CN116948132A - Modified basalt fiber/polyurethane vibration and noise reduction material with excellent comprehensive performance and preparation method thereof - Google Patents

Modified basalt fiber/polyurethane vibration and noise reduction material with excellent comprehensive performance and preparation method thereof Download PDF

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CN116948132A
CN116948132A CN202310954703.7A CN202310954703A CN116948132A CN 116948132 A CN116948132 A CN 116948132A CN 202310954703 A CN202310954703 A CN 202310954703A CN 116948132 A CN116948132 A CN 116948132A
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basalt fiber
noise reduction
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李晓东
邹美帅
葛梦晨
王硕
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Beijing Institute of Technology BIT
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Beijing Institute of Technology BIT
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Abstract

The application relates to a modified basalt fiber/polyurethane vibration and noise reduction material with excellent comprehensive performance and a preparation method thereof, belonging to the technical field of polyurethane elastomers. The material is formed by curing component A, component B and component C, and has a tensile strength of more than or equal to 12.5 MPa modified basalt fiber/polyurethane vibration/noise reduction material with elongation at break more than 700% and highest sound insulation amount more than or equal to 26dB in 1600 hz; the component C is modified chopped basalt fiber subjected to surface treatment by a silane coupling agent. The silane coupling surface treatment is carried out on the chopped basalt fiber, so that the interface compatibility between the inorganic filler matrix and the organic matrix is improved. The modified chopped basalt microfiber is used as a filler to reinforce the polyurethane elastomer, so that the material with excellent comprehensive performance is obtained.

Description

Modified basalt fiber/polyurethane vibration and noise reduction material with excellent comprehensive performance and preparation method thereof
Technical Field
The application relates to a modified basalt fiber/polyurethane vibration and noise reduction material with excellent comprehensive performance and a preparation method thereof, belonging to the technical field of polyurethane elastomers.
Background
The polyurethane elastomer material becomes one of the hot spots for research in the field of vibration-damping and noise-reducing materials by virtue of the microphase separation phenomenon of the structure and the designability of soft and hard segments. However, the application range is limited due to the self performance factors, and the filler modification is a common method for improving the polymer performance. Basalt fiber is an environment-friendly fiber filler, has certain wave absorbing and wave transmitting effects due to the excellent performances of high strength, high temperature resistance, corrosion resistance and radiation resistance, has been used for reinforcing various organic matrixes, and is widely applied to the industrial field due to low cost. The inventor researches and discovers that the basalt fiber-polyurethane vibration and noise reduction material prepared by taking basalt fiber as a reinforcing material and taking polyurethane elastomer as a matrix has the reinforced mechanical property on the premise of not losing the acoustic property, but has the problems of poor interfacial compatibility and poor dispersibility between the reinforcing material and the matrix material, so that the mechanical acoustic property of the composite material is not fully exerted, and great improvement scope and improvement space are remained.
Disclosure of Invention
In view of the above, the application aims to provide a modified basalt fiber/polyurethane vibration and noise reduction material with excellent comprehensive performance and a preparation method thereof. The surface of the fiber material is modified by the silane coupling agent, so that the interface compatibility between the inorganic filler and the organic matrix is improved, the performance of the composite material is fully exerted, and the modified basalt fiber/polyurethane vibration and noise reduction material with excellent mechanical and acoustic properties is obtained.
In order to achieve the above object, the technical scheme of the present application is as follows.
