High-temperature and high-pressure equipment and method for microscopic visual sulfur deposit seepage test

Patent metadata

Field	Value
Publication number	US-11530973-B1
Application number	US-202117509109-A
Country	US
Kind code	B1
Filing date	Oct 25, 2021
Priority date	Jun 1, 2021
Publication date	Dec 20, 2022
Grant date	Dec 20, 2022

Abstract

A high-temperature and high-pressure equipment and method for microscopic visual sulfur deposit seepage test is provided by the present disclosure, the equipment comprises an injection system, a high-temperature and high-pressure visual kettle, a pressure supply system, a data acquisition and analysis system, a fluid recovery system, and an injection branch pipe; the injection system comprises an ISCo micro-injection pump, an intermediate container, a thermostatic heating oven and a pressure meter; the intermediate container is arranged in the thermostatic heating oven, the ISCo micro-injection pump is connected to the intermediate container; the data acquisition and analysis system comprises a microscope, a high-brightness light source and a computer; the pressure supply system comprises an annular pressure tracking pump, a back pressure pump, a back pressure valve and a pressure gauge; the fluid recovery system comprises a wide neck flask with rubber stopper, a balance, a flowmeter and an exhaust gas absorber tank.

First claim

What is claimed is:

1. A high-temperature and high-pressure equipment for microscopic visual sulfur deposit seepage test, comprising an injection system, a high-temperature and high-pressure visual kettle, a pressure supply system, a data acquisition and analysis system, a fluid recovery system, and an injection branch pipe, wherein the injection system, high-temperature and high-pressure visual kettle, pressure supply system, and fluid recovery system are connected in sequence by pipes; the injection system comprises an ISCo micro-injection pump, an intermediate container, a thermostatic heating oven and a pressure meter; the intermediate container is arranged in the thermostatic heating oven, the ISCo micro-injection pump is connected to the intermediate container, and the pressure meter is set on the pipe between the ISCo micro-injection pump and the intermediate container; the data acquisition and analysis system comprises a microscope, a high-brightness light source and a computer; the pressure supply system comprises an annular pressure tracking pump, a back pressure pump, a back pressure valve and a pressure gauge; the fluid recovery system comprises a wide neck flask with rubber stopper, a balance, a flowmeter and an exhaust gas absorber tank; the thermostatic heating oven, microscope, high-brightness light source and balance are connected to the computer by a data transmission line, respectively.

2. The high-temperature and high-pressure equipment for microscopic visual sulfur deposit seepage test according to claim 1 , wherein the intermediate container comprises a first intermediate container and a second intermediate container; one ends of the first intermediate container and the second intermediate container are respectively connected to the ISCo micro-injection pump, and the other ends are respectively connected to the high-temperature and high-pressure visual kettle via a pipe; the test fluid in the intermediate container is first heated to the temperature required for the microscopic visual deposit seepage test by the thermostatic heating oven, and injected into the seepage test sample in the high-temperature and high-pressure visual kettle via the pipe under the pressure and at the flow rate both generated by the ISCo micro-injection pump as required for the test.

