CN103772234B - acetonitrile refining process - Google Patents
acetonitrile refining process Download PDFInfo
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- CN103772234B CN103772234B CN201310728261.0A CN201310728261A CN103772234B CN 103772234 B CN103772234 B CN 103772234B CN 201310728261 A CN201310728261 A CN 201310728261A CN 103772234 B CN103772234 B CN 103772234B
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Abstract
The present invention relates to acetonitrile refining process.Comprise the steps: step 1: processed is carried out to acetonitrile raw material (5); Step 2: sent in distillation tower (2) by the acetonitrile raw material (5) after processed and carry out fractionation, the gas phase acetonitrile product (8) after fractionation is discharged by the tower top of distillation tower (2).Object of the present invention is for being SILVER REAGENT acetonitrile product by pharmaceutical grade acetonitrile product manufacturing.Particularly, acetonitrile raw material sends into distillation tower after processed, in a distillation column, gradually become liquid phase in the process that the gas phase that the vaporization of tower reactor bottoms material is formed moves upward in a distillation column and flow back to distillation tower tower reactor, thus, the weight percent concentration of the acetonitrile in the gas phase acetonitrile product of being discharged by tower top is greater than the weight percent concentration of the acetonitrile in acetonitrile raw material, thus achieves refining acetonitrile.
Description
Technical field
The present invention relates to acetonitrile refining process.
Background technology
At present, in acetonitrile device, in acetonitrile product, the concentration of acetonitrile is generally 99.9%, and water content and propionitrile component are about about 500ppm, and this kind of acetonitrile product is pharmaceutical grade.But in market, SILVER REAGENT acetonitrile product (weight percent concentration of acetonitrile is 99.999%) breach is comparatively large, and the manufacturer of grade product is few.Wherein, the concentration of acetonitrile is the ratio that the weight of acetonitrile in acetonitrile product accounts for the weight of acetonitrile product.
Summary of the invention
For Problems existing in correlation technique, the object of the present invention is to provide a kind of is the acetonitrile refining process of SILVER REAGENT acetonitrile product by pharmaceutical grade acetonitrile product manufacturing.
For achieving the above object, a kind of acetonitrile refining process is provided, comprises the steps: step 1: processed is carried out to acetonitrile raw material; Step 2: sent in distillation tower by the acetonitrile raw material after processed and carry out fractionation, the gas phase acetonitrile product after fractionation is discharged by the tower top of distillation tower.
According to the present invention, in step 2, a part for the acetonitrile raw material after processed is distilled the reboiler heating of tower, to provide the heat supplied generated needed for gas phase acetonitrile product.
According to the present invention, the weight percent concentration of the acetonitrile in acetonitrile raw material is 99.9%.
According to the present invention, step 1 is embodied as: dewatering agent and acetonitrile raw material are sent into by the top of water trap; Acetonitrile raw material after processed is pumped in distillation tower by the bottom of water trap; Wherein, the water in dewatering agent and acetonitrile raw material, maintenance effect 5-10 hour in the process being moved to bottom by top.
According to the present invention, according to the temperature of overhead or the heat supplied of pressure controlling reboiler.
According to the present invention, be that tower top working pressure runs distillation tower with setting pressure; When the pressure of tower top is higher than setting pressure, reboiler reduces heat supplied; When the pressure of tower top is lower than setting pressure, reboiler improves heat supplied.
According to the present invention, by the pressure of manometry tower top; When the pressure of tower top is higher than setting pressure, pressure warning unit sends the first signal, and reboiler reduces heat supplied in response to the first signal; When the pressure of tower top is lower than setting pressure, pressure warning unit sends second signal, and reboiler improves heat supplied in response to second signal.
According to the present invention, setting pressure is positioned at the scope of-0.1 ~ 1.0MpaG.
According to the present invention, be that tower top service temperature runs distillation tower with design temperature; When the temperature of tower top is higher than design temperature, reboiler reduces heat supplied; When the temperature of tower top is lower than design temperature, reboiler improves heat supplied.
According to the present invention, by the temperature of thermometer measure tower top; When the temperature of tower top is higher than design temperature, thermometer sends the 3rd signal, and reboiler reduces heat supplied in response to the 3rd signal; When the temperature of tower top is lower than design temperature, thermometer sends the 4th signal, and reboiler improves heat supplied in response to the 4th signal.
