CN102126907B - 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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- CN102126907B CN102126907B CN201010617923.3A CN201010617923A CN102126907B CN 102126907 B CN102126907 B CN 102126907B CN 201010617923 A CN201010617923 A CN 201010617923A CN 102126907 B CN102126907 B CN 102126907B
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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 the residual detection field of agriculture, further, relate to one and utilize discoloring agent, the normal hexane of technical grade purity is become can be used for the method for the residual level of the agriculture normal hexane of the residual detection of agriculture by decolouring rectifying purification.
Background technology
Food safety is not only related to human health and life security, and is related to the sustainable development of international trade and national economy and stablizing of society, and therefore food safety is the Major Strategic that international community and national governments face.The detection of food safety is mainly for the oxious component such as content of heavy metal in foods, pesticide residue.
Pesticide residue are the principal pollutant that affect agricultural product quality and safety.The trace standard of pesticide is to weigh the Main Basis 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 agriculture, but still faced problems, unsound as standard, limit standard and technological standard do not match, and mark product reagent dependence on import etc.
In the residual detection of agriculture, detection level is generally in ppt level (10
-12), analyze and belong to trace analysis.Meanwhile, during agriculture is residual, also contain homologue, isomer, degraded product, meta-bolites and conjugates of agricultural chemicals etc., component is very complicated, once detect sample generation trace contamination, just very likely makes detected result make a mistake.Therefore in reality detects, sample pretreatment process is very important, accounts for greatly 70% left and right of workload, and its object is exactly in order to remove and the simultaneous impurity of target compound, avoids trace contamination, reduces chromatogram Interference Peaks.
For solvent used in the residual detection of agriculture, strict requirement has all been done to it especially by food safety both domestic and external mechanism.Conventional solvent, by purity grade classification, comprising: chemical pure, and its principal constituent content is high, purity is higher, exists and disturbs impurity, is applicable to chemical experiment and synthesizing and purifying preparation; 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 is high, and quality index focuses on disturbing the impurity of chromatographic peak, and stratographic analysis is special.
And do not do clearly definition for the residual level of agriculture solvent.In general, in the residual examination criteria of agriculture of the states such as European Union, the U.S. and Japan, the residual level of the agriculture solvent that regulation is used, refer to the high neat solvent by this application Operability Testing, be solvent through extraction, concentrated after after gas-chromatography-electron capture detector/nitrogen phosphorous detector/flame photometric detector/mass spectrum (GC-ECD/NPD/FPD/MS) detects, require its impurity signal lower than ppb level agriculture residual standard thing signal.Take Nippon Standard as example, by concentrated 300 times of solvent to be measured, adopt GC-ECD to detect, solvent to be measured to 60min, requires the peak height of all impurity to be not more than the half of standard solvent γ-phenyl-hexachloride (4ng/mL) peak height in the half of γ-phenyl-hexachloride retention time.Therefore, the residual level of agriculture solvent is often more paid attention to the impact of solvent on detected result.
In the residual detection of agriculture, its detection means mostly is chromatogram, comprises gas-chromatography and liquid chromatography; The maximum solvent using is acetonitrile, normal hexane, ethyl acetate etc.Because the impurity Interference Peaks that the residual level of the agriculture solvent of domestic production contains is too much, the overwhelming majority does not reach the requirement of the residual detection of agriculture, the solvent that uses in domestic Nong Can testing laboratory, it is all almost the product of the chromatographically pure rank of offshore company's production, as the product of the offshore companies 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% conventionally, that is to say, the reduction of foreign matter content reaches 0.01% (10 conventionally
-4) level, not yet relate to 10
-12or the removal technique of the impurity of low levels more, this kind of technology obviously can not meet the purification requirement of the residual level of agriculture solvent.Because the purification technique of the residual level of agriculture solvent is the trade secret of Ge great 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 the residual testing requirement of agriculture, the invention provides the residual level of a kind of agriculture normal hexane method for preparing purified, the normal hexane product foreign matter content that adopts the method for the invention to make is less than 10
-12, can meet the requirement of farming residual analysis, and simple to operate, saving cost, be with a wide range of applications.
