CN102084863B - Slow-release preparation of slow-release thiadiazine substances - Google Patents
Slow-release preparation of slow-release thiadiazine substances Download PDFInfo
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- CN102084863B CN102084863B CN2011100483802A CN201110048380A CN102084863B CN 102084863 B CN102084863 B CN 102084863B CN 2011100483802 A CN2011100483802 A CN 2011100483802A CN 201110048380 A CN201110048380 A CN 201110048380A CN 102084863 B CN102084863 B CN 102084863B
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- China
- Prior art keywords
- slow
- release
- thiadiazine
- substances
- parts
- Prior art date
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Links
- 239000000126 substance Substances 0.000 title description 2
- JZFICWYCTCCINF-UHFFFAOYSA-N Thiadiazin Chemical compound S=C1SC(C)NC(C)N1CCN1C(=S)SC(C)NC1C JZFICWYCTCCINF-UHFFFAOYSA-N 0.000 title 1
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 9
- 239000011707 mineral Substances 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 7
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 5
- 239000001116 FEMA 4028 Substances 0.000 claims abstract 2
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims abstract 2
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims abstract 2
- 229960004853 betadex Drugs 0.000 claims abstract 2
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 5
- 239000005995 Aluminium silicate Substances 0.000 abstract 1
- 235000012211 aluminium silicate Nutrition 0.000 abstract 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 abstract 1
- 239000013081 microcrystal Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 230000000694 effects Effects 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 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 5
- 239000003905 agrochemical Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000000575 pesticide Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 235000020985 whole grains Nutrition 0.000 description 3
- 241000193830 Bacillus <bacterium> Species 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003405 delayed action preparation Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000000607 poisoning effect Effects 0.000 description 2
- 241000193171 Clostridium butyricum Species 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Chemical group OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 150000001923 cyclic compounds Chemical class 0.000 description 1
- 230000006735 deficit Effects 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004503 fine granule Substances 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 230000000361 pesticidal effect Effects 0.000 description 1
- 229910052615 phyllosilicate Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012207 quantitative assay Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000013268 sustained release Methods 0.000 description 1
- 239000012730 sustained-release form Substances 0.000 description 1
Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention provides an agricultural composition, which contains ammonium salt of 2-phenylimino-3-tert butyl-5-phenyl-tetrahydro-1,3,5-thiadiazine-4-ketone, beta-cyclodextrin and microcrystal kaolin mineral serving as a carrier.
Description
The present invention relates to a kind of sustained release preparation of diazthines material of slowly-releasing.
Since modern, along with population constantly increases, for the increasing demand increase of grain, therefore, the agricultural chemicals usage amount increases day by day, but the development of agricultural chemicals has brought a large amount of environmental pollutions, and this is the great realistic problem that we have to face.Particularly; In recent years along with development of urbanization; The rural laborer constantly shifts to cities and towns, and the professional number of being engaged in agriculture reduces, by labor savings, and the requirement that the industrial structure problem that agricultural had derived from such as suitably to enlarge during the spreading during spreading strong day by day.Therefore, aspect pesticide developing, need the spreading number of times few, can safety operation, low dose but can keep the medicament of effect for a long time.
But, because the medicament spreading is inhomogeneous etc., often producing superfluous absorption, absorption and the poisoning effect that causes for the plant corpus that should protect, this is a severe impairment to the person of being engaged in agriculture.That is to say, hope that the spreading number of times is few and residual effect property is long, safe, the little technology of plant to the contaminative of environment.
So far, developed the slowly-releasing of the method control agricultural chemicals that uses resin, lyophobic dust and adsorptive support.
Yet these methods have the control effect of rate of release few, are difficult for realizing industrialization.
The prepared composition pesticide of the present invention has solved above-mentioned these existing problems; The composition pesticide that it provided, owing to controlled the rate of release of pesticide activity component from combination carrier, thereby can keep residual effect property for a long time; And can prevent the pollution of the environment, alleviate poisoning.
The diazthines compound is one type of agricultural chemicals commonly used, the present invention relates to the 2-phenylimino-3-tert-butyl group-5-phenyl-tetrahydrochysene-1,3,5-thiadiazine-4-ketone.This compound is a kind of diazthines compound of novel improved, and the present invention at first is made into ammonium salt, process more help behind the ammonium salt its in water dissolving and by plant absorbing.What use is the method for generation ammonium salt commonly used well known in the art, for example mixes transpiring moisture then with concentrated ammonia liquor.
