in culture dish, the top that grain samples then are placed on into culture dish (can be by setting
Fixed frame is achieved), fumigate at room temperature.
Sampled monitoring is learnt：After when stifling 24 is small, without any mould in the grain samples after above-mentioned suffocating treatment
Bacteria growing (is measured by microscope inspection and known), and does not have fumigant residue in the grain samples after above-mentioned suffocating treatment (by gas
Phase chromatogram is learnt with GC-MS (GC-Ms) detection and analysis)；In addition, by color difference meter observation after above-mentioned suffocating treatment
The colors of all grain samples do not occur significant change.
Grain samples after the present embodiment suffocating treatment are placed in room temperature environment, mould, bacterium tracing detection is periodically carried out,
Testing result see the table below shown：
| Resting period | 0 month | 1 month | 3 months | 6 months |
| Mould, bacteria growing situation | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium |
Illustrate that present invention can be implemented in plurality of cereals and various mould, bacterium are disposably handled under same stifling environment.
Embodiment 3：Grain fumigating is tested
Grain variety：Corn, paddy, wheat, soybean, soya bean, broad bean, potato, sweet potato etc.
Disease：Aspergillus, mould, trichoderma, cladosporium herbarum, head mold, trichoderma, staphylococcus aureus, Escherichia coli,
Bacillus megaterium, hay bacillus and pseudomonas fluorescens etc.
Fumigant：Fumigant 25 (No. CAS：754-03-0)
First fumigant is supported on silica gel particle, silica gel particle then is placed on into surface has in meshed sack, then will
The sack is placed on the bottom of glass jar, and the top that grain samples are placed on into the sack (can be by setting solid in glass jar
Determine framework to be achieved), closed glass cylinder is fumigated at room temperature.
Sampled monitoring is learnt：After when stifling 36 is small, without any mould in the grain samples after above-mentioned suffocating treatment
Bacteria growing (is measured by microscope inspection and known), and does not have fumigant residue in the grain samples after above-mentioned suffocating treatment (by gas
Phase chromatogram is learnt with GC-MS (GC-Ms) detection and analysis)；In addition, by color difference meter observation after above-mentioned suffocating treatment
The colors of grain samples do not occur significant change.
Grain samples after the present embodiment suffocating treatment are placed in room temperature environment, mould, bacterium tracing detection is periodically carried out,
Testing result see the table below shown：
| Resting period | 0 month | 1 month | 3 months | 6 months |
| Mould, bacteria growing situation | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium |
Illustrate that present invention can be implemented in plurality of cereals and various mould, bacterium are disposably handled under same stifling environment.
Embodiment 4：Grain fumigating is tested
Grain variety：Corn, paddy, wheat, soybean, soya bean, broad bean, potato, sweet potato etc.
Disease：Aspergillus, mould, trichoderma, cladosporium herbarum, head mold, trichoderma, staphylococcus aureus, Escherichia coli,
Bacillus megaterium, hay bacillus and pseudomonas fluorescens etc.
Fumigant：Fumigant 27 (No. CAS：260417-57-0)
First fumigant is supported on cyclodextrin, cyclodextrin then is placed on into surface has in meshed sack, then by the bag
Son is placed on the bottom of glass jar, and the top that grain samples are placed on into the sack (can be by setting fixed frame in glass jar
Frame is achieved), closed glass cylinder is fumigated at room temperature.
Sampled monitoring is learnt：After when stifling 30 is small, without any mould in the grain samples after above-mentioned suffocating treatment
Bacteria growing (is measured by microscope inspection and known), and does not have fumigant residue in the grain samples after above-mentioned suffocating treatment (by gas
Phase chromatogram is learnt with GC-MS (GC-Ms) detection and analysis)；In addition, by color difference meter observation after above-mentioned suffocating treatment
The colors of grain samples do not occur significant change.
Grain samples after the present embodiment suffocating treatment are placed in room temperature environment, mould, bacterium tracing detection is periodically carried out,
Testing result see the table below shown：
| Resting period | 0 month | 1 month | 3 months | 6 months |
| Mould, bacteria growing situation | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium |
Illustrate that present invention can be implemented in plurality of cereals and various mould, bacterium are disposably handled under same stifling environment.
Embodiment 5：Grain fumigating is tested
Grain variety：Corn, paddy, wheat, soybean, soya bean, broad bean, potato, sweet potato etc.
Disease：Aspergillus, mould, trichoderma, cladosporium herbarum, head mold, trichoderma, staphylococcus aureus, Escherichia coli,
Bacillus megaterium, hay bacillus and pseudomonas fluorescens etc.
Fumigant：
Fumigant 1 (No. CAS：680-15-9)；
Fumigant 10 (No. CAS：CAS:309-21-7)；
First fumigant 1 or 10 is supported on filter paper, then the filter paper be placed on to the bottom of glass jar, grain samples are put
Put in the top of filter paper, closed glass cylinder is fumigated at room temperature.
Sampled monitoring is learnt：After when stifling 24 is small, in the grain samples after any one above-mentioned fumigant suffocating treatment
There is no any fungus growth (measured and known by microscope inspection), and the grain after any one above-mentioned fumigant suffocating treatment
(learnt on sample without fumigant residue by internal standard method for gas chromatography instrument (GC-Ms) detection and analysis)；In addition, logical
Significant change does not occur for the color for crossing grain samples of the color difference meter observation after any one above-mentioned fumigant suffocating treatment.
