CN105085184B - The method of purification of liquid chromatograph-mass spectrometer isopropanol - Google Patents
The method of purification of liquid chromatograph-mass spectrometer isopropanol Download PDFInfo
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Abstract
The invention discloses a kind of methods of purification of liquid chromatography mass combined instrument isopropanol, which is characterized in that removes the impurity in raw material isopropanol by processes such as modified active carbon adsorptions, obtains liquid chromatography mass combined instrument isopropanol.The method of purification of liquid chromatography mass combined instrument isopropanol provided by the invention, the isopropanol of purity >=99.99% (wt) can be obtained, meet the high-purity requirement of liquid chromatography mass combined instrument, so that the isopropanol that purification obtains is can be applied to liquid chromatography mass combined instrument field, expands application range.
Description
Technical field
The present invention relates to solvent purifications field, more particularly to a kind of purification of liquid chromatograph-mass spectrometer isopropanol
Method.
Background technology
The on-line coupling of chromatography-mass spectroscopy combines the separating capacity of chromatography with mass spectrographic qualitative function, realizes to multiple
Miscellaneous mixture is more accurately qualitatively and quantitatively analyzed.And the pretreatment process of sample is also simplified, keep sample analysis easier.
Chromatograph-mass spectrometer coupling includes gas chromatography-mass spectrography and liquid chromatography mass combination, and LC-MS is mended each other with gas chromatography mass spectrometry
It fills, analyzes compound of different nature.
Liquid chromatography mass combined instrument (liquid Chromatograph Mass Spectrometer), abbreviation LC-MS,
It is the high end instrument in Analysis of Organic Substances market.Liquid chromatogram (LC) can be effectively by the organic matter in organic matter sample to be tested
Ingredient separates, and mass spectrum (MS) can analyze separated organic matter one by one, obtains organic matter molecular mass, structure and concentration
Etc. information.LC-MS is Analysis of Organic Substances laboratory, drug, Food Inspection room, and the departments such as production process control, quality inspection must can not
Few analysis tool.Need to use mobile phase in LC and separate organic components, common mobile phase be methanol, isopropanol,
The mixture of water and their different proportions.As the solvent of mobile phase, purity is higher, and organic matter separating effect is better in sample,
And the high solvent of purity can be avoided as much as the measured object caused by the presence of impurity and ionize insufficient phenomenon, especially
It is metal ion, is complexed with measured object in mass spectral analysis, Interference Peaks is produced in mass spectrum, so as to cause to ginsengs such as molecular weight
Several measurement causes to judge by accident, greatly reduces the precision of liquid chromatograph-mass spectrometer measurement result.
Isopropanol can dissolve a variety of organic and inorganic and gaseous matter, but its purification ten as a kind of solvent of function admirable
Divide difficulty.The preparation method of China's isopropanol liquid phase chromatorgaphy reagent seldom has been reported that, and the yield of domestic isopropanol is relatively low, pure
Degree is not also high, and high-purity isopropanol relies on import mostly, causes cost higher, and it is larger to be restrained degree by foreign technology.It is domestic
The patent for having high-purity isopropanol, application No. is give a kind of adding salt extraction-azeotropic distillation in 99119158.7 patent to combine
The method of journey refining isopropanol, this method take extraction plus the technique saltoutd purification isopropanol, and this method is only thick purifying technique,
After purification.So it is particularly urgent to develop a kind of method of isopropanol purification.
Also there is the patent of high-purity isopropanol in the country, and a kind of adding salt extraction-azeotropic distillation connection is given in patent CN1249294A
The method of conjunction process refining isopropanol, it is only thick purification that this method, which takes extraction plus the technique saltoutd purification isopropanol, this method,
Technique, the purity ＞ 99.5 (wt) after purification, the purity cannot still reach the high-purity requirement of chromatographic grade reagent, and method of purification needs
It is further improved.
Invention content
Purpose of the invention is to overcome the shortcomings in the prior art, provides a kind of liquid phase that isopropanol purity can be improved
The method of purification of chromatograph-mas spectrometer isopropanol.
