CN102114382B - Method for separating and recovering fumigation medicine - Google Patents
Method for separating and recovering fumigation medicine Download PDFInfo
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- CN102114382B CN102114382B CN 201110008530 CN201110008530A CN102114382B CN 102114382 B CN102114382 B CN 102114382B CN 201110008530 CN201110008530 CN 201110008530 CN 201110008530 A CN201110008530 A CN 201110008530A CN 102114382 B CN102114382 B CN 102114382B
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Abstract
The invention provides a method for separating and recovering fumigation medicine, which belongs to the technical field of separation. The method is characterized in that the fumigation medicine is vaporized and then mixed with synergistic agent, then the mixture enters a fumigation chamber for fumigation, and mixed gas in the fumigation chamber is recovered after the fumigation is finished, wherein the recovery processing comprises the following steps that firstly, the mixed gas is in contact with absorbent for physical absorption, the fumigation medicine is absorbed, pregnant solution is collected, absorbed tail gas is then subjected to chemical absorption treatment; and secondly, pregnant solution that is collected in the first step is rectified, the fumigation medicine and the absorbent are separated, and the recycled fumigation medicine and recycled absorbent can be used indiscriminately. The method for separating and recovering the fumigation medicine has the advantages that theselectivity of the absorbent is high, the absorption efficiency is high, the fumigation medicine can be recovered to the utmost extent and can be used repeatedly, the environment pollution is low, and the continuous operation can be achieved.
Description
Technical field
The present invention relates to a kind of separation method, relate in particular to a kind of separation and recovery method of fumigation medicament, belong to separation technology field.
Background technology
Stifling processing refers to by means of fumigation medicament gas, technology or the method in certain hour and space that can be airtight, harmful organism killed.The method is present most widely used desinsection, disinfects one of technology, no matter is that the space is stifling, or soil disinfection, and all will consume a large amount of fumigation medicaments every year, and protection has great impact on economy and environment.
In prior art, stifling the processing adopted the fumigation medicaments such as Celfume, hydrogen phosphide, cyanogen, vikane, carbon disulfide mostly.And most widely used be to adopt the methyl bromide fumigation medicament, yet due to the destruction of Celfume to ozone layer, must progressively eliminate according to the requirement of Montreal protocol, and its result of use under cryogenic conditions also is very restricted.Although scientist or scholar are engaged in the R﹠D work of Celfume substitute for a long time, up to the present, also do not have a kind of substitute can replace Celfume fully both at home and abroad.Therefore, Celfume low dose applications or be recovered recyclingly to reduce the pollution to environment, becomes one of hot research problem of current international community.
In prior art, the recovery of fumigation medicament Celfume mainly contains following three kinds of methods: scheme one, and with porous material absorption methods such as active carbons.Model and the adsorption conditions according to active carbon, the adsorption rate of Celfume can reach 10%～30% content, and adsorption rate depends primarily on free amounts of activated carbon, and the rate of adsorption is relevant with Properties of Activated Carbon, adsorption temp etc., under low-down load, the rate of recovery can reach or near 100%.But the shortcoming of the method is after active carbon reaches the active limit, the processing of must regenerating, usual way is to carry out desorb with thermal current heat activated charcoal such as superheated steam, hot nitrogen or flue gases to process, or carries out 600 ℃～900 ℃ pyrolytics and process in special installation.Therefore be subjected to that security, solid waste are many, energy consumption reaches greatly the huge restriction of device systems and is unfavorable for suitability for industrialized production.
Scheme two adopts the condensation absorption method, and the method is applicable to gas recovery in the gas phase higher at boiling point, that concentration is higher, and for the too low fumigation medicament of concentration content in low boiling, gas phase, if very low refrigerant not, it recycles difficulty, limitation is large, is unfavorable for suitability for industrialized production.
Scheme three, the reactive fluid chemiadsorption, the method is with bases or amine liquid absorption fumigating gas, it is with obvious chemical reaction and generate the absorption process of novel compound.The shortcoming of the method is that absorption efficiency is low, and more difficult to the processing again that absorbs waste liquid.
Summary of the invention
The present invention is directed to the existing defective of prior art, proposed a kind of separation and recovery method of fumigation medicament, but the method absorption efficiency is high, can reclaim to greatest extent fumigation medicament and reusable, the few continued operation of environmental pollution.
