CN107501046A - A kind of chromatogram straight alcohol and preparation method thereof, production system - Google Patents
A kind of chromatogram straight alcohol and preparation method thereof, production system Download PDFInfo
- Publication number
- CN107501046A CN107501046A CN201710755433.1A CN201710755433A CN107501046A CN 107501046 A CN107501046 A CN 107501046A CN 201710755433 A CN201710755433 A CN 201710755433A CN 107501046 A CN107501046 A CN 107501046A
- Authority
- CN
- China
- Prior art keywords
- chromatogram
- straight alcohol
- preparation
- technical grade
- rectifying
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A kind of chromatogram straight alcohol and preparation method thereof, production system, it is related to chemical products technical field of purification, the preparation method be using technical grade ethanol as raw material, successively by with the concentrated sulfuric acid, 2,4 dinitrophenylhydrazines, aluminium powder and the reaction of the first alkali, the impurity such as the amine contained in technical grade ethanol, aldehyde, ketone, ester are removed, meanwhile, operated by filtering, charcoal absorption, rectifying etc., product is further purified, obtains the chromatogram straight alcohol of high-purity.The preparation method production cost is low, and obtained chromatogram straight alcohol quality better, yield are high, meet chromatographically pure reagent requirement.The production system includes blender, filter post, the active carbon adsorption column being arranged in parallel, and it forms circulation line with reactor respectively.The gaseous phase outlet of reactor is communicated to the gas phase entrance of rectifier bottoms.For the production system dedicated for preparing chromatogram straight alcohol, production efficiency is high, and obtained product purity is high, can realize the scale industrial production of chromatogram straight alcohol.
Description
Technical field
The present invention relates to chemical products technical field of purification, in particular to a kind of chromatogram straight alcohol and its preparation side
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 straight alcohol 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.
The ethanol purification technique of domestic report is also seldom at present, and existing purifying process is all more complex and high cost, chromatogram
Straight alcohol technique is monopolized by foreign countries for a long time.Therefore, break up monopoly, reduce cost, it is low and obtained to develop a kind of production cost
Chromatogram straight alcohol quality better, yield are high, can meet the new preparation process of chromatographically pure reagent requirement, have 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 straight alcohol, and the method production cost is low, system
Chromatogram straight alcohol quality better, the yield obtained is high.
The second object of the present invention is to provide a kind of chromatogram straight alcohol, and its quality better, yield are high, meet chromatogram pure reagent
It is required that.
The third object of the present invention is to provide a kind of production system of chromatogram straight alcohol, and it is dedicated for preparing chromatographically pure
Ethanol, realize the scale industrial production of chromatogram straight alcohol.
The present invention is solved its technical problem and realized using following technical scheme.
A kind of preparation method of chromatogram straight alcohol, it includes：
Using technical grade ethanol as raw material, with strong sulfuric acid response, the first reaction solution is obtained after neutralizing filtering；
First reaction solution and DNPH are reacted, the second reaction solution is obtained after charcoal absorption；
Second reaction solution and aluminium powder and the first alkali are reacted, obtain rectifying stoste；
Rectifying is carried out to rectifying stoste.
A kind of chromatogram straight alcohol, it uses the preparation method of above-mentioned chromatogram straight alcohol to be made.
A kind of production system of chromatogram straight alcohol, it includes：
Reactor, for being heated to technical grade ethanol, and the container to be reacted with other reactants；
Filter post, for carrying out filtration treatment to technical grade ethanol；
Active carbon adsorption column, for carrying out charcoal absorption processing to technical grade ethanol；
Rectifying column, for carrying out rectifying to gaseous ethanol；
Wherein, filter post, active carbon adsorption column are arranged in parallel, and form circulation line with reactor respectively；Reactor
Gaseous phase outlet be communicated to the gas phase entrances of the rectifier bottoms.
The beneficial effect of the embodiment of the present invention is：
The embodiments of the invention provide a kind of chromatogram straight alcohol and preparation method thereof, the preparation method is by technical grade ethanol
As raw material, successively by being reacted with the concentrated sulfuric acid, DNPH, aluminium powder and the first alkali, remove and contain in technical grade ethanol
The impurity such as some amine, aldehyde, ketone, ester, meanwhile, operated by filtering, charcoal absorption, rectifying etc., product is further purified, obtains
The chromatogram straight alcohol of high-purity.The preparation method production cost is low, and obtained chromatogram straight alcohol quality better, yield are high, meet color
Compose pure reagent requirement.