In order to achieve the above object, the invention is realized by the following technical scheme：
The method of purification of liquid chromatograph-mass spectrometer isopropanol, which is characterized in that include the following steps：
A. raw material isopropanol is taken, potassium permanganate or peroxide are added thereto and is stirred, isopropanol is distilled out, removal is former
Expect isopropanol in the impurity containing double bond for example ethylene, acrylonitrile, hydrogen cyanide, methacrylaldehyde, methacrylonitrile, propenyl, oxazoles,
The impurity such as acetamide.Wherein, peroxide includes but not limited to hydrogen peroxide.
B. alkali metal oxide (including but not limited to sodium oxide molybdena), alkali gold are added in the isopropanol distilled out into step a
Belong to hydroxide (include but not limited to sodium hydroxide) or carbonate (include but not limited to sodium carbonate, sodium bicarbonate, potassium carbonate,
Saleratus), pH value is adjusted in the range of 7~8；Shaking, makes alkali metal oxide, alkali metal hydroxide or carbonate
It is fully reacted with the acid impurities in raw material isopropanol, produces precipitation of salts object；After stratification, discard water layer, and to dissolved with
The organic layer of isopropanol is filtered, and retains filtrate；
C. above-mentioned filtrate is passed through the adsorbent column equipped with modified activated carbon and carries out adsorption treatment, for removing oxidation process
The substance of the high degree of polarization of middle formation and the unsaturated organic compound of carbon-carbon double bonds etc..
D. by the isopropanol obtained by step b with the flow velocity of 0.5~30 column volume/hour be passed through equipped with grain size be 0.01~
The adsorbent column of the ion exchange resin of 0.2cm carries out ion-exchange treatment, the impurity such as removal aldehydes, metal ion to get to
The liquid chromatograph-mass spectrometer isopropanol of purity >=99.99% (wt).
Preferably, in the step a, potassium permanganate is added or while peroxide, highly basic and alkaline oxygenated is added
Object slows down the oxidisability of potassium permanganate such as sodium hydroxide and calcium oxide, while neutralizing the acidic materials that oxidation generates, and adjusts pH
Value is in 8~14 ranges.
Preferably, it in the step a, is added before potassium permanganate or peroxide, is added into raw material isopropanol more
Hole substance such as zeolite, molecular sieve, activated carbon etc. stirs 1~2 hour, and raw material isopropanol is made to be attached to activated carbon surface, increases high
The contact area of potassium manganate or peroxide and raw material isopropanol improves oxidation efficiency.Oxidizer can be reduced simultaneously, is reduced
Isopropanol is lost, and improves isopropanol yield.
Preferably, further include step a ˊ, reducing agent will be added into the isopropanol obtained by step a and stir, distill out
Isopropanol；The reducing agent is ferrous sulfate, niter cake, sodium hydrogensulfite, disodium hydrogen phosphate, ferrous oxide or bicarbonate
Sodium.The excess oxide generated in removal oxidation process.
Preferably, in the step c, modified activated carbon is that ethylenediamine tetra-acetic acid, aluminium oxide, hydroxide are adhered in surface
The activated carbon of aluminium, nitric acid, triethanolamine or hypochlorite.Ethylenediamine tetra-acetic acid, aluminium hydroxide, nitric acid, triethanolamine or secondary chlorine
The mass concentration of acid salt solution is 5~30%；The grain size of activated carbon is 20~100 mesh.
Preferably, in the step c, filtrate is passed through before the adsorbent column equipped with modified activated carbon, is first passed through and is equipped with
Grain size be 20~100 mesh, model 3A or 4A molecular sieve adsorbent column, remove moisture removal.
Preferably, isopropanol flows through the adsorbent column equipped with molecular sieve with the speed of 0.5~30 column volume/hour.
Preferably, in the step c, by the isopropanol after modified active carbon adsorption be passed through equipped with grain size be 20~
The adsorbent column of the aluminium oxide of 200 mesh removes peroxide and aldoketones impurity.
Preferably, isopropanol flows through the adsorbent column equipped with aluminium oxide with the speed of 0.5~30 column volume/hour.
Preferably, in the step d, the surface of ion exchange resin is attached with alcohol compound or acetonitrile；The alcohol
Class includes but not limited to methanol.
Preferably, further include step e, the isopropanol obtained by adsorption treatment is subjected to rectifying；Rectifying still heating temperature is
84~95 DEG C, 84~88 DEG C of isopropyl alcohol liquid temperature in kettle, distill out liquid temperature be 81~83 DEG C, control reflux ratio 10: 1~
20:1, infinite reflux 2~3 hours.
