Silane glycolate-brucite composite powder as well as preparation method and application thereof

Abstract

The invention provides silanolate-brucite composite powder as well as a preparation method and application thereof, and belongs to the technical field of photochemical detection of building materials. Active silane is modified by a natural product glycolic acid and is used for surface activation of natural high-magnesium brucite to form organic-inorganic hybrid core-shell structure composite powder, the glycolic acid silane is used as a shell, and the high-magnesium brucite is used as an inner core. According to the organic-inorganic hybrid core-shell structure composite material, a natural product derivative of silanolate and traditional inorganic mineral powder can be mutually combined together, so that the natural mineral powder not only has a visual fluorescence chromogenic function, but also has the characteristics of flame retardance and smoke suppression; according to the invention, unique advantages of glycolic acid silane and natural high-magnesium brucite are integrated on composite powder particles, so that high-valued application of natural mineral powder is realized.

Description

Technical Field

[0001] This invention relates to the field of photochemical detection technology for building materials, and in particular to a silane-magnesium hydroxide composite powder, its preparation method, and its application. Background Technology

[0002] Mineral wool binder is a core binder used in the production of various mineral wool products (such as rock wool, slag wool, and glass wool). It enables these mineral wool products to form fibrous products with certain strength, thermal insulation, and sound insulation properties, widely used in various construction projects, road sound insulation, and functional space construction. The performance of the binder directly affects the quality of the mineral wool product and the stability of the production process, profoundly impacting the final product's performance. The main components of the binder are resin matrix, functional additives, solvents, and many other components. The functional additives mainly include various additives that provide thickening, flame retardancy, water repellency, and defoaming effects. In daily use, as a functional binder, the modulation of its micro-viscosity significantly affects the wetting, penetration, and covering functions of the mineral wool binder, greatly influencing the final bonding effect of the mineral wool. Generally, mineral wool mortar with low viscosity exhibits high fluidity, facilitating easy penetration and wetting of mineral wool during bonding. This makes it suitable for bonding complex mineral wool structures with multiple layers. However, its shaping ability may be poor, leading to easy deformation during bonding. Conversely, excessively high viscosity reduces fluidity and penetration, hindering the bonding of multi-layered mineral wool structures and limiting wetting effectiveness. However, it possesses strong shaping capabilities, resisting bending or deformation during bonding. Furthermore, mineral wool mortar becomes viscous at low temperatures and thickens or loses homogeneity over extended storage, leading to excessive functional powder in certain areas and a sharp increase in application viscosity. Therefore, there is an urgent need to develop an efficient, convenient, and visual molecular-level tool for detecting the viscosity of mineral wool mortar. This tool should possess certain functional properties that allow it to be added to mineral wool mortar, responding not only to viscosity changes but also exhibiting good synergistic effects with existing functional additives to promote efficient preparation of mineral wool mortar.

[0003] Currently, most analytical methods for mineral wool slurry rely heavily on various viscometers (falling ball viscometers, rotational viscometers, oscillating viscometers, etc.). These devices are designed for the viscosity of macroscopic liquids, and their use is not only time-consuming but also has certain requirements for the sample size and quantity. More importantly, these devices struggle to achieve visualization at the molecular level. In contrast, photochemical analysis techniques incorporating natural functional organic molecules offer advantages such as better sensitivity, superior visualization, and more convenient detection methods. In particular, they can effectively avoid the shear-thinning effect that may occur in traditional viscosity measurements of slurries containing a large amount of pseudoplastic fluids. Furthermore, by loading photochemically active natural product molecules onto the main components of slurry functional additives, the functions of both can be combined, not only enhancing the value of traditional natural inorganic powders but also enabling the development of multifunctional composite powders that combine visualized colorimetric monitoring and flame retardancy.

[0004] Currently, there are few applications of using natural stone powder as a carrier for photochemical technology in the measurement of micro-area viscosity of mineral wool slurry. Summary of the Invention

[0005] The purpose of this invention is to provide a silane-magnesium hydroxide composite powder, its preparation method, and its application, in order to solve the above-mentioned technical problems.

[0006] To achieve the above-mentioned objectives, the present invention provides the following technical solution: This invention provides a silane-magnesium hydroxide composite powder, wherein the silane-magnesium hydroxide composite powder comprises a functional surface activation layer and a core. The functional surface activation layer is nucleotide silane, and the core is ultrafine high-magnesium brucite.

[0007] Furthermore, the ratio of the nucleotide silane to the ultrafine high-magnesium brucite is 1~3 mol: 10 kg; The particle size of the nucleotide silane-brucite composite powder is 1.0~4.4μm.

[0008] This invention also provides a method for preparing silane-brucite composite powder, comprising the following steps: 1) Mix nucleotide and silane solution, carry out dehydration condensation reaction, and obtain nucleotide silane activator after post-treatment; 2) After preparing the silane activator into a solution, it is mixed with ultrafine high-magnesium brucite and activated to obtain silane-brucite composite powder.

[0009] Furthermore, the particle size D of the ultrafine high-magnesium brucite... 50 The thickness ranges from 0.8 to 4.2 μm. The silane in the silane solution is 3-trimethylsilylpropynaldehyde, and the nucleotide is 5'-cytidine. The solvent in the silane solution is one or more of tetrahydrofuran, acetonitrile, dimethyl sulfoxide, and N,N-dimethylformamide. The nucleotide solution is mixed at 30~50℃, with a mixing speed of 300~900 rpm and a mixing time of 0.2~1.0 h.

