High-strength reinforcing agent for direct-current electric porcelain glaze and preparation method of high-strength reinforcing agent

Abstract

The invention discloses a high-strength reinforcing agent for direct-current electric porcelain glaze, and the high-strength reinforcing agent for direct-current electric porcelain glaze is prepared from the following raw materials in parts by mass: 100 parts of quartz sand and 7-8 parts of silane coupling agent. The quartz sand is subjected to high-temperature calcination at 850-900 DEG C, the quartz sand crystal conversion rate reaches 70% or above, the quartz sand can form a cristobalite crystal phase with higher stability through high-temperature calcination, then the quartz sand crystal is subjected to ball-milling treatment through a ball mill, the material dispersion uniformity is improved to a certain degree, and the material dispersion uniformity is improved to a certain degree. A mixture of gamma-aminopropyl triethoxy silane and gamma-glycidyl ether oxypropyl trimethoxy silane is used in the silane coupling agent, and a nano zinc oxide dispersing agent is added in the silane coupling agent, so that chemical bonding with the quartz sand is enhanced through the arrangement; the interface bonding strength is optimized; and due to the introduction of the composite rare earth oxide, glaze grains can be more refined.

Description

Technical Field

[0001] This invention relates to the field of DC electric porcelain glaze reinforcing agent technology, specifically to a high-strength reinforcing agent for DC electric porcelain glaze and its preparation method. Background Technology

[0002] With the rapid development of ultra-high voltage direct current (UHVDC) transmission technology, higher requirements have been placed on the performance of key components of transmission lines, such as insulators. Compared with AC systems, DC insulators need to withstand more severe electric field environments and thermo-mechanical stresses, thus requiring extremely stringent requirements on the mechanical strength, density, and sodium ion migration suppression capabilities of their ceramic bodies.

[0003] In traditional DC porcelain production, the use of sodium-containing raw materials is typically restricted to avoid increased conductivity and accelerated aging caused by the introduction of sodium ions. This results in a narrower firing temperature window and an increase in porcelain defects (such as microcracks and pores), which in turn limits the improvement of mechanical strength. Although existing technologies improve strength by adding nano-silica or alumina, these methods suffer from high cost, poor dispersibility, and insufficient high-temperature stability. Furthermore, they are difficult to significantly improve overall mechanical properties without altering the original chemical composition of the glaze. Therefore, we propose a high-strength reinforcing agent for DC porcelain glazes and its preparation method. Summary of the Invention

[0004] The purpose of this invention is to provide a high-strength reinforcing agent for DC electrical porcelain glaze and its preparation method, so as to solve the problems that need to be solved in the background art.

[0005] To achieve the above objectives, the present invention provides the following technical solution: a high-strength reinforcing agent for DC electrical porcelain glaze, wherein the raw materials for manufacturing the high-strength reinforcing agent for DC electrical porcelain glaze include quartz sand and silane coupling agent, wherein the mass fraction of the raw materials is 100 parts of quartz sand and 7-8 parts of silane coupling agent, wherein the silica content of the quartz sand is greater than or equal to 98%, the alumina content is ≤1.5%, and the content of other trace impurities is ≤0.5%.

[0006] The silane coupling agent is manufactured from a mixture of γ-aminopropyltriethoxysilane and γ-glycidoxypropyltrimethoxysilane, with a mass ratio of 3:2. The silane coupling agent also includes a nano zinc oxide dispersant, with the mass ratio of 100 parts silane coupling agent to 1.5-2 parts nano zinc oxide dispersant. The nano zinc oxide has a particle size ≤50nm and a surface hydroxyl content ≥3.2mmol / g.

[0007] In traditional DC porcelain production, the use of sodium-containing raw materials is usually restricted to avoid the introduction of sodium ions, which would lead to increased conductivity and accelerated aging. This results in a narrower firing temperature window, an increase in porcelain defects (such as microcracks and pores), and consequently, a limitation on the improvement of mechanical strength. While existing technologies improve strength by adding nano-silica or alumina, these methods suffer from high costs, poor dispersibility, and insufficient high-temperature stability. Furthermore, they struggle to significantly enhance overall mechanical properties without altering the original glaze's chemical composition. This invention involves calcining the quartz sand at 850℃-900℃, achieving a crystal conversion rate exceeding 70%. This high-temperature calcination allows the quartz sand to form a more stable cristobalite crystal phase. Subsequently, ball milling of the quartz sand crystals improves material dispersion uniformity to some extent. The silane coupling agent uses a mixture of γ-aminopropyltriethoxysilane and γ-glycidoxypropyltrimethoxysilane, and nano-zinc oxide dispersant is added. This configuration strengthens the chemical bond with the quartz sand, optimizes interfacial bonding strength, and the introduction of composite rare earth oxides refines the glaze grains, significantly improving mechanical properties compared to traditional glazes.