The embodiment of the present invention additionally provides a kind of production system of chromatogram straight alcohol, and it includes the filter being arranged in parallel
Post, active carbon adsorption column, filter post, active carbon adsorption column form circulation line with reactor respectively.The gas phase of reactor goes out
Mouth is communicated to the gas phase entrance of rectifier bottoms.For the production system dedicated for preparing chromatogram straight alcohol, production efficiency is high, obtains
Product purity it is high, the scale industrial production of chromatogram straight alcohol 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 straight alcohol that Fig. 1 is provided by the embodiment of the present invention 1.
Icon：100- production systems；110- reactors；111- feed pipes；112- dropping tanks；120- circulating pumps；131-
Blender；132- filter posts；133- active carbon adsorption columns；140- rectifying columns；150- condensers；160- return tanks；170- into
Product tank；171-4A molecular sieve columns；172- discharge pumps；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 straight alcohol of the embodiment of the present invention and preparation method thereof, production system are specifically described below.
The embodiments of the invention provide a kind of preparation method of chromatogram straight alcohol, it includes：
S1. using technical grade ethanol as raw material, with strong sulfuric acid response, the first reaction solution is obtained after neutralizing filtering.
Ethanol is a kind of inflammable, volatile colourless transparent liquid at normal temperatures and pressures, and hypotoxicity, neat liquid is not directly
Drink；With peat-reek, and slightly stimulate；Micro-sweet, and with irritant pungent flavour.Inflammable, its steam can be with air shape
Into explosive mixture, can be dissolved each other with water with any ratio.In the ethanol of technical grade, containing plurality of impurities such as amine, aldehyde, ketone, esters,
Need respectively to be purged them and can just obtain chromatogram straight alcohol.
The concentrated sulfuric acid can generate salt with the aminated compounds in technical grade ethanol, so as to reach the mesh for removing aminated compounds
's.But the concentrated sulfuric acid has very strong dehydration property, oxidisability, two molecules of ethanol dehydration generation ether can be made, so using
During, unsuitable excessive, the preferably 1~5mol% of technical grade ethanol of dosage of the concentrated sulfuric acid.
Meanwhile by the way of being added dropwise, the concentrated sulfuric acid will slowly dripped in the mixed process of technical grade ethanol and the concentrated sulfuric acid
Add in industrial alcohol, avoid concentrated sulfuric acid local concentration too high and instead give birth to side reaction.During the reaction of the concentrated sulfuric acid and technical grade ethanol
Between be 1~3h, by inventor's creative work find, in the time range, the concentrated sulfuric acid is to the amine in technical grade ethanol
The elimination effect of material is preferable, meanwhile, side reaction is less.Further, the concentrated sulfuric acid and technical grade ethanol intermiscibility it is poor, it is necessary to
The two is passed into blender by circulating pump and mixed, so that the two can sufficiently be mixed.
, it is necessary to carry out neutralisation treatment to solution after technical grade ethanol and strong sulfuric acid response.Neutralisation treatment is used to solution
The second alkali of middle addition, the dosage of the second alkali is depending on the dosage of the concentrated sulfuric acid.Preferably, the second alkali is sodium acid carbonate, bicarbonate
At least one of calcium and saleratus, these second alkali are alkalescents, have good cushioning effect, dense with excess
Sulfuric acid reaction generation carbon dioxide discharge, the excessively alkaline situation of solution will not be also caused even if excessive addition, meanwhile, lead to
Cross the yield of observation bubble, you can to judge whether neutralization reaction is completed.Further, above-mentioned neutralization reaction is at 50~60 DEG C
Lower progress, find that the neutralization reaction efficiency carried out in the temperature range is higher by inventor's creative work, neutralize efficiency
Preferably.
It is in being carried out to technical grade ethanol and rear, it is necessary to be filtered to impurity therein.Filtering is using by after neutralization
Technical grade ethanol, which is passed into filter post, carries out circulating filtration, and flow velocity of the technical grade ethanol in filter post is 0.1~2m/
S, circulation time are 1~3h.Preferably, filter post uses 200nm filter, using the filter of the model to technical grade
Impurity filtration result in ethanol is more preferably.
