A modified alumina carrier batch production device

Abstract

The present invention belongs to the technical field of inorganic chemical equipment, specifically a modified alumina carrier batch production device, including a salt solution preparation tank, an aging reactor, a filter plate, a peristaltic pump, a delivery pump, a pipeline high shear dispersion reactor, and a high-pressure atomizing spray gun. The device of the present invention adopts spray drop addition combined with a pipeline high shear dispersion reactor to control the coprecipitation reaction process, eliminates concentration polarization, strengthens the contact between metal salt droplets and alkali solution, can make the pH value of each area inside the alkali solution consistent, homogenizes the nucleation environment, improves the quality consistency of the product, and avoids particle agglomeration. The present invention can integrate the process of precipitation, aging, aging, solid-liquid separation, and drying in a set of devices, solves the problems of complicated steps, discontinuous operation requiring to be carried out in multiple equipment, long synthesis cycle, low production capacity, and difficulty in realizing automation, reduces labor intensity, and saves labor costs.

Description

Technical Field

[0001] The invention belongs to the technical field of inorganic chemical equipment, in particular to a device for mass production of modified alumina carriers. Background Art

[0002] Monopropellant propulsion technology is widely used in attitude and orbit control systems of various spacecraft such as rockets, spacecrafts, and satellites. It is one of the important indicators of the development level of aerospace technology in a country or region. Iridium-based catalysts represented by Ir / Al2O3 are the most commonly used catalysts for monopropellant thrusters, and a large amount of iridium is carried on various types of monopropellant catalysts. However, iridium is a rare precious metal and advanced material. There are few mineral deposits in the world and they are becoming increasingly depleted. In recent years, the price has soared (from more than 200,000 yuan / kg to nearly 1.5 million yuan / kg). Therefore, it is urgent to carry out research on non-iridium catalyst technology to replace iridium with relatively cheap and abundant active metal materials. At present, existing studies have tried to replace Ir with Ru and load it on alumina carriers to prepare Ru / Al2O3 catalysts. Although the non-iridium monopropellant catalyst is basically equivalent to iridium-based catalysts in terms of startup activity, chamber pressure decay rate and chamber pressure roughness, it is found that the alumina carrier loaded with Ru has sintering and crushing problems after long-term use, and the catalyst cannot meet the requirements of engineering applications in terms of service life. On the other hand, since hydrazine is highly toxic and seriously endangers the health of related personnel, at present, the monopropellant propulsion system is no longer limited to the traditional hydrazine liquid propellant. High-energy, green and non-toxic propellants such as hydroxylamine nitrate (HAN) propellant and ammonium dinitramide (ADN) propellant are also used in the monopropellant propulsion system. Compared with hydrazine, the adiabatic decomposition temperature of ammonium dinitramide or hydroxylamine nitrate is as high as 1300℃, which is much higher than the adiabatic decomposition temperature of hydrazine propellants (about 900℃). The maximum use temperature of the traditional monopropellant carrier-Al2O3 cannot exceed 1200℃, otherwise, the catalyst will be deactivated due to the high-temperature crystallization and volume shrinkage of the carrier. Therefore, improving the high temperature resistance of alumina carrier is the key to the engineering application of non-iridium catalysts.

[0003] At present, modifying alumina with elements such as Si, Ca, Ba, and La is an important means to improve the heat resistance and stability of alumina carriers. The modified elements are dispersed in the alumina lattice, which can inhibit the diffusion of elements on the surface of alumina and control the growth of alumina grains. Commonly used methods for preparing modified alumina include mechanical mixing, coprecipitation, sol-gel, reverse microemulsion, and template. The mechanochemical preparation process requires the use of high-energy consumption equipment, and the sol-gel, reverse microemulsion, and template preparation processes require the use of expensive organic aluminum salts and a large amount of organic solvents. The coprecipitation method uses relatively cheap soluble aluminum salts such as aluminum nitrate and aluminum sulfate and industrial alkali materials such as sodium hydroxide, ammonia or ammonium carbonate as raw materials. It has the advantages of cheap and easy-to-obtain raw materials, energy-saving and environmentally friendly preparation process, and no use of organic reagents that pollute the environment. It is the optimal technical route for achieving mass production of modified alumina. The process of preparing modified alumina carrier by coprecipitation is: first, dissolve the soluble salt of the modifying element and soluble aluminum salt such as aluminum nitrate or aluminum sulfate in water to prepare a mixed salt solution, dissolve sodium hydroxide, ammonia water or (NH3)2CO3 in water to prepare an alkaline solution, and then add the mixed salt solution dropwise to the alkaline solution to generate a modified alumina precursor precipitate. The prepared modified alumina precursor precipitate is subjected to aging, solid-liquid separation, drying, molding, and roasting to obtain a modified alumina carrier. Since the precipitation reactions of various metal ions in the mixed salt solution occur simultaneously at the same time and in the same space, the hydroxide precipitate formed can theoretically achieve atomic-level mixing. However, affected by the mass transfer rate, the droplet size and the degree of homogenization of the alkaline solution system are important factors affecting the coprecipitation process. When a mixed salt solution containing multiple metal cations is added to an alkaline solution, a large amount of hydroxide precipitation is generated on the surface of the droplets at the moment of contact. If the droplets are too large, the consumed cations will not have time to diffuse to the area, and concentration polarization will appear on the surface of the droplets. If the stirring speed of the alkaline solution is limited, the OH consumed in the alkaline solution will - If the ions cannot be replenished in time, the pH value of the precipitation area will drop. Since the solubility product of each metal salt to produce hydroxide precipitates is different, the pH value required for precipitation is also different. This concentration polarization and the fluctuation of the pH value of the alkali solution will cause the precipitate to segregate, and a co-precipitation product with uniform composition cannot be obtained.

