CN102349534A - Imidacloprid and pymetrozine compound microcapsule suspension and preparation method thereof - Google Patents
Imidacloprid and pymetrozine compound microcapsule suspension and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an imidacloprid and pymetrozine compound microcapsule suspension and a preparation method thereof, and belongs to the technical field of pesticide production. The pesticide is prepared from imidacloprid and pymetrozine serving as main active substances, a little amount of organic solvent and emulsifying agent and urea resin serving as a cyst membrane material by an interface polymerization-curing method. The toxic component of the compound microcapsule pesticide is coated by the urea resin, and the compound microcapsule pesticide has the advantages of safety, low toxicity, high efficiency, stability and the like; and meanwhile, the pesticide component in the suspension is slowly released through the cyst membrane material, so that the prevention and control time of the suspension is prolonged, and the effective utilization rate of the pesticide component is improved. The suspension is suitable for preventing and controlling pests such as rice hopper, rice thrip and the like.
Description
Technical field
The present invention relates to the preparing technical field of agricultural chemicals, relate in particular to a kind of micro-capsule suspension agricultural chemicals by Imidacloprid and Pyraphione compound and preparation method thereof.
Background technology
Along with the development of pesticide science, safe, efficient, oligosaprobic novel form like aqueous emulsion, microemulsion, aqueous suspension, spread drops, dried flowable, water dispersible granules and microcapsule formulations etc., has become formulations of pesticide new development trend.(Microcapsules is as cyst wall or cyst membrane, through chemistry, physics or physico-chemical process with macromolecular material MC) to microcapsule formulations; Pesticidal active substance is wrapped up; Forming a kind of microencapsulation with semipermeability cyst membrane, is one of novel form of the highest, the tool DEVELOPMENT PROSPECT of technology content in the current pesticides new formulation, and its advantage can be in the time of expection; With the control flow velocity pesticidal active substance is continued slowly to discharge, reach the purpose that kills off the insect pests.Have that efficiency time is long, low to environment and human toxicity, effective ingredient good stability and being difficult for by characteristics such as rain drop erosiones.
The application of microcapsules technology in pesticide industry; Take the lead in releasing parathion-methyl commodity microcapsule formulations early than U.S. Pennwalt company in 1974; The commodity that a plurality of brands and specification have been arranged at present on the market; The Imidacloprid that companies such as the parathion of producing like Pennwalt company, the Eptam that Stauffer company produces, methoprene that Zoecon company produces, the farming of Tao Shi benefit produce, the domestic report that microcapsule formulations products such as parathion, phoxim, fenthion, parathion-methyl are also arranged.
Imidacloprid (imidacloprid) and pyrrole aphid ketone (Pymetrozine) are the insecticides of two kinds of different effects mechanism.Imidacloprid belongs to nicotinic insecticide, and it is a systemic insecticide, and the tool stomach poison function is used to prevent and treat sucking pest, and is also effective to coleoptera, diptera and Lepidoptera part insect, is mainly used in crop pests such as control paddy and wheat, cotton, vegetables, fruit tree.Pyrrole aphid ketone belongs to non-lethal novel pesticide, can be used for preventing and treating most of homoptera pest, and especially aphid section, Aleyrodidae, Delphacidae insect are applicable to vegetables, paddy rice, cotton, fruit tree and multiple field crop.Multiple pulvis or the emulsifiable concentrate pesticide product that contains Imidacloprid or the agent of pyrrole aphid ketone list arranged in the market, use wider; In addition, also there is part to relate to the complex preparation of Imidacloprid and pyrrole aphid ketone, but up to now, the composite micro-capsule suspension of Imidacloprid and pyrrole aphid ketone do not arranged as yet.
Summary of the invention
The present invention seeks to; Pulvis or emulsifiable concentrate pesticide product to Imidacloprid or the agent of pyrrole aphid ketone list in the past; Existing poor stability, environmental pollution are big, the lasting period is short, the more high deficiency of control cost, develops a kind ofly to prevent and treat that spectrum is wide, drug effect is high, stability is strong, environmental pollution is little, the lasting period is long, prevent and treat lower-cost Imidacloprid and the pymtrozine composite microcapsule suspension pesticidal preparations that meets the pollution-less agriculture production requirement; Another object of the present invention is the preparation method who proposes this composite micro-capsule suspension.
