CN103772234A - Acetonitrile refining process - Google Patents
Acetonitrile refining process Download PDFInfo
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- CN103772234A CN103772234A CN201310728261.0A CN201310728261A CN103772234A CN 103772234 A CN103772234 A CN 103772234A CN 201310728261 A CN201310728261 A CN 201310728261A CN 103772234 A CN103772234 A CN 103772234A
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Abstract
The invention relates to an acetonitrile refining process. The process comprises the following steps: 1, dehydrating acetonitrile raw material (5); 2, carrying out fractional distillation on the dewatered acetonitrile raw material (5) in a distillation column (2) and discharging the distilled gas-phase acetonitrile product (8) from the top of the distillation column (2). The invention aims to prepare a medicine-grade acetonitrile product into a regent-grade acetonitrile product. Particularly, the acetonitrile raw material is dehydrated and then sent into the distillation column; in the distillation column, and when the gas phase formed by gasifying the material at the bottom of the distillation column moves up in the distillation column, the gas phase gradually changes into a liquid phase and flows back to the kettle of the distillation column; therefore, the concentration (wt%) of acetonitrile in the gas-phase acetonitrile product discharged out from the top of the column is higher than the concentration (wt%) of acetonitrile in the acetonitrile raw material and acetonitrile is refined finally.
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%, the about 500ppm of water content and propionitrile component left and right, and this kind of acetonitrile product is pharmaceutical grade.But breach is larger, and the manufacturer of SILVER REAGENT product is few for SILVER REAGENT acetonitrile product in market (weight percent concentration of acetonitrile is 99.999%).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 the problem existing in correlation technique, the object of the present invention is to provide a kind of acetonitrile refining process that pharmaceutical grade acetonitrile product is fabricated to SILVER REAGENT acetonitrile product.
For achieving the above object, provide a kind of acetonitrile refining process, comprise the steps: step 1: acetonitrile raw material is carried out to processed; Step 2: the acetonitrile raw material after processed is sent in distillation tower and carried out fractionation, and 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, generates the required heat supplied of gas phase acetonitrile product to provide.
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 that is moved to bottom by top.
According to the present invention, according to the heat supplied of the temperature of distillation tower tower top or pressure controlling reboiler.
According to the present invention, the operation distillation tower take setting pressure as tower top working pressure; When the pressure of tower top is during higher than setting pressure, reboiler reduces heat supplied; When the pressure of tower top is during 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 during higher than setting pressure, pressure warning unit sends first signal, and reboiler reduces heat supplied in response to first signal; When the pressure of tower top is during 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, the scope of be positioned at-0.1～1.0MpaG of setting pressure.
According to the present invention, the operation distillation tower take design temperature as tower top service temperature; When the temperature of tower top is during higher than design temperature, reboiler reduces heat supplied; When the temperature of tower top is during 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 during 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 during 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 ℃.
According to the present invention, also comprise the steps: in distillation tower tower reactor, to fractionate out being discharged by tower reactor of product part after gas phase acetonitrile product; When the liquid level in distillation tower is higher than setting when 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 when level value, the flow of the product that reduces to be 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 when 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 when level value, liquid level alarm sends the 6th signal, and discharging pump is in response to the 6th signal, the flow of the product that reduces to be discharged by tower reactor.
According to the present invention, setting level value is positioned at the scope of 1.0～5.0m.
Than prior art, beneficial effect of the present invention is:
1. acetonitrile raw material is sent into distillation tower after processed, in distillation tower, in the process that the gas phase that the material vaporization of tower reactor bottom forms moves upward in distillation tower, gradually become liquid phase 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, thereby has realized refining acetonitrile.
2. according to the heat supplied of pressure or the temperature control reboiler of tower top, and regulate the flow of tower reactor discharge opeing according to the liquid level of distillation tower, can further effectively guarantee refining effect, and keep stable the carrying out of acetonitrile refining process.
3. send the signal of controlling reboiler heat supplied by the pressure of manometry tower top and according to measuring result, or send the signal of controlling reboiler heat supplied by the temperature of thermometer measure tower top and according to measuring result, and measure the liquid level in distillation tower and send the flow of controlling the product of discharging according to measuring result by liquid level alarm.Can automatically control the realization of acetonitrile refining process, further accurately, effectively complete the refining of acetonitrile, keep stable the carrying out for the treatment of process, thereby the acetonitrile product after assurance is refined is SILVER REAGENT.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of carrying out the system of an embodiment of 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.
