Silent wood composite floor and preparation method thereof
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- JIANGSU KENTIER WOOD
- Filing Date
- 2025-12-31
- Publication Date
- 2026-07-21
Smart Images
Figure CN121473538B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of flooring technology, specifically relating to a sound-absorbing wood composite floor and its preparation method. Background Technology
[0002] After years of rapid development, my country's wood flooring industry has formed a multi-category, multi-specification industrial system encompassing production, sales, installation, and after-sales service, reaching a relatively mature stage. Natural solid wood laminate flooring, with its elegant appearance, durability, and good stability, has become an important material in modern building decoration. Furthermore, with the improvement of living standards, consumers' demands for flooring have expanded from basic decoration and durability to a better user experience, especially regarding sound insulation. The transmission and amplification of noise from walking and falling objects through flooring not only affects home tranquility but also becomes a pressing issue in public places such as office buildings, hospitals, and schools. Meanwhile, the surface layer of the flooring, as the part directly exposed to wear and tear and visual appeal, is crucial in terms of strength, weather resistance, and dimensional stability. While solid wood surfaces are aesthetically pleasing, they are susceptible to expansion, contraction, and cracking due to environmental humidity. Melamine-formaldehyde resin is a commonly used impregnation resin, but its brittleness after curing and its compatibility with wood fibers and toughening effect need improvement.
[0003] Therefore, there is an urgent need in this field for a sound-absorbing wood composite floor with good sound insulation and mechanical properties. Summary of the Invention
[0004] The purpose of this invention is to provide a soundproof wood composite floor and its preparation method, so as to solve the above-mentioned technical problems in the prior art.
[0005] To achieve the above objectives, the present invention adopts the following technical solution:
[0006] The technical solution provided by this invention is as follows:
[0007] In a first aspect, the present invention provides a soundproof wood composite floor, which comprises, from top to bottom, a surface layer, a soundproof layer, a substrate layer and a balancing layer, wherein the above layers are bonded together by hot melt adhesive.
[0008] Preferably, the sound-absorbing layer is irradiated cross-linked polyethylene foam (IXPE) with a thickness of 2-3 mm.
[0009] Preferably, the method for preparing the IXPE includes the following steps:
[0010] P1: High-density polyethylene (HDPE) and azodicarbonamide (ADCA) are melt-blended and extruded, then granulated after water cooling, and then vacuum dried. Under the same process conditions, the mixture is melt-blended and extruded a second time, cooled and granulated, and then vacuum dried to obtain HDPE masterbatch granules.
[0011] In the above process, low-temperature mixing and granulation are carried out; the maximum temperature of melt blending is controlled at 130℃, which is lower than the ADCA thermal decomposition initiation temperature of 200℃, and the particles do not foam; the mixing uniformity is improved by two melt blending processes, and HDPE masterbatch particles with uniform dispersion of foaming agent are obtained.
[0012] P2: HDPE masterbatch granules are fed into a single-screw extruder and calender, and solid sheets are obtained through extrusion and calendering.
[0013] P3: Solid sheets are subjected to stepwise irradiation treatment under an electron accelerator to obtain irradiated cross-linked polyethylene;
[0014] In the above process, electron beam irradiation crosslinking is performed step by step.
[0015] P4: Place the irradiated cross-linked polyethylene in a hot press, initially pressurize and then heat it, then quickly depressurize and cool to set, to obtain irradiated cross-linked polyethylene foam (IXPE).
[0016] In the above process, the initial pressurization is used to suppress the premature decomposition and expansion of the foaming agent during heating, so that the gas can be fully dissolved in the polymer matrix and reach a uniform supersaturated state. The rapid depressurization causes the system pressure to drop sharply, inducing the gas to nucleate and expand instantly and uniformly. The cross-linked network provides melt strength, stabilizes the cell structure, and obtains a foam material with high closed-cell ratio and dimensional stability.
[0017] Preferably, in P4, the heating conditions are: heating temperature of 180-200℃, heating time of 60-90s; and initial pressurization pressure of 10-15MPa.
[0018] Preferably, in P1, the mass ratio of HDPE to ADCA is 85-90:10-15; melt blending is carried out in a twin-screw extruder, with the barrel-to-die temperature of the twin-screw extruder set to 110℃, 115℃, 120℃, 125℃, and 130℃, and the screw speed at 45-55 rpm; vacuum drying conditions: vacuum drying temperature at 45-55℃ and vacuum drying time at 20-28h.
[0019] Preferably, in P2, the temperature gradient of the single-screw extrusion calender is 130℃, 135℃, 140℃, 145℃, 145℃, and the screw speed is 45-55 rpm; the thickness of the solid sheet is 1.0 mm.
[0020] Preferably, in P3, the electron beam energy of the electron accelerator is 10 MeV, the beam current intensity is 4 mA, and the power is 40 kW; the step-by-step irradiation treatment method is as follows: irradiation is performed with a single irradiation dose of 25 kGy, so that the total absorbed dose of the sheet reaches 75 kGy, and after each irradiation dose of 25 kGy, the sheet is cooled at room temperature before the next irradiation is performed, until the cumulative dose reaches 75 kGy.
[0021] Preferably, the preparation method of the surface layer includes the following steps: immersing the wood veneer in a reinforcing softening liquid, ultrasonically treating it, and drying it to obtain impregnated wood veneer; making the impregnated wood veneer into timber; and making the timber into veneer to obtain the surface layer.
