CN102126907A - Method for preparing pesticide residue grade n-hexane by purifying - Google Patents
Method for preparing pesticide residue grade n-hexane by purifying Download PDFInfo
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- CN102126907A CN102126907A CN2010106179233A CN201010617923A CN102126907A CN 102126907 A CN102126907 A CN 102126907A CN 2010106179233 A CN2010106179233 A CN 2010106179233A CN 201010617923 A CN201010617923 A CN 201010617923A CN 102126907 A CN102126907 A CN 102126907A
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Abstract
The invention discloses a method for preparing pesticide residue grade n-hexane by purifying. The method comprises the following steps of: decoloring n-hexane with a decoloring agent; and rectifying and filtering to obtain pesticide residue grade n-hexane, wherein the decoloring agent is active carbon, carbon dioxide or polymer alumina with adsorptive action or concentrated sulfuric acid with strong oxidizing property; the dosage of the decoloring agent is 1-50 percent by weight of that of the n-hexane; and decoloring time is between 3 hours and 24 hours. An n-hexane product obtained by the method has the impurity content of lower than 10-12, and can meet the requirement on pesticide residue analysis. The method has the advantages of easiness in operating, cost saving and wide market application prospect.
Description
Technical field
The present invention relates to agricultural residual detection range, further, relate to a kind of discoloring agent that utilizes, the normal hexane of technical grade purity is prepared into the method for the agricultural residual level normal hexane that can be used for agricultural residual detection by decolouring rectifying purifying.
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 Technical Barriers to Trade 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 as standard, limit standard and technological standard do not match, and mark product reagent dependence on import or the like.
In the residual detection of farming, detection level is generally in ppt level (10
-12), 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: chemical pure, and its principal constituent content height, purity are higher, exist and disturb impurity, are applicable to the preparation of chemical experiment and synthesizing and purifying; Technical grade, 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 height, quality index pays attention to disturbing the impurity of chromatographic peak, stratographic analysis special use.
And do not do clearly definition for the residual level of farming solvent.In general, 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 high neat solvent by this application Operability Testing, be that solvent is through extraction, concentrated after after gas-chromatography-electron capture detector/nitrogen phosphorous detector/flame photometric detector/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 to 60min, requires the peak height of all impurity to be not more than half of standard solvent γ-phenyl-hexachloride (4ng/mL) peak height in half of γ-phenyl-hexachloride retention time.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, its detection means mostly is chromatogram, comprises gas-chromatography and liquid chromatography; The maximum solvent that uses is acetonitrile, normal hexane, ethyl 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, the solvent that uses in the domestic agricultural residual test experience chamber, it almost all is other product of chromatographically pure level that offshore company produces, as The foreign chicken products such as Merck, Sigma-Aldrich, Fisher, J.T.Baker, price is extremely expensive, not only expends a large amount of research fundings, and makes national scientific research and analyzing and testing limited ability in foreign country.
At present, 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, the purifying that this kind technology obviously can not satisfy the residual level of farming solvent prepares requirement.Because the trade secret of the purifying 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
Too much for solving the impurity Interference Peaks that the residual level of prior art middle peasant solvent contains, purity does not reach the problem of agricultural residual detection requirement, the invention provides the residual level of a kind of farming normal hexane method for preparing purified, the normal hexane product foreign matter content that employing the method for the invention makes is less than 10
-12, can satisfy the requirement of farming residual analysis, and simple to operate, saving cost, be with a wide range of applications.
The method for preparing purified that the purpose of this invention is to provide the residual level of a kind of farming normal hexane.
Described method comprises that normal hexane carries out rectifying again behind bleaching agent bleaching, filtration makes the residual level of described farming normal hexane.Normal hexane described in present method is a normal hexane product all in the prior art, comprises raw materials such as technical grade, chemical pure, top grade are pure, chromatographically pure.
Used discoloring agent is strong adsorbing gac of the prior art, silicon-dioxide, polymer alumina, and the particle median size is between the 50-150 micron, and specific surface area is 200-600m
2/ g, also can adopt mass percent concentration more than or equal to 70% the vitriol oil as discoloring agent.