Execution step 1: acetonitrile raw material 5 is carried out to processed.Wherein, acetonitrile raw material 5 is pharmaceutical grade acetonitrile product, and 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, use water trap 1 to carry out processed to acetonitrile raw material 5, 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 that is moved to bottom by top.Above-mentioned water trap 1 is equipment well known by persons skilled in the art,, as long as water trap 1 can realize hold dewatering agent 10 and acetonitrile raw material 5 and can guarantee dewatering agent 10 and acetonitrile raw material 5 in water continuous action 5-10 hour, be also not limited to and send into dewatering agent and acetonitrile raw material from its top and by bottom, the acetonitrile raw material 5 processed discharged.Can the water in acetonitrile raw material be combined and form heavier binding substances to realize the dewatering agent of dehydrating effect and dewatering agent 10 is known to the skilled person.Certainly, alternatively in embodiment, also can use other dehydration treatment method to remove the water in acetonitrile raw material at other.
Execution step 2: the acetonitrile raw material 5 after processed is sent in distillation tower 2 and carried out fractionation, and 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, acetonitrile raw material after processed in step 1 is pumped in distillation tower 2 together with above-mentioned binding substances, can understand, in the time containing the dewatering agent of not being combined with water, this partial dehydration agent also together pumps in distillation tower 2.Certainly, in optional embodiment, can there is the step that removes binding substances, enter at binding substances that distillation tower 2 is front to be removed, only acetonitrile raw material after processed be sent into fractionation in distillation tower 2.
In the present embodiment, the reboiler 4 that a part for the acetonitrile raw material after processed is distilled tower 2 heats, and generates the required heat supplied of gas phase acetonitrile product 8 to provide.Particularly, acetonitrile raw material after processed enters distillation tower 2 and flows into tower reactor, in the process moving to tower reactor meeting and with gas-phase product heat exchange its countercurrent flow, 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 liquid phase acetonitrile, water, liquid phase propionitrile and the dewatering agent 10 of not vaporization and the heavier binding substances of water formation.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 tops are 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 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 forming 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.Above-mentioned gas-phase product and liquid product enter after distillation tower 2, gas-phase product moves to tower top, liquid product flows back to tower reactor, because the temperature of tower top is lower than the temperature of tower reactor and lower than the boiling point of water and propionitrile, gas-phase product is in the process rising, the water vapour of part and gas phase propionitrile condense into liquid phase and flow back to tower reactor, and in the process rising at gas-phase product, with the acetonitrile raw material heat exchange after the processed constantly pumping 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 heat absorption of acetonitrile raw material after processed, the vaporization of Partial Liquid Phase acetonitrile forms gas phase acetonitrile and rises.Thus, fractionate out gas phase acetonitrile product 8.Can understand, said process has been realized the reboiler 4 that a part for the acetonitrile raw material after processed is distilled to tower 2 and has been heated, and absorbs heat, and this heat provides by liquid phase acetonitrile, water and liquid phase propionitrile and generated the required heat supplied of gas phase acetonitrile product 8.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 wherein containing equals 99.999% divided by the weight of acetonitrile product.This acetonitrile product has reached SILVER REAGENT.Can understand through said process, gas phase acetonitrile in the gas phase acetonitrile product 8 being fractionated out by distillation tower 2 is made up of two portions, a part is to add the gas phase acetonitrile in the gas-phase product of thermosetting through reboiler 4, another part be in above-mentioned gas-phase product uphill process with the processed of its inverse motion after the gas phase acetonitrile that forms of acetonitrile raw material heat absorption.
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.The product fractionating out in tower reactor after gas phase acetonitrile product 8 partly pumps distillation tower 2 by discharging pump 3.Can understand, the product fractionating out after gas phase acetonitrile product 8 comprises the impurity such as above-mentioned binding substances, water, propionitrile, certainly also comprises the not liquid phase acetonitrile of vaporization of part.Above-mentioned binding substances is because weight is greater than all the other materials, it enters distillation tower 2 post-concentrations and combines in the lower floor of tower reactor, discharge by going out tower waste liquid pipeline 9 faster, to avoid entering reboiler 4 by the reboiler inlet line 13 that is connected in tower reactor sidewall, in other words, on the one hand, guarantee that reboiler inlet line 13 and the link position of tower reactor sidewall are positioned at the extreme higher position of tower reactor higher than binding substances deposition, 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 is sent into distillation tower after processed, in distillation tower, in the process that the gas phase that the material vaporization of tower reactor bottom forms moves upward in distillation tower, gradually become liquid phase and flow back to distillation tower tower reactor, thereby the weight percent concentration of the 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, thereby realize refining acetonitrile.