A kind of preparation method for chromatogram straight alcohol that the embodiment of the present invention is provided, in addition to：
S2. the first reaction solution and DNPH are reacted, the second reaction solution is obtained after charcoal absorption.
First reaction solution and DNPH are reacted, benzene is generated by DNPH and carbonyl reaction
Hydrazone, the aldehyde and ketone that are mixed with technical grade ethanol can be removed.Further, the first reaction solution reacts with DNPH
Reaction temperature be 50~60 DEG C, the reaction time is 0.5~2h.Found by inventor's creative work, in the temperature range
Interior, higher to the elimination efficiency of aldoketones impurity, effect is preferable.Preferably, the dosage of DNPH is technical grade second
1~5mol% of alcohol.
The first reaction solution reacted with DNPH carries out charcoal absorption, reaches the purpose for removal of impurities of decolourizing.
Specifically, it is that will be passed through with reacted first reaction solution of DNPH in active carbon adsorption column to carry out charcoal absorption
Circulation absorption is carried out, untill the first reaction solution is colourless.Wherein, flow velocity of first reaction solution in active carbon adsorption column is
0.1~2m/s.In the flow rates, the first reaction solution can be made sufficiently to be contacted with activated carbon, adsorption effect is preferable.
A kind of preparation method for chromatogram straight alcohol that the embodiment of the present invention is provided, in addition to：
S3. the second reaction solution and aluminium powder and the first alkali are reacted, obtains rectifying stoste.
Wherein, the second alkali is at least one of sodium hydroxide, potassium hydroxide and lithium hydroxide.Second alkali is highly basic, its
Generation meta-aluminate can be reacted with aluminium powder, while discharges hydrogen.Hydrogen can reduce the ester impurities in technical grade ethanol,
So as to be removed.The reaction temperature that second reaction solution and aluminium powder and the second alkali react is 60~78 DEG C, the reaction time is 1~
3h.Find that higher to the elimination efficiency of ester impurities in the temperature range, effect is preferable by inventor's creative work.
Further, in order to which the second reaction solution, aluminium powder and the first alkali are sufficiently mixed, three can be passed through in blender and be mixed
Close.
A kind of preparation method for chromatogram straight alcohol that the embodiment of the present invention is provided, in addition to：
S4. rectifying is carried out to rectifying stoste.
It is that rectifying is heated at 110~130 DEG C to carry out rectifying to rectifying stoste, and caused gas passes through rectifying column, is established
Infinite reflux, infinite reflux 1~3 hour, 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, take the certified products that midbarrel is extraction, namely required chromatogram straight alcohol.
Alternatively, the chromatogram straight alcohol that collection obtains can be passed into 4A molecular sieve columns and carries out circulation absorption.4A molecules
Sieve is a kind of alkali metal aluminosilicate, can adsorb water, NH3、H2S, sulfur dioxide, carbon dioxide, C2H5OH、C2H6、C2H4Etc. critical
Diameter is not more than 4A molecule, and it has preferable water removal effect, is the dehydration reagent commonly used in organic chemistry.In distillation process
Reclaimed water may be remained in and collected in obtained chromatogram straight alcohol by forming azeotropic mixture with ethanol steaming, and 4A molecular sieve columns are then
The moisture in the chromatogram straight alcohol being collected into can be further removed, improves product purity.Preferably, 4A molecular sieve adsorptions when
Between be 16~36h.In the time range, the water in chromatogram straight alcohol can sufficiently be adsorbed.Inhaled in 4A molecular sieves
After attached, chromatogram straight alcohol can also be made with this by cation exchange resin column and 200nm filters, to enter to advance to product
The purifying of one step, improve the purity of chromatogram straight alcohol.
The embodiment of the present invention additionally provides a kind of chromatogram straight alcohol, and it uses the preparation method system of above-mentioned chromatogram straight alcohol
.
