CN107382669A - Chromatographically pure n-butanol and preparation method thereof, production system - Google Patents
Chromatographically pure n-butanol and preparation method thereof, production system Download PDFInfo
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- CN107382669A CN107382669A CN201710756996.2A CN201710756996A CN107382669A CN 107382669 A CN107382669 A CN 107382669A CN 201710756996 A CN201710756996 A CN 201710756996A CN 107382669 A CN107382669 A CN 107382669A
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- 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
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
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- 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
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- 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
- C07C29/88—Separation; Purification; Use of additives, e.g. for stabilisation by treatment giving rise to a chemical modification of at least one compound
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Abstract
A kind of chromatographically pure n-butanol and preparation method thereof, production system, it is related to chemical products technical field of purification, the preparation method of chromatographically pure n-butanol is using the n-butanol of technical grade as raw material, is firstly added magnesium powder and is reacted, next is filtered, and adsorbed by 4A molecular sieves, sulfanilic acid is added afterwards to be reacted, and then carries out rectifying, the preparation method production cost is low, obtained chromatographically pure n-butanol quality better, yield are high, meet chromatographically pure reagent requirement.The production system of chromatographically pure n-butanol includes reactor, 200nm Filter columns, 4A molecular sieve columns, rectifying column, finished pot; wherein; reactor is connected with 200nm Filter columns, 4A molecular sieve columns respectively; reactor, rectifying column and finished pot are sequentially connected with; the production system realizes the scale industrial production of chromatographically pure n-butanol dedicated for preparing chromatographically pure n-butanol.
Description
Technical field
The present invention relates to chemical products technical field of purification, and more particularly to a kind of chromatographically pure n-butanol and its preparation side
Method, production system.
Background technology
Chromatographically pure refers to carry out the standard reagent or solvent used during chromatography, its ultraviolet light absorption at low wavelength
Degree under chromatographic condition, the peak of appointed compound can only occur than relatively low, 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 what China had by oneself
The standardization industry of chromatogram pure reagent has great meaning and effect.
Chromatographically pure n-butanol is one of conventional liquid chromatogram mobile phase, both at home and abroad it has been reported that a variety of n-butanols it is pure
Chemical industry skill, purification process mainly include：Including：Decolourize, absorption, rectifying, or decolourize, absorption, rectifying such as are combined at the step, this
The shortcomings that a little purification process is that product purity is not high, is unsatisfactory for scientific research requirements, or yield is not high, cost is too high.
Therefore, it is necessary to a kind of low n-butanol preparation method of production cost, and using the pure fourth of chromatogram made from this method
Alcohol quality better, yield are high, can meet chromatographically pure reagent requirement.
The content of the invention
It is an object of the invention to provide a kind of preparation method of chromatographically pure n-butanol, the method production cost is low, is made
Chromatographically pure n-butanol quality better, yield it is high.
Another object of the present invention is to provide a kind of chromatographically pure n-butanol, its quality better, yield are high, meet that chromatographically pure tries
Agent requirement.
Another object of the present invention is to provide a kind of production system of chromatographically pure n-butanol, it is dedicated for preparation chromatogram
Pure butanol, realize the scale industrial production of chromatographically pure n-butanol.
The present invention is solved its technical problem and realized using following technical scheme.
The present invention proposes a kind of preparation method of chromatographically pure n-butanol, and it comprises the following steps：
Using the n-butanol of technical grade as raw material, it is firstly added magnesium powder and is reacted, next is filtered, and passes through 4A points
Son sieve is adsorbed, and is added sulfanilic acid afterwards and is reacted, then carries out rectifying.
Further, in present pre-ferred embodiments, adding the specific method that magnesium powder is reacted is：In n-butanol
The amount ratio of addition magnesium powder, n-butanol and magnesium powder is 5~3000L：5~3000g, in 60~90 DEG C of circular responses 2~3 hours.
Further, in present pre-ferred embodiments, the specific method of filtering is：The reacted solution of magnesium powder will be added
Cycle through 200nm Filter columns and carry out circular treatment, 1~2 hour circulation time.
Further, in present pre-ferred embodiments, the specific method adsorbed by 4A molecular sieves is：Will filtering
Solution circulation afterwards, which is passed through in 4A molecular sieve columns, carries out circular treatment, 16~36 hours circulation time.
