CN101704717A - Preparation method of HPLC level isopropanol - Google Patents
Preparation method of HPLC level isopropanol Download PDFInfo
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- CN101704717A CN101704717A CN 200910185629 CN200910185629A CN101704717A CN 101704717 A CN101704717 A CN 101704717A CN 200910185629 CN200910185629 CN 200910185629 CN 200910185629 A CN200910185629 A CN 200910185629A CN 101704717 A CN101704717 A CN 101704717A
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Abstract
The invention discloses a preparation method of HPLC level isopropanol. The method takes industrial isopropanol as the raw material, adopts all-glass reaction rectification equipment, and uses a mild oxidation system consisting of ionic liquid and oxidant for oxidation and a reduction system consisting of ionic liquid and a strong reducing agent for reduction. The method prepares the high-purity HPLC level isopropanol that has low ultraviolet absorption within the range of 205-300nm by conducting light fraction removal, heavy fraction removal and three-tower rectification of finished products to remove traces of water, organics, ions and other impurities in the raw material, especially the impurities absorbed in a near ultraviolet band.
Description
Technical field
The present invention relates to a kind of preparation method of HPLC level isopropanol.It belongs to chemical production field.
Technical background
High performance liquid chromatography (HPLC) method is a kind of novel separate analytical technique that grows up beginning of the seventies late 1960s, along with updating and develop of technology, has become chemical separation at present and has used important means very widely in analyzing.It is on classical liquid chromatography basis; introduced the theory of gas-chromatography; new technologies such as high pressure liquid pump, efficient stationary phase and high sensitivity detector have been adopted; thereby have characteristics such as separation efficiency height, selectivity is good, detection sensitivity is high, analysis speed is fast, operation automation is strong, be widely used in fields such as environment measuring, environment protection, petrochemical complex, biological chemistry, organic chemistry, food sanitation, medicine industry.Along with the widespread use of liquid chromatography, grow with each passing day as the demand of the chromatographically pure level isopropanol of liquid chromatography moving phase, supply falls short of demand for product.But HPLC level isopropanol alcohol requires purity very high, and (very low absorbancy is arranged in 205～300nm) at ultraviolet band.
The HPLC level isopropanol is a kind of very important liquid chromatography solvents, and it is called as " menstruum universale ", and is easily molten with water, can and miscible in wide region with immiscible polarity and the non-polar solvent of water.
At present, to be that feed purification is refining with the technical grade Virahol normally form the HLPC level isopropanol.Rectifying is the main method of industrialization purification Virahol, comprises azeotropic distillation, extracting rectifying etc.The HLPC level isopropanol that is used for liquid chromatography moving phase is to metallic impurity wherein, and molecule content and anionic requirement are very harsh, and simple rectification process can't meet the demands.
In the prior art, Pure and applied chemistry 1986, (10), 1412-1418 discloses a kind of preparation method of ultra-clean high-purity isopropanol, with the Virahol is raw material, adds a kind of backflow in calcium oxide or the magnesium powder (making promoting agent with iodine), and fractional column is rectifying repeatedly, the isopropanol content 99.94% that obtains, water-content 600ppm.The product water content height that this method obtains, if dewater with molecular sieve, foreign matter content obviously raises, and does not reach requirement.
Japanese patent laid-open 10-109948 discloses a kind of process for purification of Virahol.Add entry in the Virahol that contains the impurity element, utilize azeotropy to add thermal distillation, remove foreign ion, Virahol is 80% in the product of distillation, and water is 20%.Because water-content is too high, the cost height that dewaters, aftertreatment difficulty.
Patent GB816796 proposes the technology that a kind of azeotropic distillation is produced the high purity Virahol, this process using ether is made entrainment agent, in tower, feed rare gas element ethene, the tower internal pressure need reach 160-170psig, and cat head is installed a deoxygenator, has avoided the danger of ether and air mixture blast, the volumetric concentration of final Virahol product is greater than 99.9%, this operation technological process complexity, facility investment is higher, and operational danger is big.