Grain samples after any one above-mentioned fumigant suffocating treatment of the present embodiment are placed in room temperature environment, periodically
Mould, bacterium tracing detection is carried out, following testing result is respectively provided with：
| Resting period | 0 month | 1 month | 3 months | 6 months |
| Mould, bacteria growing situation | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium |
Illustrate that present invention can be implemented in plurality of cereals and various mould, bacterium are disposably handled under same stifling environment.
Embodiment 6：Grain fumigating is tested
Grain variety：Corn, paddy, wheat, soybean, soya bean, broad bean, potato, sweet potato etc.
Disease：Aspergillus, mould, trichoderma, cladosporium herbarum, head mold, trichoderma, staphylococcus aureus, Escherichia coli,
Bacillus megaterium, hay bacillus and pseudomonas fluorescens etc.
Fumigant：Fumigant 9 (No. CAS：113591-64-3)
First fumigant is supported on silica gel particle, silica gel particle then is placed on into surface has in meshed sack, then will
The sack is placed on the bottom of glass jar, and the top that grain samples are placed on into the sack (can be by setting solid in glass jar
Determine framework to be achieved), closed glass cylinder is fumigated in the case where environment temperature is 40 DEG C.
Sampled monitoring is learnt：After when stifling 20 is small, without any mould in the grain samples after above-mentioned suffocating treatment
Bacteria growing (is measured by microscope inspection and known), and does not have fumigant residue in the grain samples after above-mentioned suffocating treatment (by gas
Phase chromatogram is learnt with GC-MS (GC-Ms) detection and analysis)；In addition, by color difference meter observation after above-mentioned suffocating treatment
The colors of grain samples do not occur significant change.
Grain samples after the present embodiment suffocating treatment are placed in room temperature environment, mould, bacterium tracing detection is periodically carried out,
Testing result see the table below shown：
| Resting period | 0 month | 1 month | 3 months | 6 months |
| Mould, bacteria growing situation | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium |
Illustrate that present invention can be implemented in plurality of cereals and various mould, bacterium are disposably handled under same stifling environment.
Embodiment 7：Grain fumigating is tested
Grain variety：Corn, paddy, wheat, soybean, soya bean, broad bean, potato, sweet potato etc.
Disease：Aspergillus, mould, trichoderma, cladosporium herbarum, head mold, trichoderma, staphylococcus aureus, Escherichia coli,
Bacillus megaterium, hay bacillus and pseudomonas fluorescens etc.
Fumigant：Fumigant 15
First fumigant is supported on cyclodextrin, cyclodextrin then is placed on into surface has in meshed sack, then by the bag
Son is placed on the bottom of glass jar, and the top that grain samples are placed on into the sack (can be by setting fixed frame in glass jar
Frame is achieved), closed glass cylinder is fumigated in the case where environment temperature is 30 DEG C.
Sampled monitoring is learnt：After when stifling 24 is small, without any mould in the grain samples after above-mentioned suffocating treatment
Bacteria growing (is measured by microscope inspection and known), and does not have fumigant residue in the grain samples after above-mentioned suffocating treatment (by gas
Phase chromatogram is learnt with GC-MS (GC-Ms) detection and analysis)；In addition, by color difference meter observation after above-mentioned suffocating treatment
The colors of grain samples do not occur significant change.
Grain samples after the present embodiment suffocating treatment are placed in room temperature environment, mould, bacterium tracing detection is periodically carried out,
Testing result see the table below shown：
| Resting period | 0 month | 1 month | 3 months | 6 months |
| Mould, bacteria growing situation | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium |
Illustrate that present invention can be implemented in plurality of cereals and various mould, bacterium are disposably handled under same stifling environment.
Embodiment 8：Grain fumigating is tested
Grain variety：Corn, paddy, wheat, soybean, soya bean, broad bean, potato, sweet potato etc.
Disease：Aspergillus, mould, trichoderma, cladosporium herbarum, head mold, trichoderma, staphylococcus aureus, Escherichia coli,
Bacillus megaterium, hay bacillus and pseudomonas fluorescens etc.
Fumigant：Fumigant 12 (No. CAS：1397690-78-6)
First fumigant is supported on filter paper, the filter paper then is placed on into surface has mesh, comes with fan and speed governing work(
Can hollow box in, then the box body is placed on to the bottom of glass jar, the top that grain samples are placed on into the box body (can
By setting fixed frame to be achieved in glass jar), closed glass cylinder opens fan in room temperature (wind speed is set as at a high speed)
It is lower to be fumigated.
Sampled monitoring is learnt：After when stifling 20 is small, without any mould in the grain samples after above-mentioned suffocating treatment
Bacteria growing (is measured by microscope inspection and known), and does not have fumigant residue in the grain samples after above-mentioned suffocating treatment (by gas
Phase chromatogram is learnt with GC-MS (GC-Ms) detection and analysis)；In addition, by color difference meter observation after above-mentioned suffocating treatment
The colors of grain samples do not occur significant change.
Grain samples after the present embodiment suffocating treatment are placed in room temperature environment, mould, bacterium tracing detection is periodically carried out,
Testing result see the table below shown：
| Resting period | 0 month | 1 month | 3 months | 6 months |
| Mould, bacteria growing situation | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium |
Illustrate that present invention can be implemented in plurality of cereals and various mould, bacterium are disposably handled under same stifling environment.
Embodiment 9：Grain fumigating is tested
Grain variety：Corn, paddy, wheat, soybean, soya bean, broad bean, potato, sweet potato etc.
Disease：Curculionid, lesser grain borer, casemaking clothes moth, silverfish, gelechiid, lasioderma serricorne, cockroach and Indian meal moth etc.