According to the present invention, design temperature is positioned at the scope of 30 ~ 200 DEG C.
According to the present invention, also comprise the steps: being discharged the product section after fractionating out gas phase acetonitrile product in distillation tower tower reactor by tower reactor; When the liquid level in distillation tower is higher than setting level value, increase the flow of the product of being discharged by tower reactor; When the liquid level in distillation tower is lower than setting level value, reduce the flow of the product of being discharged by tower reactor.
According to the present invention, measure the liquid level in distillation tower by liquid level alarm; When the liquid level in distillation tower is higher than setting level value, liquid level alarm sends the 5th signal, and discharging pump, in response to the 5th signal, increases the flow of the product of being discharged by tower reactor; When the liquid level in distillation tower is lower than setting level value, liquid level alarm sends the 6th signal, and discharging pump, in response to the 6th signal, reduces the flow of the product of being discharged by tower reactor.
According to the present invention, setting level value is positioned at the scope of 1.0 ~ 5.0m.
Compared to prior art, beneficial effect of the present invention is:
1. acetonitrile raw material sends into distillation tower after processed, in a distillation column, gradually become liquid phase in the process that the gas phase that the vaporization of tower reactor bottoms material is formed moves upward in a distillation column and flow back to distillation tower tower reactor, thus, the weight percent concentration of the acetonitrile in the gas phase acetonitrile product of being discharged by tower top is greater than the weight percent concentration of the acetonitrile in acetonitrile raw material, thus achieves refining acetonitrile.
2. according to the pressure of tower top or the heat supplied of temperature control reboiler, and the liquid level of foundation distillation tower regulates the flow of tower reactor discharge opeing, effectively can ensure the effect of refining further, and keeps stable the carrying out of acetonitrile refining process.
3. send by the pressure of manometry tower top the signal controlling reboiler heat supplied according to measuring result, or send by the temperature of thermometer measure tower top the signal controlling reboiler heat supplied according to measuring result, and measure the liquid level in distillation tower by liquid level alarm and send the flow of the product controlling to discharge according to measuring result.Automatically can control the realization of acetonitrile refining process, accurately, effectively complete the refining of acetonitrile further, keep the carrying out that treating process is stable, thus ensure that the acetonitrile product after refining is SILVER REAGENT.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the system of the embodiment performing acetonitrile refining method of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the invention is described.
With reference to Fig. 1, an embodiment of acetonitrile refining method of the present invention, comprises the steps.
Perform step 1: processed is carried out to acetonitrile raw material 5.Wherein, acetonitrile raw material 5 is pharmaceutical grade acetonitrile product, and namely the weight percent concentration of acetonitrile is wherein 99.9%, and in other words, the weight of acetonitrile equals 99.9% divided by the weight of acetonitrile product.In the present embodiment, water trap 1 pair of acetonitrile raw material 5 is used to carry out processed, particularly, dewatering agent 10 and acetonitrile raw material 5 are sent into by the top of water trap 1, acetonitrile raw material 5 after processed is pumped in distillation tower 2 by the bottom of water trap 1, water in dewatering agent 10 and acetonitrile raw material 5, maintenance effect 5-10 hour in the process being moved to bottom by top.Above-mentioned water trap 1 is equipment well known by persons skilled in the art, namely, as long as water trap 1 can realize holding dewatering agent 10 and acetonitrile raw material 5 and can ensureing the water continuous action 5-10 hour in dewatering agent 10 and acetonitrile raw material 5, be also not limited to from its top feeding dewatering agent and acetonitrile raw material and by bottom, the acetonitrile raw material 5 after processed discharged.And dewatering agent 10 is known to the skilled person can be combined and form heavier binding substances to realize the dewatering agent of dehydrating effect by the water in acetonitrile raw material.Certainly, in other alternatively embodiment, other dehydration treatment method also can be used to remove water in acetonitrile raw material.
Perform step 2: sent in distillation tower 2 by the acetonitrile raw material 5 after processed and carry out fractionation, the gas phase acetonitrile product 8 after fractionation is discharged by the tower top of distillation tower 2.Wherein, gas phase acetonitrile product 8 comprises the impurity such as gas phase acetonitrile and such as water vapour, and by the gas phase acetonitrile product 8 after the fractionation of processed and distillation tower 2, the weight percent concentration of acetonitrile wherein, higher than the weight percent concentration of the acetonitrile in acetonitrile raw material, can reach 99.999%.