A modified basalt fiber/polyurethane vibration/noise reduction material with excellent comprehensive performance is prepared from a component A, a component B and a component C through curing and forming, wherein the tensile strength is more than or equal to 12.5 MPa, the elongation at break is more than 700%, and the highest sound insulation amount in 1600hz is more than or equal to 26 dB;
the raw material components for preparing the component A comprise, by mass, 70-71 parts of polytetrahydrofuran ether glycol (PTMEG 2000) with a molecular weight of 2000, 19-20 parts of polyoxypropylene triol (330N) with a molecular weight of 4950, 7.4-7.6 parts of 1, 4-Butanediol (BDO), 0.1-0.15 part of deionized water, 0.8-1 part of a foam stabilizer, 0.05-0.1 part of a catalyst A1 (prepared by mixing dimethylaminoethyl ether and dipropylene glycol (DPG) according to a mass ratio of 7:3), and 0.005-0.01 part of dibutyltin dilaurate (T-12);
the component B is a prepolymer of R=6.45-6.5 formed by reacting isocyanate with PTMEG 2000; r is the number ratio of isocyanic acid radical to hydroxyl radical in the system;
the molar ratio of the active-H contained in the component A to the-NCO group contained in the component B is 1.03-1.07: 1, a step of; wherein the active-H is active-H and H in-OH of PTMEG2000 and BDO 2 The sum of active-H in O; the-NCO groups contained in the B component refer to the-NCO in the prepolymer formed after the reaction of the isocyanate with PTMEG 2000;
the component C is modified chopped basalt fiber subjected to surface treatment by a silane coupling agent, and is prepared by the following method: adding chopped basalt fibers into the silane coupling agent solution, stirring, dispersing uniformly, and drying to obtain modified chopped basalt fibers; the length of the chopped basalt fiber is 50-100 mu m, and the length-diameter ratio is 2.8-5.6; the silane coupling agent is KH550 or KH560; the mass ratio of KH550 to the chopped basalt fiber is 0.5-1:5-7; the mass ratio of KH560 to the chopped basalt fiber is 1.5-2:5-7;
the addition amount of the component C is 1-12% of the total mass of the component A and the component B.
Preferably, in preparing the A component, T-12 is first dissolved in 330N and then mixed with PTMEG2000, BDO, deionized water, a foam stabilizer and catalyst A1.
Preferably, the foam homogenizing agent in the component A is foam homogenizing silicone oil G580.
Preferably, the component B is a prepolymer formed by stirring and reacting isocyanate and PTMEG2000 in a protective gas atmosphere at 80-85 ℃ for 3.5-4.5 hours.
Preferably, the isocyanate is 4,4' -diphenylmethane diisocyanate (MDI).
Preferably, the total parts of the raw materials for preparing the component B are 100 parts, and the raw materials comprise the following components in parts by weight: 40-60 parts of MDI; 40-60 parts of PTMEG 2000.
Preferably, the water content of each of the PTMEG2000, 330N and BDO is less than or equal to 500 ppm.
Preferably, the addition amount of the component C is 5% -10% of the total mass of the component A and the component B.
Preferably, the silane coupling agent solution is prepared by mixing KH550 with water and ethanol, wherein the volume ratio of water to ethanol is 9:1; or adjusting the pH of the aqueous solution to 3.0-4.5 by using acetic acid with the mass fraction of 0.1%, and adding KH560 to prepare the aqueous solution.
The application discloses a preparation method of a modified basalt fiber/polyurethane vibration and noise reduction material with excellent comprehensive performance, which comprises the following steps:
mixing the components A and B preheated to (30+/-2) DEG C, adding the components C while stirring, mixing (25+/-5) s, vacuum defoaming, filling into a die preheated to (75+/-5) DEG C, curing for 20-30 min at (75+/-5) DEG C, and curing for 48+/-5 h at (25+/-5) DEG C to obtain the basalt fiber-polyurethane acoustic material with excellent mechanical properties.
Preferably, the rotation speed is 1800-2200r/min during stirring.
Preferably, the vacuum degree is less than or equal to 0.01 MPa in vacuum defoaming.
Advantageous effects
The application provides a modified basalt fiber/polyurethane vibration and noise reduction material with excellent comprehensive performance, which improves the interface compatibility between an inorganic filler matrix and an organic matrix by carrying out silane coupling surface treatment on chopped basalt fibers. The modified basalt fiber/polyurethane vibration/noise reduction material with excellent comprehensive performance is obtained by using the modified chopped basalt microfiber as a filler to reinforce the polyurethane elastomer, so that the mechanical property (tensile strength is more than or equal to 12.5 MPa and elongation at break is more than 700%) and the acoustic property (excellent medium-high frequency band sound insulation performance, up to 28 dB) of the prepared basalt fiber-polyurethane composite material are obviously improved, and the modified basalt fiber/polyurethane vibration/noise reduction material has a good application prospect.