[0004] In order to achieve a certain production efficiency and scale, the existing industrial coprecipitation reaction devices often use a large flow rate and high flow rate drop mode in addition to a large coprecipitation reactor. The large flow rate and high flow rate drop mode will lead to a larger droplet volume and significant concentration polarization. In addition, the stirring speed of the large precipitation reactor is limited, the pH value in the reactor has a large regional difference, and the entire reaction system is in a serious non-uniform state. Therefore, the quality consistency of the final precipitation product is often very poor.

[0005] Therefore, the existing co-precipitation method for preparing modified alumina is often carried out in a small laboratory reactor with a small volume and easy homogenization, and is carried out by slow dripping of a small amount. The synthesis efficiency of modified alumina is very low and cannot meet the needs of engineering applications. Furthermore, the current equipment for preparing modified alumina has a single function, and the process of precipitation, aging, solid-liquid separation, and drying needs to be carried out in a variety of equipment. The process is cumbersome, difficult to operate, and has a low degree of standardization and automation. Summary of the invention

[0006] In view of the above problems, the object of the present invention is to provide a mass production device for modified alumina carriers.

[0007] The objective of the present invention is achieved through the following technical solutions:

[0008] A modified alumina carrier batch production device, comprising a salt solution preparation tank, an aging reactor, a filter plate, a peristaltic pump, a delivery pump, a pipeline high shear dispersion reactor, and a high-pressure atomizing spray gun;

[0009] The salt solution preparation tank is used to prepare the mixed salt solution required for the coprecipitation reaction. The top of the salt solution preparation tank is respectively provided with a solid feeding port A and a liquid feeding port A, and the bottom of the salt solution preparation tank is provided with a salt solution discharge port;

[0010] The aging reactor is used to prepare the alkaline solution required for the co-precipitation reaction, and the aging, solid-liquid separation and drying of the precipitated product are completed in the aging reactor. The aging reactor is divided into a reactor body and a reactor cover. The top of the reactor body is open, and the reactor cover is used to close the top opening of the reactor body. The reactor cover is respectively provided with a solid feeding port B, a liquid feeding port B, a pressurizing port, an alkali solution circulation inlet, and a venting port. The filter plate is installed at the lower side of the inner cavity of the reactor body, and a plurality of filter holes are opened on the filter plate. A hollow heat conduction oil channel is opened on the inner side of the filter plate. The filter plate is also provided with a heat transfer oil inlet C and a heat transfer oil outlet C respectively connected to the hollow heat transfer oil channel, the heat transfer oil inlet C and the heat transfer oil outlet C both extend out of the kettle body, the heat transfer oil inlet C is connected to an external heat transfer oil supply network through a pipeline, the heat transfer oil outlet C is connected to an external heat transfer oil return network through a pipeline, the pressurizing port is connected to an external compressed air source through a pipeline, a filter cloth is laid on the top surface of the filter plate, and an alkali liquid circulation outlet is provided on the side wall of the kettle body and at the upper side of the whole composed of the filter plate and the filter cloth;

[0011] The pipeline high shear dispersion reactor comprises a dispersion reactor frame, a dispersion reactor motor, a reaction chamber, a stator and a rotor. The reaction chamber is a place where a co-precipitation reaction occurs between a mixed salt solution and an alkaline solution. The dispersion reactor motor and the reaction chamber are respectively arranged on the dispersion reactor frame. The stator and the rotor are respectively located in the inner cavity of the reaction chamber. The stator and the rotor are arranged in a pair and bite with each other, and a precipitation reaction space is formed between the stator and the rotor. The rotor is connected to the driving shaft of the dispersion reactor motor. The stator is fixed to the reaction chamber. A spray gun through hole is provided at the center of the stator. The reaction chamber is also provided with a feed pipe port and a discharge pipe port connected to the reaction chamber. The high-pressure atomizing spray gun has a compressed gas input port, a liquid input port and an atomized liquid spray port. The shell of the high-pressure atomizing spray gun is installed on the feed pipe port of the reaction chamber. The atomized liquid spray port of the high-pressure atomizing spray gun extends into the spray gun through hole of the stator and is connected to the precipitation reaction space.

[0012] The salt solution discharge port is connected to the input end of the peristaltic pump through a pipeline, the output end of the peristaltic pump is connected to the liquid input port of the high-pressure atomizing spray gun through a pipeline, the compressed gas input port of the high-pressure atomizing spray gun is connected to an external compressed gas source through a pipeline, the alkali solution circulation outlet is connected to the input end of the delivery pump through a pipeline, the output end of the delivery pump is connected to the feed pipe port of the reaction chamber through a pipeline, and the discharge pipe port of the reaction chamber is connected to the alkali solution circulation inlet through a pipeline.

