CN101627754B - Mixed solid preparation of chloropicrin and 1.3-dichloropropylene and manufacturing technology thereof - Google Patents

Mixed solid preparation of chloropicrin and 1.3-dichloropropylene and manufacturing technology thereof Download PDF

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CN101627754B
CN101627754B CN2009101627495A CN200910162749A CN101627754B CN 101627754 B CN101627754 B CN 101627754B CN 2009101627495 A CN2009101627495 A CN 2009101627495A CN 200910162749 A CN200910162749 A CN 200910162749A CN 101627754 B CN101627754 B CN 101627754B
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dichloropropylene
chloropicrin
solid preparation
technical material
mixed solid
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CN101627754A (en
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韩景良
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Han Jingliang
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Abstract

The invention relates to a method for compounding technical material liquid of chloropicrin and 1.3-dichloropropylene and manufacturing a solid preparation and a use method. The method for compounding technical material liquid of chloropicrin and 1.3-dichloropropylene and manufacturing a solid preparation comprises the following steps: compounding the technical material liquid of the chloropicrin and the 1.3-dichloropropylene with a certain weight percentage; heating and vaporizing; vaporizing and absorbing by using active carbon and other adsorbents, and preparing the required compound mixed solid preparation according to the required content of technical material. The mixed solid preparation is used for soil fumigation and pest control and can adopt various methods such as hole application, furrow application, broadcast seeder overturning and the like.