Particularly, in the present embodiment, pumped in distillation tower 2 by acetonitrile raw material after processed in step 1, can understand together with above-mentioned binding substances, when containing the dewatering agent be not combined with water, this partial dehydration agent also together pumps in distillation tower 2.Certainly, in an alternate embodiment of the invention, the step removing binding substances can be had, namely be removed before binding substances enters distillation tower 2, only acetonitrile raw material after processed be sent into fractionation in distillation tower 2.
In the present embodiment, the reboiler 4 that the part of the acetonitrile raw material after processed is distilled tower 2 heats, to provide the heat supplied generated needed for gas phase acetonitrile product 8.Particularly, acetonitrile raw material after processed enters distillation tower 2 and flows into tower reactor, in the process to tower reactor movement meeting and with its countercurrent flow, the gas-phase product heat exchange that flowed into distillation tower 2 by reboiler 4, a part of liquid phase acetonitrile wherein can be vaporized and be formed gas phase acetonitrile and move to tower top, and remainder falls into tower reactor.Can understand, in tower reactor, include the heavier binding substances that liquid phase acetonitrile, water, liquid phase propionitrile and the dewatering agent 10 of not vaporizing are formed with water.Above-mentioned binding substances is positioned at lower floor owing to overweighting liquid phase acetonitrile, water and liquid phase propionitrile, and liquid phase acetonitrile, water and liquid phase propionitrile are positioned at upper strata.The tower reactor sidewall of distillation tower 2 is communicated with by reboiler inlet line 13 with the bottom of reboiler 4, reboiler 4 top is communicated with by reboiler outlet line 12 with distillation tower 2, be positioned at the liquid phase acetonitrile on upper strata, water and liquid phase propionitrile flow in reboiler 4 through reboiler inlet line 13, after being heated in reboiler 4, form gas-liquid two-phase product and send distillation tower 2 back to through reboiler outlet line 12, can understand, the gas-phase product formed in reboiler 4 contains gas phase acetonitrile, water vapour and gas phase propionitrile etc., and liquid product is the liquid phase acetonitrile of not vaporizing, water and liquid phase propionitrile etc.After above-mentioned gas-phase product and liquid product enter distillation tower 2, gas-phase product moves to tower top, liquid product flows back to tower reactor, due to tower top temperature lower than tower reactor temperature and lower than the boiling point of water and propionitrile, gas-phase product is in the process risen, the water vapour of part and gas phase propionitrile condense into liquid phase and flow back to tower reactor, and in the process that gas-phase product rises, with the acetonitrile raw material heat exchange after the processed constantly pumped in distillation tower 2, gas-phase product heat release, part water vapour wherein and gas phase propionitrile condense into liquid phase and flow back to tower reactor, and the acetonitrile raw material heat absorption after processed, the vaporization of Partial Liquid Phase acetonitrile forms gas phase acetonitrile and rises.Thus, gas phase acetonitrile product 8 is fractionated out.Can understand, the reboiler 4 that the part that said process achieves the acetonitrile raw material after by processed is distilled tower 2 heats, and namely absorbs heat, and this heat provides and generates heat supplied needed for gas phase acetonitrile product 8 by liquid phase acetonitrile, water and liquid phase propionitrile.Gas phase acetonitrile product is now the acetonitrile product that the weight percent concentration of gas phase acetonitrile equals 99.999%, and the weight of the acetonitrile namely wherein contained equals 99.999% divided by the weight of acetonitrile product.This acetonitrile product reaches SILVER REAGENT.Can understand through said process, gas phase acetonitrile in the gas phase acetonitrile product 8 fractionated out by distillation tower 2 is made up of two portions, a part is the gas phase acetonitrile added through reboiler 4 in the gas-phase product of thermosetting, another part be in above-mentioned gas-phase product uphill process with the processed of its inverse motion after acetonitrile raw material to absorb heat the gas phase acetonitrile formed.