The object of this invention is to provide the method for preparing purified of the residual level of a kind of agriculture normal hexane.
Described method comprises that normal hexane carries out rectifying after bleaching agent bleaching again, filtration makes the residual level of described agriculture normal hexane.Normal hexane described in present method is normal hexane product all in prior art, comprises the raw materials such as technical grade, chemical pure, top grade are pure, chromatographically pure.
Discoloring agent used is strong adsorbing gac of the prior art, silicon-dioxide, polymer alumina, and particle median size is between 50-150 micron, and specific surface area is 200-600m
2/ g, also can adopt mass percent concentration to be more than or equal to 70% the vitriol oil as discoloring agent.
Because the residual level of agriculture is analyzed conventional gas-chromatography-electron capture detector GC-ECD as detection technique, and the feature of ECD is the impact that is subject to polar compound.Therefore select the discoloring agent strong to polar compound decolourising property, remove such impurity.This kind of discoloring agent is that gac of the prior art, silicon-dioxide, polymer alumina or mass percent concentration are more than or equal to 70% the vitriol oil, and consumption is little, and decolorizing efficiency is high,, and make the UV uv-absorbing significance in normal hexane be reduced to the residual level of agriculture index.The decoloring ability of discoloring agent and the size of its particle are inversely proportional to, and particle is less, and the impurity that can decolour is more; But the flowing time of stoste and its granular size are also inversely proportional to, and particle is less, can cause Flow of Goods and Materials overlong time, and the operating time is long.Therefore, through considering, the preferred discoloring agent granulometric range of the present invention is between 100-300 order, and particle median size is between 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, preferably 5-20%, and bleaching time is 3-24 hour;
After using, described gac, silicon-dioxide, polymer alumina recycle after 2-5 hour through 100-500 ℃ of baking.
Described method comprises:
A) decolouring
Normal hexane raw material is entered from decoloring reaction tank top, react decolouring with discoloring agent, reach after described bleaching time, decoloring reaction pot liquid is divided into two-layer, and supernatant liquid is introduced to rectification step as raw material;
B) rectifying
Normal hexane raw material after decolouring is sent into dehydrogenation tower, dehydrogenation column overhead extraction light constituent, and dehydrogenation tower tower reactor extraction material is sent into rectifying tower;
Tower bottom of rectifying tower extraction heavy constituent, rectifying tower tower top extraction normal hexane;
C) filter
The normal hexane of rectifying tower tower top extraction is sent in filtration unit and is filtered, and obtains the residual level of described agriculture normal hexane.
Concrete operations are as follows:
A, decolouring step:
Normal hexane is flowed into by decoloring reaction tank top, and after discoloring agent contact decolorization through loading in decoloring reaction tank, after bleaching time described in reaching, solution in decoloring reaction tank is divided into two-layer, discard lower floor's dark solution, supernatant liquor after decolouring is collected, and introduced in distillation system through volume pump.
B, rectification step:
Normal hexane after decolouring step, under normal pressure, is first introduced rectifying tower rectifying after dehydrogenation tower heating vaporization;
Certain embodiments: the material of dehydrogenation column overhead is successively after condensing reflux, and a part is back to dehydrogenation tower, another part is as product introduction light constituent tank; Tower reactor material after 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 reactor of described dehydrogenation tower is 2-5000 liter;
The control parameter area of the temperature of dehydrogenation tower, reflux ratio, flow velocity is:
Regulating the temperature of condensation cycle water is 0-25 ℃, start total reflux operation 0.5-3 hour, in the time that the temperature of dehydrogenation tower top reaches light constituent boiling point, in the present invention, dehydrogenation tower reflux ratio scope is 40-1, regulate reflux ratio to gather light constituent, tower reactor material enters rectifying tower as raw material through volume pump.
