CN107501031A - A kind of chromatographically pure n-hexane and preparation method thereof, production system - Google Patents
A kind of chromatographically pure n-hexane and preparation method thereof, production system Download PDFInfo
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- CN107501031A CN107501031A CN201710756073.7A CN201710756073A CN107501031A CN 107501031 A CN107501031 A CN 107501031A CN 201710756073 A CN201710756073 A CN 201710756073A CN 107501031 A CN107501031 A CN 107501031A
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
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- C07C7/005—Processes comprising at least two steps in series
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Abstract
A kind of chromatographically pure n-hexane and preparation method thereof, production system, it is related to chemical products technical field of purification, the preparation method is using technical grade n-hexane as raw material, carries out activated silica gel absorption, mixed acid nitration oxidation successively, wash depickling, dry, and rectifying is carried out in the presence of phosphorus pentoxide, the preparation method production cost is low, obtained chromatographically pure n-hexane quality better, yield are high, meet chromatographically pure reagent requirement.The production system includes adsorption tower, reactor, rectifying still, rectifying column and the finished pot being sequentially connected.For the production system dedicated for preparing chromatographically pure n-hexane, production efficiency is high, and obtained product purity is high, can realize the scale industrial production of chromatographically pure n-hexane.
Description
Technical field
The present invention relates to chemical products technical field of purification, in particular to a kind of chromatographically pure n-hexane and its preparation
Method, production system.
Background technology
Chromatographically pure refers to the standard reagent used during progress chromatography, and its UV transmittance at low wavelength compares
It is good, under chromatographic condition, only there is the peak of appointed compound, it is impossible to impurity peaks occur, chromatographically pure reagent purity is very high, except requiring
Beyond content height, also there is very high requirement to micronic dust, moisture, belong to the category of high purity reagent.Chromatographically pure n-hexane is conventional
One of liquid chromatogram mobile phase, its chromatographically pure market at home is mostly that external Reagent Company is monopolized, as Merck,
Sigma, Fisher, Tedia etc., their product, price is high, for chromatographically pure user, can cause too high cost
Consumption.
At present both at home and abroad it has been reported that the purifying process of a variety of n-hexanes, wherein main purification process includes：Decolourize,
Absorption, rectifying or decolouring/absorption-rectifying are combined, and its shortcoming is that yield is not high, or purity is not high, causes cost mistake
Height, or it is unsatisfactory for scientific research requirements.Therefore production cost is reduced, the quality of chromatographically pure n-hexane is improved, needs further to be improved.
Therefore, it is necessary to a kind of low n-hexane preparation method of production cost, and using chromatogram made from this method it is pure oneself
Alkane quality better, yield are high, can meet chromatographically pure reagent requirement.
The content of the invention
The first object of the present invention is to provide a kind of preparation method of chromatographically pure n-hexane, and the method production cost is low,
Obtained chromatographically pure n-hexane quality better, yield are high.
The second object of the present invention is to provide a kind of chromatographically pure n-hexane, and its quality better, yield are high, meets that chromatographically pure tries
Agent requirement.
The third object of the present invention is to provide a kind of production system of chromatographically pure n-hexane, and it is dedicated for preparing chromatogram
Pure hexane, realize the scale industrial production of chromatographically pure n-hexane.
The present invention is solved its technical problem and realized using following technical scheme.
A kind of preparation method of chromatographically pure n-hexane, it comprises the following steps：
Using technical grade n-hexane as raw material, activated silica gel absorption is carried out successively, mixed acid nitration oxidation, depickling is washed, does
It is dry, and rectifying is carried out in the presence of phosphorus pentoxide.
A kind of chromatographically pure n-hexane, it uses the preparation method of above-mentioned chromatographically pure n-hexane to be made.
A kind of production system of chromatographically pure n-hexane, it includes：
Adsorption tower, for carrying out activated silica gel absorption；
Reactor, washing depickling and the appearance dried are carried out for being reacted as addition mixed acid nitration, adding water
Device；
Rectifying still, rectifying column, for carrying out rectifying in the presence of phosphorus pentoxide；
Wherein, adsorption tower, reactor, rectifying still and rectifying column are sequentially connected with.
