CN107337614A - Chromatographically pure N, N dimethyl acetamide and preparation method thereof, production system - Google Patents
Chromatographically pure N, N dimethyl acetamide and preparation method thereof, production system Download PDFInfo
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- CN107337614A CN107337614A CN201710756461.5A CN201710756461A CN107337614A CN 107337614 A CN107337614 A CN 107337614A CN 201710756461 A CN201710756461 A CN 201710756461A CN 107337614 A CN107337614 A CN 107337614A
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
Abstract
A kind of chromatographically pure N, N dimethyl acetamides and preparation method thereof, production system, it is related to chemical products technical field of purification, chromatographically pure N, the preparation method of N dimethyl acetamides is to add barium monoxide in the feed first to be reacted, adsorbed secondly by activated carbon, adsorbed afterwards by 4A molecular sieves, then carry out rectifying, the preparation method production cost is low, obtained chromatographically pure N, N dimethyl acetamides quality better, yield are high, meet chromatographically pure reagent requirement.Chromatographically pure N; the production system of N dimethyl acetamides includes reactor, activated-charcoal column, 4A molecular sieve columns, rectifying column, finished pot; wherein; reactor is connected with activated-charcoal column, 4A molecular sieve columns respectively; the production system is dedicated for preparing chromatographically pure N; N dimethyl acetamides, realize the scale industrial production of chromatographically pure N, N dimethyl acetamide.
Description
Technical field
The present invention relates to chemical products technical field of purification, and more particularly to a kind of chromatographically pure DMA and
Its preparation 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 DMA is one of conventional liquid chromatogram mobile phase, both at home and abroad it has been reported that a variety of
The purifying process of DMA, purification process mainly include：Including：Decolourize, adsorb, rectifying, or decolourize, inhale
Attached, rectifying such as is combined at the step, is that product purity is not high the shortcomings that these purification process, is unsatisfactory for scientific research requirements, or yield
It is not high, cost is too high.
Therefore, it is necessary to a kind of low DMA preparation method of production cost, and using made from this method
Chromatographically pure DMA 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 DMA, the method is produced into
This is low, and obtained chromatographically pure DMA quality better, yield are high.
Another object of the present invention is to provide a kind of chromatographically pure DMA, its quality better, yield are high, full
Spectrum pure reagent requirement of standard purity.
Another object of the present invention is to provide a kind of production system of chromatographically pure DMA, its special use
In preparing chromatographically pure DMA, the scale industrial production of chromatographically pure DMA is realized.
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 DMA, and it comprises the following steps：
Using the DMA of technical grade as raw material, it is firstly added barium monoxide and is reacted, secondly by work
Property charcoal is adsorbed, and is adsorbed afterwards by 4A molecular sieves, then carries out rectifying.
Further, in present pre-ferred embodiments, adding the specific method that barium monoxide is reacted is：In N, N- bis-
Add barium monoxide in methylacetamide, the amount ratio of DMA and barium monoxide is 5~3000L：10~2000g,
Circular response 2~3 hours.
Further, in present pre-ferred embodiments, the specific method adsorbed by activated carbon is：Oxygen will be added
Change the reacted solution of barium and cycle through activated-charcoal column progress circular treatment, it is 0.1 to control flow velocity of the solution in activated-charcoal column
~2m/s, 3~5 hours circulation time.
Further, in present pre-ferred embodiments, the specific method adsorbed by 4A molecular sieves is：It will pass through
Solution circulation after charcoal absorption, which is passed through in 4A molecular sieve columns, carries out circular treatment, stream of the control solution in 4A molecular sieve columns
Speed is 0.1~2m/s, 16~36 hours circulation time.
Further, in present pre-ferred embodiments, the specific method of rectifying is：After by 4A molecular sieve adsorptions
Solution carries out heating rectifying, and caused gas passes through rectifying column, establishes infinite reflux, infinite reflux 1~3 hour, starts to produce, extraction
Certified products be finished product.
Further, in present pre-ferred embodiments, preparation method is additionally included in ion exchange, the mistake carried out after rectifying
Filter step.
A kind of chromatographically pure DMA, it uses the preparation side of above-mentioned chromatographically pure DMA
Method is made.
