Freezing sample crushing device

Abstract

The utility model belongs to the field of rock crushing or crushing, and particularly relates to a freezing sample crushing device. The frozen sample crushing device comprises a sample crushing bin and a sample crushing mechanism for crushing rocks in the sample crushing bin, and further comprises a cooling cup, and a sample crushing part of the sample crushing bin is arranged in the cooling cup; a liquid nitrogen injection port is formed in the cooling cup, and a limiting structure for limiting the movement of the sample crushing bin is also arranged on the cooling cup. The cooling cup is arranged outside the sample crushing bin, liquid nitrogen can be introduced into the cooling cup through the liquid nitrogen injection port so as to cool the sample crushing part of the sample crushing bin, the limiting structure limits movement of the sample crushing bin in the sample crushing process, and it is guaranteed that the sample crushing process is stably carried out under the freezing condition of minus 40 DEG C or below; therefore, the loss of C1-C16 hydrocarbon compounds caused in the normal-temperature sample crushing process is reduced to a great extent.

Description

Technical Field

[0001] The utility model belongs to the field of rock crushing or pulverization, and particularly relates to a freezing sample crushing device. Background Art

[0002] Shale oil refers to petroleum resources in which hydrocarbons are generated by hydrocarbon source rocks, have not undergone migration or have only undergone short-distance primary migration within the source rock, and are stored in organic shale or in sandstones, carbonate rocks and other interbeds that are closely connected and interbedded with it. Due to the characteristics of shale being dense, low-porosity and low-permeability, and the relative density and viscosity of oil being greater than that of gas, it is more difficult to flow underground. The key factor restricting the exploration and development of shale oil is not the reserve of shale oil, but how much movable amount there is in it. At present, pyrolysis parameters such as gaseous hydrocarbon S0, soluble hydrocarbon S1, and pyrolytic hydrocarbon S2 are often used to evaluate the movable amount.

[0003] The pyrolysis parameters are measured by a Rock-Eval pyrolyzer. The peak value of gaseous hydrocarbon S0 reflects the content of C1-C7 gaseous hydrocarbons. The peak value of soluble hydrocarbon S1 is mainly generated by the pyrolysis of C7-C33 hydrocarbon compounds. Among them, the melting points of C1-C16 hydrocarbon compounds are -182°C to 18.1°C, and the boiling points are -161.6°C to 280°C. These hydrocarbon compounds are greatly affected by temperature and are prone to volatilization. When obtaining pyrolysis parameters, according to the provisions of GB / T18602-2012 Rock Pyrolysis Analysis, rock samples (such as shale) need to be pulverized.

[0004] A Chinese utility model patent with an authorization announcement date of May 8, 2018 and an authorization announcement number of CN 207324928 U discloses a rock crushing device, which includes a workbench and a crushing chamber arranged on the workbench. The crushing chamber has a cover body, and a guide groove is arranged on the cover body; a fixing frame is also arranged on the workbench, a hydraulic cylinder is arranged on the fixing frame, the piston rod of the hydraulic cylinder passes through the guide groove and is arranged in the crushing chamber, and a crushing hammer is arranged at the bottom of the piston rod. The hydraulic cylinder, its piston rod and the crushing hammer constitute a sample crushing mechanism, and the sample crushing mechanism is used to crush the rock in the crushing chamber, so as to meet the subsequent analysis and testing requirements.

[0005] The above room-temperature sample crushing device has the following problems when performing pyrolysis analysis of shale movable hydrocarbons: First, during the room-temperature sample crushing process, the C1-C16 hydrocarbon compounds in the shale sample are seriously volatilized, resulting in a decrease in the values of gaseous hydrocarbon S0 and soluble hydrocarbon S1, and further causing an increase in the evaluation error of shale oil and gas; Second, impact crushing of the rock by the crushing hammer will generate local high temperature, accelerating the volatilization of C1-C16 hydrocarbon compounds and further decreasing the measured values of gaseous hydrocarbon S0 and soluble hydrocarbon S1. Content of the Utility Model

[0006] The purpose of the present utility model is to provide a freezing sample crushing device, which solves the problem that the existing conventional sample crushing device crushes shale samples at room temperature, resulting in serious escape of C1-C16 hydrocarbon compounds.