Fumigant：
Fumigant 5 (No. CAS：120801-74-3)；
Fumigant 7 (No. CAS：120801-74-3)；
Fumigant 11 (No. CAS：155820-78-3)；
Fumigant 43 (No. CAS：139631-62-2)；
First any one above-mentioned fumigant is supported on silica gel particle, it is meshed that silica gel particle then is placed on into surface tool
In sack, then the sack is placed on to the bottom of glass jar, the top that grain samples are placed on into the sack (can be by glass
Fixed frame is set to be achieved in glass cylinder), closed glass cylinder is fumigated at room temperature；Regular sampling monitoring insect therein is dead
Situation is died, following monitoring result is obtained：
Learnt by internal standard method for gas chromatography instrument (GC-Ms) detection and analysis：Through any one above-mentioned fumigant suffocating treatment
Without fumigant residue in grain samples afterwards；In addition, by color difference meter observation through the stifling place of any one above-mentioned fumigant
Significant change does not occur for the color of the grain samples after reason.
Grain samples after any one above-mentioned fumigant suffocating treatment of the present embodiment are placed in room temperature environment, periodically
Insect growing state is tracked, following testing result is obtained：
| Resting period | 0 month | 1 month | 3 months | 6 months |
| Insect survives and growing state | Without any insect | Without any insect | Without any insect | Without any insect |
Illustrate that present invention can be implemented in plurality of cereals and various insects are disposably handled under same stifling environment.
Embodiment 10：Grain fumigating is tested
Grain variety：Corn, paddy, wheat, soybean, soya bean, broad bean, potato, sweet potato etc.
Disease：Curculionid, lesser grain borer, casemaking clothes moth, silverfish, gelechiid, lasioderma serricorne, cockroach and Indian meal moth etc.
Fumigant：
Fumigant 42 (No. CAS：76876-59-0)；
Fumigant 53 (No. CAS：187143-10-8)；
Fumigant 54 (No. CAS：700-25-4)；
First any one above-mentioned fumigant is supported on silica gel particle, it is meshed that silica gel particle then is placed on into surface tool
In sack, then the sack is placed on to the bottom of glass jar, the top that grain samples are placed on into the sack (can be by glass
Fixed frame is set to be achieved in glass cylinder), closed glass cylinder is fumigated in the case where environment temperature is 40 DEG C；Periodically sampling is supervised
Insect death condition therein is surveyed, following monitoring result is obtained：
Learnt by internal standard method for gas chromatography instrument (GC-Ms) detection and analysis：Through any one above-mentioned fumigant suffocating treatment
Without fumigant residue in grain samples afterwards；In addition, by color difference meter observation through the stifling place of any one above-mentioned fumigant
The color of grain samples after reason, which has, slightly to be changed.
Grain samples after any one above-mentioned fumigant suffocating treatment of the present embodiment are placed in room temperature environment, periodically
Insect growing state is tracked, following testing result is obtained：
| Resting period | 0 month | 1 month | 3 months | 6 months |
| Insect survives and growing state | Without any insect | Without any insect | Without any insect | Without any insect |
Illustrate that present invention can be implemented in plurality of cereals and various insects are disposably handled under same stifling environment.
Embodiment 11：Grain fumigating is tested
Grain variety：Corn, paddy, wheat, soybean, soya bean, broad bean, potato, sweet potato etc.
Disease：Curculionid, lesser grain borer, casemaking clothes moth, silverfish, gelechiid, lasioderma serricorne, cockroach and Indian meal moth etc.
Fumigant：Fumigant 12 (No. CAS：1397690-78-6)
First fumigant is supported on cyclodextrin, cyclodextrin then is placed on into surface has in meshed sack, then by the bag
Son is placed on the bottom of glass jar, and the top that grain samples are placed on into the sack (can be by setting fixed frame in glass jar
Frame is achieved), closed glass cylinder is fumigated in the case where environment temperature is 30 DEG C；Regular sampling monitoring insect therein is dead
Situation, detailed results are as shown in the table：
Learnt by the detection and analysis of internal standard method for gas chromatography instrument：Do not fumigated in grain samples after above-mentioned suffocating treatment
Agent is remained；In addition, significant change does not occur for the color for observing the grain samples after above-mentioned suffocating treatment by color difference meter.
Grain samples after the present embodiment suffocating treatment are placed in room temperature environment, periodically tracking insect growing state,
Testing result see the table below shown：
| Resting period | 0 month | 1 month | 3 months | 6 months |
| Insect survives and growing state | Without any insect | Without any insect | Without any insect | Without any insect |
Illustrate that present invention can be implemented in plurality of cereals and various insects are disposably handled under same stifling environment.
Embodiment 12：Grain fumigating is tested
Grain variety：Corn, paddy, wheat, soybean, soya bean, broad bean, potato, sweet potato etc.
Disease：Curculionid, lesser grain borer, casemaking clothes moth, silverfish, gelechiid, lasioderma serricorne, cockroach and Indian meal moth etc.
Fumigant：Fumigant 28 (No. CAS：847661-06-7)
First fumigant is supported on filter paper, the filter paper then is placed on into surface has mesh, comes with fan and speed governing work(
Can hollow box in, then the box body is placed on to the bottom of glass jar, the top that grain samples are placed on into the box body (can
By setting fixed frame to be achieved in glass jar), closed glass cylinder opens fan in room temperature (wind speed is set as at a high speed)
It is lower to be fumigated；Regular sampling monitoring insect death condition therein, detailed results are as shown in the table：
Learnt by the detection and analysis of internal standard method for gas chromatography instrument：Do not fumigated in grain samples after above-mentioned suffocating treatment
Agent is remained；In addition, significant change does not occur for the color for observing the grain samples after above-mentioned suffocating treatment by color difference meter.
