CN107501067A - Chromatographically pure hexone and preparation method thereof, production system - Google Patents
Chromatographically pure hexone and preparation method thereof, production system Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/79—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C45/82—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/85—Separation; Purification; Stabilisation; Use of additives by treatment giving rise to a chemical modification
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C49/00—Ketones; Ketenes; Dimeric ketenes; Ketonic chelates
- C07C49/04—Saturated compounds containing keto groups bound to acyclic carbon atoms
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Abstract
A kind of chromatographically pure hexone and preparation method thereof, production system, belong to chemical products technical field of purification.The preparation method of chromatographically pure hexone provided by the invention is to add potassium permanganate progress oxidation reaction into technical grade methyl isobutyl ketone to obtain mixed liquor；Stirred then to aqueous sodium carbonate is added in mixed liquor, stratification, upper liquid is used to 4A molecular sieve columns, alumina adsorption post progress adsorption treatment, afterwards rectifying successively after removing subnatant.The preparation method has that production cost is low, obtained chromatographically pure hexone quality better, the advantages of yield is high.The production system of chromatographically pure hexone provided by the invention includes reactor, the blender being connected respectively with reactor, 4A molecular sieve columns and alumina adsorption post, and the rectifying column and finished pot being sequentially connected with reactor, the production system can prepare low cost, the chromatographically pure hexone of high-purity.
Description
Technical field
The present invention relates to a kind of chemical products technical field of purification, and more particularly to a kind of chromatographically pure hexone
And preparation method thereof, production system.
Background technology
Chromatographically pure refers to carry out the standard reagent or solvent used during chromatography, its ultraviolet printing opacity at low wavelength
Rate is relatively good, under chromatographic condition, the peak of appointed compound can only occurs, it is impossible to there are impurity peaks, therefore, chromatogram pure reagent
Purity requirement is very high, in addition to the requirement to appointed compound content is very high, also has to impurity contents such as micronic dust therein, moisture
Very high requirement, belong to the category of high purity reagent.At present, domestic chromatographically pure market is mostly that external Reagent Company is monopolized, such as
Merck, Sigma, Fisher, Tedia etc., external Reagent Company's price is high, for the chromatographically pure user of the country, can cause
Cost is too high.
Therefore, break monopolization of the foreign technology obstacle to the chromatographically pure technical field in China, establish the own chromatogram in China
The standardization industry of pure reagent has great meaning and effect.A kind of low hexone of production cost is needed to prepare
Method, and it is high using chromatographically pure hexone quality better, yield made from this method, it can meet that chromatogram pure reagent will
Ask.
The content of the invention
It is an object of the invention to provide a kind of preparation method of chromatographically pure hexone, the method has technique
It is simple and convenient to operate, the advantages of production cost is low, obtained chromatographically pure hexone quality better, yield are high.
Another object of the present invention is to provide a kind of chromatographically pure hexone, it has, and purity is high, impurity is few
The advantages of.
Another object of the present invention is to provide a kind of production system of chromatographically pure hexone, it can be prepared
Low cost, the chromatographically pure hexone of high-purity.
The present invention is solved its technical problem and realized using following technical scheme.
A kind of preparation method of chromatographically pure hexone, it comprises the following steps：To technical grade methyl isobutyl group
Potassium permanganate progress oxidation reaction is added in ketone and obtains mixed liquor；Then to being added in mixed liquor, aqueous sodium carbonate stirring is equal
It is even, stratification, upper liquid is used to 4A molecular sieve columns, alumina adsorption post progress adsorption treatment successively after removing subnatant,
Rectifying afterwards.
Further, in present pre-ferred embodiments, it is straight that potassium permanganate is added into technical grade methyl isobutyl ketone
Become purple to mixed liquor.
Further, in present pre-ferred embodiments, the use of sodium carbonate in the aqueous sodium carbonate in mixed liquor is added
Measure as 10~30mol% of technical grade methyl isobutyl ketone.
Further, in present pre-ferred embodiments, upper liquid is by upper liquid using 4A molecular sieve column adsorption treatments
Circulation is passed through in 4A molecular sieve columns and adsorbed, and the circulation absorption time is 16~36h, and control upper liquid is in 4A molecular sieve columns
Flow velocity is 0.1~2m/s.
