CN107652155A - A kind of method for producing the residual level n-hexane of agriculture - Google Patents
A kind of method for producing the residual level n-hexane of agriculture Download PDFInfo
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- CN107652155A CN107652155A CN201711009130.1A CN201711009130A CN107652155A CN 107652155 A CN107652155 A CN 107652155A CN 201711009130 A CN201711009130 A CN 201711009130A CN 107652155 A CN107652155 A CN 107652155A
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- hexane
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- residual level
- oxidation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/005—Processes comprising at least two steps in series
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/12—Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
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- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Water Supply & Treatment (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of production method for producing the residual level n-hexane of agriculture, its technical scheme is, using technical grade n-hexane as raw material, to comprise the following steps：(1) oxidation-adsorption：Remove sulfur-containing compound a small amount of in raw material, unsaturated hydrocarbon and hydrocarbon impurities simultaneously；(2) rectifying：Remove heavy constituent, heavy seeds, moisture and light component of part etc. in material；(3) filter:Final finished is obtained using current conventional Millipore filtration techniques UF membrane；The residual level n-hexane of agriculture that purity is more than 99% is obtained after these steps, wherein indices meet the requirements.
Description
Technical field
The present invention relates to a kind of method for producing the residual level n-hexane of agriculture.
Background technology
Food-safety problem became one of most concerned problem of people in recent years, and food security is not only related to the mankind and is good for
Health and life security, and it is related to the stabilization of international trade and the sustainable development of national economy and society, therefore food security
It is the Major Strategic that international community and national governments face.Food security is mainly residual by detecting heavy metal in food, agricultural chemicals
The whether exceeded determination of harmful components such as stay.Residues of pesticides are to influence the major pollutants of agricultural product quality and safety, and weigh agricultural production
The Main Basiss of quality safety are residues of pesticides.Residues of pesticides are in international agriculture trade often by developed country as technology
The important means of property trade measure.Solvent used in the residual detection of agriculture, International Food Safety Control testing agency has done sternly to it
The requirement of lattice.Being usually used in the organic solvent of pesticide residue analysis mainly includes acetonitrile, ethyl acetate, acetone, n-hexane etc..Not only
Meet the conventional index such as higher purity and low UV absorption, it is often more important that after the solvent concentration tens to hundred times,
Interference Peaks are not produced in the chromatogram detection of agricultural chemicals.The residual level solvent of agriculture of domestic production at present contains more impurity Interference Peaks, absolutely
Most of requirements for not reaching the residual detection of agriculture still, solvent used in domestic Nong Can testing laboratories, the overwhelming majority rely on into
The HPLC level reagents of mouth, such as product of Merck, Fisher, J.T.Baker, HoneyWell offshore company, price are extremely high
It is expensive, a large amount of research fundings are not only expended, and national scientific research is limited by foreign countries with analysis detection relevant criterion.
N-hexane is one of industrial most widely used hydro carbons reagent, and most representational nonpolar examination at present
Agent.The n-hexane typically rectifying from direct steaming gasoline, reforming raffinate oil, Aromatic raffinate or moist natural gas obtains, wherein
Contain the impurity such as hydro carbons similar in boiling point and water.Because the boiling point of wherein impurity is close with n-hexane, impurity is removed very in rectifying
Difficulty, if using precise distillation and special extract rectification technique, high energy consumption again be present, production cost is high, and yield is low, and production process is multiple
The shortcomings of miscellaneous.The report on the residual level n-hexane production method of agriculture domestic at present is very few, and after most purifications product purity
Relatively low, cost is very high, complex technical process, and products obtained therefrom can not meet the needs of scientific research.Therefore, the life of the residual level n-hexane of agriculture
Production method requires further improvement.
The content of the invention
It is an object of the invention to from technical grade n-hexane, the sulfur-bearing chemical combination in raw material is removed using oxidation-adsorption agent
Thing, unsaturated hydrocarbon and with n-hexane boiling point similar in hydrocarbon impurities, and be converted into high-boiling components and some low boilings
Impurity, then by rectifying, further remove micro water in raw material, organic matter (unsaturated hydro carbons), ion (metal from
Son, acid ion) etc. impurity, finally by micro-pore-film filtration residual impurity therein, solve the residual level solvent of prior art middle peasant
Containing more impurity Interference Peaks, the problems such as purity does not reach agriculture residual testing requirements.
