The composition composite with sulfonylurea herbicide
The application is for dividing an application
The applying date of original application is: on October 10th, 2003
Application number is: 200310110401.4
Denomination of invention is: a kind of composition that contains sulfonylurea herbicide
Technical field the present invention relates to a kind of weed killer herbicide and the composite composition of sulfonylurea herbicide, especially with weeding active compound 2-(4-methoxyl group-6-first sulphur pyrimidine-2-base) the composite composition of carbamoyl amino sulfonyl methyl benzoate (test code number HNPC-C9908).
The present China of background technology agricultural is more with the weed killer herbicide kind, benzoic acids, benzene oxygen class, diphenyl ether, sulfonylurea, amide-type, triazine, organic heterocyclic class weed killer herbicide are arranged, these weed killer herbicides or unitary agent or complex preparation are widely used in dry land weedings such as rice seedling bed, live field, transplanting paddy field and barley and wheat, rape, cotton, fiber crops, peanut, vegetables.
2-(4-methoxyl group-6-first sulphur pyrimidine-2-base) carbamoyl amino sulfonyl methyl benzoate; test code number HNPC-C9908; Chinese common name: Sulfonylurea (the following Sulfonylurea of all using); it is the noval chemical compound with obvious activity of weeding of Hunan Chemical Research Institute's invention; belong to sulfonylurea herbicide, chemical structural formula is:
The former medicine of Sulfonylurea is a white solid, and fusing point is 184-186 ℃, is mainly used in preventing and kill off of the various broad leaved weeds of wheat paddock and some grassy weeds, and its control efficiency is good.Hunan Chemical Research Institute with this compound and unitary agent application patent (compound patent No. ZL00113423.x preparation number of patent application 2003101104014), for drug effect and the safety that improves this weed killer herbicide, the work with this compound and other mixture of herbicides has been done in a large number by Hunan Chemical Research Institute.
Summary of the invention the purpose of this invention is to provide composition and the preparation method that the sulfonylurea herbicide Sulfonylurea is 2-(4-methoxyl group-6-first sulphur pyrimidine-2-base) carbamoyl amino sulfonyl methyl benzoate and other mixture of herbicides.
The present invention is to be active ingredient by weed killer herbicide Sulfonylurea and another kind of weed killer herbicide, adds a certain amount of carrier again, additive compound forms; Selected another kind of weed killer herbicide is wheat straw prestige, quizalofopethyl, 2, any in 4-D, 2 first, 4 chlorine, fluoroglycofen-ethyl, metsulfuron-methyl, Acetochlor, butachlor, Dou Er, prometryn and the clomazone; Selected carrier is one or more in white carbon, kaolin, diatomite, potter's clay, the precipitated calcium carbonate; The auxiliary agent of selecting for use is one or more among NN0, BX, MF, JFC, M-Ca, the M-Na; The percetage by weight that composition is formed is Sulfonylurea 1-25% (W/W), and another kind of weed killer herbicide is 1-50% (W/W), carrier 10-90% (W/W), auxiliary agent 5-10% (W/W).
The present composition adopts the conventional preparation method of pesticide wettable according to above prescription, after each component mixed, get final product by the comminution by gas stream machined, resulting product appearance is that white is to pale powder, fineness more than 98% less than 44 μ m, wetting time was less than 60 seconds, and the suspensibility of each active ingredient is all more than 85%, and the resolution ratio of sample each active ingredient after 54 ℃ of pressurizations are stored 14 days is all less than 5%.
The present composition is by indoor biometrics or field control effectiveness test, and the result shows that the more single agent of said composition activity of weeding all has synergistic effect preferably, and the crops wheat is had higher safety.
Embodiment
Embodiment 1
Take by weighing Sulfonylurea 10 grams, 2,4-D 20 grams, MF 1 gram, M-Ca 5 grams, diatomite are mended to 100 grams.Embodiment 1 product that processing obtains is a pale powder, and the suspensibility Sulfonylurea is 91.2%, 2, and 4-D is 85.6%, wetting time is 35 seconds, and sample was stored 14 days 54 ℃ of pressurizations, and the resolution ratio Sulfonylurea is 1.2%, 2,4-D is 4.6%, and storage back suspensibility is all more than 85%.