The object of the invention is achieved through following technical scheme:
A kind of Imidacloprid and pymtrozine composite microcapsule suspending agent; It is activated feedstock that this suspending agent can adopt the Imidacloprid of 55-65 weight % and the pyrrole aphid ketone of 35-45 weight %; Be dissolved in organic solvent earlier, and after adding emulsifying dispersant, through the pollopas polymerizing curable; Add emulsifying dispersant and high-speed stirred again, process stable micro-capsule suspension and obtain.
A kind of method for preparing Imidacloprid and pymtrozine composite microcapsule suspending agent, this method is carried out according to the following steps:
1) assembly of Imidacloprid and pyrrole aphid ketone: through indoor determination of activity, Imidacloprid and pyrrole aphid ketone is 55-65 weight % by weight: the ratio of 35-45 weight % is composite, and the co-toxicity coefficient that makes both is more than 180, and weighing, mixing are subsequent use;
2) preparation of core material: with step 1) assembly mixture and organic solvent by weight 2～5: 1 mixed, be dissolved into solution; With this solution and emulsifying dispersant 80～210: 1 mixed, stirring by weight, process the core material composition again;
3) preparation of pollopas preformed objects: with urea and formaldehyde ratio weighing in 1: 2 by weight, get the raw materials ready; Formaldehyde is poured in the reactor, added the urea of 2/3 amount earlier, adjust pH to 8.0 is heated to 50 ℃, reacts after 30 minutes, adds remaining 1/3 urea again, is heated to 70 ℃, continues reaction after 30 minutes, is cooled to room temperature, processes the pollopas preformed objects, and is subsequent use;
4) polymerization-curing of microcapsule formulations: take by weighing step (3) pollopas preformed objects; With step (2) core material composition and pollopas preformed objects 0.5～3: 1 ratio by weight, to pour in the reactor and mix, the following 2000 rev/mins of stirrings of room temperature, and adjust pH to 4.5～5.5 were carried out interface polymerization reaction 30 minutes; Again this reaction system is transferred pH to 2～3, continue reaction after 30 minutes, transfer mixing speed to 500 rev/min; And by heating up 5 ℃ speed in per 10 minutes, slowly be warming up to 30～50 ℃ after, continue to stir and be cured in 20 minutes; Transfer pH to neutral reaction system at last, finish reaction;
5) preparation of micro-capsule suspension: the consumption of pressing final products gross weight 2～5%; In step 4) microcapsule formulations polymerization-solidfied material, add emulsifying dispersant once more; And after water complements to 100% weight; After at room temperature stirring 1 hour, promptly process Imidacloprid and pymtrozine composite microcapsule suspension formulation with 400 rev/mins.
Said solvent is nitroparaffins, and said nitroparaffins can be one or more the combination solvents in nitroethane, 1-nitropropane, the 2-nitropropane.
Said emulsifying dispersant is that agricultural newborn 0201-B, 0204-C, 0204-B, OP series, tween are serial, the mixture of a kind of or any two kinds of arbitrary proportions among methylcellulose, sodium carboxymethylcellulose, gelatin, gum Arabic or the polyvinyl alcohol.
Said preparation can be used for preventing and treating insects such as rice fulgorid, white-backed planthopper, paddy rice thrips.
Beneficial effect of the present invention:
One, clear and definite through result of the test; Its co-toxicity coefficient of complex preparation of Imidacloprid and pyrrole aphid ketone can reach more than 180; Have tangible synergy advantage than two single agent: at first, composite product obviously strengthens the insecticidal activity of insects such as paddy rice brown planthopper, small brown rice planthopper and paddy rice thrips; Secondly, the control efficiency of composite product antagonism insect is outstanding, and particularly for the brown planthopper and the small brown rice planthopper that most of agricultural chemicals had been developed immunity to drugs in recent years, this product still can have the control efficiency more than 80%; At last, the more single agent of composite product can reduce control cost 15-25%.
