CN107522678A - A kind of chromatogram pure tetrahydrofuran and preparation method thereof, production system - Google Patents
A kind of chromatogram pure tetrahydrofuran and preparation method thereof, production system Download PDFInfo
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- CN107522678A CN107522678A CN201710761073.6A CN201710761073A CN107522678A CN 107522678 A CN107522678 A CN 107522678A CN 201710761073 A CN201710761073 A CN 201710761073A CN 107522678 A CN107522678 A CN 107522678A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/04—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having no double bonds between ring members or between ring members and non-ring members
- C07D307/06—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having no double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to ring carbon atoms
- C07D307/08—Preparation of tetrahydrofuran
Abstract
A kind of chromatogram pure tetrahydrofuran and preparation method thereof, production system, are related to chemical products technical field of purification, and the preparation method is using Industrial Grade Tetrahydrofuran as raw material, carries out 4A molecular sieve adsorptions successively, activated alumina absorption, obtains reaction solution；Reaction solution is subjected to reduction treatment, charcoal absorption, obtains rectifying stoste, then rectifying is carried out to rectifying stoste.The preparation method production cost is low, and obtained chromatogram pure tetrahydrofuran quality better, yield are high, meet chromatographically pure reagent requirement.The production system includes 4A molecular sieve columns, activated alumina column, Na-K alloy post and the active carbon adsorption column being arranged in parallel.The gaseous phase outlet of reactor is communicated to the gas phase entrance of rectifier bottoms.For the production system dedicated for preparing chromatogram pure tetrahydrofuran, production efficiency is high, and obtained product purity is high, can realize the scale industrial production of chromatogram pure tetrahydrofuran.
Description
Technical field
The present invention relates to chemical products technical field of purification, in particular to a kind of chromatogram pure tetrahydrofuran and its system
Preparation Method, production system.
Background technology
Chromatographically pure refers to the standard reagent used during progress chromatography, and its ultraviolet absorptivity at low wavelength compares
It is low, 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.Chromatogram pure tetrahydrofuran is normal
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.
The tetrahydrofuran purifying process of domestic report is also seldom at present, and existing purifying process is all more complex and high cost,
Chromatogram pure tetrahydrofuran technique is monopolized by foreign countries for a long time.Therefore, break up monopoly, reduce cost, it is low to develop a kind of production cost,
And obtained chromatogram pure tetrahydrofuran quality better, yield are high, the new preparation process of chromatographically pure reagent requirement can be met, had very high
Economic benefit.
The content of the invention
The first object of the present invention is to provide a kind of preparation method of chromatogram pure tetrahydrofuran, the method production cost
Low, obtained chromatogram pure tetrahydrofuran quality better, yield are high.
The second object of the present invention is to provide a kind of chromatogram pure tetrahydrofuran, and its quality better, yield are high, meet chromatographically pure
Reagent requirement.
The third object of the present invention is to provide a kind of production system of chromatogram pure tetrahydrofuran, and it is dedicated for preparing color
Pure tetrahydrofuran is composed, realizes the scale industrial production of chromatogram pure tetrahydrofuran.
The present invention is solved its technical problem and realized using following technical scheme.
A kind of preparation method of chromatogram pure tetrahydrofuran, it includes：
Using Industrial Grade Tetrahydrofuran as raw material, 4A molecular sieve adsorptions are carried out successively, activated alumina absorption, are reacted
Liquid；Reaction solution is subjected to reduction treatment, charcoal absorption, obtains rectifying stoste；Rectifying is carried out to rectifying stoste.
A kind of chromatogram pure tetrahydrofuran, it uses the preparation method of above-mentioned chromatogram pure tetrahydrofuran to be made.