Further, in present pre-ferred embodiments, upper liquid is by upper strata using alumina adsorption post adsorption treatment
Liquid circulation, which is passed through in alumina adsorption post, to be adsorbed, and the circulation absorption time is 3~6h, and control upper liquid is in alumina adsorption post
In flow velocity be 0.1~2m/s.
Further, in present pre-ferred embodiments, rectifying is to the upper liquid after being adsorbed by alumina adsorption post
Heating, caused gas passes through rectifying column, and establishes infinite reflux, infinite reflux 1~3 hour, starts to produce, and the certified products of extraction are
Finished product.
Further, in present pre-ferred embodiments, preparation method is additionally included in the ion carried out successively after rectifying and handed over
Change, filtration step.
Present invention also offers a kind of chromatographically pure hexone, and it uses above-mentioned chromatographically pure methyl-isobutyl first
The preparation method of ketone is made.
Present invention also offers a kind of production system of chromatographically pure hexone, it includes：
Reactor, for accommodating technical grade methyl isobutyl ketone, and oxidation reaction is carried out to technical grade ether and added
Heat；
Blender, for the technical grade methyl isobutyl ketone in reactor to be mixed with other raw materials；
4A molecular sieve columns, for carrying out 4A molecular sieve column absorption to technical grade methyl isobutyl ketone；
Alumina adsorption post, for carrying out alumina adsorption post absorption to technical grade methyl isobutyl ketone；
Rectifying column, for carrying out rectifying；And
Finished pot, for collecting finished product；
Wherein, reactor is connected with blender, 4A molecular sieve columns and alumina adsorption post respectively, reactor, rectifying column and
Finished pot is sequentially connected with.
Further, in present pre-ferred embodiments, in addition to be installed on reactor and blender, 4A molecular sieve columns,
Circulating pump between alumina adsorption post, and be installed on condenser, return tank at the top of rectifying column, reactor, circulating pump and
Blender forms the circulation line for carrying out circular response, and reactor, circulating pump and 4A molecular sieve columns are formed for being followed
The circulation line of ring reaction, reactor, circulating pump and alumina adsorption post form the circulation line for carrying out circulation absorption；Essence
Evaporate tower, condenser and return tank and form circulation line for carrying out infinite reflux.
The chromatographically pure hexone of the embodiment of the present invention, the preparation method of chromatographically pure hexone and its
The beneficial effect of production system is：The preparation method of the chromatographically pure hexone of the embodiment of the present invention is by technical grade
Hexone is extracted using after potassium permanganate oxidation using aqueous sodium carbonate, after removal subnatant by upper liquid successively
Adsorption treatment, afterwards rectifying are carried out by 4A molecular sieve columns, alumina adsorption post.The preparation method technique is simple and convenient to operate,
And, obtained chromatographically pure hexone quality better, yield high the advantages of low with production cost.The embodiment of the present invention carries
The production system of the chromatographically pure hexone of confession includes reactor, the blender being connected respectively with reactor, 4A point
Son sieve post, alumina adsorption post and the rectifying column being sequentially connected with reactor, finished pot, the production system can quickly, efficiently
Prepare chromatographically pure hexone.
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.
Fig. 1 is the structural representation of the production system of chromatographically pure hexone provided in an embodiment of the present invention.
Icon：001- production systems；100- reactors；101- regards cup；105- blenders；110-4A molecular sieve columns；120-
Alumina adsorption post；130- rectifying columns；140- finished pots；150- cation exchange columns；160- filters；170- feedstock transportations
Pump；180- circulating pumps；190- condensers；200- return tanks；210- finished product delivery pumps.
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.
Chromatographically pure hexone of the embodiment of the present invention and preparation method thereof, production system are carried out below specific
Explanation.