[0007] In order to achieve the above purpose, the technical solution adopted by the present utility model is:

[0008] A freezing sample crushing device includes a sample crushing chamber, and a sample crushing mechanism for crushing the rock in the sample crushing chamber. It further includes a cooling cup. The sample crushing part of the sample crushing chamber is arranged in the cooling cup. The cooling cup is provided with a liquid nitrogen injection port and a limiting structure for restricting the movement of the sample crushing chamber.

[0009] The present utility model belongs to an improved invention. By arranging a cooling cup outside the sample crushing chamber, liquid nitrogen can be introduced into the cooling cup through the liquid nitrogen injection port to cool the sample crushing part of the sample crushing chamber. The limiting structure restricts the movement of the sample crushing chamber during the sample crushing process, ensuring that the sample crushing process proceeds smoothly under the freezing condition below -40°C, thereby greatly reducing the escape of C1-C16 hydrocarbon compounds caused by the sample crushing process at room temperature.

[0010] Preferably, the cooling cup is provided with a liquid nitrogen storage bin connected to the liquid nitrogen injection port. The liquid nitrogen storage bin is provided with cooling holes for the cool air generated by the liquid nitrogen to escape. The cooling cup is further provided with a cool air storage bin communicated with the cooling holes, and the sample crushing chamber is arranged in the cool air storage bin.

[0011] Further preferably, the cooling cup includes a top plate, a bottom plate and a side wall plate. An inner cylinder plate located inside the side wall plate is also connected between the top plate and the bottom plate. There is an annular interval between the inner cylinder plate and the side wall plate. The sample crushing chamber is arranged in the inner cylinder plate. The inner cylinder plate has a cooling section and a non-hole section. The cooling holes are arranged on the cooling section, and the non-hole section and the corresponding cooling cup bottom plate and side wall plate enclose an annular liquid nitrogen storage space.

[0012] More preferably, a cooling plate spaced relatively from the bottom plate is arranged in the annular interval, and the cooling holes are arranged on the cooling plate.

[0013] Preferably, the sample crushing mechanism includes a hammer head and a hammer handle, and the hammer handle is connected with an impact grinding driving mechanism.

[0014] Preferably, the sample crushing chamber is in non-rotating fit with the bottom wall of the cooling cup; the limiting structure includes a non-rotating structure arranged on the bottom wall of the cooling cup.

[0015] Further preferably, the non-rotating structure includes a first square groove or a first square protrusion, and the bottom of the sample crushing chamber is provided with a corresponding second square protrusion or a second square groove.

[0016] More preferably, a support platform is provided on the bottom wall of the cooling cup, and the first square groove or the first square protrusion is provided on the tabletop of the support platform.

[0017] Preferably, the limiting structure further includes a circumferential blocking structure for blocking the upper end circumference of the sample crushing bin; the cooling cup has a top plate, and the circumferential blocking structure includes a sample crushing bin mounting hole provided on the top plate of the cooling cup.

[0018] Further preferably, a flanging is provided at the top of the sample crushing bin, a sealing groove corresponding to the flanging of the sample crushing bin is provided on the top plate surface around the sample crushing bin mounting hole, and a sealing ring is provided in the sealing groove; the sample crushing bin has a sealing cover, and a through hole for a corresponding component of the sample crushing mechanism to pass through is provided on the sealing cover. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 is a schematic structural diagram of the freezing sample crushing device according to an embodiment of the present invention;

[0020] Figure 2 is Figure 1 a schematic structural diagram of the sample crushing bin in

[0021] Figure 3 is Figure 1 a schematic structural diagram of the cooling cup in

[0022] Figure 4 is Figure 1 a schematic structural diagram of the support platform in

[0023] Figure 5 is Figure 1 a schematic structural diagram of the sealing cover of the sample crushing bin in

[0024] Among them, 1-sample crushing bin, 100-barrel body, 101-barrel bottom, 102-square boss, 103-flanging;

[0025] 2-cooling cup; 20-liquid nitrogen storage bin, 200-cooling holes; 21-cool air storage bin; 22-top plate, 220-sample crushing bin mounting hole, 221-sealing groove, 222-sealing ring; 23-bottom plate; 24-side wall plate; 25-inner cylinder plate; 26-liquid nitrogen injection port; 27-annular cooling plate; 28-support platform, 280-support column, 281-round platform, 282-threaded hole, 283-square groove, 284-fixing bolt; 29-pressure relief valve.