Grain samples after the present embodiment suffocating treatment are placed in room temperature environment, periodically tracking insect growing state,
Testing result see the table below shown：
| Resting period | 0 month | 1 month | 3 months | 6 months |
| Insect survives and growing state | Without any insect | Without any insect | Without any insect | Without any insect |
Illustrate that present invention can be implemented in plurality of cereals and various insects are disposably handled under same stifling environment.
Embodiment 13：Grain fumigating is tested
Grain variety：Corn, paddy, wheat, soybean, soya bean, broad bean, potato, sweet potato etc.
Disease：Curculionid, lesser grain borer, casemaking clothes moth, silverfish, gelechiid, lasioderma serricorne, cockroach and Indian meal moth etc.
Fumigant：Fumigant 33 (No. CAS：51849-05-9)
First fumigant is supported on filter paper, the filter paper then is placed on into surface has mesh, comes with fan and speed governing work(
Can hollow box in, then the box body is placed on to the bottom of glass jar, the top that grain samples are placed on into the box body (can
By setting fixed frame to be achieved in glass jar), closed glass cylinder adjusts the temperature of box body to be fumigated at 35 DEG C；
Regular sampling monitoring insect death condition therein, detailed results are as shown in the table：
Learnt by the detection and analysis of internal standard method for gas chromatography instrument：Do not fumigated in grain samples after above-mentioned suffocating treatment
Agent is remained；In addition, significant change does not occur for the color for observing the grain samples after above-mentioned suffocating treatment by color difference meter.
Grain samples after the present embodiment suffocating treatment are placed in room temperature environment, periodically tracking insect growing state,
Testing result see the table below shown：
| Resting period | 0 month | 1 month | 3 months | 6 months |
| Insect survives and growing state | Without any insect | Without any insect | Without any insect | Without any insect |
Illustrate that present invention can be implemented in plurality of cereals and various insects are disposably handled under same stifling environment.
Embodiment 14-1：Grain fumigating is tested
Grain variety：Corn, paddy, wheat, soybean, soya bean, broad bean, potato, sweet potato etc.
Disease：Aspergillus, mould, trichoderma, cladosporium herbarum, head mold, trichoderma, staphylococcus aureus, Escherichia coli,
Bacillus megaterium, hay bacillus, pseudomonas fluorescens, curculionid, lesser grain borer, casemaking clothes moth, silverfish, gelechiid, lasioderma serricorne,
Cockroach and Indian meal moth etc.
Fumigant：Fumigant 24 (No. CAS：677-25-8)
First fumigant is directly placed in culture dish, then grain samples are placed on to the top of culture dish, is smoked at room temperature
Steam；Regular sampling monitoring insect death condition therein, detailed results are as shown in the table：
Learnt by the detection and analysis of internal standard method for gas chromatography instrument：Do not fumigated in grain samples after above-mentioned suffocating treatment
Agent is remained；In addition, significant change does not occur for the color for observing the grain samples after above-mentioned suffocating treatment by color difference meter.
Grain samples after the present embodiment suffocating treatment are placed in room temperature environment, mould, bacterium, insect life is periodically tracked
Long situation, testing result see the table below shown：
| Resting period | 0 month | 1 month | 3 months | 6 months |
| Insect survives and growing state | Without any insect | Without any insect | Without any insect | Without any insect |
| Mould, bacteria growing situation | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium |
Illustrate that present invention can be implemented in plurality of cereals and various insects, mould, bacterium are disposably handled under same stifling environment.
Embodiment 14-2：Grain fumigating is tested
Grain variety：Corn, paddy, wheat, soybean, soya bean, broad bean, potato, sweet potato etc.
Disease：Aspergillus, mould, trichoderma, cladosporium herbarum, head mold, trichoderma, staphylococcus aureus, Escherichia coli,
Bacillus megaterium, hay bacillus, pseudomonas fluorescens, curculionid, lesser grain borer, casemaking clothes moth, silverfish, gelechiid, lasioderma serricorne,
Cockroach and Indian meal moth etc.
Fumigant：Fumigant 24 (No. CAS：677-25-8)
First fumigant is supported on filter paper, then the filter paper is placed on to the bottom of glass jar, then grain samples are placed on
The top (can be by setting fixed frame to be achieved in glass jar) of filter paper, closed glass cylinder is fumigated at room temperature；It is fixed
Phase sampling monitoring insect death condition therein, detailed results are as shown in the table：
Learnt by the detection and analysis of internal standard method for gas chromatography instrument：Do not fumigated in grain samples after above-mentioned suffocating treatment
Agent is remained；In addition, significant change does not occur for the color for observing the grain samples after above-mentioned suffocating treatment by color difference meter.
Grain samples after the present embodiment suffocating treatment are placed in room temperature environment, mould, bacterium, insect life is periodically tracked
Long situation, testing result see the table below shown：
| Resting period | 0 month | 1 month | 3 months | 6 months |
| Insect survives and growing state | Without any insect | Without any insect | Without any insect | Without any insect |
| Mould, bacteria growing situation | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium |
Illustrate that present invention can be implemented in plurality of cereals and various insects, mould, bacterium are disposably handled under same stifling environment.
Embodiment 14-3：Grain fumigating is tested
Grain variety：Corn, paddy, wheat, soybean, soya bean, broad bean, potato, sweet potato etc.
Disease：Aspergillus, mould, trichoderma, cladosporium herbarum, head mold, trichoderma, staphylococcus aureus, Escherichia coli,
Bacillus megaterium, hay bacillus, pseudomonas fluorescens, curculionid, lesser grain borer, casemaking clothes moth, silverfish, gelechiid, lasioderma serricorne,
Cockroach and Indian meal moth etc.