The method of purification of liquid chromatograph-mass spectrometer isopropanol provided by the invention, after potassium permanganate oxidation,
Modified active carbon adsorption and ion exchange resin carry out ion exchange and obtain the isopropanol of purity >=99.99% (wt), meet
The high-purity requirement of liquid chromatograph-mass spectrometer, makes the isopropanol that purification obtains can be applied to liquid chromatograph mass spectrography
Instrument field, expands application range.Method of purification provided by the invention has filled up the production blank of domestic high-purity isopropanol,
Cost needed for import is reduced, while alleviating the degree restrained by foreign technology.Method of purification provided by the invention also has
The advantages that low energy consumption, production process is easy, stable, suitable for industrialized production.
Specific implementation mode
The present invention is described in detail with reference to embodiment：
Embodiment 1
The method of purification of LC-MS analysis isopropanol, which is characterized in that include the following steps：
A. raw material isopropanol is taken, potassium permanganate is added thereto and carries out oxidation processes, removes such as second of the impurity containing double bond
The impurity such as alkene, acrylonitrile, hydrogen cyanide, methacrylaldehyde, methacrylonitrile, propenyl, oxazoles, acetamide.The same of potassium permanganate is added
When, sodium hydroxide and calcium oxide is added, slows down the oxidisability of potassium permanganate, while neutralizing the acidic materials that oxidation generates, adjusts
PH value is 8.After oxidation processes, isopropanol is distilled out rapidly.
A ˊ reducing agent ferrous oxide will be added into the isopropanol obtained by step a and stir, and distill out isopropanol.
B. sodium carbonate is added into the isopropanol distilled out, the pH of solution is adjusted to 7, and shaking makes sodium carbonate and raw material
Acid impurities in isopropanol fully react, and generate precipitation of salts object；Stratification discards water layer and precipitation, filters organic layer,
Retain filtrate.
C. above-mentioned filtrate is passed through the absorption equipped with the 3A molecular sieves that grain size is 50 mesh with the speed of 0.5 column volume/hour
Agent column further removes the moisture in organic layer；After absorption, aqueous isopropyl alcohol amount is controlled≤0.03%；It is utilized in this step
Molecular sieve removes moisture after extraction in isopropanol, is further continued for after molecular sieve point as moisture ＞ 0.03% is needed to change
Son sieve adsorption treatment；
And then, above-mentioned efflux is passed through with the speed of 24 column volumes/hour and is attached with ethylenediamine tetrem equipped with surface
The adsorbent column of the modified activated carbon of acid solution carries out adsorption treatment, for removing oxide-based, arene, polar compound
The impurity such as the unsaturated organic compound of class and carbon-carbon double bonds such as heterocyclic arene.Wherein, the grain size of activated carbon is 20 mesh, second
The mass concentration of ethylenediamine tetraacetic acid (EDTA) solution is 5%；
Finally, above-mentioned efflux is passed through the suction equipped with the aluminium oxide that grain size is 200 mesh with the speed of 10 column volumes/hour
Attached dose of column, for removing peroxide and aldoketones impurity.
D. by the isopropanol obtained by step c with the speed of 0.5 column volume/hour be passed through equipped with surface be attached with methanol from
The adsorbent column of sub-exchange resin, the impurity such as removal aldehydes, metal ion.It avoids metal ion in mass spectral analysis and is measured
Object is complexed and produces Interference Peaks, improves the precision of liquid chromatograph-mass spectrometer measurement result.The grain of ion exchange resin
Diameter is 0.2cm.
E. the isopropanol obtained by step c is subjected to rectifying to get to the liquid chromatography-mass spectrography of purity >=99.99% (wt)
Combined instrument isopropanol.
Known manner progress can be used in rectifying.A kind of preferred embodiment of the present invention is that rectifying still heating temperature is 84 DEG C, kettle
84 DEG C of middle isopropyl alcohol liquid temperature, distill out liquid temperature be 82 DEG C, control reflux ratio 10: 1, infinite reflux 3 hours.Smart distillate inspection
It bottles after surveying qualification, inflated with nitrogen preserves.