In addition, can be 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, the raise temperature of explanation tower top of the pressure of tower top raises, and the temperature of the pressure decreased explanation tower top 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, comprise according to the step of the heat supplied of the pressure controlling reboiler 4 of distillation tower 2 tower tops.Particularly, the operation distillation tower 2 take setting pressure as tower top working pressure, measure the pressure of tower top by pressure warning unit 16, when the pressure of tower top is during lower than setting pressure, the amount that the gas phase acetonitrile product 8 that distillation tower 2 fractionates out is described 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 forming 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 during higher than setting pressure, the excess Temperature of tower top is described, further make part water vapour or gas phase propionitrile cannot be liquefied as liquid phase and flow back to tower reactor, so in the gas phase acetonitrile product 8 of discharging, contain too much water vapour or gas phase propionitrile, this situation can reduce acetonitrile in gas phase acetonitrile product 8 concentration.Now pressure warning unit 16 sends first signal, and reboiler 4 reduces heat supplied in response to first signal, reduced thus the amount that forms gas-phase product in reboiler 4, thereby adjusting tower pressure on top surface reduces and reduce the temperature of tower top.In the time that the pressure of tower top equals setting pressure, pressure warning unit 16 does not send signal, and reboiler 4, in the time not receiving the signal that pressure warning unit 16 sends, keeps heat supplied constant.Wherein, in the present embodiment, the scope of be positioned at-0.1～1.0MpaG of setting pressure,, in application process, can select in the scope of-0.1～1.0MpaG the numerical value of setting pressure.
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.
The operation distillation tower 2 take design temperature as tower top service temperature, measure the temperature of tower top by thermometer 15, when the temperature of tower top is during lower than design temperature, occur that at tower top gas phase acetonitrile condenses into liquid phase and flow back to the phenomenon of tower reactor, 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, so that the acetonitrile raw material after the dehydration of reboiler 4 absorbs more heat to be vaporized with more gas-phase product, wherein comprise gas phase acetonitrile.Thus, the heat exchange in the process rising of more gas-phase product increases, and has improved thus the temperature of tower top, has prevented the liquefaction of gas phase acetonitrile, has guaranteed to discharge the output of gas phase acetonitrile.When the temperature of tower top is during higher than design temperature, part water vapour and gas phase propionitrile can keep gas phase to discharge with gas phase acetonitrile, can reduce the concentration of the gas phase acetonitrile of being discharged by tower top, this chronothermometer 15 sends the 3rd signal, reboiler 4 reduces heat supplied in response to the 3rd signal, now, has reduced thus the evaporating capacity of the acetonitrile raw material after the processed in reboiler 4, reduce the temperature of the gas-liquid two-phase that enters distillation tower, and then reduced the temperature of tower top.In the time that 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 ℃, in actual applications, can in the scope of 30～200 ℃, select the numerical value of design temperature.
In the present embodiment, also comprise the steps: to measure the liquid level in distillation tower 2 by liquid level alarm 14, when the liquid level in distillation tower 2 is higher than setting when level value, illustrate in tower reactor, contain to fractionate out product after gas phase acetonitrile too much, the liquid phase ethane nitrile content that causes thus entering in reboiler 4 reduces, 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 when level value, liquid level alarm 14 sends the 6th signal, discharging pump 3 is in response to the 6th signal, the flow of the product that reduces to be discharged by tower reactor.In the time that the liquid level in distillation tower 2 equals to set 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 to 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,, in actual application, can in the scope of 1.0～5.0m, select to set level value.
According to the heat supplied of pressure or the temperature control reboiler of tower top, and regulate the flow of tower reactor discharge opeing according to the liquid level of distillation tower, can further effectively guarantee refining effect, and keep stable the carrying out of acetonitrile refining process.
Send the signal of controlling reboiler heat supplied by the pressure of manometry tower top and according to measuring result, or send the signal of controlling reboiler heat supplied by the temperature of thermometer measure tower top and according to measuring result, and measure the liquid level in distillation tower and send the flow of controlling the product of discharging according to measuring result by liquid level alarm.Can automatically control the realization of acetonitrile refining process, further accurately, effectively complete the refining of acetonitrile, keep stable the carrying out for the treatment of process, thereby the acetonitrile product after assurance is refined 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 modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (14)
1. an acetonitrile refining process, is characterized in that, comprises the steps:
Step 1: acetonitrile raw material (5) is carried out to processed;
Step 2: the acetonitrile raw material (5) after processed is sent in distillation tower (2) and carried out fractionation, and the gas phase acetonitrile product (8) after fractionation is discharged by the tower top of described distillation tower (2).