Fumigant：Fumigant 24 (No. CAS：677-25-8)
First fumigant is supported on filter paper, the filter paper then is placed on into surface has mesh, comes with fan and speed governing work(
Can hollow box in, then the box body is placed on to the bottom of glass jar, the top that grain samples are placed on into the box body (can
By setting fixed frame to be achieved in glass jar), closed glass cylinder opens fan in room temperature (wind speed is set as middling speed)
It is lower to be fumigated；Regular sampling monitoring insect death condition therein, detailed results are as shown in the table：
Learnt by the detection and analysis of internal standard method for gas chromatography instrument：Do not fumigated in grain samples after above-mentioned suffocating treatment
Agent is remained；In addition, significant change does not occur for the color for observing the grain samples after above-mentioned suffocating treatment by color difference meter.
Grain samples after the present embodiment suffocating treatment are placed in room temperature environment, mould, bacterium, insect life is periodically tracked
Long situation, testing result see the table below shown：
| Resting period | 0 month | 1 month | 3 months | 6 months |
| Insect survives and growing state | Without any insect | Without any insect | Without any insect | Without any insect |
| Mould, bacteria growing situation | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium |
Illustrate that present invention can be implemented in plurality of cereals and various insects, mould, bacterium are disposably handled under same stifling environment.
Embodiment 14-4：Grain fumigating is tested
Grain variety：Corn, paddy, wheat, soybean, soya bean, broad bean, potato, sweet potato etc.
Disease：Aspergillus, mould, trichoderma, cladosporium herbarum, head mold, trichoderma, staphylococcus aureus, Escherichia coli,
Bacillus megaterium, hay bacillus, pseudomonas fluorescens, curculionid, lesser grain borer, casemaking clothes moth, silverfish, gelechiid, lasioderma serricorne,
Cockroach and Indian meal moth etc.
Fumigant：Fumigant 24 (No. CAS：677-25-8)
First fumigant is supported on filter paper, the filter paper then is placed on into surface has mesh, comes with self-heating and temperature adjustment
In the hollow box of function, then the box body is placed on to the bottom of glass jar, the top that grain samples are placed on into the box body (can
By setting fixed frame to be achieved in glass jar), closed glass cylinder adjusts the temperature of box body to be fumigated at 30 DEG C；
Regular sampling monitoring insect death condition therein, detailed results are as shown in the table：
Learnt by the detection and analysis of internal standard method for gas chromatography instrument：Do not fumigated in grain samples after above-mentioned suffocating treatment
Agent is remained；In addition, significant change does not occur for the color for observing the grain samples after above-mentioned suffocating treatment by color difference meter.
Grain samples after the present embodiment suffocating treatment are placed in room temperature environment, mould, bacterium, insect life is periodically tracked
Long situation, testing result see the table below shown：
| Resting period | 0 month | 1 month | 3 months | 6 months |
| Insect survives and growing state | Without any insect | Without any insect | Without any insect | Without any insect |
| Mould, bacteria growing situation | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium |
Illustrate that present invention can be implemented in plurality of cereals and various insects, mould, bacterium are disposably handled under same stifling environment.
Embodiment 14-5：Grain fumigating is tested
Grain variety：Corn, paddy, wheat, soybean, soya bean, broad bean, potato, sweet potato etc.
Disease：Aspergillus, mould, trichoderma, cladosporium herbarum, head mold, trichoderma, staphylococcus aureus, Escherichia coli,
Bacillus megaterium, hay bacillus, pseudomonas fluorescens, curculionid, lesser grain borer, casemaking clothes moth, silverfish, gelechiid, lasioderma serricorne,
Cockroach and Indian meal moth etc.
Fumigant：Fumigant 24 (No. CAS：677-25-8)
First fumigant is supported on filter paper, the filter paper then is placed on into surface has mesh, comes with fan speed-regulating and oneself
In the hollow box for heating temperature adjustment function, then the box body is placed on to the bottom of glass jar, grain samples are placed on the box body
Top (can by glass jar set fixed frame be achieved), closed glass cylinder, regulation box body temperature be 40
Fumigated at DEG C；Regular sampling monitoring insect death condition therein, detailed results are as shown in the table：
Learnt by the detection and analysis of internal standard method for gas chromatography instrument：Do not fumigated in grain samples after above-mentioned suffocating treatment
Agent is remained；In addition, significant change does not occur for the color for observing the grain samples after above-mentioned suffocating treatment by color difference meter.
Grain samples after the present embodiment suffocating treatment are placed in room temperature environment, mould, bacterium, insect life is periodically tracked
Long situation, testing result see the table below shown：
| Resting period | 0 month | 1 month | 3 months | 6 months |
| Insect survives and growing state | Without any insect | Without any insect | Without any insect | Without any insect |
| Mould, bacteria growing situation | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium |
Illustrate that present invention can be implemented in plurality of cereals and various insects, mould, bacterium are disposably handled under same stifling environment.
Embodiment 14-6：Grain fumigating is tested
Grain variety：Corn, paddy, wheat, soybean, soya bean, broad bean, potato, sweet potato etc.
Disease：Aspergillus, mould, trichoderma, cladosporium herbarum, head mold, trichoderma, staphylococcus aureus, Escherichia coli,
Bacillus megaterium, hay bacillus, pseudomonas fluorescens, curculionid, lesser grain borer, casemaking clothes moth, silverfish, gelechiid, lasioderma serricorne,
Cockroach and Indian meal moth etc.
