CN107382711A - Chromatographically pure glacial acetic acid and preparation method thereof, production system - Google Patents
Chromatographically pure glacial acetic acid and preparation method thereof, production system Download PDFInfo
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- CN107382711A CN107382711A CN201710756989.2A CN201710756989A CN107382711A CN 107382711 A CN107382711 A CN 107382711A CN 201710756989 A CN201710756989 A CN 201710756989A CN 107382711 A CN107382711 A CN 107382711A
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
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Abstract
A kind of chromatographically pure glacial acetic acid and preparation method thereof, production system, it is related to chemical products technical field of purification, the preparation method of chromatographically pure glacial acetic acid is the glacial acetic acid using technical grade as raw material, it is firstly added aceticanhydride to be reacted, secondly adds potassium permanganate and reacted, adsorbed afterwards by activated carbon, then rectifying is carried out, the preparation method production cost is low, and obtained chromatographically pure glacial acetic acid quality better, yield are high, meet chromatographically pure reagent requirement.The production system of chromatographically pure glacial acetic acid includes reactor, activated-charcoal column, rectifying column, finished pot; wherein; reactor is connected with activated-charcoal column; reactor, rectifying column and finished pot are sequentially connected with; the production system realizes the scale industrial production of chromatographically pure glacial acetic acid dedicated for preparing chromatographically pure glacial acetic acid.
Description
Technical field
The present invention relates to chemical products technical field of purification, and more particularly to a kind of chromatographically pure glacial acetic acid 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 glacial acetic acid is one of conventional liquid chromatogram mobile phase, both at home and abroad it has been reported that a variety of glacial acetic acids 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 glacial acetic acid preparation method of production cost, and using chromatographically pure ice second made from this method
Sour 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 glacial acetic acid, the method production cost is low, is made
Chromatographically pure glacial acetic acid quality better, yield it is high.
Another object of the present invention is to provide a kind of chromatographically pure glacial acetic acid, 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 glacial acetic acid, it is dedicated for preparation chromatogram
Pure glacial acetic acid, realize the scale industrial production of chromatographically pure glacial acetic acid.
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 glacial acetic acid, and it comprises the following steps：
Using the glacial acetic acid of technical grade as raw material, it is firstly added aceticanhydride and is reacted, secondly add potassium permanganate and carry out instead
Should, adsorbed afterwards by activated carbon, then carry out rectifying.
Further, in present pre-ferred embodiments, adding the specific method that aceticanhydride is reacted is：In glacial acetic acid
Add aceticanhydride, circular response 1~2 hour.
Further, in present pre-ferred embodiments, adding the specific method that potassium permanganate is reacted is：Adding
Potassium permanganate, circular response are added in the reacted solution of aceticanhydride, until solution no longer changes colour.
Further, in present pre-ferred embodiments, the specific method adsorbed by activated carbon is：It will add high
The circulation of potassium manganate reacted solution, which is passed through in activated-charcoal column, carries out circular treatment, controls flow velocity of the solution in activated-charcoal column to be
0.1~2m/s, untill solution is colourless.
Further, in present pre-ferred embodiments, the specific method of rectifying is：To by molten after charcoal absorption
Liquid 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 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.
A kind of chromatographically pure glacial acetic acid, it uses the preparation method of above-mentioned chromatographically pure glacial acetic acid to be made.
A kind of production system of chromatographically pure glacial acetic acid, it includes：
Reactor, the container reacted for potassium permanganate to be reacted, added as addition aceticanhydride；
Activated-charcoal column, for carrying out charcoal absorption；
Rectifying column, for carrying out rectifying；And
Finished pot, for collecting finished product,
Wherein, reactor is connected with activated-charcoal column, and reactor, rectifying column and finished pot are sequentially connected with.
Further, in present pre-ferred embodiments, production system also include being installed on reactor and activated-charcoal column it
Between circulating pump, form the circulation pipe for carrying out circular response between the top of the bottom of reactor, circulating pump and reactor
Road, the circulation line for carrying out circular treatment is formed between reactor, circulating pump and activated-charcoal column.
Further, in present pre-ferred embodiments, shape between the top of the bottom of reactor, circulating pump and reactor
Into circulation line on be provided with blender.
Chromatographically pure glacial acetic acid 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 glacial acetic acid of example is using the glacial acetic acid of technical grade as raw material, is firstly added aceticanhydride and is reacted,
Secondly add potassium permanganate to be reacted, adsorbed afterwards by activated carbon, then carry out rectifying, the preparation method is produced into
This is low, and obtained chromatographically pure glacial acetic acid quality better, yield are high, meet chromatographically pure reagent requirement.The chromatographically pure of the embodiment of the present invention
The production system of glacial acetic acid includes reactor, activated-charcoal column, rectifying column, finished pot, wherein, reactor is connected with activated-charcoal column,
Reactor, rectifying column and finished pot are sequentially connected with, and the production system realizes chromatographically pure ice dedicated for preparing chromatographically pure glacial acetic acid
The scale industrial production of acetic acid.