The embodiment of the present invention additionally provides a kind of production system of chromatogram straight alcohol, and it includes：
Reactor, for being heated to technical grade ethanol, and the container to be reacted with other reactants；
Filter post, for carrying out filtration treatment to technical grade ethanol；
Active carbon adsorption column, for carrying out charcoal absorption processing to technical grade ethanol；
Rectifying column, for carrying out rectifying to gaseous ethanol；
Wherein, filter post, active carbon adsorption column are arranged in parallel, and form circulation line with reactor respectively；Reactor
Gaseous phase outlet be communicated to the gas phase entrances 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 straight alcohol finished product, the input of condenser connects with the gaseous phase outlet at the top of rectifying column, that will collect
To gaseous ethanol be condensed into liquid；The output end of condenser is connected to the input of return tank, the output end difference of return tank
It is communicated to top and the finished pot of rectifying column.
Further, in the other preferred embodiments of the present invention, production system also includes 4A molecular sieve columns and discharge pump, into
Circulation line is formed between product tank, 4A molecular sieve columns and discharge pump.
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 straight alcohol, and shown in reference picture 1, it includes：Reactor
110th, circulating pump 120, blender 131, filter post 132, active carbon adsorption column 133 and rectifying column 140.
Wherein, be arranged in parallel between blender 131, filter post 132, active carbon adsorption column 133, and respectively with circulating pump
120 and reactor 110 form circulation line.Further, the input of circulating pump 120 and the liquid phase of the bottom of reactor 110 go out
Mouth connection, the output end of circulating pump 120 are respectively communicated to the charging of blender 131, filter post 132, active carbon adsorption column 133
End, and blender 131, filter post 132, the feed end of active carbon adsorption column 133 are provided with Valve controlling its feed end
Opening and closing.Blender 131, filter post 132, the discharge end of active carbon adsorption column 133 are communicated to the charging of reactor 110
End, any one in such blender 131, filter post 132, active carbon adsorption column 133 can be with circulating pump 120, anti-
Kettle 110 is answered to form circulation line.Also, the control for passing through valve, you can switching technical grade ethanol is in any one circulation line
It is middle to complete circulation.
The feed end of reactor 110 connects with feed pipe 111, by feed pipe 111 convey Lai technical grade ethanol exist
Circulated between reactor 110 and blender 131, filter post 132, active carbon adsorption column 133, completion mixes with other reactants
The steps such as conjunction, filtering, charcoal absorption, and the gaseous component containing ethanol is thermally formed in reactor 110.Wherein, react
Kettle 110 is preferably to use enamel glass jacket reactor 110, in chuck can admittance deep fat reactor 110 is heated.Reaction
Kettle 110 is provided with paddle agitator (not shown), and its rotating speed reaches more than 300rpm, and the material that it can be made internal obtains fully
Mixing.Reactor 110 is additionally provided with dropping tank 112, and the discharge end of dropping tank 112 is provided with flow control valve, flow control
Valve can control the concentrated sulfuric acid in dropping tank 112 to enter the speed of reactor 110, so as to reduce the generation of side reaction.
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 ethanol rectifying column 140 is entered by the gas phase entrance of the bottom of rectifying column 140, it is and complete in rectifying column 140
Into rectifying.The internal diameter of rectifying column 140 is 4~500cm, is highly 4~30m, filling glass spring filler, stainless steel Xi Ta in tower
At least one of ring, stainless steel structured packing and ceramic packing.The bottom of rectifying column 140 be filled with one section of height for 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 gaseous ethanol being collected into is condensed into liquid by condenser 150.Condenser 150 it is defeated
Go out the input that end is connected to return tank 160, the output end of return tank 160 is communicated to finished pot 170, to being obtained after condensation
Chromatogram straight alcohol be collected and be delivered to finished pot 170.Meanwhile return tank 160 connects with the top of rectifying column 140, to
By part chromatographically pure alcohol reflux to the top of rectifying column 140, to increase the efficiency of rectifying.
Production system 100 also includes 4A molecular sieve columns 171 and discharge pump 172, finished pot 170,4A molecular sieve columns 171 and into
Circulation line is formed between product pump 172, the chromatogram straight alcohol collected by return tank 160 is in finished pot 170 and 4A molecular sieves
Circulated between post 171, to remove the moisture remained in chromatogram straight alcohol.
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 straight alcohol, and its preparation method is as follows：
S1. 50L technical grade ethanol (Jinzhou Petrochemical Company, purity >=98wt%) raw material is imported into reactor 110, passes through drop
Add tank 112 that the 1mol% concentrated sulfuric acid is added dropwise into reactor 110, open the valve of blender 131, establish reactor 110, circulation
Circulation between pump 120 and blender 131, circulation time 3h.