[0008] As a further description of the above technical solution:

[0009] The method for preparing a high-strength reinforcing agent for DC electrical porcelain glaze includes the following steps:

[0010] Step 1: Raw material processing: Screen the quartz sand through a 100-mesh sieve and set aside. Then weigh out the corresponding mass fractions of quartz sand and silane coupling agent and set aside.

[0011] Step 2: Calcination treatment: The quartz sand is fed into a kiln for calcination at a temperature of 850℃-900℃ for a time of ≥8h, so that the crystal conversion rate of the quartz sand is ≥70%. After being taken out of the kiln, it is cooled to room temperature.

[0012] Step 3: Ball milling: Place the grinding balls and quartz sand into the ball mill at a mass ratio of 3:1. The mass ratio of the ball mill chamber to the quartz sand and grinding balls is 0.4-0.5:1. After the quartz sand is fed into the ball mill, the ball mill speed is 50-60 r / min, and the grinding time is 2 hours.

[0013] Step 4: Modification treatment: Place the silane coupling agent weighed in Step 1 into the ball mill. At this time, the internal temperature of the ball mill is raised to 40℃-50℃. The ball mill is used to grind until the median particle size of the quartz sand and silane coupling agent is <1.5um and the maximum particle size is <10um.

[0014] As a further description of the above technical solution:

[0015] Before the raw material processing in step one, the raw material pretreatment includes the following steps:

[0016] Step A1: Use a 100-mesh sieve to perform preliminary screening of the quartz sand. During the screening, add air separation and magnetic separation steps. Air separation removes light organic impurities, and magnetic separation removes iron filings and metal impurities.

[0017] Step A2: Place the quartz sand treated in step A1 in an environment of 60℃-80℃ for low-temperature drying until the moisture content of the quartz sand is ≤0.5% and seal it. During the low-temperature drying, use a mixer at 60-80r / min to stir.

[0018] As a further description of the above technical solution:

[0019] In step two, a tunnel-type kiln is used. The high-temperature insulation section of the kiln has a detection hole with a diameter of 50-80 mm. The inner wall of the detection hole is inlaid with high-temperature quartz glass, and a circulating water cooling jacket is installed on the outside of the high-temperature glass. An XRD detector with a focal point diameter of 5-10 mm is installed on the outside of the detection hole. The XRD detector collects diffraction data every 1-5 minutes, and then the integral areas of the characteristic diffraction peaks of crystalline quartz and cristobalite are compared.

[0020] The formula for calculating the conversion rate of quartz sand crystals is as follows:

[0021]

[0022] Where X is the conversion rate of cristobalite, I is the integral area of ​​the characteristic peak of cristobalite, Y is the integral area of ​​the characteristic peak of crystalline quartz, and Z is the integral area of ​​the characteristic peak of cristobalite.

[0023] As a further description of the above technical solution:

[0024] The XRD detector is equipped with an audible and visual alarm. When the XRD detector detects that the conversion rate of the quartz sand crystal reaches 70% or more, the audible and visual alarm is triggered.

[0025] As a further description of the above technical solution:

[0026] In step three, during ball milling, zirconia ceramic balls with a diameter of 5-8 mm are used. During the ball milling process, an inert gas, specifically nitrogen, is introduced into the mill at a flow rate of 0.3-0.5 m³ / h. 3 .

[0027] As a further description of the above technical solution:

[0028] In step four, during the modification treatment, 0.8-1.2% of a composite rare earth oxide by mass of quartz sand is added to the ball mill. The composite rare earth oxide is a mixture of lanthanum oxide and cerium oxide, and the molar ratio of lanthanum oxide to cerium oxide is 1:1.

[0029] As a further description of the above technical solution:

[0030] The high-strength reinforcing agent for DC porcelain glaze replaces 21-23% by weight of silicon dioxide in the DC porcelain glaze formulation, while the weight of the remaining components in the DC porcelain glaze formulation remains unchanged.

[0031] Compared with the prior art, the present invention has the following beneficial effects:

[0032] 1. The quartz sand of this invention is calcined at a high temperature of 850℃-900℃, so that the crystal conversion rate of quartz sand reaches more than 70%. Such high temperature calcination can make the quartz sand form a more stable cristobalite crystal phase. Then, the quartz sand crystal is ball-milled, which improves the uniformity of material dispersion to a certain extent.

[0033] 2. Secondly, the silane coupling agent uses a mixture of γ-aminopropyltriethoxysilane and γ-glycidoxypropyltrimethoxysilane, and nano zinc oxide dispersant is added to the silane coupling agent. This setting strengthens the chemical bond with quartz sand, optimizes the interfacial bonding strength, and the introduction of composite rare earth oxides can make the glaze grains finer, which significantly improves the mechanical properties compared with traditional glazes.