A kind of production system of chromatogram pure tetrahydrofuran, it includes：
Reactor, heated for accommodating Industrial Grade Tetrahydrofuran, and to Industrial Grade Tetrahydrofuran；
4A molecular sieve columns, for carrying out 4A molecular sieve adsorption processing to Industrial Grade Tetrahydrofuran；
Activated alumina column, for carrying out activated alumina adsorption treatment to Industrial Grade Tetrahydrofuran；
Na-K alloy post, for carrying out reduction treatment to Industrial Grade Tetrahydrofuran；
Active carbon adsorption column, for carrying out charcoal absorption processing to Industrial Grade Tetrahydrofuran；
Rectifying column, for carrying out rectifying to gas phase tetrahydrofuran；
Circulating pump, power is provided for the flowing of Industrial Grade Tetrahydrofuran；
Wherein, 4A molecular sieve columns, activated alumina column, Na-K alloy post, active carbon adsorption column are arranged in parallel, and respectively with
Circulating pump and reactor form circulation line；The gaseous phase outlet of reactor is communicated to the gas phase entrance of rectifier bottoms.
The beneficial effect of the embodiment of the present invention is：
The embodiments of the invention provide a kind of chromatogram pure tetrahydrofuran and preparation method thereof, the preparation method is by technical grade
Tetrahydrofuran carries out 4A molecular sieve adsorptions, activated alumina absorption, obtains reaction solution successively as raw material；Reaction solution is carried out
Reduction treatment, charcoal absorption, obtain rectifying stoste；Rectifying is carried out to rectifying stoste.The preparation method production cost is low, is made
Chromatogram pure tetrahydrofuran quality better, yield it is high, meet chromatographically pure reagent requirement.
The embodiment of the present invention additionally provides a kind of production system of chromatogram pure tetrahydrofuran, and it includes 4A points be arranged in parallel
Son sieve post, activated alumina column, Na-K alloy post and active carbon adsorption column, 4A molecular sieve columns, activated alumina column, Na-K alloy
Post, active carbon adsorption column form circulation line with circulating pump and reactor respectively.The gaseous phase outlet of reactor is communicated to rectifying column
The gas phase entrance of bottom.The production system is dedicated for preparing chromatogram pure tetrahydrofuran, and production efficiency is high, obtained product purity
Height, the scale industrial production of chromatogram pure tetrahydrofuran can be realized.
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 chromatogram pure tetrahydrofuran that Fig. 1 is provided by the embodiment of the present invention 1.
Icon：100- production systems；110- reactors；111- feed pipes；120- circulating pumps；131-4A molecular sieve columns；
132- activated alumina columns；133- Na-K alloy posts；134- active carbon adsorption columns；140- rectifying columns；150- condensers；160- is returned
Flow tank；170- finished pots；180- cation exchange columns；190- filters.
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 chromatogram pure tetrahydrofuran 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 chromatogram pure tetrahydrofuran, it includes：
S1. using Industrial Grade Tetrahydrofuran as raw material, 4A molecular sieve adsorptions are carried out successively, activated alumina absorption, are obtained
Reaction solution.
Tetrahydrofuran is a kind of aprotic solvents of middle polarity, and it is a kind of colourless, low viscosity liquid, has class
Like the smell of ether.In room temperature, itself and water energy partial miscibility.Contain more moisture in Industrial Grade Tetrahydrofuran, to it
, it is necessary to preferentially handle moisture when being purified.In embodiments of the present invention, successively using 4A molecular sieves and active oxidation
Aluminium Industrial Grade Tetrahydrofuran is dried water removal.4A molecular sieves are a kind of alkali metal aluminosilicates, can adsorb water, NH3、
H2S, sulfur dioxide, carbon dioxide, C2H5OH、C2H6、C2H4It is not more than 4A molecule Deng cut off diameter, it has preferably water removal
Effect, it is the dehydration reagent commonly used in organic chemistry.And activated alumina is a kind of porous, the solid material of high degree of dispersion,
It has very big surface area, is a kind of efficient drying agent that depth drying is carried out to minor amount of water.Water conservancy project is removed by priority twice
After skill, the moisture in Industrial Grade Tetrahydrofuran can be removed preferably, and purer tetrahydrofuran is obtained beneficial to follow-up rectifying.