[0010] Furthermore, the molar ratio of the glycosidic acid to the silane is 1:1 to 4; The dehydration condensation reaction is carried out in a high-pressure sealed tube, with the pressure controlled at 2~6 atm, the stirring temperature at 100~140℃, and the stirring time at 2.0~6.0h.

[0011] Furthermore, in step 1), the post-treatment includes distillation, precipitation, and crystallization; The distillation process involves removing the reaction solvent using a rotary evaporator at a pressure of -0.09 to -0.07 MPa. The crude product is then redispersed in a mixture of ethanol and purified water, with the volume ratio of ethanol to purified water controlled at 1:5 to 15 and the solid content controlled at 5 mg / mL to 10 mg / mL. The mixture is then allowed to stand at a low temperature of 1 to 10°C for 6 to 10 hours. The mixed solvent is then removed by vacuum filtration, with the vacuum pressure controlled at -0.09 MPa to 0.07 MPa. Neutral, fast-drying filter paper (1 to 2 layers) is used for filtration, and the flow rate is controlled at 2 to 10 mL / s. The resulting crystalline product, silane nucleotide activator, is obtained at low temperature.

[0012] Furthermore, in step 2), preparing the silane nucleotide activator into a solution involves mixing the silane nucleotide activator into a mixed solution, controlling the mixing rate at 100-600 rpm and the mixing time at 0.1-0.9 h; the mixed solution is a mixture of an alcohol solvent and water, with a volume ratio of alcohol solvent to water of 1-3:1; the alcohol solvent includes one or more of methanol, ethanol, propanol, ethylene glycol, and 1,2-propanediol; the concentration of the silane nucleotide activator in the solution is 1-5 mol / L.

[0013] Furthermore, in step 2), the mixing method involves adding the silane nucleotide active solution to the high-speed rotating brucite powder via spraying. The spraying rate is 20-100 mL / min. During the spraying process, the ultrafine high-magnesium brucite is preheated, and the stirring rate is controlled at 200-600 r / min, while the preheating temperature is controlled at 50-80℃. After spraying, the temperature is raised to 90-120℃ for activation, and the stirring rate is increased to 600-1000 r / min. The stirring is continued at the target temperature for 0.1-0.3 h, and the molar mass ratio of silane nucleotide to ultrafine high-magnesium brucite is controlled at 1-3 mol: 10 kg.

[0014] Further, in step 2), after activation, the mixture is cooled to room temperature and then further reduced to 5-15°C. Stirring continues for 0.1-0.4 hours at a rate of 100-300 r / min. Then, a cyclone separator is used for dust removal, controlling the dust removal rotation speed at 200-800 r / min, the air inlet velocity at 2-8 m / s, and the power at 100-600 W. Finally, flash drying is performed at a temperature of 180-200°C for 0.2-0.8 minutes, with an air inlet volume of 600-1200 m³ / min. 3 / h.

[0015] This invention also provides an application of nucleotide silane-magnesium hydroxide composite powder in micro-area viscosity monitoring of mineral wool slurry.

[0016] The beneficial effects of this invention are: This invention modifies active silane with natural guanylic acid and uses it for surface activation of natural high-magnesium brucite, forming an organic-inorganic hybrid core-shell composite powder. The guanylic acid silane forms the outer shell, and the high-magnesium brucite forms the core. This organic-inorganic hybrid core-shell composite material combines the natural product derivative guanylic acid silane with traditional inorganic mineral powders, giving the natural stone powder not only visual fluorescence and color-generating functions but also flame-retardant and smoke-suppressing properties. It integrates the unique advantages of guanylic acid silane and natural high-magnesium brucite into the composite powder particles, thereby achieving high-value applications of natural stone powders.

[0017] The silane-brucite composite powder provided by this invention has a relatively flexible conjugated chemical structure on its surface, which can release weak light signals in low-viscosity mineral wool slurry and strong light signals in high-viscosity mineral wool slurry. This allows for the detection and imaging of micro-area viscosity, a key physical indicator, providing a rapid, convenient, in-situ, and visualized monitoring effect for the consistency and formulation design of mineral wool slurry. This helps improve the efficiency of mineral wool slurry formulation design and facilitates rapid dilution during the construction process, thus helping construction workers find suitable construction techniques and greatly expanding the application potential of natural stone powder in mineral wool slurry.

[0018] This invention uses natural high-magnesium brucite as the main component of the composite powder. It employs silane to modify the natural product glycosidic acid, achieving controllable construction of the glycosidic acid silane. Both the natural glycosidic acid and ultrafine natural high-magnesium brucite are derived from nature, making them not only green and environmentally friendly but also abundant. This promotes the widespread application of natural products in natural stone powders, significantly contributing to the multifunctionality and greening of composite powders. Simultaneously, it conserves petroleum resources to a considerable extent, embodying the low-carbon concept. The ultrafine high-magnesium brucite itself has high whiteness, providing a certain degree of physical covering. Its main component is magnesium hydroxide, possessing both smoke-suppressing and flame-retardant properties, meeting the fire-retardant requirements of mineral wool adhesive. The natural glycosidic acid contains a large number of nitrogen-containing aromatic rings, as well as sugar rings and phosphate groups, which promote rapid charring of the substrate during combustion. It is a typical natural multi-component expandable functional system, exhibiting highly efficient synergistic flame-retardant effects with the internal high-magnesium brucite, satisfying the bonding, flame-retardant, and smoke-suppressing requirements of inorganic powders in mineral wool adhesive. Therefore, the silane-brucite composite powder of the present invention is an organic-inorganic functional composite powder achieved by combining silane-silane and high-magnesium brucite together.