Two, to existing some shortcomings parts of conventional pesticide formulation such as missible oil, pulvis, the present invention through composite, microcapsules technology, is prepared into the microcapsules suspension formulation with Imidacloprid and pyrrole aphid ketone; This product is capsule film material with the pollopas, and two kinds of farm chemical ingredients are wrapped among the nontoxic cyst membrane, not only can reduce the contact toxicity of Pesticidal products, but also improve the stability of active ingredient greatly; In addition; Because two kinds of compositions are after the capsule suitcase is wrapped up in; The release of active ingredient has obtained control preferably, makes effective control time of product obviously prolonged (seeing table 1, table 2), thereby can effectively avoid repeatedly using agricultural chemicals; Significantly reduce the input amount of agricultural chemicals, alleviate pollution environment to environment; Therefore, Imidacloprid of the present invention and pymtrozine composite microcapsule suspension pesticide meet the requirement that present pollution-less agriculture is produced, and application prospect is comparatively wide.
Embodiment
Below in conjunction with embodiment the present invention is done further detailed description, but content of the present invention is not limited thereto.
48% Imidacloprid missible oil: Xianju Pesticide Factory, Zhejiang Prov.;
25% pyrrole aphid ketone wetting powder: Jiangsu Anpon Electrochemical Co., Ltd.;
Urea: chemical plant, Gansu Province, west, Shantou, 99%;
Formaldehyde: Shijiazhuang metal and stone chemical fertilizer Co., Ltd, 38%.
Embodiment 1 (Imidacloprid, pymtrozine composite microcapsule suspending agent product one):
A kind of Imidacloprid and pymtrozine composite microcapsule suspending agent, preparation according to the following steps:
1) assembly of Imidacloprid and pyrrole aphid ketone: take by weighing Imidacloprid 12 grams and pyrrole aphid ketone 8 grams, mix, subsequent use;
2) preparation of core material: 20 gram mixtures of step 1) assembly are dissolved into solution with 3 gram nitroethanes, again this solution are mixed with 0.2 gram 0201-B, process the core material composition;
3) preparation of pollopas preformed objects: with urea and formaldehyde ratio weighing in 1: 2 by weight; Formaldehyde is poured in the reactor, added the urea of 2/3 amount again,, be heated to 50 ℃ with 5% sodium hydroxide solution adjust pH to 8.0; React after 30 minutes, add residue 1/3 urea again, be heated to 70 ℃, continue to react half an hour; Be cooled to room temperature, process the pollopas preformed objects, subsequent use;
4) polymerization-curing of microcapsule formulations: take by weighing step (3) pollopas preformed objects 7.73 grams and step (2) core material composition 23.2 grams; Pour in the reactor and mix mutually; At room temperature 2000 rev/mins of stirrings transfer to 4.5～5.5 with 5% watery hydrochloric acid with the pH value, carry out interface polymerization reaction 30 minutes; Again reaction system is transferred to 2～3 with 5% watery hydrochloric acid with the pH value; Continue reaction after 30 minutes, adjustment mixing speed to 500 rev/min, and by heating up 5 ℃ speed in per 10 minutes; After slowly being warming up to 30～50 ℃; Continue stirring and be cured in 20 minutes, with 5% sodium hydroxide solution pH value of reaction system is transferred to neutrality at last, finish reaction;
5) preparation of micro-capsule suspension product: with polymerization-solidfied material 30.93 grams and the 2 gram Tween-20s and the 1 gram polyvinyl alcohol mixing of microcapsule formulations; And after water 66.07 gram complements to 100% weight; At room temperature 400 rev/mins were stirred 1 hour, promptly processed 20% Imidacloprid and pymtrozine composite microcapsule suspension formulation 100 grams.
Embodiment 2: (Imidacloprid, pymtrozine composite microcapsule suspending agent product two)
Press Imidacloprid 14 grams, pyrrole aphid ketone 8 grams, 1-nitropropane 2 grams and agricultural newborn 0201-B 0.3 restrain encystation heart mixture fully; In capsule heart mixture 24.3 grams and pollopas preformed objects 8.1 gram (3: 1) ratios, be prepared into the polymerization-solidfied material of microcapsule formulations; Add 3 gram 0201-B and 1 gram Tween-85 at last, and water 63.6 gram supplies 100%, be prepared into 22% Imidacloprid pymtrozine composite microcapsule suspension formulation, 100 grams by embodiment 1 technology, step.
