CN101747165B - Preparation method of pesticide-residue-level acetone - Google Patents
Preparation method of pesticide-residue-level acetone Download PDFInfo
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- CN101747165B CN101747165B CN 200910163053 CN200910163053A CN101747165B CN 101747165 B CN101747165 B CN 101747165B CN 200910163053 CN200910163053 CN 200910163053 CN 200910163053 A CN200910163053 A CN 200910163053A CN 101747165 B CN101747165 B CN 101747165B
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000000447 pesticide residue Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000001179 sorption measurement Methods 0.000 claims abstract description 33
- 238000010992 reflux Methods 0.000 claims abstract description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000741 silica gel Substances 0.000 claims abstract description 20
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000010521 absorption reaction Methods 0.000 claims abstract description 9
- 230000001105 regulatory effect Effects 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000009835 boiling Methods 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 239000003039 volatile agent Substances 0.000 claims description 8
- 239000002594 sorbent Substances 0.000 claims description 7
- 238000009833 condensation Methods 0.000 claims description 6
- 230000005494 condensation Effects 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 3
- 241000237502 Ostreidae Species 0.000 claims description 2
- 235000020636 oyster Nutrition 0.000 claims description 2
- 230000008929 regeneration Effects 0.000 claims description 2
- 238000011069 regeneration method Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000009834 vaporization Methods 0.000 claims description 2
- 230000008016 vaporization Effects 0.000 claims description 2
- 238000011049 filling Methods 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 3
- 239000011550 stock solution Substances 0.000 abstract 3
- 239000012535 impurity Substances 0.000 description 23
- 239000002904 solvent Substances 0.000 description 23
- 238000009313 farming Methods 0.000 description 19
- 238000001514 detection method Methods 0.000 description 14
- 238000004458 analytical method Methods 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000004821 distillation Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 6
- 239000000470 constituent Substances 0.000 description 5
- 235000013305 food Nutrition 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000008676 import Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003891 environmental analysis Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000004186 food analysis Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 238000004454 trace mineral analysis Methods 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a preparation method of pesticide-residue-level acetone. The method comprises the following steps: (1) after the analytically pure acetone is processed by contact absorption by silica gel filled in an adsorption column, discarding the firstly 5-15% of the adsorbed stock solution, and introducing the rest 85-95% of the stock solution, which flows out of the bottom of the adsorption column, into the rectifying step; (2) and rectifying under ordinary pressure, wherein the temperature of the condensate water is 0-25 DEG C, the voltage of a heater is 100-200 V, after the total reflux operation starts for 0.5-3 hours, when the tower top temperature reaches the boiling point of acetone 56.4 DEG C, the reflux speed of the stock solution is controlled at 1-10 drops/s, and the reflux ratio is 40-1:1, excluding 1/9 of the previous distillate by volume; and regulating the reflux ratio to 1:1-10, receiving 7/9 of the product by volume until the surplus kettle solution is 1/9 by volume, stopping heating, and finishing rectifying. The method prepares the expensive pesticide-residue-level acetone from cheap analytically-pure acetone made in China, and thus, the invention has the advantage of low operating cost and has wide commercial application prospects.
Description
Technical field
The present invention relates to a kind of preparation method of pesticide-residue-level acetone, particularly relate to a kind of sorbent material that utilizes, the acetone of analytical pure purity grade is prepared into the method for the pesticide-residue-level acetone that can be used for agricultural residual detection through absorption distillation.
Background technology
Food safety not only is related to human health and life security, and is related to the sustainable development of international trade and national economy and stablizing of society, so food safety is the great strategy that international community and national governments face.The detection of food safety is primarily aimed at oxious component such as heavy metal content, pesticide residue in the food.
Pesticide residue are the principal pollutant that influence agricultural product quality and safety.The trace standard of pesticide is to weigh the main foundation of agricultural product quality and safety, in International Agricultural Trade often by developed country as the important means that tbt is set.Before and after China accession to the WTO, developed faster about the research of the residual detection of farming, but still faced problems, unsound like standard, limit standard and method standard do not match, and mark article reagent dependence on import or the like.
In the residual detection of farming, detection level is generally at ppm (10
-6) and ppb (10
-9) about, analysis belongs to trace analysis.Simultaneously, also contain homologue, isomer, degraded product, meta-bolites and conjugates of agricultural chemicals or the like during farming is residual, component is very complicated, in case detect sample generation trace contamination, detected result is made a mistake.Therefore in actual detected, the sample pretreatment process is crucial, accounts for about 70% of workload greatly, and its purpose is exactly in order to remove and the simultaneous impurity of target compound, avoids trace contamination, reduces the chromatogram Interference Peaks.