Embodiment 2
Take by weighing Sulfonylurea 20 grams, fluoroglycofen-ethyl 10 grams, BX 4 grams, M-Na 6 grams, potter's clay benefit to 100 grams.Embodiment 1 product that processing obtains is a pale powder, the suspensibility Sulfonylurea is 90.4%, fluoroglycofen-ethyl is 88.3%, wetting time is 40 seconds, sample was stored 14 days 54 ℃ of pressurizations, the resolution ratio Sulfonylurea is 0.4%, and fluoroglycofen-ethyl is 1.7%, and storage back suspensibility is for all more than 85%.
Embodiment 3
Take by weighing Sulfonylurea 5 grams, prometryn 50 grams, NNO 6 grams, M-Ca 4 grams, kaolin benefit to 100 grams.Embodiment 1 product that processing obtains is a pale powder, and the suspensibility Sulfonylurea is 89.6%, and prometryn is 87.3%, and wetting time is 43 seconds.
Embodiment 4
Taking by weighing Sulfonylurea 1 gram, Acetochlor 20 grams, NNO 4 grams, M-Ca 1 gram, white carbon 20 grams, diatomite mends to 100 grams.Embodiment 1 product that obtains of processing is a pale powder, and the suspensibility Sulfonylurea is 90.9%, Acetochlor is 93.7%, and wetting time is 45 seconds, sample was stored 14 days 54 ℃ of pressurizations, the resolution ratio Sulfonylurea is 1.4%, and Acetochlor is 1.5%, and storage back suspensibility is for all more than 85%.
Embodiment 5:
Take by weighing Sulfonylurea 5 gram, all your 25 grams, NNO 3 grams, BX 4 grams, kaolin are mended to 100 grams.Embodiment 7 products that processing obtains are pale powder, and the suspensibility Sulfonylurea is 90.6%, all you are 87.3%, and wetting time is 45 seconds, and sample was stored 14 days 54 ℃ of pressurizations, and the resolution ratio Sulfonylurea is 3.20%, and all you are 2.9%.
Below be embodiment 6-22:
| | Embodiment 6 | Embodiment 7 | Embodiment 8 | Embodiment 9 | Embodiment 10 | Embodiment 11 | Embodiment 12 | Embodiment 13 | Embodiment 14 | Embodiment 15 | Embodiment 16 | Embodiment 17 | Embodiment 18 | Embodiment 19 | Embodiment 20 | Embodiment 21 | Embodiment 22 |
| Sulfonylurea | 1 | 20 | 20 | 20 | 5 | 3 | 5 | 10 | 25 | 2 | 5 | 10 | 1 | 2 | 20 | 5 | 4 |
| 2，4-D | 50 | | | | | | | | | | | | | | | | |
| 2 first, 4 chlorine | | 20 | | | | | | | | | | | | | | | |
| Fluoroglycofen-ethyl | | | 8 | 4 | | | | | | | | | | | | | |
| Metsulfuron-methyl | | | | | 5 | | | | | | | | | | | | |
| Quizalofopethyl | | | | | | 25 | | | | | | | | | | | |
| Dicamba | | | | | | | 20 | | | | | | | | | | |
| Prometryn | | | | | | | | 50 | 25 | | | | | | | | |
| Acetochlor | | | | | | | | | | 20 | 25 | 10 | | | | | |
| All you | | | | | | | | | | | | | 20 | 20 | 20 | | |
| Butachlor | | | | | | | | | | | | | | | | 35 | |
| Clomazone | | | | | | | | | | | | | | | | | 40 |
| NNO | | | 4 | 1 | 5 | | | 6 | | 4 | 4 | 4 | 3 | 3 | 5 | 3 | |
| BX | | 1 | | | | 1 | 1 | 4 | 6 | | | | 2 | 2 | 3 | 4 | 1 |
| JFC | | | | | 1 | | | | | | | | | | | 2 | |
| M-Ca | 5 | 2 | | | | 6 | | | | 1 | 1 | | | | | | 5 |
| M-Na | | | 6 | 6 | | | | | 3 | | | 2 | | | 2 | | |
| MF | 3 | | | | | | 4 | | | | | | | | | | |
| White carbon | | | | | | 5 | 5 | | | 20 | 20 | 5 | | | | | 5 |
| Precipitated calcium carbonate | | | Supply | 20 | | | | | | | | | | | | | |