The basalt fiber-polyurethane acoustic material with excellent mechanical properties provided by the application has the advantages that the material properties and the coupling agent consumption have nonlinear relations, and critical thresholds are reserved on sound insulation and mechanical performance. The modified basalt fiber reinforced polyurethane material with good comprehensive performance can be obtained only by selecting the right coupling agent and the proper addition amount, the coupling agent improves the dispersibility of the filler in the matrix, and the basalt fiber provides skeleton support for the matrix of the material, and the three complement each other and act synergistically. Furthermore, the silane coupling agent is selected, and the binding property of different agents, fillers and matrixes is different, so that certain performance difference can be generated (for example, the binding property of KH550 and the matrixes is stronger than that of KH560, and meanwhile, after KH560 is modified, the surface of the fillers is coated with a film, so that the roughness of the materials is reduced, and the performance of the materials is influenced).
Detailed Description
The present application will be described in further detail with reference to specific examples.
Example 1
(1) And respectively adopting a water pump and an oil pump to carry out vacuum dehydration treatment on the PTMEG2000, 330N and BDO until the water content is less than or equal to 500 ppm.
(2) Dissolving 0.005 part of T-12 into 250 parts of dehydrated 330N, diluting and uniformly mixing to obtain 330N containing T-12; 70.9 parts of dehydrated PTMEG2000, 19.7 parts of dehydrated BDO containing T-12, 7.4 parts of dehydrated BDO, 0.15 part of deionized water, 1 part of foam homogenizing agent (foam homogenizing silicone oil G580) and 0.1 part of catalyst (Shanghai Zhenzhi new material science and technology Co., ltd.) are uniformly mixed to obtain a component A.
45 parts of MDI and 55 parts of PTMEG are mixed uniformly under a nitrogen protection atmosphere and reacted for 4 hours at 80 ℃ with stirring to obtain a prepolymer terminated by-NCO, which is abbreviated as a component B and has an NCO content of 12.5%.
Ball milling and crushing basalt fibers with average diameter of 17 mu m and length of 6 mm, which are purchased from Sichuan Pawalk mineral fiber products limited company, for 3min to obtain chopped basalt fibers with length of 50-100 mu m and length-diameter ratio of 2.8-5.6; mixing water and ethanol according to a volume ratio of 9:1 to obtain a solvent, sequentially adding 1 part of KH550 into each 100 parts by mass of the solvent, adding 6 parts of chopped basalt fibers into the solvent, stirring for 30min, performing ultrasonic treatment for 10min, drying the solution at 120 ℃ to obtain modified chopped basalt fibers, and taking 6 parts of modified chopped basalt fibers as a component C.
(3) The A component and the B component are respectively preheated to 30 ℃, then the preheated A component and the B component are mixed according to the mol ratio of-OH groups in the A component to-NCO groups in the B component of 1.05 (namely 53.4 parts of A component and 46.6 parts of B component) and stirred and mixed with the C component for 30s at the rotating speed of 2000 rpm, then the mixture is placed in a vacuum degree of less than or equal to 0.01 MPa for vacuum defoaming for 10min, then the mixture is placed in a die preheated to 70 ℃, then the mixture is placed in an oven at 70 ℃ for curing for 20min, and then the mixture is cured for 50h at 25 ℃ to obtain the modified basalt fiber/polyurethane vibration and noise reduction material with excellent comprehensive properties.
The tensile strength and elongation at break of the modified basalt fiber/polyurethane vibration/noise reduction material are tested according to the standard GB/T1040.3-2006, the tensile strength of the modified basalt fiber/polyurethane vibration/noise reduction material is 13.04MPa, the elongation at break is 835%, the acoustic performance is tested according to the GBT 19889-2005 by adopting an impedance tube method/standing wave tube method, and the highest sound insulation amount within 1600hz is 28dB.
Example 2
(1) And respectively adopting a water pump and an oil pump to carry out vacuum dehydration treatment on the PTMEG2000, 330N and BDO until the water content is less than or equal to 500 ppm.
(2) Dissolving 0.0045 parts of T-12 into 250 parts of dehydrated 330N, diluting and uniformly mixing to obtain 330N containing T-12; 70.8 parts of dehydrated PTMEG2000, 19.5 parts of dehydrated BDO containing T-12, 7.5 parts of dehydrated BDO, 0.1 part of deionized water, 1 part of foam homogenizing agent (foam homogenizing silicone oil G580) and 0.1 part of catalyst (Shanghai Zhenzhi new material science and technology Co., ltd.) are uniformly mixed to obtain a component A.