S2. the valve of blender 131 is closed, calcium bicarbonate is added into reactor 110, is warming up to 60 DEG C.
S3. the valve of opening filter post 132, following between reactor 110, circulating pump 120 and filter post 132 is established
Ring, coutroi velocity 0.1m/s, circulation time 3h.
S4. the valve of filter post 132 is closed, 5mol% DNPH, stirring are added into reactor 110
React 0.5h.
S5. the valve of active carbon adsorption column 133 is opened, establishes reactor 110, circulating pump 120 and active carbon adsorption column 133
Between circulation, coutroi velocity 0.1m/s, until reactor 110 in solution it is colourless when stop circulation, close charcoal absorption
The valve of post 133.
S6. 2mol% aluminium powder and 2mol% potassium hydroxide are added into reactor 110, is warming up to 78 DEG C, is opened mixed
The valve of clutch 131, circular response 1h.
S7. the valve of blender 131 is closed, the temperature of reactor 110 is risen to 110 DEG C, when the top of rectifying column 140 starts
After backflow, infinite reflux 3h, then start to produce.During extraction, reflux ratio is controlled 5:1, remove front-end volatiles 0.5L and tails
0.8L, the midbarrel of extraction is qualified chromatogram straight alcohol, and qualified chromatographically pure ethanol yield reaches more than 95%.
S8. the valve of discharge pump 172 and 4A molecular sieve columns 171 is opened, establishes finished pot 170, discharge pump 172 and 4A molecules
Sieve the circulation between adsorption column 171, coutroi velocity 0.1m/s, circulation absorption 36h.
S9. the chromatogram straight alcohol after 4A molecular sieve adsorptions 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 straight alcohol, and its preparation method is as follows：
S1. 50L technical grade ethanol (Jinzhou Petrochemical Company, purity >=98wt%) raw material is imported into reactor 110, passes through drop
Add tank 112 that the 5mol% concentrated sulfuric acid is added dropwise into reactor 110, open the valve of blender 131, establish reactor 110, circulation
Circulation between pump 120 and blender 131, circulation time 1h.
S2. the valve of blender 131 is closed, calcium bicarbonate is added into reactor 110, is warming up to 50 DEG C.
S3. the valve of opening filter post 132, following between reactor 110, circulating pump 120 and filter post 132 is established
Ring, coutroi velocity 2m/s, circulation time 1h.
S4. the valve of filter post 132 is closed, 1mol% DNPH, stirring are added into reactor 110
React 2h.
S5. the valve of active carbon adsorption column 133 is opened, establishes reactor 110, circulating pump 120 and active carbon adsorption column 133
Between circulation, coutroi velocity 2m/s, until reactor 110 in solution it is colourless when stop circulation, close active carbon adsorption column
133 valve.
S6. 5mol% aluminium powder and 5mol% potassium hydroxide are added into reactor 110, is warming up to 60 DEG C, is opened mixed
The valve of clutch 131, circular response 3h.
S7. the valve of blender 131 is closed, the temperature of reactor 110 is risen to 150 DEG C, when the top of rectifying column 140 starts
After backflow, infinite reflux 1h, then start to produce.During extraction, reflux ratio is controlled 3:1, remove front-end volatiles 0.5L and tails
0.8L, the midbarrel of extraction is qualified chromatogram straight alcohol, and qualified chromatographically pure ethanol yield reaches more than 95%.
S8. the valve of discharge pump 172 and 4A molecular sieve columns 171 is opened, establishes finished pot 170, discharge pump 172 and 4A molecules
Sieve the circulation between adsorption column 171, coutroi velocity 2m/s, circulation absorption 16h.
S9. the chromatogram straight alcohol after 4A molecular sieve adsorptions 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 straight alcohol, and its preparation method is as follows：
S1. 500L technical grade ethanol (Jinzhou Petrochemical Company, purity >=98wt%) raw material is imported into reactor 110, is passed through
The 3mol% concentrated sulfuric acid is added dropwise into reactor 110 for dropping tank 112, opens the valve of blender 131, establishes reactor 110, follows
Circulation between ring pump 120 and blender 131, circulation time 2h.