Alternatively, it is that Industrial Grade Tetrahydrofuran is passed through into 4A molecular sieves to carry out 4A molecular sieve adsorptions to Industrial Grade Tetrahydrofuran
Circulation absorption is carried out in post, circulation power can be provided by circulating pump, and circulation time is 16~36h, Industrial Grade Tetrahydrofuran
Flow velocity in 4A molecular sieve columns is 0.1~2m/s.Inventor has found by itself creative work, in the flow velocity and circulation
Between in the range of, Industrial Grade Tetrahydrofuran can be enable sufficiently to be contacted with the 4A molecular sieves in 4A molecular sieve columns, so as to
Reach a preferable water removal effect.
Alternatively, it is that the Industrial Grade Tetrahydrofuran after 4A molecular sieve adsorptions is passed through into work to carry out activated alumina absorption
Property alumina column in carry out circulation absorption, circulation power can be provided by circulating pump, and circulation time is 3~6h, by 4A point
Flow velocity of the Industrial Grade Tetrahydrofuran in activated alumina column after son sieve absorption is 0.1~2m/s.Inventor creates by itself
The property made work is found, is adsorbed using activated alumina, can further improve water removal on the basis of the water removal of 4A molecular sieves
Effect, to reach the requirement of chromatographically pure.Meanwhile in the flow velocity and in the range of circulation time, Industrial Grade Tetrahydrofuran can be enable
It is enough sufficiently to be contacted with the activated alumina in activated alumina column, so as to further lift the effect of water removal.
The embodiment of the present invention provides a kind of preparation method of chromatogram pure tetrahydrofuran, in addition to：
S2. reaction solution is subjected to reduction treatment, charcoal absorption, obtains rectifying stoste.
By in the Industrial Grade Tetrahydrofuran deposited for a long time, often containing peroxide, directly use can be to using effect
Impact, or even induce safety problem.Reduction treatment is carried out to it, peroxide can be reduced, so as to remove peroxidating
Thing.
Alternatively, it is that reaction solution is passed through in Na-K alloy post to circulate to carry out reduction treatment to reaction solution, and circulation is dynamic
Power can be provided by circulating pump, and benzophenone is added after circulating 3~6h, and continue cycling through 2~3h, and reaction solution is in Na-K alloy
Flow velocity in post is 0.1~2m/s.Benzophenone is used as indicator, and carbonyl freedom can be generated in Industrial Grade Tetrahydrofuran
Base, the presence of free radical allow it to become au bleu, and the then presence of peroxide can be quenched carbonyl radical and make blue disappearance.Add
After entering benzophenone, solution occur blueness, that is, represent peroxide substantially on be reduced.By the creative labor of inventor
It is dynamic to find, in the flow velocity and in the range of circulation time, reaction solution can be enable to be filled with the sodium in Na-K alloy post and potassium
The contact divided, makes peroxide sufficiently be reduced.
Further, before reduction treatment is carried out to reaction solution, reaction solution is first heated to 60~70 DEG C, then by reaction solution
It is passed through in Na-K alloy post.With the rise of temperature, the speed of peroxide and sodium and nak response is faster, can improve reduction effect
Rate.
It is that the reaction solution after reduction treatment is passed into active carbon adsorption column to carry out circulation absorption to carry out charcoal absorption,
Until obtained rectifying stoste is colourless.Activated carbon has the function of decolourizing, and can reduce solution further by adsorption-edulcoration
In impurity.Preferably, flow velocity of the reaction solution after reduction treatment in active carbon adsorption column is 0.1~2m/s.In the flow
In the range of, the reaction solution after reduction treatment can be enable sufficiently to be contacted with activated carbon, improve the effect of adsorption-edulcoration.
The embodiment of the present invention provides a kind of preparation method of chromatogram pure tetrahydrofuran, in addition to：
S3. rectifying is carried out to rectifying stoste.
