CN1436460A - Safe procymidone smoke agent - Google Patents

Safe procymidone smoke agent Download PDF

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Publication number
CN1436460A
CN1436460A CN 03104632 CN03104632A CN1436460A CN 1436460 A CN1436460 A CN 1436460A CN 03104632 CN03104632 CN 03104632 CN 03104632 A CN03104632 A CN 03104632A CN 1436460 A CN1436460 A CN 1436460A
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Prior art keywords
fumicants
test
fuel
adjuvant
safe
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CN1244274C (en
Inventor
张友军
剧正理
徐宝云
吴青君
朱国仁
钱洪
姜辉
吴志凤
王晓军
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Institute of Vegetables and Flowers Chinese Academy of Agricultural Sciences
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Institute of Vegetables and Flowers Chinese Academy of Agricultural Sciences
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Abstract

The safe procymidone smoke agent consists of procymidone, combustion assistant and fuel in the ratio of 12-20 to 22-25 to 35-40. The combustion assistant is one or several selected from ammonium nitrate, potassium nitrate, sodium nitrate, potassium perchlorate and potassium permanganate; and the fuel is one or several selected from corn cob, cow, dung powder, straw and bagasse. It is bagged and thus is safe without spontaneous combustion; and it has simple production process and equipment and less environmental pollution.

