Preparation method of high-purity transparent crystal fused magnesite

Abstract

The invention relates to the field of fused magnesite production, and discloses a preparation method of high-purity transparent crystal fused magnesite, which comprises the following steps: S1, raw material preparation: preparing corresponding materials in a proportioning scheme, the corresponding materials comprising magnesium oxide, zirconium oxide and aluminum oxide; s2, proportioning and mixing: accurately selecting the components according to the proportion, metering the proportioning materials by using a metering machine, and pouring the proportioning materials into the inner wall of a mixing machine for mixing by using the mixing machine; s3, melting processing: putting the mixed raw materials into an electric melting furnace, setting the furnace temperature to a proper temperature, and meanwhile, in the heating process, controlling the atmosphere in the furnace by a worker. In the melting processing process, a temperature subsection control method is used, the melting processing step is divided into four parts, and the temperature requirements in the four parts are different, so that the mixing effect of the raw materials is better facilitated, and the production quality of the fused magnesia is further improved.

Description

Technical Field

[0001] The invention relates to the technical field of fused magnesia production, in particular to a method for preparing high-purity transparent crystal fused magnesia. Background Art

[0002] Fused magnesia is an important industrial material with high purity and excellent physical and chemical properties. It is widely used in many fields, including refractory materials, electronic devices, optical components, etc.

[0003] In the process of producing and processing fused magnesia, the raw materials of the fused magnesia need to be mixed and then put into a hot melt machine. Through the continuous heating of the hot melt machine, the raw materials of the fused magnesia are heated and fused to form fused magnesia.

[0004] Considering that during the processing of electric fused magnesia raw materials by a hot melt machine, magnesia and other auxiliary materials are placed in a hot melt machine and melted at a continuous high temperature, although this method is simple, due to the constant high temperature, it is easy to cause some components to melt prematurely, while other components may melt excessively or fail to melt completely, affecting the quality of the finished product. In addition, the rapid heating and cooling process at high temperature will introduce significant internal stress in the crystal, increasing the risk of crystal cracks. Summary of the invention

[0005] In view of the deficiencies in the prior art, the present invention provides a method for preparing high-purity transparent crystalline fused magnesia, which solves the problem that under the constant high temperature of a hot melt machine, some components may melt prematurely, while other components may melt excessively or fail to melt completely, thus affecting the quality of the finished fused magnesia product.

[0006] To achieve the above object, the present invention is implemented by the following technical scheme: a method for preparing high-purity transparent crystalline fused magnesia, comprising the following steps:

[0007] S1. Raw material preparation: preparing materials corresponding to the ratio scheme, wherein the corresponding materials include magnesium oxide, zirconium oxide and aluminum oxide;

[0008] S2. Proportioning and mixing: Select each component accurately according to the proportion, use a metering machine to measure the proportioning materials, and then use a mixer to pour the proportioning materials into the inner wall of the mixer for mixing;

[0009] S3. Melting processing: Put the mixed raw materials into the electric melting furnace, set the furnace temperature to a suitable temperature, and during the heating process, the staff needs to control the atmosphere in the furnace. Inert gas needs to be used during the heating process to avoid oxidation reaction of the materials;

[0010] S301. Temperature segment control: The melt processing is divided into four stages, and the heating time and temperature of the four stages are different, which is more conducive to the mixing effect of the raw materials;

[0011] S302. Dynamic atmosphere regulation: During the entire melting process, dynamic atmosphere regulation technology (adding argon or nitrogen) is used to control the redox environment in the furnace to further improve the chemical purity and physical properties of the product;

[0012] S4. Cooling and crystallization: After melting, the liquid mixture needs to be taken out and cooled using a cooler. After the liquid mixture is cooled to room temperature, the crystals will form solid blocks. The cooler uses a slow cooling or stage cooling method to promote the growth of large crystals and improve the transparency and structural integrity of the material.

