CN206740467U - A kind of heat releases hydrocarbon pre-treatment specimen automatic preparation equipment - Google Patents

Abstract

The utility model discloses an automatic sample preparation device for pyrohydrocarbon pretreatment, comprising: a carbon dioxide adsorption device, a heating device, a cleaning device, a vacuum device, a sampling device and a control device. The utility model connects the control device with the above-mentioned devices through a circuit Connect to control the automatic operation of the above-mentioned devices. The utility model automatic sample preparation device for pretreatment of pyrohydrocarbons saves the process of manually filling sodium hydroxide, reduces the resulting problems of atmospheric dead volume, air leakage and pollution, automatically cleans the pyrotubes, and works in a unified manner The ambient temperature greatly improves the quality and preparation efficiency of the product; the device is easy to operate and eliminates potential safety hazards in the work, and is especially suitable for the preparation of soil/rock pyrohydrocarbon samples in oil and gas geochemical exploration laboratories, and the utility model passes Integrating each device, the device has strong integrity and is easy to carry, and is also suitable for on-site preparation and analysis of pyrohydrocarbon samples in the field.

Description

An automatic sample preparation device for pyrohydrocarbon pretreatment

technical field

The utility model belongs to the field of oil and gas accumulation, and relates to an automatic preparation device for pretreatment samples of pyrohydrocarbons, and a method for preparing pretreatment samples of pyrohydrocarbons by using the device, which is suitable for testing methods of pyrohydrocarbons in oil and gas geochemical exploration laboratories Soil sample preparation.

Background technique

Hydrocarbons are the main components of oil and gas reservoirs. Because hydrocarbon molecules are small and have strong permeability, they are easy to escape to the surface through the overlying strata. The hydrocarbons present in the surface medium are not only wrapped in carbonate minerals (measured by acid hydrolysis method), but also adsorbed in silicate minerals such as clay. In the laboratory, the thermal desorption method is used to desorb the adsorbed hydrocarbon gas through medium and high temperature for a predetermined time.

At present, the pyrohydrocarbon sample preparation device in the laboratory mainly fills the sample with the pyrotube, seals and vacuumizes it, then transfers it to the pyrofurnace for heating, and absorbs the carbon dioxide in it with sodium hydroxide solution. During the operation, it is necessary to change the environment of the pyrotube and the sample in it several times, and complete the alternate work of water, gas, sodium hydroxide, etc. through manual connection/disconnection. In the process of moving and combining, the ambient temperature is difficult to be uniform, and factors affecting quality such as air leakage and air dead volume will inevitably occur, resulting in the fact that there is air pollution in samples released from heat. In addition, there is a risk of damage and accidental injury to the fragile glassware when it is constantly moved, and there is a potential safety hazard of strong alkali corrosion for the staff. The cumbersome operation process is a major factor affecting work efficiency. Therefore, in the case of increasing sample volume and increasing quality requirements, the accuracy, efficiency, safety, and labor intensity of such devices have gradually become difficult to meet the requirements.

At present, there is no device in the prior art that can prepare samples for this experimental method more efficiently, with higher quality, and with greater safety. The utility model is an automatic pyrohydrocarbon sample preparation device.

Utility model content

The purpose of this utility model is to solve the problems existing in the prior art, to provide a kind of automatic sample preparation device for pyrolysis hydrocarbon pretreatment, to improve the original pyrolysis sample preparation device, and to improve the The automation of sample preparation, and the preparation of pyrohydrocarbon pretreatment samples with this device solves the problem that the ambient temperature is difficult to unify, and the phenomenon of air leakage and air dead volume in the pyrotube causes air pollution in the sample released by heat. , the pyrohydrocarbon pretreatment sample prepared by using the device has good quality and no pollution, and the preparation method is simple and easy, and the efficiency is high.

According to the utility model, an automatic sample preparation device for pyrohydrocarbon pretreatment is provided, comprising:

A carbon dioxide adsorption device for processing the sample to be tested to obtain the product;

a heating device for performing heat treatment on the carbon dioxide adsorption device;

a cleaning device for cleaning the carbon dioxide adsorption device;

A vacuum device that makes the carbon dioxide adsorption device form a vacuum environment;

a sampling device for extracting and storing the product obtained after treatment by said carbon dioxide adsorption device; and,

A control device that controls the automatic operation of the above-mentioned devices through a line.