2. acetonitrile refining process according to claim 1, is characterized in that,
In described step 2, a part for the acetonitrile raw material (5) after described processed, by the reboiler of described distillation tower (2) (4) heating, generates the required heat supplied of described gas phase acetonitrile product (8) to provide.
3. acetonitrile refining process according to claim 1, is characterized in that,
The weight percent concentration of the acetonitrile in described acetonitrile raw material (5) is 99.9%.
4. acetonitrile refining process according to claim 1, is characterized in that, described step 1 is embodied as:
Dewatering agent (10) and described acetonitrile raw material (5) are sent into by the top of water trap (1);
Acetonitrile raw material (5) after processed is pumped in described distillation tower (2) by the bottom of described water trap (1);
Wherein, the water in described dewatering agent (10) and described acetonitrile raw material (5), maintenance effect 5-10 hour in the process that is moved to described bottom by described top.
5. according to the acetonitrile refining process described in any one in claim 1 to 4, it is characterized in that,
According to the heat supplied of reboiler (4) described in the temperature of described distillation tower (2) tower top or pressure controlling.
6. acetonitrile refining process according to claim 5, is characterized in that,
Move described distillation tower (2) take setting pressure as tower top working pressure;
When the pressure of described tower top is during higher than described setting pressure, described reboiler (4) reduces heat supplied;
When the pressure of described tower top is during lower than described setting pressure, described reboiler (4) improves heat supplied.
7. acetonitrile refining process according to claim 6, is characterized in that,
Measure the pressure of described tower top by pressure warning unit (16);
When the pressure of described tower top is during higher than described setting pressure, described pressure warning unit (16) sends first signal, and described reboiler (4) reduces heat supplied in response to described first signal;
When the pressure of described tower top is during lower than described setting pressure, described pressure warning unit (16) sends second signal, and described reboiler (4) improves heat supplied in response to described second signal.
8. according to the acetonitrile refining process described in claim 6 or 7, it is characterized in that,
The scope of be positioned at-0.1～1.0MpaG of described setting pressure.
9. acetonitrile refining process according to claim 5, is characterized in that,
Move described distillation tower (2) take design temperature as tower top service temperature;
When the temperature of described tower top is during higher than described design temperature, described reboiler (4) reduces heat supplied;
When the temperature of described tower top is during lower than described design temperature, described reboiler (4) improves heat supplied.
10. acetonitrile refining process according to claim 9, is characterized in that,
Measure the temperature of described tower top by thermometer (15);
When the temperature of described tower top is during higher than described design temperature, described thermometer (15) sends the 3rd signal, and described reboiler (4) reduces heat supplied in response to described the 3rd signal;
When the temperature of described tower top is during lower than described design temperature, described thermometer (15) sends the 4th signal, and described reboiler (4) improves heat supplied in response to described the 4th signal.
11. according to the acetonitrile refining process described in claim 9 or 10, it is characterized in that,
Described design temperature is positioned at the scope of 30～200 ℃.
12. according to the acetonitrile refining process described in any one in claim 1 to 4, it is characterized in that, also comprises the steps:
Being discharged by tower reactor of product part after described gas phase acetonitrile product (8) will be fractionated out in described distillation tower (2) tower reactor;
When the liquid level in described distillation tower (2) is higher than setting when level value, increase the flow of the product of being discharged by tower reactor;
When the liquid level in described distillation tower (2) is lower than setting when level value, the flow of the product that reduces to be discharged by tower reactor.
13. acetonitrile refining process according to claim 12, is characterized in that,
Measure the liquid level in described distillation tower by liquid level alarm (14);
When the liquid level in described distillation tower (2) is higher than setting when level value, described liquid level alarm (14) sends the 5th signal, and discharging pump (3), 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 (2) is lower than setting when level value, described liquid level alarm (14) sends the 6th signal, and discharging pump (3) is in response to the 6th signal, the flow of the product that reduces to be discharged by tower reactor.
14. according to the acetonitrile refining process described in claim 12 or 13, it is characterized in that,
Described setting level value is positioned at the scope of 1.0～5.0m.
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| CN103772234B (en) | 2016-04-27 |
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