CN205528523U - High performance liquid chromatography HPLC solvent preparation purification device - Google Patents
High performance liquid chromatography HPLC solvent preparation purification device Download PDFInfo
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- CN205528523U CN205528523U CN201620134987.0U CN201620134987U CN205528523U CN 205528523 U CN205528523 U CN 205528523U CN 201620134987 U CN201620134987 U CN 201620134987U CN 205528523 U CN205528523 U CN 205528523U
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Abstract
The utility model provides a high performance liquid chromatography HPLC solvent preparation purification device, includes edulcoration device, pre -distillation tower, two -stage condensing system, vacuum rectification tower and ordinary pressure rectifying column. The edulcoration device communicates with the stills of pre -distillation tower, the top exhaust hole and the two -stage condensing system intercommunication of pre -distillation tower, first methyl alcohol conveyer pipe through taking the pump at the bottom of the pre -distillation tata and the rectifying still of vacuum rectification tower intercommunication, the top gas vent and the water condenser intercommunication of vacuum rectification tower, pass through the rectifying still intercommunication of second methyl alcohol conveyer pipe and ordinary pressure rectifying column at the bottom of the vacuum rectification tata, the top gas vent and the water condenser of ordinary pressure rectifying column communicate. This high performance liquid chromatography HPLC solvent preparation purification device's beneficial effect: its simple structure adopts and deposits edulcoration device and tertiary rectifying column, has improved the purity of high performance liquid chromatography HPLC solvent (like methyl alcohol) product, reduces purification process's running cost, and the energy consumption is low, the industrial production of being convenient for, and equipment investment cost is low, and the energy consumption is low.
Description
Technical field
This utility model relates to a kind of Chemical Solvents purification devices, especially relates to a kind of high-efficient liquid phase chromatogram HPLC molten
Agent methanol prepares purification devices.
Background technology
Chromatorgaphy reagent refers to the chemical reagent prepared for chromatography, chromatographic isolation, chromatograph.Methanol is commonly used as one
Reagents for high performance liquid chromatography, for liquid-phase chromatographic analysis, extensively apply in fields such as medication chemistry, check analysis, detections.I
The preparation method of state's methanol liquid phase chromatorgaphy reagent seldom has been reported that, and the yield of domestic methanol is relatively low, and purity is the highest, high-purity
The degree most dependence on import of methanol, causes relatively costly, is pind down degree by foreign technology bigger.
CN 105085178 A discloses the method for purification of a kind of hplc grade methanol, by wherein adding alkali to material benzenemethanol
Metal-oxide, alkali metal hydroxide or carbonate, after shaking, stratification, discard water layer, filter organic layer, by above-mentioned
Filtrate is passed through the adsorbent post equipped with modified activated carbon and carries out adsorption treatment, obtains the chromatographic grade first of purity >=99. 99 % (wt)
Alcohol, the methanol after also including absorption carries out rectification.The method of purification of this hplc grade methanol is by using the suction of modified activated carbon
Attached dose of purification of methanol, but the sorbent treatment amount that the method uses is less, and adsorbent activation is higher with regeneration cost.
KARAFIAN MAXIM;Process for Purifying Methanol by distillation,
GB1191310, crude carbinol is extracted by making extractant with water by 1970, removes less than the ether of methanol boiling point, aldehyde, ketone etc.
Low boiling impurity, then rectification separation water and methanol obtains refined methanol.The methanol purity that the method obtains is on the low side, it is impossible to meet high-efficient liquid
The requirement of phase chromatorgaphy reagent.
Xue Yunlian (ion exchange resin application on methanol is accurate, Guangdong chemical industry, 1991, (4);36-38) use 732
Type cation exchange resin eliminates readily oxidizable substance, organic substance (such as aldehyde, ketone) and hydrogen, amine etc. in methanol, improves methanol
Purity, this methanol purification process there is also the filler activator of ion exchange resin and regeneration cost is higher, treating capacity is less asks
Topic.
Presently commercially available industrial methanol all with synthetic method produce, in methanol impurity that may be present have water, acetone, formaldehyde,
Ethanol, methyl formate and trace dimethyl ether, dimethoxym ethane, ethyl acetate, acetaldehyde and ammonia.And traditional methanol rectification purifying technique is many
Using rectifying column that molten steel methanol is purified process, there is methanol purity after purification low, energy consumption is high, purification high in cost of production is asked
Topic.
Utility model content
The technical problems to be solved in the utility model is: overcome the deficiencies in the prior art, it is provided that a kind of low cost, it is thus achieved that color
Spectrum level methanol (methanol content >=99.99%), the high-efficient liquid phase chromatogram HPLC solvent of industrialized production can prepare purification devices.