[0022] Preferably, the ultrasonic treatment conditions are as follows: ultrasonic treatment frequency is 2.1-2.5kHz, ultrasonic treatment time is 10-14min, ultrasonic treatment temperature is 25-30℃, and the thickness of the wood veneer is 1-1.5mm.
[0023] Preferably, the drying method is as follows: drying at 50-60℃ to a moisture content of 25-35%, and then heating to 65-75℃ to dry to a moisture content of 12-16%.
[0024] Preferably, the preparation method of the timber is as follows: after assembling the impregnated veneer in the direction of the wood grain, hot-press it for 30-40 minutes under a pressure of 1.8-2.5 MPa and a temperature of 135-150℃, and after pressing and shaping, age it for 24-48 hours in an environment with a temperature of 25-35℃ and a relative humidity of 50-65% to obtain the timber.
[0025] Preferably, the method for preparing wood veneer from timber involves processing the timber to a thickness of 0.2-0.6 mm, trimming and sanding the back, and drying it at a mild temperature of 35-45℃ to a moisture content of 8-12%.
[0026] Preferably, the method for preparing the enhanced softening liquid involves adding triazine diquaternary ammonium salt diglycine salt and ammonia solution to melamine-formaldehyde resin, adjusting the pH, and obtaining the enhanced softening liquid.
[0027] Preferably, the ammonia solution has a mass fraction of 35 wt%; the pH is adjusted to 7.5-8.5; and the triazine diquaternary ammonium salt diglycine salt accounts for 5-8 wt% of the melamine-formaldehyde resin.
[0028] Preferably, the melamine-formaldehyde resin adhesive solution has a solid content of 50-60%, a viscosity of 10-18 mPa·s, and a pH of 7.5-8.5.
[0029] Preferably, the preparation method of the triazine bisquaternary ammonium diglycine salt includes the following steps:
[0030] S1: Add cyanuric chloride to toluene, cool, and slowly add dodecylamine solution dropwise while stirring. Continue stirring and maintaining the temperature. Monitor the reaction with thin-layer chromatography until completion. Filter, wash, dry, filter again, and evaporate under reduced pressure to obtain the triazine intermediate.
[0031] In the above process, under low temperature and alkaline conditions, the nitrogen atom of dodecylamine attacks a chlorine atom on the cyanuric chloride ring, undergoing nucleophilic substitution to generate HCl and form a CN bond; the low temperature condition inhibits the reactivity, and the monosubstituted product is obtained with high selectivity.
[0032] S2: The triazine intermediate was added to acetone, followed by the addition of ethylenediamine. The reaction was monitored by thin-layer chromatography until completion. The reaction solution was cooled to room temperature and then cooled in an ice bath. The solution was filtered, washed, and vacuum dried to constant weight to obtain product S2.
[0033] In the above process, the triazine intermediate has two chlorine atoms with lower reactivity than the first chlorine atom on cyanuric chloride. The amino group of one molecule of ethylenediamine selectively attacks the second chlorine atom on the two molecules of triazine ring, resulting in a substitution reaction, which acts as a linking arm to connect the two molecules of triazine ring.
[0034] S3: The product of S2 was mixed with N,N-dimethyl-1,3-diaminopropane and reacted. The reaction was monitored by thin-layer chromatography until the end. After cooling, acetone was added, and then bromoethane was slowly added under stirring. The temperature was increased and the reaction was monitored by thin-layer chromatography again until the end. The mixture was filtered, precipitated, stirred and cooled in an ice bath, filtered, washed and dried to obtain triazine diquaternary ammonium salt.
[0035] In the above process, firstly, the last chlorine atom at both ends of the S2 product reacts with the primary amino group of one molecule of N,N-dimethyl-1,3-diaminopropane to complete the terminal functionalization, obtaining an intermediate with a tertiary amine group at each end. Then, the added bromoethane reacts with the two tertiary amine groups at both ends of the intermediate to undergo a quaternization reaction, finally generating a symmetrical triazine bisquaternary ammonium salt bromide.
[0036] S4: The triazine diquaternary ammonium salt is converted into an aqueous solution of triazine diquaternary ammonium salt hydroxide. Under ice-water bath cooling, the aqueous solution of triazine diquaternary ammonium salt hydroxide is added dropwise to the aqueous solution of glycine. After the addition is complete, stirring is continued, impurities are removed, and the solution is dried under vacuum to obtain triazine diquaternary ammonium salt diglycine salt.
[0037] In the above process, a strongly alkaline quaternary ammonium hydroxide solution is slowly added dropwise to a glycine aqueous solution under ice bath conditions, resulting in an acid-base neutralization reaction.
[0038] Preferably, in step S1, the dodecylamine solution is prepared by adding 180-360g of dodecylamine to 400-800mL of toluene to obtain a dodecylamine solution; the ratio of cyanuric chloride to toluene is 162-324g:1.2-2.4L; the cooling temperature is -5-0℃; the stirring speed is 300-600rpm; the slow dropwise addition time is 1-2h; the incubation and stirring reaction time is 3-4h; the mobile phase for thin-layer chromatography is petroleum ether and ethyl acetate with a volume ratio of 4:1; the washing method is as follows: the filtrate is washed sequentially with 1mol / L HCl and 1mol / L NaHCO3 solution until neutral; the washing method is as follows: the filtrate is dried overnight with anhydrous sodium sulfate; the rotary evaporation temperature is 35-45℃.