Cyclodextrin is that Villers separated from the starch digestion liquid of bacillus (Bacillus) amylobacter (Bacillus Amylobacter) first in 1891 and obtains; Its correct chemical constitution is just delivered after decades; Clear and definite cyclodextrin be one type by the D2 glucopyranose units through α 21; The cyclic compound that 4 glycosidic bonds join end to end and form, common α 2, β 2 and γ 2 cyclodextrin have 6,7 and 8 glucose units respectively.Because cyclodextrin molecule particular structure, it has some novel character.
The montmorillenite class mineral that use following formula among the present invention are as carrier, and it all belongs to has the phyllosilicate of three-decker mineral.
(Al
5/3Mg
1/3)Si
4O
10(OH)
2·W
1/3·mH
2O
The present invention can also further use other carrier, like mineral matter micro powder, the granular mineral of clay etc., inorganic salts etc.Adjuvant has surfactant, stabilizing agent, physical property modifying agent, bond, colouring agent, incremental agent etc.
The present invention's solid pesticide composition has granula, fine granule and pulvis etc.It adopts conventional breaking method that active component is pulverized, and mixes with cyclodextrin then, adds carrier at last and produces.
Embodiment:
Below illustrate in greater detail the present invention for example.All expressions " parts by weight " or " weight % " of " part " in following examples, " % ".
Embodiment 1
The 30 parts of 2-phenylimino-3-tert-butyl group-5-phenyl-tetrahydrochysenes-1,3 add 60 parts of beta-schardinger dextrin-s in 5-thiadiazine-4-ketone, 570 parts of above-mentioned montmorillenite class mineral add an amount of water and mix after the mixing.The thing that mixes of above gained is placed on granulation in the comminutor that the aperture is the 0.9mm screen cloth is housed, after the shot-like particle drying, thereby whole grain makes the granula that contains active component 3%.
Embodiment 2 (granula)
The 26 parts of 2-phenylimino-3-tert-butyl group-5-phenyl-tetrahydrochysenes-1,3 add 60 parts of beta-schardinger dextrin-s in 5-thiadiazine-4-ketone, 570 parts of above-mentioned montmorillenite class mineral add an amount of water and mix after the mixing.The thing that mixes of above gained is placed on granulation in the comminutor that the aperture is the 0.9mm screen cloth is housed, after the shot-like particle drying, thereby whole grain makes the granula that contains active component 2.4%.
Embodiment 3 (granula)
The 44 parts of 2-phenylimino-3-tert-butyl group-5-phenyl-tetrahydrochysenes-1,3 add 70 parts of beta-schardinger dextrin-s in 5-thiadiazine-4-ketone, 600 parts of above-mentioned montmorillenite class mineral add an amount of water and mix after the mixing.The thing that mixes of above gained is placed on granulation in the comminutor that the aperture is the 0.9mm screen cloth is housed, after the shot-like particle drying, thereby whole grain makes the granula that contains active component 4.7%.
Embodiment 4 (stripping property test in the water)
In beaker, add entry 90ml, in 25 ℃ thermostatic chamber, left standstill 1.Get embodiment 1 prepared product 90mg, evenly be dispensed onto in this beaker.Spreading 1 day, 3, center (depth of water 1cm) water sampling after 9 days and 15 days in the beaker was with each active component of high-speed liquid chromatography analyzer quantitative assay.
According to the amount (μ g) of various active components contained in the granula of amount that is dissolved into each active component in the water (μ g) and spreading or the pulvis, obtain dissolution rate with following formula.
Dissolution rate in the water (%)=(dissolving in the active principle (μ g) in the water)/(in the granula of spreading or the pulvis contained active principle (μ g)) * 100
| Embodiment | After 1 day | After 3 days | After 9 days | After 15 days | After 30 days |
| Embodiment 1 | 17.2 | 34.4 | 46.7 | 61.4 | 72.6 |
| Embodiment 2 | 18.5 | 32.5 | 42.7 | 59.1 | 74.4 |
| Embodiment 3 | 24.1 | 36.7 | 48.6 | 63.2 | 78.1 |
| Embodiment 4 | 22.4 | 33.5 | 45.4 | 60.2 | 78.6 |
Find that through above-mentioned experiment the sustained release agent that the present invention makes has very good slow release effect.