Description

Safety-type SP 751011 fumicants
Technical field:
The present invention relates to a kind of novel agrochemical fumicants, specifically is chemistry security type SP 751011 safety fumicants.
Background technology:
China has protected ground vegetables area to increase sharply since the eighties, and various diseases are being on the rise of gray mold especially.SP 751011 has the better prevention effect to multiple diseases such as eliminating vegetable botrytis, stalk breaks.But this medicine is used the spray-on processes that adopt more in protection ground, and labour intensity is big, influence the dispenser personnel health, and spraying can the increase indoor humidity, and spreading to disease provides the control environment condition.
Fumicants is a kind of pesticides new formulation that is used to prevent and treat protection ground disease.Prevent and treat crop pest with fumicants and do not need any medical instruments, therefore not only the saving of labor, save time, economize medicine but also alleviated labour intensity; Not only improve control efficiency, can guarantee operating personnel's the dispenser safety and the pollution of minimizing environment again.Because fumigation can not increase indoor humidity, spreads to disease and causes hostile environment.
How fuel in the fumicants of prior art derive from the material of timber with wood powder, charcoal etc.Protect trees owing to all advocate in the worldwide at present, reduce and use timber, not only price is higher to use this fuel, also is unfavorable for environmental protection.
The stronger oxidant of many uses in the fumicants of prior art, the fumicants packaged by plastic film is used the work durm external packing again, perhaps uses card board package.Make the lead-in wire point with spill, need plug spill earlier during use, refire etc., use inconvenience, and very easy generation " spontaneous combustion " accident on fire.According to ground incomplete statistics such as Beijing, Henan, fumicants spontaneous combustion accident on fire only just takes place in the period of the 1984-1986 seven times more than, wherein have three times and lead to bigger economic loss, brought great difficulty and obstacle for like this production, storing and the application of fumicants.In addition, fumicants is problem such as easy moisture absorption when preserving summer, has seriously influenced effective use of fumicants.
Summary of the invention:
The packing that is difficult for when one of the technical problem to be solved in the present invention provides a kind of production, storage, use that the on fire and nonhygroscopic SP 751011 safety fumicants of spontaneous combustion takes place and above-mentioned fumicants is provided; Another technical problem that the present invention will solve is that the fuel in the fumicants does not use the timber source, to reduce cost the protection environment.
The prescription of SP 751011 fumicants provided by the invention is (weight portion):
SP 751011: combustion adjuvant: fuel=12~20: 22~25: 35~40
Described combustion adjuvant is selected from ammonium nitrate, potassium nitrate, sodium nitrate, potassium perchlorate, the potassium permanganate one or more;
Described fuel is selected from corncob, cow dung end, stalk, the bagasse one or more, uses after making powdery.
Can also include other filler in the prescription of SP 751011 fumicants provided by the invention as adjuvant, adjuvant is selected from inert substances such as land plaster, bentonite, diatomite, bentonite.Its amount ratio is (weight portion):
SP 751011: combustion adjuvant: fuel: adjuvant=12~20: 22~25: 35~40: 2~6
SP 751011 fumicants provided by the invention is a powdery, and external packing is a bag type package, and product is used paper bag packing earlier, wraps up with polyethylene film again.Also can directly wrap up with polyethylene film.Using method is to need not to remove unlap, need not twist with the fingers, and naked light is directly lighted packaging bag and got final product for one jiao.
The technological process of above-mentioned SP 751011 fumicants is: screening-pulverizing-oven dry-mixing-packing, adopt moistureproof, anti-spontaneous combustion measure in the production process.The concrete operations step is:
1, sieve respectively and handle various raw materials, remove wherein foreign material, iron content foreign material especially, in case metal object is brought into, it is on fire to avoid iron and pulverizing, mixing apparatus to bump;
2, various raw materials are pulverized separately, collision is on fire when avoiding different auxiliary agents to pulverize together;
3, the raw material of above-mentioned pulverizing are dried,, avoid moisture absorption caking to remove moisture;
4, after being measured respectively, various raw materials mix;
5, the examination and test of products;
6, product is packed into paper bag reinstalls the polyethylene film packaging bag, seals.
SP 751011 fumicants to the present invention's development has carried out following detection and test:
1, SP 751011 fumicants toxicity detects
1) acute toxic test result: enclose labour health protection research institute of the preventive medicine academy of sciences in the warp and measure, the SP 751011 fumicants is to suck median lethal dose LD to big white mouse per os acute toxic test result 50>2000 milligrams/cubic metre, belong to low-toxin farm chemicals.
2) determination of residual amount in cucumber: detect through Beijing City Agriculture and Forestry Institute plant protection environmental protection, meeting SP 751011 maximum magnitude (MRL) is the standard of 2 mg/kg.
2, the safety of SP 751011 fumicants detects
1) safety determination test: through Beijing Institute of Technology's department of chemistry engineering according to military standard and civil standards, fumicants impact sensitivity test, 50 ℃ of heat stabilization tests in 14 days, 80 ℃ of 48 hours heat runs, differential thermal decomposition run and self-ignition point testing experiment etc. below 500 ℃ have been carried out, measurement result is the safety-type fumicants, and every index meets safety standards.
3, SP 751011 fumicants storage test
Carried out 54 ± 2 ℃ of two all heat stabilization test of fumicants and summer storage test more, proved that fumicants preserves in warehouse or simple and easy storehouse, under the environmental condition of summer high temperature, can the moisture absorption, be safe.
4, humidity resistance experimental study: result of the test shows that fumicants under high temperature (34 ± 0.5 ℃), high humidity (90 ± 2%) condition, has good humidity resistance.
5, SP 751011 fumicants field control effectiveness test:
The result shows that this fumicants has good control efficiency to protection ground vegetables gray mold of cucumber, graw mold of tomato etc., and its field efficacy can reach more than 80%.
The present invention's beneficial effect against existing technologies is:
Safety is good, in preparation, storing and the process used, and can spontaneous combustion;
Fuel used is corncob, cow dung end, stalk, bagasse etc. from agricultural production by product and offcuts, and cost is low, saves timber, is beneficial to environmental protection;
Used auxiliary material is land plaster, kaolin, bentonite, diatomite, and wide material sources get final product with industrial crude product, and are cheap;