[0013] The bottom of the salt solution preparation tank is provided with a jacket A, the top of the outer wall of the jacket A is provided with a heat transfer oil inlet A, the bottom of the outer wall of the jacket A is provided with a heat transfer oil outlet A, the heat transfer oil inlet A is connected to an external heat transfer oil supply network through a pipeline, and the heat transfer oil outlet A is connected to an external heat transfer oil return network through a pipeline.

[0014] The salt solution preparation tank is provided with a mechanical stirrer.

[0015] The salt solution preparation tank is provided with a plurality of individual holes.

[0016] The kettle cover is also provided with a magnetic sealing stirrer.

[0017] A filtrate discharge port is provided at the bottom of the kettle body, and the filtrate discharge port is connected to an external waste liquid collection system through a pipeline. A valve A is provided on the pipeline connecting the filtrate discharge port and the external waste liquid collection system.

[0018] A jacket B is provided at the bottom of the kettle body, a heat transfer oil inlet B is provided at the top of the outer wall of the jacket B, a heat transfer oil outlet B is provided at the bottom of the outer wall of the jacket B, the heat transfer oil inlet B is connected to an external heat transfer oil supply network through a pipeline, the heat transfer oil outlet B is connected to an external heat transfer oil return network through a pipeline, and the heat transfer oil inlet C, heat transfer oil outlet C and alkali liquid circulation outlet pass through the jacket B respectively.

[0019] A valve B is provided on the pipeline connected between the salt solution discharge port and the input end of the peristaltic pump, a valve C is provided on the pipeline connected between the alkali solution circulation outlet and the input end of the delivery pump, and a valve D is provided on the pipeline connected between the discharge pipe port of the reaction chamber and the alkali solution circulation inlet.

[0020] A valve E is provided on the pipeline connecting the compressed gas input port of the high-pressure atomizing spray gun and the external compressed gas source, a valve F is provided on the pipeline connecting the pressurizing port and the external compressed gas source, and the solid feeding port A, the solid feeding port B and the venting port are respectively provided with switch valves.

[0021] The liquid feeding port A and the liquid feeding port B are respectively connected to an external pure water source through pipelines. A valve G is provided on the pipeline connecting the liquid feeding port A and the external pure water source, and a valve H is provided on the pipeline connecting the liquid feeding port B and the external pure water source.

[0022] The advantages and positive effects of the present invention are:

[0023] 1. The device of the present invention adopts spray dripping combined with a pipeline high-shear dispersion reactor to control the co-precipitation reaction process. Spray dripping atomizes the mixed salt solution into micron-sized droplets, which are sprayed onto the dual-interlocking stator and rotor of the pipeline high-shear dispersion reactor. The rotor runs at high speed, and the maximum speed can reach 3600rpm. On the one hand, the droplets are subjected to mechanical forces and hydraulic shear such as centrifugal extrusion, liquid layer friction, impact tearing, turbulent impact, etc. in the gap between the stator and rotor, and broken into smaller particles, eliminating concentration polarization and strengthening the contact between the metal salt droplets and the alkali solution; on the other hand, under the strong stirring action of the pipeline high-shear dispersion reactor, the pH value of each region inside the alkali solution remains consistent, homogenizing the nucleation environment. The device of the present invention eliminates the influence of concentration polarization and regional fluctuations of pH value on the structural morphology of the product, improves the quality consistency of the modified alumina product, and in addition, the dual-interlocking stator and rotor can also quickly refine the newly generated precipitate to avoid particle agglomeration.

[0024] 2. The present invention can integrate the process of precipitation, aging, solid-liquid separation and drying into a set of devices, which solves the problems of complicated steps, discontinuous operation requiring to be carried out in multiple devices, long synthesis cycle, low production capacity and difficulty in automation, reduces labor intensity and saves labor costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 It is a schematic diagram of the overall setting principle of the present invention;

[0026] Figure 2 It is a schematic diagram of the structure of the salt solution preparation tank of the present invention;

[0027] Figure 3 It is a schematic diagram of the arrangement structure of the aging reaction kettle and the filter plate of the present invention;

[0028] Figure 4 It is a structural schematic diagram of the filter plate of the present invention;

[0029] Figure 5 It is a schematic diagram of the arrangement structure of the pipeline high shear dispersion reactor and the high pressure atomizing spray gun of the present invention;

[0030] Figure 6 for Figure 5 Enlarged view of point A.