Further, in present pre-ferred embodiments, adding the specific method that sulfanilic acid is reacted is：Passing through 4A
Add sulfanilic acid in solution after molecular sieve adsorption, the amount ratio of solution and sulfanilic acid is 5~3000L：10~3500g, in 90
~110 DEG C, stirring reaction 2~3 hours.
Further, in present pre-ferred embodiments, the specific method of rectifying is：It is reacted molten to adding sulfanilic acid
Liquid carries out heating rectifying, and caused gas passes through rectifying column, establishes infinite reflux, infinite reflux 3~5 hours, starts to produce, extraction
Certified products are finished product.
Further, in present pre-ferred embodiments, preparation method is additionally included in ion exchange, the mistake carried out after rectifying
Filter step.
The present invention proposes a kind of chromatographically pure n-butanol, and it uses the preparation method of above-mentioned chromatographically pure n-butanol to be made.
The present invention proposes a kind of production system of chromatographically pure n-butanol, and it includes：
Reactor, the container reacted for sulfanilic acid to be reacted, added as addition magnesium powder；
200nm Filter columns, for being filtered；
4A molecular sieve columns, for carrying out 4A molecular sieve adsorptions；
Rectifying column, for carrying out rectifying；And
Finished pot, for collecting finished product,
Wherein, reactor is connected with 200nm Filter columns, 4A molecular sieve columns respectively, and reactor, rectifying column and finished pot are sequentially
Connection.
Further, in present pre-ferred embodiments, production system also includes being installed on reactor and 200nm filterings
Circulating pump between post, 4A molecular sieve columns, formed for being followed between the top of the bottom of reactor, circulating pump and reactor
The circulation line of ring reaction, reactor, circulating pump and 200nm Filter columns form the circulation line for carrying out circular treatment, instead
Kettle, circulating pump and 4A molecular sieve columns is answered to form the circulation line for carrying out circular treatment.
Chromatographically pure n-butanol of the embodiment of the present invention and preparation method thereof, the beneficial effect of production system are：It is of the invention real
The preparation method for applying the chromatographically pure n-butanol of example is using the n-butanol of technical grade as raw material, is firstly added magnesium powder and is reacted,
Next is filtered, and is adsorbed by 4A molecular sieves, is added sulfanilic acid afterwards and is reacted, then carries out rectifying, the system
Preparation Method production cost is low, and obtained chromatographically pure n-butanol quality better, yield are high, meet chromatographically pure reagent requirement.It is of the invention real
Applying the production system of the chromatographically pure n-butanol of example includes reactor, 200nm Filter columns, 4A molecular sieve columns, rectifying column, finished pot,
Wherein, reactor is connected with 200nm Filter columns, 4A molecular sieve columns respectively, and reactor, rectifying column and finished pot are sequentially connected with, should
Production system realizes the scale industrial production of chromatographically pure n-butanol dedicated for preparing chromatographically pure n-butanol.
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 n-butanol provided in an embodiment of the present invention.
Icon：100- production systems；001- feedstock transportation pumps；002- reactors；003- circulating pumps；004- blenders；
005-200nm Filter columns；006-4A molecular sieve columns；007- rectifying columns；008- condensers；009- return tanks；010- finished pots；
011- finished product delivery pumps；012- cation exchange columns；013- 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.
Chromatographically pure n-butanol of the embodiment of the present invention and preparation method thereof, production system are specifically described below.
The embodiment of the present invention provides a kind of preparation method of chromatographically pure n-butanol, and it comprises the following steps：By technical grade
N-butanol is firstly added magnesium powder and reacted, next is filtered, and is adsorbed by 4A molecular sieves, afterwards as raw material
Add sulfanilic acid to be reacted, then carry out rectifying, be preferably also included in the ion exchange carried out after rectifying, filtration step.This
In embodiment, the preparation method of chromatographically pure n-butanol specifically includes following steps：
S1, addition magnesium powder are reacted：Add magnesium powder in n-butanol, the amount ratio of n-butanol and magnesium powder for 5~
3000L：5~3000g, in 60~90 DEG C of circular responses 2~3 hours.