[0034] 3. Furthermore, the high-strength reinforcing agent for DC porcelain glaze of this invention effectively improves the firing defects caused by the limitation of sodium-containing raw materials in traditional glazes. The air separation and magnetic separation processes of raw material pretreatment remove organic impurities and metal filings. Low-temperature drying controls the moisture content to ≤0.5%, reducing the generation of pores and microcracks during firing. Moreover, nitrogen protection during ball milling avoids the oxidation and agglomeration of quartz sand. The uniform particle size distribution after modification further improves the sintering density of the glaze. At the same time, the special components of the reinforcing agent work synergistically to significantly reduce the migration rate of sodium ions, effectively improving the stability of DC porcelain in harsh electric field environments and delaying the aging process.

[0035] 4. Finally, the preparation process of this invention does not require complex equipment, can precisely control the transformation of quartz sand crystals, and ensure product consistency. When applied, only 21-23% of the weight of silica in the glaze needs to be replaced, without changing the original chemical composition of the glaze, making it more adaptable. Compared with traditional reinforcing materials such as nano silica and alumina, this reinforcing agent has a lower cost and excellent high-temperature stability. At the same time, the sintering temperature is reduced by 50-80℃ through the effect of composite rare earth oxides, further saving production energy consumption and providing an efficient solution for the large-scale, high-quality production of DC porcelain. Attached Figure Description

[0036] Figure 1 This is a schematic diagram of the system principle of the present invention. Detailed Implementation

[0037] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0038] Example 1:

[0039] Please see Figure 1 This invention provides a technical solution: a high-strength reinforcing agent for DC electric porcelain glaze, wherein the raw materials for manufacturing the high-strength reinforcing agent for DC electric porcelain glaze include quartz sand and silane coupling agent, wherein the mass fraction of the raw materials is 100 parts of quartz sand and 7-8 parts of silane coupling agent, wherein the silica content of the quartz sand is greater than or equal to 98%, the alumina content is ≤1.5%, and the content of other trace impurities is ≤0.5%.

[0040] The silane coupling agent is manufactured from a mixture of γ-aminopropyltriethoxysilane and γ-glycidoxypropyltrimethoxysilane, with a mass ratio of 3:2. The silane coupling agent also includes a nano zinc oxide dispersant, with the mass ratio of 100 parts silane coupling agent to 1.5-2 parts nano zinc oxide dispersant. The nano zinc oxide has a particle size ≤50nm and a surface hydroxyl content ≥3.2mmol / g.

[0041] The high-purity quartz sand, containing ≥98% silica, ≤1.5% alumina, and ≤0.5% trace impurities, avoids the formation of low-melting-point glassy phases or abnormal crystalline phases during firing, reducing defects such as microcracks and pores in the glaze layer, ensuring the density of the ceramic body, and preventing impurity ions from affecting the electrical insulation performance of the insulator. In the silane coupling agent, the amino group of γ-aminopropyltriethoxysilane readily reacts with the hydroxyl groups on the surface of the quartz sand to form a stable chemical bond, while the epoxy group of γ-glycidoxypropyltrimethoxysilane enhances its compatibility with the glaze matrix. The synergistic effect of these two components is significant. This significantly enhances the bonding strength between the reinforcing agent and the glaze interface, avoiding the problem of weak interfacial bonding when using a single coupling agent. This provides crucial support for improving the mechanical properties of the glaze layer. The addition of nano zinc oxide dispersant, with its nanoscale characteristics of ≤50nm particle size, allows it to be uniformly dispersed in the system, acting as a micro-filler to fill the microscopic voids in the glaze and improve its density. Moreover, its high activity with a surface hydroxyl content ≥3.2mmol / g allows it to fully react with silane coupling agents and quartz sand surface groups, strengthening the bonding force between components. At the same time, it inhibits the abnormal growth of quartz sand grains at high temperatures, preventing excessively large grains from increasing the brittleness of the glaze layer.

[0042] Example 2:

[0043] The method for preparing a high-strength reinforcing agent for DC electrical porcelain glaze includes the following steps:

[0044] Step 1: Raw material processing: Screen the quartz sand through a 100-mesh sieve and set aside. Then weigh out the corresponding mass fractions of quartz sand and silane coupling agent and set aside.

[0045] Step 2: Calcination treatment: The quartz sand is fed into a kiln for calcination at a temperature of 850℃-900℃ for a time of ≥8h, so that the quartz sand is transformed from a crystalline phase to a cristobalite phase, and the crystal conversion rate of the quartz sand is ≥70%. After being taken out of the kiln, it is cooled to room temperature.

[0046] Step 3: Ball milling: Place the grinding balls and quartz sand into the ball mill at a mass ratio of 3:1. The mass ratio of the ball mill chamber to the quartz sand and grinding balls is 0.4-0.5:1. After the quartz sand is fed into the ball mill, the ball mill speed is 50-60 r / min, and the grinding time is 2 hours.

