CN116333252A - Flame-retardant polyurethane vibration-damping sound-insulating pad without combustion droppings/particles and preparation method thereof - Google Patents

Flame-retardant polyurethane vibration-damping sound-insulating pad without combustion droppings/particles and preparation method thereof Download PDF

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CN116333252A
CN116333252A CN202310154297.6A CN202310154297A CN116333252A CN 116333252 A CN116333252 A CN 116333252A CN 202310154297 A CN202310154297 A CN 202310154297A CN 116333252 A CN116333252 A CN 116333252A
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component
parts
sound
polyurethane
damping
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郭亚莉
张剑平
张旭东
吴敬朋
高瑞
彭鹏
王传琦
夏义兵
于学俊
甄茂民
赵萌
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Shandong Aozo New Materials Co ltd
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Shandong Aozo New Materials Co ltd
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Abstract

The invention relates to a polyurethane vibration damping and sound insulation pad with flame retardance and no combustion droppings/particles and a preparation method thereof, and belongs to the technical field of microporous polyurethane. The vibration-damping sound-insulating pad is formed by solidifying A component and B component, wherein the A component is formed by PTMEG1000, PTMEG2000, EP330, BDO and H 2 O, foam stabilizer, BDMAE, T12, mildew inhibitor andthe flame retardant is prepared by uniformly mixing, wherein the foam homogenizing agent is a foam homogenizing agent with the brand name AK8804 of Jiangsu Midside company, and the flame retardant is EG and APP; the component B is a prepolymer with the-NCO value of 12-14 formed by stirring and reacting diisocyanate and polytetrahydrofuran ether polyol at 80-100 ℃ for 4-6 hours. The density of the vibration-damping sound-insulating pad is 200kg/m 3 ～260kg/m 3 The oxygen index is more than or equal to 26, the tensile strength is more than or equal to 1MPa, and the impact sound pressure level improvement amount is more than or equal to 30dB.

Description

Flame-retardant polyurethane vibration-damping sound-insulating pad without combustion droppings/particles and preparation method thereof
Technical Field
The invention relates to a polyurethane vibration damping and sound insulation pad with flame retardance and no combustion droppings/particles and a preparation method thereof, and belongs to the technical field of microporous polyurethane.
Background
Floor sound insulation is one of important guarantees of residential acoustic environment, and floor sound insulation difference is a problem which is not effectively solved by the residential industry in China. The resident often hears the falling sound, the footstep sound, the furniture moving sound and the like of objects of the upstairs and downstairs neighbors, and not only can the harmony of the relationship between the neighbors be affected, but also the social problem is evolved.
A flexible high-molecular material sound insulation layer (called a floating floor) is paved on the reinforced concrete floor, and a cement floor is paved on the flexible high-molecular material sound insulation layer, so that solid sound transmission can be greatly reduced. The conventional vibration damping and sound insulating materials for the floating floor mainly comprise rubber, crosslinked polyethylene and polystyrene, but the materials have the defects of poor sound insulating performance, poor durability, poor fireproof performance and the like. In addition, these materials require an increase in the laying thickness to meet the sound insulation design requirements, which results in a decrease in the actual height of use between floors and a low space utilization efficiency.
The polyurethane vibration damping and sound insulation pad has excellent vibration damping and sound insulation effects and long service life, and is an ideal floating floor sound insulation material. However, polyurethane elastomer belongs to inflammable materials, and has serious dripping phenomenon in the combustion process and serious fire hazard. Although the conventional flame retardant modification can reach the flame retardant grade above B1 grade (flame retardant), the vibration damping and sound insulation performance and durability of the flame retardant are obviously reduced, and the application value is lost.