The beneficial effect of the embodiment of the present invention is：
The embodiments of the invention provide a kind of chromatographically pure n-hexane and preparation method thereof, the preparation method be by technical grade just
Hexane aoxidizes as raw material, successively progress activated silica gel absorption, mixed acid nitration, washs depickling, dries, and in phosphorus pentoxide
In the presence of carry out rectifying, the preparation method production cost is low, and obtained chromatographically pure n-hexane quality better, yield are high, meet chromatogram
Pure reagent requirement.
The embodiment of the present invention additionally provides a kind of production system of chromatographically pure n-hexane, and it includes the absorption being sequentially connected
Tower, reactor, rectifying still, rectifying column and finished pot.The production system is dedicated for preparing chromatographically pure n-hexane, production efficiency
Height, obtained product purity is high, can realize the scale industrial production of chromatographically pure n-hexane.
Brief description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below by embodiment it is required use it is attached
Figure is briefly described, it will be appreciated that the following drawings illustrate only certain embodiments of the present invention, therefore be not construed as pair
The restriction of scope, for those of ordinary skill in the art, on the premise of not paying creative work, can also be according to this
A little accompanying drawings obtain other related accompanying drawings.
A kind of schematic flow sheet of the production system for chromatographically pure n-hexane that Fig. 1 is provided by the embodiment of the present invention 1.
Icon：100- production systems；110- adsorption towers；111- feed pipes；120- reactors；130- rectifying stills；140-
Rectifying column；150- finished pots；160- condensers；170- return tanks.
Embodiment
, below will be in the embodiment of the present invention to make the purpose, technical scheme and advantage of the embodiment of the present invention clearer
Technical scheme be clearly and completely described.Unreceipted actual conditions person, builds according to normal condition or manufacturer in embodiment
The condition of view is carried out.Agents useful for same or the unreceipted production firm person of instrument, it is the conventional production that can be obtained by commercially available purchase
Product.
A kind of chromatographically pure n-hexane of the embodiment of the present invention and preparation method thereof, production system are carried out specifically below
It is bright.
The embodiments of the invention provide a kind of preparation method of chromatographically pure n-hexane, it comprises the following steps：
S1. activated silica gel absorption is carried out using technical grade n-hexane as raw material.
Further, it is continuous by the liquid phase entrance of absorption tower bottom by delivery pump using technical grade n-hexane as raw material
In input to adsorption tower.Activated silica gel is filled with adsorption tower, optionally, activated silica gel is that ZY-9150/ZY-880 types adsorb silicon
Glue, the interior periodic replacement adsorption silica gel of adsorption tower, it is ensured that the validity of absorption.Preferably, the quantity of adsorption tower can be it is multiple, it is more
Individual adsorption tower is arranged in parallel, and when partial adsorbates tower is in adsorbed state, remaining adsorption tower is in desorption state, so can be with
Guarantee has partial adsorbates tower to may be in adsorption operation all the time, to ensure the continuity of production.Meanwhile in adsorption process,
The feed flow of technical grade n-hexane is 3~8L/h, to ensure that technical grade n-hexane can sufficiently be connect with activated silica gel
Touch, reach preferable adsorption effect.
The embodiment of the present invention provides a kind of preparation method of chromatographically pure n-hexane, in addition to：
S2. the solution after activated silica gel is adsorbed carries out mixed acid nitration oxidation.
Mixed acid nitration is added in n-hexane after being adsorbed to activated silica gel, 0.5~2h is stirred under normal temperature, stands 1~3h,
Layering obtains n-hexane layer and nitration mixture layer.Nitration mixture layer is discharged, mixed acid nitration is added again into n-hexane layer, is stirred under normal temperature
0.5~2h, 1~3h is stood, is layered and discharges nitration mixture layer, repeat, untill the nitration mixture layer of discharge is colourless.Further
Ground, the amount for adding mixed acid nitration every time is 0.5~10wt% of technical grade n-hexane, can by a small amount of multiple addition manner
To obtain more preferable oxidation effectiveness, make the purity of final products higher.