[0031] In the figure: 1 is a salt solution preparation tank, 101 is a solid feed port A, 102 is a liquid feed port A, 103 is a salt solution discharge port, and 104 is a manhole;

[0032] 2 is an aging reaction kettle, 201 is a kettle body, 2011 is an alkali solution circulation outlet, 2012 is a filtrate discharge port, 202 is a kettle cover, 2021 is a solid feed port B, 2022 is a liquid feed port B, 2023 is a pressurizing port, 2024 is an alkali solution circulation inlet, and 2025 is a venting port;

[0033] 3 is a filter plate, 301 is a filter hole, 302 is a heat transfer oil inlet C, and 303 is a heat transfer oil outlet C;

[0034] 4 is a peristaltic pump, 5 is a delivery pump;

[0035] 6 is a pipeline high shear dispersion reactor, 601 is a dispersion reactor frame, 602 is a dispersion reactor motor, 603 is a reaction chamber, 6031 is a feed pipe opening, 6032 is a discharge pipe opening, 604 is a stator, 605 is a rotor, and 606 is a precipitation reaction space;

[0036] 7 is a high pressure atomizing spray gun, 701 is a compressed gas input port, 702 is a liquid input port, and 703 is an atomized liquid spray port;

[0037] 8 is a jacket A, 801 is a heat transfer oil inlet A, and 802 is a heat transfer oil outlet A;

[0038] 9 is a jacket B, 901 is a heat transfer oil inlet B, and 902 is a heat transfer oil outlet B;

[0039] 10 is a mechanical stirrer, 11 is a magnetic sealed stirrer;

[0040] 12 is valve A, 13 is valve B, 14 is valve C, 15 is valve D, 16 is valve E, 17 is valve F, 18 is valve G, 19 is valve H, 20 is valve I, and 21 is valve J. DETAILED DESCRIPTION

[0041] The following is combined with Figure 1-6 The present invention is further described in detail.

[0042] A modified alumina carrier batch production device, such as Figure 1-6 As shown, this embodiment includes a salt solution preparation tank 1, an aging reactor 2, a filter plate 3, a peristaltic pump 4, a delivery pump 5, a pipeline high shear dispersion reactor 6, and a high-pressure atomizing spray gun 7.

[0043] The salt solution preparation tank 1 is used to prepare the mixed salt solution required for the coprecipitation reaction. The top of the salt solution preparation tank 1 is respectively provided with a solid feeding port A 101 and a liquid feeding port A 102 , and the bottom of the salt solution preparation tank 1 is provided with a salt solution discharge port 103 .

[0044] The aging reactor 2 is used to prepare the alkaline solution required for the coprecipitation reaction, and the aging, solid-liquid separation and drying of the precipitated product are all completed in the aging reactor 2. The aging reactor 2 is divided into a reactor body 201 and a reactor cover 202. The top of the reactor body 201 is open, and the reactor cover 202 is used to close the top opening of the reactor body 201. The reactor cover 202 can be connected to a reactor cover lifting device of the prior art, which is convenient for driving the reactor cover 202 to lift and lower to achieve the function of opening and closing the top opening of the reactor body 201. The reactor cover 202 is respectively provided with a solid feeding port B2021, a liquid feeding port B2022, a pressurizing port 2023, an alkali solution circulation inlet 2024, and a venting port 2025. The filter plate 3 is installed at the lower side of the inner cavity of the kettle body 201. A plurality of filter holes 301 are provided on the filter plate 3. A hollow heat transfer oil channel is provided on the inner side of the filter plate 3. A heat transfer oil inlet C 302 and a heat transfer oil outlet C 303 connected to the hollow heat transfer oil channel are also provided on the filter plate 3. The heat transfer oil inlet C 302 and the heat transfer oil outlet C 303 both extend out of the kettle body 201. The heat transfer oil inlet C 302 is connected to an external heat transfer oil supply network through a pipeline. The heat transfer oil outlet C 303 is connected to an external heat transfer oil return network through a pipeline. The pressurizing port 2023 is connected to an external compressed gas source through a pipeline. A filter cloth is laid on the top surface of the filter plate 3. An alkali liquid circulation outlet 2011 is provided on the side wall of the kettle body 201 and at the upper side of the whole composed of the filter plate 3 and the filter cloth. The filter cloth used in this embodiment is made of polyester, the thickness of the filter cloth is ≥0.5mm, and the air permeability of the filter cloth is ≥10L / (m^2*s). In this embodiment, the filter hole 301 and the hollow heat transfer oil channel of the filter plate 3 are not connected, and the setting method adopts the existing technology. The diameter of the filter hole 301 is 10-20mm. The setting method of the external heat transfer oil supply pipeline network and the external heat transfer oil return pipeline network adopts the existing technology. The whole composed of the filter plate 3 and the filter cloth is used to filter the precipitated product. By passing the heat transfer oil into the hollow heat transfer oil channel of the filter plate 3, the filter plate 3 can be heated, and then the precipitated product on the filter cloth can be dried.