Pack simplely, with low cost, insulation product contacts with outside moisture effectively;
Easy to use, to the dispenser personal security;
Production equipment is uncomplicated, and is simple for process, reduces environmental pollution.
Embodiment:
Embodiment 1
Prescription (weight portion): 20 parts of SP 751011s, 22 parts in ammonium nitrate, 40 parts of corncobs, 6 parts in diatomite
Preparation technology:
1, every kind of raw material is sieved respectively, remove wherein foreign material;
2, adopt comminution by gas stream and supporting mixing apparatus, respectively various raw materials are pulverized;
3, in the special fireproof drying room, the raw material of pulverizing are dried, to removing moisture;
4, various raw materials are measured respectively after, put into efficient mixer and mix;
5, product is through after the assay was approved, and the paper bag of packing into reinstalls the polyethylene film packaging bag, seals.
Embodiment 2
Prescription (weight portion): 12 parts of SP 751011s, 25 parts in potassium nitrate, 35 parts of corncobs, 2 parts of land plasters
Preparation technology is with embodiment 1.
Embodiment 3
Prescription (weight portion): 15 parts of SP 751011s, 10 parts in ammonium nitrate, 12 parts in potassium nitrate, 20 parts at cow dung end, 20 parts of bagasse, 3 parts of bentonites
Preparation technology is with embodiment 1.
Embodiment 4
Prescription (weight portion): 15 parts of SP 751011s, 25 parts in ammonium nitrate, 40 parts of powder of straw
Preparation technology is with embodiment 1.
Embodiment 5 SP 751011 fumicants physical property test event measured results are lighted phenomenon and are once lighted with match, and dense smoke white has certain impulse force, in the process of being fuming, does not produce
Naked light and Mars ignition temperature (℃) 100g fumicants 385 12 minutes residue ember of (branch) 100g fumicants residue of being fuming the time is loose, adularescent powder slightly, do not occur in 30 minutes the ember autoignition temperature (℃) 218 ± 3 combustion rates *(%) 85.7 safety testings *80 ± 1 ℃ of not spontaneous combustions in 7 days.50 ± 1 ℃ of not spontaneous combustions in 90 days.Annotate: *Combustion rate deducts the ratio of ash content weight and fumicants weight after the burning for fumicants weight.
*Security test: the packed fumicants of 100 grams is put into CS101-A type Constant Temp. Oven and electro-heating standing-temperature cultivator (model HH.B11-600), under 80 ± 1 ℃ of situations, observed its dieseling in continuous 7 days; Under 50 ± 1 ℃ of situations, observed its dieseling in continuous 90 days.
Embodiment 6 SP 751011 fumicants stability determination test
Random sampling from SP 751011 fumicants trial product, every sample are got 100 grams and are put into 54 ± 2 ℃ of climatic chambers, and the heat storage was taken out after 14 days, the content of effective ingredient before and after storing with gas chromatograph for determination, and calculate resolution ratio.It the results are shown in following table:
Content (%) is store (%) SP 751011 fumicants 10.18 10.01 1.67 of back content (%) before stability test two weeks of fumicants (54 ± 2 ℃) the resolution ratio title storage as a result
Laboratory test results shows that fumicants of the present invention resolution ratio under 54 ± 2 ℃ of hot storage conditions is 1.67%, meets the FAO defined less than 5% standard.
Embodiment 7 SP 751011 fumicants water content and pH measure
The water content of fumicants is lighted difficulty or ease with fumicants, and it is dense white to be fuming, and impulse force and time length have substantial connection, if water content is too much, can't light, and have a strong impact on fumicants quality quality.
Testing instruments:
(1) azeotropic method hydro-tester.
(2) pH analyzer.
Method:
(1) mensuration of moisture: (azeotropic method)
Take by weighing sample 20g (claiming accurate) and put into flask, add 100ml benzene, connect flask and other device then to 0.01g.Be heated to and boil.Continue boiling and become clear (per second backflow 2-3 drips) until distillate.When the volume of water no longer increases to recipient, keep 10 minutes again after, stop the heating.With 50ml benzene flushing condenser, till not having the globule to fall, the cooling room temperature.
The percentage composition of the moisture in the sample (X) is calculated as follows. X = V × Pt × 100 m
V in the formula---water layer volume in the recipient, ml;
M---sample is heavy, g;
Pt---temperature correction value.
(2) mensuration of sample pH value value (pH meter method)
Sample thief 10g puts into the 50ml beaker, adds 50ml distilled water, fully mixes, leaves standstill, and after waiting to precipitate, the glass electrode of wash clean and saturated calomel electrode is inserted in the beaker measure.Pointer changed when being no more than 0.1pH in two minutes, must be somebody's turn to do number and be the pH value of sample.Assay:
Figure A0310463200081
As can be seen from the table, water content up to specification<3% standard.Fumicants light and be fuming respond well, the big dense impulse force that has in vain of cigarette amount.
Embodiment 8 SP 751011 fumicants physicochemical properties
Through a series of test, fumicants prescription of the present invention meets quality control index, is safe and reliable fumicants (seeing the following form).
SP 751011 fumicants quality index actual measurement project name control index prescription measured result is lighted phenomenon and is once lighted dense smoke white and have the impulse force flames of anger and Mars to produce qualified ignition temperature, (℃) 380 ± 20 385 be fuming the time, (branch) 6-12 12 autoignition temperatures, (℃)>130 218 ± 3 one-tenth cigarette rates, (%)>75 89.51 toxicity, (LD50Mg/m 3)>500>2000 fineness is by 40 orders, (%) 90 qualified residual quantities, (mg/kg)<2 0.2735 water content, (%)<3 2.054 ± 2 ℃ storing 14 days resolution ratio<5% 1.8950 ± 1 ℃ stores qualified 80 ± 1 ℃ of not spontaneous combustion in 90 days and stores the qualified pH value 6-9 6 of not spontaneous combustion in 7 days
Embodiment 9 SP 751011 fumicants become the mensuration of cigarette rate
(1) instrument
Become the cigarette device
Gas chromatograph: day island proper Tianjin GC-9A type electron capture detector;
(2) operating procedure
1) collection of effective ingredient in the cigarette
Take by weighing 0.2g (accurately to 0.0001g) fumicants of the present invention in bottle, place in the round-bottomed flask, add 20ml dimethylbenzene absorption liquid in each absorption tube, engaging means, be heated to burning fuming (220-240 ℃) with the control-temperature electric heating cover, stop heating after 1-2 minute, cooling back provision for disengagement, and remaining residue bottle taken out from flask (for measure in the residue effective component content with), absorption liquid moves in the 250ml volumetric flask, with same absorption liquid washing round-bottomed flask, tube connector, absorption tube, cleaning solution are incorporated in the same volumetric flask, are settled to scale and treat that further the dilution back is measured.
2) selecting for use with the SP 751011 fumicants sample determination effective component content (assay method is the same) that becomes the cigarette rate to test same lot number is contrast.
3) preparation of fumicants residue effective component content solution of the present invention