Embodiment 2
The method of purification of LC-MS analysis isopropanol, which is characterized in that include the following steps：
A. raw material isopropanol is taken, potassium permanganate is added thereto and carries out oxidation processes, removes such as second of the impurity containing double bond
The impurity such as alkene, acrylonitrile, hydrogen cyanide, methacrylaldehyde, methacrylonitrile, propenyl, oxazoles, acetamide.The same of potassium permanganate is added
When, sodium hydroxide and calcium oxide is added, slows down the oxidisability of potassium permanganate, while neutralizing the acidic materials that oxidation generates, adjusts
PH value is 14.After oxidation processes, isopropanol is distilled out rapidly.
A ˊ reducing agent niter cake will be added into the isopropanol obtained by step a and stir, and distill out isopropanol.
B. potassium hydroxide is added into the above-mentioned isopropanol distilled out, the pH of solution is adjusted to 8, and shaking makes hydroxide
Potassium is fully reacted with the acid impurities in raw material isopropanol, generates precipitation of salts object；Stratification discards water layer and precipitation, mistake
Organic layer is filtered, filtrate is retained.
C. filtrate is passed through the adsorbent column equipped with the 3A molecular sieves that grain size is 20 mesh with the speed of 30 column volumes/hour,
Further remove the moisture in organic layer；After absorption, aqueous isopropyl alcohol amount is controlled≤0.03%；Molecular sieve is utilized in this step
The moisture after extraction in isopropanol is removed, is further continued for carrying out molecular sieve suction after needing to change molecular sieve such as moisture ＞ 0.03%
Attached processing；
And then, above-mentioned efflux is passed through to be attached with hypochlorite equipped with surface molten with the speed of 0.5 column volume/hour
The adsorbent column of the modified activated carbon of liquid carries out adsorption treatment, for remove oxide-based, arene, polar compounds species with
And the impurity such as the unsaturated organic compound of carbon-carbon double bonds such as heterocyclic arene.Wherein, the grain size of activated carbon is 100 mesh, secondary chlorine
The mass concentration of acid salt solution is 30%；
Finally, above-mentioned efflux is passed through with the speed of 0.5 column volume/hour equipped with the aluminium oxide that grain size is 100 mesh
Adsorbent column, for removing peroxide and aldoketones impurity.
D. by the isopropanol obtained by step c with the speed of 30 column volumes/hour be passed through equipped with surface be attached with methanol from
The adsorbent column of sub-exchange resin, the impurity such as removal aldehydes, metal ion.It avoids metal ion in mass spectral analysis and is measured
Object is complexed and produces Interference Peaks, improves the precision of liquid chromatograph-mass spectrometer measurement result.The grain of ion exchange resin
Diameter is 0.17cm.
E. the isopropanol obtained by step d is subjected to rectifying to get to the liquid chromatography-mass spectrography of purity >=99.99% (wt)
Combined instrument isopropanol.
Known manner progress can be used in rectifying.A kind of preferred embodiment of the present invention is that rectifying still heating temperature is 95 DEG C, kettle
86 DEG C of middle isopropyl alcohol liquid temperature, distill out liquid temperature be 82.4 DEG C, control reflux ratio 15: 1, infinite reflux 2 hours.Smart distillate
It bottles after detection is qualified, inflated with nitrogen preserves.
Embodiment 3
The method of purification of LC-MS analysis isopropanol, which is characterized in that include the following steps：
A. raw material isopropanol is taken, potassium permanganate is added thereto and carries out oxidation processes, removes such as second of the impurity containing double bond
The impurity such as alkene, acrylonitrile, hydrogen cyanide, methacrylaldehyde, methacrylonitrile, propenyl, oxazoles, acetamide.The same of potassium permanganate is added
When, sodium hydroxide and calcium oxide is added, slows down the oxidisability of potassium permanganate, while neutralizing the acidic materials that oxidation generates, adjusts
PH value is 10.After oxidation processes, isopropanol is distilled out rapidly.
A ˊ reducing agent disodium hydrogen phosphate will be added into the isopropanol obtained by step a and stir, and distill out isopropanol.
B. sodium oxide molybdena is added into the above-mentioned isopropanol distilled out, the pH of solution is adjusted to 7.5, and shaking makes sodium oxide molybdena
It is fully reacted with the acid impurities in raw material isopropanol, generates precipitation of salts object；Stratification discards water layer and precipitation, filtering
Organic layer retains filtrate.