Fumigant：Fumigant 24 (No. CAS：677-25-8)
First fumigant is supported on filter paper, the filter paper then is placed on into surface has mesh, comes with fan and temperature adjustment work(
Can hollow box in, then the box body is placed on to the bottom of glass jar, grain samples is placed on to the top of the box body, it is close
Glass jar is closed, the temperature of regulation box body is 30 DEG C, fumigated while opening under fan (wind speed is set as low speed)；Periodically
Sampling monitoring insect death condition therein, detailed results are as shown in the table：
Learnt by the detection and analysis of internal standard method for gas chromatography instrument：Do not fumigated in grain samples after above-mentioned suffocating treatment
Agent is remained；In addition, significant change does not occur for the color for observing the grain samples after above-mentioned suffocating treatment by color difference meter.
Grain samples after the present embodiment suffocating treatment are placed in room temperature environment, mould, bacterium, insect life is periodically tracked
Long situation, testing result see the table below shown：
| Resting period | 0 month | 1 month | 3 months | 6 months |
| Insect survives and growing state | Without any insect | Without any insect | Without any insect | Without any insect |
| Mould, bacteria growing situation | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium |
Illustrate that present invention can be implemented in plurality of cereals and various insects, mould, bacterium are disposably handled under same stifling environment.
From embodiment 14-1 to 14-6 experimental result：The wind-force and appropriate heating of closed environment and fan are conducive to
Fumigating effect, can substantially shorten fumigation time in the case where reaching identical fumigating effect.
Embodiment 15：Grain fumigating is tested
Grain variety：Corn, paddy, wheat, soybean, soya bean, broad bean, potato, sweet potato etc.
Disease：Aspergillus, mould, trichoderma, cladosporium herbarum, head mold, trichoderma, staphylococcus aureus, Escherichia coli,
Bacillus megaterium, hay bacillus, pseudomonas fluorescens, curculionid, lesser grain borer, casemaking clothes moth, silverfish, gelechiid, lasioderma serricorne,
Cockroach and Indian meal moth etc.
Fumigant：
Fumigant 16Fumigant 17
Fumigant 18Fumigant：Fumigant 19
Fumigant 20Fumigant 21
Fumigant 22
Fumigant 23
First any one above-mentioned fumigant is directly placed in culture dish, then grain samples are placed on to the top of culture dish,
Fumigate at room temperature；Regular sampling monitoring insect death condition therein, obtains following monitoring result：
Learnt by internal standard method for gas chromatography instrument (GC-Ms) detection and analysis：Through any one above-mentioned fumigant suffocating treatment
Without fumigant residue in grain samples afterwards；In addition, by color difference meter observation through the stifling place of any one above-mentioned fumigant
Significant change does not occur for the color of the grain samples after reason.
Grain samples after any one above-mentioned fumigant suffocating treatment of the present embodiment are placed in room temperature environment, periodically
Mould, bacterium, insect growing state are tracked, following testing result is obtained：
| Resting period | 0 month | 1 month | 3 months | 6 months |
| Insect survives and growing state | Without any insect | Without any insect | Without any insect | Without any insect |
| Mould, bacteria growing situation | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium |
Illustrate that present invention can be implemented in plurality of cereals and various insects, mould, bacterium are disposably handled under same stifling environment.
Embodiment 16：Grain fumigating is tested
Grain variety：Corn, paddy, wheat, soybean, soya bean, broad bean, potato, sweet potato etc.
Disease：Aspergillus, mould, trichoderma, cladosporium herbarum, head mold, trichoderma, staphylococcus aureus, Escherichia coli,
Bacillus megaterium, hay bacillus, pseudomonas fluorescens, curculionid, lesser grain borer, casemaking clothes moth, silverfish, gelechiid, lasioderma serricorne,
Cockroach and Indian meal moth etc.
Fumigant：Fumigant 13 (CAS:1536468-56-0)
First fumigant is supported on filter paper, the filter paper then is placed on into surface has mesh, comes with fan speed-regulating and oneself
In the hollow box for heating temperature adjustment function, then the box body is placed on to the bottom of glass jar, grain samples are placed on the box body
Top (can by glass jar set fixed frame be achieved), closed glass cylinder, regulation box body temperature be 40
Fumigated at DEG C；Regular sampling monitoring insect death condition therein, detailed results are as shown in the table：
Learnt by the detection and analysis of internal standard method for gas chromatography instrument：Do not fumigated in grain samples after above-mentioned suffocating treatment
Agent is remained；In addition, significant change does not occur for the color for observing the grain samples after above-mentioned suffocating treatment by color difference meter.
Grain samples after the present embodiment suffocating treatment are placed in room temperature environment, mould, bacterium, insect life is periodically tracked
Long situation, testing result see the table below shown：
| Resting period | 0 month | 1 month | 3 months | 6 months |
| Insect survives and growing state | Without any insect | Without any insect | Without any insect | Without any insect |
| Mould, bacteria growing situation | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium |
Illustrate that present invention can be implemented in plurality of cereals and various insects, mould, bacterium are disposably handled under same stifling environment.
Embodiment 17：Grain fumigating is tested
Grain variety：Corn, paddy, wheat, soybean, soya bean, broad bean, potato, sweet potato etc.
Disease：Aspergillus, mould, trichoderma, cladosporium herbarum, head mold, trichoderma, staphylococcus aureus, Escherichia coli,
Bacillus megaterium, hay bacillus, pseudomonas fluorescens, curculionid, lesser grain borer, casemaking clothes moth, silverfish, gelechiid, lasioderma serricorne,
Cockroach and Indian meal moth etc.