Rectifying: dehydrogenation tower tower reactor material enters after rectifying tower, after vaporization in rectifying tower, after overhead condensation refluxes, a part is back to rectifying tower, and another part is as product introduction products pot; Rectifying tower reactor 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 reactor of described rectifying tower is 2-5000 liter;
The control parameter area of the temperature of rectifying tower, reflux ratio, flow velocity is:
Regulating the temperature of condensation cycle water is 0-25 ℃, starts total reflux operation 0.5-3 hour, in the time that the temperature of rectifying tower top reaches normal hexane boiling point, in the present invention, reflux ratio scope is 40-1, by regulating reflux ratio to gather normal hexane component, from overhead extraction, tower reactor still raffinate pumps into heavy constituent tank.
C, filtration step:
The normal hexane product that rectifying tower tower top obtains is sent into and in filtration unit, is removed after filtering impurity and can obtain the residual level of described agriculture normal hexane;
Filtration unit can be the filtration unit conventionally adopting in prior art, and the filtering membrane in filtration unit is 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 domestic normal hexane, has made the normal hexane solvent of the residual level of agriculture by steps such as decolouring rectifying, and product foreign matter content falls in 10
-12, can meet the requirement of farming residual analysis, and simple to operate, cost-saving, there is market application foreground widely.
Accompanying drawing explanation
The method for preparing purified schematic diagram of the residual level of Fig. 1 agriculture of the present invention normal hexane
Description of reference numerals:
1-head tank 2-decoloring reaction tank 3-dehydrogenation tower 4-rectifying tower
5-light constituent tank 6-heavy constituent tank 7-filtration unit 8-products pot
Embodiment
Below in conjunction with embodiment, further illustrate the present invention.
Device parameter
1) decoloring reaction tank: 2000 liters of volumes.
Discoloring agent: silicon-dioxide high-efficiency decolorant (Qingdao meticulous silica gel Chemical Co., Ltd.), 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 raw material weight.
2) dehydrogenation tower: tower height 6m, tower internal diameter 80cm; Filler: structured packing.
Prolong be shaped as shell and tube, be highly 0.5m.
Dehydrogenation tower tower reactor: the heat-conducting oil furnace formula tower reactor of 2000 liters.
3) rectifying tower: tower height 6m, tower internal diameter 100cm; Filler: structured packing.
Prolong be shaped as shell and tube, be highly 0.5m.
Tower bottom of rectifying tower: the heat-conducting oil furnace formula tower reactor of 2000 liters.4) filtration unit: stainless steel filtering membrane, aperture is 0.22 μ m.
Flange with standard between all devices is connected with pipeline.
A decolouring
By 1500 liters of technical grade normal hexane (purity > 98%, SK company of Korea S) slowly pumped in decoloring reaction tank 2 by head tank 1, after fully mixing with 330 liters of silicon-dioxide high-efficiency decolorants, carry out decoloring reaction, bleaching time is 6 hours, collect the supernatant liquid after decolouring, as the raw material of dehydrogenation tower.
B distillation operation
Technical grade normal hexane after decolouring is pumped into dehydrogenation tower 3, regulating heat-conducting oil furnace temperature is 100 ℃, normal hexane raw material is in the 3 tower reactor heating vaporizations of dehydrogenation tower, in the time that the temperature of dehydrogenation tower 3 tower tops reaches light constituent boiling point (65-68 ℃), regulating the cooling temperature of water of condensation is 5 ℃, total reflux operation 1 hour, regulating reflux ratio is 8: 1, gathers light constituent to light constituent tank 5;
Dehydrogenation tower 3 tower reactor materials enter after rectifying tower 4, and after the interior vaporization of rectifying tower 4, after overhead condensation refluxes, a part is back to rectifying tower 4, and another part is as product introduction filtration unit 7; Tower reactor material enters heavy constituent tank 6.
Regulating tower bottom of rectifying tower heat-conducting oil furnace temperature is 100 ℃, remove the normal hexane raw material of light constituent in rectifying tower 4 tower reactor heating vaporizations, in the time that the temperature of rectifying tower 4 tower tops reaches normal hexane boiling point (68-70 ℃), regulating the cooling temperature of water of condensation is 5 ℃, total reflux operation 1 hour, regulating reflux ratio is 4: 1, gathers normal hexane crude product to products pot.
