CN104744196B - The method of purification of organic solvent-normal hexane - Google Patents
The method of purification of organic solvent-normal hexane Download PDFInfo
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- CN104744196B CN104744196B CN201310754198.8A CN201310754198A CN104744196B CN 104744196 B CN104744196 B CN 104744196B CN 201310754198 A CN201310754198 A CN 201310754198A CN 104744196 B CN104744196 B CN 104744196B
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Abstract
The invention discloses a kind of method of purification of high-purity organic solvent-normal hexane, it is characterised in that removes the impurity in raw material n-hexane by processes such as modified active carbon adsorptions, obtains high-purity organic solvent-normal hexane.The method of purification of high-purity organic solvent-normal hexane provided by the invention, can obtain purity >=99%（wt）N-hexane, meet the high-purity requirement of chromatographic grade reagent, enable the fields such as the n-hexane that purification obtains is applied to chromatography, prepared by chromatographic isolation, chromatogram, expand application.
Description
Technical field
The present invention relates to solvent purifications field, more particularly to a kind of method of purification of high-purity organic solvent-normal hexane.
Background technology
N-hexane is one of widest varsol of purposes on present industrial, and most representational nonpolar molten
Agent, all kinds of hydro carbons and halogenated hydrocarbons can be dissolved, in edible oil, printing-ink, leather, agricultural chemicals, insecticide, rubber, cosmetics, perfume (or spice)
All many-sides such as material, chemical industry polymerization, medical and electronic unit cleaning have been widely used.At present industrially from natural vapour
Rectifying obtains the technical grade normal hexane product that purity is 60~80% (wt) in oil, direct steaming gasoline and light component, wherein containing boiling
The impurity such as hydro carbons and water similar in point.Due to the boiling point of impurity close with n-hexane (such as 69 DEG C of n-hexane boiling point, methyl cyclopentane
71.8 DEG C), want to improve the purity of n-hexane, it is difficult to realize impurity removing by conventional distillation.According to precise distillation
With special extract rectification technique, high energy consumption be present, production cost is high, and yield is low, and the shortcomings of production process complexity, this also results in China
High-purity n-hexane relies on import.The report on obtaining high-purity n-hexane by absorption purification domestic at present is very few, application
Number for 200910068762.4 patent disclose by zeolite adsorption purify n-hexane method, the n-hexane purity after purification
>=98% (wt), the purity can not still meet the high-purity requirement of industrial application, and method of purification need to be improved further.
The content of the invention
The invention aims to overcome deficiency of the prior art, there is provided a kind of to improve the organic of n-hexane purity
The method of purification of solvent hexane.
To realize object above, the present invention is achieved through the following technical solutions：
The method of purification of organic solvent-normal hexane, it is characterised in that comprise the following steps：
A. raw material n-hexane is taken, after adding potassium permanganate progress oxidation processes thereto, distills out n-hexane；For removing
Unsaturated hydrocarbons impurity in raw material n-hexane.
B. the above-mentioned n-hexane distilled out is passed through adsorbent post equipped with modified activated carbon and carries out adsorption treatment, for except
Remove the unsaturated organic compound of carbon-carbon double bonds, such as alkene, aromatic hydrocarbon etc.；Obtain the high-purity organic of purity >=99% (wt)
Solvent hexane.Because carbon-carbon double bond is the group of absorbable ultraviolet-visible, so removing the organic compound of carbon-carbon double bonds
The n-hexane translucent effect of thing is also improved.
Preferably, the oxidant includes potassium permanganate or peroxide.Wherein, peroxide included but is not limited to
Hydrogen oxide.
Preferably, in the step a, add before oxidant, sulfuric acid is added into raw material n-hexane, shaking, is stood
After layering, water layer is discarded, retains organic layer.
Preferably, the volumetric concentration of the sulfuric acid is 10%.
Preferably, in the step a, add before oxidant, activated carbon, stirring 1~2 are added into raw material n-hexane
Hour.Raw material n-hexane is attached to activated carbon surface, increase the contact surface of potassium permanganate or peroxide and raw material n-hexane
Product.