The present invention utilizes ionic liquid and potassium permanganate, potassium bichromate to form the mild oxidation system, in the oxidation unsaturated compound, has avoided Virahol to be oxidized to ketone; The reduction system that adopts ionic liquid and reductive agent to form has been strengthened contacting of reductive agent and raw material, and the conversion of promotion carbonyl compound helps removing with next step rectification working process.Therefore, this novel technique has obvious superiority and innovation part, and can breaking for a long time, import HPLC level isopropanol has considerable economic and good social benefit to the technical monopoly of China.
Summary of the invention
The present invention sets out with the technical grade Virahol, utilize full glass reaction rectifying device, use gentle oxidation system, and carry out reaction of high order rectifying, with safety, efficient, the mode that is easy to industrial operation, remove water, organism (alcohol, aldehyde, ketone, ether, ester, hydro carbons etc.), the ion impurity such as (metal ion, acid ions) of trace in the raw material, particularly remove the impurity that absorption is arranged in the near ultraviolet region, preparation has the HPLC level isopropanol of low uv-absorbing in 205～300nm interval.
The present invention is achieved through the following technical solutions purpose:
1, the method for the high-purity HPLC level isopropanol of this preparation, it is characterized in that described method is: with of the mild oxidation system oxidation of industrial isopropanol elder generation by ionic liquid and oxygenant composition, pass through the reduction system reducing that ionic liquid and strong reductant are formed again, then through impurity such as the water that takes off gently, takes off heavily, the finished product three-tower rectification is removed trace in the raw material, organism, ions, particularly remove the impurity that absorption is arranged in the near ultraviolet region, obtain high-purity HPLC level isopropanol.
2, described HPLC level isopropanol preparation method is characterized in that the described ionic liquid of this oxidation system is that one or more of N-Methyl pyrrolidone hydrogen sulfate hydrochlorate, N-Methyl pyrrolidone dihydrogen phosphate, N-methylsulfonic acid base pyrrolidone hydrosulfate, N-ethyl sulfonic acid base pyrrolidone hydrosulfate, N-propanesulfonic acid base hydrosulfate combine.
3, described HPLC level isopropanol preparation method is characterized in that the described oxygenant of this oxidation system is potassium permanganate, potassium bichromate.
4, described HPLC level isopropanol preparation method is characterized in that the described ionic liquid of this reduction system is that one or more of 1-butyl-3-methyl imidazolium tetrafluoroborate, 1-butyl-3-Methylimidazole hexafluorophosphate, 1-butyl-3-N-Methylimidazoleacetic salt, 1-hexyl-3-methyl imidazolium tetrafluoroborate, 1-hexyl-3-Methylimidazole hexafluorophosphate combine.
5, described HPLC level isopropanol preparation method, one or more that it is characterized in that the described strong reductant sulphite of this reducing system, hydrosulphite, sodium borohydride, POTASSIUM BOROHYDRIDE combine.
6, described HPLC level isopropanol preparation method is characterized in that raw materials used Virahol is a technical grade, and purity is more than 99.5%; Used ionic liquid, oxygenant, reductive agent purity are analytical reagent.
7, described HPLC level isopropanol preparation method, it is characterized in that the ion liquid input quality of oxidising process is Virahol raw material 1 ‰ of quality～20 ‰ that feed intake, the input amount of oxygenant is Virahol raw material 0.1 ‰ of quality～10 ‰ that feed intake, reaction times is 1～7h, and temperature of reaction is 25～45 ℃.
8, described HPLC level isopropanol preparation method, it is characterized in that the ion liquid input amount of reduction process is Virahol raw material 1 ‰ of quality～20 ‰ that feed intake, the input amount of strong reductant is Virahol raw material 0.1 ‰ of quality～10 ‰ that feed intake, reaction times is 1～7h, and temperature of reaction is 25～40 ℃.
9, described HPLC level isopropanol preparation method is characterized in that taking off gently, take off heavy and product three-tower rectification through the Virahol after the reaction treatment, to obtain the finished product.Those of ordinary skills are enough to finish this class distillation operation according to general knowledge.
10, described HPLC level isopropanol preparation method is characterized in that described process all carries out in the glass reaction rectifying device.
