CN216955882U - High-temperature high-pressure liquid-liquid phase balance kettle - Google Patents
High-temperature high-pressure liquid-liquid phase balance kettle Download PDFInfo
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- CN216955882U CN216955882U CN202220107953.8U CN202220107953U CN216955882U CN 216955882 U CN216955882 U CN 216955882U CN 202220107953 U CN202220107953 U CN 202220107953U CN 216955882 U CN216955882 U CN 216955882U
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Abstract
The utility model discloses a high-temperature high-pressure liquid-liquid phase balance kettle, which comprises a kettle body and an upper cover arranged at the top of the kettle body; the bottom in the kettle body is provided with a stirring device, the upper cover is provided with a pressure gauge for measuring the pressure in the kettle body, and a first sampling pipe and a second sampling pipe which extend into the kettle body, the top of the first sampling pipe is provided with a first three-way valve, the top of the second sampling pipe is provided with a second three-way valve, the first sampling pipe is communicated with a first interface of the first three-way valve, the second sampling pipe is communicated with a first interface of the second three-way valve, and second interfaces of the first three-way valve and the second three-way valve are both connected with the pressure gauge; the side wall of the upper cover is provided with a pressurizing valve. The utility model has simple structure and reasonable design, can be used at high temperature and high pressure compared with the common liquid-liquid phase balance container, is particularly suitable for a wide boiling range and high viscosity liquid-liquid phase balance system, is not easy to pollute the sample during sampling, and realizes automatic sampling under pressure.
Description
Technical Field
The utility model belongs to the technical field of balance kettles, and particularly relates to a high-temperature high-pressure liquid-liquid phase balance kettle.
Background
In chemical production, for heterogeneous reaction systems, the design of a reactor and the design of a separation device are closely related to phase equilibrium. In one aspect, the phase equilibrium data defines the separation and dissolution limits of the respective species; phase equilibrium data, on the other hand, is necessary for chemical process simulation calculations. Therefore, the phase equilibrium data is very important for the chemical process designers how to design more economical and efficient reactors and separation equipment. However, sampling under high temperature, high pressure and high viscosity conditions can affect the accuracy of the phase equilibrium data, and is particularly important for the design of liquid-liquid phase equilibrium devices.
At present, a glass instrument is taken as a liquid-liquid phase equilibrium container, and sampling is carried out by using an injector, so that the measurement of the liquid-liquid phase equilibrium under the conditions of low temperature, low viscosity and normal pressure is generally limited, but engineering application and scientific research need liquid-liquid phase equilibrium data in a wider temperature and pressure range, and the measurement of the liquid-liquid phase equilibrium under the conditions of high temperature, high viscosity and high pressure is inevitably involved. And the lower layer of the sample is easily polluted by the upper liquid phase when the lower layer of the sample is taken by the injector, so that the data is inaccurate.
SUMMERY OF THE UTILITY MODEL
In order to solve the problems, the utility model aims to provide a high-temperature high-pressure liquid-liquid phase equilibrium kettle which is applicable to high temperature, high pressure and high viscosity and can realize automatic sampling of an upper layer and a lower layer respectively.
In order to achieve the purpose, the technical scheme of the utility model is as follows:
a high-temperature high-pressure liquid-liquid phase balance kettle comprises a kettle body and an upper cover arranged at the top of the kettle body; the bottom in the kettle body is provided with a stirring device, the upper cover is provided with a pressure gauge for measuring the pressure in the kettle body, and a first sampling pipe and a second sampling pipe which extend into the kettle body, the top of the first sampling pipe is provided with a first three-way valve, the top of the second sampling pipe is provided with a second three-way valve, the first sampling pipe is communicated with a first interface of the first three-way valve, the second sampling pipe is communicated with a first interface of the second three-way valve, and second interfaces of the first three-way valve and the second three-way valve are both connected with the pressure gauge; the side wall of the upper cover is provided with a pressurizing valve.
Further, a third interface of the first three-way valve is connected with a second two-way valve.
Further, a third interface of the second three-way valve is connected with a third two-way valve.
Furthermore, the bottom ends of the first sampling tube and the second sampling tube are spaced from the bottom surface of the kettle body.
Further, the diameter of the kettle body is 20 mm.
Further, the internal magnetic rotor that is provided with of cauldron, the length of magnetic rotor is less than the diameter of the cauldron body.
Further, the internal diameter of the first sampling tube and the second sampling tube is 1 mm.
Further, the first sampling tube and the second sampling tube have different lengths.
Further, the length of the first sampling tube is greater than the length of the second sampling tube.
