High-temperature closed reaction kettle resistant to strong acid and strong base

Abstract

The application provides a high-temperature closed reaction kettle resistant to strong acid and strong base, which comprises a cylindrical kettle body, symmetrically arranged upper and lower kettle covers, and a gold pressure-bearing pipe arranged in the cylindrical kettle body; the upper and lower kettle covers and the cylindrical kettle body are connected through threads; and the gap between the gold pressure-bearing pipe and the cylindrical kettle body is filled with quartz sand. The reaction kettle has the advantages of simple structure, controllable cost and higher high-temperature and high-pressure resistance than existing equipment.

Description

Technical Field

[0001] This invention relates to the field of geochemical experimental apparatus technology, and in particular to a high-temperature sealed reaction vessel resistant to strong acids and alkalis. Background Technology

[0002] The study of deep Earth mineralization processes and mechanisms is one of the current trends in metallogeny. Due to the complexity of natural geological environments, many geological phenomena and geochemical data often have multiple interpretations, making traditional ore deposit studies insufficient to address complex natural systems. Therefore, high-temperature experiments, which primarily simulate diagenetic and mineralization processes and physicochemical conditions, can identify key controlling factors in ore deposit genesis by controlling variables. High-temperature and high-pressure experiments play a crucial role in simulating crustal environments and studying mineral genesis and ore deposit formation processes. They are not only an important approach to solving a series of key scientific problems related to mineralization but also an inherent requirement for the further development of ore deposit geology.

[0003] The temperature of magma typically ranges from 700 to 1200℃, but varies depending on the composition: basaltic magma is hotter, reaching 1025–1225℃; andesitic magma is 900–1000℃; and acidic magma is the coldest, generally 735–890℃. Therefore, high-temperature experimental studies of diagenesis and mineralization processes usually employ expensive piston cylinders. However, most of this type of equipment in my country is imported, resulting in high costs not only for the equipment itself and its components but also for operation and maintenance.

[0004] Traditional titanium alloy autoclaves soften at temperatures above 350°C, but by changing the material to high-temperature stainless steel, they can withstand temperatures up to 1200°C. However, stainless steel will react with water under high-temperature conditions.

[0005] Therefore, designing a high-temperature reactor with extremely strong resistance to strong acids and alkalis is of great importance and significance for studying the interactions between various substances deep within the Earth, the material cycle in the deep Earth, and the energy flow. Summary of the Invention

[0006] This invention provides a high-temperature sealed reactor resistant to strong acids and alkalis, which, when combined with a muffle furnace, enables non-in-situ high-temperature and high-pressure diagenetic and mineralization geochemical experiments.

[0007] A high-temperature sealed reactor resistant to strong acids and alkalis includes: a cylindrical reactor body, an upper reactor cover and a lower reactor cover arranged symmetrically, and a gold pressure-bearing pipe disposed inside the cylindrical reactor body; the upper reactor cover, the lower reactor cover and the cylindrical reactor body are connected by threads; the gap between the gold pressure-bearing pipe and the cylindrical reactor body is filled with quartz sand.

[0008] Optionally, the cylindrical vessel body, upper and lower vessel covers are both made of high-temperature 310S stainless steel. The upper and lower vessel covers are modified from bolts. The inner surface of the cylindrical vessel body is tapped with internal threads, and the surface of the pressure-bearing column in the center of the upper and lower vessel covers is tapped with external threads. Preferably, the upper and lower vessel covers are modified from M12 metric bolts with a pitch of 1.75mm. The threaded connection between the pressure-bearing column and the cylindrical vessel body forms a sealed reaction vessel that can withstand a certain pressure.

[0009] Optionally, the gold pressure tube has an inner diameter of 3-3.5mm and an outer diameter of 4mm. Gold has a melting point of 1064℃, therefore this equipment can conduct geochemical experiments below 1000℃. Gold has good ductility, therefore, the gold pressure tube will not rupture within a certain experimental pressure range. Gold is chemically extremely stable, thus possessing strong corrosion resistance. These properties of gold determine that sealing the gold pressure tube not only prevents reactants and reaction solutions from reacting with stainless steel, but it can also withstand considerable pressure.

[0010] Optionally, the quartz sand filler is a uniform 1:1 mixture of <200 mesh and 40-50 mesh particles. Mixing different particle sizes not only makes the filling more compact, but also, because the quartz sand filler undergoes high-temperature expansion, both the inner and outer walls of the pressure-bearing tube within the quartz sand filler are subjected to a certain pressure. Therefore, the quartz sand filler also has the function of balancing internal and external pressure.

[0011] Optionally, the high-temperature sealed reactor can withstand a high temperature of 1000℃ and an internal pressure of 57MPa simultaneously.