[0026] 3-rock sample;

[0027] 4-liquid nitrogen tank, 40-liquid nitrogen filling pipeline, 41-liquid nitrogen filling switch;

[0028] 5-sealing cover, 50-insertion section, 51-cover top, 52-through hole;

[0029] 6 - Impact mill, 60 - Hammer handle, 61 - Hammer head;

[0030] 7 - Support; 70 - Base, 700 - Groove, 701 - Square hole, 702 - Round hole; 71 - Support rod, 710 - Nut, 711 - Tooth-shaped section; 72 - Lifting device, 720 - Handle. Detailed implementation mode

[0031] The technical concept of the present utility model is to place the sample crushing chamber in the cooling cup, and add liquid nitrogen to the cooling cup to make the sample crushing chamber in a freezing environment below -40°C; limit the movement of the sample crushing chamber through the limiting structure to improve the stability and safety during the sample crushing process, so as to realize the sample crushing of hydrocarbon source rocks such as shale under ultra-low temperature freezing conditions, reduce the escape loss of C1-C16 hydrocarbon compounds during the sample crushing process, and further improve the accuracy of shale mobile hydrocarbon evaluation.

[0032] Furthermore, the present utility model constructs a liquid nitrogen storage chamber and a cold air storage chamber, and uses the cold air generated by the liquid nitrogen to cool the sample crushing chamber. On the premise of meeting the freezing conditions, the amount of liquid nitrogen used is reduced, the safety during the sample crushing process is improved, and the operator is prevented from suffering frostbite.

[0033] Furthermore, by constructing a rotation stopping structure on the bottom wall of the cooling cup and a circumferential stopping structure for stopping the circumference of the upper end of the sample crushing chamber, the structure of the freezing sample crushing device can be further simplified, and the stability and reliability of the device during the sample crushing process can be improved.

[0034] The following combines specific embodiments to elaborate on the implementation process of the present utility model in detail.

[0035] The freezing sample crushing device of this embodiment, as Figure 1 shown, includes a sample crushing chamber 1, a cooling cup 2 and a sample crushing mechanism.

[0036] The rock sample 3 is crushed inside the sample crushing chamber 1. There is no special limitation on the shape of the sample crushing chamber 1. For example, it can be cylindrical, cup-shaped with a larger upper part and a smaller lower part, etc. The sample crushing chamber 1 can be made of heat-conducting and corrosion-resistant materials, such as stainless steel. In this embodiment, as Figure 2 shown, the sample crushing chamber 1 includes a cylindrical barrel body 100 and a mortar-shaped barrel bottom 101 connected to the lower end of the cylindrical barrel body. The bottom of the mortar-shaped barrel bottom 101 is connected with a square boss 102 extending downward, and the square boss 102 is within the downward projection range of the cylindrical barrel body 100; a flange 103 is provided at the top of the cylindrical barrel body 100.

[0037] The cooling cup 2 mainly provides a cryogenic freezing environment below -40°C for the sample crushing part of the sample crushing bin 1. The sample crushing part of the sample crushing bin 1 is the place where sample crushing is realized, such as the part below the middle of the cylindrical sample crushing bin 1. At least the sample crushing part of the sample crushing bin 1 should be placed in a cryogenic freezing environment below -40°C, or most or all of the sample crushing bin 1 can be placed in a cryogenic freezing environment below -40°C.

[0038] A liquid nitrogen storage bin 20 and a cool air storage bin 21 are provided on the cooling cup 2. A heat dissipation hole 200 is provided on the liquid nitrogen storage bin 20, and the heat dissipation hole communicates with the cool air storage bin 21. The sample crushing bin 1 is arranged in the cool air storage bin 21. The liquid nitrogen storage bin 20 is used to store liquid nitrogen. The cool air generated by the liquid nitrogen can enter the cool air storage bin 21 through the heat dissipation hole 200 and cool the cooling cup 2 therein. Adopting this design can not only meet the low-temperature freezing requirements of the cooling cup, but also reduce the consumption of liquid nitrogen and improve the safety during the use of liquid nitrogen.

