An industrial method for rapidly preparing high-purity corundum crystal firewood boudin and crystal firewood board by four-step method

Abstract

The application provides an industrial method for rapidly preparing high-purity corundum crystal fire-adjacent bauxite and crystal fire-adjacent plate by a four-step method, and belongs to the technical field of high-temperature and high-corrosion fire-adjacent melting. In order to prepare a material applied to a high-temperature smelting fire-adjacent melting strong-corrosion working condition, a new process with large-scale production, high efficiency and low cost is developed by a four-step method. The process has the advantages of short processing and manufacturing period, low production cost, high purity, high material stability in a high-temperature and high-corrosion environment, and high additional value. The material has a far-reaching industrial value in the field of fire-adjacent melting, especially in the isolation performance of friction heat generated by high-speed operation and the light-weight performance of the whole body.

Description

Technical Field

[0001] This invention belongs to the field of high-temperature and high-corrosion flaming melting technology, and relates to a method for preparing crystalline fluff and crystalline plates, particularly an industrial method for rapidly preparing high-purity corundum crystalline flaming fluff and crystalline flaming plates using a four-step process. Background Technology

[0002] In the current nuclear industry, heavy metallurgy, and chemical processing, many production environments involve high temperatures and high corrosion. These industries are large-scale, require significant initial investment, and have long operating cycles, necessitating the safe and stable operation of complete sets of equipment. Furthermore, companies have a strong focus on cost-effectiveness. In critical high-temperature and high-corrosion environments, existing materials still suffer from short production cycles and high production costs per unit. Through continuous research and practice, companies have developed a process for large-scale production of high-purity corundum crystalline materials. This process boasts a short processing cycle, low production costs, high purity, and greater material stability in high-temperature and high-corrosion environments, thus demonstrating its higher added value.

[0003] Through research and comparison, further processing of this material has shown that its insulation performance against frictional heat generated during high-speed operation and its overall lightweight properties are of greater industrial value in the field of fused melting. Summary of the Invention

[0004] The purpose of this invention is to address the aforementioned problems in existing technologies by proposing an industrial method for rapidly preparing high-purity corundum crystalline flaming fluff and crystalline flaming plates using a four-step process. This invention is designed for materials used in high-temperature smelting and flaming melting under highly corrosive conditions, and develops a new process for large-scale production with high efficiency and low cost.

[0005] The objective of this invention can be achieved through the following technical solutions:

[0006] An industrial method for rapidly preparing high-purity corundum crystalline flaming fluff and crystalline flaming plates using a four-step process is characterized by the following steps performed in a strictly temperature- and humidity-controlled workshop:

[0007] (a) In a spray atomization fresh air supply environment, industrial pure aluminum balls, mixed with industrial ultrapure water, industrial pure water aluminum nitrate, industrial pure water zirconium nitrate, malic acid, and citric acid are poured into a reaction vessel. Driven by ultrasonic oscillation, the PTFE sealed stirring paddle is turned on at the same time to raise the jacket temperature and produce a preliminary nanocomposite polymer.

[0008] (b) Under constant temperature (lower) and constant humidity (higher) workshop conditions, the nanocomposite polymer is packaged and stored, and an appropriate amount of material is measured and water-soluble povidone polymer is added at the same time.

[0009] (c) Under constant temperature and humidity conditions, the composite polymer is concentrated to a high viscosity, pumped into a centrifugal disc for spinning or blowing, and then calcined at high temperature to make high-purity corundum crystal fluff.

[0010] (d) The crystalline fluff is soaked in water, ground, and compressed into a plate to become a crystalline corundum microporous flaming plate.

[0011] Furthermore, the production environment is a constant temperature and humidity workshop, with humidity of 30%-60% and temperature of 15-25℃.

[0012] Furthermore, it features a brand-new air delivery mode and a million-level filtration purification system.

[0013] Furthermore, the weighing of materials must be carried out in a spray-atomized atmosphere, and the workshop humidification adopts an ultrapure water electric heating mode.

[0014] Furthermore, the raw materials selected are for large-scale industrial preparation: industrial pure aluminum balls, industrial ultrapure water, industrial pure hydrated aluminum nitrate, industrial pure hydrated zirconium nitrate, malic acid, and citric acid.

[0015] Furthermore, the above materials must be mixed and pumped into the reactor in a spray atomization environment, with ultrapure water as the atomization water source.

[0016] Furthermore, the mixing and stirring of materials must be driven by ultrasonic oscillation. To prevent other impurities from being mixed in during stirring, a fully PTFE-sealed stirring paddle must be used.

[0017] Furthermore, after the material reaction is complete, it needs to be filtered by a high-speed centrifuge. All parts of the centrifuge that come into contact with the material must be made of 304 stainless steel to prevent the material from being contaminated.