In the present embodiment, tower reactor diapire is communicated with the entrance of discharging pump 3 through going out tower waste liquid pipeline 9, and the outlet of discharging pump 3 is connected with pump discharge pipeline 17.Distillation tower 2 is pumped with fractionating out the product section after gas phase acetonitrile product 8 in tower reactor by discharging pump 3.Can understand, the product fractionated out after gas phase acetonitrile product 8 comprises the impurity such as above-mentioned binding substances, water, propionitrile, certainly also comprises the liquid phase acetonitrile of not vaporizing of part.Above-mentioned binding substances is greater than all the other materials due to weight, it enters the lower floor that distillation tower 2 post-concentration combines in tower reactor, discharge by going out tower waste liquid pipeline 9 faster, reboiler 4 is entered to avoid the reboiler inlet line 13 by being connected to tower reactor sidewall, in other words, on the one hand, ensure that reboiler inlet line 13 deposits with the link position of tower reactor sidewall the extreme higher position being positioned at tower reactor higher than binding substances, binding substances is constantly discharged by tower reactor on the other hand.If a small amount of binding substances enters in reboiler 4, because dewatering agent has cohesion to water, so the more difficult vaporization of water in binding substances forms water vapour.
Thus, in the present embodiment, acetonitrile raw material sends into distillation tower after processed, in a distillation column, gradually become liquid phase in the process that the gas phase that the vaporization of tower reactor bottoms material is formed moves upward in a distillation column and flow back to distillation tower tower reactor, thus the weight percent concentration of acetonitrile in the gas phase acetonitrile product 8 of being discharged by tower top is greater than the weight percent concentration of the acetonitrile in acetonitrile raw material, thus it is refining to achieve acetonitrile.
In addition, can according to the heat supplied of the temperature of tower top or pressure controlling reboiler 4, and the temperature and pressure of tower top has linear relationship, namely the pressure of tower top raises and illustrates that the temperature of tower top raises, and the pressure of tower top reduces and illustrates that the temperature of tower top reduces.Wherein, the pressure of tower top is the pressure of gas phase acetonitrile product 8 in tower top, and the temperature of tower top is the temperature of gas phase acetonitrile product 8 in tower top.
In the present embodiment, the step of the heat supplied of the pressure controlling reboiler 4 according to distillation tower 2 tower top is comprised.Particularly, be that tower top working pressure runs distillation tower 2 with setting pressure, the pressure of tower top is measured by pressure warning unit 16, when the pressure of tower top is lower than setting pressure, illustrate that the amount of the gas phase acetonitrile product 8 that distillation tower 2 fractionates out reduces, pressure warning unit 16 sends second signal, reboiler 4 improves heat supplied in response to second signal, thus, the amount of the gas-phase product formed in reboiler 1 increases, to improve the amount of the gas phase acetonitrile product 8 of being discharged by tower top and to improve the weight percent concentration of the acetonitrile in gas phase acetonitrile product 8.When the pressure of tower top is higher than setting pressure, illustrate that the temperature of tower top is too high, make part water vapour or gas phase propionitrile cannot be liquefied as liquid phase further and flow back to tower reactor, so containing too much water vapour or gas phase propionitrile in the gas phase acetonitrile product 8 of discharging, this situation can reduce acetonitrile in gas phase acetonitrile product 8 concentration.Now pressure warning unit 16 sends the first signal, and reboiler 4 reduces heat supplied in response to the first signal, thus reduce the amount forming gas-phase product in reboiler 4, thus adjusting tower pressure on top surface reduces and reduces the temperature of tower top.When the pressure of tower top equals setting pressure, pressure warning unit 16 does not send signal, and reboiler 4, when not receiving the signal that pressure warning unit 16 sends, keeps heat supplied constant.Wherein, in the present embodiment, setting pressure is positioned at the scope of-0.1 ~ 1.0MpaG, namely in application process, can select the numerical value of setting pressure in the scope of-0.1 ~ 1.0MpaG.
In the present embodiment, reboiler 4 is connected with vapour line 6 and lime set pipeline 7, and steam enters the acetonitrile raw material heat exchange after reboiler 4 and processed wherein by vapour line 6, and the vapor condenses Cheng Shui after heat release is discharged by lime set pipeline 7.