[0045] The pipeline high shear dispersion reactor 6 comprises a dispersion reactor frame 601, a dispersion reactor motor 602, a reaction chamber 603, a stator 604, and a rotor 605. The reaction chamber 603 is a place where the mixed salt solution and the alkaline solution undergo a coprecipitation reaction. The dispersion reactor motor 602 and the reaction chamber 603 are respectively arranged on the dispersion reactor frame 601. The stator 604 and the rotor 605 are respectively located in the inner cavity of the reaction chamber 603. The stator 604 and the rotor 605 are arranged in a pair and bite with each other, and a precipitation reaction space 606 is formed between the stator 604 and the rotor 605. The rotor 605 is connected to the driving shaft of the dispersion reactor motor 602, and the stator 604 is fixed to the reaction chamber 603. The above-mentioned structural arrangement of the pipeline high shear dispersion reactor 6 adopts the existing technology, and the pair and bite structure of the stator 604 and the rotor 605 can be single-layer or multi-layer. A spray gun through hole is provided at the center of the stator 604, and the reaction chamber 603 is also provided with a feed pipe port 6031 and a discharge pipe port 6032 connected to the reaction chamber 603. The high-pressure atomizing spray gun 7 has a compressed gas input port 701, a liquid input port 702 and an atomized liquid ejection port 703. The housing of the high-pressure atomizing spray gun 7 is mounted on the feed pipe port 6031 of the reaction chamber 603, and the atomized liquid ejection port 703 of the high-pressure atomizing spray gun 7 extends into the spray gun through hole of the stator 604 and is connected to the precipitation reaction space 606. In this embodiment, the high-pressure atomizing spray gun 7 adopts a commercially available product, and its atomized liquid ejection port 703 can be any one of a hollow cone atomizing nozzle, a solid cone atomizing nozzle, and a fan-shaped nozzle in the prior art.

[0046] The salt solution discharge port 103 is connected with the input end of the peristaltic pump 4 through a pipeline, the output end of the peristaltic pump 4 is connected with the liquid input port 702 of the high-pressure atomizing spray gun 7 through a pipeline, the compressed gas input port 701 of the high-pressure atomizing spray gun 7 is connected with an external compressed gas source through a pipeline, the alkali solution circulation outlet 2011 is connected with the input end of the delivery pump 5 through a pipeline, the output end of the delivery pump 5 is connected with the feed nozzle 6031 of the reaction chamber 603 through a pipeline, and the discharge nozzle 6032 of the reaction chamber 603 is connected with the alkali solution circulation inlet 2024 through a pipeline. In the present embodiment, the peristaltic pump 4 and the delivery pump 5 all adopt commercial products, and the peristaltic pump 4, the delivery pump 5 and the dispersed reactor motor 602 are all controlled by an external control system. The setting mode of the external control system in the present embodiment adopts the prior art, and can be composed of a PLC, a frequency converter, a temperature control instrument and a host computer, etc., for controlling the operation of the whole device.

[0047] Specifically, in this embodiment, a mechanical stirrer 10 is provided on the salt solution preparation tank 1, and a magnetic sealed stirrer 11 is also provided on the kettle cover 202, which is used to uniformly stir the liquid in the salt solution preparation tank 1 and the aging reactor 2. In this embodiment, the mechanical stirrer 10 and the magnetic sealed stirrer 11 are both commercially available products, and the actions are controlled by an external control system. In this embodiment, a plurality of manholes 104 are provided on the salt solution preparation tank 1 for maintenance and cleaning, and the manholes 104 are generally kept closed when the device is in normal use.

[0048] Specifically, in this embodiment, the bottom of the salt solution preparation tank 1 is provided with a jacket A8, the top of the outer wall of the jacket A8 is provided with a heat transfer oil inlet A801, and the bottom of the outer wall of the jacket A8 is provided with a heat transfer oil outlet A802. The heat transfer oil inlet A801 ​​is connected to the external heat transfer oil supply network through a pipeline, and the heat transfer oil outlet A802 is connected to the external heat transfer oil return network through a pipeline. In this embodiment, the bottom of the kettle body 201 is provided with a jacket B 9, the top of the outer wall of the jacket B 9 is provided with a heat transfer oil inlet B 901, the bottom of the outer wall of the jacket B 9 is provided with a heat transfer oil outlet B 902, the heat transfer oil inlet B 901 is connected to the external heat transfer oil supply pipeline network through a pipeline, the heat transfer oil outlet B 902 is connected to the external heat transfer oil return pipeline network through a pipeline, and the heat transfer oil inlet C 302, the heat transfer oil outlet C 303, and the alkali liquid circulation outlet 2011 are respectively passed through the jacket B 9. In this embodiment, the installation and setting structures of the jacket A 8 and the jacket B 9 are all based on the existing technology. Through the setting of the jacket A 8 and the jacket B 9, the liquid in the salt solution preparation tank 1 and the aging reaction kettle 2 can be used to heat the liquid. In this embodiment, the heat transfer oil inlet A 801, the heat transfer oil inlet B 901, the heat transfer oil inlet C 302 are all provided with valves I 20 on the pipelines connected to the external heat transfer oil supply network, and the heat transfer oil outlet A 802, the heat transfer oil outlet B 902, the heat transfer oil outlet C 303 are all provided with valves J 21 on the pipelines connected to the external heat transfer oil supply network, which are respectively used to control the heat transfer oil supply at various locations.

[0049] Specifically, in this embodiment, a filtrate discharge port 2012 is provided at the bottom of the kettle body 201, and the filtrate discharge port 2012 is connected to an external waste liquid collection system through a pipeline, and a valve A12 is provided on the pipeline connecting the filtrate discharge port 2012 and the external waste liquid collection system. The setting of the external waste liquid collection system adopts the existing technology. Through the setting of the filtrate discharge port 2012 and the valve A12, it is convenient to discharge the filtrate in the kettle body 201.