[0039] Preferably, in S2, the ratio of triazine intermediate, acetone, and ethylenediamine is 90-180g:250-500mL:14.4-28.8g; the reaction conditions are: reaction temperature of 30-35℃ and reaction time of 5-6h; the mobile phase for thin-layer chromatography is ethyl acetate and methanol in a volume ratio of 4:1; the ice bath cooling time is 0.5-1.5h; the washing method is: the filter cake is washed sequentially with acetone and distilled water, repeated 2-3 times; the vacuum drying temperature is 45-55℃.
[0040] Preferably, in S3, the ratio of the product of S2, N,N-dimethyl-1,3-diaminopropane, acetone, and bromoethane is 41.9-84g:83.2-165g:200-400mL:35.1-70g; the reaction conditions are: reaction temperature of 100-105℃ and reaction time of 8-10h; the mobile phase for thin-layer chromatography is ethyl acetate and methanol in a volume ratio of 9:1; the cooling temperature is 45-55℃; the heating reaction temperature is 50-55℃; the mobile phase for reused thin-layer chromatography is n-butanol, acetic acid, and water in a volume ratio of 4:1:1; the precipitation method is: adding 200-400mL of diethyl ether to the filtrate; stirring and cooling in an ice bath for 1.5-2.5h; the washing method is: washing 2-3 times with cold ethyl acetate.
[0041] Preferably, in step S4, the preparation method of the aqueous solution of triazine bisquaternary ammonium hydroxide is as follows: Amberlite IRA-400 anion exchange resin is thoroughly washed with deionized water, then dynamically treated with 1 mol / L NaOH solution until the effluent is strongly alkaline, and finally washed with deionized water until the effluent is neutral to obtain wet resin. The wet resin is packed into a glass chromatography column, and 10-20 g of triazine bisquaternary ammonium salt is added to 100-200 mL of deionized water. The solution is passed through the ion exchange column at a flow rate of 1-2 BV / h. The effluent is collected, and the column is washed with 50-100 mL of deionized water. The effluents are combined to obtain the aqueous solution of triazine bisquaternary ammonium hydroxide.
[0042] Preferably, in step S4, the preparation method of the glycine aqueous solution is as follows: 3-6g of glycine is added to 50-100mL of water; stirring conditions are as follows: stirring temperature is 0-5℃ and stirring time is 3.5-4.5h; impurity removal method is as follows: 200-400mL of acetone is added, and the mixture is stirred at a speed of 300-600rpm, the solid is allowed to precipitate, filtered, and the filter cake is washed with cold acetone 3-5 times; vacuum drying method is as follows: vacuum drying at 40-50℃ to constant weight.
[0043] Preferably, the substrate layer is a high-density fiberboard with a thickness of 8-12 mm and a density of 0.85-1.2 g / cm³. 3 .
[0044] Preferably, the balancing layer comprises the following components by weight: 80-95 wt% polypropylene and 5-20 wt% polyolefin elastomer (POE); the thickness of the balancing layer is 0.8-1.5 mm.
[0045] Secondly, the present invention also provides a method for preparing a sound-absorbing wood composite floor, comprising the following steps:
[0046] The surface layer, sound-absorbing layer, substrate layer, and balancing layer are coated with adhesive and then hot-pressed together to form a whole, resulting in a sound-absorbing wood composite floor.
[0047] Preferably, the amount of adhesive applied is 120-160 g / m³. 2 The pressing conditions are as follows: pressing time is 35-45 min, pressing pressure is 6-8 MPa, and pressing temperature is 140-170℃. The adhesive is polyurethane hot melt adhesive or EPI formaldehyde-free adhesive.
[0048] In summary, due to the adoption of the above technical solution, the beneficial effects of the present invention are:
[0049] 1. The IXPE prepared by this invention is a high-performance foam material. By stepwise irradiation with a high-energy electron beam, the polyethylene molecular chains generate free radicals, which then form a three-dimensional cross-linked network. The stepwise irradiation followed by cooling effectively avoids local overheating and free radical quenching, ensuring a full and uniform cross-linking reaction. This allows free radicals time and conditions to migrate and react evenly, resulting in a dense three-dimensional cross-linked network structure with uniform longitudinal cross-linking degree distribution, low internal stress, and high closed-cell rate, exhibiting excellent buffering performance. Furthermore, it is odorless and non-toxic, meeting the requirements for green building materials.
[0050] 2. The long-chain dodecyl group in the triazine-based bisquaternary ammonium diglycine salt prepared in this invention is a flexible hydrophobic chain that can be intercalated in the rigid three-dimensional network structure of melamine resin. During the resin curing process, it plays an internal plasticizing role, effectively dispersing stress, preventing the propagation of microcracks, and improving the flexibility and impact resistance of the impregnated wood veneer, making it less brittle. The triazine ring and polar groups are highly compatible with the resin structure and can participate in copolymerization or form strong intermolecular interactions, becoming part of the curing network and ensuring that toughening does not weaken mechanical strength. The glycine anion replaces the traditional bromide ion, which not only improves biocompatibility and environmental friendliness, but its -NH2 can also undergo a condensation reaction with the hydroxymethyl group in the resin, actively capturing and fixing free formaldehyde, reducing the formaldehyde release, and at the same time enhancing the interfacial bonding force of the resin-wood-additive three-phase interface.