[0047] Step 4: Modification treatment: Place the silane coupling agent weighed in Step 1 into the ball mill. At this time, the internal temperature of the ball mill is raised to 40℃-50℃. The ball mill is used to grind until the median particle size of the quartz sand and silane coupling agent is <1.5um and the maximum particle size is <10um.

[0048] The process involves using a 100-mesh sieve to screen the quartz sand, effectively removing oversized impurities and quartz sand particles, ensuring initial uniformity in raw material particle size. Precise temperature control between 850℃ and 900℃ and sufficient calcination time facilitate the efficient transformation of the quartz sand from a crystalline phase to a cristobalite phase, with a crystal conversion rate ≥70%. The cristobalite phase has a more stable structure than crystalline quartz, improving the high-temperature resistance and mechanical strength of subsequent glazes. Room temperature cooling avoids crystal structure breakage caused by rapid cooling, ensuring the stability of the quartz sand phase and providing structural support for improving the mechanical properties of the reinforcing agent. Ball milling ensures thorough mixing with the silane coupling agent in the subsequent process. The combination and modification treatment creates favorable conditions, reducing the problem of uneven particle size affecting the dispersibility of reinforcing agents. Moreover, by utilizing the ball milling effect, mechanical and chemical grinding can be carried out simultaneously. The introduction of silane coupling agents can transform the silicon-oxygen tetrahedral crystal form of silica powder into silicon-oxygen hexahedral crystal form by more than 25%. Furthermore, continuous grinding to an ultrafine particle state with a median particle size of <1.5μm and a maximum particle size of <10μm significantly increases the contact area between quartz sand and silane coupling agents, strengthening the interfacial bonding force between the two. At the same time, the ultrafine particle size can ensure that the reinforcing agent is uniformly dispersed in the subsequent glaze, avoiding glaze defects caused by agglomeration, and ultimately improving the overall performance of DC porcelain glaze.

[0049] Example 3:

[0050] Before the raw material processing in step one, the raw material pretreatment includes the following steps:

[0051] Step A1: Use a 100-mesh sieve to perform preliminary screening of the quartz sand. During the screening, add air separation and magnetic separation steps. Air separation removes light organic impurities, and magnetic separation removes iron filings and metal impurities.

[0052] Step A2: Place the quartz sand treated in step A1 in an environment of 60℃-80℃ for low-temperature drying until the moisture content of the quartz sand is ≤0.5% and seal it. During the low-temperature drying, use a mixer at 60-80r / min to stir.

[0053] The initial screening process using sieves separates quartz sand with excessively large particle sizes and lumpy impurities, preventing uneven grinding due to large particle size differences during subsequent grinding. Air classification removes light organic impurities, preventing them from easily carbonizing and forming pores during subsequent high-temperature calcination. Magnetic separation precisely adsorbs metallic impurities such as iron filings, preventing them from reducing the insulation performance of the DC porcelain and laying the foundation for the electrical performance and structural stability of the reinforcing agent. Low-temperature drying efficiently evaporates moisture from the quartz sand while preventing premature crystal phase changes caused by high-temperature drying, ensuring that the crystal phase transformation process can be precisely controlled during subsequent calcination.

[0054] In step two, a tunnel-type kiln is used. The high-temperature insulation section of the kiln has a detection hole with a diameter of 50-80 mm. The inner wall of the detection hole is inlaid with high-temperature quartz glass, and a circulating water cooling jacket is installed on the outside of the high-temperature glass. An XRD detector with a focal point diameter of 5-10 mm is installed on the outside of the detection hole. The XRD detector collects diffraction data every 1-5 minutes, and then the integral areas of the characteristic diffraction peaks of crystalline quartz and cristobalite are compared.

[0055] The formula for calculating the conversion rate of quartz sand crystals is as follows:

[0056]

[0057] Where X is the conversion rate of cristobalite, I is the integral area of ​​the characteristic peak of cristobalite, Y is the integral area of ​​the characteristic peak of crystalline quartz, and Z is the integral area of ​​the characteristic peak of cristobalite.

[0058] The XRD detector is equipped with an audible and visual alarm. When the XRD detector detects that the conversion rate of the quartz sand crystal reaches 70% or more, the audible and visual alarm is triggered.

[0059] The XRD detector can monitor the material data in real time during the calcination process. It can also detect the crystal conversion rate of quartz sand in real time using the conversion rate calculation formula. Once the crystal conversion rate reaches 70% or more, the audible and visual alarm will sound and shut down the calcination process in time to avoid waste of resources.

[0060] In step three, during ball milling, zirconia ceramic balls with a diameter of 5-8 mm are used. During the ball milling process, an inert gas, specifically nitrogen, is introduced into the mill at a flow rate of 0.3-0.5 m³ / h. 3 .

[0061] Nitrogen, as an inert gas, can prevent the surface of quartz sand from being oxidized and generating impurity oxides. It also reduces material agglomeration during ball milling and improves the uniformity of particle size distribution of the material after ball milling to a certain extent.

