A continuous flow high temperature and high pressure experimental device

A high temperature and high pressure, experimental device technology, applied in the investigation phase/state change and other directions, can solve the problems of short equilibration time, long equilibration time, and reduced equilibration time, and achieve accurate equilibrium temperature and equilibrium pressure, accurate, reliable and convenient measurement process. The effect of data collection

Active Publication Date: 2020-01-07
NANJING TECH UNIV
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AI Technical Summary

Problems solved by technology

The experimental device adopted by the distillation method is simple and easy to operate, but it needs a large amount of liquid to measure, and it is easy to produce steam condensation and overheating of the boiling liquid during the operation, resulting in large errors; Destroy the balance in the equilibrium tank, but it is limited to the determination of the system with a short time to achieve equilibrium, and the scope of application is narrow; the experimental equipment used in the static method is simple, but the balance reached in the balance tank will be destroyed to a certain extent during the sampling process state, and the reagent consumption is large, and the equilibrium time is long; the bubble dew point method can be used for the phase equilibrium data determination of multi-components, without analyzing the composition, but the accuracy is low, and the equilibrium time is long; the circulation method, especially the vapor-liquid double cycle The phase equilibrium kettle is not only beneficial to reduce the equilibrium time, but also can obtain samples that can accurately represent the real equilibrium state.
[0004] CN 200910193714.8 and CN 200910193713.3 are based on the Dvorak-Boublik kettle, and branch pipes are respectively drawn from the upper and lower parts of the boiling kettle of the Dvorak-Boublik kettle to connect with the stirring chamber to form a liquid phase internal circulation loop, which is connected with the liquid phase reflux and gas phase condensate of the original equipment The circulation forms three internal circulation loops together, and the equilibrium time is short; but because the vapor phase circulation is realized by its own phase change, the liquid phase reflux liquid needs to be cooled, so the device is only suitable for the phase equilibrium data of the system with relatively low volatility Determination, and it is impossible to obtain an accurate two-phase sample that can accurately represent the real equilibrium state, and the measurement results cannot truly reflect the equilibrium state
[0005] CN 201120229585.6 is based on two vapor-liquid balance tanks with internal circulation loops, including a vapor-phase riser, a vapor-liquid separator, a still and a temperature control cabinet. The heat preservation effect is good, and the temperature control is also accurate. It is suitable for relative volatility Determination of phase equilibria data for smaller systems, and it is not possible to obtain a two-phase sample that accurately represents the true equilibrium state
[0006] CN 201310109090.3 is based on a stainless steel visual balance kettle with constant volume, and further optimizes and improves the feeding system and sampling system. The data collection is simple, but it is only suitable for liquid-liquid two-phase equilibrium data determination, and cannot be quickly achieved. Phase Equilibrium of Mixed Systems

Method used

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  • A continuous flow high temperature and high pressure experimental device
  • A continuous flow high temperature and high pressure experimental device
  • A continuous flow high temperature and high pressure experimental device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Phase Equilibrium Data Determination:

[0051] 1. Open the high and low temperature circulation tank, set the temperature required for the operation of the balance tank 3; turn on the vacuum pump, vacuum the buffer tank 2, balance tank 3 and each pipeline to the ultimate pressure, and use the vacuum to suck 20ml of ethyl butyrate.

[0052] 2. Put a certain amount of CO 2 The gas is extracted from the gas cylinder 1, enters the buffer tank 2 through the valve V1 and the valve V2 in turn, cools down to -20°C, and then heats up to 30°C, the fluid in the carrier gas tank 2 is rapidly increased to 40MPa, and the high-pressure fluid passes through the one-way The valve V3 is sent to the phase balance tank 3 and mixed with ethyl butyrate.

[0053] 3. Turn on the non-leakage pumps 6 and 7, and the circulating flow rate is 0.5ml / min~3ml / min, respectively to carry out forced circulation of the vapor-liquid two phases.

[0054] 4. When the pressure and temperature in the balance...

Embodiment 2

[0057] Phase Equilibrium Data Determination:

[0058] 1. Open the high and low temperature circulation tank, set the temperature required for the operation of the balance tank 3; turn on the vacuum pump, vacuum the buffer tank 2, balance tank 3 and each pipeline to the ultimate pressure, and use the vacuum to suck 25ml of isobutyl acetate.

[0059] 2. Put a certain amount of CO 2 The gas is drawn from the gas cylinder 1, enters the buffer tank 2 through the valve V1 and the valve V2 in turn, cools down to -20°C, and then heats up to 70°C, the fluid in the carrier gas tank 2 is rapidly boosted to 70MPa, and the high-pressure fluid passes through the one-way valve V3 is sent to phase balance tank 3 and mixed with ethyl butyrate.

[0060] 3. Turn on the non-leakage pumps 6 and 7, and the circulation flow rate is 1ml / min~3.5ml / min, and the vapor-liquid two-phase is forced to circulate respectively.

[0061] 4. When the pressure and temperature in the balance kettle 3 are stable ...

Embodiment 3

[0064] Subsupercritical extraction experiment:

[0065] 1. Open the high and low temperature circulation tank, set the temperature required for the operation of the balance tank 3; turn on the vacuum pump, vacuum the buffer tank 2, balance tank 3 and each pipeline to the ultimate pressure, and use the vacuum to suck 30ml of engine oil.

[0066] 2. Put a certain amount of CO 2 The gas is drawn from the gas cylinder 1, enters the buffer tank 2 through the valve V1 and the valve V2 in turn, cools down to -30°C, and then heats up to 80°C, the fluid in the carrier gas tank 2 is rapidly boosted to 95MPa, and the high-pressure fluid passes through the check valve V3 is sent to phase balance kettle 3 and mixed with engine oil.

[0067] 3. Turn on the non-leakage pump 9, the circulation flow rate is 1ml / min-3.5ml / min, and the mixed system is forced to circulate, and the time for each intermittent extraction is 2h.

[0068] 4. After the extraction is completed, the extracted material ...

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Abstract

The invention relates to a continuous flowing type high temperature and high pressure experiment device. The continuous flowing type high temperature and high pressure experiment device comprises an accumulator still, a three-cycle high pressure phase equilibrium still, a separation kettle, a solvent storage tank, a first zero leak pump, a second zero leak pump, a third zero leak pump, a fourth zero leak pump, a vacuum device, a first six-way transfer valve, a second six-way transfer valve and an online analysis system. The provided continuous flowing type high temperature and high pressure experiment device is suitable for the phase equilibrium of a multicomponent system, supercritical fluid extraction, and measurement of various experimental data in high temperature and high pressure chemical reactions, a phase equilibrium sample truly representing the state is acquired, the balance time is short, the balance composition, the balance temperature and the balance pressure are accurately measured, and the experiment operation is simple and convenient.

Description

technical field [0001] The invention relates to the fields of thermodynamic phase equilibrium, reaction engineering, chemical mass transfer and chemical separation, in particular to a continuous flow high temperature and high pressure experimental device. Background technique [0002] The phase equilibrium relationship is the basic data of chemical unit operations such as distillation and absorption, and is also the basis for physical property estimation, simulation calculation, computer-aided design, chemical process optimization and equipment improvement. It is of great significance to chemical theoretical research and practical application. At present, the phase equilibrium data are mainly obtained through experimental measurement and theoretical calculation. However, due to the lack of corresponding physical parameters, it is difficult to obtain the phase equilibrium data of many substances directly by theoretical calculation. Therefore, the experimental measurement metho...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N25/12
CPCG01N25/12
Inventor 桂霞云志
Owner NANJING TECH UNIV
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