Fumicants is burnt into residual residue behind the cigarette, use the agent dissolves identical, the washing bottle with absorption liquid; Be filled in the volumetric flask, it is to be measured to be diluted to scale.
4) quantitative assay
With effective component content in the gas chromatography determination cigarette, chromatographic condition is as follows: gas chromatograph: day charged sub-acquisition detector chromatographic column of island proper Tianjin GC-9A type: column length 1.5m internal diameter 3mm glass column filler is 5%
Ov-101,190 ℃ of vaporizer temperature of Cas Chrom Q (80-100 order) column compartment temperature and 240 ℃ of carrier gas of assessor temperature: high purity nitrogen flow velocity 60ml/min external standard method is quantitative, and SP 751011 cigarette titer is prepared with diluting with benzinum after a small amount of xylene soluble.
5) calculate
Measurement result is calculated as follows under above-mentioned chromatographic run condition Cx = Hx · Cs · Qs · Vx Hs · W · QX · P
Agricultural chemicals percentage composition (%) in Cx-sample
The peak height of agricultural chemicals or peak area (mm or mm in Hx-sample 2)
The concentration of agricultural chemicals (mg/kg) in Cs-standard liquid
Qs-standard liquid sample size (microlitre)
Vx-sample constant volume (milliliter)
The peak height of agricultural chemicals or peak area (mm or mm in Hs-standard liquid 2)
W-sample claims sample weight (gram)
The sample size of QX-sample solution (microlitre)
The percentage composition of P-standard sample of pesticide (%)
(3) result and discussion
It is as shown in the table for measurement result, becomes cigarette rate and residual rate to calculate recently calculating with effective component content in effective component content and the fumicants in effective component content and the residue in the cigarette absorption liquid.
(1) fumicants of preparing by 50% SP 751011 wetting powder
Fumicants effective component content and the effective cigarette absorption liquid of one-tenth cigarette rate measurement result pesticide smoke by 50% SP 751011 WP preparation have into the effective residual rate title of cigarette rate residue component content effective constituent content component content
(%) (%) (%) (%) (%) fumicants 10.03 8.98 89.51 0.034 0.34 of the present invention
It is 89.51% that fumicants of the present invention as can be seen from the above table becomes the cigarette rate, greater than control criterion.
(2) fumicants of preparing by the former medicine of SP 751011
Effective component content and one-tenth cigarette rate measurement result fumicants title fumicants effective component content (%) become cigarette rate (%) SP 751011 fumicants 9.98 89.86
The former medicine of SP 751011 is provided by the Zhejiang Provincial Chemical Engineering Research Inst, is 89.02 through surveying former medicine content.
Can find out that from last table it is 89.86% that the SP 751011 fumicants becomes the cigarette rate, greater than the control index.
Embodiment 10 SP 751011 fumicants safety feature tests
1) SP 751011 fumicants self-ignition point test:
(1) method of testing: IEC method.
(2) result is: 218 ± 3 ℃ of fumicants of the present invention
2) SP 751011 fumicants Impact Sensitivity:
(1) test method: with the vertical instrument that drops hammer of WL-1 type, be 10 ± 0.02Kg weight, 250 ± 1mm drop height by military standard, the observation of bump SP 751011 fumicants has reactionless.
(2) result is: impact sensitivity is low, is safe insensitiveness medicament.
3) fumicants thermostability test of the present invention:
(1) test method: take by weighing three bags of the fumicants of 100 gram packings, put into 80 ℃ of incubators of constant temperature, heated continuously 48 hours, observing has no change.Use the same method, 50 ℃ of constant temperature heat 14 days observation fumicants continuously no change again.
(2) result is:
1. store under 48 hours situations the color of fumicants of the present invention, smell, the equal no change of weight and do not have decomposing phenomenon at 80 ℃.
2. store under 14 days the situation at 50 ℃, fumicants of the present invention does not have weightlessness, no color, odorlessness variation and do not have decomposing phenomenon.
4) fumicants friction sense of the present invention becomes test:
(1) test method: with MGY-1 type pendulum-type friction sensitivity instrument is that 90 pairs of fumicants of pivot angle carry out friction test, observes situation of change.
(2) result is: fumicants is misfired, and is pure sense medicament.
5) fumicants differential thermal analysis test of the present invention:
(1) test method:, measure suction, the heat release variation after the material of surveying is heated and endotherm peak temperature occurs with the differential thermal analyzer of CDR-1 type.
(2) result is: in the 0-500 ℃ of scope, the secondary endothermic peak appears in no exothermic peak, and it the results are shown in following table.
Fumicants differential thermal analysis of the present invention is 229.5 ℃ 348.5 ℃ of fumicants title first endothermic peak second endothermic peak fumicants of the present invention as a result
Embodiment 11 SP 751011 fumicants control gray mold of cucumber field control effectiveness test
One, reagent agent
1. fumicants of the present invention: the Chinese Academy of Agricultural Sciences's vegetable or flower provides
2.30% chlorothalonil smoke: farm, southern suburbs, Beijing fumicants processing factory
3.50% SP 751011 wetting powder: (commercially available, the import agricultural chemicals is the packing of Beijing means of production company)
Two, test greenhouse basic condition:
Experimental field be located in the greenhouse, farm, southern suburbs, Beijing.Arrange greenhouses for fumigation with 4, every row greenhouse is a processing, and cucumber variety is that Changchun is close perverse.The field is according to the Routine Management way.
Investigation method, every row greenhouse adopts 5 sampling methods, and the sick melon of every strain (bar) number is checked in every 10 strain totally 50 strains before the fumigation, and mark or excision.Carried out fumigation at dusk the same day, spraying was investigated emerging sick melon (bar) number in 10 days with manual 16 type knapsack sprayers after the dispenser, calculated control efficiency behind the medicine.
Three, result and analysis
Result of the test (for details see attached table) shows, the SP 751011 fumicants obviously is better than 1000 times of liquid of 50% SP 751011 wetting powder to gray mold of cucumber.This can be uniformly distributed in pesticide molecule each corner, protection ground mainly due to smog, and has reduced indoor humidity and suppressed the cause that germ spreads.Promote to demonstrate according to test and large-area applications, with every mu be 0.36 kilogram with the fumicants amount, prevent and treat more satisfactoryly, and crop safety do not had poisoning.
Front the sick melon of SP 751011 fumicants control gray mold of cucumber field control effectiveness test fumicants fumicants consumption medicine is counted behind the medicine ten days sick melon disease melon decline rate preventive effect titles kg/acre, (bar), (bar), (%), (%) 1000 times of 120 43 64.2 76.3 wettable powder contrast of fumicants 0.35 308 38 87.7 91.130% chlorothalonil smoke 0.35 250 48 80.8 87.350% SP 751011 of the present invention, (clear water)-49 74-51.0-