The embodiment of the present invention provides a kind of preparation method of chromatographically pure hexone, and it comprises the following steps：To
Potassium permanganate progress oxidation reaction is added in technical grade methyl isobutyl ketone and obtains mixed liquor；Then to adding carbon in mixed liquor
Acid sodium aqueous solution stirs, stratification, by upper liquid successively using 4A molecular sieve columns, alumina adsorption after removal subnatant
Post carries out adsorption treatment, afterwards rectifying；The ion exchange carried out after rectifying, filtration step are preferably also included in, finally obtains color
Compose pure hexone.In the present embodiment, the preparation method of chromatographically pure hexone specifically includes following steps：
S1, oxidation processes：Potassium permanganate is added into the hexone of technical grade and carries out oxidation reaction, is obtained
Layer liquid；It is well mixed then to 1~2h of aqueous sodium carbonate stirring is added in mixed liquor, stands 1~3h layerings, discharge subnatant
Retain upper liquid.Present invention preferably employs potassium permanganate as strong oxidizer, will can be mixed in technical grade methyl isobutyl ketone
Some oxidations of impurities, to carry out purification process to hexone, while preferably into technical grade methyl isobutyl ketone
Potassium permanganate is added until the color of upper liquid becomes purple, sufficiently can be contained in oxidation removal hexone
Impurity.Add mixed liquor in aqueous sodium carbonate in sodium carbonate dosage for technical grade methyl isobutyl ketone 10~
30mol%, can be while with preferable impurity-eliminating effect, and and can enough saves the dosage of sodium carbonate, finally give purity compared with
High finished product hexone；Aqueous sodium carbonate is added into mixed liquor and stirs 1~2h.
S2,4A molecular sieve column adsorb：The upper liquid of reservation is passed through in 4A molecular sieve columns and carries out circulation absorption, controls upper strata
Flow velocity of the liquid in 4A molecular sieve columns is 0.1~2m/s, and the circulation absorption time is 16~36h；Wherein, preferably circulated in upper liquid
When being passed through progress circulation absorption in 4A molecular sieve columns, flow velocity is 0.8~1.4m/s.
S2, alumina adsorption；Upper liquid after 4A molecular sieve columns are adsorbed, which is passed through in alumina adsorption post, carries out circulation suction
Attached, it is 0.1~2m/s to control flow velocity of the upper liquid in alumina adsorption post, and circulation time is 3~6h；Wherein, preferably upper
When layer liquid circulation is passed through progress circulation absorption in alumina adsorption post, flow velocity is 0.6~1.2m/s.
S3, the specific method of rectifying are：Upper liquid after being adsorbed to alumina adsorption post heats, and caused gas is by essence
Tower is evaporated, and establishes infinite reflux, infinite reflux 1~3 hour, starts to produce, the certified products of extraction are finished product.
S4, ion exchange：Rectifying is obtained into hexone ion exchange is carried out by cation exchange column.
S5, filtering：Solution obtained by ion exchange is filtered by filter, bottles, it is different to produce chromatographically pure methyl
Butyl ketone.
In the present embodiment, filter is 200nm filters.
The embodiment of the present invention provides a kind of chromatographically pure hexone, and it uses above-mentioned chromatographically pure methyl-isobutyl
The preparation method of ketone is made.
Shown in Figure 1, the embodiment of the present invention provides a kind of production system 001 of chromatographically pure hexone, its
Including for accommodating primary industry level hexone and as the reactor 100 of reaction vessel, respectively with reactor 100
Blender 105,4A molecular sieve columns 110 and the alumina adsorption post 120 of connection；For the rectifying column 130 for carrying out rectifying, use
In the finished pot 140 for collecting finished product；For carrying out the cation exchange column 150 of ion exchange；And the mistake for being filtered
Filter 160.
Wherein, the height of rectifying column 130 is 2m~30m, and internal diameter is 4cm~220cm, the western tower ring of filling stainless steel in tower,
At least one of stainless steel structured packing and ceramic packing；The model ABD1UPW3EH1+ of cation exchange column 150
IDO10-PFA-3/4 300；Filter 160 is 200nm filters, its model FLHF20010M3F300+IDO10-PFA-3/
4 300, the material of filter 160 is virgin pp or pure polytetrafluoroethylene (PTFE).
In the present embodiment, production system 001 also includes feedstock transportation pump 170, and feedstock transportation pump 170 connects with reactor 100
Connect, for raw material automatic transport to be entered in reactor 100.