11, described HPLC level isopropanol preparation method, the HPLC level isopropanol that finally obtains carries out UV through UV2550 and detects (1cm colorimetric pool, water are reference), its 220nm place absorbancy is between 0.2300-0.3000, and 254nm place absorbancy is between 0.0100-0..0200.Through Agilent 7890 carry out GC detect (chromatographic column model: HP-FFAP, column length 50m, internal diameter 0.32mm, thickness of liquid film 0.5 μ m. testing conditions: column temperature: starting temperature kept 5 minutes for 40 ℃, 10 ℃/minute kept 2 minutes after rising to 220 ℃; 220 ℃ of sampler temperature; 250 ℃ of detector temperatures .) its content is greater than 99.90%.
Characteristics of the present invention:
1. use acidic ion liquid compatible with oxygenant and reductive agent, can make the redox reaction milder, promotes oxidn agent and reducing reaches and the contacting of Virahol, and after reaction, makes the residue of generation be easy to take out from reactor, simplifies the operation.Ion liquid system can be reused simultaneously;
2. described HPLC level refining methanol method, reactor that is adopted and rectifying tower are full glass device, can guarantee that treating process do not introduce metal ion.
Embodiment
Further elaborate preparation method of the present invention below by embodiment
Embodiment 1
In glass reaction distiller I, drop into 100 kilograms of raw material Virahols, add quality and be feed intake 0.3 kilogram of the oxidant potassium permanganate of 0.5 kilogram of the ionic liquid N of quality 5 ‰-methyl-2-pyrrolidone hydrogen sulfate hydrochlorate and 3 ‰ of Virahol raw material; React 2h down for 25.0 ℃ in temperature; The Virahol 1 that obtains after oxidation is through distilling extraction to glass reaction distiller II; Residual still material is ionic liquid N-methyl-2-pyrrolidone hydrogen sulfate hydrochlorate, the oxidant potassium permanganate of complete reaction not as yet, reuses.Drop into quality at glass reaction distiller II and be feed intake 0.2 kilogram of the strong reductant S-WAT of 0.1 kilogram of the ionic liquid 1-butyl of quality (100 kilograms) 1 ‰-3-methyl imidazolium tetrafluoroborate and 2 ‰ of Virahol raw material.React 1h down for 35.0 ℃ in temperature, reduction back straight run distillation obtains Virahol 2.Residual still material is the not reductive agent S-WAT of complete reaction of ionic liquid 1-butyl-3-methyl imidazolium tetrafluoroborate Buddhist monk, reuses.Virahol 2 gas phase extraction after the redox are to rectifying tower, add thermal rectification and take off light constituent in reflux temperature is 75.0 ℃ lightness-removing column, and entering reflux temperature then is to add thermal rectification in 95.0 ℃ of weight-removing columns to take off heavy constituent; From cat head extraction material Virahol to finishing column rectifying once more, feeding temperature is 72.0 ℃ in the finishing column, tower top temperature is 82.5 ℃, reflux ratio is 3.0, reflux temperature is 80.0 ℃, and front-end volatiles are deviate from from gas phase, and after cut separates at the bottom of by still, the front and back cut is sent reactive system back to and is recycled, and obtains HPLC level isopropanol finished product from the cat head extraction.Detect (1cm colorimetric pool, water are reference) through UV, its 220nm place absorbancy is 0.2504, and 254nm place absorbancy is 0.0161, and the output of HPLC level isopropanol is 85.8 kilograms, and productive rate is 85.8%, and detecting purity through GC is 99.92%.