Claims (4)

1, SP 751011 fumicants, its prescription is (weight portion):
SP 751011: combustion adjuvant: fuel=12~20: 22~25: 35~40;
Described combustion adjuvant is selected from ammonium nitrate, potassium nitrate, sodium nitrate, potassium perchlorate, the potassium permanganate one or more;
Described fuel is selected from corncob, cow dung end, stalk, the bagasse one or more.
2, the described SP 751011 fumicants of claim 1 is characterized by and also contains adjuvant, fills a prescription to be (weight portion):
SP 751011: combustion adjuvant: fuel: adjuvant=12~20: 22~25: 35~40: 2~6;
Described adjuvant is selected from land plaster, bentonite, diatomite, bentonite.
3, claim 1 or 2 described SP 751011 fumicants is characterized by powdery.
4, claim 1 or 2 described SP 751011 fumicants, it is characterized by fumicants is bag type package, product wraps up with polyethylene film.
CN 03104632 2003-02-19 2003-02-19 Safe procymidone smoke agent Expired - Fee Related CN1244274C (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102986660A (en) * 2012-12-09 2013-03-27 大连创达技术交易市场有限公司 Preparation method of pesticide smoke agent
CN106879588A (en) * 2016-12-31 2017-06-23 新昌县云河虫害防治技术开发有限公司 Compound formulation and its application for booth vegetable pest control

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102986660A (en) * 2012-12-09 2013-03-27 大连创达技术交易市场有限公司 Preparation method of pesticide smoke agent
CN106879588A (en) * 2016-12-31 2017-06-23 新昌县云河虫害防治技术开发有限公司 Compound formulation and its application for booth vegetable pest control

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