Wherein, mixed acid nitration includes：30~70wt% the concentrated sulfuric acid, 10~40wt% concentrated nitric acid and 5~30wt%'s
Water.Found by the creative work of inventor, the mixed acid nitration formed by aforementioned proportion configuration, in oxidation, oxidation effect
Rate is higher, and oxidation effectiveness is preferable.
The embodiment of the present invention provides a kind of preparation method of chromatographically pure n-hexane, in addition to：
S3. the solution after mixed acid nitration is aoxidized carries out washing depickling, dries.
Washing the specific method of depickling is：N-hexane layer and water are mixed and stirred for 2~4h, stand 1~2h, discharges water
Layer, adds water and is repeated a number of times washing, it is preferable that washing times are 3~5 times.By washing, solution can be removed as far as possible
The acid of middle residual, it is easy to the further purification of subsequent step.
Further, drier is added into the solution after washing depickling, water removal is dried.Drier includes anhydrous chlorine
Change at least one of calcium, anhydrous sodium sulfate and anhydrous magnesium sulfate.The solution obtained after washing depickling, its water content are usually less than
Less than 1%, so the dosage of drier need not be too many.Preferably, drier can be distributed into parcel, be added to be dried molten
In liquid, stir and stand, then take out the drier of parcel, put it into thermal dehydration in closed baking oven, you can realize dry
The recycling of drying prescription, further reduces production cost.
The embodiment of the present invention provides a kind of preparation method of chromatographically pure n-hexane, in addition to：
S3. phosphorus pentoxide is added into dried solution, and carries out rectifying.
Distillation operation is carried out in rectifying still and rectifying column, by dried solution, is moved in rectifying still, in stirring
Under the conditions of add phosphorus pentoxide, in advance stir 0.5~1h.Start conduction oil circulating-heating, Oil-temperature control is at 100~150 DEG C, production
Raw gas is imported in rectifying column, starts recirculated cooling water, after starting backflow at the top of rectifying column, first 1~3h of infinite reflux, then
Start to produce.Further, reflux ratio is controlled 1~5 during extraction:1, extraction flow is 5~150L/h, removes front-end volatiles with after
Cut, it is qualified chromatographically pure n-hexane to take midbarrel.Preferably, the chromatographically pure n-hexane that collection obtains is passed through again
0.2~0.25 μm of tetrafluoro membrane filtration and barrelling.
The embodiment of the present invention additionally provides a kind of chromatographically pure n-hexane, and it uses the preparation method of above-mentioned chromatographically pure n-hexane
It is made.
The embodiment of the present invention additionally provides a kind of production system of chromatographically pure n-hexane, and it includes：
Adsorption tower, for carrying out activated silica gel absorption；
Reactor, washing depickling and the appearance dried are carried out for being reacted as addition mixed acid nitration, adding water
Device；
Rectifying still, rectifying column, for carrying out rectifying in the presence of phosphorus pentoxide；
Wherein, adsorption tower, reactor, rectifying still and rectifying column are sequentially connected with.
Further, in the other preferred embodiments of the present embodiment, production system also includes condenser, return tank and is used for
The finished pot of chromatographically pure n-hexane finished product is collected, the input of condenser connects with the gaseous phase outlet at the top of rectifying column, to incite somebody to action
The gas phase n-hexane being collected into is condensed into liquid；The output end of condenser is connected to the input of return tank, the output of return tank
End is respectively communicated to top and the finished pot of rectifying column.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
The present embodiment 1 provides a kind of production system 100 of chromatographically pure n-hexane, and shown in reference picture 1, it includes：Absorption
Tower 110, reactor 120, rectifying still 130, rectifying column 140 and finished pot 150.