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 glacial acetic acid 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- rectifying columns；007- condensers；008- return tanks；009- finished pots；010- finished product delivery pumps；011-
Cation exchange column；012- 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 glacial acetic acid 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 glacial acetic acid, and it comprises the following steps：By technical grade
Glacial acetic acid is firstly added aceticanhydride and reacted, secondly add potassium permanganate and reacted, entered afterwards by activated carbon as raw material
Row absorption, then carries out rectifying, is preferably also included in the ion exchange carried out after rectifying, filtration step.In the present embodiment, chromatogram
The preparation method of pure glacial acetic acid specifically includes following steps：
S1, addition aceticanhydride are reacted：Aceticanhydride, circular response 1~2 hour are added in glacial acetic acid.
S2, addition potassium permanganate are reacted：Potassium permanganate is added in the reacted solution of aceticanhydride is added, circulation is anti-
Should, until solution no longer changes colour.
S3, adsorbed by activated carbon：The reacted solution circulation of potassium permanganate will be added to be passed through in activated-charcoal column
Row circular treatment, untill solution is colourless.
S4, rectifying：To carrying out heating rectifying by the solution after charcoal absorption, caused gas passes through rectifying column, built
Vertical infinite reflux, 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 glacial acetic acid, and it uses the preparation method system of above-mentioned chromatographically pure glacial acetic acid
.
Shown in Figure 1, the embodiment of the present invention provides a kind of production system 100 of chromatographically pure glacial acetic acid, and it includes：For
The reactor 002 for the container that potassium permanganate is reacted is reacted, added as addition aceticanhydride；For carrying out charcoal absorption
Activated-charcoal column 005；For carrying out the rectifying column 006 of rectifying；And for collecting the finished pot 009 of finished product；For carry out from
The cation exchange column 011 that son exchanges；And the filter 012 for being filtered, wherein, reactor 002 and activated-charcoal column
005 connection, reactor 002, rectifying column 006, finished pot 009, cation exchange column 011 and filter 012 are sequentially connected with.
Wherein, what is filled in activated-charcoal column 005 is activating and regenerating type activated carbon；The height of rectifying column 006007 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 011；Filter 012
For 200nm filters, its model FLHF20010M3F300+IDO10-PFA-3/4 300, the material of filter 012 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 010, feedstock transportation pump
001 is connected with reactor 002, for raw material automatic transport to be entered in reactor 002；Finished product delivery pump 010 is installed on finished pot
Between 009 and cation exchange column 011, for by the finished product automatic transport in finished pot 009 to cation exchange column 011.
In the present embodiment, production system 100 also includes the circulating pump being installed between reactor 002 and activated-charcoal column 005
003, the circulation for carrying out circular response is formed between the top of the bottom of reactor 002, circulating pump 003 and reactor 002
Pipeline, the circulation line for carrying out circular treatment is formed between reactor 002, circulating pump 003 and activated-charcoal column 005.
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 007008, the return tank for being installed on the top of rectifying column 006
008, the circulation line for carrying out infinite reflux is formed between rectifying column 006, condenser 007 and return tank 008, fully to enter
Row 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 glacial acetic acid, and it is to use the production system 100 shown in Fig. 1, and according to following
Preparation method be made：
(1) using the glacial acetic acid of technical grade as raw material, reactor 002 is transported to by feedstock transportation pump 001, closes raw material
Delivery pump 001, start reactor 002 and stir, open the circulation pump 003, establish formed the bottom of reactor 002, circulating pump 003,
Circulation line between the top of blender 004 and reactor 002, in the glacial acetic acid into reactor 002 plus aceticanhydride, keep following
Ring 1.5 hours.
(2) potassium permanganate is added in the solution into reactor 002 (adding the reacted solution of aceticanhydride), continued cycling through
Reaction, untill solution no longer changes colour.
(3) circulation line that is formed between reactor 002, circulating pump 003, activated-charcoal column 005 is established, in reactor 002
Solution (add potassium permanganate reacted solution) cycle through activated-charcoal column 005 and carry out circular treatment, control solution exists
Flow velocity in activated-charcoal column 005 is 1m/s, untill the solution in reactor 002 is colourless.
(4) rectifying, caused gas warp are heated to the solution (i.e. by the solution after charcoal absorption) in reactor 002
Rectifying column 006 is crossed, and infinite reflux is established between rectifying column 006, condenser 007 and return tank 008, 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 009.