[0013] S5. Finishing and inspection: Mechanical cutting and grinding of the solid block, which requires the use of a cutting machine and a grinding machine, followed by inspection;

[0014] S6. Packaging and storage: According to the fragility and sensitivity of the product, use shock-proof and moisture-proof packaging materials for packaging, and store the packaged products in a suitable environment to maintain the quality of the product.

[0015] Preferably, a mixer is used in step S2, and specific mixing parameters of the mixer are: mixing time is 15-20 minutes, and mixing speed is 30 to 100 revolutions per minute.

[0016] Preferably, the heating temperature of the electric melting furnace in step S3 is above 2000° C., and the heating time is 12-14 hours.

[0017] Preferably, the inert gas in step S3 is argon or nitrogen.

[0018] Preferably, the melting process in step S301 is divided into four stages, and the heating time and temperature of the four stages are different, wherein the specific four stages are a preheating stage, a low-temperature melting stage, a high-temperature homogenization stage and a refinement temperature control stage.

[0019] Preferably, the specific cooling parameters of the cooling machine in step S4 are: the cooling temperature is room temperature 20-25° C., and the cooling time is 24-48 hours.

[0020] Preferably, a cutting machine and a grinder are required in step S5, specifically: a worker operates a cutting machine to cut the solid block, and then uses a grinder to grind the outer wall of the solid block to remove burrs on the outer wall of the fixed block, improve the appearance of the finished product, and make it into a specific shape and size according to customer needs or application requirements.

[0021] Preferably, the inspection in step S5 specifically includes: the inspection includes tests of structural integrity, transparency, thermal stability and thermal shock resistance, and the quality standard of the fused magnesia is comprehensively judged from various aspects.

[0022] Preferably, the suitable environment in step S6 is specifically: storing in a dry, cool, light-proof environment to maintain the quality of the product.

[0023] A high-purity transparent crystal fused magnesia, comprising: 95% magnesium oxide, 2% zirconium oxide, and 3% aluminum oxide.

[0024] The present invention provides a method for preparing high-purity transparent crystalline fused magnesia, which has the following beneficial effects:

[0025] 1. In the process of melting processing, the present invention uses a temperature segmented control method to divide the melting processing step into four parts, and the temperature requirements in the four parts are not the same, which is more conducive to the mixing effect of the raw materials and further improves the quality of fused magnesia production.

[0026] 2. In the process of melting processing, the present invention uses dynamic atmosphere adjustment technology to separately adjust argon or nitrogen in four parts on the basis of segmented temperature control to control the redox environment in the furnace and further improve the chemical purity and physical properties of the product.

[0027] 3. The present invention provides fused magnesia with different proportions, so that the fused magnesia with different proportions has different effects. It can be selected and used when high temperature resistant environment, excellent optical properties, corrosion resistance and specific color appearance are required, thereby improving the adaptability of fused magnesia. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 It is a flow chart of the present invention. DETAILED DESCRIPTION

[0029] The following will be combined with the drawings in the specification of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0030] Embodiment 1:

[0031] Please see attached Figure 1The embodiment of the present invention provides a high-purity transparent crystalline fused magnesia, including: magnesium oxide: 95%, zirconium oxide 2%, aluminum oxide 3%. By adding zirconium oxide and aluminum oxide to magnesium oxide, the thermal stability and thermal shock resistance of the ratio are enhanced by relying on zirconium oxide and aluminum oxide, which is suitable for applications requiring high temperature resistance and structural stability.

[0032] A method for preparing high-purity transparent crystalline fused magnesia comprises the following steps:

[0033] S1. Raw material preparation: preparing materials corresponding to the ratio scheme, wherein the corresponding materials include magnesium oxide, zirconium oxide and aluminum oxide;

[0034] S2. Proportioning and mixing: Accurately select the components according to the ratio of 95% magnesium oxide, 2% zirconium oxide, and 3% aluminum oxide, and use a metering machine to measure the proportion of the materials to ensure the accuracy of the material ratio, and then use a mixer to pour the proportioned materials into the inner wall of the mixer for mixing. The mixing time is 15 minutes and the mixing speed is 30 to 100 revolutions per minute;

[0035] S3. Melting processing: Put the mixed raw materials into an electric melting furnace and set the furnace temperature to a suitable temperature, usually above 2000°C, to ensure that all components are completely melted to form a uniform liquid mixture. The heating time is 12 hours. During the heating process, the staff needs to control the atmosphere in the furnace. Inert gas needs to be used during the heating process to avoid oxidation reaction of the material. The inert gas includes argon.