[0019] The silane-brucite composite powder provided by this invention is prepared by a simple two-step method. The preparation process is simple and easy to carry out, without the dependence on complex equipment. The main raw materials are all natural products, which have typical green and environmentally friendly attributes. They are widely available and inexpensive, and do not require complicated post-processing. They are suitable for large-scale industrial applications and can also significantly reduce the dependence on fossil materials. The overall application cost is low and it has good low-carbon recycling characteristics. It has a great role in promoting the high-value transformation of traditional low-value natural stone powders and can also greatly expand the cross-border application of natural products in traditional chemical fields, especially in the field of high-value mineral wool mortar. Attached Figure Description

[0020] Figure 1 This is a schematic diagram of the structure of DTPTDP / UMH composite powder; Figure 2 This is a schematic diagram illustrating the detection mechanism of DTPTDP / UMH composite powder for liquids with different micro-region viscosities. Figure 3 SEM image of the DTPTDP / UMH composite powder prepared in Example 1; Figure 4 The images show the spectra of the DTPTDP / UMH composite powder prepared in Example 1 in solutions of different viscosities. Figure 5 The graph shows the linear fit of the logarithmic function between the fluorescence intensity and solution viscosity of the DTPTDP / UMH composite powder prepared in Example 1. Figure 6 The absorption spectra of the DTPTDP / UMH composite powder prepared in Example 1 in different polar solvents are shown. Figure 7 The image shows the photostability test results of the DTPTDP / UMH composite powder prepared in Example 1. Figure 8 The light signal release spectrum of the DTPTDP / UMH composite powder prepared in Example 1 in mineral wool slurry of different viscosities is shown. Detailed Implementation

[0021] This invention provides a silane-magnesium hydroxide composite powder, wherein the silane-magnesium hydroxide composite powder comprises a functional surface activation layer and a core. The functional surface activation layer is nucleotide silane, and the core is ultrafine high-magnesium brucite.

[0022] Furthermore, the ratio of the nucleotide silane to the ultrafine high-magnesium brucite is 1~3 mol:10 kg, preferably 1.5~2.5 mol:10 kg, and more preferably 2 mol:10 kg; The particle size of the nucleotide silane-brucite composite powder is 1.0~4.4μm, preferably 2.0~3.0μm, and more preferably 2.5μm.

[0023] This invention also provides a method for preparing silane-brucite composite powder, comprising the following steps: 1) Mix nucleotide and silane solution, carry out dehydration condensation reaction, and obtain nucleotide silane activator after post-treatment; 2) After preparing the silane activator into a solution, it is mixed with ultrafine high-magnesium brucite and activated to obtain silane-brucite composite powder.

[0024] In this invention, the particle size D of the ultrafine high-magnesium brucite is... 50 The micrometer size is 0.8~4.2μm, preferably 1.5~3.5μm, and more preferably 2.0~3.0μm; The silane in the silane solution is 3-trimethylsilylpropynaldehyde, and the nucleotide is 5'-cytidine. The solvent in the silane solution is one or more of tetrahydrofuran, acetonitrile, dimethyl sulfoxide, and N,N-dimethylformamide. The mixing of the nucleotide solution is carried out at 30~50°C, preferably 40°C. The mixing and stirring rate is 300~900 rpm, preferably 400~700 rpm, more preferably 500~600 rpm. The mixing time is 0.2~1.0 h, preferably 0.5 h.

[0025] In this invention, the molar ratio of the nucleotide and silane is 1:1 to 4, preferably 1:2 to 3, and more preferably 1:2.5; The dehydration condensation reaction is carried out in a high-pressure sealed tube, with the pressure controlled at 2~6 atm, preferably 3~5 atm, and more preferably 3~4 atm; the stirring temperature is 100~140℃, preferably 110~130℃, and more preferably 120℃; the stirring time is 2.0~6.0h, preferably 3.0~5.0h.

[0026] In this invention, the post-treatment in step 1) includes distillation, precipitation, and crystallization; The distillation is performed in a rotary evaporator to remove the reaction solvent. The distillation pressure is -0.09 to -0.07 MPa, preferably -0.08 MPa. The crude product is redispersed in a mixture of ethanol and purified water, with the volume ratio of ethanol to purified water controlled at 1:5 to 15, preferably 1:8 to 12. The solid content is controlled at 5 mg / mL to 10 mg / mL, preferably 6 to 8 mg / mL. The mixture is then allowed to stand at a low temperature of 1 to 10°C for 6 to 10 hours, preferably at 2 to 5°C for 7 to 8 hours. The mixed solvent is then removed by vacuum filtration, with the vacuum pressure controlled at -0.09 MPa to 0.07 MPa. Neutral fast filter paper is used for filtration, with 1 to 2 layers, and the filtration flow rate is controlled at 2 to 10 mL / s, preferably 4 to 8 mL / s, and more preferably 6 to 7 mL / s. The resulting crystalline product, silane glycoside activator, is obtained by low-temperature precipitation.

[0027] In this invention, in step 2), preparing the silane nucleotide activator into a solution involves mixing the silane nucleotide activator into a mixed solution, controlling the mixing rate to be 100-600 rpm, preferably 400-500 rpm; the mixing time is 0.1-0.9 h; the mixed solution is a mixture of an alcohol solvent and water, with a volume ratio of alcohol solvent to water of 1-3:1; the alcohol solvent includes one or more of methanol, ethanol, propanol, ethylene glycol and 1,2-propanediol; the concentration of the silane nucleotide activator in the solution is 1-5 mol / L, preferably 2-4 mol / L, and more preferably 3 mol / L.