Above-mentioned purpose of the present invention is to be achieved by the following technical programs: a kind of separation and recovery method of fumigation medicament, the method is to be mixed together with synergist after fumigation medicament vaporization, enter fumatorium and fumigate processing, after processing finishes, mist in fumatorium is recycled, it is characterized in that: described recycling comprises the following steps:
A, mist is contacted with absorbent carry out Physical Absorption, absorb fumigation medicament, collect rich solution, will absorb tail gas and carry out again the chemical absorbing processing;
B, the rich solution of collecting in step a is carried out rectifying, separate fumigation medicament and absorbent, the fumigation medicament of recovery and absorbent can be applied mechanically.
In the separation and recovery method of fumigation medicament of the present invention, fumigation medicament vaporization is after fumigation medicament is first fully vaporized through vaporizer, making is mixed with the form of gas and synergist enters fumatorium, and purpose is in order to prevent that fumigated thing is subject to the dissolved corrosion of liquid fumigation medicament; Above-mentioned synergist has synergy, can add according to actual needs or not add synergist.Generally, the additive capacity of synergist is for by volume between 5%～25%.Add synergist and be conducive to shorten fumigation time, improve the using dosage of insecticidal effect and minimizing fumigation medicament.Described stifling processing is to adopt existing common technology fumigated thing to be carried out the stifling processing procedure of desinsection, sterilization.Rich solution described in step a refers to the absorption liquid after absorbent absorbs a large amount of fumigation medicaments.
In the separation and recovery method of above-mentioned fumigation medicament, described fumigation medicament can be a kind of in Celfume, vikane, cyanogen, oxirane, chloropicrin, hydrogen phosphide, carbon disulfide, cyanogen, carbonyl sulfide, Ethyl formate, iodomethane.As preferably, described fumigation medicament is a kind of in Celfume, hydrogen phosphide, oxirane, further is preferably Celfume; Wherein said synergist can be carbon dioxide.
In the separation and recovery method of above-mentioned fumigation medicament, the absorbent described in step a is organic solvent; As preferably, described absorbent is one or more in benzene, dimethylbenzene, benzinum, halogenated hydrocarbons, low-molecular-weight alcohol, low-molecular-weight ether, low-molecular-weight ketone and low-molecular-weight ester solvent.Described low-molecular-weight alcohol, low-molecular-weight ether, low-molecular-weight ketone and low-molecular-weight ester solvent are C
1～C
10Alcohol, ether, ketone, esters solvent, described halogenated hydrocarbons is chloroform, trichloroethanes etc.Further preferred, described absorbent is one or more in benzene, chloroform, trichloroethanes, acetone, ethanol, ethyl acetate.Physical Absorption temperature described in step a is freezing point～90 ℃, and Physical Absorption pressure is normal pressure.As preferably, the Physical Absorption temperature described in step a is 5 ℃～50 ℃.
Although above-mentioned Physical Absorption process adopts pressurization or cooling method operation, is conducive to fumigation medicament and absorbs, and considers economic factor, adopts suitable temperature and pressure more to be conducive to suitability for industrialized production.After absorbing, the amount that contains fumigation medicament in the absorption tail gas gas of discharge reaches minimum.Reduce on the one hand the fumigation medicament loss, thereby also reduced environmental pollution, on the other hand, also reduced chemically treated difficulty.And the method operating process simple, be conducive to suitability for industrialized production.
Physical Absorption described in step a can adopt the absorption tower group to carry out Physical Absorption, and wherein the absorption tower group can be a kind of in tray absorption columns or material filling type absorption tower.It can be that multistage absorption tower group is as adopting first grade absorption tower, two-level absorption tower group.Utilize board-like or the material filling type absorption tower, compare with void tower, be conducive to increase the contact area of gas-liquid two-phase, thereby improve assimilation effect.And utilize multistage absorption tower group, can be absorbed more completely in order to make fumigation medicament.No matter adopt board-like or the material filling type absorption tower, still adopt the multistage absorption tower, its objective is for more effective absorption fumigation medicament, reduce environmental pollution.
Chemical treatment described in step a refers to absorb with absorbing the method for tail gas by chemical reaction, removing a small amount of fumigation medicament that is not completely absorbed in tail gas, absorbs as water.Perhaps adopt the method for chemical reaction, destroy fumigation medicament, make to generate nonvolatile material, then the tail gas after absorbing (being mainly the fumigant gas of air, synergy gas, minute quantity) discharge, thereby reduction is to the pollution of atmosphere, protection of the environment.
