Double-sided magnesium oxychloride rock wool manual purification board and its preparation method
By combining modified rock wool and modified hydrophobic coatings, heat-treated nanofibers are prepared by electrospinning technology, which solves the problems of poor fire resistance, moisture resistance and mechanical properties of existing double-sided glass magnesium rock wool hand purified plates, and achieves the performance improvement of the board.
Patent Information
- Application Number
- CN202411497360.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-25
- Publication Date
- 2025-06-13
- Estimated Expiration
- 2044-10-25
AI Technical Summary
The existing double-sided glass magnesium rock wool hand-purified plates have poor fire resistance, moisture resistance and mechanical properties.
Modified rock wool and modified hydrophobic coatings are used to prepare heat-treated nanofibers through electrospinning technology, and mixed with rock wool substrate and diatomaceous earth, curing and heat-treating to form modified rock wool. At the same time, a modified hydrophobic coating is used to coat the surface of the board, and a double-sided glass magnesium rock wool hand-cleaning plate is formed after polymerization.
It significantly improves the mechanical properties, fire resistance and moisture resistance of double-sided glass magnesium rock wool hand purifier boards, and meets the industry standards of high precision and high cleanliness requirements.
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Figure BDA0005101612480000051
Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of the preparation of manual purification boards, and particularly relates to a double-sided glass magnesium rock wool manual purification board and a preparation method thereof. Background Art
[0002] With the acceleration of the global industrialization process, especially in industries with high-precision and high-cleanliness requirements such as biopharmaceuticals, medical treatment, food processing, and electronic manufacturing, higher requirements are put forward for the cleanliness, safety, and energy efficiency of the production environment. Traditional building materials often cannot fully meet these special requirements in terms of fire prevention, dust prevention, anti-static, sound insulation, heat insulation, and thermal insulation, which has promoted the research and application of double-sided glass magnesium rock wool manual purification boards.
[0003] The double-sided glass magnesium rock wool manual purification board uses a magnesium oxide board as the base material. This base material itself has excellent fire prevention, moisture resistance, corrosion resistance, etc. characteristics, and the production process is environmentally friendly, meeting the national green building material standards. At the same time, the rock wool material filled inside endows the board with excellent heat insulation and sound absorption effects, effectively improving the energy utilization efficiency and indoor comfort of the building. Through a fine composite technology, the metal outer plate, magnesium oxide core material, and rock wool layer are closely combined to form a highly integrated and structurally stable board system. This structure not only enhances the mechanical strength of the board but also significantly improves the fire prevention, dust prevention, anti-static, etc. performance, enabling it to maintain a stable use state in various harsh environments.
[0004] Patent CN 221067370 U discloses a manual magnesium oxide rock wool purification board, including a housing. Reinforcing ribs are provided on the inner sides of the housing. Multiple magnesium oxide boards are provided on the inner sides of the reinforcing ribs and inside the inserting strips. Rock wool boards are provided on the inner sides of the multiple magnesium oxide boards. Slots are provided on both sides of the housing, and inserting strips are provided on the front and back sides. A stopper is provided at a corner of the housing between the slots and the inserting strips. By directly inserting the inserting strips into the slots, the splicing of the housing is more convenient. At the same time, by rotating and flipping the housing, the position of the stopper is always at the diagonals of the four housings, avoiding gaps at the diagonals of the four housings. At the same time, by wrapping the rock wool board with two magnesium oxide boards and dispersing multiple magnesium oxide boards inside the housing through the reinforcing ribs, the fire resistance rating of the purification board is improved, the compressive strength is improved, and the surface flatness is improved. However, there is still room for improvement in the fire resistance, moisture resistance, and mechanical properties of the purification board prepared by this method. Summary of the Invention
[0005] The purpose of the present invention is to provide a double-sided glass magnesium rock wool manual purification board and a preparation method thereof, which are used to solve the technical problems of poor fire resistance, moisture resistance, and mechanical properties of the purification board in the prior art.
[0006] To achieve the above purpose, the present invention adopts the following technical solutions:
[0007] The present invention provides a double-sided glass magnesium rock wool manual purification board, which is composed of the following components in parts by weight: 20-30 parts of modified rock wool, 30-50 parts of glass magnesium board, 10-13 parts of adhesive, and 6-9 parts of modified hydrophobic coating, wherein the modified rock wool is prepared from 4,4'-diaminodiphenyl ether, pyromellitic acid dianhydride, zirconium oxychloride octahydrate, rock wool substrate and diatomaceous earth, and the modified hydrophobic agent is prepared from octafluoropentanol, isophorone diisocyanate 、 3-aminopropylene, dimethacrylate polyethylene glycol ether and acrylic acid are prepared.
[0008] Preferably, the method for preparing the modified rock wool comprises the following steps:
[0009] Q1: 4,4'-diaminodiphenyl ether is added to a container containing N,N-dimethylformamide for reaction at low temperature, followed by adding pyromellitic anhydride, and stirring thoroughly to obtain a spinning solution, and the spinning solution is prepared into nanofibers using electrospinning technology, and subjected to heat treatment to obtain heat-treated nanofibers;
[0010] Q2: Add zirconium oxychloride octahydrate to distilled water, adjust the pH with ammonia water, heat treat, wash, and vacuum dry to obtain a white powder, ultrasonically disperse the white powder into ethanol, slowly drop silane coupling agent KH-560, ultrasonically disperse, heat to reflux, centrifuge, wash, and dry to obtain a modified powder;
[0011] Q3: Ultrasonic dispersion of the modified powder in ethanol, then addition of heat-treated nanofibers, soaking, washing, drying, and heating treatment to obtain modified nanofibers;
[0012] Q4: The rock wool substrate, modified nanofibers and diatomaceous earth are mixed, cured, cleaned, dried and heat-treated to obtain modified rock wool.
