CN116903822A - Basalt fiber-polyurethane acoustic material with excellent mechanical properties and preparation method thereof - Google Patents

Basalt fiber-polyurethane acoustic material with excellent mechanical properties and preparation method thereof Download PDF

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CN116903822A
CN116903822A CN202310954978.0A CN202310954978A CN116903822A CN 116903822 A CN116903822 A CN 116903822A CN 202310954978 A CN202310954978 A CN 202310954978A CN 116903822 A CN116903822 A CN 116903822A
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basalt fiber
acoustic material
mechanical properties
parts
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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 invention relates to a basalt fiber-polyurethane acoustic material with excellent mechanical properties and a preparation method thereof, belonging to the technical field of polyurethane elastomers. The basalt fiber-polyurethane acoustic material with tensile strength more than or equal to 12 MPa and elongation at break more than 600% is obtained by curing and molding the component A, the component B and the component C; the component C is chopped basalt fibers with the length of 50 mu m-100 mu m and the length-diameter ratio of 2.8-5.6; the addition amount of the component C is 3-12% of the total mass of the component A and the component B. The basalt microfiber is used as filler to strengthen the polyurethane elastomer, and the addition amount and the filler size of the filler are accurately controlled, so that the tensile strength of the prepared basalt fiber-polyurethane acoustic material is more than or equal to 12 MPa, and the elongation at break is more than 600%.