For used solvent in the residual detection of farming, strict requirement has all been done to it especially by food safety both domestic and external mechanism.Conventional solvent comprises by the purity grade classification: CP, and its principal constituent content is high, purity is higher, exists to disturb impurity, is applicable to chemical experiment and synthetic preparation; Analytical pure, its principal constituent content is very high, purity is higher, disturbs impurity very low, is applicable to technical analysis and chemical experiment; Top grade is pure, and its principal constituent content is very high, purity is very high, is applicable to Accurate Analysis and research work, and what have can be used as primary standard; Chromatographically pure, its principal constituent content is high, and quality index pays attention to disturbing the impurity of chromatographic peak, and stratographic analysis is special-purpose.And do not do clearly definition for the residual level of farming solvent.Generally speaking; In the agricultural residual examination criteria of states such as European Union, the U.S. and Japan; The agricultural residual level solvent that regulation is used; Be meant the high neat solvent through this application Operability Testing, promptly solvent is through extraction, concentrated after after gc-electron capture detector/nitrogen phosphorous detector/FPD/mass spectrum (GC-ECD/NPD/FPD/MS) detection, require its impurity signal to be lower than ppb level farming residual standard thing signal.With the Nippon Standard is example, and solvent to be measured is concentrated 300 times, adopts GC-ECD to detect, and solvent to be measured is half the to 60min γ-phenyl-hexachloride RT, requires the peak height of all impurity to be not more than the half the of standardized solution γ-phenyl-hexachloride (4ng/mL) peak height.Therefore, the residual level of farming solvent is often more paid attention to the influence of solvent to detected result.
In the residual detection of farming, mostly its detection means is chromatogram, comprises gc and liquid chromatography; The maximum solvent that uses is acetonitrile, acetone, ETHYLE ACETATE etc.Because the impurity Interference Peaks that the agricultural residual level solvent of domestic production contains is too much; The overwhelming majority does not reach the requirement of agricultural residual detection, and the solvent that uses in the domestic agricultural residual test experience chamber almost all is other product of chromatographically pure level that offshore company produces; Like Merck, Sigma-Aldrich, Fisher, J.T.Baker etc.; Price is extremely expensive, labor research funding not only, and make national scientific research and analyzing and testing limited ability in foreign country.
At present, the traditional organic solvent purifying purifies to 99.9% or 99.99% to principal constituent from 90% usually, that is to say that the reduction of foreign matter content reaches 0.01% (10 usually
-4) level, do not relate to 10 as yet
-12Or the removal technology of the impurity of low levels more, this kind method obviously can not satisfy the preparation requirement of the residual level of farming solvent.
Because the trade secret of the preparation technology of the residual level of farming solvent to be each big reagent company, relevant document or patent report are almost blank.
Summary of the invention
In order to satisfy food analysis, the environmental analysis field demand that China becomes more and more important, solve the problem of the residual level of farming solvent dependence on import, the method that the invention provides an economy and very easily implement is used to prepare the pesticide-residue-level acetone that is applicable to farming residual analysis.
A kind of pesticide-residue-level acetone preparation method of farming residual analysis that is applicable to of the present invention is achieved in that
The preparation method of a kind of pesticide-residue-level acetone of the present invention, described preparation method comprises the steps:
One, adsorption step:
Analytical pure acetone is flowed into by adsorption column 2 tops, and after the sorbent material silica gel that in adsorption column, the loads contact absorption, flow out from the adsorption column bottom;
In described adsorption process, stoste after 5～15% the absorption before the adsorption process is discarded, stoste after the absorption of back 85～95% is introduced in the distillation system.
Two, rectification step:
After in the input of the stoste behind the adsorption step distillation system, under normal pressure, after the 3 heating vaporizations of rectifying tower still, introduce rectifying tower 4 rectifying earlier;
The material of rectifying tower top is regulated shunting through prolong 5 condensations and reflux ratio controller 6 successively, and a part is back to rectifying tower 4, and another part gets into receiving bottle 7 as product; Get rid of the front-end volatiles of 1/9 stoste volume and the residue still liquid of 1/9 stoste volume, 7/9 of the stoste volume of gained is the pesticide-residue-level acetone product.