A kind of production system of chromatographically pure DMA, it includes：
Reactor, for the container reacted as addition barium monoxide；
Activated-charcoal column, for carrying out charcoal absorption；
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 activated-charcoal column, 4A molecular sieve columns respectively, and reactor, rectifying column and finished pot sequentially connect
Connect.
Further, in present pre-ferred embodiments, production system also includes being installed on reactor and activated-charcoal column, 4A
Circulating pump between molecular sieve column, formed between the top of the bottom of reactor, circulating pump and reactor anti-for circulate
The circulation line answered, the circulation line for carrying out circulation absorption is formed between reactor, circulating pump and activated-charcoal column, reacted
The circulation line for carrying out circulation absorption is formed between kettle, circulating pump and 4A molecular sieve columns.
Further, in present pre-ferred embodiments, production system also include being installed on condenser at the top of rectifying column,
Return tank, the circulation line for carrying out infinite reflux is formed between rectifying column, condenser and return tank.
The beneficial effect of chromatographically pure DMA of the embodiment of the present invention and preparation method thereof, production system
It is：The preparation method of the chromatographically pure DMA of the embodiment of the present invention is by the DMA of technical grade
As raw material, it is firstly added barium monoxide and is reacted, adsorbed secondly by activated carbon, is inhaled afterwards by 4A molecular sieves
It is attached, rectifying is then carried out, the preparation method production cost is low, obtained chromatographically pure DMA quality better, yield
Height, meet chromatographically pure reagent requirement.The production system of the chromatographically pure DMA of the embodiment of the present invention includes reaction
Kettle, activated-charcoal column, 4A molecular sieve columns, rectifying column, finished pot, wherein, reactor connects with activated-charcoal column, 4A molecular sieve columns respectively
Connect, reactor, rectifying column and finished pot are sequentially connected with, and the production system is dedicated for preparing chromatographically pure N, N- dimethylacetamide
Amine, realize the scale industrial production of chromatographically pure DMA.
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 DMA provided in an embodiment of the present invention.
Icon：100- production systems；001- feedstock transportation pumps；002- reactors；003- circulating pumps；004- blenders；
005- activated-charcoal columns；006-4A molecular sieve columns；007- rectifying columns；008- condensers；009- return tanks；010- finished pots；011-
Finished product delivery pump；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.
Have below to chromatographically pure DMA of the embodiment of the present invention and preparation method thereof, production system
Body explanation.
The embodiment of the present invention provides a kind of preparation method of chromatographically pure DMA, and it comprises the following steps：
Using the DMA of technical grade as raw material, it is firstly added barium monoxide and is reacted, carried out secondly by activated carbon
Absorption, adsorbed afterwards by 4A molecular sieves, then carry out rectifying, be preferably also included in carried out after rectifying ion exchange,
Filtration step.In the present embodiment, the preparation method of chromatographically pure DMA specifically includes following steps：
S1, addition barium monoxide are reacted：Barium monoxide, DMA are added in DMA
Amount ratio with barium monoxide is 5~3000L：10~2000g, circular response 2~3 hours.
S2, adsorbed by activated carbon：The reacted solution of barium monoxide will be added cycle through activated-charcoal column and followed
Ring processing, it is 0.1~2m/s to control flow velocity of the solution in activated-charcoal column, 3~5 hours circulation time.
S3, adsorbed by 4A molecular sieves：It will be passed through by the solution circulation after charcoal absorption in 4A molecular sieve columns
Circular treatment is carried out, it is 0.1~2m/s to control flow velocity of the solution in 4A molecular sieve columns, 16~36 hours circulation time.
S4, rectifying：Heating rectifying being carried out by the solution after 4A molecular sieve adsorptions, caused gas passes through rectifying column,
Infinite reflux is established, infinite reflux 1~3 hour, starts to produce, the certified products of extraction are finished product.
S5, ion exchange：Solution (i.e. finished product) obtained by rectifying is subjected to ion exchange by cation exchange column.
S6, 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 DMA, and it uses above-mentioned chromatographically pure N, N- diformazan
The preparation method of yl acetamide is made.