S2. the valve of blender 131 is closed, calcium bicarbonate is added into reactor 110, is warming up to 60 DEG C.
S3. the valve of opening filter post 132, following between reactor 110, circulating pump 120 and filter post 132 is established
Ring, coutroi velocity 1m/s, circulation time 2h.
S4. the valve of filter post 132 is closed, 2mol% DNPH, stirring are added into reactor 110
React 1h.
S5. the valve of active carbon adsorption column 133 is opened, establishes reactor 110, circulating pump 120 and active carbon adsorption column 133
Between circulation, coutroi velocity 1m/s, until reactor 110 in solution it is colourless when stop circulation, close active carbon adsorption column
133 valve.
S6. 1mol% aluminium powder and 1mol% potassium hydroxide are added into reactor 110, is warming up to 70 DEG C, is opened mixed
The valve of clutch 131, circular response 2h.
S7. the valve of blender 131 is closed, the temperature of reactor 110 is risen to 120 DEG C, when the top of rectifying column 140 starts
After backflow, infinite reflux 2h, then start to produce.During extraction, reflux ratio is controlled 5:1, front-end volatiles 5L and tails 10L is removed,
The midbarrel of extraction is qualified chromatogram straight alcohol, and qualified chromatographically pure ethanol yield reaches more than 95%.
S8. the valve of discharge pump 172 and 4A molecular sieve columns 171 is opened, establishes finished pot 170, discharge pump 172 and 4A molecules
Sieve the circulation between adsorption column 171, coutroi velocity 1m/s, circulation absorption 20h.
S9. the chromatogram straight alcohol after 4A molecular sieve adsorptions is passed sequentially through into cation exchange column 180 and 200nm filters
190, and barrelling is stand-by.
Test example 1
Using the chromatogram straight alcohol that embodiment 2~4 is provided as test specimen, its ultraviolet absorptivity is detected,
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 205nm, 210nm, 220nm, 230nm, 254nm and 280nm wavelength, the testing result such as institute of table 1
Show.
The ultraviolet absorptivity testing result of the chromatogram straight alcohol of table 1.
From table 1 it follows that the chromatogram straight alcohol that the embodiment of the present invention 2~4 is provided is under 205~280nm wavelength
Ultraviolet absorptivity reached the chromatographically pure standard and agriculture residual standard of national setting, the preparation that the embodiment of the present invention is provided
Method and production equipment are preferable to the purification effect of ethanol.
Test example 2
Using the chromatogram straight alcohol that embodiment 2~4 is provided as test specimen, to its water content index, evaporation residue
Index, acidity 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, acidity, the purity detecting result of the chromatogram straight alcohol of table 2.
As can be seen from Table 2, the moisture for the chromatogram straight alcohol that the embodiment of the present invention 2~4 is provided is less than or equal to
0.002wt%, evaporation residue content are less than or equal to 0.0002wt%, and acidity is less than 0.005meq/g, are below country's setting
Chromatographically pure standard and agriculture residual standard.The purity for the chromatogram straight alcohol that the embodiment of the present invention 2~4 is provided reaches 99.9wt%,
More than the chromatographically pure standard and agriculture residual standard of country's setting.It can be seen that preparation method that the embodiment of the present invention is provided and production
Equipment is preferable to the purification effect of ethanol.
In summary, the embodiments of the invention provide a kind of chromatogram straight alcohol and preparation method thereof, the preparation method be by
Technical grade ethanol is as raw material, successively by industrial with the concentrated sulfuric acid, DNPH, aluminium powder and the reaction of the first alkali, removing
Amine, aldehyde, ketone, the impurity such as ester contained in level ethanol, meanwhile, operated by filtering, charcoal absorption, rectifying etc., it is further pure
Change product, obtain the chromatogram straight alcohol of high-purity.The preparation method production cost is low, obtained chromatogram straight alcohol quality better, production
Rate is high, meets chromatographically pure reagent requirement.
The embodiment of the present invention additionally provides a kind of production system of chromatogram straight alcohol, its blender for including being arranged in parallel,
Filter post, active carbon adsorption column, blender, filter post, active carbon adsorption column form circulation line with reactor respectively.Instead
The gaseous phase outlet of kettle is answered to be communicated to the gas phase entrance of rectifier bottoms.The production system is raw dedicated for preparing chromatogram straight alcohol
Efficiency high is produced, obtained product purity is high, can realize the scale industrial production of chromatogram straight alcohol.