According to a preferred embodiment of the present invention, the carbon dioxide adsorption device includes:

The pyrotube is vertically arranged inside the heating device, and has a liquid outlet hole on its arc-shaped bottom surface, and its top is exposed outside the heating device;

A sealing cap, covering the top of the thermorelease tube;

The rubber bowl is located below the heat release tube, and its upper surface is provided with an arc-shaped groove corresponding to the arc-shaped bottom surface of the heat release tube;

The tray is located at the bottom of the heating device, its upper surface is fixed to the rubber bowl, and its lower surface is connected to the lifter;

a lifter connected to the tray;

The alkali adding device includes a liquid storage tank and a liquid inlet pipe. One end of the liquid inlet pipe is connected to the liquid storage tank, and the other end passes through the sealing cover and leads into the pyrolysis tube.

According to some embodiments of the present invention, the diameter of the arc-shaped groove on the rubber bowl is larger than the diameter of the thermal release tube.

According to a preferred embodiment of the present invention, the lifting and lowering of the pallet is controlled by a lifter, thereby controlling the rising and falling of the rubber bowl; If the bottom of the pyrotube is attached, the bottom of the pyrotube is sealed, and the reaction can take place to process the sample; when the rubber bowl descends, its groove is separated from the bottom surface of the thermorelease tube, and the bottom of the thermorelease tube is opened. , the liquid or gas in the pyrotube is discharged through the liquid outlet hole.

According to some embodiments of the present utility model, the number of the thermorelease tube is at least one, and the number is determined according to the amount of the sample to be processed.

According to a preferred embodiment of the present invention, the number of the rubber bowls is the same as the number of the thermal release tubes.

According to some embodiments of the present invention, the lifter is not particularly limited, and may be any device capable of lifting in the art, such as a cylinder, a piston, and the like.

According to a preferred embodiment of the present utility model, a water outlet is provided at the side bottom of the heating device, and the liquid or gas flowing out of the thermal release tube can be discharged through the water outlet.

According to some embodiments of the present utility model, the heating device is a sealed heating device.

In some specific embodiments, the heating device is preferably a heatable thermostat.

According to a preferred embodiment of the utility model, the cleaning device includes:

A water storage tank that feeds water into the thermo-release tube to clean it, and is connected to the thermo-release tube via a water inlet pipe;

A water inlet pipe, one end is connected to the water storage tank, and the other end passes through the sealing cover and leads into the thermal release tube;

An air compressor blowing high-pressure air into the thermal release tube communicates with the thermal release tube through a pipeline passing through the sealing cap.

The utility model uses a cleaning device to clean the carbon dioxide absorption device. First, the water in the water storage tank enters the heat release pipe through the water inlet pipe to clean the heat release pipe and the rubber bowl; Blow high-pressure air into the release pipe to purge and clean it.

According to some embodiments of the present utility model, the vacuum device includes:

A vacuum pump and a vacuum pipeline, the vacuum pipeline passes through the sealing cover and communicates with the thermal release tube.

According to a preferred embodiment of the utility model, the sampling device includes:

The sampling tube runs through the sealing cap, and the exposed end is plugged tightly with a sealing plug;

The sampler extracts and stores the gas product in the pyrotube through the sampling tube.

In some specific embodiments, the sampler is preferably a syringe, and after the treatment is completed, a sealing plug is inserted to extract the gas product in the pyrotube.

According to some embodiments of the present utility model, the control device includes a controller, which is connected to the lifter, the heating device, the switch of the air compressor and the vacuum pump, and the valves on the water inlet pipe and the liquid inlet pipe through pipelines, To control the automatic operation of each device.

The utility model has advantages and beneficial technical effects as follows:

The utility model automatically prepares the sample for pyrohydrocarbon pretreatment, which saves the process of manually filling sodium hydroxide, reduces the problems of atmospheric dead volume, air leakage and pollution, automatically cleans the pyrotube, and works in a unified manner. The ambient temperature greatly improves the quality of the product and the preparation efficiency; the utility model device is easy to operate, reduces the labor intensity of personnel, and eliminates potential safety hazards in the work; at the same time, the utility model device occupies a small area and is especially suitable for oil and gas The preparation of soil/rock pyrohydrocarbon samples in the geochemical exploration laboratory, and the utility model integrates the various devices together, the device has strong integrity and is easy to carry, and is also suitable for field pyrohydrocarbon samples. Preparation and Analysis.