[0039] As Figure 3 shown, the cooling cup 2 has a round cup-shaped structure, including a top plate 22, a bottom plate 23, and a cylindrical side wall plate 24 connected between the top plate 22 and the bottom plate 23. An inner cylinder plate 25 located inside the cylindrical side wall plate 24 is also connected between the top plate 22 and the bottom plate 23. There is an annular interval between the inner cylinder plate 25 and the cylindrical side wall plate 24. The inner cylinder plate 25 has a perforated section and a non-perforated section connected to the lower end of the perforated section. A large number of heat dissipation holes 200 are provided on the perforated section, and there are no heat dissipation holes on the non-perforated section, which acts as a baffle to prevent liquid nitrogen from passing through. The non-perforated section and the corresponding parts on the cylindrical side wall plate 24 and the bottom plate 23 enclose an annular liquid nitrogen storage space. A liquid nitrogen injection port 26 is provided on the cylindrical side wall plate 24 corresponding to the liquid nitrogen storage bin 20. The liquid nitrogen injection port 26 is connected to a liquid nitrogen tank 4 through a liquid nitrogen filling pipeline 40. A liquid nitrogen filling switch 41 is provided on the liquid nitrogen tank 4.

[0040] In this embodiment, an annular heat dissipation plate 27 adapted to the annular interval is also provided in the annular interval between the inner cylinder plate 25 and the cylindrical side wall plate 24. The annular heat dissipation plate 27 is connected to the non-perforated section of the inner cylinder plate 25 and is arranged in parallel and spaced from the bottom plate 23 of the cooling cup. A large number of heat dissipation holes 200 are provided on the annular heat dissipation plate 27. When injecting liquid nitrogen into the liquid nitrogen storage bin 20 through the liquid nitrogen injection port, the liquid level of the liquid nitrogen should be below the annular heat dissipation plate 27. The annular heat dissipation plate 27 can reduce the disturbance of the liquid level of the liquid nitrogen during the sample crushing process, reduce the splashing of liquid nitrogen droplets towards the top plate 22 of the cooling cup, and further improve the safety during the sample crushing process.

[0041] In other embodiments, the liquid nitrogen storage bin 20 and the cool air storage bin 21 can adopt other forms, such as Figure 3In this case, the inner cylinder plate 25 is not used, and an annular partition is used at the position of the annular cooling plate 27 to divide the inner cavity of the cooling cup 2 into upper and lower cavities. The lower cavity forms a liquid nitrogen storage bin 20, and the upper cavity forms a cool air storage bin 21. Cooling holes 200 are provided on the annular partition, so that the cooling cup 2 located in the cool air storage bin 21 can be cooled by the cool air generated by the liquid nitrogen.

[0042] A limiting structure for restricting the movement of the sample crushing bin 1 is provided on the cooling cup 2. Since the crushing of rocks in the sample crushing bin 1 is generally accompanied by actions such as impact and grinding, the limiting structure can restrict the movement of the sample crushing bin during the above sample crushing actions, thereby improving the smoothness and effectiveness of the sample crushing process. By providing an anti-rotation structure on the cooling cup bottom plate 23 that cooperates with the sample crushing bin 1 and providing a circumferential blocking structure on the cooling cup top plate 22 that blocks the upper end circumference of the sample crushing bin 1, the limiting effect on the cooling cup can be well achieved.

[0043] As Figure 1 and Figure 4 shown, a support platform 28 installed on the cooling cup bottom plate 23 is provided in the inner cylinder plate 25. The cross-section of the support platform 28 is T-shaped, including a support column 280 and a frustum 281 connected to the top end of the support column 280. A threaded hole 282 for installing the support platform 28 on the cooling cup bottom plate 23 is provided on the support column 280, and a square groove 283 adapted to the square boss 102 at the bottom end of the sample crushing bin 1 is provided on the frustum 281. When the square boss 102 at the bottom end of the sample crushing bin 1 is inserted into the square groove 283 on the support platform 28, the anti-rotation fit of the sample crushing bin 1 relative to the cooling cup bottom plate 23 is achieved. In other implementation cases, the support platform 28 may not be used, and the square groove 283 may be directly provided on the cooling cup bottom plate 23 to adjust the vertical dimension of the sample crushing bin 1, so that the sample crushing bin 1 is directly in anti-rotation fit with the cooling cup bottom plate 23.