C filters
The normal hexane crude product of rectifying tower 4 overhead extractions enters in filtration unit 7, removes after filtering impurity and can obtain meeting the normal hexane of the residual level of agriculture index.
The residual level of agriculture ultraviolet absorptivity test index detects:
This experiment Instrumental model: 1901 series ultraviolet visible spectrophotometer, the quartz colorimetric utensil of 1mL.Open instrument preheating 30min, adopt and under different wave length, survey its absorbancy, making blank with distilled water or ultrapure water contrasts, detect the absorbancy index of each sample under 195nm, 210nm, 220nm, 230nm, 240nm and 250nm wavelength, the product detected result after this technology purification obtains 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 agriculture | ≤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 its UV light absorption value (the 1st row in table 1) under each wavelength is all greater than the standard value (the 3rd row in table 1) of the residual level of agriculture, after testing, its UV value (the 2nd row in table 1) is all less than the standard value of the residual level of agriculture to the product of purifying through this technological invention.
The flame ionization ditector (GC-FID) of gas-chromatography detects
This experiment Instrumental model: Agilent 6890,
Chromatographic column model: (the length 30m of Agilent company internal diameter 0.53mm thickness 3 μ m) for BP624 capillary column;
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 GC-ECD detected result
By the GC-ECD impurity detected result to product, in table 2,3 major impurity content are wherein all lower than 10
-12.
Device parameter
1) decoloring reaction tank: glass liquid distribution 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 raw material weight.
2) dehydrogenation tower: glass tower tower height 1.3m, tower internal diameter 10cm; Filler: θ ring filler.
Prolong is coil pipe type glass condenser.
Dehydrogenation tower tower reactor: the triangle round bottom glass flask of 3 liters, the heating of electrically heated pot.
3) rectifying tower: glass tower tower height 1.5m, tower internal diameter 10cm; Filler: θ ring filler.
Prolong is coil pipe type glass condenser.
Tower bottom of rectifying tower: the triangle round bottom glass flask of 3 liters, the heating of electrically heated pot.
4) filtration unit: glass solvent filter, filtering membrane aperture is 0.22 μ m.
Adapter glass with standard between all devices is connected with plastic hose.
A decolouring
2 liters of technical grade normal hexanes (purity > 98%, SK company of Korea S) are added in glass liquid distribution funnel 2, after adding 0.1 liter of vitriol oil fully to mix, carry out decoloring reaction, bleaching time is 24 hours, collects the supernatant liquid after decolouring, as the raw material of dehydrogenation tower.
B distillation operation
Technical grade normal hexane after decolouring is imported to dehydrogenation tower 3, regulate electrically heated pot voltage, slowly heating, normal hexane raw material is in the 3 tower reactor heating vaporizations of dehydrogenation tower, in the time that the temperature of dehydrogenation tower 3 tower tops reaches light constituent boiling point (65-68 ℃), regulating the cooling temperature of water of condensation is 5 ℃, total reflux operation 1.5 hours, regulating reflux ratio is 10: 1, gathers light constituent to light constituent tank 5.
Dehydrogenation tower 3 tower reactor materials enter after rectifying tower 4, and after the interior vaporization of rectifying tower 4, after overhead condensation refluxes, a part is back to rectifying tower 4, and another part is as product introduction filtration unit 7; Tower reactor material enters heavy constituent tank 6.
Regulate tower bottom of rectifying tower electrically heated pot voltage, remove the normal hexane raw material of light constituent in rectifying tower 4 tower reactor heating vaporizations, in the time that the temperature of rectifying tower 4 tower tops reaches normal hexane boiling point (68-70 ℃), regulating the cooling temperature of water of condensation is 5 ℃, total reflux operation 1.5 hours, regulating reflux ratio is 6: 1, gathers normal hexane crude product to products pot.
C filters
The normal hexane crude product of rectifying tower 4 overhead extractions enters in filtration unit 7, removes after filtering impurity and can obtain meeting the normal hexane of the residual level of agriculture index.