Activated silica gel is filled with adsorption tower 110, the feed end of adsorption tower 110 connects with feed pipe 111, by feed pipe
The technical grade n-hexane that the conveying of road 111 comes is adsorbed in adsorption tower 110 by activated silica gel, removes fraction solids impurity therein.
Wherein, activated silica gel is industrial ZY-9150/ZY-880 types adsorption silica gel, is packed full with whole adsorption tower 110, meanwhile, adsorbing
The bottom of towe of tower 110 is provided with stainless steel cloth (not shown), and effective barrier can be formed to activated silica gel, prevents activated silica gel stream
Lose.In the present embodiment, the quantity of adsorption tower 110 is two, and two adsorption towers 110 are arranged in parallel, when one of adsorption tower
110 when being in desorption state, and another adsorption tower 110 is in adsorbed state, so that two adsorption towers 110 can be transported alternately
Make, realize continuous operation.It is worth noting that, in the other preferred embodiments of the present invention, the quantity of adsorption tower 110 can also root
According to being actually needed, it is arranged to multiple, and when the partial adsorbates tower 110 is in adsorbed state, another part adsorption tower 110 is in solution
Suction state, ensure continuous operation.
The discharge end of adsorption tower 110 connects with the feed end of reactor 120, and the solution after activated silica gel absorption is in reactor
Mixed acid nitration oxidation, washing depickling and the process dried are completed in 120.Reactor 120 is provided with paddle agitator, and (figure is not
Show), its rotating speed reaches more than 300rpm, and the material that it can be made internal is sufficiently mixed.In the present embodiment, reactor
120 quantity is two, and two reactors 120 are arranged in parallel, you can, can also to be used interchangeably to ensure the continuity of operation
Simultaneously using improving the whole efficiency of production.
The discharge end of reactor 120 connects with rectifying still 130, and the gaseous phase outlet at the top of rectifying still 130 is communicated to rectifying
The bottom of tower 140, completing dried solution will heat in rectifying still 130, and form gas phase and enter in rectifying column 140
Row rectifying.Rectifying still 130 is provided with paddle agitator, and its rotating speed reaches more than 300rpm, and its internal material can be made uniform
It is heated, improve the efficiency of gasification.In the present embodiment, the quantity of rectifying still 130 is two, and two rectifying stills 130 are arranged in parallel,
The continuity of operation can be used interchangeably to ensure, can also be used simultaneously to improve the whole efficiency of production.Further,
Rectifying still 130 is 100~5000L enamel glass chuck kettle, admittance deep fat heating heating in chuck.
The internal diameter of rectifying column 140 is 4~500cm, is highly 4~30m, filling glass spring filler, stainless steel west in tower
At least one of tower ring, stainless steel structured packing and ceramic packing.The bottom of rectifying column 140 is filled with one section of height as 0.5
~2m Anhydrous potassium carbonate filler.The gaseous phase outlet at the top of rectifying column 140 connects with the input of condenser 160, condenser 160
The gas phase n-hexane being collected into is condensed into liquid.The output end of condenser 160 is connected to the input of return tank 170, backflow
The output end of tank 170 is communicated to finished pot 150, and finished product is delivered to be collected to the chromatographically pure n-hexane obtained after condensation
Tank 150.Meanwhile return tank 170 connects with the top of rectifying column 140, part chromatographically pure n-hexane is back into rectifying column
140 top, to increase the efficiency of rectifying.
Embodiment 2
The present embodiment provides a kind of chromatographically pure n-hexane, and its preparation method is as follows：
S1. technical grade n-hexane (Jinzhou Petrochemical Company, purity >=98wt%) raw material is pumped into adsorption tower 110 by centrifugation
Bottom, via the activated silica gel adsorption-edulcoration in adsorption tower 110, flowed out by the top of adsorption tower 110 and be delivered to reactor
120.Wherein, technical grade n-hexane feed flow is：5L/h.