Description

Basalt fiber-polyurethane acoustic material with excellent mechanical properties and preparation method thereof
Technical Field
The invention relates to a basalt fiber-polyurethane acoustic material with excellent mechanical properties and a preparation method thereof, belonging to the technical field of polyurethane elastomers.
Background
Since the industrial revolution, the global technology has been rapidly developed, and the aspects of human production and life are expanded by mechanization, and the physical and mental health of human beings is also endangered by vibration noise caused by mechanical operation. 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.
The conventional porous polyurethane elastomer matrix acoustic material cannot avoid defects such as bubbles and the like in the preparation process, so that theoretical mechanical properties cannot be achieved, if the pore structure of the material is excessive, the prepared polyurethane acoustic material has the defect of relatively poor mechanical properties, and in application scenes such as automobile and aircraft interior trim, the acoustic properties and the mechanical properties are difficult to be considered, so that the application range of vibration reduction and noise reduction is limited.
Disclosure of Invention
In view of the above, the invention aims to provide a basalt fiber-polyurethane acoustic material with excellent mechanical properties and a preparation method thereof. The chopped basalt fiber which is low in production cost and excellent in performance and is green and environment-friendly is selected as a filler reinforcing phase, is introduced in the preparation process of the polyurethane acoustic material matrix, the content of each component is strictly regulated and controlled, and meanwhile, the process conditions are optimized, so that the mechanical properties of the polyurethane acoustic material can be further improved under the condition that other performances are not influenced.
In order to achieve the above object, the technical scheme of the present invention is as follows.
The basalt fiber-polyurethane acoustic material with excellent mechanical properties is prepared from a basalt fiber-polyurethane acoustic material with tensile strength more than or equal to 12 MPa and elongation at break more than 600% obtained by curing and forming of a component A, a component B and a component C;
the raw material components for preparing the component A comprise, by mass, 70-72 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, 7.3-7.5 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 chopped basalt fibers with the length of 50 mu m-100 mu m and the length-diameter ratio of 2.8-5.6;
the addition amount of the component C is 3-12% 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 8% -10% of the total mass of the component A and the component B.
The invention discloses a preparation method of basalt fiber-polyurethane acoustic material with excellent mechanical properties, 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 basalt fiber-polyurethane acoustic material with excellent mechanical properties is provided by the invention, the chopped basalt microfiber is used as the filler to reinforce the polyurethane elastomer, and the tensile strength of the prepared basalt fiber-polyurethane acoustic material is more than or equal to 12 MPa and the elongation at break of the prepared basalt fiber-polyurethane acoustic material is more than 600% by precisely controlling the addition amount and the filler size of the filler, so that the basalt fiber-polyurethane acoustic material has good application prospect on the premise of not reducing the acoustic properties of a material matrix and is respectively improved by more than 30% and more than 20% compared with the matrix.
The basalt fiber-polyurethane acoustic material with excellent mechanical properties provided by the invention can obtain ideal properties only by basalt fibers with proper sizes, and excessive or insufficient basalt fibers can cause material defects, prevent material chain segment movement or influence the effect of energy dissipation. The basalt fiber can improve mechanical reinforcement for the polyurethane matrix, and the elastic polyurethane and the rigid basalt fiber are combined to have synergistic effect, so that the basalt fiber reinforced polyurethane composite material has good mechanical, acoustic and other performances.
Detailed Description
The present invention 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%.
3 parts of basalt fiber with average diameter of 17 mu m and length of 6 mm purchased from Sichuan Pawalk mineral fiber products Co., ltd. Are crushed by ball milling for 3min to obtain chopped basalt fiber with length of 50-100 mu m and length-diameter ratio of 2.8-5.6 as a C component.
(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 48h at 25 ℃ to obtain the basalt fiber-polyurethane acoustic material with excellent mechanical properties.
And carrying out microscopic morphological characterization on the basalt fiber-polyurethane acoustic material, wherein the SEM result shows that the tensile section of the basalt fiber-polyurethane acoustic material has no obvious bubbles, which indicates that the defoaming is complete in the preparation process. The tensile strength and the elongation at break of the basalt fiber-polyurethane acoustic material were tested with reference to standard GB/T1040.3-2006, and the tensile strength and the elongation at break of the basalt fiber-polyurethane acoustic material were measured to be 12.13 MPa and 622.97%.
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%.
9 parts of basalt fibers with average diameter of 17 mu m and length of 6 mm purchased from Sichuan Pawalk mineral fiber products Co., ltd. Are crushed by ball milling for 3min to obtain chopped basalt fibers with length of 50-100 mu m and length-diameter ratio of 2.8-5.6 as a C component.
(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 48h at 28 ℃ to obtain the basalt fiber-polyurethane acoustic material with excellent mechanical properties.
The microscopic appearance of the basalt fiber-polyurethane acoustic material is characterized, and it can be observed that basalt fibers in the prepared polyurethane elastomer are inserted into a matrix, embedded around cells and arranged in an anisotropic manner. The tensile strength and the elongation at break of the basalt fiber-polyurethane acoustic material were tested with reference to standard GB/T1040.3-2006, and the tensile strength and the elongation at break of the basalt fiber-polyurethane acoustic material were measured to be 13.28MPa and 770.99%.
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 0.005 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%.
3 parts of basalt fibers with average diameter of 17 mu m and length of 6 mm purchased from Sichuan Pawalk mineral fiber products limited company are crushed by ball milling for 5min to obtain chopped basalt fibers with length of 50 mu m and length-diameter ratio of 2.8 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 mold preheated to 70 ℃ under the vacuum degree of less than or equal to 0.01 MPa for 10min for vacuum defoaming, and then the mixture is placed in an oven at 70 ℃ for curing for 20min and then cured for 48h at 25 ℃ to obtain the basalt fiber-polyurethane acoustic material.
And carrying out microscopic morphological characterization on the basalt fiber-polyurethane acoustic material, wherein the SEM result shows that the basalt fiber-polyurethane acoustic material has no obvious bubbles, which indicates that the defoaming is complete in the preparation process. The tensile strength and the elongation at break of the basalt fiber-polyurethane acoustic material were tested with reference to standard GB/T1040.3-2006, and the tensile strength and the elongation at break of the basalt fiber-polyurethane acoustic material were measured to be 10.14 MPa and 541.98%.
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 were mixed homogeneously under a nitrogen atmosphere and reacted at 80℃with stirring for 4. 4h to give a prepolymer terminated with-NCO, abbreviated as component B and having an NCO content of 12.5%.
15 parts of basalt fibers with average diameter of 17 mu m and length of 6 mm purchased from Sichuan Pawalk mineral fiber products Co., ltd. Are crushed by ball milling for 3min to obtain chopped basalt fibers with length of 50-100 mu m and length-diameter ratio of 2.8-5.6 as a C component.
(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 mold preheated to 70 ℃ under the vacuum degree of less than or equal to 0.01 MPa for 10min for vacuum defoaming, and then the mixture is placed in an oven at 70 ℃ for curing for 20min and then cured for 48h at 25 ℃ to obtain the basalt fiber-polyurethane acoustic material.
And carrying out microscopic morphological characterization on the basalt fiber-polyurethane acoustic material, wherein the SEM result shows that the basalt fiber-polyurethane acoustic material has no obvious bubbles on the tensile section, which indicates that the defoaming is complete in the preparation process. The basalt fiber-polyurethane acoustic material is tested for tensile strength and elongation at break with reference to standard GB/T1040.3-2006, and the tensile strength of the polyurethane elastomer is 10.37 MPa and the elongation at break is 611.60%.
According to the mechanical properties of the materials in examples 1-2 and comparative examples 1-2, the tensile strength and the elongation at break of the polyurethane elastomer are obviously improved by introducing the chopped basalt fiber as the reinforcing phase of the polyurethane matrix. Under the condition of the same basalt fiber addition amount, only basalt fiber fillers with proper sizes (controlled by ball milling crushing time) can obtain good performance, the crushing time is too long, the basalt fiber size is too short, and external impact cannot be effectively supported, conducted or even dissipated, so that the mechanical property of the composite material is poor. In addition, under the basalt fiber with the same size, the filler addition amount of the composite material has an optimal threshold value, and the composite material performance and the basalt fiber addition amount are not in a linear relationship.
In view of the foregoing, it will be appreciated that the invention includes but is not limited to the foregoing embodiments, any equivalent or partial modification made within the spirit and principles of the invention.