S2, filtering：The reacted solution of magnesium powder will be added cycle through 200nm Filter columns and carry out circular treatment, during circulation
Between 1~2 hour.
S3, adsorbed by 4A molecular sieves：Solution circulation after filtering is passed through in 4A molecular sieve columns and carried out at circulation
Reason, 16~36 hours circulation time.
S4, addition sulfanilic acid are reacted：Sulfanilic acid, solution and sulphur are added in the solution after by 4A molecular sieve adsorptions
The amount ratio of amino acid is 5~3000L：10~3500g, in 90~110 DEG C, stirring reaction 2~3 hours.
S5, rectifying：Heating rectifying is carried out to adding the reacted solution of sulfanilic acid, caused gas passes through rectifying column, built
Vertical infinite reflux, infinite reflux 3~5 hours, starts to produce, the certified products of extraction are finished product.
S6, ion exchange：Solution (i.e. finished product) obtained by rectifying is subjected to ion exchange by cation exchange column.
S7, filtering：Solution obtained by ion exchange is filtered by filter, bottles, produces chromatographically pure hexamethylene.
In the present embodiment, filter is 200nm filters.
The embodiment of the present invention provides a kind of chromatographically pure n-butanol, and it uses the preparation method system of above-mentioned chromatographically pure n-butanol
.
Shown in Figure 1, the embodiment of the present invention provides a kind of production system 100 of chromatographically pure n-butanol, and it includes：For
The reactor 002 for the container that sulfanilic acid is reacted is reacted, added as addition magnesium powder；For the 200nm filtered
Filter column 005；For carrying out the 4A molecular sieve columns 006 of 4A molecular sieve adsorptions；For carrying out the rectifying column 007 of rectifying；And use
In the finished pot 010 for collecting finished product；For carrying out the cation exchange column 012 of ion exchange；And the mistake for being filtered
Filter 013, wherein, reactor 002 is connected with 200nm Filter columns 005,4A molecular sieve columns 006 respectively, reactor 002, rectifying column
007th, finished pot 010, cation exchange column 012 and filter 013 are sequentially connected with.
Wherein, what is filled in 4A molecular sieve columns 006 is activating and regenerating type 4A molecular sieves；The height of rectifying column 007 be 2m~
30m, internal diameter are 4cm~220cm, load glass spring filler, the western tower ring of stainless steel, stainless steel structured packing and ceramics in tower and fill out
At least one of material；The model ABD1UPW3EH1+IDO10-PFA-3/4 300 of cation exchange column 012；Filter 013
For 200nm filters, its model FLHF20010M3F300+IDO10-PFA-3/4 300, the material of filter 013 is pure poly- third
Alkene or pure polytetrafluoroethylene (PTFE).
In the present embodiment, production system 100 also includes feedstock transportation pump 001 and finished product delivery pump 011, feedstock transportation pump
001 is connected with reactor 002, for raw material automatic transport to be entered in reactor 002；Finished product delivery pump 011 is installed on finished pot
Between 010 and cation exchange column 012, for by the finished product automatic transport in finished pot 010 to cation exchange column 012.
In the present embodiment, production system 100 also includes being installed on reactor 002 and 200nm Filter columns 005,4A molecular sieves
Circulating pump 003 between post 006, formed between the top of the bottom of reactor 002, circulating pump 003 and reactor 002 be used for into
The circulation line of row circular response, reactor 002, circulating pump 003 and 200nm Filter columns 005 are formed for carrying out circular treatment
Circulation line, reactor 002, circulating pump 003 and 4A molecular sieve columns 006 form the circulation line for carrying out circular treatment.
In the present embodiment, the circulation pipe that is formed between the top of the bottom of reactor 002, circulating pump 003 and reactor 002
Blender 004 is provided with road, specifically, the bottom of reactor 002, circulating pump 003, the top of blender 004 and reactor 002
Portion forms circulation line.
In the present embodiment, production system 100 also includes condenser 008, the return tank 009 for being installed on the top of rectifying column 007,
Rectifying column 007, condenser 008 and return tank 009 form the circulation line for carrying out infinite reflux, fully to carry out rectifying.