[0012] Furthermore, the present invention also provides an experimental method for carrying out rock-rock reactions using a high-temperature and high-pressure reactor, comprising:

[0013] Step S1: Place the known weight of rock reactant and pure water into a gold tube that is welded at one end, and use a micro laser spot welding machine to weld the other end.

[0014] Step S2: Insert the pressure-bearing column on the lower kettle cover into the cylindrical kettle body and tighten it with threads. Then pour in a certain thickness of quartz sand filler. After placing the sealed gold pressure-bearing tube into the kettle body, pour in quartz sand filler again so that the gold pressure-bearing tube is completely wrapped by the quartz sand filler. Finally, put on the upper kettle cover and tighten the reactor to prevent the gold tube from bursting at high temperature.

[0015] Step S3: Place the high-temperature and high-pressure reactor into a high-temperature device to conduct a rock-rock reaction experiment.

[0016] For a gold-filled pressure tube, the ratio of the volume of pure water inside to the total volume of the gold-filled pressure tube excluding rock reactants is the filling degree of the reaction chamber (fill degree inside the gold tube = V). 水 / (V 总体积 -V岩石样品 )).

[0017] The beneficial effects of the technical solution provided by this invention include at least the following:

[0018] The experimental device of this invention has a simple structure, controllable production cost, can withstand high temperature and high pressure significantly higher than the load-bearing capacity of existing equipment, and has excellent corrosion resistance. It can carry out experimental research on diagenesis and mineralization processes within a wide temperature and pressure range. Attached Figure Description

[0019] To more clearly illustrate the technical solutions in the embodiments of the present invention, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0020] Figure 1 This is a schematic diagram of the high-temperature sealed reactor assembly of the present invention, wherein 1-upper reactor cover; 2-cylindrical reactor body; 3-lower reactor cover; 4-quartz sand packing; 5-gold pressure-bearing pipe;

[0021] Figure 2 The dimensions of the high-temperature sealed reactor of the present invention are shown in Figure 1, wherein (A) is the cylindrical reactor body, (B) is the reactor lid, and (C) is the gold pressure-bearing pipe.

[0022] Figure 3 The temperature and pressure curve inside the gold pressure pipe during the experiment with a pure water filling degree of 0.1 in this invention;

[0023] Figure 4 The temperature and pressure curve inside the gold pressure tube during the experiment with a pure water filling degree of 0.05 according to the present invention. Detailed Implementation

[0024] To make the objectives, technical solutions, and advantages of the present invention clearer, the technical solutions of the present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.

[0025] A high-temperature sealed reactor consists of a cylindrical vessel body, upper and lower vessel covers, and a sealed gold pressure-bearing pipe.

[0026] The cylindrical vessel body and upper and lower vessel covers are made of high-temperature stainless steel 310S. The upper and lower vessel covers are modified from M12 metric bolts, and the cylindrical vessel body is tapped with matching internal threads. The two fit tightly together to form a relatively sealed reaction vessel. The gold pressure-bearing pipe and quartz sand packing, which are sealed by a micro-welding machine, are placed into the high-pressure vessel. The upper and lower vessel cap screws are tightened to ensure that the pressure-transmitting medium, quartz sand, and the pressure-bearing gold pipe are in close contact.

[0027] In the specific design, the vessel body is a cylindrical hollow structure with an inner diameter of 10.1 mm, an outer diameter of 20 mm, and a height of 55 mm. Both ends are tapped with M12 internal threads with a thread depth of 15 mm. The vessel cap screw, modified from an M12 hexagonal screw, is 20 mm long, with a diameter of 17.7 mm and a head thickness of 12 mm. The hexagonal hole depth is 6 mm, and the cross-side depth is 10 mm. The thread pitch on both the vessel body and the cap is 1.75 mm. The gold pressure-bearing tube can be customized to different sizes according to different experimental requirements, with a maximum outer diameter of 10.5 mm and no requirement for the inner diameter. The gold pressure-bearing tube used in this experiment has an inner diameter of 3.5 mm and an outer diameter of 4 mm. The quartz sand filler material outside the gold tube has a particle size of 40-50 mesh, is ground in batches, passed through a 200-mesh sieve, and the quartz sand with a particle size <200 mesh is selected. The two are then uniformly mixed and used as the pressure transmission medium.