3. A high-temperature and high-pressure method for microscopic visual sulfur deposit seepage test according to claim 2 , comprising the following steps:
S 1 : putting the core slice holder with seepage test sample into the high-temperature and high-pressure visual kettle and fix it, setting the temperature to 115° C. on the thermostat, opening the valve G after the temperature in the kettle rises to 93° C., setting the pressure of the annular pressure tracking pump to 29 MPa to establish an annular pressure while opening the balance and the hydrogen sulfide gas monitor at the same time, then opening the valve F, and setting the pressure of back pressure pump to 35 MPa to establish a back pressure;
S 2 : turning on the high-brightness light source and the microscope, and adjusting the focal length of the microscope until the seepage test sample on the computer is clearly visible and meets the preset definition requirements of the test;
S 3 : opening the thermostatic heating oven and setting the temperature to 115° C., heating the fluid in the first intermediate container and the second intermediate container to 115° C., and then keeping it at a constant temperature;
S 4 : setting the flow rate of the ISCO micro-injection pump to 0.1 ml/min, opening the valve A, valve C and valve D, pressing the “Start” button of the ISCO micro-injection pump to inject the liquid sulfur in the first intermediate container into the core slice holder;
S 5 : clicking “Start Recording” on the computer to store the real-time recorded images on the computer, monitoring the fluid change and sulfur distribution in the core slice holder in real time through the screen of the computer, pressing the “Pause” button on the ISCO micro-injection pump to stop injection when it is observed that there is basically no change in the images acquired by the computer and the fluid volume in the wide neck flask with rubber stopper is 2 PV, and then safely disposing of the liquid sulfur in the wide neck flask with rubber stopper;
S 6 : first closing the valve C and valve D, then open the valve B and valve E, then setting a constant speed for the ISCO micro-injection pump for displacement, setting the displacement speed to 0.1 mL/min, pressing the “Start” button to inject carbon dioxide gas containing sulfur powder, programing with VB language whenever the image observed by the microscope changes once, and storing the real-time saved images in the computer, and monitoring the sulfur deposit pattern through the screen of the computer; pressing the “Pause” button on the ISCo micro-injection pump to stop injection when it is observed that there is basically no change in the images acquired by the computer and no further change in the balance; and
S 7 : closing all valves, turn off the high-brightness light source, the back pressure pump and the annular pressure tracking pump, removing the core slice holder, and cleaning each device; safely disposing of the fluid in the wide neck flask with rubber stopper and the gas in the exhaust gas absorber tank; the microscopic visual sulfur deposit seepage test at high temperature and high pressure is completed.

4. The high-temperature and high-pressure equipment for microscopic visual sulfur deposit seepage test according to claim 1 , wherein the microscope is set above the high-temperature and high-pressure visual kettle and the lens of the microscope is aligned with the seepage test sample at the core slice holder in the kettle; the high-brightness light source is an LED lamp, located below the lens of the microscope and above the high-temperature and high-pressure visual kettle.

5. The high-temperature and high-pressure equipment for microscopic visual sulfur deposit seepage test according to claim 1 , wherein the high-temperature and high-pressure visual kettle comprises an internal thermal conductive cylinder, an external insulated cylinder, a thermostat and a core slice holder; the internal thermal conductive cylinder is set inside the external insulated cylinder, a resistive heater is provided between the internal thermal conductive cylinder and the external insulated cylinder, and connected to the thermostat via a data transmission line; the core slice holder is fixed inside the internal thermal conductive cylinder during microscopic deposit seepage test, and is used to hold the seepage test sample.

6. The high-temperature and high-pressure equipment for microscopic visual sulfur deposit seepage test according to claim 5 , wherein an inlet of the core slice holder [ 15 ] is connected with the intermediate container through the injection branch pipe [ 36 ], and an outlet of the core slice holder is connected with a back pressure valve through a pipeline.

7. The high-temperature and high-pressure equipment for microscopic visual sulfur deposit seepage test according to claim 1 , wherein the supply system comprises an annular pressure tracking pump, a back pressure pump, a back pressure valve and a pressure gauge, wherein the annular pressure tracking pump is connected to the high-temperature and high-pressure visual kettle via a pipeline and used to provide annular pressure for the high-temperature and high-pressure visual kettle; the back pressure pump is connected to the back pressure valve and used to provide back pressure for high-temperature and high-pressure visual kettle; the pressure gauge is set on the pipe between the back pressure valve and the high-temperature and high-pressure visual kettle and used to collec

Assignees

• Univ Southwest Petroleum

Inventors

• Guo Xiao
• Shi Ziming
• Zhou Li
• Wang Shengyuan
• Luo Jun
• Li Linkai
• Zhou Ming
• Ma Jingjing
• Wang Li
• Kong Bing

Classifications

• G01N21/0303

  Optical path conditioning in cuvettes, e.g. windows; adapted optical elements or systems; path modifying or adjustment (G01N21/031 - G01N21/15 take precedence) · CPC title

• G01N15/0826 Primary

  and measuring fluid flow rate, i.e. permeation rate or pressure change · CPC title

• G01N15/0893

  by measuring weight or volume of sorbed fluid, e.g. B.E.T. method · CPC title

• G01N2015/0846

  by use of radiation, e.g. transmitted or reflected light · CPC title

• G01M3/226

  for containers, e.g. radiators · CPC title