To realize object above, the present invention is achieved through the following technical solutions：
A kind of method for producing the residual level n-hexane of agriculture, described method are：Industrial n-hexane is first passed through into oxidation-adsorption agent
Remove a small amount of sulfur-containing compound in raw material, unsaturated hydrocarbon and with n-hexane boiling point similar in impurity, Ran Houtong
Cross rectifying and further remove the impurity such as a small amount of moisture in raw material n-hexane, organic matter, ion, removed finally by micro-pore-film filtration
Remaining impurity is gone to obtain finished product.
As present invention further optimization, a kind of production method of the residual level n-hexane of above-mentioned agriculture, this method is successively
Comprise the steps：
(1) oxidation-adsorption：By raw material n-hexane by being pumped into reactor, n-hexane quality 0.1%- is added in reactor
0.5% oxidation-adsorption agent, 69-71 DEG C of backflow 2h is heated to, obtains n-hexane 1.
(2) rectifying：The above-mentioned n-hexane 1 treated by oxidation-adsorption is steamed into atmospheric tower and carries out atmospheric distillation,
Rectifying is heated in the lightness-removing column that reflux temperature is 30.0-38 DEG C and takes off light component, is 70.0-78 DEG C of de- weight subsequently into reflux temperature
Rectifying is heated in tower and takes off heavy constituent；From overhead extraction material n-hexane to finishing column rectifying again, finishing column tower top pressure 0.05-
0.08Mpa, feeding temperature are 40.0-50 DEG C, and tower top temperature is 71.0 DEG C, reflux ratio 3.0, and reflux temperature is 70.0-78 DEG C,
Front-end volatiles are deviate from from gas phase, and tails is separated by bottom, and front and rear cut sends reaction system recycling back to.
(3) filter：The material of rectifying column extraction removes remaining miscellaneous by the filtration tank equipped with 0.2 μm of bore filter film again
Matter.
Further, the method for the residual level n-hexane of above-mentioned production agriculture, described oxidation-adsorption agent are potassium ferrate or high ferro
Sour sodium.
Further, the method for the residual level n-hexane of above-mentioned production agriculture, described micro porous filtration membrane aperture are 0.2-1 μm.
Further, the method for the residual level n-hexane of above-mentioned production agriculture, raw materials used n-hexane are technical grade, purity 95%
More than；
Further, the method for the residual level n-hexane of above-mentioned production agriculture, reactor used and destilling tower are enamel reaction dress
Put.
Compared with prior art, the n-hexane produced described in method provided by the invention, UV2550 carry out UV detections (1cm
Colorimetric pool, water do reference), at its 195nm absorbance between 0.6086~0.8076, at 210nm absorbance 0.1338~
Between 0.1803.GC detection (chromatogram column type numbers are carried out through Agilent 6820：HP-FFAP, column length 30m, internal diameter 0.53mm, liquid
1.0 μm of testing conditions of film thickness：Column temperature：40 DEG C of initial temperature is kept for 5 minutes, 10 DEG C/min rise to 220 DEG C after kept for 2 points
Clock；200 DEG C of injector temperature；250 DEG C of its contents of of detector temperature illustrate obtained by method provided by the invention more than 99.90%
The product purity arrived is high, and production method is simple.
Embodiment
The present invention is elaborated further with reference to specific embodiment, but not formed to any of the present invention
Limitation, the modification of anyone limited number of time made in the claims in the present invention protection domain are still protected in the claim of the present invention
Within the scope of shield.
Embodiment 1
A kind of production method of the residual level n-hexane of agriculture, its step are as follows：
(1) oxidation-adsorption：By raw material n-hexane by being pumped into reactor, oxidation-adsorption agent ferric acid is added in reactor
Potassium, the addition of oxidation-adsorption agent are the 0.1% of n-hexane quality, are heated to 69 DEG C of backflow 2h, obtain n-hexane 1.
(2) rectifying：Finally the above-mentioned n-hexane treated by oxidation-adsorption is steamed into atmospheric tower and carries out atmospheric distillation,
Rectifying is heated in the lightness-removing column that reflux temperature is 30.0 DEG C and takes off light component, is in 70.0 DEG C of weight-removing columns subsequently into reflux temperature
Heat rectifying and take off heavy constituent；From overhead extraction material n-hexane to finishing column rectifying again, finishing column tower top pressure 0.05Mpa,
Feeding temperature is 40.0 DEG C, and tower top temperature is 71.0 DEG C, and reflux ratio 3.0, reflux temperature is 70.0 DEG C, and front-end volatiles take off from gas phase
Go out, tails is separated by bottom, and front and rear cut sends reaction system recycling back to.
(3) filter：The material of rectifying column extraction removes remaining miscellaneous by the filtration tank equipped with 0.2 μm of bore filter film again
Matter.