In the present embodiment, production system 001 also include being installed on reactor 100 and blender 105,4A molecular sieve columns 110,
Circulating pump 180 between alumina adsorption post 120, the bottom of reactor 100, circulating pump 180, blender 105, reactor 100
Top between form the circulation line for carrying out circular response, the bottom of reactor 100, circulating pump 180,4A molecular sieve columns
110th, the circulation line for carrying out circular response, the bottom of reactor 100, circulating pump are formed between the top of reactor 100
180th, the circulation line for carrying out circulation absorption is formed between the top of alumina adsorption post 120, reactor 100.
In the present embodiment, production system 001 also includes condenser 190, the return tank 200 for being installed on the top of rectifying column 130,
Rectifying column 130, condenser 190 and return tank 200 form the circulation line for carrying out infinite reflux, fully to carry out rectifying.
In the present embodiment, the bottom of finished pot 140 is communicated with finished product delivery pump 210, and finished product delivery pump 210 has been sequentially communicated
Cation exchange column 150 and the filter 160 for being filtered.
In the present embodiment, it is additionally provided with the pipeline between reactor 100 and circulating pump 180 regarding cup 101, staff can be with
By checking the color of reaction solution depending on cup 101, in order to carry out operation.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
The present embodiment provides a kind of chromatographically pure hexone, and it is to use the production system 001 shown in Fig. 1, and
It is made according to following preparation methods：
S101, oxidation processes：Technical grade methyl isobutyl ketone is added to by reactor 100 by feedstock transportation pump 170
It is interior, feedstock transportation pump 170 is closed, reactor 100 and 4A molecular sieve columns 110, aluminum oxide are blocked by valve (not shown)
Pipeline between pipeline between adsorption column 120, and connection reactor 100 and blender 105, and open the circulation pump 180, build
The circulation line for standing the top of the bottom for forming reactor 100, circulating pump 180, blender 105 and reactor 100 is circulated,
Cyclic oxidation reaction is carried out then to potassium permanganate is added in reactor 100, until the color of the solution in reactor 100 becomes
Purple；
S102, extraction processing：Aqueous sodium carbonate circulation stirring 1h is added into reactor 100, is then turned off circulating pump
180 stand, and discharge subnatant after solution layering in question response kettle 100, retain upper liquid.Wherein；Carbonic acid in aqueous sodium carbonate
The addition of sodium is the 15mol% of technical grade methyl isobutyl ketone addition.
S103,4A molecular sieve column adsorb：The pipeline blocked by valve between reactor 100 and blender 105, Yi Jilian
Logical pipeline between reactor 100 and 4A molecular sieve columns 110, open the circulation pump 180, establish and form the bottom of reactor 100, follow
The circulation line at the top of ring pump 180,4A molecular sieve columns 110 and reactor 100 carries out circulation absorption, is controlled by circulating pump 180
Flow velocity of the upper liquid processed in 4A molecular sieve columns is 1.5m/s, circulation absorption 24h.
S104, alumina adsorption；Close circulating pump 180, by valve block reactor 100 and 4A molecular sieve columns 110 it
Between pipeline, and connection reactor 100 and alumina adsorption post 120 between pipeline, open the circulation pump 180, establish formed
The bottom of reactor 100, circulating pump 180, the circulation line at top of alumina adsorption post 120 and reactor 100 are circulated
Absorption, and it is 0.9m/s, circulation time 5h to control flow velocity of the upper liquid in alumina adsorption post by circulating pump 180.
S105, rectifying；Circulating pump 180 is closed, starts rectifying, caused gas warp to the liquid heating in reactor 100
Rectifying column 130 is crossed, and infinite reflux is established between rectifying column 130, condenser 190 and return tank 200, infinite reflux 2 hours, then
Start to produce, remove slop cut before and after extraction, extraction midbarrel certified products (i.e. finished product) are transported to finished pot 140.
S106, ion exchange and filtering：Using finished product delivery pump 210 by rectifying obtains in finished pot 140 methyl tert-butyl
Base ketone passes sequentially through cation exchange column 150 and carries out ion exchange and filtered by filter 160, bottles, produces color
Compose pure hexone.