[0051] 3. The sound-absorbing wood composite flooring prepared by this invention utilizes a scientific composite design consisting of a high-performance IXPE sound-absorbing layer, a toughened environmentally friendly surface layer, a high-density fiber substrate, and an elastic balancing layer. Each layer has complementary functions and a well-matched interface: IXPE provides excellent acoustic cushioning, low compression set, and prevents collapse over long-term use; the modified surface layer combines high surface hardness, high wear resistance, and crack resistance; the balancing layer uses a PP and POE blend system to effectively offset moisture expansion and contraction stress, ensuring dimensional stability; and formaldehyde-free adhesive is used for bonding, eliminating secondary pollution. The final product is a wood composite flooring with excellent sound insulation, high mechanical strength, environmental safety, and durability, which can be widely used in residences, hospitals, schools, and other places with stringent requirements for sound environment and health. Attached Figure Description
[0052] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0053] Figure 1 This is a photograph of the sound-absorbing wood composite flooring of the present invention;
[0054] Figure 2 This is a line graph showing the sound insulation performance of the silent wood composite flooring of the present invention;
[0055] Figure 3 This is a bar chart showing the wear resistance of the silent wood composite flooring of the present invention. Detailed Implementation
[0056] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0057] Preparation Example 1
[0058] This preparation example discloses a method for preparing IXPE, including the following steps:
[0059] P1: HDPE and ADCA are melt-blended in a twin-screw extruder. The barrel to die temperature of the twin-screw extruder is set to 110℃, 115℃, 120℃, 125℃, and 130℃, and the screw speed is 50 rpm. The blended extrudate is then cooled with water and granulated. After being vacuum dried at 50℃ for 24 hours, it is fed back into the twin-screw extruder for a second extrusion, cooling, and granulation under the same process conditions to obtain HDPE masterbatch granules.
[0060] P2: HDPE masterbatch granules are fed into a single-screw extruder and calender with a temperature gradient of 130℃, 135℃, 140℃, 145℃, and 145℃, and a screw speed of 50 rpm. After extrusion and calendering, a solid sheet with a thickness of 1.0 mm is obtained.
[0061] P3: The solid sheet is placed under an electron accelerator for irradiation treatment; the electron beam energy of the electron accelerator is 10MeV, the beam current intensity is 4mA, and the power is 40kW; the sheet is irradiated in stages with a single irradiation dose of 25kGy, so that the total absorbed dose of the sheet reaches 75kGy. After each irradiation dose of 25kGy, the sheet is cooled at room temperature before the next irradiation is performed, until the cumulative dose reaches 75kGy, thus obtaining irradiated cross-linked polyethylene.
[0062] P4: Place the irradiated cross-linked polyethylene in a hot press, initially pressurize it at 10-15 MPa, then heat it at 180-200℃ for 60-90 seconds, then quickly depressurize it, cool and solidify it to obtain irradiated cross-linked polyethylene foam (IXPE).
[0063] The thickness of the IXPE is 2.5 mm. Tests show that the IXPE has a crosslinking degree of 70%, a compressive strength of 230 kPa, a closed-cell rate of >95%, and a thermal conductivity of 0.034 W / (m·K).
[0064] Preparation Example 2
[0065] This preparation example discloses a method for preparing a surface layer, including the following steps:
[0066] The preparation method of the surface layer includes the following steps: immersing a 1.5mm thick wood veneer in a reinforcing softening liquid, ultrasonically treating it at 30℃ and a frequency of 2.3kHz for 12 minutes, drying it at 55℃ to a moisture content of 30%, then heating it to 70℃ and drying it to a moisture content of 14% to obtain an impregnated wood veneer; assembling the impregnated veneer along the grain direction, hot-pressing it at a pressure of 2.1MPa and a temperature of 145℃ for 35 minutes, pressing it into shape, and aging it at a temperature of 30℃ and a relative humidity of 57% for 36 hours to obtain a timber strip; processing the timber strip to a thickness of 0.4mm, trimming it, sanding the back, and drying it at a mild temperature of 40℃ to a moisture content of 10% to obtain the surface layer.
[0067] The method for preparing the enhanced softening liquid is as follows: triazine diquaternary ammonium salt diglycine salt and 35wt% ammonia solution are added to melamine-formaldehyde resin, and the pH is adjusted to 8.
[0068] The triazine diquaternary ammonium salt diglycine salt accounts for 7 wt% of the melamine-formaldehyde resin.
[0069] The preparation method of the triazine bisquaternary ammonium diglycine salt includes the following steps:
[0070] S1: 243g of cyanuric chloride was added to 1.8L of toluene and cooled to -3℃. 270g of dodecylamine was added to 600mL of toluene to obtain a dodecylamine solution. The dodecylamine solution was slowly added dropwise over 1.5h while stirring at 450rpm. The reaction was continued for 3.5h with stirring. The reaction was monitored by thin-layer chromatography until completion. The solution was filtered, and the filtrate was washed successively with 1mol / L HCl and 1mol / L NaHCO3 solution until neutral. The solution was dried overnight with anhydrous sodium sulfate, filtered, and the filtrate was evaporated under reduced pressure at 40℃ to obtain a triazine intermediate.
[0071] The mobile phase for thin-layer chromatography was petroleum ether and ethyl acetate in a volume ratio of 4:1.