Preferably, in the step a, after adding oxidant, flow back 0.5~3 hour.
Preferably, in the step b, modified activated carbon is that surface attachment has aluminium hydroxide, zinc hydroxide, ethylenediamine tetraacetic
One kind or any several activated carbon in acetic acid, triethanolamine, nitric acid.
Preferably, in addition to step b ˊ, the n-hexane obtained by the step b is passed through into the adsorbent equipped with molecular sieve
Post, for removing moisture.
Preferably, in addition to step b 〞, by the n-hexane obtained by the step b by the adsorbent post equipped with silica gel,
For removing alkane and fragrant hydrocarbon impurity.
Preferably, in addition to step c, the n-hexane obtained by adsorption treatment is subjected to rectifying；Rectifying still heating-up temperature is
100~200 DEG C, n-hexane fluid temperature is 70~90 DEG C in kettle, to go out liquid temperature degree be 67~69 DEG C, control reflux ratio be 1: 4~
5。
The method of purification of organic solvent-normal hexane provided by the invention, purity is obtained by the process of modified active carbon adsorption
>=99% (wt) high-purity solvent hexane, compared with the n-hexane of domestic production, purity further improves, make that purification obtains just oneself
Alkane can be applied to the fields such as chromatography, chromatographic isolation, chromatogram preparation, expand application.In addition, compared with precise distillation and
Special extract rectification technique, method of purification provided by the invention, yield >=95%, high income, energy consumption are low, production cost is low, produced
Journey is easy, it is stable, suitable for industrialized production.
Embodiment
The present invention is described in detail with reference to embodiment：
Embodiment 1
The method of purification of organic solvent-normal hexane, comprises the following steps：
A. raw material n-hexane is taken, adds the sulfuric acid that volumetric concentration is 10% thereto, shakes, after stratification, discards acid
Layer, retain organic layer；Activated carbon is added in above-mentioned organic layer, after stirring 1 hour, addition potassium permanganate is aoxidized, and is returned
Stream distills out rapidly n-hexane after 1 hour.
B. n-hexane step a obtained, by the adsorbent post equipped with modified activated carbon, is further removed and contained with speed
There are the unsaturated organic compound of carbon-carbon double bond, such as aromatic hydrocarbon, alkene.Wherein activated carbon is immersed in salpeter solution, made
Activated carbon surface adheres to salpeter solution, so as to obtain modified activated carbon.
The obtained n-hexanes of step b are passed through the adsorbent post equipped with molecular sieve by b ˊ, further remove moisture；After absorption, just
Hexane water content control is ≤0.01%；In this step the moisture after extraction in n-hexane, such as moisture are removed using molecular sieve
Content ＞ 0.03% is further continued for carrying out molecular sieve adsorption processing after need to changing molecular sieve.
The obtained n-hexanes of step b ˊ are passed through the adsorbent post equipped with silica gel by b 〞, further remove alkane and aromatic hydrocarbon
The impurity such as impurity.
C. the n-hexane obtained by step b 〞 is subjected to rectifying, rectifying still heating-up temperature is 100 DEG C, n-hexane liquid temperature in kettle
Spend for 70 DEG C, go out liquid temperature degree and be 67 DEG C, control reflux ratio to be 1: 4.Bottled after smart distillate detection is qualified, inflated with nitrogen preserves, i.e.,
Obtain the high-purity organic solvent-normal hexane of purity >=99%.
Embodiment 2
The method of purification of organic solvent-normal hexane, comprises the following steps：
A. raw material n-hexane is taken, adds the sulfuric acid that volumetric concentration is 10% thereto, shakes, after stratification, discards acid
Layer, retain organic layer；Activated carbon is added in above-mentioned organic layer, after stirring 2 hours, addition potassium permanganate is aoxidized, and is returned
Stream distills out rapidly n-hexane after 3 hours.
B. n-hexane step a obtained, by the adsorbent post equipped with modified activated carbon, is further removed and contained with speed
There are the unsaturated organic compound of carbon-carbon double bond, such as aromatic hydrocarbon, alkene.Activated carbon is wherein immersed in the second two of liquid successively
In amine tetraacethyl and triethanolamine, make activated carbon attachment ethylenediamine tetra-acetic acid and triethanolamine, so as to obtain modified activated carbon.