[0036] S301. Temperature segment control: The melt processing is divided into four stages, and the heating time and temperature of the four stages are different, which is more conducive to the mixing effect of the raw materials;

[0037] Preheating stage: preheat the raw materials to 500°C for 1-2 hours to remove any residual moisture and volatile impurities;

[0038] Low temperature melting stage: The temperature gradually rises to 1500°C. This stage is mainly to allow the magnesium oxide to slowly melt to avoid structural damage caused by sudden high temperature;

[0039] High temperature homogenization stage: The temperature is quickly raised to the set maximum temperature (2200°C) and maintained for 1-2 hours to ensure that all ingredients are thoroughly integrated;

[0040] Refined temperature control stage: In this stage, the temperature will be fine-tuned according to the feedback data of crystal growth, and the heating power and time will be adjusted to optimize the crystal growth conditions;

[0041] The specific adjustment of heating power and time is:

[0042] Temperature Monitoring: Use an accurate temperature sensor (thermocouple) to monitor the temperature of the crystal in real time.

[0043] Temperature fine-tuning: When the temperature is higher than the target setting value, reduce the heating power to 65%; when the temperature is lower than the target setting value, increase the heating power to 75%.

[0044] Time interval: record data every 10 minutes and adjust according to data trends.

[0045] S302. Dynamic atmosphere regulation: During the entire melting process, dynamic atmosphere regulation technology (adding argon or nitrogen) is used to control the redox environment in the furnace to further improve the chemical purity and physical properties of the product;

[0046] Warm-up phase

[0047] Objective: During the preheating stage, the main purpose is to remove moisture and volatile impurities from the material while preventing premature oxidation of the material.

[0048] Atmosphere setting: Use argon gas with a purity of 99% and a flow rate of 2 (L / min).

[0049] Duration: 1-2 hours.

[0050] Function: Argon is an inert gas that can effectively prevent oxidation of materials during the preheating stage and maintain chemical purity.

[0051] Low temperature melting stage

[0052] Goal: At this stage, the goal is to slowly heat the material to the melting point, promoting uniform melting without creating thermal stresses.

[0053] Atmosphere settings: Argon flow was increased to 5 L / min to enhance protection against any potential oxidation reactions.

[0054] Duration: Adjusted during the temperature increase from 500℃ to 1500℃.

[0055] Function: High flow of argon can create a more stable and protective environment, reducing the risk of oxidation

[0056] High temperature homogenization stage

[0057] Goal: To ensure that the materials are thoroughly melted and evenly mixed when the maximum temperature is reached.

[0058] Atmosphere setting: Introduce a mixture of nitrogen and argon in a ratio of 1:1 with a total flow rate of 10 L / min.

[0059] Duration: The period during which high temperature is maintained.

[0060] Function: Nitrogen can participate in regulating the redox reaction, promote the reduction of oxides, and improve the electrical and mechanical properties of the final product.

[0061] Refined temperature control stage

[0062] Goal: Fine-tune temperature and atmosphere to optimize crystal growth conditions.

[0063] Atmosphere setting: Continue to use the mixed atmosphere of argon and nitrogen, adjust the ratio to 2:1, adjust the total flow rate to 8L / min, and adjust dynamically according to the real-time monitoring data.

[0064] Duration: The entire process of crystal growth.

[0065] Function: The atmosphere adjustment at this stage is more refined, which can more accurately control the defects and stress inside the crystal and ensure high-quality growth of the crystal.