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 n-butanol, and it is to use the production system 100 shown in Fig. 1, and according to following
Preparation method be made：
(1) using the n-butanol of technical grade as raw material, reactor 002 is transported to by feedstock transportation pump 001, closes raw material
Delivery pump 001, reactor 002 is warming up to 75 DEG C, starts reactor 002 and stir, open the circulation pump 003, establish and form reaction
The bottom of kettle 002, circulating pump 003, blender 004 and reactor 002 top between circulation line, into reactor 002
1500L n-butanols add magnesium powder 1500g, circular response 2.5 hours in circulation line of the solution in reactor 002.
(2) circulation line formed between reactor 002, circulating pump 003 and 200nm Filter columns 005, reactor are established
Solution (adding the reacted solution of magnesium powder) in 002 cycles through 200nm Filter columns 005 and carries out circular treatment, circulation 1.5
Hour.
(3) circulation line formed between reactor 002, circulating pump 003,4A molecular sieve columns 006, reactor 002 are established
Interior solution (solution after filtering) cycles through 4A molecular sieve columns 006 and carries out circular treatment, circulates 24 hours, stops following
Ring, reactor 002 is kept to stir.
(4) sulfanilic acid is added in the 1400L solution into reactor 002 (i.e. by the solution after 4A molecular sieve adsorptions)
1600g, reactor 002 is warming up to 100 DEG C, stirring reaction 2.5 hours, stops reactor 002 and stirs.
(5) solution (adding the reacted solution of sulfanilic acid) heating rectifying of reactor 002, caused gas are passed through
Rectifying column 007, and infinite reflux is established between rectifying column 007, condenser 008 and return tank 009, infinite reflux 4 hours, Ran Houkai
Begin to produce, slop cut before and after extraction, produce middle right rail (i.e. finished product) and be delivered to finished pot 010.
(6) start finished product delivery pump 011, the solution (finished product i.e. obtained by rectifying) in finished pot 010 is passed through into cation
Exchange column 012 carries out ion exchange.
(7) solution obtained by ion exchange is filtered by filter 013, packing bottling, that is, is obtaining chromatographically pure just
Butanol, yield reach more than 95%.
Embodiment 2
The present embodiment provides a kind of chromatographically pure n-butanol, and it is to use the production system 100 shown in Fig. 1, and according to following
Preparation method be made：
(1) using the n-butanol of technical grade as raw material, reactor 002 is transported to by feedstock transportation pump 001, closes raw material
Delivery pump 001, reactor 002 is warming up to 60 DEG C, starts reactor 002 and stir, open the circulation pump 003, establish and form reaction
The bottom of kettle 002, circulating pump 003, blender 004 and reactor 002 top between circulation line, into reactor 002
500L n-butanols add magnesium powder 100g, circular response 2 hours in circulation line of the solution in reactor 002.
(2) circulation line formed between reactor 002, circulating pump 003 and 200nm Filter columns 005, reactor are established
Solution (adding the reacted solution of magnesium powder) in 002 cycles through 200nm Filter columns 005 and carries out circular treatment, and circulation 1 is small
When.
(3) circulation line formed between reactor 002, circulating pump 003,4A molecular sieve columns 006, reactor 002 are established
Interior solution (solution after filtering) cycles through 4A molecular sieve columns 006 and carries out circular treatment, circulates 36 hours, stops following
Ring, reactor 002 is kept to stir.
(4) sulfanilic acid is added in the 480L solution into reactor 002 (i.e. by the solution after 4A molecular sieve adsorptions)
3000g, reactor 002 is warming up to 110 DEG C, stirring reaction 3 hours, stops reactor 002 and stirs.
(5) solution (adding the reacted solution of sulfanilic acid) heating rectifying of reactor 002, caused gas are passed through
Rectifying column 007, and infinite reflux is established between rectifying column 007, condenser 008 and return tank 009, infinite reflux 5 hours, Ran Houkai
Begin to produce, slop cut before and after extraction, produce middle right rail (i.e. finished product) and be delivered to finished pot 010.
(6) start finished product delivery pump 011, the solution (finished product i.e. obtained by rectifying) in finished pot 010 is passed through into cation
Exchange column 012 carries out ion exchange.
(7) solution obtained by ion exchange is filtered by filter 013, packing bottling, that is, is obtaining chromatographically pure just
Butanol, yield reach more than 95%.