The n-hexane that b ˊ obtain step b, by the adsorbent post equipped with molecular sieve, further removes moisture with speed；Inhale
Attached, n-hexane water content control is ≤0.01%；The moisture after extraction in n-hexane is removed using molecular sieve in this step,
It is further continued for carrying out molecular sieve adsorption processing after need to changing molecular sieve such as moisture ＞ 0.03%.
The n-hexane that b 〞 obtain step b ˊ with speed by the adsorbent post equipped with silica gel, further remove alkane and
The impurity such as fragrant hydrocarbon impurity.
C. the n-hexane obtained by step b 〞 is subjected to rectifying, rectifying still heating-up temperature is 200 DEG C, n-hexane liquid temperature in kettle
Spend for 90 DEG C, go out liquid temperature degree and be 69 DEG C, control reflux ratio to be 1: 5.Bottled after smart distillate detection is qualified, inflated with nitrogen preserves, i.e.,
Obtain the high-purity organic solvent-normal hexane of purity >=99%.
Embodiment 3
The method of purification of organic solvent-normal hexane, comprises the following steps：
A. raw material n-hexane is taken, adds the sulfuric acid that volumetric concentration is 10% thereto, shakes, after stratification, discards acid
Layer, retain organic layer；Activated carbon is added in above-mentioned organic layer, after stirring 1.5 hours, addition potassium permanganate is aoxidized, and
After backflow 0.5 hour, n-hexane is distilled out rapidly.
B. n-hexane step a obtained, by the adsorbent post equipped with modified activated carbon, is further removed and contained with speed
There are the unsaturated organic compound of carbon-carbon double bond, such as aromatic hydrocarbon, alkene.It is molten that activated carbon is wherein immersed in zinc hydroxide successively
In liquid, activated carbon is set to adhere to zinc hydroxide solution, so as to obtain modified activated carbon.
The n-hexane that b ˊ obtain step b, by the adsorbent post equipped with molecular sieve, further removes moisture with speed；Inhale
Attached, n-hexane water content control is ≤0.01%；The moisture after extraction in n-hexane is removed using molecular sieve in this step,
It is further continued for carrying out molecular sieve adsorption processing after need to changing molecular sieve such as moisture ＞ 0.03%；
The n-hexane that b 〞 obtain step b ˊ with speed by the adsorbent post equipped with silica gel, further remove alkane and
The impurity such as fragrant hydrocarbon impurity.
C. the n-hexane obtained by step b 〞 is subjected to rectifying, rectifying still heating-up temperature is 150 DEG C, n-hexane liquid temperature in kettle
Spend for 80 DEG C, go out liquid temperature degree and be 68 DEG C, control reflux ratio to be 1: 4.5.To be bottled after smart distillate detection is qualified, inflated with nitrogen preserves,
Produce the high-purity organic solvent-normal hexane of purity >=99%.
Embodiment 4
The method of purification of organic solvent-normal hexane, comprises the following steps：
A. raw material n-hexane is taken, adds the sulfuric acid that volumetric concentration is 10% thereto, shakes, after stratification, discards acid
Layer, retain organic layer；Activated carbon is added in above-mentioned organic layer, after stirring 1 hour, addition potassium permanganate is aoxidized, and is returned
Stream distills out rapidly n-hexane after 1.5 hours.
B. n-hexane step a obtained, by the adsorbent post equipped with modified activated carbon, is further removed and contained with speed
There are the unsaturated organic compound of carbon-carbon double bond, such as aromatic hydrocarbon, alkene.It is molten that activated carbon is wherein immersed in sodium hydroxide successively
In liquid, activated carbon is set to adhere to sodium hydroxide solution, so as to obtain modified activated carbon.