[0066] S4. Cooling and crystallization: After melting, the liquid mixture needs to be taken out and cooled using a cooler. After the liquid mixture is cooled to room temperature, the crystals will form solid blocks. The cooling temperature is 20-25°C at room temperature, and the cooling time is 24-48 hours. The cooler adopts a slow cooling or stage cooling method to promote the growth of large crystals and improve the transparency and structural integrity of the material.

[0067] S5. Finishing and inspection: Mechanical cutting and grinding of the solid block requires the use of a cutting machine and a grinding machine. The staff operates the cutting machine to cut the solid block, and then grinds the outer wall of the solid block with a grinding machine to remove burrs on the outer wall of the fixed block, improve the appearance of the finished product, and make it into a specific shape and size according to customer needs or application requirements;

[0068] Then the inspection is carried out, including the test of structural integrity, transparency, thermal stability and thermal shock resistance, to comprehensively judge the quality standard of fused magnesia from all aspects;

[0069] S6. Packaging and storage: According to the fragility and sensitivity of the product, use shock-proof and moisture-proof packaging materials for packaging, and store the packaged products in a dry, cool, light-proof environment to maintain the quality of the product.

[0070] In order to better understand the difference between the fused magnesia produced by the temperature segmentation control method of the present invention and the fused magnesia produced by the conventional method, the two groups of fused magnesia are compared to judge the effectiveness of the temperature segmentation control method:

[0071] Basic Materials:

[0072] 10 groups of fused magnesia produced by temperature segmentation control method

[0073] 10 groups of fused magnesia made by conventional method

[0074] Simulation experimental data:

[0075] Sample preparation: Ten batches of samples were taken for analysis for each method.

[0076] Testing indicators: crystal structure, purity, physical and chemical stability, particle size distribution.

[0077] Crystal structure: X-ray diffraction (XRD) was used to evaluate the regularity and phase purity of the crystals.

[0078] Purity and stability: Assessed by spectroscopic analysis and chemical stability testing.

[0079] Particle Size: Use a particle size analyzer to measure and compare the uniformity and distribution of particle size.

[0080]

[0081]

[0082] Data Analysis:

[0083] Crystal quality: Fused magnesia produced by the temperature segmentation control method shows higher crystal regularity and purity, because the precise control of temperature helps to form a more complete lattice structure.

[0084] Purity: The samples prepared by the temperature segmented control method have higher purity and contain fewer impurities, which may be due to the precise control at the key temperature points to reduce the mixing of impurities.

[0085] Particle size distribution: Fused magnesia using the step-by-step temperature control method has a more uniform particle size distribution. This is probably because the fine control of temperature allows for a more uniform distribution of thermal energy, which in turn affects crystal growth rate and results.

[0086] Chemical and physical stability: The fused magnesia prepared by the temperature-stage control method exhibited better chemical and physical stability, which indicates that temperature control is crucial to improving material properties.

[0087] in conclusion:

[0088] It is clearly stated that the quality parameters of the fused magnesia produced by the temperature segmented control method are better than those of the fused magnesia produced by the conventional method.

[0089] Embodiment 2:

[0090] A high-purity transparent crystal fused magnesia comprises 97% magnesium oxide and 3% lanthanum. Lanthanum is added to magnesium oxide to increase the refractive index and optical transparency of the material, so the material is suitable for applications requiring excellent optical properties.

[0091] Embodiment three:

[0092] A high-purity transparent crystalline fused magnesia, comprising: 98% magnesium oxide, 1% silicon dioxide, and 1% aluminum oxide. By adding appropriate amounts of silicon dioxide and aluminum oxide to magnesium oxide, heat resistance and corrosion resistance can be increased without excessively affecting transparency, and it is suitable for cost-sensitive applications.

[0093] Embodiment 4:

[0094] A high-purity transparent crystalline fused magnesia comprises: 96% magnesium oxide, 2% silicon dioxide and 2% iron oxide. Chromium and iron are added to the magnesium oxide so that the addition of chromium and iron can change the color and partial optical properties of the crystal, and the magnesia is suitable for materials requiring specific color or appearance.