C. above-mentioned filtrate is passed through with the speed of 15 column volumes/hour equipped with the adsorbent column that grain size is 100 mesh molecular sieves,
Further remove the moisture in organic layer；After absorption, aqueous isopropyl alcohol amount is controlled≤0.03%；Molecular sieve is utilized in this step
The moisture after extraction in isopropanol is removed, is further continued for carrying out molecular sieve suction after needing to change molecular sieve such as moisture ＞ 0.03%
Attached processing；
And then, above-mentioned efflux is passed through adsorbent column equipped with aluminium oxide with the speed of 30 column volumes/hour, be equipped with
The adsorbent column of silica gel and be attached with equipped with surface salpeter solution modified activated carbon adsorbent column carry out adsorption treatment, be used for
Remove the unsaturated organic compound such as heterocyclic arene of oxide-based, arene, polar compounds species and carbon-carbon double bonds
Equal impurity.Wherein, the grain size of activated carbon is 55 mesh, and the mass concentration of salpeter solution is 19%；
Finally, above-mentioned efflux is passed through the suction equipped with the aluminium oxide that grain size is 20 mesh with the speed of 30 column volumes/hour
Attached dose of column, for removing peroxide and aldoketones impurity.
D. by the isopropanol obtained by step c with the speed of 21 column volumes/hour be passed through equipped with surface be attached with acetonitrile from
The adsorbent column of sub-exchange resin, the impurity such as removal aldehydes, metal ion.It avoids metal ion in mass spectral analysis and is measured
Object is complexed and produces Interference Peaks, improves the precision of liquid chromatograph-mass spectrometer measurement result.The grain of ion exchange resin
Diameter is 0.01cm.
E. the isopropanol obtained by step d is subjected to rectifying to get to the liquid chromatography-mass spectrography of purity >=99.99% (wt)
Combined instrument isopropanol.
Known manner progress can be used in rectifying.A kind of preferred embodiment of the present invention is that rectifying still heating temperature is 90 DEG C, kettle
88 DEG C of middle isopropyl alcohol liquid temperature, distill out liquid temperature be 83 DEG C, control reflux ratio 20: 1, infinite reflux 2.5 hours.Smart distillate
It bottles after detection is qualified, inflated with nitrogen preserves.
Embodiment 4
The method of purification of LC-MS analysis isopropanol, which is characterized in that include the following steps：
A. raw material isopropanol is taken, potassium permanganate is added thereto and carries out oxidation processes, removes the impurity containing double bond
Such as ethylene, acrylonitrile, hydrogen cyanide, methacrylaldehyde, methacrylonitrile, propenyl, oxazoles, acetamide impurity.Potassium permanganate is added
While, potassium hydroxide and calcium oxide is added, slows down the oxidisability of potassium permanganate, while neutralizing the acidic materials that oxidation generates,
It is 9 to adjust pH value.After oxidation processes, isopropanol is distilled out rapidly.
A ˊ reducing agent ferrous sulfate will be added into the isopropanol obtained by step a and stir, and distill out isopropanol.
B. potassium hydroxide is added into the above-mentioned isopropanol distilled out, the pH of solution is adjusted to 8, and shaking makes hydroxide
Potassium is fully reacted with the acid impurities in raw material isopropanol, generates precipitation of salts object；Stratification discards water layer and precipitation, mistake
Organic layer is filtered, filtrate is retained.
C. above-mentioned filtrate is passed through with the speed of 24 column volumes/hour equipped with the adsorbent that grain size is 65 molecules of interest sieve
Column further removes the moisture in organic layer；After absorption, aqueous isopropyl alcohol amount is controlled≤0.03%；It utilizes and divides in this step
Son screens out the moisture in isopropanol after extraction, is further continued for carrying out molecule after needing to change molecular sieve such as moisture ＞ 0.03%
Sieve adsorption treatment；
And then, above-mentioned efflux is passed through to be attached with triethanolamine equipped with surface molten with the speed of 12 column volumes/hour
The adsorbent column of the modified activated carbon of liquid carries out adsorption treatment, for remove oxide-based, arene, polar compounds species with
And the impurity such as the unsaturated organic compound of carbon-carbon double bonds such as heterocyclic arene.Wherein, the grain size of activated carbon is 76 mesh, three ethyl alcohol
The mass concentration of amine aqueous solution is 27%；
Finally, above-mentioned efflux is passed through the suction equipped with the aluminium oxide that grain size is 135 mesh with the speed of 16 column volumes/hour
Attached dose of column, for removing peroxide and aldoketones impurity.