Gas-chromatography-electron capture detector GC-ECD is as detection technique because the residual level analysis of farming is used always, and the characteristics of ECD are the influences that are subject to polar compound.Therefore select the discoloring agent strong, remove such impurity the polar compound decolourising property.This kind discoloring agent is gac of the prior art, silicon-dioxide, polymer alumina or mass percent concentration more than or equal to 70% the vitriol oil, and consumption is little, the decolorizing efficiency height,, and make the UV uv-absorbing significance in the normal hexane be reduced to the residual level of farming index.The decoloring ability of discoloring agent and its particulate size are inversely proportional to, and particle is more little, and the impurity that can decolour is many more; But the flowing time of stoste and its granular size also are inversely proportional to, and particle is more little, can cause the Flow of Goods and Materials overlong time, and promptly the operating time is long.Therefore, through taking all factors into consideration, the preferred discoloring agent granulometric range of the present invention is between the 100-300 order, and promptly the particle median size is between the 50-150 micron, and specific surface area is 200-600m
2/ g.
The consumption of described discoloring agent is the 1-50% of normal hexane consumption, preferred 5-20%, and bleaching time is 3-24 hour;
Described gac, silicon-dioxide, polymer alumina use after 100-500 ℃ of baking recycled after 2-5 hour.
Described method comprises:
A) decolouring
The normal hexane raw material is entered from the decoloring reaction tank top, with discoloring agent reaction decolouring, reach described bleaching time after, the decoloring reaction pot liquid is divided into two-layer, and supernatant liquid is introduced rectification step as raw material;
B) rectifying
Normal hexane raw material after decolouring is sent into the dehydrogenation tower, dehydrogenation column overhead extraction light constituent, and dehydrogenation Tata still extraction material is sent into rectifying tower;
Rectifying Tata still extraction heavy constituent, rectifying tower cat head extraction normal hexane;
C) filter
The normal hexane of rectifying tower cat head extraction is sent in the filtration unit and is filtered, and obtains the residual level of described farming normal hexane.
Concrete operations are as follows:
A, decolouring step:
Normal hexane is flowed into by the decoloring reaction tank top, and after the discoloring agent contact decolorization of in the decoloring reaction jar, loading, after reaching described bleaching time, solution in the decoloring reaction jar is divided into two-layer, discard lower floor's dark solution, to collect through the supernatant liquor after the decolouring, and introduce in the distillation system through volume pump.
B, rectification step:
Under normal pressure, after dehydrogenation tower heating vaporization, introduce rectifying tower rectifying through the normal hexane after the decolouring step earlier;
Certain embodiments: behind condensing reflux, a part is back to the dehydrogenation tower to the material of dehydrogenation column overhead successively, and another part enters the light constituent jar as product; Tower still material after the dehydrogenation is sent into rectifying tower and is carried out rectifying;
In described dehydrogenation rectifying, the height of dehydrogenation tower is 1.0-10m, and internal diameter is 5-100cm, and inner stuffing can be θ ring, structured packing or dumped packing.
The volume of the tower still of described dehydrogenation tower is the 2-5000 liter;
The controlled variable scope of the temperature of dehydrogenation tower, reflux ratio, flow velocity is:
The temperature of regulating condensation cycle water is 0-25 ℃, beginning total reflux operation 0.5-3 hour, when the temperature of dehydrogenation cat head reached the light constituent boiling point, dehydrogenation tower reflux ratio scope was 40-1 among the present invention, regulate reflux ratio and gather light constituent, tower still material enters rectifying tower as raw material through volume pump.
Rectifying: after dehydrogenation Tata still material entered rectifying tower, vaporization in rectifying tower was after after the overhead condensation backflow, a part is back to rectifying tower, and another part enters the product jar as product; Rectifying tower still material enters residual liquid tank.
The height of rectifying tower is 1.0-10m, and internal diameter is 5-80cm, and inner stuffing can be θ ring, structured packing or dumped packing.