Disclosure of Invention
In view of the above, the invention aims to provide a polyurethane vibration damping and sound insulation pad with flame retardance and no combustion droppings/particles and a preparation method thereof.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
a polyurethane vibration-damping and sound-insulating pad with flame retardance and no combustion droppings/particles is prepared from a component A and a component B through curing and forming to obtain a polyurethane vibration-damping and sound-insulating pad with the density of 200kg/m 3 ～260kg/m 3 A microporous polyurethane vibration-damping and sound-insulating pad with an oxygen index of 26 or more, a tensile strength of 1MPa or more and an impact sound pressure level improvement of 30dB or more;
the component A is prepared by uniformly mixing polyether polyol, a chain extender, a foaming agent, a foam homogenizing agent, a catalyst, a flame retardant and a mildew preventive; the polyether polyol comprises polytetrahydrofuran ether glycol (PTMEG 1000) with molecular weight of 1000, polytetrahydrofuran ether glycol (PTMEG 2000) with molecular weight of 2000 and polyoxypropylene triol (EP 330) with molecular weight of 5000; the chain extender is 1, 4-Butanediol (BDO); the foaming agent is H 2 O; the foam homogenizing agent is a foam homogenizing agent with the brand AK8804 of Jiangsu Maillard company; the catalyst comprises bis (dimethylaminoethyl) ether (BDMAE) and dibutyltin dilaurate (T12); the flame retardant is Expandable Graphite (EG) and ammonium polyphosphate (APP);
the total mass of the raw materials for preparing the component A is 100 parts, and the raw materials comprise the following components in parts by mass:
Figure BDA0004091748930000021
Figure BDA0004091748930000031
the component B is a prepolymer with the-NCO value between 12 and 14 formed by stirring and reacting diisocyanate and polytetrahydrofuran ether polyol at the temperature of 80-100 ℃ for 4-6 hours;
the total mass of the raw materials for preparing the component B is 100 parts, and the raw materials comprise the following components in parts by mass:
45-55 parts of diisocyanate;
45-55 parts of polytetrahydrofuran ether polyol;
the molar ratio of the active-H contained in the component A to the-NCO group contained in the component B is 1.00:0.98-1.03. Wherein the active-H is active-H and H in polyalcohol-OH 2 The sum of active-H in O; the-NCO groups contained in the B component are the-NCO groups remaining after the reaction of the isocyanate with the polytetrahydrofuran ether polyol, i.e.the-NCO groups in the prepolymer.
The component A comprises the following components:
preferably, the mildew inhibitor is a polyurethane mildew inhibitor with the brand name KP-M100 produced by the Buddha science popularization company or a polyurethane mildew inhibitor with the brand name M8 produced by the Dongguan Guangsi remote company.
Preferably, the raw material components and the mass parts thereof are as follows, based on 100 parts of the total mass of the raw materials for preparing the component A:
Figure BDA0004091748930000032
Figure BDA0004091748930000041
preferably, the EG particle size is 100-200 meshes, and the expansion rate is 250-300 mL/g.
Preferably, the particle size of the APP is 1500-2000 meshes.
Preferably, the mass ratio of EG to APP is 1:0.35-0.45. More preferably, the mass ratio of EG to APP is 1:0.4.
The component B comprises the following components:
preferably, the diisocyanate is diphenylmethane diisocyanate (MDI); the polytetrahydrofuran ether polyol is PTMEG1000.
Preferably, the raw material components and the mass parts thereof are as follows, based on 100 parts of the total mass of the raw materials for preparing the component B:
1000 45 to 50 parts of PTMEG;
50-55 parts of MDI.
Preferably, the molar ratio of the active-H contained in the A component to the-NCO groups contained in the B component is 1.00:0.99-1.01.
The invention discloses a preparation method of a polyurethane vibration damping and sound insulating pad for flame retardation and no combustion droppings/particles, which comprises the following steps: preheating the component A to 30-34 ℃ and preheating the component B to 38-42 ℃, and then pouring the preheated component A and the preheated component B into a die preheated to 60-70 ℃ for curing and forming to obtain the flame-retardant polyurethane vibration-damping sound-insulating pad without combustion droppings/particles.
Preferably, the curing and molding temperature is 60-70 ℃ and the time is 10-15 min.
Advantageous effects
(1) According to the flame-retardant microporous polyurethane vibration-damping sound-insulating pad without the combustion of the droppings/particles, after flame retardation modification by adding APP and EG, the oxygen index can reach more than 26, the flame retardation grade reaches B2, and the droppings/particles cannot be generated during combustion.
(2) EG is added independently, so that although the problem of molten drops can be solved, a large gap exists between the expanded carbon layers, the bonding force between the expanded carbon layers and a matrix is weak, the phenomenon that flame drops with carbon residues (hereinafter referred to as slag dropping phenomenon) easily occurs, and the oxygen index is not obviously improved; the oxygen index can be improved by singly adding APP, but in order to solve the problem of molten drop, a large amount of APP is required to be added, so that the rigidity is increased, the viscosity is increased, and the technological performance is reduced; in the invention, EG and APP are compounded for use, the synergistic effect of the EG and APP can be effectively exerted, the heated and decomposed product of the APP can fill the gaps of the expanded carbon layer, the density of the expanded carbon layer is increased, heat and air can be well isolated, the flame retardant performance is greatly improved, and the total addition amount of the flame retardant is reduced on the premise of equivalent oxygen index.