D. by the isopropanol obtained by step c with the speed of 14 column volumes/hour be passed through equipped with surface be attached with methanol from
The adsorbent column of sub-exchange resin, the impurity such as removal aldehydes, metal ion.It avoids metal ion in mass spectral analysis and is measured
Object is complexed and produces Interference Peaks, improves the precision of liquid chromatograph-mass spectrometer measurement result.The grain of ion exchange resin
Diameter is 0.09cm.
E. the isopropanol obtained by step d is subjected to rectifying to get to the liquid chromatography-mass spectrography of purity >=99.99% (wt)
Combined instrument isopropanol.
Known manner progress can be used in rectifying.A kind of preferred embodiment of the present invention is that rectifying still heating temperature is 87 DEG C, kettle
85 DEG C of middle isopropyl alcohol liquid temperature, distill out liquid temperature be 81 DEG C, control reflux ratio 13: 1, infinite reflux 2.8 hours.Smart distillate
It bottles after detection is qualified, inflated with nitrogen preserves.
Embodiment 5
The method of purification of LC-MS analysis isopropanol, which is characterized in that include the following steps：
A. raw material isopropanol is taken, potassium permanganate is added thereto and carries out oxidation processes, removes such as second of the impurity containing double bond
The impurity such as alkene, acrylonitrile, hydrogen cyanide, methacrylaldehyde, methacrylonitrile, propenyl, oxazoles, acetamide.The same of hydrogen peroxide is added
When, potassium hydroxide and calcium oxide is added, slows down the oxidisability of potassium permanganate, while neutralizing the acidic materials that oxidation generates, adjusts
PH value is 8.5.After oxidation processes, isopropanol is distilled out rapidly.
A ˊ reducing agent sodium hydrogensulfite will be added into the isopropanol obtained by step a and stir, and distill out isopropanol.
B. potassium hydroxide is added into the above-mentioned isopropanol distilled out, the pH of solution is adjusted to 7.4, and shaking makes hydrogen-oxygen
Change potassium fully to react with the acid impurities in raw material isopropanol, generates precipitation of salts object；Stratification discards water layer and precipitation,
Organic layer is filtered, filtrate is retained.
C. above-mentioned filtrate is passed through with the speed of 23 column volumes/hour equipped with the adsorbent that grain size is 60 molecules of interest sieve
Column further removes the moisture in organic layer；After absorption, aqueous isopropyl alcohol amount is controlled≤0.03%；It utilizes and divides in this step
Son screens out the moisture in isopropanol after extraction, is further continued for carrying out molecule after needing to change molecular sieve such as moisture ＞ 0.03%
Sieve adsorption treatment；
And then, above-mentioned efflux is passed through with the speed of 9 column volumes/hour and is attached with aluminum hydroxide solution equipped with surface
Modified activated carbon adsorbent column carry out adsorption treatment, for remove oxide-based, arene, polar compounds species and
The impurity such as the unsaturated organic compound of carbon-carbon double bonds such as heterocyclic arene.Wherein, the grain size of activated carbon is 57 mesh, aluminium hydroxide
The mass concentration of solution is 8%；
Finally, above-mentioned efflux is passed through the suction equipped with the aluminium oxide that grain size is 50 mesh with the speed of 20 column volumes/hour
Attached dose of column, for removing peroxide and aldoketones impurity.
D., isopropanol obtained by step c is passed through to the ion that acetonitrile is attached with equipped with surface with the speed of 3 column volumes/hour
The adsorbent column of exchanger resin, the impurity such as removal aldehydes, metal ion.Avoid metal ion in mass spectral analysis with measured object
It is complexed and produces Interference Peaks, improve the precision of liquid chromatograph-mass spectrometer measurement result.The grain size of ion exchange resin
For 0.11cm.
E. the isopropanol obtained by step d is subjected to rectifying to get to the liquid chromatography-mass spectrography of purity >=99.99% (wt)
Combined instrument isopropanol.