Compared with the prior art, the utility model has the beneficial effects that:
according to the utility model, the first sampling tube, the first three-way valve and the pressure gauge form a gas pipeline, and the second sampling tube, the second three-way valve and the pressure gauge form a gas pipeline, so that the pressure of the first sampling tube, the pressure of the second sampling tube and the pressure of the kettle body are the same, the feed liquid is prevented from being pressed into the sampling tubes, and the phase balance data is more accurate; the temperature measuring range of the balance kettle is 20-250 ℃, the pressure range is 0-10Mpa, the measuring range is wide, and the pressure can be increased and released at any time; the balance kettle can automatically sample under pressure, and is suitable for high-viscosity samples and low-viscosity samples.
Furthermore, the length of the first sampling tube is greater than that of the second sampling tube, so that liquid with different heights in the kettle body is formed, the sample in the kettle body is not easily polluted, and automatic sampling can be realized under high pressure.
Furthermore, the kettle body is connected with the kettle cover through threads, so that the kettle is convenient to mount and dismount.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Fig. 2 is a schematic view of a heating module.
In the figure, 1 is a kettle body, 2 is an upper cover, 3 is a pressure gauge, 4 is a first sampling tube, 5 is a second sampling tube, 6 is a first two-way valve, 7 is a first three-way valve, 8 is a second three-way valve, 9 is a second two-way valve, 10 is a third two-way valve, 11 is a magnetic rotor, and 12 is a heating module.
Detailed Description
The present invention will be described with reference to the accompanying drawings.
Referring to fig. 1 and 2, the high-temperature and high-pressure liquid-liquid phase equilibrium still of the present invention includes a still body 1 and an upper cover 2 disposed on the top of the still body 1. The bottom is provided with agitating unit in the cauldron body 1, be provided with the manometer 3 that is used for measuring the internal pressure of cauldron body 1 on the upper cover 2 and stretch into first sampling tube 4 and the second sampling tube 5 in the cauldron body 1, the top of first sampling tube 4 is provided with first three-way valve 7, the top of second sampling tube 5 is provided with second three-way valve 8 to first sampling tube 4 is linked together with the first interface of first three-way valve 7, second sampling tube 5 is linked together with the first interface of second three-way valve 8, the second interface of first three-way valve 7 and second three-way valve 8 all links to each other with manometer 3. The third port of the first three-way valve 7 is also connected to the second two-way valve 9, and the third port of the second three-way valve 8 is also connected to the third two-way valve 10. The lower ends of the first sampling tube 4 and the second sampling tube 5 penetrate through the upper cover 2 to be fixed with the upper cover and keep a certain distance with the bottom of the balance kettle.
The side wall of the upper cover 2 is provided with a pressurizing valve 6.
The kettle body 1 is a stainless steel cylinder with the diameter of 20 mm.
A magnetic rotor 11 is placed at the bottom of the kettle body 1, and the length of the magnetic rotor 11 is slightly smaller than the diameter of the kettle body.
The temperature measuring range of the equilibrium kettle is 20-250 ℃, and the pressure measuring range is 0-10 Mpa.
The first sampling tube 4 and the second sampling tube 5 are both stainless steel tubes with the inner diameter of 1 mm. The first sampling tube 4 and the second sampling tube 5 have different lengths, and the length of the first sampling tube 4 is greater than that of the second sampling tube 5.
The first sampling pipe 4 is connected with a first three-way valve 7 and a second two-way valve 9 to form a lower layer solution sampling pipeline.
The second sampling pipe 5 is connected with a second three-way valve 8 and a third two-way valve 10 to form an upper solution sampling pipeline.
The first sampling pipe 4 and the first three-way valve 7 are connected with the pressure gauge 3 to form a gas pipeline, and the second sampling pipe 5 and the second three-way valve 8 are connected with the pressure gauge 3 to form a gas pipeline.
The experimental steps for determining the liquid-liquid phase balance of the high-viscosity liquid by the high-temperature high-pressure liquid-liquid phase balance kettle are as follows:
step one, a sample is loaded and the device is sealed. Firstly, the magnetic rotor 11 is put into the kettle body 1, then a certain amount of experimental samples (glycerol, diethyl carbonate and ethanol) are put into the kettle body 1, and finally the kettle body 1 and the upper cover 2 are sealed firmly.
And step two, evacuating the device and replacing the gas. The first two-way valve 7 and the second two-way valve 8 are closed, the pressurizing valve 6 is opened, and the second ports of the second two-way valve 9 and the third two-way valve 10 are opened. And connecting the nitrogen source with the pressurizing valve 6, opening the nitrogen source, closing the gas source when the value of the pressure gauge 3 of the balance kettle rises to 1.2Mpa, and opening the nitrogen source again after the gas in the balance kettle is slowly emptied. The process of vacuumizing and filling nitrogen is repeated for several times, other gases in the device and the pipeline are replaced, the pressurizing valve 6 is closed, and the nitrogen source is dismounted.
And step three, setting phase equilibrium temperature and stirring speed. The equilibrium still was placed in the heating module 12 shown in fig. 2 (the heating module was an existing cylindrical module), and the whole apparatus was placed on a magnetic heating stirrer, and the temperature and stirring rate were set. After stirring for 3 hours, the mixture was allowed to stand for 4 hours.