[0044] A sample crushing bin installation hole 220 is provided on the cooling cup top plate 22. The barrel part of the sample crushing bin 1 passes through the sample crushing bin installation hole 220 and is installed on the anti-rotation structure on the cooling cup bottom plate 23, and the circumferential blocking of the upper barrel of the sample crushing bin 1 is achieved by the hole wall of the sample crushing bin installation hole 220. Figure 1 、 Figure 3 In this case, a sealing groove 221 is also provided between the sample crushing bin flange 103 and the corresponding surface of the cooling cup top plate 22, and a sealing ring 222 adapted to the sample crushing bin flange 103 is provided in the sealing groove 221, so that the sealing between the sample crushing bin 1 and the cooling cup 2 can be achieved, and the cool air in the cool air storage bin 21 can be prevented from escaping. A pressure relief valve 29 is also provided on the cooling cup top plate 22. The pressure relief valve 29 can relieve pressure when the pressure in the cooling cup 2 reaches a certain level, thereby improving safety.

[0045] Furthermore, as Figure 5As shown in the figure, the sample crushing bin 1 is also provided with a sealing cover 5. The cross-section of the sealing cover 5 is T-shaped, including an insertion section 50 and a cover top 51 connected to the insertion section 50. A through hole 52 penetrating the cover top 51 and the insertion section 50 is provided in the middle of the sealing cover 5, and the corresponding component of the sample crushing mechanism passes through the through hole 52. The sealing cover 5 ensures the sealing performance of the sample crushing bin 1 during the freezing sample crushing process, reducing the escape of cold air and other components during the sample crushing process.

[0046] The sample crushing mechanism is used to crush the rock sample 3 in the sample crushing bin 1. The sample crushing mechanism can adopt various forms. It can be an impact crushing device that uses a reciprocating element to achieve crushing, or it can be an impact grinder 6 that can perform both impact and grinding simultaneously. The working mechanism of the impact grinder 6 is the same as that of an impact drill. It uses the hammering and rotational grinding actions of the hammer head of the impact grinder 6 to achieve efficient crushing of the rock sample 3.

[0047] Figure 1 In it, the sample crushing mechanism includes an impact grinder 6. The impact grinder includes a hammer handle 60 and a hammer head 61. The hammer handle 60 passes through the through hole 52 of the sealing cover 5 of the sample crushing bin, and the hammer handle 60 is connected to the impact grinding drive mechanism of the impact grinder 6 to drive the hammer head 61 to perform impact grinding and crushing on the rock sample 3. The hammer head 61 is in the shape of a garlic hammer, and the outer diameter of the hammer head 61 is slightly smaller than the inner diameter of the sample crushing bin 1. The hammer head 61 has a hemispherical hammer surface adapted to the garlic mortar-shaped bottom 101 of the sample crushing bin 1.

[0048] The freezing sample crushing device also includes a bracket 7. The bracket 7 is used to fix the sample crushing mechanism and the cooling cup 2. As Figure 1 shown in the figure, the bracket 7 includes a base 70 and a support rod 71 fixedly connected to the base 70. An elevating device 72 is connected to the support rod 71, and the elevating device 72 is connected to the above-mentioned sample crushing mechanism. During operation, the height of the sample crushing mechanism is adjusted through the elevating device 72 to a suitable height.

[0049] The base 70 is a square plate with a downward groove 700. The lower end of the support rod 71 is provided with a thread. The lower end of the support rod 71 passes through the square hole 701 on the base 70 and enters the groove 700, and the fixing of the support rod 71 is achieved through a matching nut 710. The upper end of the support rod 71 has a toothed section 711. The elevating device 72 includes an elevating frame and a handle 720 that cooperate with the toothed section 711. The side of the elevating frame away from the support rod 71 is connected to the impact grinder 6. A circular hole 702 is provided in the middle of the base 70, and a fixing bolt 284 passes through the circular hole 702 and is threadedly connected to the threaded hole 282 of the support table 28.