The volume of the tower still of described rectifying tower is the 2-5000 liter;
The controlled variable scope of the temperature of rectifying tower, reflux ratio, flow velocity is:
The temperature of regulating condensation cycle water is 0-25 ℃, and beginning total reflux operation 0.5-3 hour is when the temperature of rectifying tower top reaches the normal hexane boiling point, the reflux ratio scope is 40-1 among the present invention, gather the normal hexane component by regulating reflux ratio, from the cat head extraction, tower still still raffinate then pumps into the heavy constituent jar.
C, filtration step:
The normal hexane product that the rectifying tower cat head obtains is sent into and is removed impurity in the filtration unit after filtering and can obtain the residual level of described farming normal hexane;
Filtration unit can be the filtration unit that adopts usually in the prior art, and the filtering membrane in the filtration unit is an organic phase, and the aperture of filtering membrane is 0.10-1.20 μ m.
Compared to the purification techniques of traditional organic solvent, the present invention utilizes cheap homemade normal hexane, has made agricultural residual grade normal hexane solvent by steps such as decolouring rectifying, and the product foreign matter content falls in 10
-12, can satisfy the requirement of farming residual analysis, and simple to operate, save cost, have market application foreground widely.
Description of drawings
The method for preparing purified synoptic diagram of the residual level of Fig. 1 farming of the present invention normal hexane
Description of reference numerals:
1-head tank 2-decoloring reaction jar 3-dehydrogenation tower 4-rectifying tower
5-light constituent jar 6-heavy constituent jar 7-filtration unit 8-product jar
Embodiment
Below in conjunction with embodiment, further specify the present invention.
Embodiment 1
Device parameter
1) decoloring reaction jar: 2000 liters of volumes.
Discoloring agent: silicon-dioxide high-efficiency decolorant (the meticulous silica gel chemical industry in Qingdao company limited), specification is 200 orders, and median size is 100 microns, and specific surface area is 500m
2/ g; The consumption of high-efficiency decolorant is 22% of a raw material weight.
2) dehydrogenation tower: tower height 6m, tower internal diameter 80cm; Filler: structured packing.
Prolong be shaped as shell and tube, highly be 0.5m.
Dehydrogenation Tata still: 2000 liters heat-conducting oil furnace formula tower still.
3) rectifying tower: tower height 6m, tower internal diameter 100cm; Filler: structured packing.
Prolong be shaped as shell and tube, highly be 0.5m.
Rectifying Tata still: 2000 liters heat-conducting oil furnace formula tower still.4) filtration unit: stainless steel filtering membrane, aperture are 0.22 μ m.
Between all devices with the flange and the pipe connection of standard.
The a decolouring
With 1500 liters of technical grade normal hexane (purity＞98%, Korea S SK company) slowly pumps in the decoloring reaction jar 2 by head tank 1, through with 330 liters of abundant mixings of silicon-dioxide high-efficiency decolorant after, carry out decoloring reaction, bleaching time is 6 hours, collect the supernatant liquid after decolouring, as the raw material of dehydrogenation tower.
The b distillation operation
Technical grade normal hexane after the decolouring is pumped into dehydrogenation tower 3, regulating the heat-conducting oil furnace temperature is 100 ℃, the normal hexane raw material is in dehydrogenation tower 3 tower stills heating vaporization, when the temperature of dehydrogenation tower 3 cats head reaches the light constituent boiling point (65-68 ℃), the cooling temperature of regulating water of condensation is 5 ℃, total reflux operation 1 hour, regulating reflux ratio is 8: 1, gathers light constituent to light constituent jar 5;
After dehydrogenation tower 3 tower still materials entered rectifying tower 4, vaporization in rectifying tower 4 was after after the overhead condensation backflow, a part is back to rectifying tower 4, and another part enters filtration unit 7 as product; Tower still material enters heavy constituent jar 6.
Regulating rectifying Tata still heat-conducting oil furnace temperature is 100 ℃, the normal hexane raw material of removing light constituent is in rectifying tower 4 tower stills heating vaporization, when the temperature of rectifying tower 4 cats head reaches the normal hexane boiling point (68-70 ℃), the cooling temperature of regulating water of condensation is 5 ℃, total reflux operation 1 hour, regulating reflux ratio is 4: 1, gathers the normal hexane crude product to the product jar.