S2. after the technical grade n-hexane 50L after absorption being added into reactor 120, configuration is added into reactor 120
Good mixed acid nitration (distilled water of the 30wt% concentrated sulfuric acid, 40wt% concentrated nitric acid and 30wt%) 2.5L, start under normal temperature and stir
Mix, 0.5h is stirred under rotating speed 400rpm, then stands 1h, separate the nitration mixture layer of lower floor；2.5L is added again into reactor 120
Mixed acid nitration, 0.5h is stirred, separate nitration mixture layer after standing 1h, repeat, until the nitration mixture layer separated is colourless.
S3. the water for 5L being added into reactor 120 is washed, and stirs 1h, the water layer of lower floor is separated after standing 1h, is repeated
Operation 3 times.
S4. 1.5kg anhydrous calcium chlorides are added into reactor 120, anhydrous calcium chloride is distributed into parcel, adds reactor
In 120,1h is stirred, 1h is stood, is separated off calcium chloride, obtains rectifying stoste.
S5. above-mentioned rectifying stoste is delivered in rectifying still 130, and 100g phosphorus pentoxides is added into rectifying still 130,
Stir 0.5h.Start conduction oil circulating-heating, Oil-temperature control starts recirculated cooling water at 110 DEG C, when the top of rectifying column 140 is opened
Begin after backflow, infinite reflux 3h, then start to produce.During extraction, reflux ratio is controlled 3:1, remove front-end volatiles 0.2L and tails
0.5L, the midbarrel of extraction is qualified chromatographically pure n-hexane, and qualified chromatographically pure n-hexane yield reaches more than 98%.
S6. above-mentioned qualified chromatographically pure n-hexane is passed through into 0.22 μm of tetrafluoro membrane filtration, and barrelling is stand-by.
Embodiment 3
The present embodiment provides a kind of chromatographically pure n-hexane, and its preparation method is as follows：
S1. technical grade n-hexane (Jinzhou Petrochemical Company, purity >=98wt%) raw material is pumped into adsorption tower 110 by centrifugation
Bottom, via the activated silica gel adsorption-edulcoration in adsorption tower 110, flowed out by the top of adsorption tower 110 and be delivered to reactor
120.Wherein, technical grade n-hexane feed flow is：5L/h.
S2. after the technical grade n-hexane 500L after absorption being added into reactor 120, add and match somebody with somebody into reactor 120
Mixed acid nitration (distilled water of the 70wt% concentrated sulfuric acid, the 10wt% concentrated nitric acid and 20wt%) 25L put, start under normal temperature and stir
Mix, 0.5h is stirred under rotating speed 400rpm, then stands 1h, separate the nitration mixture layer of lower floor；25L is added again into reactor 120
Mixed acid nitration, 0.5h is stirred, separate nitration mixture layer after standing 1h, repeat, until the nitration mixture layer separated is colourless.
S3. the water for 50L being added into reactor 120 is washed, and stirs 2h, and the water layer of lower floor, weight are separated after standing 1h
Operate 3 times again.
S4. 15kg anhydrous calcium chlorides are added into reactor 120, anhydrous calcium chloride is distributed into parcel, adds reactor 120
It is interior, 1h is stirred, 1h is stood, separates calcium chloride, obtain rectifying stoste.
S5. above-mentioned rectifying stoste is delivered in rectifying still 130, and the oxidations of 1500g five two is added into rectifying still 130
Phosphorus, stir 0.5h.Start conduction oil circulating-heating, Oil-temperature control starts recirculated cooling water at 110 DEG C, when the top of rectifying column 140
After starting backflow, infinite reflux 3h, then start to produce.During extraction, reflux ratio is controlled 3:1, remove front-end volatiles 1.5L and evaporated with after
Divide 5L, the midbarrel of extraction is qualified chromatographically pure n-hexane, and qualified chromatographically pure n-hexane yield reaches more than 96%.
S6. above-mentioned qualified chromatographically pure n-hexane is passed through into 0.22 μm of tetrafluoro membrane filtration, and barrelling is stand-by.