Description of drawings

Fig. 1 is the structural representation of the automatic sample preparation device for pyrohydrocarbon pretreatment of the utility model;

Fig. 2 is the structural representation of sealing cap and sampling device of the present utility model;

Explanation of reference numerals: 1, carbon dioxide adsorption device; 101, thermorelease tube; 102, rubber bowl; 103, sealing cover; 104, tray; 105, lifter; 106, alkali adding device; 107, liquid outlet hole; 108, Groove; 2, heating device; 201, water outlet; 3, cleaning device; 301, water storage tank; 302, water inlet pipe; 303, air compressor; 4, vacuum device; 5, sampling device; 501, sampling tube; 502, sealing plug; 503, sampler.

detailed description

The content of the present utility model will be further elaborated below in conjunction with accompanying drawing and specific embodiment:

As shown in Figure 1, the automatic sample preparation device for pyrohydrocarbon pretreatment of the present invention includes: a carbon dioxide adsorption device 1, a heating device 2, a cleaning device 3, a vacuum device 4, a sampling device 5 and a control device.

Among them, the carbon dioxide adsorption device 1 is used to process the sample to be tested to obtain the processed product, including: a pyrotube 101 , a sealing cover 103 , a rubber bowl 102 , a tray 104 , a lifter 105 and an alkali adding device 106 . Pyrotube 101 is vertically arranged in the inside of heating device 2, has a liquid outlet 107 on its arc-shaped bottom surface, its top is exposed outside the heating device, and its top has a sealing cover 103 to keep it sealed. There is a rubber bowl 102, the upper surface of the rubber bowl 102 is provided with an arc-shaped groove 108 corresponding to the arc-shaped bottom surface of the heat release tube 101, and the diameter of the arc-shaped groove 108 on the rubber bowl 102 is larger than that of the heat release tube 101 The diameter of the rubber bowl 102 is fixed on the tray 104, the tray 104 is located at the bottom of the heating device 2, and the lower surface is connected with a lifter 105; through the rise and fall of the lifter 105, the rise and fall of the rubber bowl 102 can be controlled. When rubber bowl 102 rises, its groove 108 fits with the bottom surface of pyrotube 101, then the bottom of pyrotube 101 is sealed, can react, and sample is processed; When rubber bowl 102 descends, its groove 108 Separated from the bottom surface of the thermal release tube 101, the bottom of the thermal release tube 101 is open, and the liquid or gas in the thermal release tube can be discharged through the liquid outlet; the number of the thermal release tube 101 can be one or more, and its quantity depends on the It is determined by the amount of processed samples. Correspondingly, the number of rubber bowls 102 is the same as the number of thermal release tubes 101. The alkali adding device 106 includes a liquid storage tank and a liquid inlet pipe, one end of the liquid inlet pipe is connected to the liquid storage tank, and the other end passes through the sealing cover and passes into the pyrolysis tube, and the lye in the liquid storage tank is added to the pyrolysis pipe 101 inside.

The heating device 2 can be sealed and is a heatable thermostat. A water outlet 201 is provided at the bottom of its side, and the liquid or gas flowing out from the pyrotube 101 can be discharged through the water outlet 201 .

The cleaning device 3 includes a water storage tank 301, a water inlet pipe 302 and an air compressor 303. One end of the water inlet pipe 302 is connected to the water storage tank 301, and the other end passes through the sealing cover 103 and enters the heat release pipe 101, and the water storage tank 301 The water sent into the thermal release tube 101 is cleaned; the air compressor 303 communicates with the thermal release tube 101 through the pipeline passing through the sealing cover 103, and blows high-pressure air into the thermal release tube.

The vacuum device 4 includes a vacuum pump and a vacuum pipeline that passes through the sealing cover and communicates with the thermorelease tube, and vacuumizes the thermorelease tube.

The sampling device 5 comprises a sampling tube 501 and a sampler 503 (as shown in Figure 2 ), the sampling tube 501 runs through the sealing cap, and its exposed end is plugged tightly with a sealing plug 502, and the sampler 503 extracts the thermal release via the sampling tube. Gas products in the tube.

The control device is not shown in the accompanying drawings, and it may include a controller or computer, which is connected with the switch of the lifter, heating device, air compressor and vacuum pump, and the valve on the water inlet pipe and the liquid inlet pipe through pipelines, To control the automatic operation of each device.

The working process of the utility model device is as follows:

(1) Control the lifter to descend through the control device, so that the rubber bowl is separated from the heat release tube;

(2) Control the cleaning device to clean the carbon dioxide adsorption device, including first washing with water in the water storage tank, and then controlling the air compressor to blow high-pressure air to it; at the same time, controlling the heating The water outlet of the device is opened, and the cleaned liquid is discharged through the water outlet of the heating device;

(3) Control the water outlet of the heating device to close, control the heating device to heat up, dry the carbon dioxide adsorption device, then control the water outlet of the heating device to open, and cool to room temperature;

(4) Control the lifter to rise, make the rubber bowl and the heat release tube fit together, and seal the bottom of the heat release tube;

(5) Open the sealing cover, add the sample to be tested in the thermorelease tube, control the vacuum device to evacuate the thermorelease tube through the control device, then control the water outlet of the heating device to close, and control the heating device to heat up And keep, then control the water outlet of the heating device to open, cool to room temperature;

(6) Adding sodium hydroxide solution into the pyrotube by controlling the alkali adding device through a control device to absorb carbon dioxide to obtain a processed product;

(7) Open the sealing plug, and extract the product obtained after the treatment through a sampler, to obtain final product.