(3) Further, the EG particle size is too small, the flame retardant effect is poor, the particle size is too large, the dispersibility in a matrix is poor, the closed cell rate of the microporous polyurethane elastomer can be influenced, and the EG particle size is optimally selected to be 100-200 meshes. EG expansion rate is too small, flame retardant effect is poor, expansion rate is too large, binding force with a substrate is weakened, slag dropping phenomenon is easy to occur, and EG optimal expansion rate is 250-300 mL/g. APP particle size is too large, poor dispersibility in a matrix can affect the closed cell rate of the microporous polyurethane elastomer, and the optimal particle size of APP is 1500-2000 meshes. When the APP consumption is relatively small, the heated and decomposed product cannot effectively fill the gaps of the expanded carbon layer, the strength of the carbon layer is low, the bonding force between the carbon layer and the matrix is weak, and the falling phenomenon is easy to occur; when the APP consumption is relatively more, the rigidity can be increased, and when the mass ratio of EG to APP is 1:0.35-0.45, the synergistic effect of EG and APP can be better exerted, the oxygen index is high, the total consumption of the flame retardant which does not produce combustion drips/particles is minimum, the performance such as other mechanics, sound insulation and the like is not influenced, and the use effect of the vibration reduction pad is ensured.
(4) The total consumption of the flame retardant is continuously increased, and the flame retardant performance can be further increased, but the performance such as sound insulation and the like can be influenced, and the normal use of the vibration reduction pad is influenced.
(5) The service life of the vibration-damping sound-insulating pad can be the same as that of a building over 50 years, the standard impact sound level of the polyurethane vibration-damping sound-insulating pad with the thickness of 6mm is only 57dB, and the related requirements of GB/T50118 (bedroom and living room separated floor of common residential building < 75dB, high-requirement residence < 65 dB) are met.
Detailed Description
The present invention will be described in further detail with reference to specific examples. Wherein the process is conventional unless otherwise specified and the starting materials are commercially available from the public sources unless otherwise specified.
In the following examples:
the mildew preventive is polyurethane mildew preventive with the brand name KP-M100 produced by the company Praeparata of Buddha.
The foam homogenizing agent is AK8804 from Jiangsu Midsider company.
Example 1:
(1) 15 parts of PTMEG2000, 25 parts of PTMEG1000, 32 parts of EP330, 8 parts of BDO and 0.4 part of H 2 Uniformly mixing O, 0.8 part of foam stabilizer, 0.4 part of mildew preventive, 0.18 part of BDMAE, 0.020 part of T-12, 13 parts of EG and 5.2 parts of APP to obtain a component A; 50 parts of MDI and 50 parts of PTMEG1000 are mixed and stirred to react for 4 hours at 85 ℃ under the protection of nitrogen, so as to obtain a component B with the-NCO value of 12.57%;
(2) According to the molar ratio of the active-H in the component A to the-NCO group in the component B of 1.00:1.00, uniformly mixing the component A preheated to 32 ℃ and the component B preheated to 40 ℃ by a double-component polyurethane casting machine, casting into a mould preheated to 60-70 ℃ for curing and forming (the polyurethane vibration-damping and sound-insulating pad with different densities can be obtained by controlling the casting amount), and obtaining the flame-retardant polyurethane vibration-damping and sound-insulating pad without burning drips/particles.
Comparative example 1:
(1) 17 parts of PTMEG2000, 25 parts of PTMEG1000, 30 parts of EP330, 8 parts of BDO and 0.4 part of H 2 Uniformly mixing O, 0.8 part of foam homogenizing agent, 0.6 part of mildew preventive, 0.18 part of BDMAE, 0.020 part of T-12, 15 parts of EG and 3 parts of APP to obtain a component A; 50 parts of MDI and 50 parts of PTMEG1000 are mixed and stirred to react for 4 hours at 85 ℃ under the protection of nitrogen, so as to obtain a component B with the-NCO value of 12.57%;
(2) And (3) according to the molar ratio of the active-H in the component A to the-NCO group in the component B of 1.00:1.00, uniformly mixing the component A preheated to 32 ℃ and the component B preheated to 40 ℃ by a double-component polyurethane casting machine, and casting into a mould preheated to 60-70 ℃ for curing and forming to obtain the polyurethane vibration-damping and sound-insulating pad without combustion droppings/particles.