It is that rectifying is heated at 90~130 DEG C to carry out rectifying to rectifying stoste, and caused gas passes through rectifying column, is established complete
Backflow, infinite reflux 3~5 hours, starts to produce, and reflux ratio control is 5~1 during extraction：1, flow is controlled in 0.3~150L/h,
After removing front-end volatiles and tails, the certified products that midbarrel is extraction, namely required chromatogram pure tetrahydrofuran are taken.It is preferred that
Ground, the chromatogram pure tetrahydrofuran that can obtain collection do further pure by cation exchange column and 200nm filters again
Change, the purity of product is further lifted.
Preferably, the whole process of purification of Industrial Grade Tetrahydrofuran is carried out under nitrogen protection.Nitrogen protection can be kept away
Exempt from the oxygen in tetrahydrofuran and air to react generation peroxide, ensure the quality of purifying.
The embodiment of the present invention additionally provides a kind of chromatogram pure tetrahydrofuran, and it uses the preparation of above-mentioned chromatogram pure tetrahydrofuran
Method is made.
The embodiment of the present invention additionally provides a kind of production system of chromatogram pure tetrahydrofuran, and it includes：
Reactor, heated for accommodating Industrial Grade Tetrahydrofuran, and to Industrial Grade Tetrahydrofuran；
4A molecular sieve columns, for carrying out 4A molecular sieve adsorption processing to Industrial Grade Tetrahydrofuran；
Activated alumina column, for carrying out activated alumina adsorption treatment to Industrial Grade Tetrahydrofuran；
Na-K alloy post, for carrying out reduction treatment to Industrial Grade Tetrahydrofuran；
Active carbon adsorption column, for carrying out charcoal absorption processing to Industrial Grade Tetrahydrofuran；
Rectifying column, for carrying out rectifying to gas phase tetrahydrofuran；
Circulating pump, power is provided for the flowing of Industrial Grade Tetrahydrofuran；
Wherein, 4A molecular sieve columns, activated alumina column, Na-K alloy post, active carbon adsorption column are arranged in parallel, and respectively with
Circulating pump and reactor form circulation line；The gaseous phase outlet of reactor is communicated to the gas phase entrance of rectifier bottoms.
Further, in the other preferred embodiments of the present invention, production system also includes condenser, return tank and for receiving
Collect the finished pot of chromatogram pure tetrahydrofuran finished product, the input of condenser connects with the gaseous phase outlet at the top of rectifying column, to incite somebody to action
The gas phase tetrahydrofuran being collected into is condensed into liquid；The output end of condenser is connected to the input of return tank, return tank it is defeated
Go out top and finished pot that end is respectively communicated to 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 chromatogram pure tetrahydrofuran, and shown in reference picture 1, it includes：Instead
Answer kettle 110,4A molecular sieve columns 131, activated alumina column 132, Na-K alloy post 133, active carbon adsorption column 134, rectifying column 140
With circulating pump 120.
Wherein, between 4A molecular sieve columns 131, activated alumina column 132, Na-K alloy post 133, active carbon adsorption column 134
It is arranged in parallel, and forms circulation line with circulating pump 120 and reactor 110 respectively.Further, the input of circulating pump 120
Connected with the liquid-phase outlet of the bottom of reactor 110, the output end of circulating pump 120 is respectively communicated to 4A molecular sieve columns 131, active oxygen
Change aluminium post 132, Na-K alloy post 133, the feed end of active carbon adsorption column 134, and 4A molecular sieve columns 131, activated alumina
Post 132, Na-K alloy post 133, the feed end of active carbon adsorption column 134 are provided with the opening and closing of its feed end of Valve controlling.4A
Molecular sieve column 131, activated alumina column 132, Na-K alloy post 133, the discharge end of active carbon adsorption column 134 are communicated to reaction
The feed end of kettle 110, such 4A molecular sieve columns 131, activated alumina column 132, Na-K alloy post 133, active carbon adsorption column 134
In any one can with circulating pump 120, reactor 110 formed circulation line.Also, the control for passing through valve, you can
Switching Industrial Grade Tetrahydrofuran completes circulation in any one circulation line.