[0072] S2: 135g of triazine intermediate was added to 325mL of acetone, followed by 22g of ethylenediamine. The mixture was reacted at 33℃ for 5.5h. Thin-layer chromatography was used to monitor the reaction until completion. The reaction solution was cooled to room temperature and then cooled in an ice bath for 1h. The mixture was filtered, and the filter cake was washed with acetone and distilled water in sequence, repeated 3 times. The mixture was then dried under vacuum at 50℃ to constant weight to obtain product S2.
[0073] The mobile phase for thin-layer chromatography was ethyl acetate and methanol in a volume ratio of 4:1.
[0074] S3: 62g of product S2 was mixed with 126g of N,N-dimethyl-1,3-diaminopropane and reacted at 103℃ for 9h. The reaction was monitored by thin-layer chromatography until completion. The reaction solution was cooled to 50℃, 300mL of acetone was added, and then 52.5g of bromoethane was slowly added with stirring. The temperature was raised to 53℃ and the reaction was monitored by thin-layer chromatography again until completion. The mixture was filtered, and 300mL of diethyl ether was added to the filtrate to precipitate the product. The mixture was stirred and cooled in an ice bath for 2h to allow the product to precipitate. The product was then filtered, washed, and dried to obtain triazine diquaternary ammonium salt.
[0075] The mobile phase for thin-layer chromatography was ethyl acetate and methanol in a volume ratio of 9:1; the mobile phase for reused thin-layer chromatography was n-butanol, acetic acid and water in a volume ratio of 4:1:1.
[0076] S4: The anion exchange resin Amberlite IRA-400 was thoroughly washed with deionized water, then dynamically treated with 1 mol / L NaOH solution until the effluent was strongly alkaline. Finally, it was washed with deionized water until the effluent was neutral to obtain wet resin. The wet resin was packed into a glass chromatography column, and 15 g of triazine diquaternary ammonium salt was added to 150 mL of deionized water. The solution was passed through the ion exchange column at a flow rate of 1.5 BV / h. The effluent was collected, and the column was washed with 75 mL of deionized water. The effluents were combined to obtain an aqueous solution of triazine diquaternary ammonium salt hydroxide. Under ice-water bath cooling, the hydroxide was added dropwise to 75 mL of aqueous solution containing 4.5 g of glycine. After the addition was complete, the mixture was stirred at 3 °C for 4 h. 300 mL of acetone was added, and the mixture was stirred at 450 rpm. The solid was allowed to precipitate, filtered, and the filter cake was washed with cold acetone 3-5 times. The mixture was then vacuum dried at 45 °C to constant weight to obtain triazine diquaternary ammonium salt diglycine salt.
[0077] Example 1
[0078] This embodiment discloses a method for preparing a sound-absorbing wood composite floor, including the following steps:
[0079] The wood is processed to a density of 1 g / cm³ 3 The high-density fiberboard with a thickness of 10 mm is used as the substrate layer, which is existing technology. At 165°C, the surface layer prepared in Preparation Example 2, the irradiated cross-linked polyethylene foam prepared in Preparation Example 1 as the sound-absorbing layer, the substrate layer, and the balancing layer are coated with polyurethane hot melt adhesive until the adhesive coating amount reaches 140 g / m². 2 At a pressure of 7MPa, hot-pressed for 40 minutes, the two parts are bonded together to form a single unit.
[0080] The balancing layer comprises the following components by weight: 91 wt% polypropylene and 9 wt% polyolefin elastomer (POE); the thickness of the balancing layer is 1.1 mm.
[0081] Example 2
[0082] This embodiment discloses a method for preparing a sound-absorbing wood composite floor, including the following steps:
[0083] The wood is processed to a density of 0.85 g / cm³. 3 The high-density fiberboard with a thickness of 12 mm is used as the substrate layer, which is existing technology. At 140°C, the surface layer prepared in Preparation Example 2, the irradiated cross-linked polyethylene foam prepared in Preparation Example 1 as the sound-absorbing layer, the substrate layer, and the balancing layer are coated with EPI formaldehyde-free adhesive until the adhesive coating amount reaches 160 g / m². 2 At a pressure of 6MPa, hot-pressed for 45 minutes, the two parts are bonded together to form a single unit.
[0084] The balancing layer comprises the following components by weight: 80 wt% polypropylene and 20 wt% polyolefin elastomer (POE); the thickness of the balancing layer is 0.8 mm.
[0085] Example 3
[0086] This embodiment discloses a method for preparing a sound-absorbing wood composite floor, including the following steps:
[0087] The wood is processed to a density of 1.2 g / cm³. 3 The high-density fiberboard with a thickness of 8 mm is used as the substrate layer, which is existing technology. At 170°C, the surface layer prepared in Preparation Example 2, the irradiated cross-linked polyethylene foam prepared in Preparation Example 1 as the sound-absorbing layer, the substrate layer, and the balancing layer are coated with polyurethane hot melt adhesive until the adhesive coating amount reaches 120 g / m². 2 At a pressure of 8MPa, hot-pressed for 35 minutes, the two parts are bonded together to form a single unit.
[0088] The balancing layer comprises the following components by weight: 95 wt% polypropylene and 5 wt% polyolefin elastomer (POE); the thickness of the balancing layer is 1.5 mm.