This utility model solves its technical problem and be the technical scheme is that a kind of high-efficient liquid phase chromatogram HPLC solvent system
Standby purification devices: include knot screen, pre-distillation column, condensed in two stages system, vacuum rectification tower and atmospheric distillation tower；Described remove impurity
Device includes the premixing tank connected with methanol feedstock bucket, adds iodine device and deposition filter；The described iodine device that adds is arranged on premix
Above tank, add iodine to premixing tank；Being provided with agitating device in described premixing tank, the bottom of premixing tank is provided with the feed liquid conveying of band pump
Pipe, described feed liquid conveying pipe is connected with deposition filter；Described deposition filter is provided with alkali liquor adding tube；Described precipitation filters
Device connects with the distillating still of pre-distillation column；The top vent of described pre-distillation column and condensed in two stages system connectivity；Condensed in two stages
The condensate discharge pipe of system connects with pre-tower backflash, then refluxes by being pumped back into pre-distillation column；Described pre-distillation column tower
The end, is connected with the rectifying still of vacuum rectification tower by the first methanol conveying pipe of band pump, the top vent of vacuum rectification tower and water
Condenser connects；The condensate discharge pipe of water condenser connects with rectification under vacuum backflash；Pass through at the bottom of described vacuum rectification tower tower
Second methanol conveying pipe connects with the rectifying still of atmospheric distillation tower, and the top vent of atmospheric distillation tower connects with water condenser.
Further, described high-efficient liquid phase chromatogram HPLC solvent is prepared purification devices and is also included drying tube, and described drying tube is pacified
Being contained in the tail gas discharging pipe end of condensed in two stages system, water condenser, described condensed in two stages system, the cooling water of water condenser enter
Mouth connects with technical cooling bucket.
Further, described rectification under vacuum backflash and atmospheric pressure reflux groove are by pipeline and hplc grade methanol storage tank, accident liquid
Storage tank connects.
Further, described condensed in two stages system includes primary condenser and secondary condenser, the gas of described primary condenser
Body channel middle and pre-distillation column overhead vapor outlet；The on-condensible gas outlet of described primary condenser and secondary condensation
Connect in the middle part of the secondary gas passage of device, bottom described primary condenser and secondary condenser, be provided with discharging tube, described discharging tube with
Pre-tower backflash connects.
The operation principle of purification devices prepared by this utility model a kind of high-efficient liquid phase chromatogram HPLC solvent: knot screen leads to
Cross in methanol, add iodine, and in the basic conditions by the ethanol in methanol, aldehyde, the Impurity removal of ketone, then pass through pre-distillation column
Distillation, by the tower top temperature of control pre-distillation column at 60 ~ 62 DEG C, by low boiling impurity in methanol (such as dimethyl ether, methyl formate
Deng) remove；Then the methanol removing light component is passed through vacuum rectification tower and carries out rectification, by controlling the tower top of vacuum rectification tower
Temperature is at 120 ~ 125 DEG C, by high-boiling-point impurity in methanol (such as isopropanol, normal propyl alcohol, sec-butyl alcohol, isobutanol, n-butyl alcohol, first contracting
Aldehyde, ethyl acetate etc.) remove；Finally, then add in decompression methanol solution at the bottom of rectifying tower is re-fed into atmospheric distillation tower and carry out the
Three rectification, removes the trace impurity (such as water) in methanol, finally obtains the methanol meeting efficient liquid phase chromatographic analysis requirement.
The beneficial effect of purification devices prepared by this utility model a kind of high-efficient liquid phase chromatogram HPLC solvent: its simple in construction,
Use removing impurity by means of precipitation device and three grades of rectifying columns, improve the purity of high-efficient liquid phase chromatogram HPLC solvent (such as methanol) product, fall
The operating cost of low purifying process, energy consumption is low, it is simple to industrialized production, and equipment investment cost is low, and energy consumption is low.
Accompanying drawing explanation
Fig. 1 is the structural representation that purification devices prepared by a kind of high-efficient liquid phase chromatogram HPLC solvent.
Detailed description of the invention
Below in conjunction with drawings and Examples, the utility model is described in further detail.