Embodiment 2
In glass reaction distiller I, drop into 100 kilograms of raw material Virahols, add quality and be feed intake 0.1 kilogram of the oxidant potassium permanganate of 0.2 kilogram of the ionic liquid N of quality 2 ‰-methyl-2-pyrrolidone dihydrogen phosphate and 0.1 ‰ of Virahol raw material; React 3h down for 35.0 ℃ in temperature; The Virahol 1 distillation extraction that obtains after oxidation is to glass reaction distiller II; Residual still material is ionic liquid N-methyl-2-pyrrolidone dihydrogen phosphate, the oxidant potassium permanganate of complete reaction not as yet, reuses.Drop into quality at glass reaction distiller II and be feed intake 1 kilogram of the strong reductant potassium sulfite of 0.3 kilogram of the ionic liquid 1-butyl of quality (100 kilograms) 3 ‰-3-Methylimidazole hexafluorophosphate and 10 ‰ of Virahol raw material.React 2h down for 30.0 ℃ in temperature, reduction back straight run distillation obtains Virahol 2.Residual still material is the not reductive agent potassium sulfite of complete reaction of ionic liquid 1-butyl-3-Methylimidazole hexafluorophosphate Buddhist monk, reuses.Virahol gas phase extraction after the redox is to rectifying tower, adds thermal rectification and take off light constituent in reflux temperature is 72.0 ℃ lightness-removing column, and entering reflux temperature then is to add thermal rectification in 96.0 ℃ of weight-removing columns to take off heavy constituent; From cat head extraction material Virahol to finishing column rectifying once more, feeding temperature is 72.0 ℃ in the finishing column, tower top temperature is 82.5 ℃, reflux ratio is 3.0, reflux temperature is 80.0 ℃, and front-end volatiles are deviate from from gas phase, and after cut separates at the bottom of by still, the front and back cut is sent reactive system back to and is recycled, and obtains HPLC level isopropanol finished product from the cat head extraction.Detect (1cm colorimetric pool, water are reference) through UV, its 220nm place absorbancy is 0.2654, and 254nm place absorbancy is 0.0183, and the output of HPLC level isopropanol is 86.2 kilograms, and productive rate is 86.2%, and detecting purity through GC is 99.93%.
Embodiment 3
In glass reaction distiller I, drop into 100 kilograms of raw material Virahols, add quality and be feed intake 0.8 kilogram of the oxygenant potassium bichromate of 0.5 kilogram of the ionic liquid N of quality 5 ‰-methylsulfonic acid base pyrrolidone hydrosulfate and 0.8 ‰ of Virahol raw material; React 3h down for 35.0 ℃ in temperature; The Virahol 1 distillation extraction that obtains after oxidation is to glass reaction distiller II; Residual still material is the not oxygenant potassium bichromate of complete reaction of ionic liquid N-methylsulfonic acid base pyrrolidone hydrosulfate Buddhist monk, reuses.Drop into quality at glass reaction distiller II and be feed intake 0.2 kilogram of the strong reductant potassium sulfite of 0.1 kilogram of the ionic liquid 1-butyl of quality (100 kilograms) 1 ‰-3-N-Methylimidazoleacetic salt and 2 ‰ of Virahol raw material, 0.2 kilogram of 2 ‰ strong reductant POTASSIUM BOROHYDRIDE.React 2h down for 40.0 ℃ in temperature, reduction back straight run distillation obtains Virahol 2.Residual still material is that ionic liquid 1-butyl-3-N-Methylimidazoleacetic salt reaches as yet not the reductive agent potassium sulfite and the POTASSIUM BOROHYDRIDE of complete reaction, reuses.Virahol 2 gas phase extraction after the redox are to rectifying tower, add thermal rectification and take off light constituent in reflux temperature is 73.0 ℃ lightness-removing column, and entering reflux temperature then is to add thermal rectification in 95.0 ℃ of weight-removing columns to take off heavy constituent; From cat head extraction material Virahol to finishing column rectifying once more, feeding temperature is 72.0 ℃ in the finishing column, tower top temperature is 82.5 ℃, reflux ratio is 3.0, reflux temperature is 80.0 ℃, and front-end volatiles are deviate from from gas phase, and after cut separates at the bottom of by still, the front and back cut is sent reactive system back to and is recycled, and obtains HPLC level isopropanol finished product from the cat head extraction.Detect (1cm colorimetric pool, water are reference) through UV, its 220nm place absorbancy is 0.2348, and 254nm place absorbancy is 0.0108, and the output of HPLC level isopropanol is 86.3 kilograms, and productive rate is 86.3%, and detecting purity through GC is 99.97%.