[0013] In the above process, 4,4'-diaminodiphenyl ether and pyromellitic anhydride are first used as raw materials to prepare heat-treated nanofibers, and then zirconium oxychloride octahydrate, ammonia water and silane coupling agent KH-560 are used as raw materials to prepare modified powders. Then, the modified powder nanolayer is in situ grown on the surface of the heat-treated nanofibers by in-situ polar adsorption technology to prepare modified nanofibers with a core-shell structure, and then the rock wool substrate, the modified nanofibers and diatomaceous earth are used as raw materials to prepare modified rock wool, wherein the synthesis reaction formula of the heat-treated nanofibers is as follows:
[0014]
[0015] Preferably, in Q1, the dosage ratio of 4,4'-diaminodiphenyl ether, N,N-dimethylformamide and pyromellitic dianhydride is (9.25 - 12.03) g : (130 - 169) mL : (10.08 - 13.1) g. The low-temperature reaction temperature is 0 - 3 °C, the reaction time is 2 - 3 h, the sufficient stirring time is 3 - 5 h. The parameters of the electrospinning technique are: the ambient temperature is 25 °C, the ambient humidity is 40%, the spinning voltage is 20 - 22 kV, the syringe propulsion speed is 0.8 mL / h. Using an aluminum foil as the receiving substrate and closely attaching it to the receiving roller, the distance between the receiving roller and the syringe is 18 cm, the roller rotation speed is 450 rpm, the spinning time is 10 - 12 h. The heat treatment process is: heating from room temperature to 100 °C in 0.5 h and holding for 2 h, then heating to 300 °C in 2 h and holding for 2 h.
[0016] Preferably, in Q2, the dosage ratio of zirconium oxychloride octahydrate and distilled water is (32.25 - 38.7) g : (1 - 1.2) L. Adjust the pH to 9.8 - 10.2, the heat treatment temperature is 180 - 200 °C, the time is 2 - 4 h. After washing with distilled water, wash with absolute ethanol. The dosage ratio of the white powder, ethanol and silane coupling agent KH-560 is (1 - 3) g : (6 - 10) mL : (2 - 4) mL. The ultrasonic dispersion time is 30 - 45 min, and the ultrasonic dispersion time after adding the silane coupling agent KH-560 is 30 - 60 min. The reflux time is 5 - 7 h.
[0017] Preferably, in Q3, the dosage ratio of the modified powder, ethanol and heat-treated nanofibers is (1 - 3) g : (8 - 12) mL : (2 - 4) g. The soaking time is 4 - 7 h, wash with deionized water, the drying time is 20 - 24 h. The heating treatment is: heating from room temperature to 400 °C in 2 h and holding for 1 h. In Q4, the mass ratio of the rock wool substrate, modified nanofibers and diatomite is (30 - 50) : (3 - 6) : (8 - 12).
[0018] Preferably, the preparation method of the modified hydrophobic coating includes the following steps:
[0019] S1: Dissolve octafluoropentanol and isophorone diisocyanate in acetone respectively, then mix and add dibutyltin dilaurate, and then pour it into a three-necked flask equipped with a condensing reflux device, a nitrogen protection device and an electric stirrer. After the reaction is complete, cool down, add 3-aminopropene and continue to react, heat to remove acetone to obtain fluorinated alcohol.
[0020] S2: Heat polyethylene glycol dimethacrylate, then add acrylic acid and 1-butyl-3-methylimidazolium tetrafluoroborate into a container, stir until evenly mixed, cool, add fluorinated alcohol and 2,2-diethoxyacetophenone, and stir magnetically until evenly mixed to obtain a modified hydrophobic coating.
[0021] In the above process, the synthesis reaction formula of the modified hydrophobic coating is as follows:
[0022]
[0023] Preferably, in S1, the molar ratio of octafluoropentanol, isophorone diisocyanate, and 3-aminopropene is (0.9 - 1.1):(0.8 - 1.1):(1 - 1.2), the reaction temperature is 60 - 80 °C, and the reaction time is 3 - 5 h.
[0024] Preferably, in S2, the dosage ratio of polyethylene glycol dimethacrylate, acrylic acid, 1-butyl-3-methylimidazolium tetrafluoroborate, fluorinated alcohol, and 2,2-diethoxyacetophenone is (0.12 - 0.18) g:(0.3 - 0.45) mL:(0.23 - 0.34) mL:(2.23 - 3.34) g:(0.05 - 0.075) mL, the heating temperature is 60 - 70 °C, the stirring time is 1 - 2 h, and the magnetic stirring time is 5 - 10 min.
[0025] Preferably, the preparation method of the double-sided glass magnesium rock wool manual purification board includes the following steps:
[0026] Step (1): Evenly apply an adhesive on the surfaces of the modified rock wool and the glass magnesium board, then combine the two and compact them to obtain a double-sided glass magnesium rock wool board.
[0027] Step (2): Evenly apply the modified hydrophobic coating on the surface of the double-sided glass magnesium rock wool board, then place it in an ultraviolet box and polymerize for 2 - 4 h to obtain a double-sided glass magnesium rock wool manual purification board.