The feed end of reactor 110 connects with feed pipe 111, by feed pipe 111 convey Lai technical grade tetrahydrochysene furan
Mutter reactor 110 and 4A molecular sieve columns 131, activated alumina column 132, Na-K alloy post 133, active carbon adsorption column 134 it
Between circulate, complete the steps such as 4A molecular sieve adsorptions, activated alumina absorption, reduction treatment, charcoal absorption, and in reactor
The gaseous component containing tetrahydrofuran is thermally formed in 110.Wherein, reactor 110 is preferably to use enamel glass jacketed reaction
Kettle 110, in chuck can admittance deep fat reactor 110 is heated.Reactor 110 is provided with paddle agitator (not shown),
Its rotating speed reaches more than 300rpm, and the material that it can be made internal is sufficiently mixed.
The gaseous phase outlet at the top of reactor 110 is communicated to the gas phase entrance of the bottom of rectifying column 140, is produced in reactor 110
The gaseous component containing tetrahydrofuran rectifying column 140 is entered by the gas phase entrance of the bottom of rectifying column 140, and in rectifying column 140
Middle completion rectifying.The internal diameter of rectifying column 140 is 4~500cm, is highly 4~30m, filling glass spring filler, stainless steel in tower
At least one of western tower ring, stainless steel structured packing and ceramic packing.The bottom of rectifying column 140 is filled with one section of height
0.5~2m Anhydrous potassium carbonate filler.
Production system 100 also includes condenser 150, return tank 160 and finished pot 170, and the gas phase at the top of rectifying column 140 goes out
Mouth is connected with the input of condenser 150, and the gas phase tetrahydrofuran being collected into is condensed into liquid by condenser 150.Condenser 150
Output end be connected to the input of return tank 160, the output end of return tank 160 is communicated to finished pot 170, after to condensation
Obtained chromatogram pure tetrahydrofuran, which is collected, is delivered to finished pot 170.Meanwhile the top of return tank 160 and rectifying column 140 connects
It is logical, part chromatogram pure tetrahydrofuran to be back to the top of rectifying column 140, to increase the efficiency of rectifying.
Production system 100 also includes cation exchange column 180 and filter 190,200nm filter 190, and cation is handed over
Change post 180 and filter 190 further to final products can be purified, improve product purity.
Embodiment 2
The present embodiment provides a kind of chromatogram pure tetrahydrofuran, and its preparation method is as follows：
S1. under nitrogen protection, into reactor 110 import 50L Industrial Grade Tetrahydrofuran (Jinzhou Petrochemical Company, purity >=
98wt%) raw material, open the valve of 4A molecular sieve columns 131, establish reactor 110, circulating pump 120 and 4A molecular sieve columns 131 it
Between circulation, coutroi velocity 2m/s, circulation time 16h.
S2. the valve of 4A molecular sieve columns 131 is closed, the valve of activated alumina column 132 is opened, establishes reactor 110, follows
Circulation between ring pump 120 and activated alumina column 132, coutroi velocity 2m/s, circulation time 3h.
S3. the valve of activated alumina column 132 is closed, the temperature of reactor 110 is risen to 63 DEG C, and open Na-K alloy
The valve of post 133, the circulation established between reactor 110, circulating pump 120 and Na-K alloy post 133, coutroi velocity 2m/s, is followed
Ring time 3h, 500g benzophenone is added into reactor 110, continues cycling through 2h.
S4. the valve of Na-K alloy post 133 is closed, the valve of active carbon adsorption column 134 is opened, establishes reactor 110, follows
Circulation between ring pump 120 and active carbon adsorption column 134, coutroi velocity 2m/s, until the blueness of solution disappears in reactor 110
When stop circulation.
