CN116370990A - Negative pressure rectification process method - Google Patents
Negative pressure rectification process method Download PDFInfo
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- CN116370990A CN116370990A CN202310087670.0A CN202310087670A CN116370990A CN 116370990 A CN116370990 A CN 116370990A CN 202310087670 A CN202310087670 A CN 202310087670A CN 116370990 A CN116370990 A CN 116370990A
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- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000001704 evaporation Methods 0.000 claims abstract description 17
- 239000011550 stock solution Substances 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 239000007791 liquid phase Substances 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 238000004821 distillation Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000012528 membrane Substances 0.000 claims abstract description 4
- 238000009833 condensation Methods 0.000 claims abstract description 3
- 230000005494 condensation Effects 0.000 claims abstract description 3
- 230000008020 evaporation Effects 0.000 claims description 13
- 238000005086 pumping Methods 0.000 claims description 6
- 238000002242 deionisation method Methods 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 238000000605 extraction Methods 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 description 10
- 239000012071 phase Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/42—Regulation; Control
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a negative pressure rectification process method, which relates to the technical field of negative pressure rectification and comprises the following steps: starting the rectifying tower, and conveying the stock solution into the rectifying tower through a feed pipe for heating and evaporating; the first negative pressure container and the second negative pressure container are communicated with the rectifying tower in turn to carry out negative pressure air extraction; the mixing container conveys the steam extracted by the first pump and the second pump to the condenser for condensation, and collects the condensed liquid phase; and collecting the azeotrope of the water and the stock solution obtained by preliminary distillation, and dehydrating by using a permeable membrane. According to the invention, the first pump, the second control valve, the second pump and the first control valve are controlled to start and stop in turn, so that the first negative pressure container and the second negative pressure container are communicated with the rectifying tower in turn to perform negative pressure air suction, the rectifying tower can be connected with other equipment without directly passing through an air suction pump, the problem that the efficiency is affected by negative pressure backflow of steam is avoided, and meanwhile, the negative pressure in the rectifying tower can be controlled better.
Description
Technical Field
The invention relates to the technical field of negative pressure rectification, in particular to a negative pressure rectification process method.
Background
The rectification is a separation process for separating the components by utilizing the difference in volatility of the components in the mixture, and common equipment comprises a plate type rectification tower and a packed rectification tower. The principle and the equipment flow of the precise rectification are the same as those of the common rectification, but the relative volatility among the components in the system to be separated is smaller (< 1.05-1.10), so that the high-efficiency precise packing is adopted to realize the separation and purification of the components to be separated. Rectification is usually carried out in a rectifying tower, and gas-liquid two phases are in countercurrent contact to carry out phase-to-phase heat and mass transfer. The volatile components in the liquid phase enter the gas phase, and the less volatile components in the gas phase are transferred to the liquid phase, so that almost pure volatile components can be obtained at the top of the tower and almost pure less volatile components can be obtained at the bottom of the tower. The feed liquid is added from the middle part of the tower, and the tower section above the feed inlet is used for further thickening volatile components in rising steam, which is called a rectifying section; and a tower section below the feed inlet is used for extracting volatile components from the descending liquid and is called stripping section. And condensing vapor led out from the top of the tower, wherein a part of condensate is used as reflux liquid and returns to the rectifying tower from the top of the tower, and the rest distillate is the top product. The liquid extracted from the bottom of the tower is gasified by the reboiler, the vapor rises along the tower, and the rest liquid is used as the bottom product. The ratio of the liquid quantity flowing back into the tower at the top of the tower to the product quantity at the top of the tower is called reflux ratio, the size of the reflux ratio can influence the separation effect and energy consumption of the rectification operation, and materials with higher boiling points are distilled by negative pressure to reduce the temperature during separation and prevent the materials from decomposing; for heat-sensitive materials, they decompose at around the boiling point for a long time and must be distilled under negative pressure.
In the existing negative pressure rectification, a closed tank body is generally adopted to ensure certain negative pressure and then work, but the method changes the air pressure along with the generation of steam, and the closed tank body is unfavorable for extracting steam.
Disclosure of Invention
The invention aims to provide a negative pressure rectification process method to solve the defects in the prior art.