Shown in Figure 1, the embodiment of the present invention provides a kind of production system 100 of chromatographically pure DMA,
It includes：For as the reactor 002 for adding the container that barium monoxide is reacted；For carrying out the activated carbon of charcoal absorption
Post 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 for receiving
Collect the finished pot 010 of finished product；For carrying out the cation exchange column 012 of ion exchange；And the filter for being filtered
013, wherein, reactor 002 is connected with activated-charcoal column 005,4A molecular sieve columns 006 respectively, reactor 002, rectifying column 007, into
Product tank 010, cation exchange column 012 and filter 013 are sequentially connected with.
Wherein, what is filled in activated-charcoal column 005 is activating and regenerating type activated carbon；What is filled in 4A molecular sieve columns 006 is living
Change regenerative 4A molecular sieves；The height of rectifying column 007 is 2m~30m, and internal diameter is 4cm~220cm, loads glass spring in tower and fills out
At least one of material, the western tower ring of stainless steel, stainless steel structured packing and ceramic packing；The model of cation exchange column 012
ABD1UPW3EH1+IDO10-PFA-3/4 300；Filter 013 is 200nm filters, its model FLHF20010M3F300+
IDO10-PFA-3/4 300, the material of filter 013 are virgin pp 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 activated-charcoal column 005,4A molecular sieve columns
Circulating pump 003 between 006, formed for carrying out between the top of the bottom of reactor 002, circulating pump 003 and reactor 002
The circulation line of circular response, formed between reactor 002, circulating pump 003 and activated-charcoal column 005 for carrying out circulation absorption
Circulation line, the circulation pipe for carrying out circulation absorption is formed between reactor 002, circulating pump 003 and 4A molecular sieve columns 006
Road.
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 DMA, and it is to use the production system 100 shown in Fig. 1,
And it is made according to following preparation methods：
(1) using the DMA of technical grade as raw material, reactor is transported to by feedstock transportation pump 001
002, feedstock transportation pump 001 is closed, starts reactor 002 and stirs, open the circulation pump 003, establish the bottom for forming reactor 002
Portion, circulating pump 003, blender 004 and reactor 002 top between circulation line, the 1500L N into reactor 002,
In N- dimethyl acetamides plus barium monoxide 1000g, solution in reactor 002 circular response 2.5 hours in circulation line.
(2) circulation line that is formed between reactor 002, circulating pump 003 and activated-charcoal column 005 is established, in reactor 002
Solution (add barium monoxide reacted solution) cycle through activated-charcoal column 005 and carry out circular treatment, control solution is in work
Flow velocity in property charcoal post 005 is 1m/s, 4.5 hours circulation time.
(3) circulation line formed between reactor 002, circulating pump 003,4A molecular sieve columns 006, reactor 002 are established
Interior solution cycles through 4A molecular sieve columns 006 (i.e. by the solution after charcoal absorption) and carries out circular treatment, controls solution
Flow velocity in 4A molecular sieve columns 006 is 1m/s, 24 hours circulation time.
(4) rectifying, caused gas warp are heated to the solution of reactor 002 (i.e. by the solution after 4A molecular sieve adsorptions)
Rectifying column 007 is crossed, and infinite reflux is established between rectifying column 007, condenser 008 and return tank 009, infinite reflux 2 hours, then
Start to produce, slop cut before and after removing, produce middle right rail (i.e. finished product) and be delivered to finished pot 010.
(5) 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.
(6) solution obtained by ion exchange is filtered by filter 013, packing bottling, that is, obtains chromatographically pure N,
N- dimethyl acetamides, yield reach more than 95%.
Embodiment 2
The present embodiment provides a kind of chromatographically pure DMA, and it is to use the production system 100 shown in Fig. 1,
And it is made according to following preparation methods：
(1) using the DMA of technical grade as raw material, reactor is transported to by feedstock transportation pump 001
002, feedstock transportation pump 001 is closed, starts reactor 002 and stirs, open the circulation pump 003, establish the bottom for forming reactor 002
Portion, circulating pump 003, blender 004 and reactor 002 top between circulation line, 500L N, N- into reactor 002
In dimethyl acetamide plus barium monoxide 100g, solution in reactor 002 circular response 3 hours in circulation line.