Be that tower top service temperature runs distillation tower 2 with design temperature, the temperature of tower top is measured by thermometer 15, when the temperature of tower top is lower than design temperature, occur that gas phase acetonitrile condenses into the phenomenon that liquid phase flows back to tower reactor at tower top, the output of gas phase acetonitrile product 8 reduces and affects the content of acetonitrile wherein, this chronothermometer 15 sends the 4th signal, reboiler 4 improves heat supplied in response to the 4th signal, to make the acetonitrile raw material after the dehydration of reboiler 4 absorb more heat to be vaporized with more gas-phase product, wherein comprise gas phase acetonitrile.Thus, the heat exchange in the process risen of more gas-phase product increases, and which thereby enhances the temperature of tower top, prevents gas phase acetonitrile to liquefy, ensure that the output of discharging gas phase acetonitrile.When the temperature of tower top is higher than design temperature, part water vapour and gas phase propionitrile can keep gas phase to discharge with gas phase acetonitrile, the concentration of the gas phase acetonitrile of being discharged by tower top can be reduced, this chronothermometer 15 sends the 3rd signal, reboiler 4 reduces heat supplied in response to the 3rd signal, now, thus reduces the evaporating capacity of the acetonitrile raw material after the processed in reboiler 4, reduce the temperature of the gas-liquid two-phase entering distillation tower, and then reduce the temperature of tower top.When tower top temperature equals design temperature, thermometer 15 does not send signal, and the heat supplied of reboiler remains unchanged.Wherein, in the present embodiment, design temperature is positioned at the scope of 30 ~ 200 DEG C, namely in actual applications, can select the numerical value of design temperature in the scope of 30 ~ 200 DEG C.
In the present embodiment, also comprise the steps: the liquid level measured by liquid level alarm 14 in distillation tower 2, when the liquid level in distillation tower 2 is higher than setting level value, illustrate contain in tower reactor to fractionate out the product after gas phase acetonitrile too much, the liquid phase ethane nitrile content entered in reboiler 4 is caused to reduce thus, affect the vaporization of liquid phase acetonitrile, now liquid level alarm 14 sends the 5th signal, discharging pump 3 is in response to the 5th signal, increase the flow of the product of being discharged by tower reactor, when the liquid level in distillation tower 2 is lower than setting level value, liquid level alarm 14 sends the 6th signal, discharging pump 3 is in response to the 6th signal, reduce the flow of the product of being discharged by tower reactor.When the liquid level in distillation tower 2 equals setting level value, liquid level alarm 14 does not send signal, and the flow of the product of being discharged by tower reactor remains unchanged.Certainly, also above-mentioned discharging pump 3 can be replaced with valve, also can realize the above-mentioned control for flow.Wherein, in the present embodiment, setting level value is positioned at the scope of 1.0 ~ 5.0m, namely in actual application, can select to set level value in the scope of 1.0 ~ 5.0m.
According to the pressure of tower top or the heat supplied of temperature control reboiler, and the liquid level of foundation distillation tower regulates the flow of tower reactor discharge opeing, effectively can ensure the effect of refining further, and keeps stable the carrying out of acetonitrile refining process.
The signal controlling reboiler heat supplied is sent according to measuring result by the pressure of manometry tower top, or send by the temperature of thermometer measure tower top the signal controlling reboiler heat supplied according to measuring result, and measure the liquid level in distillation tower by liquid level alarm and send the flow of the product controlling to discharge according to measuring result.Automatically can control the realization of acetonitrile refining process, accurately, effectively complete the refining of acetonitrile further, keep the carrying out that treating process is stable, thus ensure that the acetonitrile product after refining is SILVER REAGENT.
These are only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (7)
1. an acetonitrile refining process, is characterized in that, comprises the steps:
Step 1: processed is carried out to acetonitrile raw material;
Step 2: sent in distillation tower by the acetonitrile raw material after processed and carry out fractionation, the gas phase acetonitrile product after fractionation is discharged by the tower top of described distillation tower;
Wherein, the weight percent concentration of the acetonitrile in described acetonitrile raw material is 99.9%;
Described step 1 is embodied as: dewatering agent and described acetonitrile raw material are sent into by the top of water trap; Acetonitrile raw material after processed is pumped in described distillation tower by the bottom of described water trap; Wherein, the water in described dewatering agent and described acetonitrile raw material, maintenance effect 5-10 hour in the process being moved to described bottom by described top;
In described step 2, a part for the acetonitrile raw material after described processed is heated by the reboiler of described distillation tower, to provide the heat supplied generated needed for described gas phase acetonitrile product;
The heat supplied of reboiler according to the temperature of described overhead or pressure controlling;
Be that tower top working pressure runs described distillation tower with setting pressure, described setting pressure is positioned at the scope of-0.1 ~ 1.0MpaG;
Be that tower top service temperature runs described distillation tower with design temperature, described design temperature is positioned at the scope of 30 ~ 200 DEG C;
Measure the liquid level in described distillation tower by liquid level alarm, described setting level value is positioned at the scope of 1.0 ~ 5.0m.