S5. the temperature of reactor 110 is risen to 100 DEG C, maintains rectifying pressure within 20kPa, when the top of rectifying column 140
After starting backflow, infinite reflux 5h, then start to produce.During extraction, reflux ratio is controlled 5:1, remove front-end volatiles 0.5L and evaporated with after
Divide 0.8L, the midbarrel of extraction is qualified chromatogram pure tetrahydrofuran, and qualified chromatogram pure tetrahydrofuran yield reaches
More than 95%.
S6. above-mentioned qualified chromatogram pure tetrahydrofuran is passed sequentially through into cation exchange column 180 and 200nm filters
190, and barrelling is stand-by.
Embodiment 3
The present embodiment provides a kind of chromatogram pure tetrahydrofuran, and its preparation method is as follows：
S1. under nitrogen protection, into reactor 110 import 50L Industrial Grade Tetrahydrofuran (Jinzhou Petrochemical Company, purity >=
98wt%) raw material, open the valve of 4A molecular sieve columns 131, establish reactor 110, circulating pump 120 and 4A molecular sieve columns 131 it
Between circulation, coutroi velocity 0.1m/s, circulation time 36h.
S2. the valve of 4A molecular sieve columns 131 is closed, the valve of activated alumina column 132 is opened, establishes reactor 110, follows
Circulation between ring pump 120 and activated alumina column 132, coutroi velocity 0.1m/s, circulation time 6h.
S3. the valve of activated alumina column 132 is closed, the temperature of reactor 110 is risen to 60 DEG C, and open Na-K alloy
The valve of post 133, the circulation established between reactor 110, circulating pump 120 and Na-K alloy post 133, coutroi velocity 0.1m/s,
Circulation time 3h, 500g benzophenone is added into reactor 110, continues cycling through 3h.
S4. the valve of Na-K alloy post 133 is closed, the valve of active carbon adsorption column 134 is opened, establishes reactor 110, follows
Circulation between ring pump 120 and active carbon adsorption column 134, coutroi velocity 0.1m/s, until the blueness of solution disappears in reactor 110
Stop circulation during mistake.
S5. the temperature of reactor 110 is risen to 90 DEG C, maintains rectifying pressure within 20kPa, when the top of rectifying column 140
After starting backflow, infinite reflux 3h, then start to produce.During extraction, reflux ratio is controlled 1:1, remove front-end volatiles 0.5L and evaporated with after
Divide 0.8L, the midbarrel of extraction is qualified chromatogram pure tetrahydrofuran, and qualified chromatogram pure tetrahydrofuran yield reaches
More than 95%.
S6. above-mentioned qualified chromatogram pure tetrahydrofuran is passed sequentially through into cation exchange column 180 and 200nm filters
190, and barrelling is stand-by.
Embodiment 4
The present embodiment provides a kind of chromatogram pure tetrahydrofuran, and its preparation method is as follows：
S1. under nitrogen protection, into reactor 110 import 500L Industrial Grade Tetrahydrofuran (Jinzhou Petrochemical Company, purity >=
98wt%) raw material, open the valve of 4A molecular sieve columns 131, establish reactor 110, circulating pump 120 and 4A molecular sieve columns 131 it
Between circulation, coutroi velocity 2m/s, circulation time 24h.
S2. the valve of 4A molecular sieve columns 131 is closed, the valve of activated alumina column 132 is opened, establishes reactor 110, follows
Circulation between ring pump 120 and activated alumina column 132, coutroi velocity 1m/s, circulation time 3h.
S3. the valve of activated alumina column 132 is closed, the temperature of reactor 110 is risen to 63 DEG C, and open Na-K alloy
The valve of post 133, the circulation established between reactor 110, circulating pump 120 and Na-K alloy post 133, coutroi velocity 1m/s, is followed
Ring time 6h, 500g benzophenone is added into reactor 110, continues cycling through 3h.
S4. the valve of Na-K alloy post 133 is closed, the valve of active carbon adsorption column 134 is opened, establishes reactor 110, follows
Circulation between ring pump 120 and active carbon adsorption column 134, coutroi velocity 1m/s, until the blueness of solution disappears in reactor 110
When stop circulation.