In the separation and recovery method of above-mentioned fumigation medicament, wherein the rectification temperature described in step b is reflux temperature, and described rectifying pressure is normal pressure.
Described rectifying is the difference according to the volatility between fumigation medicament and absorbent, by being warming up to backflow, circulating in rectifying column in the mode of interior backflow, and realizes the method that fumigation medicament separates with absorbent; The method operating process is simple, is conducive to suitability for industrialized production.
In sum, the present invention has the following advantages:
1, the separation and recovery method of fumigation medicament of the present invention absorbent used selective high, volatility is low, corrosivity is little, viscosity is low, absorption efficiency is high.
2, the separation and recovery method technique of fumigation medicament of the present invention is simple, but continued operation production is conducive to suitability for industrialized production.
3, the separation and recovery method of fumigation medicament of the present invention, separative efficiency is high, and the fumigation medicament of recovery and absorption can repeat to apply mechanically, and are conducive to environmental contamination reduction, reduce production costs.
Description of drawings
Fig. 1 is the process chart of the separation and recovery method of fumigation medicament of the present invention.
The specific embodiment
Below by specific embodiment, technical scheme of the present invention is described in further detail; But the present invention is not limited to these embodiment.
Embodiment 1
after the fumigation medicament Celfume is made vaporization fully through vaporizer, cushioning in-tank mixing with the synergist carbon dioxide again, wherein the addition of synergist carbon dioxide is volume ratio 10%, after fully mixing, pass in fumatorium fumigated thing is fumigated processing, after stifling processing finishes, mist in fumatorium is passed through the one-level tray absorption columns from the bottom, mist is with the superficial linear velocity in a column process tray absorption columns of 2cm/s～10cm/s, simultaneously, tower top spray-absorption agent chloroform from tray absorption columns, make the reverse contact of gas-liquid two-phase, absorb the fumigation medicament Celfume, whole absorption process, under normal pressure, controlling the absorption temperature is 5 ℃～15 ℃, carry out absorption operation, collect rich solution, and will absorb tail gas and pass into and carry out chemical absorbing in next absorption tower and process, destroy fumigation medicament, wherein chemical absorbing absorbent used is the amine liquid flux, make Celfume and amine liquid generation chemical reaction, make into the nonvolatile matter MB, thereby destruction Celfume, and final tail gas is after treatment drained into atmosphere.
the rich solution that the upper step was collected changes in rectifying column, be warming up to 60 ℃ and make backflow, under normal pressure, carry out rectifying, utilize the difference of volatility between Celfume and absorbent chloroform, by interior backflow, Celfume is separated with absorbent, being about to Celfume separates from the top of rectifying column, through after the drying device drying of tower top, pass through again compressor, pass through at last condensation liquefaction, be collected into pans, after rectifying finishes, the Celfume that recovery is good is packed in special cylinder, the Celfume that obtains can be reused, realize regeneration, the absorbent of separating can be applied mechanically again.
Embodiment 2
after the fumigation medicament Celfume is made vaporization fully through vaporizer, cushioning in-tank mixing with the synergist carbon dioxide again, wherein the addition of synergist carbon dioxide is volume ratio 15%, after fully mixing, pass in fumatorium fumigated thing is fumigated processing, after stifling processing finishes, mist in fumatorium is passed through secondary tray absorption columns group from the bottom, mist is with the superficial linear velocity in a column process tray absorption columns of 5cm/s～15cm/s, simultaneously, tower top spray-absorption agent dimethylbenzene from tray absorption columns, make the reverse contact of gas-liquid two-phase, absorb the fumigation medicament Celfume, whole absorption process, under normal pressure, controlling the absorption temperature is 25 ℃～35 ℃, carry out absorption operation, collect rich solution, and will absorb tail gas and pass into and carry out chemical absorbing in next absorption tower and process, chemical absorbing processing wherein is consistent with the method in embodiment 1, repeat no more.