[0050] Specifically, in this embodiment, a valve B 13 is provided on the pipeline connected between the salt solution discharge port 103 and the input end of the peristaltic pump 4, a valve C 14 is provided on the pipeline connected between the alkali solution circulation outlet 2011 and the input end of the delivery pump 5, a valve D 15 is provided on the pipeline connected between the discharge pipe port 6032 of the reaction chamber 603 and the alkali solution circulation inlet 2024, a valve E 16 is provided on the pipeline connected between the compressed gas input port 701 of the high-pressure atomizing spray gun 7 and the external compressed gas source, a valve F 17 is provided on the pipeline connected between the pressurizing port 2023 and the external compressed gas source, a switch valve is provided on the solid feeding port A 101, the solid feeding port B 2021, and the venting port 2025, respectively, the liquid feeding port A 102 and the liquid feeding port B 2022 are respectively connected to the external pure water source through pipelines, and the liquid feeding port A 103 is connected to the external pure water source through pipelines. A valve G 18 is provided on the pipeline connected between the liquid feed port B 2022 and the external pure water source, and a valve H 19 is provided on the pipeline connected between the liquid feed port B 2022 and the external pure water source. In this embodiment, the configuration of the external pure water source and the external compressed gas source adopts the existing technology, and the compressed gas supplied by the external compressed gas source can be one of air, nitrogen or argon. In this embodiment, all the valves in the above places can adopt commercially available solenoid valve products, and the actions are controlled by an external control system.

[0051] The principle and working process of the batch production device of the modified alumina carrier provided by the present invention are described below by taking the synthesis of Ba modified alumina carrier as an example, as described below:

[0052] 1) A certain amount of pure water is added into the salt solution preparation tank 1 from the liquid feeding port A102, and the amount of water added is controlled by an external control system, and the control method is the prior art; the rotation speed of the mechanical stirrer 10 is set to 60 rpm by the external control system, and stirring is started; a certain amount of aluminum nitrate and barium nitrate raw materials are weighed according to the stoichiometric ratio and added into the salt solution preparation tank 1 from the solid feeding port A101, and the temperature in the salt solution preparation tank 1 is set to 70°C, and heat transfer oil is circulated into the jacket A8 from the heat transfer oil inlet A801 ​​and the heat transfer oil outlet A802 to heat the salt solution preparation tank 1, and the aluminum nitrate and barium nitrate are stirred until they are completely dissolved and the temperature is kept constant at 70°C for standby use.

[0053] 2) Add a certain amount of pure water to the kettle body 201 of the aging reactor 2, and the amount of water added is controlled by an external control system, which is a prior art; set the temperature in the aging reactor 2 to 70°C, and introduce heat transfer oil into the jacket B 9 through the heat transfer oil inlet B 901 and the heat transfer oil outlet B 902 to heat the kettle body 201; set the speed of the magnetic sealed agitator 11 to 100 rpm through the external control system, and start stirring; weigh a certain amount of (NH3)2CO3 and put it into the aging reactor 2 from the solid feeding port B 2021, and stir until the (NH3)2CO3 is completely dissolved and the temperature is kept constant at 70°C;

[0054] The flow rate of the delivery pump 5 is set to 30L / min through the external control system, and the delivery pump 5 and the related control valves are turned on to allow the (NH3)2CO3 solution to flow from the aging reactor 2 through the alkali solution circulation outlet 2011, the delivery pump 5, the feed pipe port 6031, the reaction chamber 603, the discharge pipe port 6032 and the alkali solution circulation inlet 2024 in sequence, and finally circulate back to the aging reactor 2. The speed of the magnetic sealed agitator 11 is maintained at 100rpm, and stirring is performed while circulating to allow the circulated liquid to be quickly mixed with the liquid in the reactor.

[0055] 3) When the alkali solution circulation reaches a stable state, the rotating speed of the dispersion reactor motor 602 of the pipeline high shear dispersion reactor 6 is set to 3600rpm, and the dispersion reactor motor 602 is turned on. When the pipeline high shear dispersion reactor 6 reaches the set rotating speed and is in stable operation, the intake pressure and flow of the high-pressure atomizing spray gun 7 are set by an external control system through an external compressed air source, and high-pressure air is injected into the high-pressure atomizing spray gun 7 from the compressed gas input port 701. The control of intake pressure and flow is a prior art; after the air flow is stabilized, the peristaltic pump 4 is turned on, and the mixed salt solution in the salt solution preparation tank 1 is pumped into the atomizing chamber inside the high-pressure atomizing spray gun 7 from the salt solution discharge port 103. In the atomizing chamber inside the high-pressure atomizing spray gun 7, the salt solution meets the high-pressure air flow and is atomized into micron-level droplets, which are sprayed into the precipitation reaction space 606 in the form of a hollow cone through the atomized liquid ejection port 703. The rotor 605 is operated at a speed of 3600rpm. The droplets in the gap between the stator 605 and the stator 604 are subjected to mechanical forces and hydraulic shear such as centrifugal extrusion, liquid layer friction, impact tearing, turbulent impact, etc., and are broken into smaller nano-scale liquid particles. After the nano-scale liquid particles come into contact with the alkali solution in the reaction chamber 603, they are immediately nucleated and solid precipitates are generated. The generated solid precipitates are collided and ground by the rotor 605 that rotates in a high-speed dual meshing manner with the stator 604, and are broken into smaller particles, thereby avoiding the agglomeration of the precipitates. The alkali solution rotates at a high speed driven by the rotor 605, generating a strong centrifugal force. Under the action of the centrifugal force, the newly generated precipitated particles are thrown out of the reaction chamber 603 together with the reacted alkali solution, and enter the aging reactor 2 through the discharge pipe port 6032 and the alkali solution circulation inlet 2024. The alkali solution circulated back from the aging reactor 2 is quickly sucked into the reaction chamber 603 through the feed pipe port 6031 of the reaction chamber 603, and continues to undergo precipitation reaction with the droplets sprayed by the high-pressure atomizing spray gun 7.