44 parts of MDI and 56 parts of PTMEG are mixed uniformly under a nitrogen protection atmosphere and reacted for 4.2 hours under stirring at 85 ℃ to obtain a prepolymer terminated by-NCO, which is abbreviated as a component B and has an NCO content of 12.6%.
Ball milling and crushing basalt fibers with average diameter of 17 mu m and length of 6 mm, which are purchased from Sichuan Pawalk mineral fiber products limited company, for 3min to obtain chopped basalt fibers with length of 50-100 mu m and length-diameter ratio of 2.8-5.6; adjusting the pH value of the aqueous solution to 3.0-4.5 by using acetic acid with the mass fraction of 0.1%, then dropwise adding a silane coupling agent KH560, sequentially adding 1.5 parts of KH560 into every 100 parts of solvent, adding 6 parts of chopped basalt fibers into the solvent, stirring for 30min, performing ultrasonic treatment for 10min, drying the solution at 120 ℃ to obtain modified chopped basalt fibers, and taking 6 parts of modified chopped basalt fibers as a component C.
(3) The A component and the B component are respectively preheated to 28 ℃, then the preheated A component and the B component are mixed according to the mol ratio of-OH groups in the A component to-NCO groups in the B component of 1.07 (namely 53 parts of A component and 47 parts of B component) and stirred and mixed for 30s at the rotation speed of 2200 rpm, then the mixture is placed in a condition that the vacuum degree is less than or equal to 0.01 MPa for vacuum defoamation for 8min, and then the mixture is placed in a mould preheated to 75 ℃, then the mixture is placed in an oven at 75 ℃ for curing for 20min, and then the mixture is cured for 50h at 28 ℃ to obtain the modified basalt fiber/polyurethane vibration/noise reduction material with excellent comprehensive properties.
The tensile strength and the elongation at break of the modified basalt fiber/polyurethane vibration and noise reduction material are tested according to the standard GB/T1040.3-2006, and the tensile strength of the modified basalt fiber/polyurethane vibration and noise reduction material is 12.75MPa and the elongation at break is 704%. Acoustic performance was tested by impedance tube/standing wave tube method with reference to GBT 19889-2005, with a maximum sound insulation of 27dB at 1600 hz.
Comparative example 1
(1) And respectively adopting a water pump and an oil pump to carry out vacuum dehydration treatment on the PTMEG2000, 330N and BDO until the water content is less than or equal to 500 ppm.
(2) Dissolving 0.0045 parts of T-12 into 250 parts of dehydrated 330N, diluting and uniformly mixing to obtain 330N containing T-12; 70.8 parts of dehydrated PTMEG2000, 19.5 parts of dehydrated BDO containing T-12, 7.5 parts of dehydrated BDO, 0.1 part of deionized water, 1 part of foam homogenizing agent (foam homogenizing silicone oil G580) and 0.1 part of catalyst (Shanghai Zhenzhi new material science and technology Co., ltd.) are uniformly mixed to obtain a component A.
44 parts of MDI and 56 parts of PTMEG are mixed uniformly under a nitrogen protection atmosphere and reacted for 4.2 hours under stirring at 85 ℃ to obtain a prepolymer terminated by-NCO, which is abbreviated as a component B and has an NCO content of 12.6%.
Ball milling and crushing basalt fibers with average diameter of 17 mu m and length of 6 mm, which are purchased from Sichuan Pawalk mineral fiber products limited company, for 3min to obtain chopped basalt fibers with length of 50-100 mu m and length-diameter ratio of 2.8-5.6; regulating the pH value of the aqueous solution to 3.0-4.5 by using acetic acid with the mass fraction of 0.1%, then dropwise adding a silane coupling agent KH560, sequentially adding 1 part of KH560 into each 100 parts by mass of solvent, adding 6 parts of chopped basalt fibers into the solvent, stirring for 30min, performing ultrasonic treatment for 10min, drying the solution at 120 ℃ to obtain modified chopped basalt fibers, and taking 6 parts of modified chopped basalt fibers as a component C.
(3) The A component and the B component are respectively preheated to 28 ℃, then the preheated A component and the B component are mixed according to the mol ratio of-OH groups in the A component to-NCO groups in the B component of 1.07 (namely 53 parts of A component and 47 parts of B component) and stirred and mixed for 30s at the rotation speed of 2200 rpm, then the mixture is placed in a condition that the vacuum degree is less than or equal to 0.01 MPa for vacuum defoamation for 8min, and then the mixture is placed in a mould preheated to 75 ℃, then the mixture is placed in an oven at 75 ℃ for curing for 20min, and then the mixture is cured for 50h at 28 ℃ to obtain the modified basalt fiber/polyurethane vibration and noise reduction material.