The rich solution that the upper step was collected changes in rectifying column, be warming up to 110 ℃ of backflows, carry out rectifying, utilize the difference of volatility between Celfume and absorbent dimethylbenzene, by interior backflow, Celfume is separated with dimethylbenzene, be about to Celfume and separate from the top of rectifying column, through after the drying device drying of tower top, pass through again compressor, at last by condensation liquefaction, to pans, after rectifying finishes, the Celfume that recovery is good is packed in special cylinder, the Celfume that obtains can be reused, and realizes regeneration, and the absorbent of separating can be applied mechanically.
Embodiment 3
after the fumigation medicament Celfume is made vaporization fully through vaporizer, cushioning in-tank mixing with the synergist carbon dioxide again, wherein the addition of synergist carbon dioxide is volume ratio 10%, after fully mixing, pass in fumatorium fumigated thing is fumigated processing, after stifling processing finishes, mist in fumatorium is passed through one-level tray absorption columns group from the bottom, mist is with the superficial linear velocity in a column process one-level tray absorption columns of 10cm/s～15cm/s, simultaneously, from the one-level tray absorption columns tower top spray-absorption agent benzene/dimethylbenzene mixeding liquid volume ratio is 1: 1, make the reverse contact of gas-liquid two-phase, absorb the fumigation medicament Celfume, whole absorption process, under normal pressure, controlling the absorption temperature is 15 ℃～25 ℃, carry out absorption operation, collect rich solution, and will absorb tail gas and pass into and carry out chemical absorbing in next absorption tower and process, chemical absorbing processing wherein is consistent with the method in embodiment 1, repeat no more.
the rich solution that the upper step was collected changes in rectifying column, be warming up to 110 ℃ of backflows, carry out rectifying, utilize the difference of volatility between Celfume and absorbent benzene/dimethylbenzene mixed liquor, by interior backflow, Celfume is separated with benzene/dimethylbenzene mixed liquor, being about to Celfume separates from the top of rectifying column, through after the drying device drying of tower top, pass through again compressor, pass through at last condensation liquefaction, to pans, after rectifying finishes, the Celfume that recovery is good is packed in special cylinder, the Celfume that obtains can be reused, realize regeneration, the absorbent of separating can be applied mechanically.
Embodiment 4
after fumigation medicament hydrogen phosphide is made vaporization fully through vaporizer, cushioning in-tank mixing with the synergist carbon dioxide again, wherein the addition of synergist carbon dioxide is volume ratio 10%, after fully mixing, pass in fumatorium fumigated thing is fumigated processing, after stifling processing finishes, mist in fumatorium is passed through the one-level tray absorption columns from the bottom, mist is with the superficial linear velocity in a column process tray absorption columns of 5cm/s～15cm/s, simultaneously, tower top spray-absorption agent ethanol from tray absorption columns, make the reverse contact of gas-liquid two-phase, absorb fumigation medicament hydrogen phosphide, whole absorption process, under normal pressure, controlling the absorption temperature is 25 ℃～35 ℃, carry out absorption operation, collect rich solution, and will absorb tail gas and pass into and carry out chemical absorbing in next absorption tower and process, chemical absorbing is wherein processed can adopt Chinese patent application (publication number: after the method CN1386567A) is processed, at last tail gas is drained in atmosphere.
The rich solution that the upper step was collected changes in rectifying column, be warming up to 110 ℃ of backflows, carry out rectifying, utilize the difference of volatility between hydrogen phosphide and absorbent ethanol, by interior backflow, with hydrogen phosphide and separation of ethanol, be about to hydrogen phosphide and separate from the top of rectifying column, through after the drying device drying of tower top, then pass through compressor, pass through at last condensation liquefaction, to pans, after rectifying finished, the hydrogen phosphide that recovery is good was packed in special cylinder, the hydrogen phosphide that obtains can be reused, and the absorbent ethanol of separating can be applied mechanically again.
Embodiment 5
after fumigation medicament hydrogen phosphide is made vaporization fully through vaporizer, cushioning in-tank mixing with the synergist carbon dioxide again, wherein the addition of synergist carbon dioxide is volume ratio 16%, after fully mixing, pass in fumatorium fumigated thing is fumigated processing, after stifling processing finishes, mist in fumatorium is passed through the one-level tray absorption columns from the bottom, mist is with the superficial linear velocity in a column process tray absorption columns of 10cm/s～15cm/s, simultaneously, tower top spray-absorption agent benzinum from the material filling type absorption tower, make the reverse contact of gas-liquid two-phase, absorb fumigation medicament hydrogen phosphide, whole absorption process, under normal pressure, controlling the absorption temperature is 50 ℃～75 ℃, carry out absorption operation, collect rich solution, and will absorb tail gas and pass into and carry out chemical absorbing in next absorption tower and process, chemical absorbing is wherein processed consistent with the method for embodiment 4, repeat no more.