C filters
The normal hexane crude product of rectifying tower 4 cat head extraction enters in the filtration unit 7, removes the normal hexane that impurity can obtain meeting the residual level of farming index after filtering.
Test 1
The residual level of farming ultraviolet absorptivity test index detects:
This experiment China National Instruments Import ﹠ Export Corporation device model: 1901 series ultraviolet visible spectrophotometer, the quartz colorimetric utensil of 1mL.Open instrument preheating 30min, its absorbancy is surveyed in employing under different wave length, do blank contrast with distilled water or ultrapure water, detect the absorbancy index of each sample under 195nm, 210nm, 220nm, 230nm, 240nm and 250nm wavelength, the product detected result after this technology purifying prepares is as shown in table 1:
The UV detected result of table 1 rectifying product
| Wavelength | 195(nm) | 210(nm) | 220(nm) | 230(nm) | 240(nm) | 250(nm) |
| Raw material | 2.018 | 2.572 | 2.744 | 2.783 | 0.931 | 0.659 |
| Product | 0.934 | 0.246 | 0.081 | 0.032 | -0.001 | -0.016 |
| The residual grade standard of farming | ≤1.00 | ≤0.3 | ≤0.2 | ≤0.1 | ≤0.04 | ≤0.02 |
As shown in Table 1: the normal hexane raw material of technical grade under each wavelength its UV light absorption value (in the table 1 the 1st row) all greater than the standard value (the 3rd is capable in the table 1) of the residual level of farming, the product of purifying through this technological invention after testing, its UV value (the 2nd row in the table 1) is all less than the standard value of the residual level of farming.
The flame ionization ditector of gas-chromatography (GC-FID) detects
This experiment China National Instruments Import ﹠ Export Corporation device model: Agilent 6890,
Chromatographic column model: BP624 capillary column (the length 30m of Agilent company internal diameter 0.53mm thickness 3 μ m);
Sample size: 1 μ L, shunting in 50: 1; 40 ℃ of (5min) 10 ℃/min of column temperature, 260 ℃ (5min);
280 ℃ of 250 ℃ of detector temperatures of injector temperature;
Carrier gas: nitrogen (0.4MPa), hydrogen (0.3MPa);
Carrier gas column flow rate: 1ml/min.
Table 2 rectifying product the GC-ECD detected result
See Table 2 by the GC-ECD impurity detected result to product, 3 major impurity content wherein all are lower than 10
-12
Device parameter
1) decoloring reaction jar: glass separating funnel, 2.5 liters of volumes.
Discoloring agent: the vitriol oil (Beijing chemical reagent factory), concentration is 98%; The consumption of the vitriol oil is 5% of a raw material weight.
2) dehydrogenation tower: the high 1.3m of glass Tata, tower internal diameter 10cm; Filler: θ ring filler.
Prolong is the coil pipe type glass condenser.
Dehydrogenation Tata still: 3 liters triangle round bottom glass flask, the heating of electrically heated pot.
3) rectifying tower: the high 1.5m of glass Tata, tower internal diameter 10cm; Filler: θ ring filler.
Prolong is the coil pipe type glass condenser.
Rectifying Tata still: 3 liters triangle round bottom glass flask, the heating of electrically heated pot.
4) filtration unit: glass solvent filter, filtering membrane aperture are 0.22 μ m.
Adapter glass with standard between all devices is connected with plastic hose.
The a decolouring
2 liters of technical grade normal hexanes (purity＞98%, Korea S SK company) are added in the glass separating funnel 2, adds 0.1 liter of abundant mixing of the vitriol oil after, carry out decoloring reaction, bleaching time is 24 hours, collects the supernatant liquid after decolouring, as the raw material of dehydrogenation tower.
The b distillation operation
Technical grade normal hexane after the decolouring is imported dehydrogenation tower 3, regulate electrically heated pot voltage, slowly heating, the normal hexane raw material is in dehydrogenation tower 3 tower stills heating vaporization, when the temperature of dehydrogenation tower 3 cats head reaches the light constituent boiling point (65-68 ℃), the cooling temperature of regulating water of condensation is 5 ℃, total reflux operation 1.5 hours, regulating reflux ratio is 10: 1, gathers light constituent to light constituent jar 5.