[0018] Furthermore, for large-scale production, in the initial concentration stage, the original water ring pump vacuum concentration method is abandoned, and a screw vacuum pump is used for concentration. This greatly increases the active power output of the motor, reduces production costs, and improves concentration efficiency.

[0019] Furthermore, the material concentrated to a reasonable viscosity is centrifuged or blown into the air. The ambient temperature for filament formation is 85-95℃, and the humidity is controlled at 15-30%. The temperature of the make-up air is strictly controlled, and a circulating air system is used to significantly reduce the re-input power of heating, thereby significantly reducing production costs.

[0020] Furthermore, after high-temperature calcination, it becomes high-purity corundum crystalline fluff. In the packaging and processing of the crystalline fluff, it is strictly necessary to use ultrapure water in a spray atomization environment to prevent contamination of the material.

[0021] Furthermore, the crystalline flocs are introduced into a crusher for rapid crushing. The entire process must be carried out in a high-humidity atomized spray environment, with humidity ranging from 80% to 95%.

[0022] Furthermore, the material fragments are introduced into a mixing tank, water containing an appropriate amount of curing binder is added, and the mixture is stirred and dispersed at high speed, with most particles reaching a diameter of 2-20 micrometers.

[0023] Furthermore, the dispersion slurry is poured into a high-speed vibrating tank, where it vibrates to remove most of the moisture. At the same time, the hydraulic extrusion plate is activated to form a standard-sized template or a special-shaped mold. Then, it is placed in an oven to dry, which can produce a high-purity crystalline fire-tracing plate or other special-shaped fire-tracing components.

[0024] To provide a detailed description of the above-described technical solution of the present invention, the following steps are employed:

[0025] (1) Strictly control the temperature and humidity in the production workshop to ensure that all the raw materials selected can perform their functions. At the same time, it also greatly ensures the safety of workshop operators. Some raw materials are flammable, explosive, and volatile.

[0026] (2) In the material feeding and feeding process, spray atomization is strictly added, and the atomization amount can be adjusted by frequency conversion according to the amount of material.

[0027] (3) Mix industrial pure aluminum balls, hydrated aluminum nitrate, hydrated zirconium nitrate and ultrapure water in a molar ratio of 5:1:0.03:250.

[0028] (4) To maintain high purity, the workshop's air supply system is 100% fresh air, and the air filtration adopts a million-level purification system.

[0029] (5) After the materials are mixed, ultrapure water is used to guide them into the reactor. The stirring shaft is sealed with PTFE and fluororubber, eliminating the secondary pollution of the materials caused by the original graphite packing and excitation stirring.

[0030] (6) An ultrasonic oscillation system is installed in the stirring tank to make the materials mix more evenly and the reaction more thorough.

[0031] (7) The temperature of the reactor jacket is increased at a rate of 5℃ / min. When the temperature reaches 90℃, the temperature is stopped and the mixture is stirred for 2 hours until the material becomes clear and transparent.

[0032] (8) Centrifuge the above transparent and clear materials, filter them precisely, mix them together, raise the temperature, and adjust the material viscosity to 20 MPa under the negative pressure control of the screw vacuum pump. It can be guaranteed for one year.

[0033] (9) Continue to concentrate the above materials to a suitable viscosity, pump them into a centrifugal disc or spray them, and calcine them at high temperature.

[0034] (10) The calcined material is poured into the crusher under atomized spraying environment, crushed and mixed with an aqueous solution containing binder, centrifuged at high speed, then poured into a vibrating tank carrying four eccentric rotating motors, then injected into a mold, compressed under high pressure to remove water, and then transferred to an oven to dry, to obtain a high-purity corundum crystal fire-tracing plate or other irregular fire-tracing components.

[0035] Compared with existing technologies, this industrial method for rapidly preparing high-purity corundum crystalline flaming fluff and crystalline flaming plates using a four-step process has the following advantages:

[0036] 1. In order to prepare materials for use in high-temperature smelting and highly corrosive fusion environments, this invention has developed a new four-step process for large-scale production with high efficiency and low cost. This process has a short processing cycle, low production cost, high purity, and higher material stability in high-temperature and highly corrosive environments, thus demonstrating its high added value. Further processing of this material, especially in the field of fusion, enhances its insulation performance against frictional heat generated by high-speed operation and its lightweight properties, which have promising industrial value.

[0037] 2. This invention, by strictly controlling the temperature and humidity in the production workshop, maximizes the performance of all selected raw materials, prevents the dangers of some raw materials being flammable, explosive, or volatile, and ensures the safety of workshop operators.