[0056] 4) After the reaction is completed, the pipeline high shear dispersion reactor 6, the salt solution preparation tank 1, the delivery pump 5 and the peristaltic pump 4 are closed, the temperature in the aging reactor 2 is maintained at 70° C., and the precipitate is aged for four hours under stirring; after four hours, the supply of the heat transfer oil is closed, the heating is stopped, and the aging liquid is cooled to room temperature under stirring by the magnetic sealed agitator 11; all valves on the kettle cover 202 of the aging reactor 2 are closed, the magnetic sealed agitator 11 is stopped, the filtrate discharge port 2012 is opened, and then the pressure port 202 is opened. 3. The pressure of the compressed gas input to the aging reactor 2 is set to 0.5 MPa through the external control system. Under the pressure, the liquid in the aging reactor 2 is filtered by the filter cloth and discharged out of the reactor through the filtrate discharge port 2012. It is collected by the external waste liquid collection system and treated as waste liquid. The solid precipitate is intercepted in the reactor by the filter cloth; when no filtrate is discharged from the filtrate discharge port 2012, the pressurization port 2023 is closed, the venting port 2025 is opened, the heat transfer oil temperature is set to 120 degrees Celsius, the heat transfer oil inlet C 302 and the heat transfer oil outlet C 303 are opened, and heating and drying are carried out for ten hours.

[0057] During the drying process, in order to speed up the drying process, the vent 2025 can be connected to a vacuum pump via a condenser while closing the filtrate discharge port 2012, and drying can be performed under vacuum conditions.

[0058] 5) After drying, the kettle cover 202 is opened to take out the material, and then the material is crushed, formed, granulated and calcined to prepare a Ba-modified alumina carrier; the crushing, forming, granulation and calcination of the precipitate are prior art. The Ba-modified alumina produced by the device proposed in the present invention is formed and initially calcined, and the carrier is tested for high temperature sintering resistance at 1300°C, and the volume shrinkage is ≤5%. The initial calcination temperature is 450°C to 600°C.

Claims

1. A modified alumina carrier batch production device, characterized in that: It comprises a salt solution preparation tank (1), an aging reactor (2), a filter plate (3), a peristaltic pump (4), a delivery pump (5), a pipeline high shear dispersion reactor (6), and a high-pressure atomizing spray gun (7); The salt solution preparation tank (1) is used to prepare a mixed salt solution required for a co-precipitation reaction. The top of the salt solution preparation tank (1) is provided with a solid feed port A (101) and a liquid feed port A (102), and the bottom of the salt solution preparation tank (1) is provided with a salt solution discharge port (103); The aging reactor (2) is used to prepare the alkaline solution required for the co-precipitation reaction, and the aging, solid-liquid separation and drying of the precipitated product are completed in the aging reactor (2). The aging reactor (2) is divided into a reactor body (201) and a reactor cover (202). The top end of the reactor body (201) is open, and the reactor cover (202) is used to close the top end opening of the reactor body (201). The reactor cover (202) is respectively provided with a solid feeding port B (2021), a liquid feeding port B (2022), a pressurizing port (2023), an alkali solution circulation inlet (2024), and a venting port (2025). The filter plate (3) is installed at the lower side of the inner cavity of the reactor body (201). The filter plate (3) is provided with a plurality of filter holes (301). The filter plate (3) A hollow heat transfer oil passage is provided on the inner side of the filter plate (3); a heat transfer oil inlet C (302) and a heat transfer oil outlet C (303) which are connected to the hollow heat transfer oil passage are respectively provided on the filter plate (3); the heat transfer oil inlet C (302) and the heat transfer oil outlet C (303) both extend out of the kettle body (201); the heat transfer oil inlet C (302) is connected to an external heat transfer oil supply network through a pipeline; the heat transfer oil outlet C (303) is connected to an external heat transfer oil return network through a pipeline; the pressurizing port (2023) is connected to an external compressed air source through a pipeline; a filter cloth is laid on the top surface of the filter plate (3); and an alkali liquid circulation outlet (2011) is provided on the side wall of the kettle body (201) and at an upper position of the whole consisting of the filter plate (3) and the filter cloth; The pipeline high shear dispersion reactor (6) comprises a dispersion reactor frame (601), a dispersion reactor motor (602), a reaction chamber (603), a stator (604), and a rotor (605). The reaction chamber (603) is a place where a mixed salt solution and an alkaline solution undergo a co-precipitation reaction. The dispersion reactor motor (602) and the reaction chamber (603) are respectively arranged on the dispersion reactor frame (601). The stator (604) and the rotor (605) are respectively located in the inner cavity of the reaction chamber (603). The stator (604) and the rotor (605) are arranged in a mutually coupled engagement manner, and a precipitation reaction space (606) is formed between the stator (604) and the rotor (605). The rotor (605) and the dispersion reactor motor (601) are connected to each other. The reaction chamber (603) is connected to the driving shaft of the reaction chamber (602), the stator (604) is fixedly connected to the reaction chamber (603), a spray gun through hole is provided at the center of the stator (604), the reaction chamber (603) is also provided with a feed pipe opening (6031) and a discharge pipe opening (6032) which are connected to the reaction chamber (603), the high-pressure atomizing spray gun (7) has a compressed gas input port (701), a liquid input port (702) and an atomized liquid spray port (703), the housing of the high-pressure atomizing spray gun (7) is installed on the feed pipe opening (6031) of the reaction chamber (603), the atomized liquid spray port (703) of the high-pressure atomizing spray gun (7) extends into the spray gun through hole of the stator (604) and is connected to the precipitation reaction space (606); The salt solution discharge port (103) is connected to the input end of the peristaltic pump (4) through a pipeline, the output end of the peristaltic pump (4) is connected to the liquid input port (702) of the high-pressure atomizing spray gun (7) through a pipeline, the compressed gas input port (701) of the high-pressure atomizing spray gun (7) is connected to an external compressed gas source through a pipeline, the alkali solution circulation outlet (2011) is connected to the input end of the delivery pump (5) through a pipeline, the output end of the delivery pump (5) is connected to the feed pipe port (6031) of the reaction chamber (603) through a pipeline, and the discharge pipe port (6032) of the reaction chamber (603) is connected to the alkali solution circulation inlet (2024) through a pipeline.