In practical implementation,
In the described adsorption step, said silica gel is the commercially available prod, and its molecular formula is H
2SiO
3, specification is the 100-300 order, and particle diameter is 50～150 microns, and specific surface area is 200～600m
2/ g;
Said silica gel is white or the oyster white granular solids with open vesicular structure;
In the described adsorption step, the consumption of silica gel is 20～50% of a raw material weight, and the tamped density of adsorption column is 200～800kg/m
3
Said silica gel uses after 150～300 ℃ of bakings can be recycled after the manipulation of regeneration in 2～5 hours;
In the described adsorption step, stoste is flowed through behind the adsorption column, and the stoste with preceding 5～15% discards, and the stoste of back 85～95% is introduced in the distillation system;
In described rectification step, the height of described rectifying tower 4 is 1.5～4m, and internal diameter is 1～20cm, and inner stuffing is the θ ring;
Prolong be shaped as coil pipe type, highly be 0.5～1m, internal diameter is 1～20cm;
The volume of described rectifying still is 2～20L;
In described rectification step, the controlled variable scope and the control method of the temperature of described rectifying tower 4, reflux ratio, flow velocity are:
The temperature of regulating water of condensation is 0～25 ℃, and beginning total reflux operation 0.5～3 hour is when the temperature of rectifying tower top reaches 56.4 ℃ of acetone boiling temperatures; The return velocity of control stoste is 1～10 droplet/second; Reflux ratio is 40～1: 1, preferred 30～10: 1, get rid of the front-end volatiles of 1/9 volume; Regulating reflux ratio then is 1: 1～10, receives the product of 7/9 volume, is till 1/9 the stoste until residue still liquid, stops heating, finishes rectifying;
Described rectifying still heater voltage is 100～200V.
Because the residual level of farming is analyzed GC-ECD commonly used as detection method, and the characteristics of ECD are the influences that are subject to polar compound.Therefore select the strong silica gel of polar compound adsorptivity to remove such impurity as sorbent material.The adsorptive power of silica gel and its particulate size are inversely proportional to, and particle is more little, and adsorbable impurity is many more; But the flowing time of stoste and its particle size also are inversely proportional to, and particle is more little, can cause the Flow of Goods and Materials overlong time, and promptly the running time is long.Therefore, through taking all factors into consideration, the present invention selects the silica gel particle scope between 100～300 orders, and promptly a footpath is about 50～150 microns, and specific surface area is 200～600m
2/ g.
At the beginning of rectification system began, owing to do not reach dynamic balance state in the tower, some influenced farming residual analysis, and content is 10
-12About impurity steamed easily; Therefore, the present invention is following for the control of its reflux ratio: at first regulating reflux ratio is 40～1: 1, preferred 30～10: 1, steam the front-end volatiles of 1/9 volume, and system reaches balance in the tower afterwards, and therefore regulating reflux ratio is 1: thus 1～10 receive product.Remain 1/9 still liquid at last.Impurity in front-end volatiles and the still liquid is than higher, and content is greater than 10
-12, in order to guarantee the requirement that reaches of product, cast out this two portions, the stoste of totally 2/9 volume.
Compared to the method for purification of traditional organic solvent, the present invention utilizes cheap homemade analytical pure acetone, has made the acetone soln of agricultural residual level, and running cost is low.And the product foreign matter content that makes falls in 10
-12, can satisfy the requirement of farming residual analysis, have considerable market application foreground.
Description of drawings
Figure one pesticide-residue-level acetone preparation method synoptic diagram of the present invention
Embodiment
Embodiment 1
1. device parameter:
Adsorption column internal diameter 4cm, length 70cm;
Sorbent material: silica gel, the molecular formula of silica gel are H
2SiO
3, specification is the 100-300 order, and particle diameter is 50～150 microns, and specific surface area is 200～600m
2/ g; The consumption of silica gel is 35% of a raw material weight
Rectifying tower size: tower height 3m, tower internal diameter 10cm; Filler: θ ring.
Prolong be shaped as coil pipe type, highly be 1m, internal diameter is 10cm.
The four neck round-bottomed flasks of tower still: 20L.
Glass ground joint with standard between all devices connects.
2. adsorption operations:
Slowly pour 10L analytical pure acetone into adsorption column, discard preceding 10% solvent, all solvent 9L after collecting.
3. distillation operation: the solvent to collecting after the adsorption operations carries out distillation operation; At first the cooling temperature of water of condensation is 0 ℃, and the adjusting heater voltage is 120V, total reflux operation 1h; When the temperature of rectifying tower top reached 56.4 ℃, the return velocity of control stoste was 5 droplets/second.Change reflux ratio and be under 20: 1 the condition and collect front-end volatiles 1L, under the condition of reflux ratio, regather cut 7L then at 1: 5.Residue still liquid 1L stops heating.
4. agricultural residual level index detected result:
1) test condition:
A) gas chromatograph: the 6890N of Anjelen Sci. & Tech. Inc type, detector are ECD.