After dehydrogenation tower 3 tower still materials entered rectifying tower 4, vaporization in rectifying tower 4 was after after the overhead condensation backflow, a part is back to rectifying tower 4, and another part enters filtration unit 7 as product; Tower still material enters heavy constituent jar 6.
Regulate rectifying Tata still electrically heated pot voltage, the normal hexane raw material of removing light constituent is in rectifying tower 4 tower stills heating vaporization, when the temperature of rectifying tower 4 cats head reaches the normal hexane boiling point (68-70 ℃), the cooling temperature of regulating water of condensation is 5 ℃, total reflux operation 1.5 hours, regulating reflux ratio is 6: 1, gathers the normal hexane crude product to the product jar.
C filters
The normal hexane crude product of rectifying tower 4 cat head extraction enters in the filtration unit 7, removes the normal hexane that impurity can obtain meeting the residual level of farming index after filtering.
Test 3
The residual level of farming ultraviolet absorptivity test index detects:
This experiment China National Instruments Import ﹠ Export Corporation device model: HITACHI U-3900, the quartz colorimetric utensil of 1mL.Open instrument preheating 30min, its absorbancy is surveyed in employing under different wave length, do blank contrast with distilled water or ultrapure water, detect the absorbancy index of each sample under 195nm, 210nm, 220nm, 230nm, 240nm and 250nm wavelength, the product detected result after this technology purifying prepares is as shown in table 3:
The UV detected result of table 3 rectifying product
| Wavelength | 195(nm) | 210(nm) | 220(nm) | 230(nm) | 240(nm) | 250(nm) |
| Raw material | 2.080 | 2.637 | 2.845 | 2.951 | 2.998 | 2.659 |
| Product | 0.725 | 0.202 | 0.168 | 0.086 | 0.034 | 0.014 |
| The residual grade standard of farming | ≤1.00 | ≤0.3 | ≤0.2 | ≤0.1 | ≤0.04 | ≤0.02 |
As shown in Table 3: the normal hexane raw material of technical grade under each wavelength its UV light absorption value (in the table 3 the 1st row) all greater than the standard value (the 3rd is capable in the table 3) of the residual level of farming, the product of purifying through the present invention after testing, its UV value (the 2nd row in the table 3) is all less than the standard value of the residual level of farming.
Test 4
The flame ionization ditector of gas-chromatography (GC-FID) detects
This experiment China National Instruments Import ﹠ Export Corporation device model: Agilent 6890,
Chromatographic column model: BP624 capillary column (the length 30m of Agilent company internal diameter 0.53mm thickness 3 μ m);
Sample size: 1 μ L, shunting in 50: 1; 40 ℃ of (5min) 10 ℃/min of column temperature, 260 ℃ (5min);
280 ℃ of 250 ℃ of detector temperatures of injector temperature;
Carrier gas: nitrogen (0.4MPa), hydrogen (0.3MPa);
Carrier gas column flow rate: 1ml/min.
Table 4 rectifying product the GC-ECD detected result
See Table 4 by the GC-ECD impurity detected result to product, 2 major impurity content wherein all are lower than the residual level of farming reagent standard.
Claims (8)
1. the method for preparing purified of the residual level of farming normal hexane is characterized in that:
Described method comprises that normal hexane carries out rectifying again behind bleaching agent bleaching, filtration makes the residual level of described farming normal hexane;
Described discoloring agent is the vitriol oil that has adsorbing gac, silicon-dioxide, polymer alumina or have the strong oxidizing property energy.
2. the method for preparing purified of the residual level of farming as claimed in claim 1 normal hexane is characterized in that:
A footpath median size of described gac, silicon-dioxide, polymer alumina is between the 50-150 micron, and specific surface area is 200-600m
2/ g;
The described vitriol oil is a mass percent concentration more than or equal to 70% aqueous sulfuric acid.
3. the method for preparing purified of the residual level of farming as claimed in claim 1 or 2 normal hexane is characterized in that:
The consumption of described discoloring agent is that the 1-50wt% bleaching time of normal hexane consumption is 3-24 hour.