In order to achieve the above object, the present invention provides the following technical solutions: a negative pressure rectification process method comprises the following steps:
step one, starting a rectifying tower, and conveying a stock solution into the rectifying tower through a feed pipe for heating and evaporating;
step two, adding two groups of containers which are a first negative pressure container and a second negative pressure container at the top of the rectifying tower, installing a first control valve and a second control valve on the first negative pressure container and the second negative pressure container, enabling pipelines of the first control valve and the second control valve to extend into the rectifying tower, installing a first pump and a second pump above the first negative pressure container and the second negative pressure container respectively, pumping the internal air of the first negative pressure container and the second negative pressure container, enabling the first pump and the second pump to be connected to a mixing container together, when steam is generated in the rectifying tower, firstly opening the first control valve and the second pump, closing the second control valve and the first pump, enabling the steam in the second negative pressure container to be pumped away, conveying the steam to the mixing container, enabling the second negative pressure container to form negative pressure, and then opening the second control valve and the first pump, closing the first control valve and the second pump, utilizing the negative pressure in the original second negative pressure container, absorbing steam from the rectifying tower to form negative pressure inside the rectifying tower, at the moment, pumping the steam in the first negative pressure container into the mixing container by the first pump to form negative pressure in the first negative pressure container, then opening the first control valve and the second pump, closing the second control valve and the first pump to pump the steam from the rectifying tower by the first negative pressure container, forming negative pressure in the rectifying tower, pumping the steam in the second negative pressure container, forming negative pressure in the second negative pressure container, sequentially circulating, leading the first negative pressure container and the second negative pressure container to be communicated with the rectifying tower in turn for negative pressure pumping, further leading the rectifying tower not to be directly connected with other equipment by the pumping pump, avoiding the problem that the efficiency is affected by the steam due to negative pressure backflow, the negative pressure in the rectifying tower can be better controlled;
step three, the steam pumped by the first pump and the second pump is conveyed to a condenser by the mixing container to be condensed, and the condensed liquid phase is collected;
collecting the azeotrope of water and stock solution obtained by preliminary distillation, removing metal molecules contained in the azeotrope by a deionization method, and dehydrating the azeotrope by a permeable membrane;
preferably, in the first step, a sprayer is arranged at one end of the feed pipe in the rectifying tower, and stock solution is sprayed into the rectifying tower to evaporate through the sprayer so as to improve the evaporation speed.
Preferably, the liquid phase in the rectifying tower is conveyed into a secondary distillation heater through a pipeline for secondary heating and evaporation, the evaporated steam enters the rectifying tower, and the liquid phase obtained by evaporation is an azeotrope of water and stock solution.
Preferably, the feed pipe penetrates through the preheater and then is led into the rectifying tower, the preheater is a resistance heater, and the heating resistor is arranged around the feed pipe to primarily heat the raw liquid conveyed in the feed pipe, so that the evaporation efficiency of the raw liquid in the rectifying tower is quickened.
Preferably, the temperature of the negative pressure evaporation and the negative pressure rectification is 150-180 ℃ and the pressure is 12-15KPa (A).
In the technical scheme, the invention has the technical effects and advantages that:
according to the invention, the two groups of containers at the top of the rectifying tower are used, and the first pump, the second control valve, the second pump and the first control valve are controlled in turn, so that the first negative pressure container and the second negative pressure container are communicated with the rectifying tower in turn to carry out negative pressure air suction, the rectifying tower can be connected with other equipment without directly passing through an air suction pump, the problem that the efficiency is affected by negative pressure backflow of steam is avoided, and meanwhile, the negative pressure in the rectifying tower can be controlled better.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments described in the present invention, and other drawings may be obtained according to these drawings for a person having ordinary skill in the art.
FIG. 1 is a diagram of a rectification apparatus employed in the present invention.
Reference numerals illustrate:
1. a rectifying tower; 2. a feed pipe; 3. a condenser; 4. a secondary distillation heater; 5. a preheater;
a1, a first pump; a2, a second pump; c1, a first negative pressure container; c2, a second negative pressure container; s1, a first control valve; s2, a second control valve; D. a mixing vessel.
Detailed Description
In order to make the technical scheme of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the accompanying drawings.