According to GB/T 29173-2012 pyrohydrocarbon determination, gas chromatography is used to analyze the extracted and prepared samples by gas chromatography. Compared with samples prepared manually, the content of hydrocarbon components obtained by analysis of samples prepared by this device is relatively stable. There are phenomena such as low levels caused by air pollution. Using the prior art to prepare the pre-treatment samples of pyro-release hydrocarbons, each group of 12 samples takes about 2 hours; while using the device and method of the utility model to prepare the pre-treatment samples of pyro-release hydrocarbons, it only takes 55 minutes, Great time saver. The utility model has an automatic sample preparation device for pyrohydrocarbon pretreatment, which reduces the transfer of samples and avoids pollution.

It should be noted that the above-mentioned embodiments are only used to explain the present utility model, and do not constitute any limitation to the present utility model. The present invention has been described with reference to typical embodiments, but it is understood that the words which have been used therein are words of description and explanation rather than words of limitation. The utility model can be modified within the scope of the claims of the utility model according to regulations, and the utility model can be revised without departing from the scope and spirit of the utility model.

Claims (9)

1. a kind of heat releases hydrocarbon pre-treatment specimen automatic preparation equipment, including：

Testing sample is handled to obtain the carbon dioxide adsorption device of product；

The heater heated to the carbon dioxide adsorption device；

The cleaning device of cleaning treatment is carried out to the carbon dioxide adsorption device；

The carbon dioxide adsorption device is set to form the vacuum plant of vacuum environment；

Extract and store the sampler of the product obtained after carbon dioxide adsorption device processing；And

The control device of the automatic running of above-mentioned each device is controlled by circuit.

2. device according to claim 1, it is characterised in that the carbon dioxide adsorption device includes：

Heat releases pipe, is vertically arranged inside the heater, is provided with fluid hole on its circular arc bottom surface, its top is exposed Outside heater；

Seal closure, Gai Re release the top of pipe；

Rubber bowl, the lower section of pipe is released positioned at the heat, its upper surface is provided with circle corresponding with the circular arc bottom surface that the heat releases pipe Arc groove；

The rubber bowl, lower surface connection lifter are fixed in pallet, the bottom in the heater, its upper surface；

Lifter, it is connected with the pallet；

Adder-subtractor, including fluid reservoir and feed tube, described feed tube one end connect NaOH solution tank NaOH, and the other end runs through the seal closure The heat is passed through to release in pipe.

3. device according to claim 2, it is characterised in that the diameter of the circular groove on the rubber bowl is more than institute State the diameter that heat releases pipe.

4. the device according to Claims 2 or 3, it is characterised in that when the rubber bowl rises, its groove and the heat The bottom surface fitting of pipe is released, then the heat releases the sealed bottom of pipe；When the rubber bowl declines, its groove releases pipe with the heat Bottom surface separates, then heat releases the bottom opening of pipe.

5. device according to claim 1, it is characterised in that the side bottom of the heater is provided with delivery port.

6. device according to claim 1, it is characterised in that the cleaning device includes：

The water tank that water inlet is cleaned to it in pipe is released to heat, connecting the heat via water inlet pipe releases pipe；

Water inlet pipe, one end connection water tank, the other end are passed through the heat through seal closure and released in pipe；

The air compressor machine that pressure-air is blown into pipe is released to the heat, pipe is released by connecting heat through the pipeline of seal closure.

7. device according to claim 1, it is characterised in that the vacuum plant includes：

Vavuum pump and vacuum line, the pipeline are released pipe with heat through seal closure and connected.

8. device according to claim 1, it is characterised in that the sampler includes：

Probe tube, through seal closure, the one end being exposed is stoppered with sealing-plug；

Sampler, extracted by probe tube and store the hot gaseous product released in pipe.

9. device according to claim 1, it is characterised in that the control device, including controller, its by pipeline with Lifter, heater, the switch of air compressor machine and vavuum pump, and water inlet pipe are connected with the valve on feed tube, to control The automatic running of each device.