2. The modified alumina carrier batch production device according to claim 1, characterized in that: The bottom of the salt solution preparation tank (1) is provided with a jacket A (8), the top of the outer wall of the jacket A (8) is provided with a heat transfer oil inlet A (801), and the bottom of the outer wall of the jacket A (8) is provided with a heat transfer oil outlet A (802), the heat transfer oil inlet A (801) is connected to an external heat transfer oil supply network through a pipeline, and the heat transfer oil outlet A (802) is connected to an external heat transfer oil return network through a pipeline.

3. The modified alumina carrier batch production device according to claim 1, characterized in that: The salt solution preparation tank (1) is provided with a mechanical stirrer (10).

4. The modified alumina carrier batch production device according to claim 1, characterized in that: The salt solution preparation tank (1) is provided with a plurality of individual holes (104).

5. The modified alumina carrier batch production device according to claim 1, characterized in that: The kettle cover (202) is also provided with a stirrer (11) for magnetic sealing.

6. The modified alumina carrier batch production device according to claim 1, characterized in that: A filtrate discharge port (2012) is provided at the bottom of the kettle body (201), and the filtrate discharge port (2012) is connected to an external waste liquid collection system through a pipeline, and a valve A (12) is provided on the pipeline connecting the filtrate discharge port (2012) and the external waste liquid collection system.

7. The modified alumina carrier batch production device according to claim 1, characterized in that: The bottom of the kettle body (201) is provided with a jacket B (9), the top of the outer wall of the jacket B (9) is provided with a heat transfer oil inlet B (901), and the bottom of the outer wall of the jacket B (9) is provided with a heat transfer oil outlet B (902). The heat transfer oil inlet B (901) is connected to an external heat transfer oil supply network through a pipeline, and the heat transfer oil outlet B (902) is connected to an external heat transfer oil return network through a pipeline. The heat transfer oil inlet C (302), the heat transfer oil outlet C (303), and the alkali liquid circulation outlet (2011) respectively pass through the jacket B (9).

8. The modified alumina carrier batch production device according to claim 1, characterized in that: A valve B (13) is provided on the pipeline connecting the salt solution discharge port (103) and the input end of the peristaltic pump (4), a valve C (14) is provided on the pipeline connecting the alkali solution circulation outlet (2011) and the input end of the delivery pump (5), and a valve D (15) is provided on the pipeline connecting the discharge port (6032) of the reaction chamber (603) and the alkali solution circulation inlet (2024).

9. The modified alumina carrier batch production device according to claim 1, characterized in that: A valve E (16) is provided on the pipeline connecting the compressed gas input port (701) of the high-pressure atomizing spray gun (7) and the external compressed gas source, a valve F (17) is provided on the pipeline connecting the pressurizing port (2023) and the external compressed gas source, and a switch valve is provided on the solid feeding port A (101), the solid feeding port B (2021) and the venting port (2025) respectively.

10. The modified alumina carrier batch production device according to claim 1, characterized in that: The liquid feed port A (102) and the liquid feed port B (2022) are respectively connected to an external pure water source through pipelines. A valve G (18) is provided on the pipeline connecting the liquid feed port A (102) and the external pure water source, and a valve H (19) is provided on the pipeline connecting the liquid feed port B (2022) and the external pure water source.

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