[0028] In this invention, in step 2), the mixing method involves adding the silane nucleotide active solution to the high-speed rotating brucite powder via spraying. The spraying rate is 20-100 mL / min, preferably 40-80 mL / min. During the spraying process, the ultrafine high-magnesium brucite is preheated, and the stirring rate is controlled at 200-600 r / min, preferably 400-500 r / min. The preheating temperature is controlled at 50-80℃. After spraying, the temperature is raised to 90-120℃ for activation, preferably 100-110℃. The stirring rate is increased to 600-1000 r / min, preferably 700-800 r / min. The mixture is continuously stirred at the target temperature for 0.1-0.3 h, and the molar mass ratio of silane nucleotide to ultrafine high-magnesium brucite is controlled at 1-3 mol:10 kg, preferably 1.5-2.5 mol:10 kg, and more preferably 2 mol:10 kg.

[0029] In this invention, in step 2), after activation, the mixture is cooled to room temperature and further reduced to 5-15°C, preferably 8-12°C, and more preferably 10°C; stirring continues for 0.1-0.4 hours at a stirring rate of 100-300 r / min, preferably 150-250 r / min, and more preferably 200 r / min; then, a cyclone separator is used to separate and remove dust, controlling the dust removal rotation speed to 200-800 r / min, preferably 300-700 r / min, and more preferably 400-500 r / min; the air inlet velocity is 2-8 m / s, preferably 3-5 m / s; the power is 100-600 W, preferably 200-500 W; and then flash drying is further performed at a drying temperature of 180-200°C for 0.2-0.8 minutes, with an air inlet volume of 600-1200 m³ / min. 3 / h, preferably 700~1100m 3 / h, further preferably 800~1000m 3 / h.

[0030] In this invention, when the molar mass ratio of silane to ultrafine high-magnesium brucite is less than 1 mol: 10 kg, the amount of silane added may be too low, making it difficult to effectively modify and cover the ultrafine high-magnesium brucite, and also making it difficult to form a good functional coating layer. This will further reduce the subsequent loading of silane on the surface, resulting in a poor overall modification effect. However, when the molar mass ratio of silane to ultrafine high-magnesium brucite is higher than 3 mol: 10 kg, the amount of silane added may be too high, and may even cause multiple ultrafine high-magnesium brucite powder particles to be wrapped together, passively increasing the particle size. This will also lead to excessive enrichment of silane on the surface, resulting in uneven dispersion during processing and low spray modification efficiency.

[0031] This invention also provides an application of nucleotide silane-magnesium hydroxide composite powder in micro-area viscosity monitoring of mineral wool slurry.

[0032] In this invention, the method of application includes: mixing silane-magnesium hydroxide composite powder with mineral wool slurry, and determining the micro-area viscosity of the mineral wool slurry by detecting the intensity of the light signal.

[0033] The technical solutions provided by the present invention will be described in detail below with reference to the embodiments, but they should not be construed as limiting the scope of protection of the present invention.

[0034] Example 1

[0035] (1) 323.6 g of nucleotide acid (1 mol) was added to acetonitrile and stirred at 500 rpm for 0.6 h at 45 °C. Then, 252.5 g of silane was added to the nucleotide acid solution and placed in a high-pressure sealed tube. The pressure was controlled at 4 atm, the stirring temperature was 120 °C, and the stirring time was 4.0 h until the reaction was completed, and crude product of nucleotide acid silane activator was obtained. The nucleotide acid was 5'-cytidine acid, and the silane was 3-trimethylsilylpropynaldehyde. The post-processing mainly involves distillation, precipitation, and crystallization. The distillation process involves removing the reaction solvent in a rotary evaporator at a pressure of -0.08 MPa. The crude product is then redispersed as a solid in a mixture of ethanol and purified water, with the volume ratio of ethanol to purified water controlled at 1:10 and the solid content controlled at 8 mg / mL. The mixture is then allowed to stand for 8 hours at a low temperature (5°C). The mixed solvent is then removed by vacuum filtration, with the vacuum pressure controlled at -0.08 MPa. Neutral, fast-drying filter paper is used for filtration, with one layer, and the filtration flow rate controlled at 6 mL / s. The resulting crystallized product, silane glycoside surfactant, is obtained at low temperature.

[0036] (2) 862.8 g of silane activator was added to a mixed solution of ethanol and purified water, the volume ratio of ethanol to purified water was controlled at 2:1, the mixing rate was controlled at 300 rpm, the mixing time was 0.5 h, and the mixture was directly mixed at room temperature. The concentration of the silane activator solution was 3 mol / L. The active solution of silane nucleotide was added to 10 kg of high-speed rotating brucite powder by spraying at a spray rate of 60 mL / min. The ultrafine high-magnesium brucite was preheated before spraying, and the stirring rate was controlled at 400 r / min and the preheating temperature was controlled at 60°C. After spraying, the temperature was raised to 100°C and the stirring rate was increased to 800 r / min. The mixture was stirred continuously at the target temperature for 0.2 h. After stirring, the mixture was cooled to room temperature, then further cooled to 10°C, and stirred for another 0.2 hours at a stirring rate of 200 r / min. Following this, a cyclone separator was used for dust removal, with the dust removal rotation speed controlled at 600 r / min, the air inlet velocity at 5 m / s, and the power at 300 W. Subsequent flash drying was then performed at 190°C for 0.5 minutes, with an air inlet volume of 900 m³ / min. 3 / h, silane-magnesium hydroxide composite powder was obtained with a median particle size of 1.0~4.4μm.