[0028] In summary, due to the adoption of the above technical solutions, the beneficial effects of the present invention are as follows:
[0029] 1. The present invention first uses 4,4'-diaminodiphenyl ether, pyromellitic dianhydride, zirconium oxychloride octahydrate, silane coupling agent KH-560, rock wool substrate, and diatomaceous earth as raw materials to prepare modified rock wool. Subsequently, octafluoropentanol, isophorone diisocyanate, 3-aminopropene, polyethylene glycol dimethacrylate, acrylic acid, and 2,2-diethoxyacetophenone are used as raw materials to prepare a modified hydrophobic coating. Placing the modified rock wool between the glass magnesium boards and coating the modified hydrophobic coating on the surface of the glass magnesium boards can effectively improve the mechanical properties, fire resistance, and moisture resistance of the double-sided glass magnesium rock wool manual purification board.
[0030] 2. The present invention uses 4,4'-diaminodiphenyl ether and pyromellitic dianhydride as raw materials to prepare heat-treated nanofibers. Subsequently, zirconium oxychloride octahydrate and silane coupling agent KH-560 are used as raw materials to prepare a modified powder. The two are compounded to prepare modified nanofibers. The heat-treated nanofibers have excellent mechanical properties. As a reinforcing phase, they are added to the rock wool substrate to play a framework role, significantly improving the overall mechanical properties of the modified rock wool. Moreover, the small size and high specific surface area of the heat-treated nanofibers enable them to be evenly distributed in the rock wool substrate, forming an effective stress transfer network, enhancing the strength and toughness of the rock wool. The modified nanofibers have a core-shell structure, which not only retains the original high-strength characteristics of the nanofibers but also increases the interfacial bonding force and overall stability of the material, enhancing the mechanical properties of the modified rock wool. The modified powder has excellent fire resistance, which can further protect the rock wool substrate from high-temperature damage. Moreover, the rock wool substrate and diatomite have a porous structure. The existence of the pore structure enables them to absorb and store a large amount of heat during the combustion process, reducing the surface temperature of the material and delaying the combustion rate. At the same time, the presence of the modified powder can also increase the hydrophobic property of the modified rock wool, improving the moisture-proof property of the manual purification board.
[0031] 3. The present invention uses octafluoropentanol, isophorone diisocyanate, 3-aminopropene, polyethylene glycol dimethacrylate, acrylic acid, and 2,2-diethoxyacetophenone as raw materials to prepare a modified hydrophobic coating. As a fluorinated alcohol compound, octafluoropentanol contains fluorine atoms in its molecule with extremely strong electronegativity and a small atomic radius, enabling the fluorinated chain segments to closely pack when arranging on the material surface, forming a low surface energy barrier layer. As a result, water molecules are difficult to wet and spread on the coating surface, endowing the coating with excellent hydrophobic properties. Moreover, the formed cross-linked structure enhances the cohesion and stability of the coating, making the coating denser and tougher, which is beneficial to the persistence of the hydrophobic property. Detailed implementation manners
[0032] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.
[0033] Example 1: This example discloses a preparation method of modified rock wool, including the following steps:
[0034] Q1: Add 10.64 g of 4,4'-diaminodiphenyl ether into a container containing 149.5 mL of N,N-dimethylformamide, react at 0 °C for 2 h, then add 11.59 g of pyromellitic dianhydride, stir well for 3 h to obtain a spinning solution. Use the electrospinning technique to prepare nanofibers from the spinning solution. The parameters of the electrospinning technique are as follows: the ambient temperature is 25 °C, the ambient humidity is 40%, the spinning voltage is 20 kV, the syringe pushing speed is 0.8 mL / h, use an aluminum foil as the receiving substrate and closely attach it to the receiving roller. The distance between the receiving roller and the syringe is 18 cm, the roller rotation speed is 450 rpm, the spinning time is 12 h, and perform heat treatment. The treatment process is as follows: heat up from room temperature to 100 °C in 0.5 h and keep warm for 2 h, then heat up to 300 °C in 2 h and keep warm for 2 h to obtain heat-treated nanofibers;
[0035] Q2: Add 35.48 g of zirconium oxychloride octahydrate into 1.1 L of distilled water, adjust the pH = 10.2 with ammonia water, heat-treat at 200 °C for 4 h, wash with distilled water, then wash with absolute ethanol, and dry in vacuum to obtain a white powder. Disperse 2 g of the white powder ultrasonically in 8 mL of ethanol for 45 min, slowly dropwise add 3 mL of silane coupling agent KH-560, ultrasonically disperse for 30 min and then heat reflux for 5 h, centrifuge, wash, and dry to obtain a modified powder;
[0036] Q3: Ultrasonically disperse 2 g of the modified powder in 10 mL of ethanol, then add 3 g of the heat-treated nanofibers, soak for 6 h, wash with deionized water, dry for 24 h, and perform temperature-rising treatment: heat up from room temperature to 400 °C in 2 h and keep warm for 1 h to obtain modified nanofibers;
[0037] Q4: Mix 40 g of rock wool substrate, 4.5 g of modified nanofibers and 10 g of diatomite, cure, wash, dry, and perform heat treatment to obtain modified rock wool.