Embodiment 2
The present embodiment provides a kind of chromatographically pure hexone, and it is to use the production system 001 shown in Fig. 1, and
It is made according to following preparation methods：
S201, oxidation processes：Technical grade methyl isobutyl ketone is added to by reactor 100 by feedstock transportation pump 170
It is interior, feedstock transportation pump 170 is closed, is blocked by valve between reactor 100 and 4A molecular sieve columns 110, alumina adsorption post 120
Pipeline, and the pipeline between connection reactor 100 and blender 105, and open the circulation pump 180, foundation forms reactor
100 bottom, circulating pump 180, the circulation line at top of blender 105 and reactor 100 are circulated, then to reactor
Potassium permanganate is added in 100 and carries out cyclic oxidation reaction, until the color of the solution in reactor 100 becomes purple；
S202, extraction processing：Aqueous sodium carbonate circulation stirring 2h is added into reactor 100, is then turned off circulating pump
180 stand, and discharge subnatant after solution layering in question response kettle 100, retain upper liquid.Wherein；Carbonic acid in aqueous sodium carbonate
The addition of sodium is the 25mol% of technical grade methyl isobutyl ketone addition.
S203,4A molecular sieve column adsorb：The pipeline blocked by valve between reactor 100 and blender 105, Yi Jilian
Logical pipeline between reactor 100 and 4A molecular sieve columns 110, open the circulation pump 180, establish and form the bottom of reactor 100, follow
The circulation line at the top of ring pump 180,4A molecular sieve columns 110 and reactor 100 carries out circulation absorption, is controlled by circulating pump 180
Flow velocity of the hexone processed in 4A molecular sieve columns is 1.5m/s, circulation absorption 18h.
S204, alumina adsorption；Close circulating pump 180, by valve block reactor 100 and 4A molecular sieve columns 110 it
Between pipeline, and connection reactor 100 and alumina adsorption post 120 between pipeline, open the circulation pump 180, establish formed
The bottom of reactor 100, circulating pump 180, the circulation line at top of alumina adsorption post 120 and reactor 100 are circulated
Absorption, and it is 1.8m/s to control flow velocity of the hexone in alumina adsorption post by circulating pump 180, circulation time
For 4h.
S205, rectifying；Circulating pump 180 is closed, starts rectifying, caused gas warp to the liquid heating in reactor 100
Rectifying column 130 is crossed, and infinite reflux is established between rectifying column 130, condenser 190 and return tank 200, infinite reflux 1.5 hours, so
After start to produce, remove extraction before and after slop cut, extraction midbarrel certified products (i.e. finished product) be transported to finished pot 140.
S206, ion exchange and filtering：Using finished product delivery pump 210 by rectifying obtains in finished pot 140 methyl tert-butyl
Base ketone passes sequentially through cation exchange column 150 and carries out ion exchange and filtered by filter 160, bottles, produces color
Compose pure hexone.
Embodiment 3
The present embodiment provides a kind of chromatographically pure hexone, and it is to use the production system 001 shown in Fig. 1, and
It is made according to following preparation methods：
S301, oxidation processes：Technical grade methyl isobutyl ketone is added to by reactor 100 by feedstock transportation pump 170
It is interior, feedstock transportation pump 170 is closed, is blocked by valve between reactor 100 and 4A molecular sieve columns 110, alumina adsorption post 120
Pipeline, and the pipeline between connection reactor 100 and blender 105, and open the circulation pump 180, foundation forms reactor
100 bottom, circulating pump 180, the circulation line at top of blender 105 and reactor 100 are circulated, then to reactor
Potassium permanganate is added in 100 and carries out cyclic oxidation reaction, until the color of the solution in reactor 100 becomes purple；
S302, extraction processing：Aqueous sodium carbonate circulation stirring 1.5h is added into reactor 100, is then turned off circulating
Pump 180 is stood, and is discharged subnatant after solution layering in question response kettle 100, is retained upper liquid.Wherein；Carbon in aqueous sodium carbonate
The addition of sour sodium is the 30mol% of technical grade methyl isobutyl ketone addition.
S303,4A molecular sieve column adsorb：Close circulating pump 180, by valve block reactor 100 and blender 105 it
Between pipeline, and the pipeline between connection reactor 100 and 4A molecular sieve columns 110, open the circulation pump 180, establish formed it is anti-
The circulation line at the top of the bottom of kettle 100, circulating pump 180,4A molecular sieve columns 110 and reactor 100 is answered to carry out circulation absorption,
It is 1.2m/s, circulation absorption 35h to control flow velocity of the hexone in 4A molecular sieve columns by circulating pump 180.