| Diatomite | Supply | | | Supply | Supply | | Supply | | | Supply | Supply | Supply | | | | | Supply |
| Kaolin | | Supply | | | | Supply | | Supply | Supply | | | | Supply | Supply | Supply | | |
| Potter's clay | | | | | | | | | | | | | | | | Supply | |
Further specify biologically active and the toxicity and the field efficacy of this composition product with table 1-table 9
Table 1 Sulfonylurea and 2, and the joint toxicity of 4-D (target: piemarker, potted plant cauline leaf is handled)
| Medicament and proportioning | Regression equation | Correlation coefficient | ?IC
90(g/ mu)
| Co-toxicity coefficient | Conclusion |
| Sulfonylurea 2,4-D embodiment 1 embodiment 6 | ?Y＝56.1035+19.7510x ?Y＝20.1629+15.7673x ?Y＝68.2285+14.3527x ?Y＝5.3153+29.7644x | ??0.8374 ??0.9751 ??0.9247 ??0.9991 | ????1.72 ????4.43 ????1.52 ????2.85 | ? ? ???191.08 ???151.79 | Synergy synergy |
The joint toxicity (target: recessed amaranth, potted plant cauline leaf processing) that table 2 Sulfonylurea and fluoroglycofen-ethyl are composite
| Medicament and proportioning | Regression equation | Correlation coefficient | ?IC
50(g/ mu)
| Co-toxicity coefficient | Conclusion |
| Sulfonylurea fluoroglycofen-ethyl embodiment 2 embodiment 8 embodiment 9 | ??Y＝20.8696+12.8696x ??Y＝47.0408+116.3265x ??Y＝75.1521+30.0679x ??Y＝35+93.5776x ??Y＝25.2174+38.5771x | ??0.9569 ??0.8885 ??0.9832 ??0.9972 ??0.8884 | ????5.37 ????0.37 ????0.49 ????0.59 ????1.68 | ? ? ??199.10 ??187.24 ??143.42 | Synergy synergy synergy |
The joint toxicity (target: Amaranthus retroflexus, potted plant cauline leaf processing) that table 3 Sulfonylurea and prometryn are composite
| Medicament and proportioning | Regression equation | Correlation coefficient | ?IC
90(g/ mu)
| Co-toxicity coefficient | Conclusion |
| Sulfonylurea prometryn embodiment 3 embodiment 13 embodiment 14 | ??Y＝35.5234+16.2615x ??Y＝82.5+0.4839x ??Y＝70+2.9091x ??Y＝76.4583+2.2670x ??Y＝6.8011+76.4583x | ??0.8597 ??0.9333 ??0.9592 ??0.8612 ??0.8612 | ????3.55 ????15.50 ????6.87 ????5.97 ????1.99 | ? ? ????174.29 ????166.34 ????290.30 | Synergy synergy synergy |
The joint toxicity of table 4 table 1 Sulfonylurea and Acetochlor (target: recessed amaranth, potted plant soil treatment)
| Test is handled | Regression equation | Correlation coefficient | ?IC
90(g/ mu)
| Co-toxicity coefficient | Conclusion |
| Sulfonylurea Acetochlor embodiment 4 product embodiments 15 product embodiments 16 product embodiments 17 products | ??Y＝53.33+5.71x ??Y＝34.79+1.69x ??Y＝57.67+2.40x ??Y＝61.1+2.1x ??Y＝68.5+3.1x ??Y＝64.8+5.1x | ??0.7247 ??0.8949 ??0.7659 ??0.77 ??0.79 ??0.84 | ????6.42 ????32.65 ????13.49 ????13.7 ????6.86 ????6.9 | ? ? ??202.59 ??173.79 ??282.91 ??155.14 | Synergy synergy synergy synergy |
Table 4 Sulfonylurea and your joint toxicities (target: recessed amaranth, potted plant soil treatment) all
| Test is handled | Regression equation | Correlation coefficient | ?IC
90(g/ mu)
| Co-toxicity coefficient | Conclusion |
| Sulfonylurea is that embodiment 5 products all | ?Y＝53.3+5.7x ?Y＝48.9+1.7x ?Y＝61.4+3.87x | ????0.72 ????0.71 ????0.86 | ????6.4 ????27.7 ????7.4 | ? ? ??240.77 | Synergy |