B) gas chromatographic column: Anjelen Sci. & Tech. Inc, model HP-5, length 60m, internal diameter 0.32mm, thickness 0.25 μ m.
C) GC-ECD condition: injector temperature: 250 ℃; Detector temperature: 260 ℃; Column temperature: 200 ℃, constant temperature mode keeps 60min; Sample size: 1 μ L; Splitting ratio: 50: 1; Carrier gas: high pure nitrogen; Flow velocity: 1mL/min.
2) drafting of the detection of standard substance and typical curve:
Working concentration is that γ-phenyl-hexachloride standardized solution of 100ng/mL dilutes successively, and γ-phenyl-hexachloride working standard solution of preparation 2～50ng/mL adopts above-mentioned GC-ECD method to detect.According to drawing standard curve as a result, calculating γ-phenyl-hexachloride concentration is the pairing peak height of 2ng/mL.
The detected result of standard substance shows that the RT of γ-phenyl-hexachloride is 5.5min; Therefore with this understanding; Farming residual level index foundation up to standard is: after solvent to be measured concentrates 300 times; Within the 5.5min to 60min of GC-ECD spectrogram, the concentration that the impurity peak height is converted out by above-mentioned typical curve is not more than 2ng/mL.
The raw material detected result is as shown in table 1:
The GC-ECD detected result of table 1 raw material
| The impurity numbering | The GC-ECD RT (min) of impurity | The concentration (ng/mL) of conversion |
| 1 | 6.3 | 5.01 |
| 2 | 6.6 | 3.80 |
| 3 | 8.4 | 3.59 |
| 4 | 22.6 | 3.30 |
| 5 | 48.8 | 8.57 |
Test result shows the peak that has 5 to exceed standard.
Product detected result after rectifying is as shown in table 2:
The GC-ECD detected result of table 2 rectifying product
| The impurity numbering | The GC-ECD RT (min) of impurity | The concentration (ng/mL) of conversion |
| 1 | ?6.6 | 0.44 |
5 impurity peaks in the raw material only detect 1, and conversion concentration＜2ng/mL, and promptly product reaches the residual level of farming index.
1. device parameter:
Adsorption column internal diameter 3cm, length 40cm;
Sorbent material: silica gel, the molecular formula of silica gel are H
2SiO
3, specification is the 100-300 order, and particle diameter is 50～150 microns, and specific surface area is 200～600m
2/ g; The consumption of silica gel is 22% of a raw material weight
Rectifying tower size: tower height 1.5m, tower internal diameter 3cm; Filler: θ ring.
Prolong be shaped as coil pipe type, highly be 0.5m, internal diameter is 3cm.
The four neck round-bottomed flasks of tower still: 10L.
Glass ground joint with standard between all devices connects.
2. adsorption operations:
Slowly pour 5L analytical pure acetone into adsorption column, discard preceding 10% solvent, all solvent 4.5L after collecting.
3. distillation operation: the solvent to collecting after the adsorption operations carries out distillation operation; At first the cooling temperature of water of condensation is 6 ℃, and the adjusting heater voltage is 100V, total reflux operation 2h; When the temperature of rectifying tower top reached 77.0 ℃, the return velocity of control stoste was 6 droplets/second.Change reflux ratio and be under 5: 1 the condition and collect front-end volatiles 0.5L, under the condition of reflux ratio, regather cut 3.5L then at 1: 9.Residue still liquid 0.5L stops heating.
4. agricultural residual level index detected result:
1) test condition: with embodiment 1.
2) drafting of the detection of standard substance and typical curve: with embodiment 1.
The raw material detected result is with embodiment 1.
Product detected result after rectifying is as shown in table 3:
The GC-ECD detected result of table 3 rectifying product
| The impurity numbering | The GC-ECD RT (min) of impurity | The concentration (ng/mL) of conversion |
| 1 | ?6.6 | 0.50 |
6 impurity peaks in the raw material only detect 1, and conversion concentration＜2ng/mL, and promptly product reaches the residual level of farming index.