[0038] This example discloses a preparation method of a modified hydrophobic coating, including the following steps:
[0039] S1: Dissolve 1.37 g of octafluoropentanol and 1.19 mL of isophorone diisocyanate in 10 mL of acetone respectively, then mix and add 0.03 g of dibutyltin dilaurate, and then pour it into a three-necked flask equipped with a condensing reflux device, a nitrogen protection device and an electric stirrer. React at 70 °C for 3 h, then cool down, add 0.49 mL of 3-aminopropene and continue to react, heat to remove acetone to obtain a fluorinated alcohol;
[0040] S2: Heat 0.15 g of polyethylene glycol dimethacrylate at 60 °C, then add 0.375 mL of acrylic acid and 0.28 mL of 1-butyl-3-methylimidazolium tetrafluoroborate to a container, stir for 2 h until evenly mixed, cool, add 2.76 g of fluorinated alcohol and 0.065 mL of 2,2-diethoxyacetophenone, and stir magnetically for 10 min until evenly mixed to obtain a modified hydrophobic coating.
[0041] This example discloses a double-sided magnesium oxychloride rock wool manual purification board, which is composed of the following components in parts by weight: 25 parts of modified rock wool, 40 parts of magnesium oxychloride board, 11.5 parts of polyurethane adhesive, and 7.5 parts of modified hydrophobic coating.
[0042] This example discloses a preparation method of a double-sided magnesium oxychloride rock wool manual purification board, which includes the following steps:
[0043] Step (1): Evenly apply the adhesive on the surfaces of the modified rock wool and the magnesium oxychloride board, then combine the two, and compact them to obtain a double-sided magnesium oxychloride rock wool board;
[0044] Step (2): Evenly apply the modified hydrophobic coating on the surface of the double-sided magnesium oxychloride rock wool board, then place it in an ultraviolet box, and after polymerization for 2 h, obtain a double-sided magnesium oxychloride rock wool manual purification board.
[0045] Example 2: This example discloses a preparation method of modified rock wool, which includes the following steps:
[0046] Q1: Add 9.25 g of 4,4'-diaminodiphenyl ether to a container containing 130 mL of N,N-dimethylformamide, react at 0 °C for 2 h, then add 10.08 g of pyromellitic dianhydride, stir well for 3 h to obtain a spinning solution, and use electrospinning technology to prepare the spinning solution into nanofibers. The parameters of the electrospinning technology are: the ambient temperature is 25 °C, the ambient humidity is 40%, the spinning voltage is 20 kV, the syringe propulsion speed is 0.8 mL / h, use an aluminum foil as the receiving substrate and closely attach it to the receiving roller, the distance between the receiving roller and the syringe is 18 cm, the roller rotation speed is 450 rpm, the spinning time is 12 h, and perform heat treatment. The treatment process is: heat from room temperature to 100 °C in 0.5 h and keep warm for 2 h, then heat to 300 °C in 2 h and keep warm for 2 h to obtain heat-treated nanofibers;
[0047] Q2: Add 32.25 g of zirconium oxychloride octahydrate to 1 L of distilled water, adjust the pH to 10.2 with ammonia water, heat-treat at 200 °C for 4 h, wash with distilled water, then wash with absolute ethanol, and dry in vacuum to obtain a white powder. Disperse 1 g of the white powder ultrasonically in 10 mL of ethanol for 45 min, slowly add 4 mL of silane coupling agent KH-560, ultrasonically disperse for 30 min, then heat under reflux for 5 h, centrifuge, wash, and dry to obtain a modified powder;
[0048] Q3: Disperse 1 g of the modified powder ultrasonically in 12 mL of ethanol, then add 4 g of heat-treated nanofibers, soak for 6 h, wash with deionized water, dry for 24 h, and perform a temperature-raising treatment: heat from room temperature to 400 °C over 2 h and hold for 1 h to obtain modified nanofibers;
[0049] Q4: Mix 30 g of rock wool substrate, 6 g of modified nanofibers, and 12 g of diatomite, cure, wash, dry, and heat-treat to obtain modified rock wool.
[0050] This example discloses a preparation method of a modified hydrophobic coating, which includes the following steps:
[0051] S1: Dissolve 1.51 g of octafluoropentanol and 1.38 mL of isophorone diisocyanate in 10 mL of acetone respectively, then mix them and add 0.03 g of dibutyltin dilaurate, and then pour them into a three-necked flask equipped with a condensing reflux device, a nitrogen protection device, and an electric stirrer. After reacting at 70 °C for 3 h, cool down, add 0.44 mL of 3-aminopropene and continue to react, and heat to remove acetone to obtain a fluorinated alcohol;
[0052] S2: Heat 0.18 g of polyethylene glycol dimethacrylate at 60 °C, then add 0.45 mL of acrylic acid and 0.23 mL of 1-butyl-3-methylimidazolium tetrafluoroborate to a container, stir for 2 h until evenly mixed, cool down, add 2.23 g of the fluorinated alcohol and 0.05 mL of 2,2-diethoxyacetophenone, and stir magnetically for 10 min until evenly mixed to obtain a modified hydrophobic coating.
[0053] This example discloses a double-sided glass magnesium rock wool manual purification board, which is composed of the following components in parts by weight: 20 parts of modified rock wool, 50 parts of glass magnesium board, 10 parts of polyurethane adhesive, and 9 parts of modified hydrophobic coating.
[0054] This example discloses a preparation method of a double-sided glass magnesium rock wool manual purification board, which includes the following steps:
[0055] Step (1): Evenly apply the adhesive on the surfaces of the modified rock wool and the glass magnesium board, then combine the two and compact them to obtain a double-sided glass magnesium rock wool board;
[0056] Step (2): Uniformly apply the modified hydrophobic coating on the surface of the double-sided glass magnesium rock wool board, and then place it in an ultraviolet box. After polymerization for 2 h, a double-sided glass magnesium rock wool manual purification board is obtained.