the rich solution that the upper step was collected changes in rectifying column, be warming up to 80 ℃ of backflows, carry out rectifying, utilize the difference of volatility between hydrogen phosphide and absorbent benzinum, by interior backflow, hydrogen phosphide is separated with benzinum, being about to hydrogen phosphide separates from the top of rectifying column, through after the drying device drying of tower top, pass through again compressor, pass through at last condensation liquefaction, be collected into pans, after rectifying finishes, the hydrogen phosphide that recovery is good is packed in special cylinder, the hydrogen phosphide that obtains can be reused, realize regeneration, the absorbent benzinum of separating can be applied mechanically again.
Specific embodiment described in the present invention is only to the explanation for example of the present invention's spirit.Those skilled in the art can make various modifications or replenish or adopt similar mode to substitute described specific embodiment, but can't depart from spirit of the present invention or surmount the defined scope of appended claims.
Although the present invention has been made a detailed description and has quoted as proof some specific embodiments, to those skilled in the art, only otherwise it is obvious leaving that the spirit and scope of the present invention can make various changes or revise.
Claims (3)
1. the separation and recovery method of a fumigation medicament, comprise and to be mixed together with synergist after fumigation medicament vaporization, enter fumatorium and fumigate processing, after processing finishes, mist in fumatorium is recycled, described fumigation medicament is hydrogen phosphide, it is characterized in that: described recycling comprises the following steps:
A, make mist carry out reverse the contact with absorbent benzinum two-phase, under normal pressure, control and absorb temperature carry out Physical Absorption under 50 ℃～75 ℃, absorb fumigation medicament, collect rich solution, will absorb tail gas and carry out again the chemical absorbing processing;
B, the rich solution of collecting in step a is carried out rectifying, separate fumigation medicament hydrogen phosphide and absorbent benzinum, the fumigation medicament of recovery and absorbent can be applied mechanically.
2. the separation and recovery method of fumigation medicament according to claim 1, it is characterized in that: described synergist is carbon dioxide.
3. the separation and recovery method of fumigation medicament according to claim 1 and 2, it is characterized in that: the rectification temperature described in step b is reflux temperature, described rectifying pressure is normal pressure.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016137337A1 (en) * | 2015-02-25 | 2016-09-01 | Genera Limited | Method and apparatus for fumigant gas capture |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102728605A (en) * | 2012-06-29 | 2012-10-17 | 大连东泰产业废弃物处理有限公司 | Harmless treatment method for aluminum phosphide fumigation residues |
| CN103349895B (en) * | 2013-07-03 | 2016-06-22 | 浙江工业大学 | The device of a kind of chemically based absorbing and removing vikane and technique |
| CN105876590A (en) * | 2014-09-10 | 2016-08-24 | 中国检验检疫科学研究院 | Novel ethyl formate quantitative dosing system |
| CN107485971B (en) * | 2017-07-28 | 2019-06-21 | 浙江工业大学 | A kind of recyclable device and its recovery process remaining fumigant vikane |
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| WO1997026796A1 (en) * | 1996-01-24 | 1997-07-31 | Halozone Technologies, Inc. | Recycling and recovery of methyl bromide fumigant |
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| CN1199921C (en) * | 2002-07-23 | 2005-05-04 | 浙江新安化工集团股份有限公司 | Technique for cleanly recovering byproduct methyl chloride of glyphosate acid |
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| CN1156952A (en) * | 1994-07-05 | 1997-08-13 | 联邦科学及工业研究组织 | Cyanogen fumigants and method of fumigation using cyanogen |
| WO1997026796A1 (en) * | 1996-01-24 | 1997-07-31 | Halozone Technologies, Inc. | Recycling and recovery of methyl bromide fumigant |
| CN1386567A (en) * | 2002-03-29 | 2002-12-25 | 上海烟草（集团）公司 | Process for removing PH3 from residual gas after fumigant insect killing |
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| WO2016137337A1 (en) * | 2015-02-25 | 2016-09-01 | Genera Limited | Method and apparatus for fumigant gas capture |
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