4. the method for preparing purified of the residual level of farming as claimed in claim 3 normal hexane is characterized in that:
The consumption of described sorbent material class discoloring agent is the 5-20% of normal hexane consumption.
5. the method for preparing purified of the residual level of farming as claimed in claim 3 normal hexane is characterized in that:
Described gac, silicon-dioxide, polymer alumina use after 100-500 ℃ of baking recycled after 2-5 hour.
6. the method for preparing purified of the residual level of farming as claimed in claim 3 normal hexane is characterized in that described method comprises:
A) decolouring
The normal hexane raw material is entered from the decoloring reaction tank top, with discoloring agent reaction, reach described bleaching time after, the decoloring reaction pot liquid is divided into two-layer, discards dark lower floor solution, and supernatant liquid is introduced rectification step as raw material;
B) rectifying
Normal hexane raw material after decolouring is sent into the dehydrogenation tower, and dehydrogenation column overhead extraction light constituent is to the light constituent jar, and dehydrogenation Tata still extraction material is sent into rectifying tower;
Rectifying Tata still extraction heavy constituent are to the heavy constituent jar, rectifying tower cat head extraction normal hexane;
C) filter
The normal hexane of rectifying tower cat head extraction is sent in the filtration unit and is filtered, and obtains the residual level of described farming normal hexane.
7. the method for preparing purified of the residual level of farming as claimed in claim 6 normal hexane is characterized in that:
The height of described dehydrogenation tower is 1.0-10m, and internal diameter is 5-100cm, and inner stuffing is θ ring, structured packing or dumped packing;
The height of described rectifying tower is 1.0-10m, and internal diameter is 5-80cm, and inner stuffing is θ ring, structured packing or dumped packing.
8. the method for preparing purified of the residual level of farming as claimed in claim 6 normal hexane is characterized in that:
Filtering membrane in the described filtration unit is an organic phase, and the aperture of filtering membrane is 0.10-1.20 μ m.
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| CN104722266A (en) * | 2015-02-13 | 2015-06-24 | 濮阳市联众兴业化工有限公司 | Discoloring agent and method for discoloring five-carbon hexaalkane by using same |
| CN104744196A (en) * | 2013-12-31 | 2015-07-01 | 上海星可高纯溶剂有限公司 | Purifying method of high-purity organic solvent n-hexane |
| CN105085138A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of high-purity organic solvent n-hexane |
| CN105085137A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of high-purity organic solvent n-octane |
| CN105085139A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of high-purity organic solvent n-heptane |
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| CN107652155A (en) * | 2017-10-25 | 2018-02-02 | 广东工业大学 | A kind of method for producing the residual level n-hexane of agriculture |
| CN108017504A (en) * | 2018-01-26 | 2018-05-11 | 上海星可高纯溶剂有限公司 | The method of purification of n-hexane |
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| CN105085138A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of high-purity organic solvent n-hexane |
| CN105085137A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of high-purity organic solvent n-octane |
| CN105085139A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of high-purity organic solvent n-heptane |
| CN105085139B (en) * | 2014-05-16 | 2017-11-10 | 上海星可高纯溶剂有限公司 | The method of purification of organic solvent normal heptane |
| CN104722266A (en) * | 2015-02-13 | 2015-06-24 | 濮阳市联众兴业化工有限公司 | Discoloring agent and method for discoloring five-carbon hexaalkane by using same |
| CN106365943A (en) * | 2016-08-31 | 2017-02-01 | 中国船舶重工集团公司第七八研究所 | Preparation method of pesticide residue level benzene |
| CN106365943B (en) * | 2016-08-31 | 2019-02-12 | 中国船舶重工集团公司第七一八研究所 | A kind of preparation method of the residual grade benzene of agriculture |
| CN107652155A (en) * | 2017-10-25 | 2018-02-02 | 广东工业大学 | A kind of method for producing the residual level n-hexane of agriculture |
| CN108017504A (en) * | 2018-01-26 | 2018-05-11 | 上海星可高纯溶剂有限公司 | The method of purification of n-hexane |
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