[0062] In step four, during the modification treatment, 0.8-1.2% of a composite rare earth oxide by mass of quartz sand is added to the ball mill. The composite rare earth oxide is a mixture of lanthanum oxide and cerium oxide, and the molar ratio of lanthanum oxide to cerium oxide is 1:1.

[0063] Among them, composite rare earth oxides can be added as grain boundary regulators to promote the uniform spreading of the glass phase in the glaze during high-temperature calcination, reduce the sintering temperature of the glaze, and refine the grain size of the glaze to 2-5 μm. This results in improved mechanical properties such as fracture toughness and Vickers hardness of the DC porcelain glaze layer with added reinforcing agent compared to traditional glazes without added reinforcing agent, and a reduction in sodium ion migration rate of more than 55%.

[0064] The high-strength reinforcing agent for DC porcelain glaze replaces 21-23% by weight of silicon dioxide in the DC porcelain glaze formulation, while the weight of the remaining components in the DC porcelain glaze formulation remains unchanged.

[0065] When applied, only 21-23% of the silica in the glaze needs to be replaced without changing the original chemical composition of the glaze, making it more adaptable. Compared with traditional reinforcing materials such as nano silica and alumina, this reinforcing agent has a lower cost and excellent high-temperature stability. At the same time, it reduces the sintering temperature by 50-80℃ through the action of composite rare earth oxides, further saving production energy consumption and providing an efficient solution for the large-scale, high-quality production of DC porcelain.

[0066] Example 4:

[0067] A high-strength reinforcing agent for DC electrical porcelain glaze, wherein the raw materials for manufacturing the high-strength reinforcing agent for DC electrical porcelain glaze include quartz sand and silane coupling agent, wherein the mass fraction of the raw materials is 100 parts quartz sand and 7 parts silane coupling agent, wherein the silica content of the quartz sand is greater than or equal to 98%, the alumina content is ≤1.5%, and the content of other trace impurities is ≤0.5%.

[0068] The silane coupling agent is manufactured from a mixture of γ-aminopropyltriethoxysilane and γ-glycidoxypropyltrimethoxysilane, with a mass ratio of 3:2. The silane coupling agent also includes a nano zinc oxide dispersant, with the mass ratio of 100 parts silane coupling agent to 1.5 parts nano zinc oxide dispersant. The nano zinc oxide has a particle size ≤50nm and a surface hydroxyl content ≥3.2mmol / g.

[0069] The method for preparing a high-strength reinforcing agent for DC electrical porcelain glaze includes the following steps:

[0070] Step 1: Raw material processing: Screen the quartz sand through a 100-mesh sieve and set aside. Then weigh out the corresponding mass fractions of quartz sand and silane coupling agent and set aside.

[0071] Step 2: The quartz sand is fed into a kiln for calcination at a temperature of 850°C for ≥8 hours, so that the quartz sand crystal conversion rate is ≥70%. After being taken out of the kiln, it is cooled to room temperature.

[0072] Step 3: Ball milling: Place the grinding balls and quartz sand into the ball mill at a mass ratio of 3:1. The mass ratio of the ball mill chamber to the quartz sand and grinding balls is 0.4:1. After the quartz sand is fed into the ball mill, the ball mill speed is 50 r / min, and the grinding time is 2 hours.

[0073] Step 4: Modification treatment: Place the silane coupling agent weighed in Step 1 into the ball mill. At this time, the internal temperature of the ball mill is raised to 40°C. Grind the quartz sand and silane coupling agent until the median particle size is <1.5 μm and the maximum particle size is <10 μm.

[0074] Before the raw material processing in step one, the raw material pretreatment includes the following steps:

[0075] Step A1: Use a 100-mesh sieve to perform preliminary screening of the quartz sand. During the screening, add air separation and magnetic separation steps. Air separation removes light organic impurities, and magnetic separation removes iron filings and metal impurities.

[0076] Step A2: Place the quartz sand treated in step A1 in a 60°C environment for low-temperature drying until the moisture content of the quartz sand is ≤0.5% and seal it. During the low-temperature drying, use a 60r / min mixer to stir.

[0077] In step two, a tunnel-type kiln is used. The high-temperature insulation section of the kiln has a 50mm diameter detection hole. The inner wall of the detection hole is inlaid with high-temperature quartz glass, and a circulating water cooling jacket is installed on the outside of the high-temperature glass. An XRD detector with a 5mm focal diameter is installed on the outside of the detection hole. The XRD detector collects diffraction data every 1 minute, and then the integral areas of the characteristic diffraction peaks of crystalline quartz and cristobalite are compared.

[0078] The formula for calculating the conversion rate of quartz sand crystals is as follows:

[0079]

[0080] Where X is the conversion rate of cristobalite, I is the integral area of ​​the characteristic peak of cristobalite, Y is the integral area of ​​the characteristic peak of crystalline quartz, and Z is the integral area of ​​the characteristic peak of cristobalite.