Table 4 is seen in the reaction conditions contrast of the foregoing description
The reaction conditions contrast of table 4 embodiment
| Absorption discards the stoste volume | The sorbent material consumption | Tamped density | Adsorption column is high | The adsorption column internal diameter | The rectifying tower height | The tower internal diameter | Prolong | ||
| Scope | |||||||||
| 5～15％ | 20～50％ | 200～800 kg/m 3 | 30～ |
2～6cm | 1.5～4m | 1～20cm | 0.5～1m | ||
| Embodiment 1 | 10％ | 35％ | 500 kg/m 3 | 70cm | 4cm | 3m | | 1m | |
| Embodiment | |||||||||
| 2 | 10％ | 22％ | 600 kg/m 3 | 40cm | 3cm | 1.5m | 3cm | 0.5m | |
| The prolong internal diameter | Condensate temperature | The rectifying still volume | Total reflux operation hour | Return velocity | Preceding reflux ratio | Back reflux ratio | Heater voltage | ||
| Scope | 1～20cm | 0～25 |
2～20L | 0.5～3h | 1～10 droplet/second | 40～1∶1 | 1∶1～10 | 100～200V | |
| Embodiment 1 | 10cm | 0 | 20L | 1h | 5 droplets/second | 20∶1 | 1∶5 | | |
| Embodiment | |||||||||
| 2 | |
6 | 10L | 2h | 6 droplets/second | 5∶1 | 1∶9 | 100V |
Comparative Examples 1
With above-mentioned detection method, the pesticide-residue-level acetone that detects certain Overseas Company is as comparison, result such as table 5:
The pesticide-residue-level acetone GC-ECD detected result of certain Overseas Company of table 5
| The impurity numbering | The GC-ECD RT (min) of impurity | The concentration (ng/mL) of conversion |
| 1 | 6.6 | 0.59 |
| 2 | 8.4 | 0.84 |
Claims (2)
1. the preparation method of a pesticide-residue-level acetone, described preparation method comprises the steps:
One, adsorption step:
Analytical pure acetone is flowed into by adsorption column (2) top, and after the sorbent material silica gel of filling in adsorption column (2) the contact absorption, flow out from adsorption column (2) bottom;
In described adsorption process, stoste after 5～15% the absorption before the adsorption process is discarded, stoste after the absorption of back 85～95% is introduced rectification step;
In the described adsorption step, the molecular formula of silica gel is H
2SiO
3, specification is the 100-300 order, and particle diameter is 50～150 microns, and specific surface area is 200～600m
2/ g;
Said silica gel is white or the oyster white granular solids with open vesicular structure;
Two, rectification step:
Under normal pressure, after rectifying tower still (3) heating vaporization, introduce rectifying tower (4) rectifying through the stoste behind the adsorption step earlier;
The material on rectifying tower (4) top is regulated shunting through prolong (5) condensation and reflux ratio controller (6) successively, and a part is back to rectifying tower (4), and another part gets into receiving bottle (7) as product; Get rid of the front-end volatiles of 1/9 stoste volume and the residue still liquid of 1/9 stoste volume, 7/9 of the stoste volume of gained is the pesticide-residue-level acetone product;
In described rectification step, the height of rectifying tower (4) is 1.5～4m, and internal diameter is 1～20cm, and inner stuffing is the θ ring;
Rectifying tower (4) top prolong be shaped as coil pipe type, highly be 0.5～1m, internal diameter is 1～20cm;
The volume of described rectifying still is 2～20L;
The controlled variable scope and the control method of the temperature of described rectifying tower (4), reflux ratio, flow velocity are:
The temperature of regulating water of condensation is 0～25 ℃, beginning total reflux operation 0.5～3 hour, and when the temperature of rectifying tower top reached the acetone boiling temperature, the return velocity of control stoste was 1～10 droplet/second, reflux ratio is 40～1:1, gets rid of the front-end volatiles of 1/9 stoste volume; Regulating reflux ratio then is 1:1～10, receives the product of 7/9 stoste volume, is till 1/9 the stoste until residue still liquid, stops heating, finishes rectifying;
Described rectifying still heater voltage is 100～200V.
2. the preparation method of pesticide-residue-level acetone as claimed in claim 1 is characterized in that:
The consumption of said silica gel is 20～50% of a raw material weight, and the tamped density of adsorption column is 200～800kg/m
3;
Said silica gel uses after 150～300 ℃ of bakings recycled after the manipulation of regeneration in 2～5 hours.
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|---|---|---|---|
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|---|---|---|---|
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3330741A (en) * | 1963-03-12 | 1967-07-11 | Hoechst Ag | Distillation process for purifying acetone |
| GB1264481A (en) * | 1968-09-28 | 1972-02-23 | ||
| CN101190879A (en) * | 2007-12-21 | 2008-06-04 | 天津大学 | Magnetization rectification method for reclaiming acetone from waste acetone menstruum |
-
2009
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3330741A (en) * | 1963-03-12 | 1967-07-11 | Hoechst Ag | Distillation process for purifying acetone |
| GB1264481A (en) * | 1968-09-28 | 1972-02-23 | ||
| CN101190879A (en) * | 2007-12-21 | 2008-06-04 | 天津大学 | Magnetization rectification method for reclaiming acetone from waste acetone menstruum |
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