Claims (1)
1.
OneKind of agricultural is used composition, and it contains the 2-phenylimino-3-tert-butyl group-5-phenyl-tetrahydrochysene-1,3, the ammonium salt of 5-thiadiazine-4-ketone, beta cyclodextrin and as the montmorillenite class mineral of carrier.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100483802A CN102084863B (en) | 2011-03-01 | 2011-03-01 | Slow-release preparation of slow-release thiadiazine substances |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100483802A CN102084863B (en) | 2011-03-01 | 2011-03-01 | Slow-release preparation of slow-release thiadiazine substances |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102084863A CN102084863A (en) | 2011-06-08 |
| CN102084863B true CN102084863B (en) | 2012-03-28 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011100483802A Expired - Fee Related CN102084863B (en) | 2011-03-01 | 2011-03-01 | Slow-release preparation of slow-release thiadiazine substances |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102084863B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104351176A (en) * | 2014-11-11 | 2015-02-18 | 济南新起点医药科技有限公司 | Allicin controlled release formulation |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61197503A (en) * | 1985-02-25 | 1986-09-01 | Nippon Nohyaku Co Ltd | Agricultural chemical composition |
| AU748665B2 (en) * | 1997-07-23 | 2002-06-06 | Kanesho Soil Treatment Sprl/Bvba | Plant protection products in the form of a granulate with controlled release of the active agent |
| CN101385475A (en) * | 2007-12-27 | 2009-03-18 | 广东省中药研究所 | Slow-release natural insecticide |
| CN101390513B (en) * | 2008-10-17 | 2011-10-05 | 中国农业大学 | Uniconazole-cyclodextrin clathrate, preparation method and use thereof |
| CN101946811B (en) * | 2010-08-26 | 2013-07-31 | 天津绿新低温科技有限公司 | Microencapsulated botanical insect-resist agent |
-
2011
- 2011-03-01 CN CN2011100483802A patent/CN102084863B/en not_active Expired - Fee Related
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| Publication number | Publication date |
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| CN102084863A (en) | 2011-06-08 |
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Owner name: NINGBO YINZHOU HAOSI RUIPU BIOTECHNOLOGY CO., LTD. Free format text: FORMER OWNER: LIU PENG Effective date: 20120129 |
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| C41 | Transfer of patent application or patent right or utility model | ||
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| CB03 | Change of inventor or designer information |
Inventor after: Liu Peng Inventor after: Jiang Miao Inventor before: Liu Peng |
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| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: LIU PENG TO: LIU PENG JIANG MIAO Free format text: CORRECT: ADDRESS; FROM: 100061 CHONGWEN, BEIJING TO: 315100 NINGBO, ZHEJIANG PROVINCE |
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Effective date of registration: 20120129 Address after: 315100 Zhejiang city of Ningbo province Yinzhou District River Street 4 No. 11 Kaixuan tomorrow Applicant after: NINGBO YINZHOU HAOSIRUIPU BIOTECHNOLOGY CO.,LTD. Address before: 100061 Room 601, jade building, Guangming Road, No. 11, Chongwen District, Beijing Applicant before: Liu Peng |
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Owner name: JIANGSU HUAXIN HIGH-TECH ENTERPRISE CO., LTD. Free format text: FORMER OWNER: NINGBO YINZHOU HAOSI RUIPU BIOTECHNOLOGY CO., LTD. Effective date: 20130719 |
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Free format text: CORRECT: ADDRESS; FROM: 315100 NINGBO, ZHEJIANG PROVINCE TO: 226602 NANTONG, JIANGSU PROVINCE |
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Effective date of registration: 20130719 Address after: 226602 No. 288 Changjiang West Road, Haian County, Nantong, Jiangsu Patentee after: Jiangsu Huaxin hi tech Innovation Co.,Ltd. Address before: 315100 Zhejiang city of Ningbo province Yinzhou District River Street 4 No. 11 Kaixuan tomorrow Patentee before: NINGBO YINZHOU HAOSIRUIPU BIOTECHNOLOGY CO.,LTD. |
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Granted publication date: 20120328 |