CN1415202A - Solid dosage forms of chloropicrin and its preparation - Google Patents

Solid dosage forms of chloropicrin and its preparation Download PDF

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Publication number
CN1415202A
CN1415202A CN 02131752 CN02131752A CN1415202A CN 1415202 A CN1415202 A CN 1415202A CN 02131752 CN02131752 CN 02131752 CN 02131752 A CN02131752 A CN 02131752A CN 1415202 A CN1415202 A CN 1415202A
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chloropicrin
formulation
adsorbent
active carbon
solid dosage
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CN1211013C (en
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韩景良
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Zhu Longyou
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Abstract

A slowly-released solid chloropicrin for wood, grains, medicine, etc features that the one or two of activated carbon, diatomite, argil and aluminium oxide are used as adsorbent. It is prepared through activating, drying and adsorbing the vapour of chloropicrin. Its advantages are high insecticiding and bactericiding effect, high utilization rate, and and no odour.

Description

The solid dosage forms of chloropicrin and method for making thereof
Technical field
The present invention relates to insecticide, a kind of formulation of soil disinfectant, concrete is a kind of formulation that contains trichloronitromethane.
Background technology
The international name of chloropicrin (chemical name is a trichloronitromethane) Chloropicrin, its mp-64 ℃, bp112.4 ℃, d 20 41.656, water-soluble hardly, be dissolved in ether, acetone and other organic solvent.Be used as insecticide (BP 2387) since 1908.Because chloropicrin is volatile, chemical property is stable, and noresidue is widely used in for many years that silo is stifling, the soil-fumigating desinsection, and soil disinfection, stiflingly kill mouse, aspects such as timber and medicinal material fumigant insect killing, its effect is remarkable.Even to this day chloropicrin is still one of principal item of this respect medication.Chloropicrin uses former medicine mostly, and storage is stifling to be to hang bag (or curtain), sprays chloropicrin thereon, the smoked 50~72h in sealing warehouse, and soil-fumigating then is with special syringe chloropicrin to be injected soil, then with plastic foil lining, blinding.In addition, can also with iodomethane, Ethide, or ethylene dibromide is made into mix preparation and uses.Because chloropicrin has strong and stimulating (to mucous membrane), chloropicrin commonly used joins conduct caution agent in other fumigant, leaks as fumigant, and people can (0.075mg/L) find and can in time handle in the presence of Trace Chloropicrin, in addition, also have and chloropicrin is mixed with emulsion uses.In fact, chloropicrin is except stoste, on commodity market, still do not have fixing formulation, the soil fumigant commodity (CHARLES.R.WORTHING etc. " THE PESTICIDE MANUAL " Published by The British Crop Protection Council 1983) that constitute by chloropicrin, 1.2-dichloropropane and 1.3-dichloropropylene of Di-Trapex by name only occurred.
Because chloropicrin belongs to high malicious chemicals (30min gets final product the causing death under the 0.8mg/L), both made is in open building, there is 1 chloropicrin to fall on the ground, people will tear near it, tears flow together and try to be the first and leave away, so the user often need be loaded with breathing mask and other safety devices, and the former medicine highly volatile of chloropicrin in addition, utilization ratio of drug is very low during use, particularly the soil-fumigating availability only is about 10%, and other parts have vapored away, so the former medicine of chloropicrin uses not only dangerous but also uneconomical.
Except that the above document of quoting, also quote following document:
H. Martin " version P311 in 1979 of pesticide species handbook Chemical Industry Press.
The long time refined son of Lang Shanglu " up-to-date agricultural chemicals デ- Block ヅ Network " the SOFT SCIENCEINC of Fu Chi, TOKYO, JAPAN nineteen eighty-two P50~51.
Summary of the invention
At the shortcoming that above-mentioned existing product exists, the object of the invention provides a kind of novel form of chloropicrin, improves its safety in utilization, improves the availability of medicine when using simultaneously.
Basic point of the present invention is that chloropicrin is adsorbed on a kind of nonhazardous, the pollution-free solid absorbent, and this solid absorption formulation can slowly discharge chloropicrin when using, prolong its residual effect, and its concrete technical scheme is:
(1) adsorbent is adsorbed preceding activation, then dry, seal stand-by;
(2) chloropicrin steam will be housed and feed in the above-mentioned adsorbent, reach requirement to adsorbent weightening finish till;
(3) adsorbent that will adsorb chloropicrin makes its quality homogeneous through mixing, package encapsulation.Wherein adsorbent is that one or both mixtures are formed in active carbon, diatomite, carclazyte, the aluminium oxide etc., have after the activation certain adsorbing capacity all can, be best with the active carbon; Adsorbent can be a powdery, can be granular, also can grain, powder mix to use, and is for well, the most suitable with 0.1~1.0mm especially with granular.These adsorbents carrier as chemical catalyst commonly used, activation method all is a conventional method.Can use other activation equipment during activation, as activation pot or post activation, then in the high temperature furnace drying; Also can in tourie, activate, just can adsorb usefulness after activation, the drying,, influence the adsorbing capacity of chloropicrin in order to avoid adsorb other gas (vapour).During absorption, can adsorb under normal temperature, normal pressure, but adsorption rate is slower, if be with negative pressure (i.e. decompression) in the adsorption tanks