S304, alumina adsorption；Close circulating pump 180, by valve block reactor 100 and 4A molecular sieve columns 110 it
Between pipeline, and connection reactor 100 and alumina adsorption post 120 between pipeline, open the circulation pump 180, establish formed
The bottom of reactor 100, circulating pump 180, the circulation line at top of alumina adsorption post 120 and reactor 100 are circulated
Absorption, and it is 0.8m/s to control flow velocity of the hexone in alumina adsorption post by circulating pump 180, circulation time
For 5h.
S305, rectifying；Circulating pump 180 is closed, starts rectifying, caused gas warp to the liquid heating in reactor 100
Rectifying column 130 is crossed, and infinite reflux is established between rectifying column 130, condenser 190 and return tank 200, infinite reflux 2 hours, then
Start to produce, remove slop cut before and after extraction, extraction midbarrel certified products (i.e. finished product) are transported to finished pot 140.
S306, ion exchange and filtering：Using finished product delivery pump 210 by rectifying obtains in finished pot 140 methyl tert-butyl
Base ketone passes sequentially through cation exchange column 150 and carries out ion exchange and filtered by filter 160, bottles, produces color
Compose pure hexone.
The chromatographically pure hexone in the embodiment of the present invention is detected below in conjunction with experiment.
The indices requirement of the chromatographically pure hexone of table 1
First, UV transmittance detection is carried out to the chromatographically pure hexone in embodiment 1~3：The instrument used
Model Shanghai spectrum ultraviolet specrophotometer SP-752 types, using 1cm quartz colorimetric utensils, after spectrophotometer start, preheating
After half an hour, start to detect, compareed using air, detect each sample in 335nm, 340nm, 360nm, 380nm,
UV transmittance under 400nm wavelength, it is as a result as follows：
The UV transmittance testing result of the chromatographically pure hexone of table 2
| Wavelength | 335nm | 340nm | 360nm | 380nm | 400nm |
| Raw material | 1 | 0.7 | 0.3 | 0.12 | 0.07 |
| Embodiment 1 | 0.55 | 0.3 | 0.05 | 0.006 | 0.005 |
| Embodiment 2 | 0.40 | 0.3 | 0.045 | 0.005 | 0.004 |
| Embodiment 3 | 0.40 | 0.25 | 0.045 | 0.005 | 0.004 |
| Chromatographically pure standard | ≤1 | ≤0.4 | ≤0.08 | ≤0.01 | ≤0.01 |
2nd, water content Indexs measure is carried out to the chromatographically pure hexone in embodiment 1~3, evaporation residue refers to
Mark detection and purity Indexs measure：Water content Indexs measure instrument model：Metrohm 831KF are led in Switzerland ten thousand；Evaporate residual
Slag Indexs measure instrument：Assay balance, evaporating dish, water bath with thermostatic control evaporation, baking oven；Purity Indexs measure instrument：
The flame ionization ditector (GC-FID) of the gas-chromatographies of Agilent 6890.Testing result is as follows：
Moisture, evaporation residue, the purity detecting of the chromatographically pure hexone of table 3
It can be seen that by above-mentioned testing result：The properties of the chromatographically pure hexone of the embodiment of the present invention refer to
Mark is substantially better than chromatographically pure hexone standard.
In summary, the preparation method technique of the chromatographically pure hexone of the embodiment of the present invention is simple, operation side
Just, it can produce to obtain that cost is low, the high chromatographically pure hexone of quality better, yield；The chromatogram of the embodiment of the present invention
The production system of pure hexone can be rapidly and efficiently production chromatographically pure hexone, realize chromatographically pure first
The scale industrial production of base isobutyl ketone.
Embodiments described above is part of the embodiment of the present invention, rather than whole embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made
Every other embodiment, belongs to the scope of protection of the invention.
Claims (10)
1. a kind of preparation method of chromatographically pure hexone, it is characterised in that it comprises the following steps：To technical grade first
Potassium permanganate progress oxidation reaction is added in base isobutyl ketone and obtains mixed liquor；Then to adding sodium carbonate in the mixed liquor
The aqueous solution stirs, stratification, enters upper liquid using 4A molecular sieve columns, alumina adsorption post successively after removing subnatant
Row adsorption treatment, afterwards rectifying.