Embodiment 3
The present embodiment provides a kind of chromatographically pure n-butanol, and it is to use the production system 100 shown in Fig. 1, and according to following
Preparation method be made：
(1) using the n-butanol of technical grade as raw material, reactor 002 is transported to by feedstock transportation pump 001, closes raw material
Delivery pump 001, reactor 002 is warming up to 90 DEG C, starts reactor 002 and stir, open the circulation pump 003, establish and form reaction
The bottom of kettle 002, circulating pump 003, blender 004 and reactor 002 top between circulation line, into reactor 002
3000L n-butanols add magnesium powder 3000g, circular response 3 hours in circulation line of the solution in reactor 002.
(2) circulation line formed between reactor 002, circulating pump 003 and 200nm Filter columns 005, reactor are established
Solution (adding the reacted solution of magnesium powder) in 002 cycles through 200nm Filter columns 005 and carries out circular treatment, and circulation 2 is small
When.
(3) circulation line formed between reactor 002, circulating pump 003,4A molecular sieve columns 006, reactor 002 are established
Interior solution (solution after filtering) cycles through 4A molecular sieve columns 006 and carries out circular treatment, circulates 16 hours, stops following
Ring, reactor 002 is kept to stir.
(4) sulfanilic acid is added in the 2900L solution into reactor 002 (i.e. by the solution after 4A molecular sieve adsorptions)
200g, reactor 002 is warming up to 90 DEG C, stirring reaction 2 hours, stops reactor 002 and stirs.
(5) solution (adding the reacted solution of sulfanilic acid) heating rectifying of reactor 002, caused gas are passed through
Rectifying column 007, and infinite reflux is established between rectifying column 007, condenser 008 and return tank 009, infinite reflux 3 hours, Ran Houkai
Begin to produce, slop cut before and after extraction, produce middle right rail (i.e. finished product) and be delivered to finished pot 010.
(6) start finished product delivery pump 011, the solution (finished product i.e. obtained by rectifying) in finished pot 010 is passed through into cation
Exchange column 012 carries out ion exchange.
(7) solution obtained by ion exchange is filtered by filter 013, packing bottling, that is, is obtaining chromatographically pure just
Butanol, yield reach more than 95%.
The chromatographically pure n-butanol in the embodiment of the present invention is detected below in conjunction with experiment.
The indices requirement of the chromatographically pure n-butanol of table 1
First, ultraviolet absorptivity detection is carried out to the chromatographically pure n-butanol in embodiment 1~3, it is as a result as follows：
The ultraviolet absorptivity testing result of the chromatographically pure n-butanol of table 2
| Wavelength | 215nm | 220nm | 240nm | 260nm | 280nm | 400nm |
| Raw material | 1 | 0.8 | 0.5 | 0.12 | 0.07 | 0.04 |
| Embodiment 1 | 0.65 | 0.35 | 0.05 | 0.012 | 0.006 | 0.004 |
| Embodiment 2 | 0.60 | 0.30 | 0.04 | 0.01 | 0.006 | 0.004 |
| Embodiment 3 | 0.60 | 0.30 | 0.04 | 0.01 | 0.005 | 0.003 |
| Chromatographically pure standard | ≤1 | ≤0.5 | ≤0.1 | ≤0.04 | ≤0.01 | ≤0.01 |
| Agriculture residual standard | ≤1 | ≤0.5 | ≤0.1 | ≤0.04 | ≤0.01 | ≤0.01 |
2nd, the chromatographically pure n-butanol in embodiment 1~3 is carried out water content Indexs measure, evaporation residue Indexs measure and
Purity Indexs measure：Water content Indexs measure instrument model：Metrohm 831KF are led in Switzerland ten thousand；Evaporation residue index is examined
Survey instrument：Assay balance, evaporating dish, water bath with thermostatic control evaporation, baking oven；Purity Indexs measure instrument：Agilent
The flame ionization ditector (GC-FID) of 6890 gas-chromatographies.Testing result is as follows：
Moisture, evaporation residue, the purity detecting result of the chromatographically pure n-butanol of table 3
It can be seen that by above-mentioned testing result：The property indices of the chromatographically pure n-butanol of the embodiment of the present invention are substantially excellent
In chromatographically pure n-butanol standard.