Fumigant：Fumigant 14 (No. CAS：1536468-56-0)
First fumigant is supported on filter paper, the filter paper then is placed on into surface has mesh, comes with self-heating and temperature adjustment
In the hollow box of function, then the box body is placed on to the bottom of glass jar, the top that grain samples are placed on into the box body (can
By setting fixed frame to be achieved in glass jar), closed glass cylinder adjusts the temperature of box body to be fumigated at 30 DEG C；
Regular sampling monitoring insect death condition therein, detailed results are as shown in the table：
Learnt by the detection and analysis of internal standard method for gas chromatography instrument：Do not fumigated in grain samples after above-mentioned suffocating treatment
Agent is remained；In addition, significant change does not occur for the color for observing the grain samples after above-mentioned suffocating treatment by color difference meter.
Grain samples after the present embodiment suffocating treatment are placed in room temperature environment, mould, bacterium, insect life is periodically tracked
Long situation, testing result see the table below shown：
| Resting period | 0 month | 1 month | 3 months | 6 months |
| Insect survives and growing state | Without any insect | Without any insect | Without any insect | Without any insect |
| Mould, bacteria growing situation | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium |
Illustrate that present invention can be implemented in plurality of cereals and various insects, mould, bacterium are disposably handled under same stifling environment.
Embodiment 18：Grain fumigating is tested
Grain variety：Corn, paddy, wheat, soybean, soya bean, broad bean, potato, sweet potato etc.
Disease：Aspergillus, mould, trichoderma, cladosporium herbarum, head mold, trichoderma, staphylococcus aureus, Escherichia coli,
Bacillus megaterium, hay bacillus, pseudomonas fluorescens, curculionid, lesser grain borer, casemaking clothes moth, silverfish, gelechiid, lasioderma serricorne,
Cockroach and Indian meal moth etc.
Fumigant：Fumigant 4 (No. CAS：756-21-8)
First fumigant is supported on filter paper, the filter paper then is placed on into surface has mesh, comes with fan and speed governing work(
Can hollow box in, then the box body is placed on to the bottom of glass jar, the top that grain samples are placed on into the box body (can
By setting fixed frame to be achieved in glass jar), closed glass cylinder opens fan in room temperature (wind speed is set as middling speed)
It is lower to be fumigated；Regular sampling monitoring insect death condition therein, detailed results are as shown in the table：
Learnt by the detection and analysis of internal standard method for gas chromatography instrument：Do not fumigated in grain samples after above-mentioned suffocating treatment
Agent is remained；In addition, significant change does not occur for the color for observing the grain samples after above-mentioned suffocating treatment by color difference meter.
Grain samples after the present embodiment suffocating treatment are placed in room temperature environment, mould, bacterium, insect life is periodically tracked
Long situation, testing result see the table below shown：
| Resting period | 0 month | 1 month | 3 months | 6 months |
| Insect survives and growing state | Without any insect | Without any insect | Without any insect | Without any insect |
| Mould, bacteria growing situation | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium |
Illustrate that present invention can be implemented in plurality of cereals and various insects, mould, bacterium are disposably handled under same stifling environment.
Embodiment 19：Grain fumigating is tested
Grain variety：Corn, paddy, wheat, soybean, soya bean, broad bean, potato, sweet potato etc.
Disease：Aspergillus, mould, trichoderma, cladosporium herbarum, head mold, trichoderma, staphylococcus aureus, Escherichia coli,
Bacillus megaterium, hay bacillus, pseudomonas fluorescens, curculionid, lesser grain borer, casemaking clothes moth, silverfish, gelechiid, lasioderma serricorne,
Cockroach and Indian meal moth etc.
Fumigant：
Fumigant 2 (No. CAS：815-36-1)；
Fumigant 8 (No. CAS：2927-22-2)；
Fumigant 26 (No. CAS：154264-08-1)；
Fumigant 45 (No. CAS：2674-37-5)；
First any one above-mentioned fumigant is supported on filter paper, then the filter paper be placed on to the bottom of glass jar, then by grain
Food sample is placed on the top (can be by setting fixed frame to be achieved in glass jar) of filter paper, closed glass cylinder, in room
Temperature is lower stifling；Regular sampling monitoring insect death condition therein, obtains following testing result：
Learnt by internal standard method for gas chromatography instrument (GC-Ms) detection and analysis：Through any one above-mentioned fumigant suffocating treatment
Without fumigant residue in grain samples afterwards；In addition, by color difference meter observation through the stifling place of any one above-mentioned fumigant
Significant change does not occur for the color of the grain samples after reason.
Grain samples after any one above-mentioned fumigant suffocating treatment of the present embodiment are placed in room temperature environment, periodically
Mould, bacterium, insect growing state are tracked, following testing result is obtained：
| Resting period | 0 month | 1 month | 3 months | 6 months |
| Insect survives and growing state | Without any insect | Without any insect | Without any insect | Without any insect |
| Mould, bacteria growing situation | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium |
Illustrate that present invention can be implemented in plurality of cereals and various insects, mould, bacterium are disposably handled under same stifling environment.
Embodiment 20：Grain fumigating is tested
Grain variety：Corn, paddy, wheat, soybean, soya bean, broad bean, potato, sweet potato etc.
Disease：Aspergillus, mould, trichoderma, cladosporium herbarum, head mold, trichoderma, staphylococcus aureus, Escherichia coli,
Bacillus megaterium, hay bacillus, pseudomonas fluorescens, curculionid, lesser grain borer, casemaking clothes moth, silverfish, gelechiid, lasioderma serricorne,
Cockroach and Indian meal moth etc.