(2) circulation line that is formed between reactor 002, circulating pump 003 and activated-charcoal column 005 is established, in reactor 002
Solution (add barium monoxide reacted solution) cycle through activated-charcoal column 005 and carry out circular treatment, control solution is in work
Flow velocity in property charcoal post 005 is 0.2m/s, 5 hours circulation time.
(3) circulation line formed between reactor 002, circulating pump 003,4A molecular sieve columns 006, reactor 002 are established
Interior solution cycles through 4A molecular sieve columns 006 (i.e. by the solution after charcoal absorption) and carries out circular treatment, controls solution
Flow velocity in 4A molecular sieve columns 006 is 0.2m/s, 36 hours circulation time.
(4) rectifying, caused gas warp are heated to the solution of reactor 002 (i.e. by the solution after 4A molecular sieve adsorptions)
Rectifying column 007 is crossed, and infinite reflux is established between rectifying column 007, condenser 008 and return tank 009, infinite reflux 1 hour, then
Start to produce, slop cut before and after removing, produce middle right rail (i.e. finished product) and be delivered to finished pot 010.
(5) 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.
(6) solution obtained by ion exchange is filtered by filter 013, packing bottling, that is, obtains chromatographically pure N,
N- dimethyl acetamides, yield reach more than 95%.
Embodiment 3
The present embodiment provides a kind of chromatographically pure DMA, and it is to use the production system 100 shown in Fig. 1,
And it is made according to following preparation methods：
(1) using the DMA of technical grade as raw material, reactor is transported to by feedstock transportation pump 001
002, feedstock transportation pump 001 is closed, starts reactor 002 and stirs, open the circulation pump 003, establish the bottom for forming reactor 002
Portion, circulating pump 003, blender 004 and reactor 002 top between circulation line, the 3000L N into reactor 002,
In N- dimethyl acetamides plus barium monoxide 2000g, solution in reactor 002 circular response 2 hours in circulation line.
(2) circulation line that is formed between reactor 002, circulating pump 003 and activated-charcoal column 005 is established, in reactor 002
Solution (add barium monoxide reacted solution) cycle through activated-charcoal column 005 and carry out circular treatment, control solution is in work
Flow velocity in property charcoal post 005 is 2m/s, 3 hours circulation time.
(3) circulation line formed between reactor 002, circulating pump 003,4A molecular sieve columns 006, reactor 002 are established
Interior solution cycles through 4A molecular sieve columns 006 (i.e. by the solution after charcoal absorption) and carries out circular treatment, controls solution
Flow velocity in 4A molecular sieve columns 006 is 2m/s, 16 hours circulation time.
(4) rectifying, caused gas warp are heated to the solution of reactor 002 (i.e. by the solution after 4A molecular sieve adsorptions)
Rectifying column 007 is crossed, and infinite reflux is established between rectifying column 007, condenser 008 and return tank 009, infinite reflux 3 hours, then
Start to produce, slop cut before and after removing, produce middle right rail (i.e. finished product) and be delivered to finished pot 010.
(5) 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.
(6) solution obtained by ion exchange is filtered by filter 013, packing bottling, that is, obtains chromatographically pure N,
N- dimethyl acetamides, yield reach more than 95%.
The chromatographically pure DMA in the embodiment of the present invention is detected below in conjunction with experiment.