[0057] Example 3: This example discloses a preparation method of modified rock wool, including the following steps:
[0058] Q1: Add 12.03 g of 4,4'-diaminodiphenyl ether to a container containing 169 mL of N,N-dimethylformamide, react at 0 °C for 2 h, then add 13.1 g of pyromellitic dianhydride, and stir well for 3 h to obtain a spinning solution. Use the electrospinning technique to prepare the spinning solution into nanofibers. The parameters of the electrospinning technique are: the ambient temperature is 25 °C, the ambient humidity is 40%, the spinning voltage is 20 kV, the syringe propulsion speed is 0.8 mL / h, use an aluminum foil as the receiving substrate and closely attach it to the receiving roller. The distance between the receiving roller and the syringe is 18 cm, the roller rotation speed is 450 rpm, the spinning time is 12 h, and perform heat treatment. The treatment process is: heat up from room temperature to 100 °C in 0.5 h and keep warm for 2 h, then heat up to 300 °C in 2 h and keep warm for 2 h to obtain heat-treated nanofibers;
[0059] Q2: Add 38.7 g of zirconium oxychloride octahydrate to 1.2 L of distilled water, adjust the pH = 10.2 with ammonia water, heat-treat at 200 °C for 4 h, wash with distilled water, then wash with absolute ethanol, and dry in vacuum to obtain a white powder. Disperse 3 g of the white powder in 6 mL of ethanol by ultrasonic dispersion for 45 min, slowly add 2 mL of silane coupling agent KH-560, ultrasonic disperse for 30 min and then heat reflux for 5 h, centrifuge, wash, and dry to obtain a modified powder;
[0060] Q3: Disperse 3 g of the modified powder in 8 mL of ethanol by ultrasonic dispersion, then add 2 g of the heat-treated nanofibers, soak for 6 h, wash with deionized water, dry for 24 h, and perform temperature-raising treatment: heat up from room temperature to 400 °C in 2 h and keep warm for 1 h to obtain modified nanofibers;
[0061] Q4: Mix 50 g of rock wool substrate, 3 g of modified nanofibers, and 8 g of diatomite, cure, wash, dry, and perform heat treatment to obtain modified rock wool.
[0062] This example discloses a preparation method of a modified hydrophobic coating, including the following steps:
[0063] S1: Dissolve 1.23 g of octafluoropentanol and 1 mL of isophorone diisocyanate in 10 mL of acetone respectively. Then mix them and add 0.03 g of dibutyltin dilaurate. Then pour the mixture into a three-necked flask equipped with a condenser reflux device, a nitrogen protection device and an electric stirrer. After reacting at 70 °C for 3 h, cool down, add 0.53 mL of 3-aminopropene and continue to react. Heat to remove acetone to obtain fluorinated alcohol.
[0064] S2: Heat 0.12 g of polyethylene glycol dimethacrylate at 60 °C. Then add 0.3 mL of acrylic acid and 0.34 mL of 1-butyl-3-methylimidazolium tetrafluoroborate to a container, stir for 2 h until evenly mixed, cool down, add 3.34 g of fluorinated alcohol and 0.075 mL of 2,2-diethoxyacetophenone, and stir magnetically for 10 min until evenly mixed to obtain a modified hydrophobic coating.
[0065] This example discloses a double-sided glass magnesium rock wool manual purification board, which is composed of the following components in parts by weight: 30 parts of modified rock wool, 30 parts of glass magnesium board, 13 parts of polyurethane adhesive, and 6 parts of modified hydrophobic coating.
[0066] This example discloses a preparation method of a double-sided glass magnesium rock wool manual purification board, which includes the following steps:
[0067] Step (1): Evenly apply the adhesive on the surfaces of the modified rock wool and the glass magnesium board, then combine the two, and compact them to obtain a double-sided glass magnesium rock wool board.
[0068] Step (2): Evenly apply the modified hydrophobic coating on the surface of the double-sided glass magnesium rock wool board, then put it into an ultraviolet box, and polymerize for 2 h to obtain a double-sided glass magnesium rock wool manual purification board.
[0069] Example 4: This example discloses a preparation method of modified rock wool, which includes the following steps:
[0070] Q1: Add 9.95 g of 4,4'-diaminodiphenyl ether to a container containing 139.8 mL of N,N-dimethylformamide, react at 0 °C for 2 h, then add 12.35 g of pyromellitic dianhydride, stir well for 3 h to obtain a spinning solution. Use electrospinning technology to prepare the spinning solution into nanofibers. The parameters of the electrospinning technology are: the ambient temperature is 25 °C, the ambient humidity is 40%, the spinning voltage is 20 kV, the syringe propulsion speed is 0.8 mL / h, use an aluminum foil as the receiving substrate and closely attach it to the receiving roller. The distance between the receiving roller and the syringe is 18 cm, the roller rotation speed is 450 rpm, the spinning time is 12 h, and heat treatment is carried out. The treatment process is: heat from room temperature to 100 °C in 0.5 h and keep warm for 2 h, then heat to 300 °C in 2 h and keep warm for 2 h to obtain heat-treated nanofibers.