[0089] Example 4
[0090] This embodiment discloses a method for preparing a sound-absorbing wood composite floor, including the following steps:
[0091] The wood is processed to a density of 0.9 g / cm³. 3 The high-density fiberboard with a thickness of 11 mm is used as the substrate layer, which is existing technology. At 145°C, the surface layer prepared in Preparation Example 2, the irradiated cross-linked polyethylene foam prepared in Preparation Example 1 as the sound-absorbing layer, the substrate layer, and the balancing layer are coated with EPI formaldehyde-free adhesive until the adhesive coating amount reaches 150 g / m². 2 At a pressure of 7MPa, hot-pressed for 40 minutes, the two parts are bonded together to form a single unit.
[0092] The balancing layer comprises the following components by weight: 85 wt% polypropylene and 15 wt% polyolefin elastomer (POE); the thickness of the balancing layer is 0.9 mm.
[0093] Example 5
[0094] This embodiment discloses a method for preparing a sound-absorbing wood composite floor, including the following steps:
[0095] The wood is processed to a density of 1.1 g / cm³. 3 The high-density fiberboard with a thickness of 9 mm is used as the substrate layer, which is existing technology. At 165°C, the surface layer prepared in Preparation Example 2, the irradiated cross-linked polyethylene foam prepared in Preparation Example 1 as the sound-absorbing layer, the substrate layer, and the balancing layer are coated with polyurethane hot melt adhesive until the adhesive coating amount reaches 130 g / m². 2 At a pressure of 8MPa, hot-pressed for 35 minutes, the two parts are bonded together to form a single unit.
[0096] The balancing layer specifically comprises the following components by weight: 90 wt% polypropylene and 10 wt% polyolefin elastomer (POE); the thickness of the balancing layer is 1.3 mm.
[0097] Comparative Example 1
[0098] Compared with Example 1, Comparative Example 1 did not contain triazine diquaternary ammonium salt diglycinate in the softening solution during the preparation of the soundproof wood composite flooring, while other conditions remained unchanged.
[0099] Comparative Example 2
[0100] Compared with Example 1, Comparative Example 2 used triazine diquaternary ammonium salt, the product prepared by S3, instead of triazine diquaternary ammonium salt diglycine salt in the preparation of silent wood composite flooring, while other conditions remained unchanged.
[0101] Comparative Example 3
[0102] Compared with Example 1, Comparative Example 3 used 2.5mm thick EVA foam pads purchased from Hebei Shijiazhuang Great Wall Rubber & Plastic Co., Ltd. instead of IXPE in the process of preparing the soundproof wood composite flooring, while keeping other conditions unchanged.
[0103] Comparative Example 4
[0104] Compared to Example 1, in Comparative Example 4, the IXPE was not subjected to stepwise irradiation during the preparation of the sound-absorbing wood composite flooring. Instead, it underwent a single 75 kGy irradiation while all other conditions remained unchanged.
[0105] Noise reduction performance test method: Drop ball test, using a decibel meter to measure the maximum decibel value when the ball is dropped. The ball mass (g) is 65, the drop height (cm) is 100, the measurement position is 1m away from the sound source (m), repeated 5 times, and the average maximum sound pressure level (dB) is taken; the degree of impregnation peeling is tested according to the national standard GB / T 18103-2013 "Solid Wood Composite Flooring"; formaldehyde emission: formaldehyde emission E1 ≤ 1.5mg / L; surface abrasion resistance, abrasion revolutions, household grade II ≥ 4000; surface stain and corrosion resistance; surface crack resistance; moisture content (%); elastic modulus (MPa); surface hardness (H); the test results are shown in Table 1 and Table 2:
[0106] Table 1
[0107]
[0108] Table 2
[0109]
[0110] Based on Tables 1 and 2, and from Examples 1-5 and Comparative Examples 1-4, the sound-absorbing wood composite flooring prepared in Example 1 of the present invention has good mechanical properties and sound-absorbing properties.
[0111] Comparison of Comparative Example 1 and Examples 1-5 shows that, due to the high rigidity, high crosslinking density, but brittle three-dimensional network of melamine-formaldehyde resin after curing, the absence of triazine diquaternary ammonium salt and diglycine salt will reduce the hardness and cause cracking in the silent wood composite flooring. Comparison of Comparative Example 2 and Examples 1-5 shows that, replacing triazine diquaternary ammonium salt with the product prepared by S3, because bromide ions are inert and non-reactive small molecule anions, their dispersion stability in the melamine-formaldehyde resin solution is poor due to the ionic effect, affecting the uniform penetration and distribution in the wood. Furthermore, the absence of -NH2 on the glycine group participating in the hydroxymethylation or condensation reaction of the melamine-formaldehyde resin, thus fixing some free formaldehyde, results in a higher formaldehyde release. Comparison of Comparative Example 3 and Examples 1-5 shows that... After IXPE was replaced with EVA, the foaming material had a low degree of cross-linking and a weaker cell structure strength, resulting in lower ball drop noise, greater deformation and slower rebound during impact, with some energy being converted into internal friction and plastic deformation, leading to greater noise and a tendency for the silencing effect to weaken. As can be seen from the comparison between Comparative Example 4 and Examples 1-5, a single high-dose irradiation can cause excessive absorption of the surface layer and a sudden rise in temperature, leading to over-cross-linking or even degradation of the surface. However, due to heat accumulation and limited oxygen diffusion, the internal cross-linking is insufficient, resulting in an uneven cross-linking structure. Under long-term pressure, the weak parts are prone to irreversible collapse, and the uneven cell structure reduces the impact energy absorption and rebound efficiency, thus increasing noise. Furthermore, the surface of the IXPE sheet becomes slightly brittle due to over-irradiation, affecting the uniformity of hot pressing, which leads to a decrease in the interlayer bonding force between the sheet and the substrate layer, and the impregnation peel performance is unqualified.