[0081] In step three, during ball milling, zirconia ceramic balls with a diameter of 5 mm are used. During the ball milling process, an inert gas, specifically nitrogen, is introduced into the mill at a flow rate of 0.3 m³ / min.3 .

[0082] In step four, during the modification treatment, a composite rare earth oxide, accounting for 0.8% of the mass of the quartz sand, is added into the ball mill. The composite rare earth oxide is a mixture of lanthanum oxide and cerium oxide, and the molar ratio of lanthanum oxide to cerium oxide is 1:1.

[0083] The high-strength reinforcing agent for DC porcelain glaze replaces 21% by weight of silicon dioxide in the DC porcelain glaze formulation, while the weight of the remaining components in the DC porcelain glaze formulation remains unchanged.

[0084] Example 5:

[0085] A high-strength reinforcing agent for DC electrical porcelain glaze, wherein the raw materials for manufacturing the high-strength reinforcing agent for DC electrical porcelain glaze include quartz sand and silane coupling agent, wherein the mass fraction of the raw materials is 100 parts quartz sand and 8 parts silane coupling agent, wherein the silica content of the quartz sand is greater than or equal to 98%, the alumina content is ≤1.5%, and the content of other trace impurities is ≤0.5%.

[0086] The silane coupling agent is manufactured from a mixture of γ-aminopropyltriethoxysilane and γ-glycidoxypropyltrimethoxysilane, with a mass ratio of 3:2. The silane coupling agent also includes a nano zinc oxide dispersant, with the mass ratio of 100 parts silane coupling agent to 2 parts nano zinc oxide dispersant. The nano zinc oxide has a particle size ≤50nm and a surface hydroxyl content ≥3.2mmol / g.

[0087] The method for preparing a high-strength reinforcing agent for DC electrical porcelain glaze includes the following steps:

[0088] Step 1: Raw material processing: Screen the quartz sand through a 100-mesh sieve and set aside. Then weigh out the corresponding mass fractions of quartz sand and silane coupling agent and set aside.

[0089] Step 2: The quartz sand is fed into a kiln for calcination at a temperature of 900℃ for ≥8 hours, so that the quartz sand crystal conversion rate is ≥70%. After being taken out of the kiln, it is cooled to room temperature.

[0090] Step 3: Ball milling: Place the grinding balls and quartz sand into the ball mill at a mass ratio of 3:1. The mass ratio of the ball mill chamber to the quartz sand and grinding balls is 0.5:1. After the quartz sand is fed into the ball mill, the ball mill speed is 60 r / min, and the grinding time is 2 hours.

[0091] Step 4: Modification treatment: Place the silane coupling agent weighed in Step 1 into the ball mill. At this time, the internal temperature of the ball mill is raised to 50°C. The ball mill is used to grind until the median particle size of the quartz sand and silane coupling agent is <1.5 μm and the maximum particle size is <10 μm.

[0092] Before the raw material processing in step one, the raw material pretreatment includes the following steps:

[0093] Step A1: Use a 100-mesh sieve to perform preliminary screening of the quartz sand. During the screening, add air separation and magnetic separation steps. Air separation removes light organic impurities, and magnetic separation removes iron filings and metal impurities.

[0094] Step A2: Place the quartz sand treated in step A1 in an 80°C environment for low-temperature drying until the moisture content of the quartz sand is ≤0.5% and seal it. During the low-temperature drying, use an 80r / min mixer to stir.

[0095] In step two, a tunnel-type kiln is used. The high-temperature insulation section of the kiln has detection holes with a diameter of 50-80 mm. The inner wall of the detection hole is inlaid with high-temperature quartz glass, and a circulating water cooling jacket is installed on the outside of the high-temperature glass. An XRD detector with a focal diameter of 10 mm is conveniently installed outside the detection hole. The XRD detector collects diffraction data every 5 minutes, and then the integral areas of the characteristic diffraction peaks of crystalline quartz and cristobalite are compared.

[0096] The formula for calculating the conversion rate of quartz sand crystals is as follows:

[0097]

[0098] Where X is the conversion rate of cristobalite, I is the integral area of ​​the characteristic peak of cristobalite, Y is the integral area of ​​the characteristic peak of crystalline quartz, and Z is the integral area of ​​the characteristic peak of cristobalite.

[0099] In step three, during ball milling, zirconia ceramic balls with a diameter of 8 mm are used. During the ball milling process, an inert gas, specifically nitrogen, is introduced into the mill at a flow rate of 0.5 m³ / min. 3 .

[0100] In step four, during the modification treatment, a composite rare earth oxide, accounting for 1.2% of the mass of the quartz sand, is added to the ball mill. The composite rare earth oxide is a mixture of lanthanum oxide and cerium oxide, and the molar ratio of lanthanum oxide to cerium oxide is 1:1.