Embodiment 4
Add to drop into 100 kilograms of raw material Virahols in glass reaction distiller I, quality is feed intake 0.5 kilogram of the oxidant potassium permanganate of 0.2 kilogram of 0.2 kilogram of the ionic liquid N of quality 2 ‰-methyl-2-pyrrolidone hydrogen sulfate hydrochlorate, 2 ‰ N-ethyl sulfonic acid base pyrrolidone hydrosulfate and 0.5 ‰ of Virahol raw material; React 2h down for 25.0 ℃ in temperature; The Virahol 1 distillation extraction that obtains after oxidation is to glass reaction distiller II; Residual still material is the not oxidant potassium permanganate of complete reaction of ionic liquid N-methyl-2-pyrrolidone hydrogen sulfate hydrochlorate, N-ethyl sulfonic acid base pyrrolidone hydrosulfate Buddhist monk, reuses.Drop into quality at glass reaction distiller II and be feed intake 0.3 kilogram of the strong reductant sodium bisulfite of 0.6 kilogram of 6 ‰ ionic liquid 1-hexyl of quality (100 kilograms)-3-methyl imidazolium tetrafluoroborate and 3 ‰ of Virahol raw material.React 5h down for 35.0 ℃ in temperature, reduction back straight run distillation obtains Virahol 2.Residual still material is the not reductive agent sodium bisulfite of complete reaction of ionic liquid 1-hexyl-3-methyl imidazolium tetrafluoroborate Buddhist monk, reuses.Virahol 2 gas phase extraction after the redox are to rectifying tower, add thermal rectification and take off light constituent in reflux temperature is 70.0 ℃ lightness-removing column, and entering reflux temperature then is to add thermal rectification in 99.0 ℃ of weight-removing columns to take off heavy constituent; From cat head extraction material Virahol to finishing column rectifying once more, feeding temperature is 72.0 ℃ in the finishing column, tower top temperature is 82.5 ℃, reflux ratio is 3.0, reflux temperature is 80.0 ℃, and front-end volatiles are deviate from from gas phase, and after cut separates at the bottom of by still, the front and back cut is sent reactive system back to and is recycled, and obtains HPLC level isopropanol finished product from the cat head extraction.Detect (1cm colorimetric pool, water are reference) through UV, its 220nm place absorbancy is 0.2546, and 254nm place absorbancy is 0.0166, and the output of HPLC level isopropanol is 85.9 kilograms, and productive rate is 85.9%, and detecting purity through GC is 99.96%.
Embodiment 5
In glass reaction distiller I, drop into 100 kilograms of raw material Virahols, add quality and be feed intake 0.2 kilogram of the oxidant potassium permanganate of 0.8 kilogram of the ionic liquid N of quality 8 ‰-propanesulfonic acid base hydrosulfate and 2 ‰ of Virahol raw material; React 3h down for 40.0 ℃ in temperature; The Virahol 1 distillation extraction that obtains after oxidation is to glass reaction distiller II; Residual still material is the not oxidant potassium permanganate of complete reaction of ionic liquid N-propanesulfonic acid base hydrosulfate Buddhist monk, reuse. drop into quality at glass reaction distiller II and be feed intake 0.5 kilogram of the ionic liquid 1-hexyl of quality (100 kilograms) 5 ‰-3-Methylimidazole hexafluorophosphate of Virahol raw material, 0.2 kilogram of 0.5 kilogram of 5 ‰ ionic liquid 1-hexyl-3-N-Methylimidazoleacetic salt and 2 ‰ strong reductant sodium borohydride. at 30.0 ℃ of temperature reaction 2h down, it is ionic liquid 1-hexyl-3-Methylimidazole hexafluorophosphate that reduction back straight run distillation obtains Virahol 2. residual still material, 1-hexyl-3-N-Methylimidazoleacetic salt Buddhist monk is the borane reducing agent sodium hydride of complete reaction not, to reuse. the Virahol 2 gas phase extraction after the redox are to rectifying tower, add thermal rectification and take off light constituent in reflux temperature is 74.0 ℃ lightness-removing column, entering reflux temperature then is to add thermal rectification in 99.0 ℃ of weight-removing columns to take off heavy constituent; From cat head extraction material Virahol to finishing column rectifying once more, feeding temperature is 72.0 ℃ in the finishing column, tower top temperature is 82.5 ℃, reflux ratio is 3.0, reflux temperature is 80.0 ℃, front-end volatiles are deviate from from gas phase, after cut separates at the bottom of by still, and the front and back cut is sent reactive system back to and recycled, and obtains HPLC level isopropanol finished product from the cat head extraction. detect (1cm colorimetric pool through UV, water is reference), its 220nm place absorbancy is 0.2228, and 254nm place absorbancy is 0.0175, and the output of HPLC level isopropanol is 88.4 kilograms, productive rate is 88.4%, and detecting purity through GC is 99.98%.