(4) measure of farming residual analysis compound
The residual level criterion of agriculture:Gained sample is in addition to meeting chromatographic grade index, after 100 times of concentration, with GC-FID gas phases
Chromatograph, all miscellaneous peaks detected (with sec-n-octyl alcohol standard specimen ratio of peak compared with) low 5 μ g/L.With GC-ECD gas chromatographs, inspection
Measure all miscellaneous peaks (with Heptachlor epoxide standard specimen ratio of peak compared with) low 10ng/L.So through being refining to obtain it is high it is pure oneself
Alkane, just meet the residual level normal hexane product standard of agriculture.
(5) the residual Testing index of rectifying product agriculture:
Embodiment 2
A kind of production method of the residual level n-hexane of agriculture, its step are as follows：
(1) oxidation-adsorption：By raw material n-hexane by being pumped into reactor, oxidation-adsorption agent ferric acid is added in reactor
Sodium, the addition of oxidation-adsorption agent are the 0.3% of n-hexane quality, are heated to 70 DEG C of backflow 2h, obtain n-hexane 1.
(2) rectifying：Finally by it is above-mentioned by oxidation-adsorption treat n-hexane be transferred to rectifying column carry out rectifying, will just oneself
Alkane distillation gas phase is produced to rectifying column, and rectifying is heated in the lightness-removing column that reflux temperature is 35.0 DEG C and takes off light component, subsequently into
Reflux temperature is to heat rectifying in 74.0 DEG C of weight-removing columns to take off heavy constituent；It is smart again from overhead extraction material n-hexane to finishing column
Evaporate, finishing column tower top pressure 0.07Mpa, feeding temperature is 45.0 DEG C, and tower top temperature is 71.0 DEG C, reflux ratio 3.0, backflow temperature
Spend for 74.0 DEG C, front-end volatiles are deviate from from gas phase, and tails is separated by bottom, and front and rear cut sends reaction system recycling back to.
(3) filter：The material of rectifying column extraction removes remaining miscellaneous by the filtration tank equipped with 0.5 μm of bore filter film again
Matter.
(4) measure of farming residual analysis compound
The residual level criterion of agriculture:Gained sample is in addition to meeting chromatographic grade index, after 100 times of concentration, with GC-FID gas phases
Chromatograph, all miscellaneous peaks detected (with sec-n-octyl alcohol standard specimen ratio of peak compared with) low 5 μ g/L.With GC-ECD gas chromatographs, inspection
Measure all miscellaneous peaks (with Heptachlor epoxide standard specimen ratio of peak compared with) low 10ng/L.So through being refining to obtain it is high it is pure oneself
Alkane, just meet the residual level normal hexane product standard of agriculture.
(5) the residual Testing index of rectifying product agriculture:
Embodiment 3
A kind of production method of the residual level n-hexane of agriculture, its step are as follows：
(1) oxidation-adsorption：By raw material n-hexane by being pumped into reactor, oxidation-adsorption agent ferric acid is added in reactor
Potassium, the addition of oxidant are the 0.5% of n-hexane quality, are heated to 71 DEG C of backflow 3h, obtain n-hexane 1
(2) rectifying：Then the above-mentioned n-hexane treated by oxidation-adsorption is transferred to rectifying column afterwards and carries out rectifying, will just
Hexane distillation gas phase is produced to rectifying column, and rectifying is heated in the lightness-removing column that reflux temperature is 38.0 DEG C and takes off light component, Ran Houjin
Enter reflux temperature and take off heavy constituent to heat rectifying in 78.0 DEG C of weight-removing columns；It is smart again from overhead extraction material n-hexane to finishing column
Evaporate, finishing column tower top pressure 0.08Mpa, feeding temperature is 50.0 DEG C, and tower top temperature is 71.0 DEG C, reflux ratio 3.0, backflow temperature
Spend for 78.0 DEG C, front-end volatiles are deviate from from gas phase, and tails is separated by bottom, and front and rear cut sends reaction system recycling back to.
(3) filter：The material of rectifying column extraction removes residual impurity by the filtration tank equipped with 1 μm of bore filter film again.
(4) measure of farming residual analysis compound
The residual level criterion of agriculture:Gained sample is in addition to meeting chromatographic grade index, after 100 times of concentration, with GC-FID gas phases
Chromatograph, all miscellaneous peaks detected (with sec-n-octyl alcohol standard specimen ratio of peak compared with) low 5 μ g/L.With GC-ECD gas chromatographs, inspection
Measure all miscellaneous peaks (with Heptachlor epoxide standard specimen ratio of peak compared with) low 10ng/L.So through being refining to obtain it is high it is pure oneself
Alkane, just meet the residual level normal hexane product standard of agriculture.