[0101] The high-strength reinforcing agent for DC porcelain glaze replaces 23% by weight of silicon dioxide in the DC porcelain glaze formulation, while the weight of the remaining components in the DC porcelain glaze formulation remains unchanged.

[0102] Example 6:

[0103] A high-strength reinforcing agent for DC electrical porcelain glaze, wherein the raw materials for manufacturing the high-strength reinforcing agent for DC electrical porcelain glaze include quartz sand and silane coupling agent, wherein the mass fraction of the raw materials is 100 parts of quartz sand and 7.5 parts of silane coupling agent, wherein the silica content of the quartz sand is greater than or equal to 98%, the alumina content is ≤1.5%, and the content of other trace impurities is ≤0.5%.

[0104] The silane coupling agent is manufactured from a mixture of γ-aminopropyltriethoxysilane and γ-glycidoxypropyltrimethoxysilane, with a mass ratio of 3:2. The silane coupling agent also includes a nano zinc oxide dispersant, with the mass ratio of 100 parts silane coupling agent to 1.8 parts nano zinc oxide dispersant. The nano zinc oxide has a particle size ≤50nm and a surface hydroxyl content ≥3.2mmol / g.

[0105] The method for preparing a high-strength reinforcing agent for DC electrical porcelain glaze includes the following steps:

[0106] Step 1: Raw material processing: Screen the quartz sand through a 100-mesh sieve and set aside. Then weigh out the corresponding mass fractions of quartz sand and silane coupling agent and set aside.

[0107] Step 2: The quartz sand is fed into a kiln for calcination at a temperature of 875℃ for a duration of ≥8 hours, so that the quartz sand crystal conversion rate is ≥70%. After being taken out of the kiln, it is cooled to room temperature.

[0108] Step 3: Ball milling: Place the grinding balls and quartz sand into the ball mill at a mass ratio of 3:1. The mass ratio of the ball mill chamber to the quartz sand and grinding balls is 0.45:1. After the quartz sand is fed into the ball mill, the ball mill speed is 55 r / min, and the grinding time is 2 hours.

[0109] Step 4: Modification treatment: Place the silane coupling agent weighed in Step 1 into the ball mill. At this time, the internal temperature of the ball mill is raised to 45°C. Grind the quartz sand and silane coupling agent until the median particle size is <1.5 μm and the maximum particle size is <10 μm.

[0110] Before the raw material processing in step one, the raw material pretreatment includes the following steps:

[0111] Step A1: Use a 100-mesh sieve to perform preliminary screening of the quartz sand. During the screening, add air separation and magnetic separation steps. Air separation removes light organic impurities, and magnetic separation removes iron filings and metal impurities.

[0112] Step A2: Place the quartz sand treated in step A1 in a 70°C environment for low-temperature drying until the moisture content of the quartz sand is ≤0.5% and seal it. During the low-temperature drying, use a 70r / min mixer to stir.

[0113] In step two, a tunnel-type kiln is used. The high-temperature insulation section of the kiln has a 65mm diameter detection hole. The inner wall of the detection hole is inlaid with high-temperature quartz glass, and a circulating water cooling jacket is installed on the outside of the high-temperature glass. An XRD detector with a 7mm focal diameter is installed on the outside of the detection hole. The XRD detector collects diffraction data every 4 minutes, and then the integral areas of the characteristic diffraction peaks of crystalline quartz and cristobalite are compared.

[0114] The formula for calculating the conversion rate of quartz sand crystals is as follows:

[0115]

[0116] Where X is the conversion rate of cristobalite, I is the integral area of ​​the characteristic peak of cristobalite, Y is the integral area of ​​the characteristic peak of crystalline quartz, and Z is the integral area of ​​the characteristic peak of cristobalite.

[0117] In step three, during ball milling, zirconia ceramic balls with a diameter of 6 mm are used. During the ball milling process, an inert gas, specifically nitrogen, is introduced into the mill at a flow rate of 0.4 m³ / min. 3 .

[0118] In step four, during the modification treatment, a composite rare earth oxide, accounting for 1% of the mass of the quartz sand, is added to the ball mill. The composite rare earth oxide is a mixture of lanthanum oxide and cerium oxide, and the molar ratio of lanthanum oxide to cerium oxide is 1:1.

[0119] The high-strength reinforcing agent for DC porcelain glaze replaces 22% by weight of silicon dioxide in the DC porcelain glaze formulation, while the weight of the remaining components in the DC porcelain glaze formulation remains unchanged.

[0120] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A high-strength reinforcing agent for direct current ceramic glaze, characterized in that: The raw materials for manufacturing the high-strength reinforcing agent used in DC electric porcelain glaze include quartz sand and silane coupling agent. The mass fraction of the raw materials is 100 parts quartz sand and 7-8 parts silane coupling agent. The silica content of the quartz sand is greater than or equal to 98%, the alumina content is ≤1.5%, and the content of other trace impurities is ≤0.5%.