| Embodiment 18 product embodiments 19 product embodiments 20 products | ??Y＝60.9+1.9x ??Y＝61.7+1.7x ??Y＝69.4+9.4x | ??0.79 ??0.85 ??0.75 | ????15.4 ????16.4 ????2.2 | ????155.26 ????129.67 ????472.60 | Synergy synergy synergy |
The joint toxicity of table 5 Sulfonylurea and butachlor (target: recessed amaranth, potted plant soil treatment)
| Test is handled | Regression equation | Correlation coefficient | ??IC
90(g/cm
2)
| ???CTC | Conclusion |
| C9908 butachlor embodiment 21 products | ??Y＝53.33+5.71X ??Y＝20.1629+15.7673X ??Y＝68.2285+14.3527X | ??0.7247 ??0.9751 ??0.9247 | ????6.42 ????4.43 ????1.52 | ? ? ??191.08 | Synergy |
The joint toxicity of table 6 Sulfonylurea and clomazone (target: piemarker, potted plant soil treatment)
| Test is handled | Regression equation | Correlation coefficient | ??IC
90(g/cm
2)
| ????CTC | Conclusion |
| C9908 clomazone embodiment 22 products | ??Y＝34.501+19.38X ??Y＝25.334+10.82X ??Y＝32.798+18.97X | ??0.9486 ??0.9567 ??0.9631 | ????1.75 ????8.69 ????2.00 | ? ? ??318.0 | Synergy |
Table 7 embodiment 7 prevents and kill off wheat paddock weeds result of the test
| Embodiment 7 | Investigate object | Consumption (g/ mu) |
| ????10 | ????20 | ????30 | ????40 |
| 45 days strain preventive effect fresh weight preventive effects are to crop safety behind the total preventive effect medicine of weeds | 34.89% 81.78% 93.83% safety | 52.34% 90.23% 95.31% safety | 57.7% 91.09% 95.99% safety | 66.76% 92.48% 97.61% safety |
Table 8 embodiment 10 prevents and kill off wheat paddock weeds result of the test
| | Investigate object | Consumption (g/ mu) |
| ??????5 | ????10 | ????20 | ????30 |
| Embodiment 10 | After the dispenser 14 days preventive effects to lamb's-quarters to the total preventive effect medicine of the preventive effect of Amaranthus retroflexus after 28 days preventive effect fresh weight preventive effects to lamb's-quarters to crop safety | 6.3% 67.0% 66.7% 38.9% 87.8% safety | 22.7% 95.3% 71.1% 66.3% 80.3% safety | 42.3% 100% 76.7% 86.2% 97.2% safety | 67.8% 90.4% 82.6% 68.6% 90.3% safety |
Table 9 embodiment 11 and 12 prevents and kill off wheat paddock weeds result of the test
| Embodiment 11 | Investigate object amur foxtail fresh weight preventive effect ox chickweed fresh weight preventive effect Hairy Bittercress fresh weight preventive effect | Consumption (g/ mu) |
| ??10 ??45.6％ ??96.8％ ??98.2％ | ??20 ??82.6％ ??99.2％ ??98.7％ | ???30 ???92.1％ ???98.2％ ???98.2％ | ???40 ???92.0％ ???100％ ???100％ |
| | Stellaria alsine Grim. fresh weight preventive effect | | ??95.4％ | ??98.9％ | ??97.4％ | ??100％ |
| | To crop safety | | Safety | Safety | Safety | Safety |
| | Controlling object | Consumption (g/ mu) |
| ?????5 | ??10 | ???15 | ???20 |
| Embodiment 12 | The total preventive effect amur foxtail of the preventive effect weeds fresh weight preventive effect chickweed fresh weight preventive effect of the preventive effect broad leaved weed of amur foxtail is to crop safety | 65.8% 47.3% 62.1% 82.9% 87.7% safety | 72.5% 59.1% 69.9% 89.4% 95.1% safety | 82.8% 71.7% 80.6% 97.0% 95.7% safety | 86.4% 76.4% 84.4% 98.6% 96.4% safety |