slightly, during the chloropicrin constant-temperature evaporation, adsorption rate can be soon; If the chloropicrin heating evaporation, normal temperature and pressure absorption down, then adsorption rate is faster; If adsorption tanks are with negative pressure slightly, the chloropicrin heating evaporation, then adsorption rate can be faster, and the mode of adsorbing heating evaporation with normal temperature and pressure down is more suitable.Chloropicrin is volatile, and the vapour pressure under the different temperatures is: 5.7mmHg/0 ℃, and 18.3mmHg/20 ℃, 23.8mmHg/25 ℃, 80.8mmHg/30 ℃.Absorption is wanted coadaptation mutually with evaporation, should accelerate adsorption rate, and non-vaporising adsorb and the chloropicrin effusion too soon again, so temperature is advisable with 80~boiling point when evaporating.The solid dosage forms of this chloropicrin contains chloropicrin 5~40%, with 20~30% for well.Chloropicrin solid dosage forms product is to pack substantially with the two layers of plastic bag, does not have the pungent taste of chloropicrin, during use plastic sack is cut off, and little pungent is only arranged, and can be with breathing mask.Begin to discharge chloropicrin at 10 ℃, imbed soil layer 20cm in actual use after, chloropicrin can discharge gradually, equally with former drug effect fruit kills all soil insects and germ, and residual effect can reach 15-30 days.Utilization ratio of drug greatly improves, medication 45g/m during the chloropicrin soil treatment 2And chloropicrin solid dosage forms of the present invention is only used 5-20g/m 2Just reach effect same.The adsorbent that the present invention selects for use does not produce pollution, particularly active carbon to soil and heat effect in addition in soil.Equally, this product can be used all occasions that are suitable for chloropicrin, and is equally effective.And safety, much economic.
The characteristics that had with existing product comparison the present invention are:
(1) product is that the transportation of solid dosage forms and safety in utilization have had outstanding raising, and is under in order to be effective preceding topic, easy to use, consumption is low, cost reduces significantly, drug slow discharges and residual effect is long; This is unique so far chloropicrin solid dosage forms.
(2) make this formulation with the method for absorption and show an interesting new approach, technology is reasonable, and method is easy, and three-waste free discharge, and environment is not had any impact.
Embodiment embodiment 1, the test of powdered activated carbon absorption chloropicrin
Pack in the glass absorption tower through steam activation and dry powdered activated carbon 20g,, be sandwiched in from level to level therebetween with handling clean small porcelain ring for ease of logical vapour, suitable for reading is the tail gas exhaust outlet, connect 4% sodium nitrate ethanolic solution, end opening is a blow vent, and chloropicrin heating evaporation gas is installed.Chloropicrin is heated to 80~boiling point, stops ventilation behind the 2h, and the active carbon of taking-up absorption is crossed and screened out the porcelain ring, active carbon weightening finish 3g, and solution detects no chloride existence in the tail gas absorption bottle.Example 2, the diatomite adsorption chloropicrin
Device is as example 1, and the activated and dry particle diameter of packing in the absorption tower is about the diatomite granule 20g of 0.5mm, absorption chloropicrin 2g.Example 3, granular active carbon absorption chloropicrin
The particle diameter of packing in the absorption tower be the activated carbon grain of 0.35~0.84mm (sieve get No. 20 and No. 45 standard screens between particle) 100g, chloropicrin is heated to 80~boiling point, 5h absorbs weightening finish 20%, 12h weightening finish 40%.The drug effect of example 4 chloropicrin solid dosage formss
(1) test tank, area 10m 2, the thick 20cm of soil layer sneaks into mole cricket, cutworm, nematode (band host peanut, soybean root) and unknown small worm are some, and earthworm several.With the granular active carbon formulation of 25% chloropicrin, with 15g chloropicrin/m 2Amount is imbedded in the soil, and the survey of digging in 7 days sees that worm is all dead, connects earthworm and fails to escape by luck.In soil, place insect behind the first quarter moon again, also dead clean after 7 days.
(2) warehouse is stifling.Grain depot is stacked in the gunnysack loading, by every cubic metre of dispensing 15g (solid chloropicrin formulation), the two layers of plastic bag that is packaged as 500g is pricked plurality of holes, places grain buttress upper, middle and lower and gunnysack parlor.Sealing (shut with adhesive tape entirely in door, window and gas leakage place, in order to avoid the gas leakage poor effect), 15~25 ℃ of room temperatures, open after three days warehouse gate, window, insect completely without.Past this storehouse former medicine of chloropicrin, 35~70g/m 2, pull rope in the storehouse and completely hang the piece of sack, essential breathing mask and the rubber gloves of carrying of people, and protective garment, very inconvenient, obtain effect same.
(3) control booth eggplant test
Plant the eggplant plastic tunnel for many years, verticillium wilt has every year, and the dawn increases the weight of in recent years, and every kind of practice ground is 666.7m 2
Medicine variety and consumption: 66.7% chloropicrin emulsion, 9kg; 25% chloropicrin solid dosage forms 3kg; 250 times of liquid 20kg of 25% carbendazol wettable powder; Irradiation is watered; All in the field planting ditch, sealing booth 10 days, after open the canopy primitive groove and break ground, sat the water field planting in 7 days, its result is as follows:
Handle medicine diseased plant rate % relative control effect %
Chloropicrin emulsion 17.83 90.34
Chloropicrin solid dosage forms 17.50 790
Carbendazim 56.31 71.02
Blank 86.55