[0071] Q2: Add 33.87 g of zirconium oxychloride octahydrate to 1.05 L of distilled water. Adjust the pH to 10.2 with ammonia water. After heat treatment at 200 °C for 4 h, wash with distilled water and then with absolute ethanol. Dry in vacuum to obtain a white powder. Disperse 1.5 g of the white powder ultrasonically in 7 mL of ethanol for 45 min. Slowly add 2.5 mL of silane coupling agent KH-560 and ultrasonically disperse for 30 min, then heat under reflux for 5 h. Centrifuge, wash, and dry to obtain a modified powder;
[0072] Q3: Disperse 1.5 g of the modified powder ultrasonically in 11 mL of ethanol, then add 2.5 g of heat-treated nanofibers, soak for 6 h, wash with deionized water, and dry for 24 h. Carry out a temperature-raising treatment: heat from room temperature to 400 °C over 2 h and hold for 1 h to obtain modified nanofibers;
[0073] Q4: Mix 35 g of rock wool substrate, 4 g of modified nanofibers, and 11 g of diatomite, cure, wash, dry, and heat-treat to obtain modified rock wool.
[0074] This example discloses a preparation method of a modified hydrophobic coating, including the following steps:
[0075] S1: Dissolve 1.44 g of octafluoropentanol and 1.09 mL of isophorone diisocyanate in 10 mL of acetone respectively. Then mix them and add 0.03 g of dibutyltin dilaurate. Pour the mixture into a three-necked flask equipped with a condensing reflux device, a nitrogen protection device, and an electric stirrer. After reacting at 70 °C for 3 h, cool down, add 0.47 mL of 3-aminopropene and continue to react. Heat to remove acetone to obtain a fluorinated alcohol;
[0076] S2: Heat 0.16 g of polyethylene glycol dimethacrylate at 60 °C. Then add 0.35 mL of acrylic acid and 0.25 mL of 1-butyl-3-methylimidazolium tetrafluoroborate to a container, stir for 2 h until evenly mixed, cool down, add 2.55 g of the fluorinated alcohol and 0.055 mL of 2,2-diethoxyacetophenone, and magnetically stir for 10 min until evenly mixed to obtain a modified hydrophobic coating.
[0077] This example discloses a double-sided glass magnesium rock wool manual purification board, which is composed of the following components in parts by weight: 22 parts of modified rock wool, 45 parts of glass magnesium board, 12 parts of polyurethane adhesive, and 7 parts of modified hydrophobic coating.
[0078] This example discloses a preparation method of a double-sided glass magnesium rock wool manual purification board, including the following steps:
[0079] Step (1): Evenly apply the adhesive on the surfaces of the modified rock wool and the glass magnesium board, then combine the two and compact them to obtain a double-sided glass magnesium rock wool board;
[0080] Step (2): Evenly apply the modified hydrophobic coating on the surface of the double-sided glass magnesium rock wool board, and then place it in an ultraviolet box. After polymerization for 2 h, a double-sided glass magnesium rock wool manual purification board is obtained.
[0081] Example 5: This example discloses a preparation method of modified rock wool, including the following steps:
[0082] Q1: Add 11.34 g of 4,4'-diaminodiphenyl ether into a container containing 159.3 mL of N,N-dimethylformamide, react at 0 °C for 2 h, then add 10.84 g of pyromellitic dianhydride, and fully stir for 3 h to obtain a spinning solution. Use the electrospinning technology to prepare the spinning solution into nanofibers. The parameters of the electrospinning technology are: the ambient temperature is 25 °C, the ambient humidity is 40%, the spinning voltage is 20 kV, the syringe propulsion speed is 0.8 mL / h, use an aluminum foil as the receiving substrate and closely attach it to the receiving roller. The distance between the receiving roller and the syringe is 18 cm, the roller rotation speed is 450 rpm, the spinning time is 12 h, and perform heat treatment. The treatment process is: heat up from room temperature to 100 °C in 0.5 h and keep warm for 2 h, then heat up to 300 °C in 2 h and keep warm for 2 h to obtain heat-treated nanofibers;
[0083] Q2: Add 37.09 g of zirconium oxychloride octahydrate into 1.15 L of distilled water, adjust the pH = 10.2 with ammonia water, heat-treat at 200 °C for 4 h, wash with distilled water, then wash with absolute ethanol, and dry in vacuum to obtain a white powder. Ultrasonically disperse 2.5 g of the white powder in 9 mL of ethanol, ultrasonically disperse for 45 min, slowly dropwise add 3.5 mL of silane coupling agent KH-560, ultrasonically disperse for 30 min and then heat reflux for 5 h, centrifuge, wash, and dry to obtain a modified powder;
[0084] Q3: Ultrasonically disperse 2.5 g of the modified powder in 9 mL of ethanol, then add 3.5 g of heat-treated nanofibers, soak for 6 h, wash with deionized water, dry for 24 h, and perform temperature-raising treatment: heat up from room temperature to 400 °C in 2 h and keep warm for 1 h to obtain modified nanofibers;
[0085] Q4: Mix 45 g of rock wool substrate, 5 g of modified nanofibers, and 9 g of diatomite, cure, wash, dry, and perform heat treatment to obtain modified rock wool.
[0086] This example discloses a preparation method of a modified hydrophobic coating, including the following steps:
[0087] S1: Dissolve 1.3 g of octafluoropentanol and 1.28 mL of isophorone diisocyanate in 10 mL of acetone respectively. Then mix them and add 0.03 g of dibutyltin dilaurate. Next, pour the mixture into a three-necked flask equipped with a condensing reflux device, a nitrogen protection device, and an electric stirrer. After reacting at 70 °C for 3 h, cool down the temperature, add 0.51 mL of 3-aminopropene and continue the reaction. Heat to remove acetone to obtain fluorinated alcohol.