The tensile strength and the elongation at break of the modified basalt fiber/polyurethane vibration and noise reduction material are tested according to the standard GB/T1040.3-2006, and the tensile strength of the modified basalt fiber/polyurethane vibration and noise reduction material is 10.57MPa and the elongation at break is 515.62%. Acoustic performance was tested by impedance tube/standing wave tube method with reference to GBT 19889-2005, with a maximum sound insulation of 23dB at 1600 hz.
Comparative example 2
(1) And respectively adopting a water pump and an oil pump to carry out vacuum dehydration treatment on the PTMEG2000, 330N and BDO until the water content is less than or equal to 500 ppm.
(2) Dissolving 0.005 part of T-12 into 250 parts of dehydrated 330N, diluting and uniformly mixing to obtain 330N containing T-12; 70.9 parts of dehydrated PTMEG2000, 19.7 parts of dehydrated BDO containing T-12, 7.4 parts of dehydrated BDO, 0.15 part of deionized water, 1 part of foam homogenizing agent (foam homogenizing silicone oil G580) and 0.1 part of catalyst (Shanghai Zhenzhi new material science and technology Co., ltd.) are uniformly mixed to obtain a component A.
45 parts of MDI and 55 parts of PTMEG are mixed uniformly under a nitrogen protection atmosphere and reacted for 4 hours at 80 ℃ with stirring to obtain a prepolymer terminated by-NCO, which is abbreviated as a component B and has an NCO content of 12.5%.
Ball milling and crushing basalt fibers with average diameter of 17 mu m and length of 6 mm, which are purchased from Sichuan Pawalk mineral fiber products limited company, for 3min to obtain chopped basalt fibers with length of 50-100 mu m and length-diameter ratio of 2.8-5.6; mixing water and ethanol according to a volume ratio of 9:1 to obtain a solvent, sequentially adding 2 parts of KH550 into each 100 parts by mass of the solvent, adding 6 parts of chopped basalt fibers into the solvent, stirring for 30min, performing ultrasonic treatment for 10min, drying the solution at 120 ℃ to obtain modified chopped basalt fibers, and taking 6 parts of modified chopped basalt fibers as a component C.
(3) The A component and the B component are respectively preheated to 30 ℃, then the preheated A component and the B component are mixed according to the mol ratio of-OH groups in the A component to-NCO groups in the B component of 1.05 (namely 53.4 parts of A component and 46.6 parts of B component) and stirred and mixed with the C component for 30s at the rotating speed of 2000 rpm, then the mixture is placed in a vacuum degree of less than or equal to 0.01 MPa for vacuum defoaming for 10min, then the mixture is placed in a die preheated to 70 ℃, then the mixture is placed in an oven at 70 ℃ for curing for 20min, and then the mixture is cured for 50h at 25 ℃ to obtain the modified basalt fiber/polyurethane vibration-damping noise-reducing material.
The tensile strength and elongation at break of the modified basalt fiber/polyurethane vibration/noise reduction material are tested according to the standard GB/T1040.3-2006, the tensile strength of the modified basalt fiber/polyurethane vibration/noise reduction material is 9.95MPa, the elongation at break is 577.73%, the acoustic performance is tested according to the GBT 19889-2005 by adopting an impedance tube method/standing wave tube method, and the highest sound insulation amount is 25dB within 1600 hz.
In view of the foregoing, it will be appreciated that the application includes but is not limited to the foregoing embodiments, any equivalent or partial modification made within the spirit and principles of the application.