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 straight alcohol, it is characterised in that it includes：
Using technical grade ethanol as raw material, with strong sulfuric acid response, the first reaction solution is obtained after neutralizing filtering；Described first is reacted
Liquid is reacted with DNPH, and the second reaction solution is obtained after charcoal absorption；By second reaction solution and aluminium powder and the
One alkali reacts, and obtains rectifying stoste；Rectifying is carried out to the rectifying stoste.
2. the preparation method of chromatogram straight alcohol according to claim 1, it is characterised in that the technical grade ethanol with it is described
Strong sulfuric acid response is that the concentrated sulfuric acid is added drop-wise in the technical grade ethanol, and the reaction time is 1~3h；Preferably, it is described dense
The dosage of sulfuric acid is 1~5mol% of the technical grade ethanol.
3. the preparation method of chromatogram straight alcohol according to claim 1, it is characterised in that neutralize filtering be to it is described dense
The second alkali is added in the technical grade ethanol after sulfuric acid reaction to be neutralized, and is passed into filter post and is circulated throughout
Filter；Preferably, second alkali is at least one of sodium acid carbonate, calcium bicarbonate and saleratus；Preferably, the industry
Level ethanol is 50~60 DEG C with the reaction temperature that second alkali is neutralized.
4. the preparation method of chromatogram straight alcohol according to claim 1, it is characterised in that first reaction solution and 2,4-
The reaction temperature of dinitrophenylhydrazine reaction is 50~60 DEG C, and the reaction time is 0.5~2h；Preferably, 2, the 4- dinitro benzenes
The dosage of hydrazine is 1~5mol% of the technical grade ethanol.
5. the preparation method of chromatogram straight alcohol according to claim 1, it is characterised in that carry out charcoal absorption be by with
Reacted first reaction solution of DNPH, which is passed through in active carbon adsorption column, carries out circulation absorption, until institute
State the first reaction solution it is colourless untill；Preferably, flow velocity of first reaction solution in the active carbon adsorption column be 0.1~
2m/s。
6. the preparation method of chromatogram straight alcohol according to claim 3, it is characterised in that second reaction solution with it is described
Aluminium powder and the reaction temperature of second alkali reaction are 60~78 DEG C, and the reaction time is 1~3h；Preferably, second alkali is
At least one of sodium hydroxide, potassium hydroxide and lithium hydroxide.
7. the preparation method of chromatogram straight alcohol according to claim 1, it is characterised in that essence is carried out to the rectifying stoste
It is that rectifying is heated at 110~150 DEG C to evaporate, and caused gas passes through rectifying column, establishes infinite reflux, infinite reflux 1~3 hour, opens
Begin to produce, the certified products of extraction are finished product.
8. a kind of chromatogram straight alcohol, it is characterised in that it uses the chromatogram straight alcohol as described in any one of claim 1~7
Preparation method is made.
9. a kind of production system of chromatogram straight alcohol, it is characterised in that it includes：
Reactor, for being heated to technical grade ethanol, and the container to be reacted with other reactants；
Filter post, for carrying out filtration treatment to technical grade ethanol；
Active carbon adsorption column, for carrying out charcoal absorption processing to technical grade ethanol；
Rectifying column, for carrying out rectifying to gaseous ethanol；
Wherein, the filter post, the active carbon adsorption column are arranged in parallel, and form circulation pipe with the reactor respectively
Road；The gaseous phase outlet of the reactor is communicated to the gas phase entrance of the rectifier bottoms.