Comparative example 2:
(1) 20 parts of PTMEG2000, 30 parts of PTMEG1000, 32 parts of EP330, 8 parts of BDO and 0.4 part of H 2 Uniformly mixing O, 0.8 part of foam homogenizing agent, 0.6 part of mildew preventive, 0.18 part of BDMAE, 0.020 part of T-12, 5 parts of EG and 3 parts of APP to obtain a component A; 50 parts of MDI and 50 parts of PTMEG1000 are mixed and stirred to react for 4 hours at 85 ℃ under the protection of nitrogen, so as to obtain a component B with the-NCO value of 12.57;
(2) And (3) according to the molar ratio of the active-H in the component A to the-NCO group in the component B of 1.00:1.00, uniformly mixing the component A preheated to 32 ℃ and the component B preheated to 40 ℃ by a double-component polyurethane casting machine, and casting into a mould preheated to 60-70 ℃ for curing and forming to obtain the polyurethane vibration-damping and sound-insulating pad with combustion drips/particles.
Comparative example 3:
(1) 20 parts of PTMEG2000, 35 parts of PTMEG1000, 35 parts of EP330, 8 parts of BDO and 0.4 part of H 2 Uniformly mixing O, 0.8 part of foam homogenizing agent, 0.6 part of mildew preventive, 0.18 part of BDMAE and 0.020 part of T-12 to obtain a component A; 50 parts of MDI and 50 parts of PTMEG1000 are mixed and stirred to react for 4 hours at 85 ℃ under the protection of nitrogen, so as to obtain a component B with the-NCO value of 12.57;
(2) And (3) according to the molar ratio of the active-H in the component A to the-NCO group in the component B of 1.00:1.00, uniformly mixing the component A preheated to 32 ℃ and the component B preheated to 40 ℃ by a double-component polyurethane casting machine, and casting into a mould preheated to 60-70 ℃ for curing and forming to obtain the polyurethane vibration-damping and sound-insulating pad with combustion drips/particles.
Comparative example 4:
(1) 17 parts of PTMEG2000, 25 parts of PTMEG1000, 30.2 parts of EP330, 8 parts of BDO and 0.4 part of H 2 Uniformly mixing O, 0.8 part of foam homogenizing agent, 0.4 part of mildew preventive, 0.18 part of BDMAE, 0.020 part of T-12 and 18 parts of EG to obtain a component A; 50 parts of MDI and 50 parts of PTMEG1000 are mixed and stirred to react for 4 hours at 85 ℃ under the protection of nitrogen, so as to obtain a component B with the-NCO value of 12.57;
(2) And (3) according to the molar ratio of the active-H in the component A to the-NCO group in the component B of 1.00:1.00, uniformly mixing the component A preheated to 32 ℃ and the component B preheated to 40 ℃ by a double-component polyurethane casting machine, and casting into a mould preheated to 60-70 ℃ for curing and forming to obtain the polyurethane vibration-damping and sound-insulating pad with combustion drips/particles.
Comparative example 5:
(1) 20 parts of PTMEG2000, 25 parts of PTMEG1000, 35 parts of EP330, 8 parts of BDO and 0.4 part of H 2 Uniformly mixing O, 0.8 part of foam homogenizing agent, 0.6 part of mildew preventive, 0.18 part of BDMAE, 0.020 part of T-12 and 10 parts of APP to obtain a component A; 50 parts of MDI and 50 parts of PTMEG1000 are mixed and stirred to react for 4 hours at 85 ℃ under the protection of nitrogen, so as to obtain a component B with the-NCO value of 12.57;
(2) And (3) according to the molar ratio of the active-H in the component A to the-NCO group in the component B of 1.00:1.00, uniformly mixing the component A preheated to 32 ℃ and the component B preheated to 40 ℃ by a double-component polyurethane casting machine, and casting into a mould preheated to 60-70 ℃ for curing and forming to obtain the polyurethane vibration-damping and sound-insulating pad with the oxygen index of more than 26 and burning drips/particles.
The polyurethane vibration damping and sound insulating pad prepared in the example and the comparative example are respectively subjected to various performance tests according to corresponding standards; wherein, the oxygen index is reference standard GB/T2406, the combustion drips test reference standard GB/T2408-2008 method B, the tensile strength and elongation at break test reference standard GB/T10654, the compression set test reference standard GB/T10653 (70 ℃,22h,30% compression), the impact sound pressure level improvement test reference GB/T19889.8-2006.
The results of the performance tests of the examples and comparative examples are shown in Table 1.
TABLE 1
Figure BDA0004091748930000091
As shown by the test results in Table 1, the polyurethane vibration-damping and sound-insulating pad prepared in the embodiment 1 has excellent flame retardant property, mechanical property and sound-insulating effect, and can meet the use requirements of the vibration-damping and sound-insulating pad for the building floating floor.