[0112] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.
[0113] The preferred embodiments of the present invention disclosed above are merely illustrative of the invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the invention to specific implementations. Clearly, many modifications and variations can be made based on the content of this specification. This specification selects and specifically describes these embodiments to better explain the principles and practical applications of the invention, thereby enabling those skilled in the art to better understand and utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims
1. A sound-absorbing wood composite floor, characterized in that, The soundproof wood composite flooring comprises, from top to bottom, a surface layer, a soundproof layer, a substrate layer, and a balance layer, which are bonded together with hot melt adhesive. The preparation method of the surface layer includes the following steps: immersing the wood veneer in a reinforcing softening liquid, ultrasonically treating it, and drying it to obtain impregnated wood veneer; making the impregnated wood veneer into timber; and making the timber into veneer to obtain the surface layer. The enhanced softening solution is obtained by adding triazine diquaternary ammonium salt diglycinate and ammonia solution to melamine-formaldehyde resin and adjusting the pH. The preparation method of the triazine diquaternary ammonium salt diglycine salt includes the following steps: S1: Add cyanuric chloride to toluene, cool, and slowly add dodecylamine solution dropwise under stirring. Continue stirring and maintaining the temperature. Monitor the reaction with thin-layer chromatography until completion. Filter, wash, dry, filter again, and rotary evaporate under reduced pressure to obtain the triazine intermediate; S2: Add the triazine intermediate to acetone, then add ethylenediamine to react. Monitor the reaction with thin-layer chromatography until completion. Cool the reaction solution to room temperature and cool in an ice bath. Filter, wash, and vacuum dry to constant weight to obtain product S2; S3: React product S2 with N,N-dimethyl... The reaction was carried out by mixing triazine-1,3-diaminopropane and monitored by thin-layer chromatography until completion. After cooling, acetone was added, followed by the slow addition of bromoethane under stirring. The temperature was increased, and the reaction was monitored by thin-layer chromatography again until completion. The mixture was filtered, precipitated, stirred, and cooled in an ice bath. After filtration, washing, and drying, triazine-2-diaminopropane was obtained. S4: The triazine-2-diaminopropane was converted into an aqueous solution of triazine-2-diaminopropane hydroxide. Under ice-water bath cooling, the aqueous solution of triazine-2-diaminopropane hydroxide was added dropwise to an aqueous solution of glycine. After the addition was completed, stirring was continued, impurities were removed, and the mixture was dried under vacuum to obtain triazine-2-diaminopropane diglycinate.
2. The soundproof wood composite flooring according to claim 1, characterized in that, The sound-absorbing layer is made of IXPE with a thickness of 2-3 mm; the substrate layer is made of high-density fiberboard with a thickness of 8-12 mm; the balancing layer specifically includes the following components by weight: 80-95 wt% polypropylene, 5-20 wt% polyolefin elastomer (POE), with a thickness of 0.8-1.5 mm.
3. The sound-absorbing wood composite flooring according to claim 1, characterized in that, The preparation method of IXPE includes the following steps: P1: HDPE and ADCA are melt-blended and extruded, then granulated after water cooling, and then vacuum dried. Under the same process conditions, the mixture is melt-blended and extruded again, cooled and granulated, and then vacuum dried to obtain HDPE masterbatch granules. P2: HDPE masterbatch granules are fed into a single-screw extruder and calender, and solid sheets are obtained through extrusion and calendering. P3: Solid sheets are subjected to stepwise irradiation treatment under an electron accelerator to obtain irradiated cross-linked polyethylene; P4: Place the irradiated cross-linked polyethylene in a hot press, initially pressurize and then heat it, then quickly depressurize and cool to set, to obtain irradiated cross-linked polyethylene foam (IXPE).
4. The sound-absorbing wood composite flooring according to claim 3, characterized in that, In P1, the mass ratio of HDPE to ADCA is 85-90:10-15; melt blending is carried out in a twin-screw extruder, with the barrel-to-die temperature set at 110℃, 115℃, 120℃, 125℃, and 130℃, and the screw speed at 45-55 rpm; vacuum drying conditions: vacuum drying temperature at 45-55℃, vacuum drying time at 20-28 hours; In P2, the temperature gradient of the single-screw extrusion calender is 130℃, 135℃, 140℃, 145℃, and 145℃, with the screw speed at 45-55 rpm; The thickness of the core sheet is 1.0 mm; in P3, the electron beam energy of the electron accelerator is 10 MeV, the beam current intensity is 4 mA, and the power is 40 kW; the step-by-step irradiation treatment method is as follows: irradiation is performed with a single irradiation dose of 25 kGy, so that the total absorbed dose of the sheet reaches 75 kGy, and after each irradiation dose of 25 kGy, the sheet is cooled at room temperature before the next irradiation, until the cumulative dose reaches 75 kGy; in P4, the heating conditions are as follows: heating temperature is 180-200℃, heating time is 60-90s; the initial pressurization pressure is 10-15 MPa.