The indices requirement of the chromatographically pure DMA of table 1
First, ultraviolet absorptivity detection is carried out to the chromatographically pure DMA in embodiment 1~3, it is as a result as follows：
The ultraviolet absorptivity testing result of the chromatographically pure DMA of table 2
| Wavelength | 270nm | 280nm | 290nm | 310nm | 320nm | 360nm |
| Raw material | 1 | 0.61 | 0.32 | 0.16 | 0.1 | 0.06 |
| Embodiment 1 | 0.7 | 0.21 | 0.06 | 0.03 | 0.015 | 0.005 |
| Embodiment 2 | 0.65 | 0.20 | 0.06 | 0.03 | 0.012 | 0.005 |
| Embodiment 3 | 0.65 | 0.20 | 0.052 | 0.026 | 0.012 | 0.004 |
| Chromatographically pure standard | ≤1 | ≤0.3 | ≤0.15 | ≤0.05 | ≤0.03 | ≤0.01 |
| Agriculture residual standard | ≤1 | ≤0.3 | ≤0.15 | ≤0.05 | ≤0.03 | ≤0.01 |
2nd, water content Indexs measure, evaporation residue are carried out to the chromatographically pure DMA in embodiment 1~3
Indexs measure and purity Indexs measure：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；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 result of the chromatographically pure DMA of table 3
It can be seen that by above-mentioned testing result：The properties of the chromatographically pure DMA of the embodiment of the present invention
Index is substantially better than chromatographically pure DMA standard.
In summary, the production cost of the preparation method of the chromatographically pure DMA of the embodiment of the present invention is low,
Obtained chromatographically pure DMA quality better, yield are high, meet chromatographically pure reagent requirement；The color of the embodiment of the present invention
The production system of pure DMA is composed dedicated for preparing chromatographically pure DMA, realizes chromatographically pure N,
The scale industrial production of N- dimethyl acetamides.
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 DMA, it is characterised in that it comprises the following steps：
Using the DMA of technical grade as raw material, it is firstly added barium monoxide and is reacted, secondly by activated carbon
Adsorbed, adsorbed afterwards by 4A molecular sieves, then carry out rectifying.
2. the preparation method of chromatographically pure DMA according to claim 1, it is characterised in that add oxidation
The specific method that barium is reacted is：Add barium monoxide in DMA, the DMA and
The amount ratio of the barium monoxide is 5~3000L：10~2000g, circular response 2~3 hours.
3. the preparation method of chromatographically pure DMA according to claim 1, it is characterised in that pass through activity
The specific method that charcoal is adsorbed is：The reacted solution of barium monoxide will be added and cycle through activated-charcoal column progress circular treatment,
It is 0.1~2m/s to control flow velocity of the solution in the activated-charcoal column, 3~5 hours circulation time.
4. the preparation method of chromatographically pure DMA according to claim 1, it is characterised in that pass through 4A points
Son sieves the specific method adsorbed：Circulated being passed through by the solution circulation after charcoal absorption in 4A molecular sieve columns
Processing, it is 0.1~2m/s to control flow velocity of the solution in the 4A molecular sieve columns, 16~36 hours circulation time.
5. the preparation method of chromatographically pure DMA according to claim 1, it is characterised in that the tool of rectifying
Body method is：Heating rectifying will be carried out by the solution after 4A molecular sieve adsorptions, caused gas passes through rectifying column, establishes complete return
Stream, infinite reflux 1~3 hour, starts to produce, the certified products of extraction are finished product.
6. the preparation method of chromatographically pure DMA according to claim 1, it is characterised in that the preparation
Method is additionally included in the ion exchange carried out after rectifying, filtration step.
7. a kind of chromatographically pure DMA, it is characterised in that it is used as any one of claim 1 to 6
The preparation method of chromatographically pure DMA be made.
8. a kind of production system of chromatographically pure DMA, it is characterised in that it includes：
Reactor, for the container reacted as addition barium monoxide；
Activated-charcoal column, for carrying out charcoal absorption；
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 activated-charcoal column, the 4A molecular sieve columns respectively, the reactor, the rectifying
Tower and the finished pot are sequentially connected with.
9. the production system of chromatographically pure DMA according to claim 8, it is characterised in that the production
System also includes the circulating pump being installed between the reactor and the activated-charcoal column, the 4A molecular sieve columns, the reaction
The circulation line for carrying out circular response is formed between the top of the bottom of kettle, the circulating pump and the reactor, it is described
Form the circulation line for carrying out circulation absorption between reactor, the circulating pump and the activated-charcoal column, the reactor,
The circulation line for carrying out circulation absorption is formed between the circulating pump and the 4A molecular sieve columns.
10. the production system of chromatographically pure DMA according to claim 9, it is characterised in that described anti-
Answer and be provided with blender on the circulation line formed between the top of the bottom of kettle, the circulating pump and the reactor.
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