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. The utility model provides a fire-retardant polyurethane damping sound insulation pad of no combustion drippage/particle which characterized in that: the vibration-damping sound-insulating pad is formed by curing the component A and the component B, and has the density of 200kg/m 3 ～260kg/m 3 A microporous polyurethane vibration-damping and sound-insulating pad with an oxygen index of 26 or more, a tensile strength of 1MPa or more and an impact sound pressure level improvement of 30dB or more;
the A component is composed of PTMEG1000, PTMEG2000, EP330, BDO, H 2 O, a foam stabilizer, BDMAE, T12, a mildew inhibitor and a flame retardant are uniformly mixed to prepare the flame retardant; the foam homogenizing agent is a foam homogenizing agent with the brand AK8804 of Jiangsu Maillard company; the flame retardant is EG and APP;
the total mass of the raw materials for preparing the component A is 100 parts, and the raw materials comprise the following components in parts by mass:
Figure FDA0004091748920000011
the component B is a prepolymer with the-NCO value between 12 and 14 formed by stirring and reacting diisocyanate and polytetrahydrofuran ether polyol at the temperature of 80-100 ℃ for 4-6 hours;
the total mass of the raw materials for preparing the component B is 100 parts, and the raw materials comprise the following components in parts by mass:
45-55 parts of diisocyanate;
45-55 parts of polytetrahydrofuran ether polyol;
the molar ratio of the active-H contained in the component A to the-NCO group contained in the component B is 1.00:0.98-1.03.
2. A flame retardant, non-combustible drop/particle polyurethane vibration dampening and sound insulating mat as defined in claim 1, wherein: in the component A, the mildew inhibitor is a polyurethane mildew inhibitor with the brand name of KP-M100 produced by the Utility model company of Buddha or a polyurethane mildew inhibitor with the brand name of M8 produced by the Dongguan Guangsi remote company.
3. A flame retardant, non-combustible drop/particle polyurethane vibration dampening and sound insulating mat as defined in claim 1, wherein: the total mass of the raw materials for preparing the component A is 100 parts, and the raw materials comprise the following components in parts by mass:
Figure FDA0004091748920000021
4. a polyurethane vibration damping and sound insulating mat for fire retardant, non-burning drips/particles as claimed in any one of claims 1 to 3, wherein: in the component A, the granularity of the EG is 100-200 meshes, and the expansion rate is 250-300 mL/g.
5. A polyurethane vibration damping and sound insulating mat for fire retardant, non-burning drips/particles as claimed in any one of claims 1 to 3, wherein: in the component A, the granularity of the APP is 1500-2000 meshes.
6. A polyurethane vibration damping and sound insulating mat for fire retardant, non-burning drips/particles as claimed in any one of claims 1 to 3, wherein: in the component A, the mass ratio of EG to APP is 1:0.35-0.45.
7. A flame retardant, non-combustible drop/particle polyurethane vibration dampening and sound insulating mat as defined in claim 1, wherein: in the component B, diisocyanate is MDI; the polytetrahydrofuran ether polyol is PTMEG1000;
the total mass of the raw materials for preparing the component B is 100 parts, and the raw materials comprise the following components in parts by mass:
1000 45 to 50 parts of PTMEG;
50-55 parts of MDI.
8. A flame retardant, non-combustible drop/particle polyurethane vibration dampening and sound insulating mat as defined in claim 1, wherein: the molar ratio of the active-H contained in the component A to the-NCO group contained in the component B is 1.00:0.99-1.01.
9. A method for preparing the polyurethane vibration damping and sound insulating pad of flame retardant and non-combustion dropper/particle according to any one of claims 1 to 8, which is characterized in that: the method comprises the following steps: preheating the component A to 30-34 ℃ and preheating the component B to 38-42 ℃, and then pouring the preheated component A and the preheated component B into a die preheated to 60-70 ℃ for curing and forming to obtain the flame-retardant polyurethane vibration-damping sound-insulating pad without combustion droppings/particles.
10. The method for preparing the polyurethane vibration damping and sound insulating pad with flame retardance and no combustion droppings/particles as claimed in claim 9, wherein the method comprises the following steps of: the curing and molding temperature is 60-70 ℃ and the curing and molding time is 10-15 min.
CN202310154297.6A 2023-02-23 2023-02-23 Flame-retardant polyurethane vibration-damping sound-insulating pad without combustion droppings/particles and preparation method thereof Pending CN116333252A (en)

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