Examples
The invention provides a negative pressure rectification process method shown in figure 1, which comprises the following steps:
step one, starting a rectifying tower 1, and conveying a stock solution into the rectifying tower 1 through a feed pipe 2 for heating and evaporating;
step two, two groups of containers are additionally arranged at the top of the rectifying tower 1, namely a first negative pressure container C1 and a second negative pressure container C2, a first control valve S1 and a second control valve S2 are arranged on the first negative pressure container C1 and the second negative pressure container C2, pipelines of the first control valve S1 and the second control valve S2 extend into the rectifying tower 1, a first pump A1 and a second pump A2 are arranged above the first negative pressure container C1 and the second negative pressure container C2, the internal air of the first negative pressure container C1 and the second negative pressure container C2 is extracted, the first pump A1 and the second pump A2 are connected to a mixing container D together, when steam is generated in the rectifying tower 1, the first control valve S1 and the second pump A2 are firstly opened, the second control valve S2 and the first pump A1 are closed, the steam in the second negative pressure container C2 is pumped away and is conveyed to the mixing container D, the second negative pressure container C2 is made to form negative pressure, then the second control valve S2 and the first pump A1 are opened, the first control valve S1 and the second pump A2 are closed, steam is sucked from the rectifying tower 1 by utilizing the negative pressure in the original second negative pressure container C2, so that the inside of the rectifying tower 1 is also made to form negative pressure, at the moment, the steam in the first negative pressure container C1 is pumped into the mixing container D by the first pump A1, so that the negative pressure is formed in the first negative pressure container C1, then the first control valve S1 and the second pump A2 are opened, the second control valve S2 and the first pump A1 are closed, so that the first negative pressure container C1 pumps the steam from the rectifying tower 1, so that the negative pressure is formed in the rectifying tower 1, the steam in the second negative pressure container C2 is pumped away, so that the negative pressure is formed in the second negative pressure container C2, the first negative pressure container C1 and the second negative pressure container C2 are communicated with the rectifying tower 1 in turn to carry out negative pressure, the rectifying tower 1 can be connected with other equipment without a suction pump, so that the problem that the efficiency is affected by the negative pressure backflow of steam is avoided, and meanwhile, the negative pressure in the rectifying tower 1 can be better controlled;
step three, the mixing container D conveys the steam extracted by the first pump A1 and the second pump A2 to the condenser 3 for condensation, and collects the condensed liquid phase;
collecting the azeotrope of water and stock solution obtained by preliminary distillation, removing metal molecules contained in the azeotrope by a deionization method, and dehydrating the azeotrope by a permeable membrane;
furthermore, in the above technical scheme, in the first step, a sprayer is disposed at one end of the feed pipe 2 inside the rectifying tower 1, and the raw liquid is sprayed into the rectifying tower 1 to evaporate by the sprayer, so as to increase the evaporation speed.
Further, in the above technical scheme, the liquid phase in the rectifying tower 1 is conveyed into the secondary distillation heater 4 through a pipeline to be subjected to secondary heating evaporation, the evaporated steam enters the rectifying tower 1, and the liquid phase obtained by evaporation is an azeotrope of water and the stock solution.
Furthermore, in the above technical scheme, the feed pipe 2 passes through the preheater 5 and then is led into the rectifying tower 1, the preheater 5 is a resistive heater, and the heating resistor is arranged around the feed pipe 2 to primarily heat the stock solution conveyed in the feed pipe 2, thereby accelerating the evaporation efficiency of the stock solution in the rectifying tower 1.
Further, in the technical scheme, the temperature of the negative pressure evaporation and the negative pressure rectification is 150-180 ℃ and the pressure is 12-15KPa (A);
working principle: by using two groups of containers at the top of the rectifying tower 1, namely a first negative pressure container C1 and a second negative pressure container C2, when steam is generated in the rectifying tower 1, a first control valve S1 and a second pump A2 are firstly opened, the second control valve S2 and the first pump A1 are closed, the steam in the second negative pressure container C2 is pumped away and is conveyed into a mixing container D, the second negative pressure container C2 is formed into negative pressure, then the second control valve S2 and the first pump A1 are opened, the first control valve S1 and the second pump A2 are closed, the steam is sucked from the rectifying tower 1 by utilizing the negative pressure in the original second negative pressure container C2, so that the negative pressure is also formed inside the rectifying tower 1, and at the moment, the steam in the first negative pressure container C1 is pumped into the mixing container D by the first pump A1, so that the negative pressure is formed in the first negative pressure container C1, then, the first control valve S1 and the second pump A2 are opened, the second control valve S2 and the first pump A1 are closed, so that the first negative pressure container C1 is used for extracting steam from the rectifying tower 1, negative pressure is formed in the rectifying tower 1, the steam in the second negative pressure container C2 is extracted, negative pressure is formed in the second negative pressure container C2, the first pump A1, the second control valve S2, the second pump A2 and the first control valve S1 are sequentially circulated, start and stop control is carried out on the first pump A1, the second control valve S2 and the second pump A2 in turn, the first negative pressure container C1 and the second negative pressure container C2 are communicated with the rectifying tower 1 in turn to carry out negative pressure air extraction, the rectifying tower 1 can be connected with other equipment without directly through an air extraction pump, the problem that the efficiency is affected due to negative pressure backflow of the steam is avoided, and meanwhile, the negative pressure in the rectifying tower 1 can be better controlled.