Embodiment 3: (Imidacloprid, pymtrozine composite microcapsule suspending agent product three)
Press Imidacloprid 12 grams, pyrrole aphid ketone 9 grams, 2-nitropropane 4 grams and 0.1 gram polysorbas20 and 0.2 gram polysorbate60, preparation encystation heart mixture; In capsule heart mixture 25.3 grams and pollopas preformed objects 8.5 gram (3: 1) ratios, be prepared into the polymerization-solidfied material of microcapsule formulations; Add 2 gram OP-5 and 1 gram gelatin at last, and water 63.2 gram supplies 100%, be prepared into 21% Imidacloprid pymtrozine composite microcapsule suspension formulation, 100 grams by embodiment 1 technology, step.
Embodiment 4: (Imidacloprid, pymtrozine composite microcapsule suspending agent product four)
Press Imidacloprid 19 grams, pyrrole aphid ketone 19 grams, 2-nitropropane 4 grams and the agricultural newborn 0204-B of 0.3 gram, preparation encystation heart mixture; In capsule heart mixture 42.3 grams and pollopas preformed objects 42.3 gram (1: 1) ratios, be prepared into the polymerization-solidfied material of microcapsule formulations; Add 3 gram 0201-B and 1 gram gum Arabic at last, and water 11.4 gram supplies 100%, be prepared into 38% Imidacloprid pymtrozine composite microcapsule suspension formulation, 100 grams by embodiment 1 technology, step.
Embodiment 5: (Imidacloprid, pymtrozine composite microcapsule suspending agent product five)
Press Imidacloprid 20 grams, pyrrole aphid ketone 10 grams add nitroethane 7 grams and the agricultural newborn 0204-C of 0.3 gram, preparation encystation heart mixture; In capsule heart mixture 37.3 grams and pollopas preformed objects 18.7 gram (2: 1) ratios, be prepared into the polymerization-solidfied material of microcapsule formulations; Add 1.5 gram OP-10 and 0.5 gram polyvinyl alcohol at last, and water 42 gram supplies 100%, be prepared into 30% Imidacloprid pymtrozine composite microcapsule suspension formulation, 100 grams by embodiment 1 technology, step.
Embodiment 6: (Imidacloprid, pymtrozine composite microcapsule suspending agent product six)
Press Imidacloprid 16.5 grams, pyrrole aphid ketone 13.5 grams, nitroethane 12 grams and the agricultural newborn 0204-B of 0.3 gram, preparation encystation heart mixture; In capsule heart mixture 42.3 grams and pollopas preformed objects 42.3 gram (1: 1) ratios, be prepared into the polymerization-solidfied material of microcapsule formulations; Add 3 gram 0204-B and 1 gram sodium carboxymethylcellulose at last, and water 11.4 gram supplies 100%, be prepared into 30% Imidacloprid pymtrozine composite microcapsule suspension formulation, 100 grams by embodiment 1 technology, step.
Embodiment 7: (Imidacloprid, pymtrozine composite microcapsule suspending agent product seven)
Press Imidacloprid 30 grams, pyrrole aphid ketone 25 grams add nitroethane 7 grams and the agricultural newborn OP-5 of 0.3 gram, preparation encystation heart mixture; In capsule heart mixture 62.3 grams and pollopas preformed objects 20.8 gram (3: 1) ratios, be prepared into the polymerization-solidfied material of microcapsule formulations; Add 3 gram Tween-85s and 2 gram methylcellulose at last, and water 11.9 gram supplies 100%, be prepared into 55% Imidacloprid pymtrozine composite microcapsule suspension formulation, 100 grams by embodiment 1 technology, step.
Embodiment 8: (Imidacloprid, pymtrozine composite microcapsule suspending agent product eight)
Press Imidacloprid 26 grams, pyrrole aphid ketone 14 grams add nitroethane 5 grams and agricultural newborn 0201-B 0.3 gram, preparation encystation heart mixture; In capsule heart mixture 45.3 grams and pollopas preformed objects 45.3 gram (1: 1) ratios, be prepared into the polymerization-solidfied material of microcapsule formulations; Add 3 gram 0201-B and 1 gram polyvinyl alcohol at last, and water 5.4 gram supplies 100%, be prepared into 40% Imidacloprid pymtrozine composite microcapsule suspension formulation, 100 grams by embodiment 1 technology, step.