2. The high-strength reinforcing agent for DC electrical porcelain glaze according to claim 1, characterized in that: The silane coupling agent is manufactured from a mixture of γ-aminopropyltriethoxysilane and γ-glycidoxypropyltrimethoxysilane, with a mass ratio of 3:

2. The silane coupling agent also includes a nano zinc oxide dispersant, with the mass ratio of 100 parts silane coupling agent to 1.5-2 parts nano zinc oxide dispersant. The nano zinc oxide has a particle size ≤50nm and a surface hydroxyl content ≥3.2mmol / g.

3. A method for preparing a high-strength reinforcing agent for DC electrical porcelain glaze, applicable to the high-strength reinforcing agent for DC electrical porcelain glaze as described in any one of claims 1-2, characterized in that: The method for preparing a high-strength reinforcing agent for DC electrical porcelain glaze includes the following steps: Step 1: Raw material processing: Screen the quartz sand through a 100-mesh sieve and set aside. Then weigh out the corresponding mass fractions of quartz sand and silane coupling agent and set aside. Step 2: Calcination treatment: The quartz sand is fed into a kiln for calcination at a temperature of 850℃-900℃ for a time of ≥8h, so that the crystal conversion rate of the quartz sand is ≥70%. After being taken out of the kiln, it is cooled to room temperature. Step 3: Ball milling: Place the grinding balls and quartz sand into the ball mill at a mass ratio of 3:

1. The mass ratio of the ball mill chamber to the quartz sand and grinding balls is 0.4-0.5:

1. After the quartz sand is fed into the ball mill, the ball mill speed is 50-60 r / min, and the grinding time is 2 hours. Step 4: Modification treatment: Place the silane coupling agent weighed in Step 1 into the ball mill. At this time, the internal temperature of the ball mill is raised to 40℃-50℃. The ball mill is used to grind until the median particle size of the quartz sand and silane coupling agent is <1.5um and the maximum particle size is <10um.

4. The method for preparing a high-strength reinforcing agent for DC electrical porcelain glaze according to claim 3, characterized in that: Before the raw material processing in step one, the raw material pretreatment includes the following steps: Step A1: Use a 100-mesh sieve to perform preliminary screening of the quartz sand. During the screening, add air separation and magnetic separation steps. Air separation removes light organic impurities, and magnetic separation removes iron filings and metal impurities. Step A2: Place the quartz sand treated in step A1 in an environment of 60℃-80℃ for low-temperature drying until the moisture content of the quartz sand is ≤0.5% and seal it. During the low-temperature drying, use a mixer at 60-80r / min to stir.

5. The method for preparing a high-strength reinforcing agent for DC electrical porcelain glaze according to claim 4, characterized in that: In step two, a tunnel-type kiln is used. The high-temperature insulation section of the kiln has a detection hole with a diameter of 50-80 mm. The inner wall of the detection hole is inlaid with high-temperature quartz glass, and a circulating water cooling jacket is installed on the outside of the high-temperature glass. An XRD detector with a focal point diameter of 5-10 mm is installed on the outside of the detection hole. The XRD detector collects diffraction data every 1-5 minutes, and then the integral areas of the characteristic diffraction peaks of crystalline quartz and cristobalite are compared. The formula for calculating the conversion rate of quartz sand crystals is as follows: Where X is the conversion rate of cristobalite, I is the integral area of ​​the characteristic peak of cristobalite, Y is the integral area of ​​the characteristic peak of crystalline quartz, and Z is the integral area of ​​the characteristic peak of cristobalite.

6. The method for preparing a high-strength reinforcing agent for DC electrical porcelain glaze according to claim 5, characterized in that: The XRD detector is equipped with an audible and visual alarm. When the XRD detector detects that the conversion rate of the quartz sand crystal reaches 70% or more, the audible and visual alarm is triggered.

7. The method for preparing a high-strength reinforcing agent for DC electrical porcelain glaze according to claim 6, characterized in that: In step three, during ball milling, zirconia ceramic balls with a diameter of 5-8 mm are used. During the ball milling process, an inert gas, specifically nitrogen, is introduced into the mill at a flow rate of 0.3-0.5 m³ / h. 3 .

8. The method for preparing a high-strength reinforcing agent for DC electrical porcelain glaze according to claim 7, characterized in that: In step four, during the modification treatment, 0.8-1.2% of a composite rare earth oxide by mass of quartz sand is added to the ball mill. The composite rare earth oxide is a mixture of lanthanum oxide and cerium oxide, with a molar ratio of lanthanum oxide to cerium oxide of 1:

1.

9. An application of a high-strength reinforcing agent for DC electrical porcelain glaze, as described in claim 1, characterized in that: The high-strength reinforcing agent for DC porcelain glaze replaces 21-23% by weight of silicon dioxide in the DC porcelain glaze formulation, while the weight of the remaining components in the DC porcelain glaze formulation remains unchanged.

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