Description

Solids mixing formulation and the manufacturing technology thereof of chloropicrin and 1.3---dichloropropylene
Technical field
The present invention relates to a kind of formulation of insecticide, soil fumigant, concrete for to contain 1.3---a kind of formulation of dichloropropylene and chloropicrin.
Technical background
1.3--dichloropropylene, English name: 1.3--1,3-dichloropropene; 1,3-dichloropropylene, international numbering: 33528 CAS:542-75-6, another name: 1.3---D or 3---Chloroallyl chlorine, molecular formula: C3H4Cl2; ClCH=CHCH2Cl.Molecular weight: 111.00, fusing point-84 ℃, boiling point: 112 ℃ (cis), 104 ℃ (trans), relative density 1.2170 (suitable), 1.2240 (instead), gas density 3.8g/L (20 ℃).Be colourless volatile liquid, the smell like chloroform is arranged.Risk markings: 7 (flammable liquids), agricultural, as soil fumigant, preservative, is mixed and is made soil fumigant with dichloropropane.Fungi and soil insect there is certain control efficiency.
Chloropicrin, chemical name are trichloronitromethane, international name: chloropicrin, and its mp-64 ℃, bp112.4 ℃, d204 1.656, and is water-soluble hardly, is dissolved in ether, acetone and other organic solvent.Since 1908 as insecticide (BP2387). because chloropicrin is volatile, stable chemical nature, noresidue is used for grain fumigating, soil-fumigating desinsection for many years always, and soil disinfection, stiflingly kill mouse, the aspects such as timber and medicinal material fumigant insect killing.
Above-mentioned two kinds of chemicals, there are many problems in agriculture application practice proof.As 1.3---dichloropropylene, ground temperature be lower than 15 ℃, and more than the processing time needed for three weeks, weather was than cold district mostly, easily farming season and can't using by mistake., because underground water is had pollution,, U.S. law regulation 1.3---dichloropropylene need to have certain buffer zone with the population residence, adopt the chemigation method to need the 30.5m buffer strip in addition; Be 91.5m and adopt the injection buffer strip.And only better to the nematode effect, general to the fungi effect.Chloropicrin is used for soil-fumigating, and action need band breathing mask and special syringe, also need overlay film after dispenser, needs certain sealing BHT, and very loaded down with trivial details, control efficiency is better to fungi, and anti-nematode is general.So have chloropicrin liquid and 1.3 on market---dichloropropylene liquid mix formulation.As commodity sellings such as Telonec-17 (if 78.3%1.3--dichloropropylene+16.5 chlorinations) and Telonec-35 (61.8%1.3---dichloropropylene+35 chloropicrins).Such intermixture, although after mixing, but expanding prevention is composed, and owing to being all volatile liquid, dosage is very large.---1.3 dichloropropylene (92%) content mu formulation rate needs 18---24kg, chloropicrin (98%) content mu formulation rate needs 30kg, and utilization ratio of drug is extremely low.Enter in a large number atmosphere during the loose gas of the toxic gas that can't decompose, not only waste medicine and strengthen the dispenser expense, and to environment, caused severe contamination.Therefore, chloropicrin and 1.3---the former medicine of dichloropropylene uses not only dangerous but also uneconomical.
Summary of the invention
Shortcoming for above-mentioned existing product exists the purpose of this invention is to provide a kind of chloropicrin and 1.3---the mixing formulation of dichloropropylene, improve its safety in utilization, improve simultaneously utilization ratio of drug, with its reach drug effect better, wider purpose.
Basic point of the present invention is to make chloropicrin and 1.3---the former medicine of dichloropropylene is adsorbed on a kind of nonhazardous, pollution-free solid absorbent, and when this solid dosage forms is used, the slow release medicine of energy, extend drug effect, and its concrete technical scheme is;
1, adsorbent is adsorbed front activation, then dry, seal stand-by.
2, will fill chloropicrin and 1.3---the mixed vapour of the certain ratio of dichloropropylene passes in above-mentioned adsorbent, till reaching requirement to the adsorbent increment.
The adsorbent that 3, will adsorb mist, make its quality even through mixing, packaging closures.
Wherein, adsorbent is one or both compositions of mixtures such as active carbon, atlapulgite, activated alumina, polymeric adsorbent, have after activation certain adsorbing capacity all can, take active carbon as best, especially with 0.1---1.0mm is the most suitable.Can separately use equipment during the adsorbent activation,, as activation pot or post activation, also can activate in adsorption tanks, just can do absorption after drying, use.Can carry out at normal temperatures and pressures during absorption, but adsorption rate is slow, if adsorption tanks negative pressure slightly, during the mixed liquor constant-temperature evaporation, adsorption rate can be hurry up; The evaporation if mixed liquor is heated, adsorption rate can be faster.Mode with absorption heating evaporation under normal temperature and pressure is more suitable.Absorption is wanted the phase coadaptation with evaporation, should accelerate adsorption rate, and non-vaporising does not adsorb too soon and makes mist effusion again, thus while evaporating temperature with 70 ℃---boiling point is advisable.This 1.3---the hybrid solid formulation of dichloropropylene and chloropicrin is with the different different contents that form of both proportionings, and 1: 2 to 5: otherwise 5 or, total content is with 20---30% for well.Product, take plastic bottle as basic packing, is opened bottle cap and is taken during use, little pungent is only arranged, and need not breathing mask.Product is imbedded soil layer 15 in actual use---and after 20cm, available gas ground temperature, starting release more than 10 ℃, is accelerated with Rise of Geotemperature later gradually, and last desorption is closely zero.Equally with former drug effect fruit kill soil insect and germ, its control is composed wider, and residual effect can reach more than 6 months.Utilization ratio of drug greatly improves, safety, economy, the effect that plays cover crop that can be more effective, more lasting.
Compare with existing product, the characteristics that the present invention has are;
1, product is solid dosage forms, uses with the safety of fortune storage outstanding the raising arranged.Under in order to be effective prerequisite, easy to use, purposes wide,, cost decrease few with former dose, sustained release and the drug effect phase long, be so far unique 1.3---the hybrid solid formulation of dichloropropylene and chloropicrin.
2, make this formulation with absorption method, show an interesting new approach, technique is reasonable, and method is easy, and three-waste free discharge, and environment is not had any impact.
Embodiment
Embodiment 1 granular activated carbon absorption 1.3---dichloropropylene and chloropicrin test
The granular activated carbon 16g that packs into activated and dry in the glass adsorption tower, suitable for reading is the tail gas exhaust outlet, connects the adsorption tanks of in-built active carbon.End opening is blow vent, and mixing material (1.3---the former medicine of dichloropropylene and the former medicine of chloropicrin) is installed, and heating evaporation is gas, is heated to 70 ℃---boiling point, stop ventilation after 3 hours, and take out absorption activated carbon, weightening finish 4g weighs.Tail gas is surveyed and is existed without chloride.
Embodiment 2 atlapulgite absorption 1.3---dichloropropylene and chloropicrin test
Device is as example 1, and the carclazyte particle of packing into activated, dried in adsorption tower, particle diameter are 0.5mm particle 200g, absorption 1.3---dichloropropylene and chloropicrin mist 40g.
Embodiment 3 activated alumina absorption 1.3---dichloropropylene and chloropicrin test
The particle that the particle diameter of packing in adsorption tower is 0.35---0.84mm activated alumina (sieve and get 20---between No. 45 standard screens) 100g, mixture is heated to 70 ℃~boiling point, stopped the supple of gas or steam in 4 hours, absorption weightening finish weightening finish 40% in 20%, 6 hour.
Embodiment 4 1.3---the drug effect of dichloropropylene and chloropicrin solid dosage forms (1: 3)
By to the tomato in plastic greenhouse test of pesticide effectiveness, every strain 3g that spreads manuer in holes, every square metre approximately 25---30g, observed in 150 days, well developed root system, disease-free generation, control efficiency is more than 98%.

Claims (1)

1. one kind with chloropicrin liquid and the composite solid dosage forms of 1.3-dichloropropylene liquid, it is characterized in that preparing by the following method: the granular activated carbon 16g that packs into activated and dry in the glass adsorption tower, suitable for reading is the tail gas exhaust outlet, connects the adsorption tanks of in-built active carbon, and end opening is blow vent, the mixing material of the former medicine of 1.3-dichloropropylene and the former medicine of chloropicrin is installed, heating evaporation is gas, is heated to 70 ℃ ~ boiling point, and 3 as a child stopped ventilation, take out absorption activated carbon, weightening finish 4g weighs; Tail gas is surveyed and is existed without chloride.
CN2009101627495A 2009-08-13 2009-08-13 Mixed solid preparation of chloropicrin and 1.3-dichloropropylene and manufacturing technology thereof Active CN101627754B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101878767A (en) * 2010-07-18 2010-11-10 齐冰 Mixture for soil disinfection and weeding
CN101971835A (en) * 2010-09-26 2011-02-16 韩景良 Soil particle fumigant
CN103109802A (en) * 2013-02-26 2013-05-22 韩景良 Preparation method and application of 1,3-dichloropropene solid slow-release preparation
WO2018222785A1 (en) 2017-06-01 2018-12-06 Regents Of The University Of California Calcium l-lactate frameworks as naturally degradable carriers

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