2. the preparation method of chromatographically pure hexone according to claim 1, it is characterised in that to the industry
The potassium permanganate is added in level hexone until the mixed liquor becomes purple.
3. the preparation method of chromatographically pure hexone according to claim 2, it is characterised in that add described mixed
The dosage for closing sodium carbonate in the aqueous sodium carbonate in liquid is 10~30mol% of the technical grade methyl isobutyl ketone.
4. the preparation method of chromatographically pure hexone according to claim 1, it is characterised in that the upper liquid
The use of the 4A molecular sieve columns adsorption treatment is that upper liquid circulation is passed through in the 4A molecular sieve columns to be adsorbed, circulates
Adsorption time is 16~36h, and it is 0.1~2m/s to control flow velocity of the upper liquid in the 4A molecular sieve columns.
5. the preparation method of chromatographically pure hexone according to claim 1, it is characterised in that the upper liquid
The use of the alumina adsorption post adsorption treatment is that upper liquid circulation is passed through in the alumina adsorption post to be adsorbed,
The circulation absorption time is 3~6h, and it is 0.1~2m/s to control flow velocity of the upper liquid in the alumina adsorption post.
6. the preparation method of chromatographically pure hexone according to claim 1, it is characterised in that the rectifying is
Upper liquid after being adsorbed by alumina adsorption post is heated, caused gas passes through rectifying column, and establishes infinite reflux, infinite reflux
1~3 hour, start to produce, the certified products of extraction are finished product.
7. the preparation method of chromatographically pure hexone according to claim 1, it is characterised in that the preparation side
Method is additionally included in the ion exchange carried out successively after rectifying, filtration step.
8. a kind of chromatographically pure hexone, it is characterised in that it is used as any one of claim 1 to 7
The preparation method of chromatographically pure hexone is made.
9. a kind of production system of chromatographically pure hexone, it is characterised in that it includes：
Reactor, oxidation reaction is carried out for accommodating technical grade methyl isobutyl ketone, and to technical grade methyl isobutyl ketone
And heating；
Blender, for the technical grade methyl isobutyl ketone in reactor to be mixed with other raw materials；
4A molecular sieve columns, for carrying out 4A molecular sieve column absorption to technical grade methyl isobutyl ketone；
Alumina adsorption post, for carrying out alumina adsorption post absorption to technical grade methyl isobutyl ketone；
Rectifying column, for carrying out rectifying；And
Finished pot, for collecting finished product；
Wherein, the reactor is connected with the blender, the 4A molecular sieve columns and the alumina adsorption post respectively, described
Reactor, the rectifying column and the finished pot are sequentially connected with.
10. the production system of chromatographically pure hexone according to claim 9, it is characterised in that also include peace
Loaded on the circulating pump between the reactor and the blender, the 4A molecular sieve columns, the alumina adsorption post, Yi Jian
Loaded on the condenser at the top of the rectifying column, return tank, the reactor, the circulating pump and the blender formed be used for into
The circulation line of row circular response, the reactor, the circulating pump and the 4A molecular sieve columns are formed for circulate instead
The circulation line answered, the reactor, the circulating pump and the alumina adsorption post are formed for carrying out following for circulation absorption
Endless tube road；The rectifying column, the condenser and the return tank form the circulation line for carrying out infinite reflux.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102040496A (en) * | 2010-12-29 | 2011-05-04 | 天津市康科德科技有限公司 | Purification method of high-purity organic solvent 4-methyl-2-pentanone |
| CN103420792A (en) * | 2012-05-14 | 2013-12-04 | 浙江新化化工股份有限公司 | Combined production method of isopropanol and methyl isobutyl ketone |
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2017
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102040496A (en) * | 2010-12-29 | 2011-05-04 | 天津市康科德科技有限公司 | Purification method of high-purity organic solvent 4-methyl-2-pentanone |
| CN103420792A (en) * | 2012-05-14 | 2013-12-04 | 浙江新化化工股份有限公司 | Combined production method of isopropanol and methyl isobutyl ketone |
Non-Patent Citations (1)
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| 郭掌珍，张渊编著: "《环境POPs监测分析方法》", June 2013, 中国农业科学技术出版社 * |
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