Embodiment 1
With reference to Fig. 1, purification devices prepared by a kind of high-efficient liquid phase chromatogram HPLC solvent of the present utility model: include that remove impurity fills
Put, pre-distillation column 7, condensed in two stages system, vacuum rectification tower 14 and atmospheric distillation tower 20；Described knot screen includes former with methanol
Charging basket 1 connection premixing tank 2, add iodine device 3 and deposition filter 4；The described iodine device 3 that adds is arranged on above premixing tank 2, in advance
Mixed tank 2 adds iodine；Being provided with agitating device in described premixing tank 2, the bottom of premixing tank 2 is provided with the feed liquid conveying pipe of band pump, described
Feed liquid conveying pipe is connected with deposition filter 4；Described deposition filter 4 is provided with alkali liquor adding tube 6；Described deposition filter 4
Connect with the distillating still 5 of pre-distillation column 7；The top vent of described pre-distillation column 7 and condensed in two stages system connectivity；Condensed in two stages
The condensate discharge pipe of system connects with pre-tower backflash 8, then refluxes by being pumped back into pre-distillation column 7；Described pre-distillation column 7
Connected with the rectifying still 16 of vacuum rectification tower 14 by the first methanol conveying pipe 24 of band pump at the bottom of tower, the top of vacuum rectification tower 14
Air vent connects with water condenser 18；The condensate discharge pipe of water condenser 18 connects with rectification under vacuum backflash 15；Described subtract
Connected with the rectifying still 21 of atmospheric distillation tower 20 by the second methanol conveying pipe 23 at the bottom of pressure rectifying column 14 tower, atmospheric distillation tower 20
Top vent connects with water condenser 18,
Described high-efficient liquid phase chromatogram HPLC solvent is prepared purification devices and is also included that drying tube 13, described drying tube 13 are arranged on
Condensed in two stages system, the tail gas discharging pipe end of water condenser 18.Described condensed in two stages system, the cooling water of water condenser 18 enter
Mouth connects with technical cooling bucket 11.
Described rectification under vacuum backflash 15 and atmospheric pressure reflux groove 19 are stored up with hplc grade methanol storage tank 17, accident liquid by pipeline
Tank 22 connects.
Described condensed in two stages system includes primary condenser 9 and secondary condenser 10, and the gas of described primary condenser 9 leads to
With pre-distillation column 7 overhead vapor outlet in the middle part of road；The on-condensible gas outlet 12 of described primary condenser 9 and secondary condensation
Connect in the middle part of the secondary gas passage of device 10, bottom described primary condenser 9 and secondary condenser 10, be provided with discharging tube, described discharge opeing
Pipe connects with pre-tower backflash 8.
A kind of high-efficient liquid phase chromatogram HPLC solvent of the present embodiment prepares the purification devices method for methanol purification, with sky
So the industrial grade benzenemethanol of gas synthesis is as raw material, comprises the following steps:
1) remove impurity pretreatment: add the 4.0%(w/w of methanol weight in methanol feedstock) iodine, it is pumped to after stirring and evenly mixing
In the NaOH solution of 1.0mol/L, stand 12h after mixing, filter, remove ethanol, aldehyde and ketone impurity in methanol；
2) pre-distillation: filtrate pump is delivered to pre-distillation column 7 and distills, the operating condition of pre-distillation column 7: tower top temperature: 61
DEG C, reflux ratio: 1.2；Remove the boiling point impurity less than methanol；The tower top of pre-distillation column 7 uses the condensed in two stages system of series connection to enter
Row condensation, the liquid that condensation obtains enters pre-tower backflash 8, then is pumped to pre-distillation column 7 overhead reflux；
3) rectification under vacuum: the methanol solution deviating from light component flowed out bottom pre-distillation column 7 is pumped to vacuum rectification tower
Carry out rectification under vacuum in the rectifying still 16 of 14, remove the boiling point impurity higher than methanol；The operating condition of vacuum rectification tower 14: tower top
Temperature: 125 DEG C, pressure in tower: 0.55MPa, reflux ratio: 1.5；Vacuum rectification tower 14 top connects with water condenser 18；Decompression
A methanol solution part in rectifying column 14 sends vacuum rectification tower 14 overhead reflux back to through vacuum tower reflux pump, and methanol steam is water cooled
Rectification under vacuum backflash 15 is entered after condenser 18 condensation；Methanol in rectification under vacuum backflash 15 qualified methanol after analyzing send
Enter hplc grade methanol storage tank 17, in underproof feeding accident liquid storage tank 22；
4) atmospheric distillation: the methanol solution flowed out bottom vacuum rectification tower 14 utilizes pressure reduction feeding atmospheric distillation tower 20 to carry out
Rectification for the third time, removes the water in methanol solution and alcohols impurity；The operating condition of atmospheric distillation tower 20: tower top temperature: 65 DEG C,
Tower top pressure: 0.02MPa, reflux ratio: 1.5；The methanol steam condensed device condensation heel row of atmospheric distillation tower 20 tower top is to normal pressure
Backflash 19, the methanol that the methanol in atmospheric pressure reflux groove 19 is qualified after analyzing sends into hplc grade methanol storage tank 17, underproof
In feeding accident liquid storage tank 22.