(5) start finished product delivery pump 010, the solution (finished product i.e. obtained by rectifying) in finished pot 009 is passed through into cation
Exchange column 011 carries out ion exchange.
(6) solution obtained by ion exchange is filtered by filter 012, packing bottling, that is, obtains chromatographically pure ice
Acetic acid, yield reach more than 95%.
Embodiment 2
The present embodiment provides a kind of chromatographically pure glacial acetic acid, and it is to use the production system 100 shown in Fig. 1, and according to following
Preparation method be made：
(1) using the glacial acetic acid of technical grade as raw material, reactor 002 is transported to by feedstock transportation pump 001, closes raw material
Delivery pump 001, start reactor 002 and stir, open the circulation pump 003, establish formed the bottom of reactor 002, circulating pump 003,
Circulation line between the top of blender 004 and reactor 002, in the glacial acetic acid into reactor 002 plus aceticanhydride, keep following
Ring 1 hour.
(2) potassium permanganate is added in the solution into reactor 002 (adding the reacted solution of aceticanhydride), continued cycling through
Reaction, untill solution no longer changes colour.
(3) circulation line that is formed between reactor 002, circulating pump 003, activated-charcoal column 005 is established, in reactor 002
Solution (add potassium permanganate reacted solution) cycle through activated-charcoal column 005 and carry out circular treatment, control solution exists
Flow velocity in activated-charcoal column 005 is 0.2m/s, untill the solution in reactor 002 is colourless.
(4) rectifying, caused gas warp are heated to the solution (i.e. by the solution after charcoal absorption) in reactor 002
Rectifying column 006 is crossed, and infinite reflux is established between rectifying column 006, condenser 007 and return tank 008, 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 009.
(5) start finished product delivery pump 010, the solution (finished product i.e. obtained by rectifying) in finished pot 009 is passed through into cation
Exchange column 011 carries out ion exchange.
(6) solution obtained by ion exchange is filtered by filter 012, packing bottling, that is, obtains chromatographically pure ice
Acetic acid, yield reach more than 95%.
Embodiment 3
The present embodiment provides a kind of chromatographically pure glacial acetic acid, and it is to use the production system 100 shown in Fig. 1, and according to following
Preparation method be made：
(1) using the glacial acetic acid of technical grade as raw material, reactor 002 is transported to by feedstock transportation pump 001, closes raw material
Delivery pump 001, start reactor 002 and stir, open the circulation pump 003, establish formed the bottom of reactor 002, circulating pump 003,
Circulation line between the top of blender 004 and reactor 002, in the glacial acetic acid into reactor 002 plus aceticanhydride, keep following
Ring 2 hours.
(2) potassium permanganate is added in the solution into reactor 002 (adding the reacted solution of aceticanhydride), continued cycling through
Reaction, untill solution no longer changes colour.
(3) circulation line that is formed between reactor 002, circulating pump 003, activated-charcoal column 005 is established, in reactor 002
Solution (add potassium permanganate reacted solution) cycle through activated-charcoal column 005 and carry out circular treatment, control solution exists
Flow velocity in activated-charcoal column 005 is 2m/s, untill the solution in reactor 002 is colourless.
(4) rectifying, caused gas warp are heated to the solution (i.e. by the solution after charcoal absorption) in reactor 002
Rectifying column 006 is crossed, and infinite reflux is established between rectifying column 006, condenser 007 and return tank 008, 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 009.
(5) start finished product delivery pump 010, the solution (finished product i.e. obtained by rectifying) in finished pot 009 is passed through into cation
Exchange column 011 carries out ion exchange.
(6) solution obtained by ion exchange is filtered by filter 012, packing bottling, that is, obtains chromatographically pure ice
Acetic acid, yield reach more than 95%.
The chromatographically pure glacial acetic acid in the embodiment of the present invention is detected below in conjunction with experiment.
The indices requirement of the chromatographically pure glacial acetic acid of table 1
First, ultraviolet absorptivity detection is carried out to the chromatographically pure glacial acetic acid in embodiment 1~3, it is as a result as follows：
The ultraviolet absorptivity testing result of the chromatographically pure glacial acetic acid of table 2
| Wavelength | 255nm | 260nm | 270nm | 280nm | 350nm |
| Raw material | 0.5 | 0.3 | 0.18 | 0.12 | 0.075 |
| Embodiment 1 | 0.26 | 0.05 | 0.025 | 0.008 | 0.005 |
| Embodiment 2 | 0.25 | 0.047 | 0.025 | 0.007 | 0.004 |
| Embodiment 3 | 0.25 | 0.046 | 0.023 | 0.007 | 0.004 |
| Chromatographically pure standard | ≤1 | ≤0.07 | ≤0.06 | ≤0.05 | ≤0.02 |
| Agriculture residual standard | ≤1 | ≤0.07 | ≤0.06 | ≤0.05 | ≤0.02 |
2nd, the chromatographically pure glacial acetic acid 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 glacial acetic acid of table 3
It can be seen that by above-mentioned testing result：The property indices of the chromatographically pure glacial acetic acid of the embodiment of the present invention are substantially excellent
In chromatographically pure glacial acetic acid standard.