Fumigant：Fumigant 3 (No. CAS：18225-68-8)
First fumigant is supported on filter paper, the filter paper then is placed on into surface has mesh, comes with fan and temperature adjustment work(
Can hollow box in, then the box body is placed on to the bottom of glass jar, grain samples is placed on to the top of the box body, it is close
Glass jar is closed, the temperature of regulation box body is 30 DEG C, fumigated while opening under fan (wind speed is set as low speed)；Periodically
Sampling monitoring insect death condition therein, detailed results are as shown in the table：
Learnt by the detection and analysis of internal standard method for gas chromatography instrument：Do not fumigated in grain samples after above-mentioned suffocating treatment
Agent is remained；In addition, significant change does not occur for the color for observing the grain samples after above-mentioned suffocating treatment by color difference meter.
Grain samples after the present embodiment suffocating treatment are placed in room temperature environment, mould, bacterium, insect life is periodically tracked
Long situation, testing result see the table below shown：
| Resting period | 0 month | 1 month | 3 months | 6 months |
| Insect survives and growing state | Without any insect | Without any insect | Without any insect | Without any insect |
| Mould, bacteria growing situation | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium | Without any mould, bacterium |
Illustrate that present invention can be implemented in plurality of cereals and various insects, mould, bacterium are disposably handled under same stifling environment.
Finally it is necessary that described herein is that the foregoing is only the present invention preferably embodiment, but the guarantor of the present invention
Shield scope be not limited thereto, any one skilled in the art the invention discloses technical scope in, can be light
The change or replacement being readily conceivable that, should all be included within the scope of the present invention.
Claims (10)
1. a kind of fumigating method for being used to prevent and treat grain entomophthora, it is characterised in that including following operation：In room temperature to 40 DEG C of rings
Under border, fumigant is placed on to lower section or/and the surrounding of grain heap；The fumigant is with formula I：Or
Formula II：The compound of shown chemical constitution, wherein, in the formula I：X is halogen or hydroxyl；Y1And Y2
It is each independently selected from H or F；R1For R3Substituted C1-C10Alkyl, R3Substituted C2-C10Alkylene, R3Substituted benzene
Base, R3Substituted benzyl, R3Substituted C3-C8Cycloalkyl, R3Substituted C3-C8Cycloalkenyl group or R3Substituted adamantane
Base；The R3Selected from hydrogen, hydroxyl, halogen, C1-C3Alkyl, C2-C3At least one of alkylene；The formula II
In：X is halogen or hydroxyl；R2For R3Substituted C1-C4Alkyl, R3Substituted C2-C4Alkylene, R3Substituted phenyl,
R3Substituted benzyl, R3Substituted C3-C8Cycloalkyl, R3Substituted C3-C8Cycloalkenyl group or R3Substituted adamantyl；
The R3Selected from hydrogen, hydroxyl, halogen, C1-C3Alkyl, C2-C3At least one of alkylene.
2. fumigating method according to claim 1, it is characterised in that in the formula I：X be F, Cl, Br or
OH；Y1And Y2It is simultaneously F or Y1、Y2One of them is F；R1For R3Substituted C1-C10Alkyl, R3Substitution
C2-C10Alkylene, R3Substituted phenyl, R3Substituted benzyl, R3Substituted C3-C6Cycloalkyl, R3Substituted C3-C6Ring
Alkylene or R3Substituted adamantyl；The R3Selected from hydrogen, hydroxyl, fluorine, chlorine, bromine, methyl, ethyl, isopropyl,
At least one of pi-allyl.
3. fumigating method according to claim 2, it is characterised in that in the formula I：X is F or Cl；Y1With
Y2It is simultaneously F；R1For R3Substituted C1-C4Alkyl, R3Substituted C2-C4Alkylene, R3Substituted phenyl or R3
Substituted C3-C6Cycloalkyl；The R3Selected from least one of hydrogen, hydroxyl, fluorine, chlorine.
4. fumigating method according to claim 1, it is characterised in that in the formula II：X be F, Cl, Br or
OH；R2For R3Substituted C1-C4Alkyl, R3Substituted C2-C4Alkylene, R3Substituted phenyl, R3Substituted benzyl,
R3Substituted C3-C7Cycloalkyl, R3Substituted C3-C7Cycloalkenyl group or R3Substituted adamantyl；The R3Selected from hydrogen,
At least one of hydroxyl, fluorine, chlorine, bromine, methyl, ethyl, isopropyl, pi-allyl.
5. fumigating method according to claim 4, it is characterised in that in the formula II：X is F or Cl；R2For
R3Substituted C1-C4Alkyl, R3Substituted C2-C4Alkylene, R3Substituted C3-C7Cycloalkyl or R3Substituted phenyl；
The R3Selected from least one of hydrogen, hydroxyl, fluorine, chlorine.
6. fumigating method according to claim 1, it is characterised in that：At room temperature, fumigant is placed on closed environment
In grain heap lower section or/and surrounding.
7. fumigating method according to claim 1, it is characterised in that：The fumigant is supported on suction-operated
On carrier material, described carrier material includes but is not limited to filter paper, silica gel, filter membrane, cotton, sponge or cloth.
8. fumigating method according to claim 7, it is characterised in that：The carrier material for being loaded with fumigant is placed on tool
In the mouth of oriented external diffusion or the hollow devices of mesh face, described hollow devices include but is not limited to case structure, box structure,
Cage construction or sack.
9. fumigating method according to claim 8, it is characterised in that：The hollow devices have fan and speed-regulating function.
10. fumigating method according to claim 8 or claim 9, it is characterised in that：The hollow devices have self-heating and tune
Temperature function.
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| CN106973990B (en) | 2019-12-10 |
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