[0038] 3. In the material feeding and dispensing process of this invention, spray atomization is strictly added, and the atomization amount can be adjusted by frequency conversion according to the amount of material.

[0039] 4. In order to maintain high purity, the workshop's air supply system is 100% fresh air, and the air filtration adopts a million-level purification system.

[0040] 5. In this invention, after the materials are mixed, ultrapure water is used to guide them into the reactor. The stirring shaft is sealed with PTFE and fluororubber, eliminating the secondary contamination of the materials caused by the original graphite packing and magnetic stirring. Attached Figure Description

[0041] Figure 1 This is a flowchart of the process flow of the present invention.

[0042] Figure 2 This is a schematic diagram of the structure of the enamel-lined glass reactor in an embodiment of the present invention.

[0043] Figure 3 This is a schematic diagram of the material vibration tank in an embodiment of the present invention. Detailed Implementation

[0044] The following are specific embodiments of the present invention, which are described in conjunction with the accompanying drawings to further illustrate the technical solutions of the present invention. However, the present invention is not limited to these embodiments.

[0045] like Figures 1-2 As shown in the figure, this embodiment provides an industrial method for rapidly preparing high-purity corundum crystalline flaming fluff and crystalline flaming plates using a four-step process. The specific implementation process is as follows:

[0046] (1) Production and ingredient preparation environment conditions: The production workshop is a fully enclosed cleanroom with an external Class 1 million cleanroom air conditioning supply and return system with constant temperature and humidity. Ultrapure water heating is used for humidity compensation in the workshop. The temperature is controlled at 15℃ and the humidity at 80%.

[0047] (2) Selection of raw materials:

[0048] The water source is industrial ultrapure water with a pH of 7 and a resistance of 18 megohms.

[0049] Zirconium nitrate hydrate, industrial purity 99.99%.

[0050] Aluminum nitrate hydrate, industrial purity 99.99%.

[0051] Industrial-grade malic acid, industrial-grade citric acid.

[0052] Industrial pure aluminum balls, 99.99%, 350 mesh.

[0053] (3) Industrial production equipment: industrial ultrapure water purifiers, enamel-lined glass reactors, such as... Figure 1 As shown, the system includes a PTFE packing agitator, a high-frequency ultrasonic oscillating shaft, a constant-temperature hot water heater, a double-funnel dry mixing tank (all-plastic), a high-speed tubular centrifuge, a negative pressure spray tower system, a positive pressure spray atomization system, and a vibrating tank equipped with four eccentric vibrating motors. Figure 2 Hydraulic extrusion press.

[0054] (4) Production process:

[0055] Step 1: In a strictly controlled temperature and humidity workshop, with fresh air supply at 20°C and 70% humidity, weigh out 135 kg of industrial pure aluminum balls and 35 kg of industrial pure hydrated zirconium carbonate according to the specified ratio. Add the materials to the mixing vessel under atomized spray conditions and stir until moistened. Then, weigh out 675 kg of hydrated aluminum nitrate and pour it into the mixing vessel under atomized spray conditions (using ultrapure water). Slowly stir all the materials together. After the materials are evenly mixed, use 300 kg of ultrapure water to carry the materials through a funnel into a glass-lined reactor. Finally, rinse all the materials with pure water and let them flow into the glass-lined reactor. A total of 2000 kg of ultrapure water is used. Start stirring and activate the ultrasonic vibration inside the glass-lined reactor to heat the reactor to the reaction temperature of 95°C. Stop heating once the materials begin to react. After observing the material and waiting for the solution to clarify, the material was released and allowed to stand for four hours. The material was then centrifuged at high speed and filtered to obtain a 20-50 nanometer composite polymer with a pH of 3.5 under a scanning electron microscope.

[0056] Mix the two composite polymers in the specified proportions, stir and heat, control the temperature of the material in the glass-lined reactor, and begin vacuum concentration for approximately 3-5 hours. Control the viscosity of the secondary composite polymer and then stop concentration. Pour the mixture into a blue light-proof container. This composite polymer can maintain its stability for one year.

[0057] Step 2: Take more than 2 tons of material and concentrate it. Control the condensate temperature at 11℃, the jacketed kettle temperature at 40℃, and the vacuum degree at -0.099MPa to -0.1MPa. When the concentrated viscosity reaches about 1000MPa, pump the material into a centrifugal spinning disc or spray it. Control the centrifugal speed at 18000r / min, the spray pressure at 0.2MPa, and the air pressure at 0.3MPa. Control the drying environment of the material at 85℃-95℃ and the humidity at 12%-19%. Then, convey it to the calcining furnace via a mesh belt.