In summary, the production cost of the preparation method of the chromatographically pure glacial acetic acid of the embodiment of the present invention is low, obtained chromatogram
Pure glacial acetic acid quality better, yield are high, meet chromatographically pure reagent requirement；The production system of the chromatographically pure glacial acetic acid of the embodiment of the present invention
Dedicated for preparing chromatographically pure glacial acetic acid, the scale industrial production of chromatographically pure glacial acetic acid 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 glacial acetic acid, it is characterised in that it comprises the following steps：
Using the glacial acetic acid of technical grade as raw material, it is firstly added aceticanhydride and is reacted, secondly adds potassium permanganate and reacted, it
Adsorbed afterwards by activated carbon, then carry out rectifying.
2. the preparation method of chromatographically pure glacial acetic acid according to claim 1, it is characterised in that add what aceticanhydride was reacted
Specific method is：Aceticanhydride, circular response 1~2 hour are added in glacial acetic acid.
3. the preparation method of chromatographically pure glacial acetic acid according to claim 1, it is characterised in that add potassium permanganate and carry out instead
The specific method answered is：Potassium permanganate, circular response are added in the reacted solution of aceticanhydride is added, until solution no longer becomes
Color.
4. the preparation method of chromatographically pure glacial acetic acid according to claim 1, it is characterised in that adsorbed by activated carbon
Specific method be：The circulation of potassium permanganate reacted solution will be added it is passed through in activated-charcoal column and carry out circular treatment, control is molten
Flow velocity of the liquid in activated-charcoal column is 0.1~2m/s, untill solution is colourless.
5. the preparation method of chromatographically pure glacial acetic acid according to claim 1, it is characterised in that the specific method of rectifying is：
To carrying out heating rectifying by the solution after charcoal absorption, caused gas passes through rectifying column, establishes infinite reflux, infinite reflux 1
~3 hours, start to produce, the certified products of extraction are finished product.
6. the preparation method of chromatographically pure glacial acetic acid 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.
7. a kind of chromatographically pure glacial acetic acid, it is characterised in that it uses the chromatographically pure ice as any one of claim 1 to 6
The preparation method of acetic acid is made.
8. a kind of production system of chromatographically pure glacial acetic acid, it is characterised in that it includes：
Reactor, the container reacted for potassium permanganate to be reacted, added as addition aceticanhydride；
Activated-charcoal column, for carrying out charcoal absorption；
Rectifying column, for carrying out rectifying；And
Finished pot, for collecting finished product,
Wherein, the reactor is connected with the activated-charcoal column, and the reactor, the rectifying column and the finished pot sequentially connect
Connect.
9. the production system of chromatographically pure glacial acetic acid 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 bottom of the reactor, the circulating pump and described
The circulation line for carrying out circular response, the reactor, the circulating pump and the work are formed between the top of reactor
The circulation line for carrying out circular treatment is formed between property charcoal post.
10. the production system of chromatographically pure glacial acetic acid according to claim 9, it is characterised in that the bottom of the reactor,
Blender is provided with the circulation line formed between the top of the circulating pump and the reactor.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1562938A (en) * | 2003-12-16 | 2005-01-12 | 上海吴泾化工有限公司 | Method for preparing hyperpure acetic acid and equipment |
| CN102746136A (en) * | 2012-07-20 | 2012-10-24 | 太仓沪试试剂有限公司 | Purification method for glacial acetic acid |
| CN103265424A (en) * | 2013-05-16 | 2013-08-28 | 吴江创新印染厂 | Cationic glacial acetic acid and purification method thereof |
-
2017
- 2017-08-29 CN CN201710756989.2A patent/CN107382711A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1562938A (en) * | 2003-12-16 | 2005-01-12 | 上海吴泾化工有限公司 | Method for preparing hyperpure acetic acid and equipment |
| CN102746136A (en) * | 2012-07-20 | 2012-10-24 | 太仓沪试试剂有限公司 | Purification method for glacial acetic acid |
| CN103265424A (en) * | 2013-05-16 | 2013-08-28 | 吴江创新印染厂 | Cationic glacial acetic acid and purification method thereof |
Non-Patent Citations (1)
| Title |
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| 威尔弗雷德 L.F.阿玛瑞高，林英杰等: "有机化学品的纯化", 《实验室化学品纯化手册》 * |
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