The n-hexane that b ˊ obtain step b, by the adsorbent post equipped with molecular sieve, further removes moisture with speed；Inhale
Attached, n-hexane water content control is ≤0.01%；The moisture after extraction in n-hexane is removed using molecular sieve in this step,
It is further continued for carrying out molecular sieve adsorption processing after need to changing molecular sieve such as moisture ＞ 0.03%；
The n-hexane that b 〞 obtain step b ˊ with speed by the adsorbent post equipped with silica gel, further remove alkane and
The impurity such as fragrant hydrocarbon impurity.
C. the n-hexane obtained by step b 〞 is subjected to rectifying, rectifying still heating-up temperature is 180 DEG C, n-hexane liquid temperature in kettle
Spend for 85 DEG C, go out liquid temperature degree and be 68 DEG C, control reflux ratio to be 1: 5.Bottled after smart distillate detection is qualified, inflated with nitrogen preserves, i.e.,
Obtain the high-purity organic solvent-normal hexane of purity >=99%.
The technical indicator of high-purity organic solvent-normal hexane after the purification of embodiment 1~4 is as shown in Table 1：
Table one
Embodiment in the present invention is only used for that the present invention will be described, and is not construed as limiting the scope of claims limitation,
Other substantially equivalent replacements that those skilled in that art are contemplated that, all fall in the scope of protection of the present invention.
Claims (9)
1. the method for purification of organic solvent-normal hexane, it is characterised in that comprise the following steps：
A. raw material n-hexane is taken, oxidant is added thereto and stirs, heating distills out n-hexane；
B. the above-mentioned n-hexane distilled out is passed through adsorbent post equipped with modified activated carbon and carries out adsorption treatment, obtain purity >=
99% (wt) high-purity organic solvent-normal hexane；
In the step b, modified activated carbon is that surface attachment has aluminium hydroxide, zinc hydroxide, ethylenediamine tetra-acetic acid, triethanolamine
In one kind or any several activated carbon.
2. the deduction method of organic solvent-normal hexane according to claim 1, it is characterised in that the oxidant includes height
Potassium manganate or peroxide.
3. the deduction method of organic solvent-normal hexane according to claim 1, it is characterised in that in the step a, add
Before oxidant, sulfuric acid is added into raw material n-hexane, is shaken, after stratification, is discarded acid layer, retain having dissolved with n-hexane
Machine layer.
4. the method for purification of organic solvent-normal hexane according to claim 3, it is characterised in that the volume of the sulfuric acid is dense
Spend for 10%.
5. the method for purification of organic solvent-normal hexane according to claim 1, it is characterised in that in the step a, add
Before oxidant, activated carbon is added into raw material n-hexane, is stirred 1~2 hour.
6. the deduction method of organic solvent-normal hexane according to claim 1, it is characterised in that in the step a, add
After oxidant, flow back 0.5~3 hour.
7. the method for purification of organic solvent-normal hexane according to claim 1, it is characterised in that, will also including step b ˊ
N-hexane obtained by the step b passes through the adsorbent post equipped with molecular sieve.
8. the method for purification of organic solvent-normal hexane according to claim 1, it is characterised in that, will also including step b 〞
N-hexane obtained by the step b passes through the adsorbent post equipped with silica gel.
9. the method for purification of the organic solvent-normal hexane according to any of the above-described claim, it is characterised in that also include
Step c, the n-hexane obtained by adsorption treatment is subjected to rectifying；Rectifying still heating-up temperature is 100~200 DEG C, n-hexane liquid in kettle
It is 67~69 DEG C that temperature, which is 70~90 DEG C, goes out liquid temperature degree, controls reflux ratio to be 1: 4~5.
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| CN106278783A (en) * | 2016-08-17 | 2017-01-04 | 太仓沪试试剂有限公司 | A kind of purification process of normal hexane |
| CN107353178B (en) * | 2017-06-26 | 2020-08-11 | 江苏南大光电材料股份有限公司 | Preparation method of ultra-pure carbon tetrachloride |
| CN107501031A (en) * | 2017-08-29 | 2017-12-22 | 湖北工程学院 | A kind of chromatographically pure n-hexane and preparation method thereof, production system |
| CN110713429B (en) * | 2019-10-29 | 2022-05-03 | 天津康科德医药化工有限公司 | Method for purifying chromatographically pure hexane |
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