Test 3
The residual level of agriculture ultraviolet absorptivity test index detects:
This experiment Instrumental model: HITACHI U-3900, the quartz colorimetric utensil of 1mL.Open instrument preheating 30min, adopt and under different wave length, survey its absorbancy, making blank with distilled water or ultrapure water contrasts, detect the absorbancy index of each sample under 195nm, 210nm, 220nm, 230nm, 240nm and 250nm wavelength, the product detected result after this technology purification obtains 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 agriculture | ≤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 its UV light absorption value (the 1st row in table 3) under each wavelength is all greater than the standard value (the 3rd row in table 3) of the residual level of agriculture, after testing, its UV value (the 2nd row in table 3) is all less than the standard value of the residual level of agriculture to the product of purifying through the present invention.
Test 4
The flame ionization ditector (GC-FID) of gas-chromatography detects
This experiment Instrumental model: Agilent 6890,
Chromatographic column model: (the length 30m of Agilent company internal diameter 0.53mm thickness 3 μ m) for BP624 capillary column;
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 GC-ECD detected result
By the GC-ECD impurity detected result to product, in table 4,2 major impurity content are wherein all lower than the residual level of agriculture reagent standard.
Claims (2)
1. a method for preparing purified for the residual level of agriculture normal hexane, is characterized in that:
Described method comprises that normal hexane carries out rectifying after bleaching agent bleaching again, filtration makes the residual level of described agriculture normal hexane;
Described method comprises the steps:
A) decolouring
Normal hexane raw material is sent into from decoloring reaction tank top, reacted with discoloring agent, reach after described bleaching time, decoloring reaction pot liquid is divided into two-layer, discards dark lower floor solution, and supernatant liquid is sent into rectification step as raw material;
B) rectifying
Normal hexane after decolouring is sent into lightness-removing column, and lightness-removing column overhead extraction light constituent is to light constituent tank, and lightness-removing column tower reactor extraction material is sent into rectifying tower;
Tower bottom of rectifying tower extraction heavy constituent is to heavy constituent tank, rectifying tower tower top extraction normal hexane;
C) filter
The normal hexane of rectifying tower tower top extraction is sent in filtration unit and is filtered, and obtains the residual level of described agriculture normal hexane;
Described discoloring agent is the vitriol oil with strong oxidizing property energy;
The described vitriol oil is that mass percent concentration is more than or equal to 70% aqueous sulfuric acid;
The consumption of described discoloring agent is that the 1-50wt% bleaching time of normal hexane consumption is 3-24 hour;
The height of described lightness-removing column 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.
2. the method for preparing purified of the residual level of agriculture as claimed in claim 1 normal hexane, is characterized in that:
Filtering membrane in described filtration unit is organic phase, and the aperture of filtering membrane is 0.10-1.20 μ m.
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| CN104744196B (en) * | 2013-12-31 | 2017-11-10 | 上海星可高纯溶剂有限公司 | The method of purification of organic solvent-normal hexane |
| 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 |
| CN105085137B (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 octane |
| CN105085138B (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 hexane |
| 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 |
| 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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| CN101544531A (en) * | 2009-05-06 | 2009-09-30 | 天津市康科德科技有限公司 | Method for purifying high-purity organic solvent-normal hexane for scientific research |
| CN101747165A (en) * | 2009-08-21 | 2010-06-23 | 中国计量科学研究院 | Preparation method of pesticide-residue-level acetone |
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| CN101148390B (en) * | 2007-10-12 | 2010-11-24 | 中国石化扬子石油化工有限公司 | Technique for extracting high-pure normal hexane product by pressure swing adsorption |
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| CN101544531A (en) * | 2009-05-06 | 2009-09-30 | 天津市康科德科技有限公司 | Method for purifying high-purity organic solvent-normal hexane for scientific research |
| CN101747165A (en) * | 2009-08-21 | 2010-06-23 | 中国计量科学研究院 | Preparation method of pesticide-residue-level acetone |
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