Test example 1
Using the chromatographically pure n-hexane that embodiment 2 and 3 is provided as test specimen, its UV transmittance is examined
Survey, specific detection mode is as follows：
Test apparatus is：Shanghai spectrum ultraviolet specrophotometer SP-752 types, using 1cm quartz colorimetric utensils.Spectrophotometric
After meter start, after preheating 0.5h, start to detect, reference is done using redistilled water or deionized water, detect each test sample
UV transmittance of the product under 220nm, 230nm, 240nm, 250nm, 254nm and 260nm wavelength, the testing result such as institute of table 1
Show.
The UV transmittance testing result of the chromatographically pure n-hexane of table 1.
| Wavelength | 220nm | 230nm | 240nm | 250nm | 254nm | 260nm |
| Raw material | 65.5% | 77% | 87.4% | 92% | 92.5% | 93.4% |
| Embodiment 2 | 86.5% | 94.1% | 97.3% | 99.1% | 99.8% | 100% |
| Embodiment 3 | 87.3% | 94.6% | 97.7% | 99.5% | 99.8% | 100% |
| Chromatographically pure standard | >=80% | >=90% | >=95% | >=98% | >=98% | >=98% |
| Agriculture residual standard | >=80% | >=90% | >=95% | >=98% | >=98% | >=98% |
From table 1 it follows that the chromatographically pure n-hexane that the embodiment of the present invention 2 and 3 is provided is in 220~260nm wavelength
Under UV transmittance exceeded the chromatographically pure standard and agriculture residual standard of national setting, the system that the embodiment of the present invention is provided
Preparation Method and production equipment are preferable to the purification effect of n-hexane.
Test example 2
It is residual to its water content index, evaporation using the chromatographically pure n-hexane that embodiment 2 and 3 is provided as test specimen
Slag index and purity index are detected：Water content Indexs measure instrument model：Metrohm 831KF are led in Switzerland ten thousand；Steam
Send out residue Indexs measure instrument：Assay balance, evaporating dish, water bath with thermostatic control evaporation, baking oven；Instrument used in purity Indexs measure
Device：The flame ionization ditector (GC-FID) of the gas-chromatographies of Agilent 6890.Testing result is as shown in table 2：
Moisture, evaporation residue, the purity detecting result of the chromatographically pure n-hexane of table 2.
| Moisture | Evaporation residue | Purity | |
| Embodiment 2 | ≤ 0.01wt% | ≤ 0.003wt% | >=99.9wt% |
| Embodiment 3 | ≤ 0.01wt% | ≤ 0.003wt% | >=99.9wt% |
| Chromatographically pure standard | ≤ 0.02wt% | ≤ 0.005wt% | >=98wt% |
| Agriculture residual standard | ≤ 0.02wt% | ≤ 0.005wt% | >=98wt% |
As can be seen from Table 2, the moisture for the chromatographically pure n-hexane that the embodiment of the present invention 2 and 3 is provided is less than or equal to
0.01wt%, evaporation residue content are less than or equal to 0.003wt%, are below the chromatographically pure standard and the residual mark of agriculture of country's setting
It is accurate.The purity for the chromatographically pure n-hexane that the embodiment of the present invention 2 and 3 is provided reaches 99.9wt%, more than the chromatogram of country's setting
Pure standard and agriculture residual standard.It can be seen that the purifying of preparation method and production equipment that the embodiment of the present invention is provided to n-hexane
Effect is preferable.
In summary, the embodiments of the invention provide a kind of chromatographically pure n-hexane and preparation method thereof, the preparation method to be
Aoxidized technical grade n-hexane as raw material, successively progress activated silica gel absorption, mixed acid nitration, wash depickling, dry, and five
Aoxidize and carry out rectifying in the presence of two phosphorus, the preparation method production cost is low, obtained chromatographically pure n-hexane quality better, yield
Height, meet chromatographically pure reagent requirement.