Claims (6)

1, a kind of formulation of chloropicrin is characterized in that containing the solid absorption formulation of 5~40% chloropicrins, is that the adsorbents adsorb chloropicrin by activation forms; Adsorbent is a powdery or/and in the granular active carbon, diatomite, carclazyte, aluminium oxide one or both.
2, chloropicrin formulation according to claim 1, it is characterized in that described chloropicrin adsorbent type be contain 20~30% chloropicrins, adsorbent is the formulation of active carbon.
3,, it is characterized in that its particle diameter of described active carbon is the granular active carbon of 0.1~1.0mm according to the formulation of the described chloropicrin of claim 2.
4, a kind of method for making of chloropicrin formulation, the method that it is characterized in that the adsorbents adsorb chloropicrin, its technology is with one or both are activated, dry in activated carbon of sorbent, diatomite, carclazyte, the aluminium oxide, the steam of chloropicrin is fed adsorb, and treats that adsorbent weightening finish 5~40% forms.
5, the method for making of chloropicrin formulation according to claim 4 is characterized in that described chloropicrin steam is the steam that chloropicrin generates through heating evaporation.
6, the method for making of chloropicrin formulation according to claim 5, temperature is 80~boiling point when it is characterized in that the evaporation of described chloropicrin.
CN 02131752 2002-09-16 2002-09-16 Solid dosage forms of chloropicrin and its preparation Expired - Fee Related CN1211013C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 02131752 CN1211013C (en) 2002-09-16 2002-09-16 Solid dosage forms of chloropicrin and its preparation

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Application Number Priority Date Filing Date Title
CN 02131752 CN1211013C (en) 2002-09-16 2002-09-16 Solid dosage forms of chloropicrin and its preparation

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CN1415202A true CN1415202A (en) 2003-05-07
CN1211013C CN1211013C (en) 2005-07-20

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1714553A3 (en) * 2005-04-20 2010-09-29 Giuseppe Dr. Votta System and plant for producing hard granules holding absorbed gaseous chloropicrin
CN107509725A (en) * 2017-08-18 2017-12-26 朱龙友 A kind of production method containing the solid agent of sustained release highly effective pesticide and manufacturing equipment and the solid agent of compounding

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1714553A3 (en) * 2005-04-20 2010-09-29 Giuseppe Dr. Votta System and plant for producing hard granules holding absorbed gaseous chloropicrin
CN107509725A (en) * 2017-08-18 2017-12-26 朱龙友 A kind of production method containing the solid agent of sustained release highly effective pesticide and manufacturing equipment and the solid agent of compounding

Also Published As

Publication number Publication date
CN1211013C (en) 2005-07-20

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Address after: Liaoning province Yingkou Xiongyue town Yingkou Xiongyue acid pump limited liability company

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