[0037] Example 2

[0038] (1) 323.6 g of nucleotide acid (1 mol) was added to acetonitrile and stirred at 900 rpm for 1.0 h at 30 °C. Then, 126.2 g of silane was added to the nucleotide acid solution and placed in a high-pressure sealed tube. The pressure was controlled at 2 atm, the stirring temperature was 100 °C, and the stirring time was 6.0 h until the reaction was completed, and crude product of nucleotide acid silane activator was obtained. The nucleotide acid was 5'-cytidine acid, and the silane was 3-trimethylsilylpropynaldehyde. The post-processing mainly involves distillation, precipitation, and crystallization. The distillation process involves removing the reaction solvent in a rotary evaporator at a pressure of -0.09 MPa. The crude product is then redispersed as a solid in a mixture of ethanol and purified water, with the volume ratio of ethanol to purified water controlled at 1:5 and the solid content controlled at 5 mg / mL. The mixture is then allowed to stand at a low temperature (1°C) for 6 hours. The mixed solvent is then removed by vacuum filtration, with the vacuum pressure controlled at -0.09 MPa. Neutral fast filter paper (2 layers) is used for vacuum filtration, and the flow rate is controlled at 2 mL / s to obtain the crystalline product, silane nucleotide activator, precipitated at low temperature.

[0039] (2) 431.1g of silane glycoside activator was added to a mixed solution of ethanol and purified water, the volume ratio of ethanol to purified water was controlled at 1:1, the mixing rate was controlled at 100rpm, the mixing time was 0.9h, and the mixture was directly mixed at room temperature. The concentration of the silane glycoside activator solution was 1mol / L. The active solution of silane nucleotide was added to 10 kg of high-speed rotating brucite powder by spraying at a spray rate of 20 mL / min. The ultrafine high-magnesium brucite was preheated before spraying, and the stirring rate was controlled at 200 r / min and the preheating temperature was controlled at 50°C. After spraying, the temperature was raised to 90°C and the stirring rate was increased to 600 r / min. The mixture was stirred continuously at the target temperature for 0.3 h. After stirring, the mixture was cooled to room temperature, then further cooled to 5°C, and stirred for another 0.1 hours at a stirring rate of 100 r / min. Following this, a cyclone separator was used for dust removal, with the dust removal rotation speed controlled at 200 r / min, the air inlet velocity at 2 m / s, and the power at 100 W. Subsequent flash drying was then performed at 180°C for 0.2 minutes, with an air inlet volume of 600 m³ / min. 3 / h, silane-magnesium hydroxide composite powder was obtained with a median particle size of 1.0~4.4μm.

[0040] Example 3

[0041] (1) 323.6 g of nucleotide acid (1 mol) was added to acetonitrile and stirred at 300 rpm for 0.2 h at 50 °C. Then, 504.8 g of silane was added to the nucleotide acid solution and placed in a high-pressure sealed tube. The pressure was controlled at 6 atm, the stirring temperature was 140 °C, and the stirring time was 2.0 h until the reaction was completed, and crude product of nucleotide acid silane activator was obtained. The nucleotide acid was 5'-cytidine acid, and the silane was 3-trimethylsilylpropynaldehyde. The post-processing mainly involves distillation, precipitation, and crystallization. The distillation process involves removing the reaction solvent in a rotary evaporator at a pressure of -0.07 MPa. The crude product is then redispersed as a solid in a mixture of ethanol and purified water, with the volume ratio of ethanol to purified water controlled at 1:15 and the solid content controlled at 10 mg / mL. The mixture is then allowed to stand for 10 hours at a low temperature (10°C). The mixed solvent is then removed by vacuum filtration, with the vacuum pressure controlled at -0.07 MPa. Neutral, fast-drying filter paper is used for filtration, with one layer and the filtration flow rate controlled at 10 mL / s, yielding the crystalline product, silane nucleotide activator, precipitated at low temperature.

[0042] (2) 1293.3g of silane glycosidic acid activator was added to a mixed solution of ethanol and purified water, the volume ratio of ethanol to purified water was controlled at 1:1, the mixing rate was controlled at 600rpm, the mixing time was 0.1h, and the mixture was directly mixed at room temperature. The concentration of the silane glycosidic acid activator solution was 5mol / L. The silane nucleotide active solution was added to 10 kg of high-speed rotating brucite powder by spraying at a rate of 100 mL / min. The ultrafine high-magnesium brucite was preheated before spraying, and the stirring rate was controlled at 600 r / min. The preheating temperature was controlled at 80°C. After spraying, the temperature was raised to 120°C and the stirring rate was increased to 1000 r / min. The mixture was stirred continuously at the target temperature for 0.1 h. After stirring, the mixture was cooled to room temperature, then further cooled to 15°C, and stirred for another 0.4 hours at a stirring rate of 300 r / min. Following this, a cyclone separator was used for dust removal, with the dust removal rotation speed controlled at 800 r / min, the air inlet velocity at 8 m / s, and the power at 600 W. Subsequent flash drying was then performed at 200°C for 0.8 minutes, with an air inlet volume of 1200 m³ / min. 3 / h, silane-magnesium hydroxide composite powder was obtained with a median particle size of 1.0~4.4μm.