Claims (10)

1. A basalt fiber-polyurethane acoustic material with excellent mechanical properties is characterized in that: the basalt fiber-polyurethane acoustic material with tensile strength more than or equal to 12 MPa and elongation at break more than 600% is obtained by curing and molding the component A, the component B and the component C;
the raw material components for preparing the component A comprise the following components in parts by mass: 70-72 parts of PTMEG2000, 19-20 parts of 330N, 7.3-7.5 parts of BDO, 0.1-0.15 part of deionized water, 0.8-1 part of foam stabilizer, 0.05-0.1 part of 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 chopped basalt fibers with the length of 50 mu m-100 mu m and the length-diameter ratio of 2.8-5.6;
the addition amount of the component C is 3-12% of the total mass of the component A and the component B.
2. The basalt fiber-polyurethane acoustic material with excellent mechanical properties according to claim 1, wherein: 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 basalt fiber-polyurethane acoustic material with excellent mechanical properties according to claim 1, wherein: the foam homogenizing agent in the component A is foam homogenizing silicone oil G580.
4. The basalt fiber-polyurethane acoustic material with excellent mechanical properties according to claim 1, wherein: 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 basalt fiber-polyurethane acoustic material with excellent mechanical properties according to claim 4, wherein: the isocyanate is MDI.
6. The basalt fiber-polyurethane acoustic material with excellent mechanical properties according to claim 5, wherein: 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.
7. The basalt fiber-polyurethane acoustic material with excellent mechanical properties according to claim 1, wherein: the water content of the PTMEG2000, 330N and BDO is less than or equal to 500 ppm.
8. The basalt fiber-polyurethane acoustic material with excellent mechanical properties according to claim 1, wherein: the addition amount of the component C is 8% -10% of the total mass of the component A and the component B.
9. A method for preparing the basalt fiber-polyurethane acoustic material with excellent mechanical properties 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 basalt fiber-polyurethane acoustic material with excellent mechanical properties 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.
CN202310954978.0A 2023-08-01 2023-08-01 Basalt fiber-polyurethane acoustic material with excellent mechanical properties and preparation method thereof Pending CN116903822A (en)

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