S5. the temperature of reactor 110 is risen to 130 DEG C, maintains rectifying pressure within 20kPa, 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 5L and tails
10L, the midbarrel of extraction is qualified chromatogram pure tetrahydrofuran, qualified chromatogram pure tetrahydrofuran yield reach 95% with
On.
S6. above-mentioned qualified chromatogram pure tetrahydrofuran is passed sequentially through into cation exchange column 180 and 200nm filters
190, and barrelling is stand-by.
Test example 1
Using the chromatogram pure tetrahydrofuran that embodiment 2~4 is provided as test specimen, its ultraviolet absorptivity 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
Ultraviolet absorptivity of the product under 210nm, 215nm, 230nm and 254nm wavelength, testing result are as shown in table 1.
The ultraviolet absorptivity testing result of the chromatogram pure tetrahydrofuran of table 1.
From table 1 it follows that the chromatogram pure tetrahydrofuran that the embodiment of the present invention 2~4 is provided is in 210~254nm ripples
Ultraviolet absorptivity under long reaches the chromatographically pure standard and agriculture residual standard of country's setting, the system that the embodiment of the present invention is provided
Preparation Method and production equipment are preferable to the purification effect of tetrahydrofuran.
Test example 2
Using the chromatogram pure tetrahydrofuran that embodiment 2~4 is provided as test specimen, to its water content index, evaporation
Residue index and purity index are detected：Water content Indexs measure instrument model：Metrohm 831KF are led in Switzerland ten thousand；
Evaporation 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 chromatogram pure tetrahydrofuran of table 2.
As can be seen from Table 2, the moisture for the chromatogram pure tetrahydrofuran that the embodiment of the present invention 2~4 is provided reaches
0.001wt%, evaporation residue content are less than or equal to 0.0003wt%, are below the chromatographically pure standard and the residual mark of agriculture of country's setting
It is accurate.The purity for the chromatogram pure tetrahydrofuran that the embodiment of the present invention 2~4 is provided reaches 99.9wt%, more than the color of country's setting
Compose pure standard and agriculture residual standard.It can be seen that preparation method and production equipment that the embodiment of the present invention is provided are to tetrahydrofuran
Purification effect is preferable.
In summary, the embodiments of the invention provide a kind of chromatogram pure tetrahydrofuran and preparation method thereof, the preparation method
It is using Industrial Grade Tetrahydrofuran as raw material, carries out 4A molecular sieve adsorptions successively, activated alumina absorption, obtain reaction solution；Will
Reaction solution carries out reduction treatment, charcoal absorption, obtains rectifying stoste；Rectifying is carried out to rectifying stoste.The preparation method produces
Cost is low, and obtained chromatogram pure tetrahydrofuran quality better, yield are high, meet chromatographically pure reagent requirement.
The embodiment of the present invention additionally provides a kind of production system of chromatogram pure tetrahydrofuran, and it includes 4A points be arranged in parallel
Son sieve post, activated alumina column, Na-K alloy post and active carbon adsorption column, 4A molecular sieve columns, activated alumina column, Na-K alloy
Post, active carbon adsorption column form circulation line with circulating pump and reactor respectively.The gaseous phase outlet of reactor is communicated to rectifying column
The gas phase entrance of bottom.The production system is dedicated for preparing chromatogram pure tetrahydrofuran, and production efficiency is high, obtained product purity
Height, the scale industrial production of chromatogram pure tetrahydrofuran can be realized.
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 chromatogram pure tetrahydrofuran, it is characterised in that it includes：
Using Industrial Grade Tetrahydrofuran as raw material, 4A molecular sieve adsorptions are carried out successively, activated alumina absorption, obtain reaction solution；
The reaction solution is subjected to reduction treatment, charcoal absorption, obtains rectifying stoste；Rectifying is carried out to the rectifying stoste.