[0043] Comparative Example 1

[0044] (1) Same as Example 1; (2) 215.6g of silane glycosidic acid activator was added to a mixed solution of ethanol and purified water, the volume ratio of ethanol to purified water was controlled at 2:1, the mixing rate was controlled at 300rpm, the mixing time was 0.5h, and the mixture was directly mixed at room temperature. The concentration of the silane glycosidic acid activator solution was 3mol / L. The active solution of silane nucleotide was added to 10 kg of high-speed rotating brucite powder by spraying at a spray rate of 60 mL / min. The ultrafine high-magnesium brucite was preheated before spraying, and the stirring rate was controlled at 400 r / min and the preheating temperature was controlled at 60°C. After spraying, the temperature was raised to 100°C and the stirring rate was increased to 800 r / min. The mixture was stirred continuously at the target temperature for 0.2 h. After stirring, the mixture was cooled to room temperature, then further cooled to 10°C, and stirred for another 0.2 hours at a stirring rate of 200 r / min. Following this, a cyclone separator was used for dust removal, with the dust removal rotation speed controlled at 600 r / min, the air inlet velocity at 5 m / s, and the power at 300 W. Subsequent flash drying was then performed at 190°C for 0.5 minutes, with an air inlet volume of 900 m³ / min. 3 / h, silane-magnesium hydroxide composite powder was obtained with a median particle size of 1.0~4.4μm.

[0045] Comparative Example 2

[0046] (1) Same as Example 1; (2) 1724.4g of silane glycoside activator was added to a mixed solution of ethanol and purified water, the volume ratio of ethanol to purified water was controlled at 2:1, the mixing rate was controlled at 300rpm, the mixing time was 0.5h, and the mixture was directly mixed at room temperature. The concentration of the silane glycoside activator solution was 3mol / L. The active solution of silane nucleotide was added to 10 kg of high-speed rotating brucite powder by spraying at a spray rate of 60 mL / min. The ultrafine high-magnesium brucite was preheated before spraying, and the stirring rate was controlled at 400 r / min and the preheating temperature was controlled at 60°C. After spraying, the temperature was raised to 100°C and the stirring rate was increased to 800 r / min. The mixture was stirred continuously at the target temperature for 0.2 h. After stirring, the mixture was cooled to room temperature, then further cooled to 10°C, and stirred for another 0.2 hours at a stirring rate of 200 r / min. Following this, a cyclone separator was used for dust removal, with the dust removal rotation speed controlled at 600 r / min, the air inlet velocity at 5 m / s, and the power at 300 W. Subsequent flash drying was then performed at 190°C for 0.5 minutes, with an air inlet volume of 900 m³ / min. 3 / h, silane-magnesium hydroxide composite powder was obtained with a median particle size of 1.0~10.8μm.

[0047] Comparative Example 3

[0048] Unrefined, ultrafine high-magnesium brucite.

[0049] Performance testing

[0050] 1. The oil absorption value and specific surface area of ​​the nucleotide silane-brucite composite powders prepared in Examples 1-3 and Comparative Examples 1-3, as well as the ultrafine high magnesium brucite in Comparative Example 3, were tested. The test results are shown in Table 1. Oil absorption: tested according to DB / T5211.15-2014 standard; Specific surface area: tested using BET specific surface area.

[0051] Table 1. Oil absorption value and specific surface area test results of the nucleotide silane-brucite composite powders prepared in Examples 1-3 and Comparative Examples 1-3, as well as ultrafine high-magnesium brucite.

[0052] As can be seen from the test results of Examples 1-3 in Table 1, after adding a suitable molar concentration of natural nucleotide silane to modify UMH, the oil absorption value of the composite powder decreased significantly, from a maximum of 58 mL / 100g to 26 mL / 100g. This may be because the natural nucleotide silane on the surface can effectively coat the internal UMH, effectively shielding the surface hydroxyl groups of ultrafine high-magnesium brucite and reducing the polarity of the overall composite powder. In addition, the specific surface area of ​​the composite powder increased significantly, which may be related to the passivation of surface polarity. The introduction of natural nucleotide silane can improve the dispersion state of the powder, effectively reduce the agglomeration effect between powders, and form better dispersed particles.

[0053] In contrast, when the amount of natural bismuth substrate added is too small (molar mass ratio below 1 mol:10 kg, as in Comparative Example 1) or too large (molar mass ratio above 3 mol:10 kg, as in Comparative Example 2), it exhibits a poor modification effect on UMH. This is reflected in the limited decrease in oil absorption value, only decreasing from the original 58 mL / 100 g to 45~52 mL / 100 g, while the oil absorption value remains relatively high. Regarding specific surface area, when the amount of natural bismuth substrate added is too small or too large, the increase in specific surface area is not significant. This may be because when the molar ratio of natural bismuth substrate is low, the modification effect on UMH is limited, making it difficult to achieve a good shielding effect, thus easily leading to agglomeration. When the molar ratio of natural bismuth substrate is too large, it may coat multiple UMH powder particles together, passively reducing the specific surface area. These results indicate that adding an appropriate proportion of natural bismuth substrate can effectively improve the surface polarity of natural UMH and the overall performance of the bismuth substrate-brucite composite powder.

[0054] 2. Figure 3 The image shows a SEM image of the silane-brucite composite powder prepared in Example 1; (The image is from...) Figure 3 It can be seen that the surface of the composite powder also has a relatively uniform and dense coating layer, and the entire composite powder is wrapped with particles, indicating that the natural nucleotide silane has a good coating effect on the surface of ultrafine high magnesium brucite.

[0055] 3. Spectroscopic testing of DTPTDP / UMH composite powder

[0056] (1) Spectroscopic testing of DTPTDP / UMH composite powder in solution atmospheres of different viscosities: Solutions of different viscosities were prepared using glycerol and deionized water with different volume fractions. The DTPTDP / UMH composite powder prepared in Example 1 was added to these solutions. Before testing, the solution was allowed to stand at room temperature for a period of time. The concentration of the added DTPTDP / UMH composite powder in the solution was controlled to be 10 μM, and the excitation wavelength was 310 nm. The measured spectra are shown below. Figure 4 As shown, the data is listed in Table 2.