[0058] Step 3: In a meticulously controlled workshop with a spray atomization environment, humidity is maintained at 80%-90%, and the water source is industrial ultrapure water. The calcined high-purity corundum crystal flocs are poured into a crusher, with the speed controlled at 15 r / min. During peak crushing periods, the spray atomization rate is increased. The crushed material is then poured into a stirred tank under the guidance of an aqueous solution, with a 10% solids content binder added to the solution. The stirred tank and centrifuge disc are then turned on. The length of the stirred material is controlled to be 2-20 micrometers.

[0059] Step 4: Pour the above water-soluble materials into a vibrating tank or mold for irregularly shaped components, such as... Figure 2 The vibrating trough is driven by four eccentric motors installed in four directions, with the operating frequency set to 30Hz. The vibration in four directions can greatly improve its coagulation effect. It is then subjected to secondary drainage and extrusion using a hydraulic press, with the pressure controlled at 0.8MPa. Finally, it is transferred to an oven for drying to obtain high-purity corundum crystal tracing plates or irregularly shaped tracing components.

[0060] The working principle and structural features of the enamel-lined glass reactor used in this invention are as follows:

[0061] 1. This vessel is a forged steel welded vessel with an inner lining of glass enamel and a double-layer jacketed design, in which circulating hot and cold media flow.

[0062] 2. The seal between the rotating agitator and the vessel lid is a PTFE disc.

[0063] 3. The entire vessel is equipped with material temperature detection and cavity pressure detection.

[0064] 4. Most importantly, an ultrasonic oscillator is installed on the lower side of the reactor, which has extremely high mixing reaction efficiency for fine materials.

[0065] Before use, the vessel cavity should be cleaned. Material input can be done through the manhole or by backflow from the discharge port. The optimal material input volume is one-third of the vessel cavity volume, which is just enough to submerge the agitator a short distance. Sufficient space should be left in the upper layer for rapid expansion during violent reactions.

[0066] The stirring speed of the servo motor and the frequency of the ultrasonic oscillation are set according to the required mixing rate of the material. The circulating hot and cold media in the jacket must be filled completely during the initial commissioning phase; sudden temperature changes are prohibited. After the material reaction is complete, discharge it from the discharge port and clean the reactor cavity promptly.

[0067] The specific embodiments described herein are merely illustrative of the spirit of the invention. Those skilled in the art to which this invention pertains may make various modifications or additions to the described specific embodiments or use similar methods to substitute them, without departing from the spirit of the invention or exceeding the scope defined by the appended claims.

Claims

1. An industrial method for the rapid preparation of high-purity corundum crystalline companion fireboard using a four-step process, characterized by, In a strict constant temperature and humidity workshop, the following steps are realized: (a) In the environment of spraying atomization of fresh air, industrial pure aluminum ball, mixed industrial ultra-pure water, industrial pure aluminum nitrate, industrial pure zirconium nitrate, malic acid, citric acid, are poured into the reaction kettle, under the drive of ultrasonic oscillation, while the four fluorine sealing stirring paddle is opened, the jacket temperature is improved, and the preliminary nano composite is produced; (b) Under the constant temperature and humidity workshop condition, the nano composite is stored, and the appropriate amount of material is measured, and the water-soluble povidone polymer is added; (c) Under the constant temperature and humidity workshop condition, the composite is concentrated to high viscosity, pumped into the centrifugal disc for spinning or blowing, and then high temperature calcination is carried out, and high purity corundum crystal fluff is made; (d) The crystal fluff is immersed in water and ground, compressed into a plate, and becomes a crystal corundum microporous fire plate.

2. The industrial method for rapidly preparing high-purity corundum crystal fire plate by four-step method according to claim 1, characterized in that, The atomized water source in step (a) is ultra-pure water.

3. The industrial method for rapidly preparing high-purity corundum crystal fire board by four-step method according to claim 1, characterized in that, After the material reaction is completed, it needs to pass through a high-speed centrifuge for filtration. The centrifuge must be made of all stainless steel 304 materials in contact with the material to prevent the material from being contaminated.

4. The industrial method for rapidly preparing high-purity corundum crystal fire board by four-step method according to claim 1, characterized in that, The material is concentrated, and the material concentrated to a reasonable viscosity is centrifuged or blown into a silk environment with a temperature of 85-95℃ and a humidity of 15-30%. The strict control of air temperature is adopted, and a circulating air system is used to greatly reduce the input power of heating, thereby greatly reducing the production cost.

5. The industrial method for rapidly preparing high-purity corundum crystal fire board by four-step method according to claim 1, characterized in that, In step (d), the crystal fluff is introduced into the crusher and quickly crushed. The whole link must be in a high humidity atomization spraying environment with a humidity of 80%-95%.

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