The physicochemical property of the methanol that this device purification process obtains: methanol content >=99.99%, moisture w%≤0.01%；Steam
Send out residue≤0.002%；Carbonyl compound (in terms of CO): 0.005%, methanol yield >=97.5%.Ultraviolet under 254nm or 260nm
Absorbance≤0.01.
The operation principle of purification devices prepared by this utility model a kind of high-efficient liquid phase chromatogram HPLC solvent: knot screen leads to
Cross in methanol, add iodine, and in the basic conditions by the ethanol in methanol, aldehyde, the Impurity removal of ketone, then by pre-distillation column 7
Distillation, by the tower top temperature of control pre-distillation column 7 at 60 ~ 62 DEG C, by low boiling impurity in methanol (such as dimethyl ether, formic acid first
Ester etc.) remove；Then the methanol removing light component is passed through vacuum rectification tower 14 and carries out rectification, by controlling vacuum rectification tower 14
Tower top temperature at 120 ~ 125 DEG C, by high-boiling-point impurity in methanol (such as isopropanol, normal propyl alcohol, sec-butyl alcohol, isobutanol, positive fourth
Alcohol, dimethoxym ethane, ethyl acetate etc.) remove；Finally, then add the methanol solution at the bottom of vacuum rectification tower 14 tower and be re-fed into atmospheric distillation tower
Carry out third time rectification in 20, remove the trace impurity (such as water) in methanol, finally obtain and meet efficient liquid phase chromatographic analysis and want
The methanol asked.
Claims (4)
1. purification devices prepared by a high-efficient liquid phase chromatogram HPLC solvent, it is characterised in that include knot screen, pre-distillation column,
Condensed in two stages system, vacuum rectification tower and atmospheric distillation tower；Premixing tank that described knot screen includes connecting with methanol feedstock bucket,
Add iodine device and deposition filter；The described iodine device that adds is arranged on above premixing tank, adds iodine to premixing tank；In described premixing tank
Being provided with agitating device, the bottom of premixing tank is provided with the feed liquid conveying pipe of band pump, and described feed liquid conveying pipe is connected with deposition filter；
Described deposition filter is provided with alkali liquor adding tube；Described deposition filter connects with the distillating still of pre-distillation column；Described pre-steaming
Evaporate top vent and the condensed in two stages system connectivity of tower；The condensate discharge pipe of condensed in two stages system is with pre-tower backflash even
Logical, then reflux by being pumped back into pre-distillation column；By the first methanol conveying pipe and the decompression of band pump at the bottom of described pre-distillation column tower
The rectifying still connection of rectifying column, the top vent of vacuum rectification tower connects with water condenser；The condensate discharge of water condenser
Pipe connects with rectification under vacuum backflash；By the rectification of the second methanol conveying pipe with atmospheric distillation tower at the bottom of described vacuum rectification tower tower
Still connects, and the top vent of atmospheric distillation tower connects with water condenser.
2. purification devices prepared by high-efficient liquid phase chromatogram HPLC solvent as claimed in claim 1, it is characterised in that described efficient liquid phase
Chromatograph HPLC solvent is prepared purification devices and is also included that drying tube, described drying tube are arranged on condensed in two stages system, water condenser
Tail gas discharging pipe end.
3. as described in Claims 2 or 3, purification devices prepared by high-efficient liquid phase chromatogram HPLC solvent, it is characterised in that described decompression
Rectification backflash and atmospheric pressure reflux groove are connected with hplc grade methanol storage tank, accident liquid storage tank by pipeline.
4. as described in Claims 2 or 3, purification devices prepared by high-efficient liquid phase chromatogram HPLC solvent, it is characterised in that described two-stage
Condenser system includes primary condenser and secondary condenser, with pre-distillation column top in the middle part of the gas passage of described primary condenser
Steam (vapor) outlet connects；The on-condensible gas outlet of described primary condenser connects in the middle part of the secondary gas passage of secondary condenser,
Being provided with discharging tube bottom described primary condenser and secondary condenser, described discharging tube connects with pre-tower backflash.
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| CN201620134987.0U CN205528523U (en) | 2016-02-23 | 2016-02-23 | High performance liquid chromatography HPLC solvent preparation purification device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116785744A (en) * | 2023-06-25 | 2023-09-22 | 新疆广汇新能源有限公司 | High-efficiency crude methanol rectifying device and method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116785744A (en) * | 2023-06-25 | 2023-09-22 | 新疆广汇新能源有限公司 | High-efficiency crude methanol rectifying device and method |
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