In summary, the production cost of the preparation method of the chromatographically pure n-butanol of the embodiment of the present invention is low, obtained chromatogram
Pure butanol quality better, yield are high, meet chromatographically pure reagent requirement；The production system of the chromatographically pure n-butanol of the embodiment of the present invention
Dedicated for preparing chromatographically pure n-butanol, the scale industrial production of chromatographically pure n-butanol is realized.
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 n-butanol, it is characterised in that it comprises the following steps：
Using the n-butanol of technical grade as raw material, it is firstly added magnesium powder and is reacted, next is filtered, and passes through 4A molecular sieves
Adsorbed, add sulfanilic acid afterwards and reacted, then carry out rectifying.
2. the preparation method of chromatographically pure n-butanol according to claim 1, it is characterised in that add what magnesium powder was reacted
Specific method is：Add magnesium powder in n-butanol, the amount ratio of the n-butanol and the magnesium powder is 5~3000L：5~
3000g, in 60~90 DEG C of circular responses 2~3 hours.
3. the preparation method of chromatographically pure n-butanol according to claim 1, it is characterised in that the specific method of filtering is：
The reacted solution of magnesium powder will be added and cycle through 200nm Filter columns progress circular treatment, 1~2 hour circulation time.
4. the preparation method of chromatographically pure n-butanol according to claim 1, it is characterised in that inhaled by 4A molecular sieves
Attached specific method is：Solution circulation after filtering is passed through in 4A molecular sieve columns and carries out circular treatment, circulation time 16~36
Hour.
5. the preparation method of chromatographically pure n-butanol according to claim 1, it is characterised in that add sulfanilic acid and reacted
Specific method be：The use of sulfanilic acid, the solution and the sulfanilic acid is added in the solution after by 4A molecular sieve adsorptions
It is 5~3000L to measure ratio：10~3500g, in 90~110 DEG C, stirring reaction 2~3 hours.
6. the preparation method of chromatographically pure n-butanol according to claim 1, it is characterised in that the specific method of rectifying is：
Heating rectifying is carried out to adding the reacted solution of sulfanilic acid, 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.
7. the preparation method of chromatographically pure n-butanol according to claim 1, it is characterised in that the preparation method also includes
The ion exchange that is carried out after rectifying, filtration step.
8. a kind of chromatographically pure n-butanol, it is characterised in that it uses the chromatogram as any one of claim 1 to 7 pure
The preparation method of butanol is made.
9. a kind of production system of chromatographically pure n-butanol, it is characterised in that it includes：
Reactor, the container reacted for sulfanilic acid to be reacted, added as addition magnesium powder；
200nm Filter columns, for being filtered；
4A molecular sieve columns, for carrying out 4A molecular sieve adsorptions；
Rectifying column, for carrying out rectifying；And
Finished pot, for collecting finished product,
Wherein, the reactor is connected with the 200nm Filter columns, the 4A molecular sieve columns respectively, the reactor, the essence
Evaporate tower and the finished pot is sequentially connected with.
10. the production system of chromatographically pure n-butanol according to claim 9, it is characterised in that the production system is also wrapped
Include the circulating pump being installed between the reactor and the 200nm Filter columns, the 4A molecular sieve columns, the bottom of the reactor
Form the circulation line for carrying out circular response between the top in portion, the circulating pump and the reactor, the reactor,
The circulating pump and the 200nm Filter columns form the circulation line for carrying out circular treatment, the reactor, the circulation
Pump and the 4A molecular sieve columns form the circulation line for carrying out circular treatment.
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| CN103508847A (en) * | 2013-09-30 | 2014-01-15 | 天津大学 | Method and device for recycling high-purity butyl alcohol by dehydrating butyl alcohol |
| CN104557457A (en) * | 2014-11-28 | 2015-04-29 | 天津大学 | Reactive distillation method and reactive distillation device for producing butanol by hydrogenating butyraldehyde |
| CN106397125A (en) * | 2015-08-03 | 2017-02-15 | 天津市光复科技发展有限公司 | Preparation method for combined production of chromatographically pure isobutanol and high-purity chromatographic standard isobutanol |
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