While certain exemplary embodiments of the present invention have been described above by way of illustration only, it will be apparent to those of ordinary skill in the art that modifications may be made to the described embodiments in various different ways without departing from the spirit and scope of the invention. Accordingly, the drawings and description are to be regarded as illustrative in nature and not as restrictive of the scope of the invention, which is defined by the appended claims.
Claims (5)
1. The negative pressure rectification process method is characterized by comprising the following steps of:
step one, starting a rectifying tower (1), and conveying a stock solution into the rectifying tower (1) through a feed pipe (2) for heating and evaporating;
step two, two groups of containers are additionally arranged at the top of the rectifying tower (1), namely a first negative pressure container (C1) and a second negative pressure container (C2), a first control valve (S1) and a second control valve (S2) are arranged on the first negative pressure container (C1) and the second negative pressure container (C2), pipelines of the first control valve (S1) and the second control valve (S2) extend into the rectifying tower (1), a first pump (A1) and a second pump (A2) are respectively arranged above the first negative pressure container (C1) and the second negative pressure container (C2), the internal air of the first negative pressure container (C1) and the second negative pressure container (C2) is pumped, when steam is generated in the rectifying tower (1), the first control valve (S1) and the second pump (A2) are firstly opened, the second control valve (S2) and the first pump (A1) are closed, the second negative pressure container (C2) is led to be pumped to the first negative pressure container (C1) and the second negative pressure container (C2) by the first pump (C2), and then the negative pressure container (C2) is formed in the rectifying tower (C2) and the second negative pressure container (C2) is opened, the method comprises the steps that steam in a first negative pressure container (C1) is pumped into a mixing container (D) by a first pump (A1), negative pressure is formed in the first negative pressure container (C1), then a first control valve (S1) and a second pump (A2) are opened, a second control valve (S2) and the first pump (A1) are closed, the first negative pressure container (C1) pumps the steam from a rectifying tower (1), negative pressure is formed in the rectifying tower (1), steam in a second negative pressure container (C2) is pumped away, negative pressure is formed in the second negative pressure container (C2), and the first negative pressure container (C1) and the second negative pressure container (C2) are sequentially circulated, and are communicated with the rectifying tower (1) in turn to conduct negative pressure pumping;
step three, the mixing container (D) conveys the steam extracted by the first pump (A1) and the second pump (A2) to a condenser (3) for condensation, and the condensed liquid phase is collected;
and step four, collecting the azeotrope of the water and the stock solution obtained by preliminary distillation, removing metal molecules contained in the azeotrope by a deionization method, and dehydrating the azeotrope by a permeable membrane.
2. The negative pressure rectification process of claim 1, wherein: in the first step, a sprayer is arranged at one end of the feed pipe (2) in the rectifying tower (1), and stock solution is sprayed into the rectifying tower (1) to be evaporated through the sprayer.
3. The negative pressure rectification process of claim 1, wherein: the liquid phase in the rectifying tower (1) is conveyed into a secondary distillation heater (4) through a pipeline for secondary heating and evaporation, the evaporated steam enters the rectifying tower (1), and the liquid phase obtained by evaporation is an azeotrope of water and stock solution.
4. The negative pressure rectification process of claim 1, wherein: the feed pipe (2) passes through the preheater (5) and then is led into the rectifying tower (1), the preheater (5) is a resistance heater, and a heating resistor is arranged around the feed pipe (2) to primarily heat the stock solution conveyed in the feed pipe (2).
5. The negative pressure rectification process of claim 1, wherein: the temperature of the negative pressure evaporation and the negative pressure rectification is 150-180 ℃, and the pressure is 12-15KPa (A).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310087670.0A CN116370990A (en) | 2023-02-09 | 2023-02-09 | Negative pressure rectification process method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310087670.0A CN116370990A (en) | 2023-02-09 | 2023-02-09 | Negative pressure rectification process method |
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| Publication Number | Publication Date |
|---|---|
| CN116370990A true CN116370990A (en) | 2023-07-04 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310087670.0A Pending CN116370990A (en) | 2023-02-09 | 2023-02-09 | Negative pressure rectification process method |
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| Country | Link |
|---|---|
| CN (1) | CN116370990A (en) |
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2023
- 2023-02-09 CN CN202310087670.0A patent/CN116370990A/en active Pending
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