Known manner progress can be used in rectifying.A kind of preferred embodiment of the present invention is that rectifying still heating temperature is 92 DEG C, kettle
87 DEG C of middle isopropyl alcohol liquid temperature, distill out liquid temperature be 82.5 DEG C, control reflux ratio 18: 1, infinite reflux 2.4 hours.Rectifying goes out
It bottles after liquid detection is qualified, inflated with nitrogen preserves.
The technical indicator of LC-MS analysis isopropanol after Examples 1 to 5 purification is as shown in Table 1：
Table one
As shown in Table 1, liquid chromatograph-mass spectrometer isopropanol made from the method for purification provided through the invention,
Purity is further increased by 99.5% to 99.99%, and evaporation residue, water content, metal (K, Na) content all substantially reduce.Yield
Not less than 95%, the yield of more traditional method of purification 80% greatly improves.It is 195nm, 200nm, 210nm and 230nm to wavelength
The light transmittance of incident light also greatly improved compared with raw material, improve the optical property of liquid chromatograph-mass spectrometer isopropanol.
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 (6)
1. the method for purification of liquid chromatograph-mass spectrometer isopropanol, which is characterized in that include the following steps：
A. raw material isopropanol is taken, after potassium permanganate or peroxide are added thereto and stirs, distills out isopropanol；
B. alkali metal oxide, alkali metal hydroxide or carbonate are added in the isopropanol distilled out into step a, shake,
After stratification, water layer is discarded, filters organic layer, retains filtrate；
C. above-mentioned filtrate is passed through the adsorbent column equipped with modified activated carbon and carries out adsorption treatment；
D. the isopropanol obtained by step c is passed through the adsorbent column equipped with ion exchange resin and carries out ion-exchange treatment, obtained
The liquid chromatograph-mass spectrometer isopropanol of purity >=99.99% (wt)；
In the step c, modified activated carbon is that aluminium oxide, triethanolamine or aluminium hydroxide activated carbon are adhered in surface.
2. the method for purification of liquid chromatograph-mass spectrometer isopropanol according to claim 1, which is characterized in that institute
It states in step a, while potassium permanganate or peroxide is added, highly basic and basic anhydride is added.
3. the method for purification of liquid chromatograph-mass spectrometer isopropanol according to claim 1, which is characterized in that institute
It states in step a, is added before potassium permanganate or peroxide, porous mass is added into raw material isopropanol, stir 1~2 hour.
4. the method for purification of liquid chromatograph-mass spectrometer isopropanol according to claim 1, which is characterized in that institute
It states in step c, filtrate is passed through before the adsorbent column equipped with modified activated carbon, is first passed through the adsorbent column equipped with molecular sieve.
5. the method for purification of liquid chromatograph-mass spectrometer isopropanol according to claim 1, which is characterized in that institute
It states in step c, filtrate is passed through after the adsorbent column equipped with modified activated carbon, is passed through the adsorbent column equipped with aluminium oxide.
6. the method for purification of the liquid chromatograph-mass spectrometer isopropanol according to any of the above-described claim, special
Sign is, further includes step e, and the isopropanol obtained by adsorption treatment is carried out rectifying.
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| CN100398502C (en) * | 2004-02-27 | 2008-07-02 | 上海化学试剂研究所 | Method for preparing hyperpure isopropyl alcohol |
| CN1332918C (en) * | 2006-04-24 | 2007-08-22 | 广东西陇化工有限公司 | Method for preparing ultra high-purity alcohol compound |
| CN101570468B (en) * | 2009-06-15 | 2012-03-28 | 天津市康科德科技有限公司 | Method for preparing pesticide residue grade chromatographic ethanol |
| CN102060663A (en) * | 2009-11-18 | 2011-05-18 | 天津市康科德科技有限公司 | Method for preparing chromatographic pure isopropanol |
| CN102746115A (en) * | 2012-07-18 | 2012-10-24 | 天津康科德医药化工有限公司 | Purification method for high-purity organic solvent normal propyl alcohol |
| CN102942447B (en) * | 2012-10-13 | 2015-09-30 | 江苏盈天化学有限公司 | A kind of process for purification of electronic-grade isopropanol recovering liquid |
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