2. the preparation method of chromatogram pure tetrahydrofuran according to claim 1, it is characterised in that to the technical grade tetrahydrochysene
It is that the Industrial Grade Tetrahydrofuran is passed through in 4A molecular sieve columns to carry out circulation absorption that furans, which carries out 4A molecular sieve adsorptions, during circulation
Between be 16~36h, it is preferable that flow velocity of the Industrial Grade Tetrahydrofuran in the 4A molecular sieve columns is 0.1~2m/s.
3. the preparation method of chromatogram pure tetrahydrofuran according to claim 2, it is characterised in that carry out activated alumina suction
Attached is that the Industrial Grade Tetrahydrofuran after 4A molecular sieve adsorptions is passed through in activated alumina column to carry out circulation absorption, is followed
The ring time is 3~6h, it is preferable that the Industrial Grade Tetrahydrofuran after 4A molecular sieve adsorptions is in the activated alumina column
In flow velocity be 0.1~2m/s.
4. the preparation method of chromatogram pure tetrahydrofuran according to claim 1, it is characterised in that carried out to the reaction solution
Reduction treatment is that the reaction solution is passed through in Na-K alloy post to be circulated, and adds benzophenone after circulating 3~6h, and continue
Circulate 2~3h, it is preferable that flow velocity of the reaction solution in the Na-K alloy post is 0.1~2m/s.
5. the preparation method of chromatogram pure tetrahydrofuran according to claim 4, it is characterised in that enter to the reaction solution
Before row reduction treatment, the reaction solution is first heated to 60~70 DEG C, then the reaction solution is passed through in the Na-K alloy post.
6. the preparation method of chromatogram pure tetrahydrofuran according to claim 1, it is characterised in that carrying out charcoal absorption is
The reaction solution after reduction treatment is passed into active carbon adsorption column and carries out circulation absorption, until the obtained rectifying is former
Liquid is colourless, it is preferable that flow velocity of the reaction solution in the active carbon adsorption column after reduction treatment is 0.1~2m/s.
7. the preparation method of chromatogram pure tetrahydrofuran according to claim 1, it is characterised in that enter to the rectifying stoste
Row rectifying is that rectifying is heated at 90~130 DEG C, and caused gas passes through rectifying column, establishes infinite reflux, infinite reflux 3~5 hours,
Start to produce, the certified products of extraction are finished product.
8. a kind of chromatogram pure tetrahydrofuran, it is characterised in that it uses the chromatographically pure four as described in any one of claim 1~7
The preparation method of hydrogen furans is made.
9. a kind of production system of chromatogram pure tetrahydrofuran, it is characterised in that it includes：
Reactor, heated for accommodating Industrial Grade Tetrahydrofuran, and to Industrial Grade Tetrahydrofuran；
4A molecular sieve columns, for carrying out 4A molecular sieve adsorption processing to Industrial Grade Tetrahydrofuran；
Activated alumina column, for carrying out activated alumina adsorption treatment to Industrial Grade Tetrahydrofuran；
Na-K alloy post, for carrying out reduction treatment to Industrial Grade Tetrahydrofuran；
Active carbon adsorption column, for carrying out charcoal absorption processing to Industrial Grade Tetrahydrofuran；
Rectifying column, for carrying out rectifying to gas phase tetrahydrofuran；
Circulating pump, power is provided for the flowing of Industrial Grade Tetrahydrofuran；
Wherein, the 4A molecular sieve columns, the activated alumina column, the Na-K alloy post, the active carbon adsorption column are in parallel
Set, and form circulation line with the circulating pump and the reactor respectively；The gaseous phase outlet of the reactor is communicated to institute
State the gas phase entrance of rectifier bottoms.
10. the production system of chromatogram pure tetrahydrofuran according to claim 9, it is characterised in that the production system is also
Including condenser, return tank and finished pot for collecting chromatogram pure tetrahydrofuran finished product, the input of the condenser and institute
The gaseous phase outlet connection at the top of rectifying column is stated, the gas phase being collected into tetrahydrofuran is condensed into liquid；The condenser
Output end is connected to the input of the return tank, the output end of the return tank be respectively communicated to the rectifying column top and
The finished pot.
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