Test Example 1: (Imidacloprid pyrrole aphid ketone micro-capsule suspension control paddy rice brown planthopper field control effectiveness test)
Test period: in September, 2010;
Test place: Huzhou, Zhejiang;
Subjects: paddy rice brown planthopper;
Test medicine: 30% Imidacloprid pyrrole aphid ketone microcapsule formulations (product five);
Contrast medicament: 48% Imidacloprid missible oil (Xianju Pesticide Factory, Zhejiang Prov.); 25% pyrrole aphid ketone wetting powder (Jiangsu Anpon Electrochemical Co., Ltd.)
Composite microcapsule formulations of table 1 the present invention and the test of former prescription agent control paddy rice brown planthopper effect comparison
This shows that Imidacloprid pyrrole aphid ketone micro-capsule suspension of the present invention control paddy rice brown planthopper is compared 48% Imidacloprid missible oil and 25% pyrrole aphid ketone wetting powder has better effect.
Test 2 (Imidacloprid pyrrole aphid ketone micro-capsule suspension control paddy rice thrips field control effectiveness test)
Test period: in June, 2010;
Test place: Zhejiang Hangzhou;
Subjects: paddy rice thrips;
Test medicine: 20% Imidacloprid pyrrole aphid ketone microcapsule formulations (product one);
Contrast medicament: 48% Imidacloprid missible oil (Xianju Pesticide Factory, Zhejiang Prov.); 25% pyrrole aphid ketone wetting powder (Jiangsu Anpon Electrochemical Co., Ltd.).
Composite microcapsule formulations of table 2 the present invention and the test of former prescription agent waterproof rice thrips effect comparison
This shows that Imidacloprid pyrrole aphid ketone micro-capsule suspension of the present invention control paddy rice thrips is compared 48% Imidacloprid missible oil and 25% pyrrole aphid ketone wetting powder has better effect.
Test Example 3: (Imidacloprid pyrrole aphid ketone micro-capsule suspension control paddy rice brown planthopper field control effectiveness test)
Test period: in September, 2010;
Test place: Huzhou, Zhejiang;
Subjects: paddy rice brown planthopper;
Test medicine: 38% Imidacloprid pyrrole aphid ketone microcapsule formulations (product four);
The contrast medicament: Imidacloprid and pyrrole aphid ketone are 38% with the active component gross weight wherein with the composite missible oil that forms of 1: 1 weight ratio, and emulsifier op-10 is 12 weight %, and solvent xylene is that 50 weight % are mixed with 38% Imidacloprid and pyrrole aphid ketone cream preparation.
Composite microcapsule formulations of table 3 the present invention and Imidacloprid and the test of pyrrole aphid ketone missible oil control paddy rice brown planthopper effect comparison
This shows, be in the weight ratio of Imidacloprid and pyrrole aphid ketone under 1: 1 the situation that of the present invention 38% Imidacloprid pyrrole aphid ketone micro-capsule suspension control paddy rice brown planthopper is compared 38% Imidacloprid and pyrrole aphid ketone cream preparation and has better effect.
Imidacloprid of the present invention and pymtrozine composite microcapsule suspending agent and preparation method thereof are described through concrete embodiment.Those skilled in the art can use for reference links such as content appropriate change raw material of the present invention, process conditions and realize corresponding other purpose; Its relevant change does not all break away from content of the present invention; All similar replacements and change will become apparent to those skilled in the art that all to be regarded as and are included within the scope of the present invention.
Claims (2)
1. Imidacloprid and pymtrozine composite microcapsule suspending agent; It is characterized in that: said suspending agent is an activated feedstock with the Imidacloprid of 55-65 weight % and the pyrrole aphid ketone of 35-45 weight %; Be dissolved in organic solvent earlier, and after adding emulsifying dispersant, through the Lauxite polymerizing curable; Add emulsifying dispersant and high-speed stirred again, process stable micro-capsule suspension and obtain; Wherein said organic solvent is nitroparaffins, and said nitroparaffins can be one or more the combination solvents in nitroethane, 1-nitropropane, the 2-nitropropane; Said emulsifying dispersant is that agricultural newborn 0201-B, 0204-C, 0204-B, OP series, tween are serial, the mixture of a kind of or any two kinds of arbitrary proportions among methylcellulose, sodium carboxymethylcellulose, gelatin, gum Arabic or the polyvinyl alcohol.