[0088] S2: Heat 0.14 g of polyethylene glycol dimethacrylate at 60 °C. Then add 0.42 mL of acrylic acid and 0.32 mL of 1-butyl-3-methylimidazolium tetrafluoroborate to a container, stir for 2 h until evenly mixed, cool down, add 3.05 g of fluorinated alcohol and 0.06 mL of 2,2-diethoxyacetophenone, and stir magnetically for 10 min until evenly mixed to obtain a modified hydrophobic coating.
[0089] This example discloses a double-sided glass magnesium rock wool manual purification board, which is composed of the following components in parts by weight: 28 parts of modified rock wool, 35 parts of glass magnesium board, 11 parts of polyurethane adhesive, and 8 parts of modified hydrophobic coating.
[0090] This example discloses a preparation method of a double-sided glass magnesium rock wool manual purification board, which includes the following steps:
[0091] Step (1): Evenly apply the adhesive on the surfaces of the modified rock wool and the glass magnesium board, then combine the two and compact them to obtain a double-sided glass magnesium rock wool board.
[0092] Step (2): Evenly apply the modified hydrophobic coating on the surface of the double-sided glass magnesium rock wool board, then put it into an ultraviolet box and polymerize for 2 h to obtain a double-sided glass magnesium rock wool manual purification board.
[0093] Comparative example 1: Compared with Example 1, in the process of preparing modified rock wool in Comparative example 1, zirconium oxychloride octahydrate is not added, and other conditions remain unchanged.
[0094] Comparative example 2: Compared with Example 1, in the process of preparing the modified hydrophobic coating in Comparative example 2, octafluoropentanol is not added, and other conditions remain unchanged.
[0095] Comparative example 3: Compared with Example 1, in the process of preparing the double-sided glass magnesium rock wool manual purification board in Comparative example 3, the rock wool substrate is used to replace the modified rock wool, and other conditions remain unchanged.
[0096] Comparative example 4: Compared with Example 1, in the process of preparing the double-sided glass magnesium rock wool manual purification board in Comparative example 4, the modified hydrophobic coating is not coated, and other conditions remain unchanged.
[0097] Experimental Example: The prepared sample was immersed in clear water. After 12 hours of immersion, it was taken out and the weight of the sample before and after the experiment was measured. According to the water absorption rate = (m 后 -m 前 / m 前 )×100%, the combustion performance of the sample was tested according to GB 8624-2012, and the compressive performance of the sample was tested according to GB / T 50081-2019. The test results are shown in Table 1:
[0098] Table 1
[0099] Project Water Absorption Rate / % Combustion Rating Compressive Strength / MPa Example 1 1.94 A1 72.8 Example 2 1.98 A1 71.9 Example 3 1.99 A1 71.3 Example 4 1.96 A1 71.6 Example 5 1.97 A1 71.5 Comparative Example 1 2.43 A2 65.4 Comparative Example 2 2.74 A1 71.4 Comparative Example 3 2.57 A2 63.2 Comparative Example 4 2.76 A1 71.3
[0100] It can be seen from the test results in Table 1 that the double-sided glass magnesium rock wool manual purification board prepared in Examples 1-5 of the present invention has excellent moisture-proof performance, fire resistance and mechanical properties. By comparing Comparative Example 1 with Examples 1-5, it can be seen that adding zirconium oxychloride octahydrate can effectively improve the moisture-proof performance, fire resistance and mechanical properties of the double-sided glass magnesium rock wool manual purification board; by comparing Comparative Example 2 with Examples 1-5, it can be seen that adding octafluoropentanol can effectively improve the moisture-proof performance of the double-sided glass magnesium rock wool manual purification board; by comparing Comparative Example 3 with Examples 1-5, it can be seen that the use of modified rock wool can effectively improve the double-sided glass magnesium rock wool manual purification board with excellent moisture-proof performance, fire resistance and mechanical properties; by comparing Comparative Example 4 with Examples 1-5, it can be seen that coating with a modified hydrophobic coating can effectively improve the moisture-proof performance of the double-sided glass magnesium rock wool manual purification board.
[0101] The above is only a preferred specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any person skilled in the art within the technical scope disclosed by the present invention, according to the technical solution and inventive concept of the present invention, makes equivalent substitutions or changes, and should be covered by the protection scope of the present invention.
[0102] The preferred embodiments of the present invention disclosed above are only used to help explain the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the present invention to only the specific embodiments. Obviously, according to the content of this specification, many modifications and changes can be made. The present specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can understand and utilize the present invention well. The present invention is only limited by the claims and their full scope and equivalents.