5. The sound-absorbing wood composite flooring according to claim 1, characterized in that, Ultrasonic treatment conditions: ultrasonic treatment frequency 2.1-2.5kHz, ultrasonic treatment time 10-14min, ultrasonic treatment temperature 25-30℃; wood veneer thickness 1-1.5mm; drying method: dry at 50-60℃ to a moisture content of 25-35%, then raise the temperature to 65-75℃ and dry to a moisture content of 12-16%; timber preparation method: after assembling the impregnated veneer along the grain direction, ... The wood is hot-pressed for 30-40 minutes under a pressure of 1.8-2.5 MPa and a temperature of 135-150℃. After pressing and shaping, it is aged for 24-48 hours in an environment with a temperature of 25-35℃ and a relative humidity of 50-65% to obtain timber. The preparation method of making veneer from the timber is as follows: the timber is processed into a thickness of 0.2-0.6 mm, trimmed, sanded on the back, and dried under mild conditions of 35-45℃ to a moisture content of 8-12%.
6. The sound-absorbing wood composite flooring according to claim 1, characterized in that, The ammonia solution has a mass fraction of 35 wt%; the pH is adjusted to 7.5-8.5; the triazine diquaternary ammonium salt diglycine salt accounts for 5-8 wt% of the melamine-formaldehyde resin; the solid content of the melamine-formaldehyde resin adhesive solution is 50-60%, the viscosity is 10-18 mPa·s, and the pH is 7.5-8.
5.
7. The sound-absorbing wood composite flooring according to claim 1, characterized in that, In step S1, the dodecylamine solution is prepared as follows: 180-360g of dodecylamine is added to 400-800mL of toluene to obtain a dodecylamine solution; the ratio of cyanuric chloride to toluene is 162-324g:1.2-2.4L; the cooling temperature is -5 to 0℃; the stirring speed is 300-600rpm; the slow dropwise addition time is 1-2h; the reaction time with stirring and maintaining the temperature is 3-4h; the mobile phase for thin-layer chromatography is petroleum ether and ethyl acetate with a volume ratio of 4:1; the washing method is: the filtrate is washed sequentially with 1mol / L HCl and 1mol / L... Wash with NaHCO3 solution until neutral; washing method: dry with anhydrous sodium sulfate overnight; rotary evaporation temperature: 35-45℃; in S2, the molar ratio of triazine intermediate, acetone, and ethylenediamine is 90-180g:250-500mL:14.4-28.8g; reaction conditions: reaction temperature: 30-35℃, reaction time: 5-6h; the mobile phase for thin-layer chromatography is ethyl acetate and methanol in a volume ratio of 4:1; ice bath cooling time: 0.5-1.5h; washing method: wash the filter cake with acetone and distilled water sequentially, repeating 2-3 times; vacuum drying temperature: 45-55℃; in S3, the molar ratio of S2 product, N,N-dimethyl-1,3-diaminopropane, acetone, and bromoethane is 41.9-8 4g:83.2-165g:200-400mL:35.1-70g; Reaction conditions: reaction temperature 100-105℃, reaction time 8-10h; Mobile phase for thin-layer chromatography: ethyl acetate and methanol (volume ratio 9:1); Cooling temperature 45-55℃; Heating temperature 50-55℃; Mobile phase for reused thin-layer chromatography: n-butanol, acetic acid, and water (volume ratio 4:1:1); Precipitation method: add 200-400mL of diethyl ether to the filtrate; stirring and cooling in an ice bath for 1.5-2.5h; Washing method: wash 2-3 times with cold ethyl acetate; In S4, the preparation method of the triazine bisquaternary ammonium hydroxide aqueous solution is: using anion exchange resin Amberlite IRA-400 is thoroughly washed with deionized water, then dynamically treated with 1 mol / L NaOH solution until the effluent is strongly alkaline, and finally washed with deionized water until the effluent is neutral to obtain wet resin. The wet resin is packed into a glass chromatography column, and 10-20 g of triazine bisquaternary ammonium salt is added to 100-200 mL of deionized water. The solution is passed through the ion exchange column at a flow rate of 1-2 BV / h, and the effluent is collected. The column is washed with 50-100 mL of deionized water, and the effluents are combined to obtain an aqueous solution of triazine bisquaternary ammonium salt hydroxide. In step S4, the preparation method of the glycine aqueous solution is as follows: 3-6 g of glycine is added to 50-100 mL of water; the stirring conditions are: stirring temperature is 0-5℃, and stirring time is 3.5-4 minutes.5 hours; Impurity removal method: Add 200-400 mL of acetone and stir the mixture at 300-600 rpm. Allow it to stand to precipitate the solid, filter, and wash the filter cake 3-5 times with cold acetone; Vacuum drying method: Vacuum dry at 40-50℃ to constant weight.
8. A method for preparing a sound-absorbing wood composite floor according to any one of claims 1-7, characterized in that, Includes the following steps: The surface layer, sound-absorbing layer, substrate layer and balance layer are glued together and hot-pressed to form a whole, resulting in sound-absorbing wood composite flooring; The amount of adhesive applied is 120-160g / m² 2 Pressing conditions: pressing time is 35-45 min, pressing pressure is 6-8 MPa, pressing temperature is 140-170℃, and the adhesive is polyurethane hot melt adhesive or EPI formaldehyde-free adhesive.