(5) the residual Testing index of rectifying product agriculture:
Claims (6)
- A kind of 1. method for producing the residual level n-hexane of agriculture, it is characterised in that this method is：Industrial n-hexane is first passed through into oxidation to inhale Attached dose remove a small amount of sulfur-containing compound in raw material, unsaturated hydrocarbon and with n-hexane boiling point similar in impurity, so A small amount of moisture, organic matter, the ionic impurity in raw material n-hexane are further removed by rectifying afterwards, finally by micro-pore-film filtration Remove remaining impurity and obtain finished product.
- 2. the production method of the residual level n-hexane of a kind of agriculture according to claim 1, it is characterised in that this method includes successively Following step：(1) oxidation-adsorption：By raw material n-hexane by being pumped into reactor, n-hexane quality 0.1%- is added in reactor 0.5% oxidation-adsorption agent, 69-71 DEG C of backflow 2h is heated to, obtains n-hexane 1.(2) rectifying：The above-mentioned n-hexane 1 treated by oxidation-adsorption is steamed into atmospheric tower and carries out atmospheric distillation, is being flowed back Rectifying is heated in the lightness-removing column that temperature is 30.0-38 DEG C and takes off light component, is in 70.0-78 DEG C of weight-removing column subsequently into reflux temperature Heat rectifying and take off heavy constituent；From overhead extraction material n-hexane to finishing column rectifying again, finishing column tower top pressure 0.05- 0.08Mpa, feeding temperature are 40.0-50 DEG C, and tower top temperature is 71.0 DEG C, reflux ratio 3.0, and reflux temperature is 70.0-78 DEG C, Front-end volatiles are deviate from from gas phase, and tails is separated by bottom, and front and rear cut sends reaction system recycling back to.(3) filter：The material of rectifying column extraction removes residual impurity by the filtration tank equipped with 0.2 μm of bore filter film again.
- 3. the method for the production residual level n-hexane of agriculture according to claim 1 or claim 2, it is characterised in that described oxidation-adsorption agent It is potassium ferrate or Na2Fe04.
- 4. the method for the production residual level n-hexane of agriculture according to claim 1 or claim 2, it is characterised in that described micropore filtering film Aperture is 0.2-1 μm.
- 5. the method for the residual level n-hexane of agriculture is produced according to claim 1, it is characterised in that raw materials used n-hexane is industry Level, purity are more than 95%.
- 6. the method for the residual level n-hexane of agriculture is produced according to claim 1, it is characterised in that reactor and destilling tower used For enamel reaction unit.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711009130.1A CN107652155A (en) | 2017-10-25 | 2017-10-25 | A kind of method for producing the residual level n-hexane of agriculture |
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| CN201711009130.1A CN107652155A (en) | 2017-10-25 | 2017-10-25 | A kind of method for producing the residual level n-hexane of agriculture |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110668909A (en) * | 2019-10-23 | 2020-01-10 | 成都市科隆化学品有限公司 | Purification method of environment-friendly n-hexane |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6326156B2 (en) * | 1979-12-27 | 1988-05-28 | Nisshin Spinning | |
| CN101712588A (en) * | 2009-11-26 | 2010-05-26 | 安徽时联特种溶剂股份有限公司 | Method for preparing high-purity liquid chromatographic grade normal paraffin |
| CN102126907A (en) * | 2010-12-31 | 2011-07-20 | 中国计量科学研究院 | Method for preparing pesticide residue grade n-hexane by purifying |
| CN105085140A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of n-hexane for liquid chromatography-mass spectrometer |
| 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 |
-
2017
- 2017-10-25 CN CN201711009130.1A patent/CN107652155A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6326156B2 (en) * | 1979-12-27 | 1988-05-28 | Nisshin Spinning | |
| CN101712588A (en) * | 2009-11-26 | 2010-05-26 | 安徽时联特种溶剂股份有限公司 | Method for preparing high-purity liquid chromatographic grade normal paraffin |
| CN102126907A (en) * | 2010-12-31 | 2011-07-20 | 中国计量科学研究院 | Method for preparing pesticide residue grade n-hexane by purifying |
| CN105085140A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of n-hexane for liquid chromatography-mass spectrometer |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 陆晓华等: "《环境污染控制原理》", 28 February 2010, 华中科技大学出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110668909A (en) * | 2019-10-23 | 2020-01-10 | 成都市科隆化学品有限公司 | Purification method of environment-friendly n-hexane |
| CN110668909B (en) * | 2019-10-23 | 2022-03-01 | 成都市科隆化学品有限公司 | Purification method of environment-friendly n-hexane |
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