[0057] Table 2 Optical signal intensity of DTPTDP / UMH composite powder in solution atmospheres of different viscosities

[0058] from Figure 4As shown in Table 2, the intensity of the emitted light signal becomes more and more significant as the solution viscosity gradually increases (1.0 cP~956.0 cP), indicating that the DTPTDP / UMH composite powder can have a good response effect to the viscosity of the micro-area. This may be because the chemical structure of the large number of natural nucleotide silanes on the surface contains freely rotating conjugated triple bonds, which can rotate freely in the low viscosity solution atmosphere, but the rotation is restricted in the high viscosity solution atmosphere. The excited state energy is converted from non-radiative transition to radiative transition, and the light signal appears to be strong, increasing by about 41 times overall (as shown in Table 2). It can be seen that the DTPTDP / UMH composite powder can achieve in-situ, efficient and visualized detection of micro-area viscosity.

[0059] Figure 5 The graph shows the logarithmic function linear fit of the fluorescence intensity and solution viscosity (Table 2) of the DTPTDP / UMH composite powder prepared in Example 1; Figure 5 It can be seen that the logarithmic function of luminescence intensity and the logarithmic function of viscosity exhibit a typical linear relationship, indicating that the light intensity emitted by the probe is well dependent on viscosity, and its viscosity sensitivity coefficient is 0.55, indicating that it has good sensitivity to viscosity and is suitable for use as a micro-area viscosity measurement in mineral wool slurry.

[0060] (2) Absorption spectra of DTPTDP / UMH composite powder in different polar solvents: Mineral wool adhesive requires the addition of various solvents due to functional requirements, resulting in significant differences in polarity. Therefore, the signal stability of DTPTDP / UMH composite powder in various solvent systems is crucial.

[0061] Test solutions of 10 mM DTPTDP / UMH composite powder were prepared using different solvents: The DTPTDP / UMH composite powder prepared in Example 1 was added to six common solvents: dimethyl sulfoxide, methanol, purified water, tetrahydrofuran, ethyl acetate, and dichloromethane. The absorption spectra of the powder in these solvents of different polarities were measured at room temperature. The results are shown below. Figure 6 As shown.

[0062] from Figure 6 It can be seen that the absorption spectral peaks of the DTPTDP / UMH composite powder in various solvents of different polarities are basically around 310 nm, and the absorbance is also relatively similar (all around 0.9), indicating that it is inert to changes in solution polarity and has low dependence on solvent polarity. This demonstrates that the DTPTDP / UMH composite powder is suitable for use in solvents of various polarities.

[0063] (3) Light stability test of DTPTDP / UMH composite powder: A 10 μM DTPTDP / UMH composite powder solution was prepared using a solvent and added to a high-viscosity solution (99% v / v glycerol). The solution was then irradiated for different durations (0 min, 10 min, 20 min, 30 min, and 60 min) under a 365 nm excitation source. The photostability of the powder within 60 min under different irradiation durations was tested, and the results are as follows: Figure 7 As shown. From Figure 7 It can be seen that the DTPTDP / UMH composite powder can still release strong light signals under long-term irradiation, and its light stability is excellent. It is suitable for long-term existence in mineral wool slurry and can exert its effectiveness. It is not easily photobleached by ultraviolet radiation.

[0064] (4) Application of DTPTDP / UMH composite powder in mineral wool mortar of different viscosities: The DTPTDP / UMH composite powder prepared in Example 1 was dispersed in three different mineral wool pastes under stirring conditions. The stirring speed was 600 r / min, the stirring temperature was 25℃, and the stirring time was 2 h. The concentration of the DTPTDP / UMH composite powder in the mineral wool paste was 10 μM. The light signal intensity was detected using a handheld ultraviolet lamp, and the results are as follows: Figure 8 As shown.

[0065] from Figure 8 It can be seen that the apparent signal intensity of the three mineral wool slurries is not the same, indicating that their viscosities are not the same and there are significant differences. The DTPTDP / UMH composite powder can effectively sense this change in the above mineral wool slurries, and the specific values ​​are shown in Table 3.

[0066] The components and contents of mineral wool slurry 1 in Table 3 are as follows: 15.0 parts phenolic resin, 10.0 parts sodium silicate, 60.0 parts purified water, 0.2 parts hydroxyethyl cellulose, 0.2 parts sodium polyacrylate, 2.0 parts silicone emulsion, and 5 parts DTPTDP / UMH composite powder obtained in Example 1; the viscosity of this mineral wool slurry 1 is 238.8 cP. The composition and content of mineral wool slurry 2 are as follows: 2.0 parts hydroxyethyl cellulose, 55.0 parts purified water, and the rest are the same as those of mineral wool slurry 1; the viscosity of this mineral wool slurry 2 is 675.9 cP. The composition and content of mineral wool slurry 3 are as follows: 8.0 parts of hydroxyethyl cellulose and 50.0 parts of purified water. The other components are the same as those of mineral wool slurry 1. The viscosity of this mineral wool slurry 3 is 871.2 cP.

[0067] Table 3 Optical signal intensity of DTPTDP / UMH composite powder in mineral wool slurry of different viscosities

[0068] The results show that the DTPTDP / UMH composite powder has a good response effect to mineral wool mortars of different viscosities, and its response is positively correlated with the viscosity. Therefore, the intensity of the surface signal can be used to perceive the change in viscosity, which can provide a visual reference and judgment for the preparation process of mineral wool mortars and the consistency adjustment in on-site construction.