The embodiment of the present invention additionally provides a kind of production system of chromatographically pure n-hexane, and it includes the absorption being sequentially connected
Tower, reactor, rectifying still, rectifying column and finished pot.The production system is dedicated for preparing chromatographically pure n-hexane, production efficiency
Height, obtained product purity is high, can realize the scale industrial production of chromatographically pure n-hexane.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.Within the spirit and principles of the invention, that is made any repaiies
Change, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (10)
1. a kind of preparation method of chromatographically pure n-hexane, it is characterised in that it comprises the following steps：
Aoxidized technical grade n-hexane as raw material, successively progress activated silica gel absorption, mixed acid nitration, wash depickling, dry, and
Rectifying is carried out in the presence of phosphorus pentoxide.
2. the preparation method of chromatographically pure n-hexane according to claim 1, it is characterised in that carry out technical grade n-hexane
Activated silica gel absorption is that the technical grade n-hexane is adsorbed using the adsorption tower filled with activated silica gel, it is preferable that institute
The feed flow for stating technical grade n-hexane is 3~8L/h.
3. the preparation method of chromatographically pure n-hexane according to claim 1, it is characterised in that the mixed acid nitration includes：
30~70wt% the concentrated sulfuric acid, 10~40wt% concentrated nitric acid and 5~30wt% water.
4. the preparation method of chromatographically pure n-hexane according to claim 3, it is characterised in that mixed acid nitration oxidation is to pass through
The technical grade n-hexane crossed after active silica gel absorption is mixed with the mixed acid nitration, and 0.5~2h is stirred under normal temperature, stands 1
~3h, layering obtain n-hexane layer and nitration mixture layer, discharge nitration mixture layer；The mixed acid nitration will be continuously added in the n-hexane layer
And standing is stirred, discharge nitration mixture layer；Repeat until the nitration mixture layer of discharge is colourless.
5. the preparation method of chromatographically pure n-hexane according to claim 1, it is characterised in that after being aoxidized to mixed acid nitration
It is that the solution after mixed acid nitration is aoxidized mixes with water that solution, which carries out washing depickling, stands heel row water-yielding stratum, it is preferable that stir
It is 2~4h to mix the time, and time of repose is 1~2h, it is preferable that is repeated a number of times washing.
6. the preparation method of chromatographically pure n-hexane according to claim 1, it is characterised in that to the solution after washing depickling
The specific method being dried is：Solution after washing depickling is mixed into 1~2h with anhydrous calcium chloride, stands 1~2h.
7. the preparation method of chromatographically pure n-hexane according to claim 1, it is characterised in that carry out the specific method of rectifying
It is：Phosphorus pentoxide is added in solution after the drying, and carries out heating rectifying, caused gas passes through rectifying column, establishes complete
Backflow, infinite reflux 1~3 hour, starts to produce, the certified products of extraction are finished product.
8. a kind of chromatographically pure n-hexane, it is characterised in that it uses the chromatogram as any one of claim 1 to 7 pure
The preparation method of hexane is made.
9. a kind of production system of chromatographically pure n-hexane, it is characterised in that it includes：
Adsorption tower, for carrying out activated silica gel absorption；
Reactor, washing depickling and the appearance dried are carried out for being reacted as the addition mixed acid nitration, adding water
Device；
Rectifying still, rectifying column, for carrying out rectifying in the presence of phosphorus pentoxide；
Wherein, the adsorption tower, the reactor, the rectifying still and the rectifying column are sequentially connected with.
10. the production system of chromatographically pure n-hexane according to claim 9, it is characterised in that the production system is also wrapped
Include condenser, return tank and the finished pot for collecting chromatographically pure n-hexane finished product, the input of the condenser and the essence
The gaseous phase outlet connection of top of tower is evaporated, the gas phase being collected into n-hexane is condensed into liquid；The output end of the condenser
Be connected to the input of the return tank, the output end of the return tank be respectively communicated to the rectifying column top and it is described into
Product tank.
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| CN108017504A (en) * | 2018-01-26 | 2018-05-11 | 上海星可高纯溶剂有限公司 | The method of purification of n-hexane |
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