[0095] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for preparing high-purity transparent crystalline fused magnesia, It is characterized in that The following steps are involved: S1. Raw material preparation: preparing materials corresponding to the ratio scheme, wherein the corresponding materials include magnesium oxide, zirconium oxide and aluminum oxide; S2. Proportioning and mixing: Select each component accurately according to the proportion, use a metering machine to measure the proportioning materials, and then use a mixer to pour the proportioning materials into the inner wall of the mixer for mixing; S3. Melting processing: Put the mixed raw materials into the electric melting furnace, set the furnace temperature to a suitable temperature, and during the heating process, the staff needs to control the atmosphere in the furnace. Inert gas needs to be used during the heating process to avoid oxidation reaction of the materials; S301. Temperature segment control: The melt processing is divided into four stages, and the heating time and temperature of the four stages are different, which is more conducive to the mixing effect of the raw materials; S302. Dynamic atmosphere regulation: During the entire melting process, dynamic atmosphere regulation technology (adding argon or nitrogen) is used to control the redox environment in the furnace to further improve the chemical purity and physical properties of the product; S4. Cooling and crystallization: After melting, the liquid mixture needs to be taken out and cooled using a cooler. After the liquid mixture is cooled to room temperature, the crystals will form solid blocks. The cooler uses a slow cooling or stage cooling method to promote the growth of large crystals and improve the transparency and structural integrity of the material. S5. Finishing and inspection: Mechanical cutting and grinding of the solid block, which requires the use of a cutting machine and a grinding machine, followed by inspection; S6. Packaging and storage: According to the fragility and sensitivity of the product, use shock-proof and moisture-proof packaging materials for packaging, and store the packaged products in a suitable environment to maintain the quality of the product.

2. A method for preparing high-purity transparent crystalline fused magnesia according to claim 1, It is characterized in that A mixer is used in step S2, and specific mixing parameters of the mixer are: mixing time is 15-20 minutes, and mixing speed is 30 to 100 revolutions per minute.

3. A method for preparing high-purity transparent crystalline fused magnesia according to claim 1, It is characterized in that The heating temperature of the electric melting furnace in step S3 is above 2000° C., and the heating time is 12-14 hours.

4. A method for preparing high-purity transparent crystalline fused magnesia according to claim 1, It is characterized in that The inert gas in step S3 is specifically argon or nitrogen.

5. A method for preparing high-purity transparent crystalline fused magnesia according to claim 1, It is characterized in that The melting process in step S301 is divided into four stages, and the heating time and temperature of the four stages are different. The specific four stages are a preheating stage, a low-temperature melting stage, a high-temperature homogenization stage, and a refinement temperature control stage.

6. A method for preparing high-purity transparent crystalline fused magnesia according to claim 1, It is characterized in that The specific cooling parameters of the cooling machine in step S4 are: the cooling temperature is room temperature 20-25° C., and the cooling time is 24-48 hours.

7. A method for preparing high-purity transparent crystalline fused magnesia according to claim 1, It is characterized in that The step S5 requires the use of a cutting machine and a grinding machine. Specifically, a worker operates a cutting machine to cut the solid block, and then uses a grinding machine to grind the outer wall of the solid block to remove burrs on the outer wall of the fixed block, improve the appearance of the finished product, and make it into a specific shape and size according to customer needs or application requirements.

8. A method for preparing high-purity transparent crystalline fused magnesia according to claim 1, It is characterized in that The inspection in step S5 is specifically as follows: the inspection includes testing of structural integrity, transparency, thermal stability and thermal shock resistance, and comprehensively judging the quality standard of the fused magnesia from various aspects.

9. A method for preparing high-purity transparent crystalline fused magnesia according to claim 1, It is characterized in that The suitable environment in step S6 is specifically: storing in a dry, cool, light-proof environment to maintain the quality of the product.

10. A high-purity transparent crystalline fused magnesia according to any one of claims 1 to 9, It is characterized in that include: Magnesium oxide: 95%, zirconium oxide 2%, aluminum oxide 3%.

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