[0028] According to the above design scheme, we fabricated the experimental device and conducted preliminary experiments to verify its sealing and pressure-bearing performance. The experimental steps are as follows:

[0029] Step 1: First, use a microscopic laser spot welder to seal one end of the gold tube. Then, fill the tube with distilled water and weigh it to calculate the total volume of the gold tube as 0.2 cm³. 3 After drying the gold tube, place 0.30g of rock powder and a small amount of distilled water (0.01g). (At this point, the sample's water content is approximately 3.3%.) The degree of pure water filling in the gold pressure tube varies depending on the density of the rock; for example, phosphate rock has a density of 3g / cm³. 3 At this point, the formula for calculating the pure water filling degree inside the gold pressure tube is (V_water / (V_total volume - V_rock sample) = 0.01 / (0.2 - 0.3 / 3) = 0.1). The pure water filling degree of 0.1 in the entire sample system is then the density of the system excluding the rock. After pressing the open end of the gold tube tightly, it is sealed using a micro-laser spot welding machine.

[0030] Step 2: Insert the pressure-bearing column on the lower vessel cover into the cylindrical vessel body and tighten it with the thread. Pour in 3mm thick quartz sand filler. Insert the sealed gold pressure-bearing tube into the center of the vessel body and fill it with quartz sand filler so that the pressure-bearing gold tube is completely wrapped by the quartz sand filler. Finally, put on the upper vessel cover and tighten the reactor.

[0031] Step 3: Place the entire sealed reactor in a muffle furnace and heat it to 1000°C for 2 hours, then hold it at that temperature for 1 hour. After the entire heating and holding process is completed, slowly cool the reactor (to room temperature in about 3 hours).

[0032] Step 4: After opening the device, weigh the entire gold pressure-bearing tube and compare it with the weighing result of the sample tube that was welded and sealed before the experiment. If the mass remains unchanged, it indicates that the gold pressure-bearing tube has not leaked.

[0033] Step 5, according to the equation of state for the pure water isochoric system H2O calculated from the NIST Chemistry WebBook and SRD website, the internal pressure of the system at 1000℃ is 57 MPa. Figure 3 , Figure 4 At high temperatures, H2O will react with the rock, reducing the system density. Therefore, the internal pressure that the gold pressure pipe must withstand should be lower than the calculated value.

[0034] The above results demonstrate that this high-temperature sealed reactor can withstand an internal pressure of approximately 57 MPa and a temperature of approximately 1000 °C, far exceeding that of commonly used titanium alloy reactors. Furthermore, this reactor does not react with any system, thus possessing a wide experimental range. Therefore, this reactor can be used to conduct experimental studies on various diagenetic and mineralization processes within a broad temperature and pressure range. The experimental cost is also significantly reduced compared to previous experimental equipment.

[0035] The above description is merely a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention should be included within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.

Claims

1. A high-temperature sealed reaction vessel resistant to strong acids and alkalis, characterized in that, include: The vessel is cylindrical, with symmetrically arranged upper and lower lids, and a gold pressure-bearing pipe inside the cylindrical vessel. During use, both ends of the gold pressure-bearing pipe are welded and sealed. The upper and lower lids are connected to the cylindrical vessel by threads. The gap between the gold pressure-bearing pipe and the cylindrical vessel is filled with quartz sand.

2. The high-temperature sealed reactor according to claim 1, characterized in that, The cylindrical vessel body, with both the upper and lower lids made of high-temperature 310S stainless steel, is modified from bolts. The inner surface of the cylindrical vessel body is tapped with internal threads, and the surface of the pressure-bearing column in the middle of the upper and lower lids is tapped with external threads.

3. The high-temperature sealed reactor according to claim 2, characterized in that, The upper and lower lids were modified from M12 metric bolts with a pitch of 1.75 mm.

4. The high-temperature sealed reactor according to claim 1, characterized in that, The gold pressure pipe has an inner diameter of 3-3.5 mm and an outer diameter of 4 mm.

5. The high-temperature sealed reactor according to claim 1, characterized in that, The quartz sand filler is a 1:1 uniform mixture of <200 mesh and 40-50 mesh particles.

6. The high-temperature sealed reactor according to claim 1, characterized in that, The high-temperature sealed reactor can withstand a high temperature of 1000 ℃ and an internal pressure of 57 MPa at the same time.

7. An experimental method for conducting rock-rock reactions using the high-temperature closed reactor described in any one of claims 1-6, comprising: Step S1: Place the known weight of rock reactant and pure water into a gold tube that is welded at one end, and use a micro laser spot welding machine to weld the other end. Step S2: Insert the pressure-bearing column on the lower kettle cover into the cylindrical kettle body and tighten it with threads. Then pour in a certain thickness of quartz sand filler. After placing the sealed gold pressure-bearing tube into the kettle body, pour in quartz sand filler again so that the gold pressure-bearing tube is completely wrapped by the quartz sand filler. Finally, put on the upper kettle cover and tighten the reactor to prevent the gold tube from bursting at high temperature. Step S3: Place the high-temperature and high-pressure reactor into a high-temperature device to conduct a rock-rock reaction experiment.

Images