[0069] As can be seen from the above embodiments, this invention combines natural bismuth sub-nucleotide silane (DTPTDP) with naturally occurring brucite (UMH) to prepare a bismuth sub-nucleotide silane-brucite composite powder based on the natural product cytidine. This fully utilizes the rotatability of the conjugated triple bond structure of DTPTDP to detect the viscosity of mineral wool slurry. Furthermore, the addition of sinapic acid (DTPTDP) not only reduces the surface polarity of natural ultrafine brucite and improves its compatibility in the mineral wool slurry base, but also significantly reduces the oil absorption value of natural ultrafine brucite, offering a significant advantage in improving the overall performance of the composite powder.

[0070] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A glycosylated silane-brucite composite powder, characterized by, The silane-ribonucleotide and brucite composite powder comprises a functional surface activation layer and a core; The functional surface activation layer is silane-ribonucleotide, and the core is superfine high-magnesium brucite. 2.The silane-silicate brucite composite powder according to claim 1, characterized in that, The silane-ribonucleotide and superfine high-magnesium brucite are used in a ratio of 1-3 mol:10 kg. The silane-ribonucleotide and brucite composite powder has a particle size of 1.0-4.4 μm.

3. The method for producing the silane-silicate glycolate composite powder according to claim 1 or 2, characterized by, The method comprises the following steps: 1) mixing a silane solution and a ribonucleotide solution to perform a dehydration condensation reaction, and obtaining a silane-ribonucleotide activator after post-treatment; 2) mixing the silane-ribonucleotide activator prepared into a solution with superfine high-magnesium brucite to perform activation, and obtaining a silane-ribonucleotide and brucite composite powder.

4. The method for preparing the nucleotide silane-brucite composite powder according to claim 3, characterized in that, The particle size D of the superfine high-magnesium brucite is 0.8-4.2 μm. 50 0.8-4.2 μm. The silane in the silane solution is 3-trimethylsilyl propargyl aldehyde, the ribonucleotide is 5'-cytidylic acid, the solvent in the silane solution is one or more of tetrahydrofuran, acetonitrile, dimethyl sulfoxide and N,N-dimethylformamide, the mixing of the ribonucleotide solution is performed at 30-50 ℃, the mixing stirring rate is 300-900 rpm, and the mixing time is 0.2-1.0 h.

5. The method for preparing the nucleotide silane-brucite composite powder according to claim 4, characterized in that, The molar ratio of the ribonucleotide and the silane is 1:1-4. The dehydration condensation reaction is performed in a high-pressure sealed tube, the pressure is controlled at 2-6 atm, the stirring temperature is 100-140 ℃, and the stirring time is 2.0-6.0 h.

6. The method for preparing the silane-silicate acid hydrate composite powder according to claim 3 or 5, characterized in that, In step 1), the post-treatment comprises distillation, precipitation and crystallization. The distillation is to remove the reaction solvent under a rotary evaporator, the pressure of the distillation is -0.09 to -0.07 MPa, the crude product is redispersed into a mixed solution of ethanol and purified water, the volume ratio of ethanol and purified water is controlled at 1:5-15, the solid content is controlled at 5 mg / mL-10 mg / mL, then the mixture is placed in a low-temperature environment of 1-10 ℃ for 6-10 h, and then the mixed solvent is removed by suction filtration under a reduced pressure of -0.09 MPa to 0.07 MPa, the suction filtration is performed using neutral rapid filter paper, 1-2 layers, the suction filtration flow rate is controlled at 2-10 mL / s, and a crystalline product of the silane-ribonucleotide activator is obtained by low-temperature precipitation.

7. The method for preparing the nucleotide silane-brucite composite powder according to claim 6, characterized in that, In step 2), the preparation of the silane-ribonucleotide activator into a solution is to mix the silane-ribonucleotide activator into a mixed solution, the mixing rate is controlled at 100-600 rpm, and the mixing time is 0.1-0.9 h; the mixed solution is a mixture of an alcohol solvent and water, the volume ratio of the alcohol solvent and water is 1-3:1, the alcohol solvent comprises one or more of methanol, ethanol, propanol, ethylene glycol and 1,2-propanediol, and the concentration of the silane-ribonucleotide activator in the solution is 1-5 mol / L.

8. The method for preparing the silane-silicate acid hydrate composite powder according to claim 3 or 7, characterized in that, In the step 2), the mixing is achieved by spraying the silane solution into the high-speed rotating brucite powder, the spraying rate is 20-100 mL / min, the superfine high-magnesium brucite is preheated during the spraying process, the stirring rate is controlled to be 200-600 r / min, the preheating temperature is controlled to be 50-80℃; after the spraying is completed, the temperature is raised to 90-120℃ for activation, the stirring rate is raised to 600-1000 r / min, the stirring is continuously performed at the target temperature for 0.1-0.3 h, and the molar mass ratio of the silane to the superfine high-magnesium brucite is controlled to be 1-3 mol:10 kg.

9. The method for preparing the nucleotide silane-brucite composite powder according to claim 8, characterized in that, In the step 2), after the activation is finished, the temperature is cooled to room temperature, and then the temperature is further reduced to 5-15℃, the stirring is continuously performed for 0.1-0.4h at a stirring speed of 100-300r / min, then the dust is separated by a cyclone separator, the rotating speed for dust removal is controlled to be 200-800r / min, the air inlet speed is 2-8m / s, and the power is 100-600W, then flash drying is further performed, the drying temperature is 180-200℃, the drying time is 0.2-0.8min, and the air inlet amount is 600-1200m 3 / h.

10. Application of the silane-brucite composite powder in claim 1 or 2 in mineral wool slurry micro-zone viscosity monitoring.

Images