Claims
1. Double-sided glass magnesium rock wool manual purification board, characterized in that: The invention is composed of the following components in parts by weight: 20-30 parts of modified rock wool, 30-50 parts of glass magnesium board, 10-13 parts of adhesive, and 6-9 parts of modified hydrophobic coating, wherein the modified rock wool is prepared from 4,4'-diaminodiphenyl ether, pyromellitic acid dianhydride, zirconium oxychloride octahydrate, rock wool substrate and diatomaceous earth, and the modified hydrophobic agent is prepared from octafluoropentanol, isophorone diisocyanate, 3-aminopropylene, dimethacrylate polyethylene glycol ether and acrylic acid. The preparation method of the modified rock wool comprises the following steps: Q1: 4,4'-diaminodiphenyl ether is added to a container containing N,N-dimethylformamide for reaction at low temperature, followed by adding pyromellitic anhydride, and stirring thoroughly to obtain a spinning solution, and the spinning solution is prepared into nanofibers using electrospinning technology, and subjected to heat treatment to obtain heat-treated nanofibers; Q2: Add zirconium oxychloride octahydrate to distilled water, adjust the pH with ammonia water, heat treat, wash, and vacuum dry to obtain a white powder, ultrasonically disperse the white powder into ethanol, slowly drop silane coupling agent KH-560, ultrasonically disperse, heat to reflux, centrifuge, wash, and dry to obtain a modified powder; Q3: Ultrasonic dispersion of the modified powder in ethanol, then addition of heat-treated nanofibers, soaking, washing, drying, and heating treatment to obtain modified nanofibers; Q4: Mixing the rock wool substrate, modified nanofibers and diatomaceous earth, curing, cleaning, drying and heat treating to obtain modified rock wool; The preparation method of the modified hydrophobic coating comprises the following steps: S1: Dissolve octafluoropentanol and isophorone diisocyanate in acetone respectively, then mix and add dibutyltin dilaurate, and then pour into a three-necked flask equipped with a condensing reflux device, a nitrogen protection device and an electric stirrer. After the reaction is complete, cool down, add 3-aminopropylene to continue the reaction, heat to remove acetone, and obtain a fluorine-containing alcohol; S2: Heat the dimethacrylate polyethylene glycol ether, then add acrylic acid and 1-butyl-3-methylimidazole tetrafluoroborate into a container, stir until the mixture is uniform, cool, add fluorinated alcohol and 2,2-diethoxyacetophenone, and stir magnetically until the mixture is uniform to obtain a modified hydrophobic coating.
2. The double-sided glass magnesium rock wool manual purification board according to claim 1 is characterized in that: In the Q1, the dosage ratio of 4,4'-diaminodiphenyl ether, N,N-dimethylformamide and pyromellitic anhydride is (9.25-12.03) g: (130-169) mL: (10.08-13.1) g, the low-temperature reaction temperature is 0-3°C, the reaction time is 2-3h, the sufficient stirring time is 3-5h, and the parameters of the electrospinning technology are: the ambient temperature is 25°C, the ambient humidity is 40%, the spinning voltage is 20-22kV, the syringe propulsion speed is 0.8mL / h, the aluminum foil is used as the receiving substrate and is closely attached to the receiving roller, the distance between the receiving roller and the syringe is 18cm, the roller speed is 450rpm, the spinning time is 10-12h, and the heating treatment process is: from room temperature to 100°C for 0.5h and kept warm for 2h, and then heated to 300°C for 2h and kept warm for 2h.
3. The double-sided glass magnesium rock wool manual purification board according to claim 1 is characterized in that: In the Q2, the dosage ratio of zirconium oxychloride octahydrate and distilled water is (32.25-38.7) g: (1-1.2) L, the pH is adjusted to 9.8-10.2, the heating temperature is 180-200°C, the time is 2-4 h, and after washing with distilled water, it is washed with anhydrous ethanol. The dosage ratio of white powder, ethanol and silane coupling agent KH-560 is (1-3) g: (6-10) mL: (2-4) mL, the ultrasonic dispersion time is 30-45 min, the ultrasonic dispersion time after adding the silane coupling agent KH-560 is 30-60 min, and the reflux time is 5-7 h.
4. The double-sided glass magnesium rock wool manual purification board according to claim 1 is characterized in that: In Q3, the dosage ratio of modified powder, ethanol and heat-treated nanofibers is (1-3) g: (8-12) mL: (2-4) g, the soaking time is 4-7 hours, washed with deionized water, the drying time is 20-24 hours, and the heating treatment is: from room temperature to 400°C over 2 hours and kept warm for 1 hour; in Q4, the mass ratio of rock wool substrate, modified nanofibers and diatomaceous earth is (30-50): (3-6): (8-12).
5. The double-sided glass magnesium rock wool manual purification board according to claim 1 is characterized in that: In the S1, the molar ratio of octafluoropentanol, isophorone diisocyanate and 3-aminopropylene is (0.9-1.1): (0.8-1.1): (1-1.2), the reaction temperature is 60-80° C., and the reaction time is 3-5 h.
6. The double-sided glass magnesium rock wool manual purification board according to claim 1 is characterized in that: In S2, the dosage ratio of dimethacrylate polyethylene glycol ether, acrylic acid, 1-butyl-3-methylimidazole tetrafluoroborate, fluorinated alcohol and 2,2-diethoxyacetophenone is (0.12-0.18) g: (0.3-0.45) mL: (0.23-0.34) mL: (2.23-3.34) g: (0.05-0.075) mL, the heating temperature is 60-70° C., the stirring time is 1-2 h, and the magnetic stirring time is 5-10 min.
7. The method for preparing the double-sided glass magnesium rock wool manual purification board according to any one of claims 1 to 6, characterized in that: The following steps are involved: Step (1): evenly apply the adhesive on the surface of the modified rock wool and the glass magnesium board, and then combine and compact the two to obtain a double-sided glass magnesium rock wool board; Step (2): evenly apply the modified hydrophobic coating on the surface of the double-sided glass magnesium rock wool board, and then put it into a UV box. After polymerization for 2-4 hours, a double-sided glass magnesium rock wool manual purification board is obtained.
Citation Information
Patent Citations
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