2. acetonitrile refining process according to claim 1, is characterized in that,
When the pressure of described tower top is higher than described setting pressure, described reboiler reduces heat supplied;
When the pressure of described tower top is lower than described setting pressure, described reboiler improves heat supplied.
3. acetonitrile refining process according to claim 2, is characterized in that,
By the pressure of tower top described in manometry;
When the pressure of described tower top is higher than described setting pressure, described pressure warning unit sends the first signal, and described reboiler reduces heat supplied in response to described first signal;
When the pressure of described tower top is lower than described setting pressure, described pressure warning unit sends second signal, and described reboiler improves heat supplied in response to described second signal.
4. acetonitrile refining process according to claim 1, is characterized in that,
When the temperature of described tower top is higher than described design temperature, described reboiler reduces heat supplied;
When the temperature of described tower top is lower than described design temperature, described reboiler improves heat supplied.
5. acetonitrile refining process according to claim 4, is characterized in that,
By the temperature of tower top described in thermometer measure;
When the temperature of described tower top is higher than described design temperature, described thermometer sends the 3rd signal, and described reboiler reduces heat supplied in response to described 3rd signal;
When the temperature of described tower top is lower than described design temperature, described thermometer sends the 4th signal, and described reboiler improves heat supplied in response to described 4th signal.
6. acetonitrile refining process according to claim 1, is characterized in that, also comprises the steps:
By being discharged by tower reactor of the product section after fractionating out described gas phase acetonitrile product in described distillation tower tower reactor;
When the liquid level in described distillation tower is higher than setting level value, increase the flow of the product of being discharged by tower reactor;
When the liquid level in described distillation tower is lower than setting level value, reduce the flow of the product of being discharged by tower reactor.
7. acetonitrile refining process according to claim 6, is characterized in that,
When the liquid level in described distillation tower is higher than setting level value, described liquid level alarm sends the 5th signal, and discharging pump, in response to the 5th signal, increases the flow of the product of being discharged by tower reactor;
When the liquid level in described distillation tower is lower than setting level value, described liquid level alarm sends the 6th signal, and discharging pump, in response to the 6th signal, reduces the flow of the product of being discharged by tower reactor.
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| CN106890478A (en) * | 2015-12-21 | 2017-06-27 | 赵志峰 | High purity reagent acetonitrile removes formaldehyde, acetaldehyde adsorbent equipment |
| CN109704990B (en) * | 2017-10-26 | 2022-02-01 | 中国石油化工股份有限公司 | Refining method of high-purity acetonitrile |
| CN108543506B (en) * | 2018-03-13 | 2020-09-11 | 中国石油集团东北炼化工程有限公司吉林设计院 | Reactor for recovering acetonitrile as by-product in acrylonitrile production process |
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| CN101171233A (en) * | 2005-05-10 | 2008-04-30 | 旭化成化学株式会社 | High-purity acetonitrile and process for producing the same |
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| US8071816B2 (en) * | 2008-06-30 | 2011-12-06 | 3M Innovative Properties Company | Hydrofluoroacetal compounds and processes for their preparation and use |
| US20120073954A1 (en) * | 2010-09-28 | 2012-03-29 | Romas Cesas | Recovery of acetonitrile from a waste stream |
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| CN101171233A (en) * | 2005-05-10 | 2008-04-30 | 旭化成化学株式会社 | High-purity acetonitrile and process for producing the same |
| CN1736530A (en) * | 2005-07-26 | 2006-02-22 | 天津大学 | Method for separating acetonitrile-methylbenzene azeotropic mixture by continuous extractive distillation |
| CN102633679A (en) * | 2012-04-01 | 2012-08-15 | 中国天辰工程有限公司 | Continuous purification method for crude acetonitrile |
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Effective date of registration: 20190529 Address after: 132002 3-6 and 9-13 floors of Block A, Jihua Economic and Trade Center, Tongtan Road, Changyi District, Jilin Province Patentee after: PetroChina Jilin Chemical Engineering Co., Ltd. Address before: 132002 East End Economic and Trade Building of Tongtan Road, Jilin Province Patentee before: Jilin Design Institute of Northeast Refining & Chemical Engineering Co., Ltd., CNPC |