2. method for preparing said Imidacloprid of claim 1 and pymtrozine composite microcapsule suspending agent is characterized in that this method carries out according to the following steps:
1) assembly of Imidacloprid and pyrrole aphid ketone: through indoor determination of activity, Imidacloprid and pyrrole aphid ketone is 55-65 weight % by weight: the ratio of 35-45 weight % is composite, and the co-toxicity coefficient that makes both is more than 180, and weighing, mixing are subsequent use;
2) preparation of core material: with step 1) assembly mixture and organic solvent by weight 2～5: 1 mixed, be dissolved into solution; With this solution and emulsifying dispersant 80～210: 1 mixed, stirring by weight, process the core material composition again;
3) preparation of pollopas preformed objects: with urea and formaldehyde ratio weighing in 1: 2 by weight, get the raw materials ready; Formaldehyde is poured in the reactor, added the urea of 2/3 amount earlier, adjust pH to 8.0 is heated to 50 ℃, reacts after 30 minutes, adds remaining 1/3 urea again, is heated to 70 ℃, continues reaction after 30 minutes, is cooled to room temperature, processes the pollopas preformed objects, and is subsequent use;
4) polymerization-curing of microcapsule formulations: take by weighing step (3) pollopas preformed objects; With step (2) core material composition and pollopas preformed objects 0.5～3: 1 ratio by weight, to pour in the reactor and mix, the following 2000 rev/mins of stirrings of room temperature, and adjust pH to 4.5～5.5 were carried out interface polymerization reaction 30 minutes; Again this reaction system is transferred pH to 2～3, continue reaction after 30 minutes, transfer mixing speed to 500 rev/min; And by heating up 5 ℃ speed in per 10 minutes, slowly be warming up to 30～50 ℃ after, continue to stir and be cured in 20 minutes; Transfer pH to neutral reaction system at last, finish reaction;
5) preparation of micro-capsule suspension: the consumption of pressing final products gross weight 2～5%; In step 4) microcapsule formulations polymerization-solidfied material, add emulsifying dispersant once more; And after water complements to 100% weight; After at room temperature stirring 1 hour, promptly process Imidacloprid and pymtrozine composite microcapsule suspension formulation with 400 rev/mins.
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| CN102599165A (en) * | 2012-02-21 | 2012-07-25 | 广东中迅农科股份有限公司 | Azoxystrobin microcapsule suspending agent and preparation method thereof |
| CN103210933A (en) * | 2013-03-24 | 2013-07-24 | 广东中迅农科股份有限公司 | Bispyribac-sodium and penoxsulam-containing pesticide microcapsule suspending agent |
| CN103329908A (en) * | 2013-03-24 | 2013-10-02 | 广东中迅农科股份有限公司 | Pymetrozine microcapsule suspending agent and preparation method thereof |
| CN103651505A (en) * | 2013-12-04 | 2014-03-26 | 南京农业大学 | Compound insecticide comprising imidacloprid and pymetrozine |
| CN103918701A (en) * | 2014-04-25 | 2014-07-16 | 中国计量学院 | Preparation method of Nadiwen-imidacloprid mixed formula preparation |
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| CN102599165A (en) * | 2012-02-21 | 2012-07-25 | 广东中迅农科股份有限公司 | Azoxystrobin microcapsule suspending agent and preparation method thereof |
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| CN103651505A (en) * | 2013-12-04 | 2014-03-26 | 南京农业大学 | Compound insecticide comprising imidacloprid and pymetrozine |
| CN103918701A (en) * | 2014-04-25 | 2014-07-16 | 中国计量学院 | Preparation method of Nadiwen-imidacloprid mixed formula preparation |
| CN103918701B (en) * | 2014-04-25 | 2016-03-09 | 中国计量学院 | A kind of taking is opposed surely and the preparation method of Imidacloprid mixing formula preparation |
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Application publication date: 20120215 |