Embodiment 6
In glass reaction distiller I, drop into 100 kilograms of raw material Virahols, add quality and be feed intake 1 kilogram of the oxidant potassium permanganate of 1 kilogram of the ionic liquid N of quality 10 ‰-methylsulfonic acid base pyrrolidone hydrosulfate and 10 ‰ of Virahol raw material; React 6h down for 40.0 ℃ in temperature; The Virahol 1 distillation extraction that obtains after oxidation is to glass reaction distiller II; Residual still material is the not oxidant potassium permanganate of complete reaction of ionic liquid N-methylsulfonic acid base pyrrolidone hydrosulfate Buddhist monk, reuses.Drop into quality at glass reaction distiller II and be feed intake 0.4 kilogram of the strong reductant POTASSIUM BOROHYDRIDE of 0.3 kilogram of the ionic liquid 1-hexyl of quality (100 kilograms) 3 ‰-3-Methylimidazole hexafluorophosphate and 4 ‰ of Virahol raw material.React 2h down for 30.0 ℃ in temperature, straight run distillation obtains Virahol 2 after reducing.Residual still material is the not borane reducing agent potassium hydride KH of complete reaction of ionic liquid 1-hexyl-3-Methylimidazole hexafluorophosphate Buddhist monk, reuses.Virahol 2 gas phase extraction after the redox are to rectifying tower, add thermal rectification and take off light constituent in reflux temperature is 69.0 ℃ lightness-removing column, and entering reflux temperature then is to add thermal rectification in 95.0 ℃ of weight-removing columns to take off heavy constituent; From cat head extraction material Virahol to finishing column rectifying once more, feeding temperature is 72.0 ℃ in the finishing column, tower top temperature is 82.5 ℃, reflux ratio is 3.0, reflux temperature is 80.0 ℃, and front-end volatiles are deviate from from gas phase, and after cut separates at the bottom of by still, the front and back cut is sent reactive system back to and is recycled, and obtains HPLC level isopropanol finished product from the cat head extraction.Detect (1cm colorimetric pool, water are reference) through UV, its 220nm place absorbancy is 0.2238, and 254nm place absorbancy is 0.0132, and the output of HPLC level isopropanol is 96.8 kilograms, and productive rate is 96.8%, and detecting purity through GC is 99.95%.
Embodiment 7
In glass reaction distiller I, drop into 100 kilograms of raw material Virahols, add quality and be Virahol raw material feed intake 0.1 kilogram of ionic liquid N-0.3 kilogram of the methylsulfonic acid base pyrrolidone hydrosulfate, 3 ‰ 0.3 kilogram of N-ethyl sulfonic acid base pyrrolidone hydrosulfate of quality 3 ‰ and 1 ‰ oxidant potassium permanganate; React 3h down for 40.0 ℃ in temperature; The Virahol 1 distillation extraction that obtains after oxidation is to glass reaction distiller II; Residual still material is the not oxidant potassium permanganate of complete reaction of ionic liquid N-methylsulfonic acid base pyrrolidone hydrosulfate, N-ethyl sulfonic acid base pyrrolidone hydrosulfate Buddhist monk, reuses.Drop into quality at glass reaction distiller II and be feed intake 0.01 kilogram of the strong reductant sodium borohydride of 0.5 kilogram of the ionic liquid 1-hexyl of quality (100 kilograms) 5 ‰-3-Methylimidazole hexafluorophosphate and 0.1 ‰ of Virahol raw material.React 2h down for 30.0 ℃ in temperature, straight run distillation obtains Virahol 2 after reducing.Residual still material is the not borane reducing agent sodium hydride of complete reaction of ionic liquid 1-hexyl-3-Methylimidazole hexafluorophosphate Buddhist monk, reuses.Virahol 2 gas phase extraction after the redox are to rectifying tower, add thermal rectification and take off light constituent in reflux temperature is 73.0 ℃ lightness-removing column, and entering reflux temperature then is to add thermal rectification in 98.0 ℃ of weight-removing columns to take off heavy constituent; From cat head extraction material Virahol to finishing column rectifying once more, feeding temperature is 72.0 ℃ in the finishing column, tower top temperature is 82.5 ℃, reflux ratio is 3.0, reflux temperature is 80.0 ℃, and front-end volatiles are deviate from from gas phase, and after cut separates at the bottom of by still, the front and back cut is sent reactive system back to and is recycled, and obtains HPLC level isopropanol finished product from the cat head extraction.Detect (1cm colorimetric pool, water are reference) through UV, its 220nm place absorbancy is 0.2262, and 254nm place absorbancy is 0.0135, and the output of HPLC level isopropanol is 87.4 kilograms, and productive rate is 87.4%, and detecting purity through GC is 99.97%.