[0050] The process of freezing and crushing samples using the above-mentioned device is as follows: Place the sample crushing chamber 1 into the cooling cup 2, open the liquid nitrogen filling switch 41 of the liquid nitrogen tank 4, and fill the liquid nitrogen storage chamber 20 in the cooling cup 2 with liquid nitrogen through the liquid nitrogen filling pipeline 40. The cold air generated by the liquid nitrogen quickly cools down the sample crushing chamber 1 through the cooling holes 200. Put an appropriate amount of lacustrine shale sample into the sample crushing chamber 1, rotate the handle 720 of the rotary lifting device 72 to adjust the impact grinder 6 to a suitable position, start the switch of the control circuit to hammer and grind the lacustrine shale sample. After the lacustrine shale sample is crushed, raise the impact grinder 6, and take out the crushed lacustrine shale sample for pyrolysis analysis and testing.

[0051] Compare the S1 values of the soluble hydrocarbons in the freezing and crushing samples and the normal-temperature crushing samples using the freezing and crushing device of the present utility model. The S1 value of the soluble hydrocarbons in the freezing and crushing samples is significantly higher than that in the normal-temperature crushing samples, which proves that the device can effectively reduce the volatilization of C1-C16 hydrocarbon compounds during the sample crushing process of lacustrine shale samples, thus creating good conditions for the accurate evaluation of the content of movable hydrocarbons.

Claims

1. A freezing sample crushing device, comprising a sample crushing chamber and a sample crushing mechanism for crushing rocks in the sample crushing chamber, characterized in that: It also includes a cooling cup, in which the sample crushing part of the sample crushing chamber is arranged; the cooling cup is provided with a liquid nitrogen injection port and a limiting structure for limiting the movement of the sample crushing chamber.

2. The freezing sample crushing device according to claim 1, characterized in that: The cooling cup is provided with a liquid nitrogen storage bin connected to the liquid nitrogen injection port, and the liquid nitrogen storage bin is provided with a cooling hole for the cool air generated by the liquid nitrogen to escape outward; the cooling cup is also provided with a cool air storage bin connected to the cooling hole, and the sample crushing bin is arranged in the cool air storage bin.

3. The freezing and crushing device according to claim 2, characterized in that: The cooling cup includes a top plate, a bottom plate and a side wall plate, and an inner cylinder plate located on the inner side of the side wall plate is connected between the top plate and the bottom plate, and an annular gap is provided between the inner cylinder plate and the side wall plate; the sample crushing bin is arranged in the inner cylinder plate, and the inner cylinder plate has a cooling section and a non-porous section, and the cooling section is provided with the cooling holes, and the non-porous section and the corresponding cooling cup bottom plate and side wall plate form an annular liquid nitrogen storage space.

4. The freezing and crushing device according to claim 3, characterized in that: A cooling plate is provided in the annular space and is spaced relative to the bottom plate. The cooling holes are provided on the cooling plate.

5. The freezing and crushing sample device according to claim 1, characterized in that: The sample crushing mechanism includes a hammer head and a hammer handle, and the hammer handle is connected to an impact grinding drive mechanism.

6. The freezing and crushing sample device according to claim 1 or 5, characterized in that: The sample crushing chamber is anti-rotationally matched with the bottom wall of the cooling cup; the limiting structure includes an anti-rotation structure arranged on the bottom wall of the cooling cup.

7. The freezing and crushing sample device according to claim 6, characterized in that: The anti-rotation structure includes a first square groove or a first square protrusion, and the bottom of the sample crushing chamber is provided with a corresponding second square protrusion or a second square groove.

8. The freezing and crushing sample device according to claim 7, characterized in that: A support platform is provided on the bottom wall of the cooling cup, and the first square groove or the first square protrusion is provided on the surface of the support platform.

9. The freezing and crushing sample device according to claim 6, characterized in that: The limiting structure also includes a circumferential stopping structure for stopping the upper end of the sample crushing bin in the circumferential direction; the cooling cup has a top plate, and the circumferential stopping structure includes a sample crushing bin mounting hole arranged on the top plate of the cooling cup.

10. The freezing and crushing sample device according to claim 9, characterized in that: The top of the sample crushing bin is provided with a flange, and the top plate surface around the sample crushing bin mounting hole is provided with a sealing groove corresponding to the sample crushing bin flange, and a sealing ring is provided in the sealing groove; the sample crushing bin has a sealing cover, and the sealing cover is provided with a through hole for the corresponding components of the sample crushing mechanism to pass through.

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