And step four, sampling and analyzing the sample. Firstly, taking down a lower layer sample, opening a third interface of the first three-way valve 7, simultaneously opening the second two-way valve 9, and closing a first interface of the second two-way valve 9 when the lower layer sample flows out of about 1 mL. Similarly, the first port of the second three-way valve 8 is opened, and the third two-way valve 10 is opened to take the upper layer sample. Then, the upper and lower samples were diluted, respectively, and the concentrations of the substances contained in each phase were analyzed by gas chromatography.
The working principle of the utility model is as follows:
after the reagent is added into the kettle body 1, the upper cover 2 and the kettle body 1 are sealed, first interfaces of the first three-way valve 7 and the second three-way valve 8 are opened, then a nitrogen source is connected with the pressure valve 6, inert gas is filled into the nitrogen source to increase the system pressure, and then the pressure valve 6 is closed and the gas source is detached. At the moment, the pressure in the two sampling tubes is the same as that in the kettle body, so that liquid is effectively prevented from being pressed into the sampling tubes. During sampling, firstly, a lower layer liquid sample is taken down, a third interface of the first three-way valve 7 is opened, meanwhile, the second two-way valve 9 is opened, and the lower layer sample automatically flows out under the driving of pressure. Similarly, the third port of the second three-way valve 8 is opened, the third two-way valve 10 is opened, and the upper layer sample is taken.
The utility model has the advantages that: the structure is simple, the design is reasonable, compared with the common container for liquid-liquid phase balance, the device can be used under high temperature and high pressure, and is particularly suitable for a wide boiling range and high viscosity liquid-liquid phase balance system, the sample is not easy to be polluted during sampling, and the automatic sampling under pressure is realized.
The basic principles and main features of the present invention and the advantages thereof are described above, and any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A high-temperature high-pressure liquid-liquid phase balance kettle is characterized by comprising a kettle body (1) and an upper cover (2) arranged at the top of the kettle body (1); the bottom in the kettle body (1) is provided with a stirring device, the upper cover (2) is provided with a pressure gauge (3) for measuring the pressure in the kettle body (1) and a first sampling pipe (4) and a second sampling pipe (5) which extend into the kettle body (1), the top of the first sampling pipe (4) is provided with a first three-way valve (7), the top of the second sampling pipe (5) is provided with a second three-way valve (8), the first sampling pipe (4) is communicated with a first interface of the first three-way valve (7), the second sampling pipe (5) is communicated with a first interface of the second three-way valve (8), and second interfaces of the first three-way valve (7) and the second three-way valve (8) are connected with the pressure gauge (3); the side wall of the upper cover (2) is provided with a pressure valve (6).
2. A high temperature and high pressure liquid-liquid phase equilibrium still as claimed in claim 1 wherein the third port of the first three-way valve (7) is connected to a second two-way valve (9).
3. A high temperature and high pressure liquid-liquid phase equilibrium still according to claim 1, wherein the third port of the second three-way valve (8) is connected with a third two-way valve (10).
4. A high temperature and high pressure liquid-liquid phase equilibrium still as claimed in claim 1 wherein the bottom ends of the first sampling tube (4) and the second sampling tube (5) are spaced from the bottom surface of the still body (1).
5. A high temperature and high pressure liquid-liquid phase equilibrium still as claimed in claim 1 wherein the diameter of said still body (1) is 20 mm.
6. A high temperature and high pressure liquid-liquid phase equilibrium still according to claim 1, characterized in that the magnetic rotor (11) is arranged in the still body (1), and the length of the magnetic rotor (11) is less than the diameter of the still body (1).
7. A high temperature and high pressure liquid-liquid phase equilibrium still according to claim 1, wherein the inner diameters of the first sampling tube (4) and the second sampling tube (5) are both 1 mm.
8. A high temperature and pressure liquid-liquid phase equilibrium still according to claim 1, wherein the length of the first sampling tube (4) is different from that of the second sampling tube (5).
9. A high temperature and pressure liquid-liquid phase equilibrium still according to claim 1, wherein the length of the first sampling tube (4) is longer than the length of the second sampling tube (5).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202220107953.8U CN216955882U (en) | 2022-01-15 | 2022-01-15 | High-temperature high-pressure liquid-liquid phase balance kettle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202220107953.8U CN216955882U (en) | 2022-01-15 | 2022-01-15 | High-temperature high-pressure liquid-liquid phase balance kettle |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN216955882U true CN216955882U (en) | 2022-07-12 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202220107953.8U Active CN216955882U (en) | 2022-01-15 | 2022-01-15 | High-temperature high-pressure liquid-liquid phase balance kettle |
Country Status (1)
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|---|---|
| CN (1) | CN216955882U (en) |
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- 2022-01-15 CN CN202220107953.8U patent/CN216955882U/en active Active
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