10. the production system of chromatogram straight alcohol according to claim 9, it is characterised in that the production system also includes
Condenser, return tank and the finished pot for collecting chromatogram straight alcohol finished product, the input of the condenser and the rectifying column
The gaseous phase outlet connection at top, the gaseous ethanol being collected into is condensed into liquid；The output end of the condenser is connected to
The input of the return tank, the output end of the return tank are respectively communicated to the top of the rectifying column and the finished pot.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710755433.1A CN107501046A (en) | 2017-08-29 | 2017-08-29 | A kind of chromatogram straight alcohol and preparation method thereof, production system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710755433.1A CN107501046A (en) | 2017-08-29 | 2017-08-29 | A kind of chromatogram straight alcohol and preparation method thereof, production system |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107501046A true CN107501046A (en) | 2017-12-22 |
Family
ID=60694049
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710755433.1A Pending CN107501046A (en) | 2017-08-29 | 2017-08-29 | A kind of chromatogram straight alcohol and preparation method thereof, production system |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107501046A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111718238A (en) * | 2020-07-28 | 2020-09-29 | 武汉弗顿控股有限公司 | Process for producing chromatographic pure ethanol |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101570468A (en) * | 2009-06-15 | 2009-11-04 | 天津市康科德科技有限公司 | Method for preparing pesticide residue grade chromatographic ethanol |
| CN102584543A (en) * | 2011-12-26 | 2012-07-18 | 天津市康科德科技有限公司 | Preparation method of chromatographic-grade organic solvent ethylene glycol monomethyl ether |
| CN103342626A (en) * | 2013-07-31 | 2013-10-09 | 北京旭阳化工技术研究院有限公司 | Preparation method of chromatographic grade methanol |
-
2017
- 2017-08-29 CN CN201710755433.1A patent/CN107501046A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101570468A (en) * | 2009-06-15 | 2009-11-04 | 天津市康科德科技有限公司 | Method for preparing pesticide residue grade chromatographic ethanol |
| CN102584543A (en) * | 2011-12-26 | 2012-07-18 | 天津市康科德科技有限公司 | Preparation method of chromatographic-grade organic solvent ethylene glycol monomethyl ether |
| CN103342626A (en) * | 2013-07-31 | 2013-10-09 | 北京旭阳化工技术研究院有限公司 | Preparation method of chromatographic grade methanol |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111718238A (en) * | 2020-07-28 | 2020-09-29 | 武汉弗顿控股有限公司 | Process for producing chromatographic pure ethanol |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107382776A (en) | A kind of trifluoroacetic acid aqueous solution and preparation method thereof, production system | |
| Cohen | Practical organic chemistry | |
| CN102276483B (en) | Production method of oamino pheylmethyl ether | |
| AU2008202331A1 (en) | Process for preparing alkali metal alkoxides | |
| CN101591244B (en) | Semi-continuous production process for acetyl tributyl citrate | |
| CN102153752A (en) | Method and device for preparing high-boiling-point silicone oil | |
| CN107501046A (en) | A kind of chromatogram straight alcohol and preparation method thereof, production system | |
| CN107501056A (en) | A kind of chromatogram absolute ether and preparation method thereof, production system | |
| CN109438250B (en) | High-yield preparation method of high-purity dimethyl diallyl ammonium chloride monomer | |
| CN104722248A (en) | Device and process for producing dioctyl terephthalate by virtue of reactive distillation of waste polyester | |
| CN102976897A (en) | Method for purifying tetrafluoro propanol | |
| CN114405062A (en) | Method for reducing acid value in benzaldehyde by using composite filler column | |
| CN206502761U (en) | A kind of recovery purification system of ionic liquid after synthesizing P-Al molecular sieve catalyst reaction | |
| CN207210295U (en) | A kind of ethanol purification system and chromatographically pure alcohol production system | |
| CN105170046B (en) | A kind of DMP Neutralisation treatment methods | |
| CN107324984A (en) | Chromatogram pure acetone and preparation method thereof, production system | |
| CN105367779B (en) | The process for purification of isomery alcohol polyethers | |
| CN107586820A (en) | A kind of method that Momordica grosvenori albumen is produced in sweet tea glucoside extraction waste liquid from Momordica grosvenori | |
| CN104646058B (en) | Copper-containing complex catalyst and preparation method and application thereof | |
| CN208104255U (en) | A kind of n-hexane purification system and chromatographically pure n-hexane production system | |
| CN107501031A (en) | A kind of chromatographically pure n-hexane and preparation method thereof, production system | |
| CN207031312U (en) | The purifying plant of trihydroxyethyl isocyanuric ester | |
| CN107501040A (en) | Chromatographically pure chloro-normal butane and preparation method thereof, production system | |
| CN107324972A (en) | A kind of chromatographically pure tert-butyl alcohol and preparation method thereof, production system | |
| CN106278901B (en) | A kind of method of nitromethane purifying |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171222 |
|
| RJ01 | Rejection of invention patent application after publication |