Claims (10)
1. method for preparing high-purity HPLC level isopropanol, it is characterized in that described method is: with of the mild oxidation system oxidation of industrial isopropanol elder generation by ionic liquid and oxygenant composition, pass through the reduction system reducing that ionic liquid and strong reductant are formed again, then through impurity such as the water that takes off gently, takes off heavily, the finished product three-tower rectification is removed trace in the raw material, organism, ions, particularly remove the impurity that absorption is arranged in the near ultraviolet region, obtain high-purity HPLC level isopropanol.
2. described HPLC level isopropanol preparation method is characterized in that the described ionic liquid of this oxidation system is that one or more of N-Methyl pyrrolidone hydrogen sulfate hydrochlorate, N-Methyl pyrrolidone dihydrogen phosphate, N-methylsulfonic acid base pyrrolidone hydrosulfate, N-ethyl sulfonic acid base pyrrolidone hydrosulfate, N-propanesulfonic acid base hydrosulfate combine.
3. described HPLC level isopropanol preparation method is characterized in that the described oxygenant of this oxidation system is potassium permanganate, potassium bichromate.
4. described HPLC level isopropanol preparation method is characterized in that the described ionic liquid of this reduction system is that one or more of 1-butyl-3-methyl imidazolium tetrafluoroborate, 1-butyl-3-Methylimidazole hexafluorophosphate, 1-butyl-3-N-Methylimidazoleacetic salt, 1-hexyl-3-methyl imidazolium tetrafluoroborate, 1-hexyl-3-Methylimidazole hexafluorophosphate combine.
5. described HPLC level isopropanol preparation method, one or more that it is characterized in that the described strong reductant sulphite of this reducing system, hydrosulphite, sodium borohydride, POTASSIUM BOROHYDRIDE combine.
6. described HPLC level isopropanol preparation method is characterized in that raw materials used Virahol is a technical grade, and purity is more than 99.5%; Used ionic liquid, oxygenant, reductive agent purity are analytical reagent.
7. described HPLC level isopropanol preparation method, it is characterized in that the ion liquid input quality of oxidising process is Virahol raw material 1 ‰ of quality～20 ‰ that feed intake, the input amount of oxygenant is Virahol raw material 0.1 ‰ of quality～10 ‰ that feed intake, and the reaction times is 1～7h, and temperature of reaction is 25～45 ℃.
8. described HPLC level isopropanol preparation method, it is characterized in that the ion liquid input amount of reduction process is Virahol raw material 1 ‰ of quality～20 ‰ that feed intake, the input amount of strong reductant is Virahol raw material 0.1 ‰ of quality～10 ‰ that feed intake, and the reaction times is 1～7h, and temperature of reaction is 25～40 ℃.
9. described HPLC level isopropanol preparation method is characterized in that taking off gently, take off heavy and product three-tower rectification through the Virahol after the reaction treatment, to obtain the finished product.Those of ordinary skills are enough to finish this class distillation operation according to general knowledge.
10. described HPLC level isopropanol preparation method is characterized in that described process all carries out in the glass reaction rectifying device.
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