Claims (10)

1. A modified basalt fiber/polyurethane vibration/noise reduction material with excellent comprehensive performance is characterized in that: the modified basalt fiber/polyurethane vibration/noise reduction material is prepared by curing and molding the component A, the component B and the component C, and has the tensile strength of more than or equal to 12.5 MPa, the elongation at break of more than 700 percent and the highest sound insulation amount within 1600hz of more than or equal to 26 dB;
the raw material components for preparing the component A comprise, by mass, 70-71 parts of PTMEG2000, 19-20 parts of 330N, 7.4-7.6 parts of BDO, 0.1-0.15 part of deionized water, 0.8-1 part of a foam stabilizer, 0.05-0.1 part of a catalyst A and 0.005-0.01 part of T-12;
the component B is a prepolymer of R=6.45-6.5 formed by reacting isocyanate with PTMEG 2000; r is the number ratio of isocyanic acid radical to hydroxyl radical in the system;
the molar ratio of the active-H contained in the component A to the-NCO group contained in the component B is 1.03-1.07: 1, a step of;
the component C is modified chopped basalt fiber subjected to surface treatment by a silane coupling agent, and is prepared by the following method: adding chopped basalt fibers into the silane coupling agent solution, stirring, dispersing uniformly, and drying to obtain modified chopped basalt fibers; the length of the chopped basalt fiber is 50-100 mu m, and the length-diameter ratio is 2.8-5.6; the silane coupling agent is KH550 or KH560; the mass ratio of KH550 to the chopped basalt fiber is 0.5-1:5-7; the mass ratio of KH560 to the chopped basalt fiber is 1.5-2:5-7;
the addition amount of the component C is 1-12% of the total mass of the component A and the component B.
2. The modified basalt fiber/polyurethane vibration/noise reduction material with excellent comprehensive performance according to claim 1, which is characterized in that: in preparing the A component, T-12 is dissolved in 330N and then mixed with PTMEG2000, BDO, deionized water, a foam stabilizer and catalyst A1.
3. The modified basalt fiber/polyurethane vibration/noise reduction material with excellent comprehensive performance according to claim 1, which is characterized in that: the foam homogenizing agent in the component A is foam homogenizing silicone oil G580.
4. The modified basalt fiber/polyurethane vibration/noise reduction material with excellent comprehensive performance according to claim 1, which is characterized in that: the component B is a prepolymer formed by stirring and reacting isocyanate and PTMEG2000 in a protective gas atmosphere at 80-85 ℃ for 3.5-4.5 hours.
5. The modified basalt fiber/polyurethane vibration/noise reduction material with excellent comprehensive performance according to claim 1, which is characterized in that: the isocyanate is MDI;
the total parts of raw materials for preparing the component B are 100 parts, and the raw materials comprise the following components in parts by mass: 40-60 parts of MDI; 40-60 parts of PTMEG 2000.
6. The modified basalt fiber/polyurethane vibration/noise reduction material with excellent comprehensive performance according to claim 1, which is characterized in that: the water content of the PTMEG2000, 330N and BDO is less than or equal to 500 ppm.
7. The modified basalt fiber/polyurethane vibration/noise reduction material with excellent comprehensive performance according to claim 1, which is characterized in that: the addition amount of the component C is 5% -10% of the total mass of the component A and the component B.
8. The modified basalt fiber/polyurethane vibration/noise reduction material with excellent comprehensive performance according to claim 1, which is characterized in that: the silane coupling agent solution is prepared by mixing KH550 with water and ethanol, and the volume ratio of water to ethanol is 9:1; or adjusting the pH of the aqueous solution to 3.0-4.5 by using acetic acid with the mass fraction of 0.1%, and adding KH560 to prepare the aqueous solution.
9. A method for preparing the modified basalt fiber/polyurethane vibration/noise reduction material with excellent comprehensive performance according to any one of claims 1 to 8, which is characterized in that: the method comprises the following steps:
mixing the components A and B preheated to (30+/-2) DEG C, adding the components C while stirring, mixing (25+/-5) s, vacuum defoaming, filling into a die preheated to (75+/-5) DEG C, curing for 20-30 min at (75+/-5) DEG C, and curing for 48+/-5 h at (25+/-5) DEG C to obtain the basalt fiber-polyurethane acoustic material with excellent mechanical properties.
10. The method for preparing the modified basalt fiber/polyurethane vibration/noise reduction material with excellent comprehensive performance according to claim 9, which is characterized in that: the rotation speed is 1800-2200 r/min during stirring; the vacuum degree is less than or equal to 0.01 MPa during vacuum defoaming.
CN202310954703.7A 2023-08-01 2023-08-01 Modified basalt fiber/polyurethane vibration and noise reduction material with excellent comprehensive performance and preparation method thereof Pending CN116948132A (en)

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