CN111218106A - Flame-retardant aging-resistant ineffectiveness polyurethane composite wave-absorbing material - Google Patents
Flame-retardant aging-resistant ineffectiveness polyurethane composite wave-absorbing material Download PDFInfo
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Abstract
The invention provides a flame-retardant aging-resistant invalid polyurethane composite wave-absorbing material, which is prepared from the following components in parts by mass through a polymerization reaction: 100 parts of polyether polyol, 30-60 parts of toluene diisocyanate, 0.05-0.4 part of nano carbon sol, 0.2-0.5 part of nano white carbon black, 10-20 parts of deionized water, 5-20 parts of dimethyl methyl phosphate, 2-8 parts of graphene oxide, 10-20 parts of ferrite, 2-10 parts of zirconium oxide, 2-8 parts of zinc borate, 0.02-0.4 part of stannous octoate, 0.03-0.6 part of triethylene diamine, 0.2-3 parts of organic silicon surfactant and 2-8 parts of sodium bicarbonate. The flame-retardant aging-resistant ineffective polyurethane composite wave-absorbing material provided by the invention has the characteristics of low smoke, low toxicity, flame retardancy, wide distribution of absorption frequency of absorption waves and the like. The invention also provides a preparation method of the flame-retardant aging-resistant ineffective polyurethane composite wave-absorbing material.
Description
Technical Field
The invention belongs to the technical field of functional materials, and particularly relates to a flame-retardant, aging-resistant and ineffective polyurethane composite wave-absorbing material and a preparation method thereof.
Background
The wave-absorbing material is a material which can absorb most of electromagnetic waves projected on the surface of the wave-absorbing material and convert the electromagnetic waves into other forms of energy without reflection. With the development of modern science and technology, the influence of electromagnetic wave radiation on the environment is increasing day by day. At an airport, airplane flights are mistakenly clicked because the airplane cannot take off due to electromagnetic wave interference; in hospitals, mobile phones often interfere with the normal operation of various electronic medical instruments. In addition, the electromagnetic radiation causes direct and indirect damage to human bodies through thermal effect, non-thermal effect and cumulative effect. Therefore, the wave-absorbing material, which is a material capable of resisting and weakening electromagnetic wave radiation, is a major subject of material science to be found for treating electromagnetic pollution.
The polyurethane foam has the characteristics of porosity, small relative density, temperature resistance, ageing resistance, organic solvent corrosion resistance, easiness in molding and processing and the like, and is widely applied to wave-absorbing materials. At present, the wave absorbing agent is mainly added into a hard polyurethane foam system and then injected into a mould for reaction and foaming, or the soft polyurethane foam is cut into a preset shape and dipped in the wave absorbing agent solution to prepare the polyurethane foam composite wave absorbing material, and the materials have the defects of complex manufacturing process, single function, easy shedding of the wave absorbing auxiliary agent, flammability and the like.
Chinese patent CN200910029840.X 'foaming type high resilience polyurethane wave-absorbing material and preparation method thereof' discloses a polyurethane wave-absorbing material prepared by using raw materials such as absorption aid, fire retardant and the like. But the material has the defects of large size, complex manufacturing process and the like. How to improve the wave-absorbing performance and improve the flame retardant performance, the manufacturing process is simple, and the pollution reduction is a key problem in the development of the wave-absorbing material.
Disclosure of Invention
In view of the above, the present invention provides a polyurethane composite wave-absorbing material with flame retardation, aging resistance and failure resistance and a preparation method thereof, so as to solve the above problems.
The invention provides a flame-retardant aging-resistant invalid polyurethane composite wave-absorbing material which is prepared by carrying out polymerization reaction on the following components in parts by mass: 100 parts of polyether polyol, 30-60 parts of toluene diisocyanate, 0.05-0.4 part of nano carbon sol, 0.2-0.5 part of nano white carbon black, 10-20 parts of deionized water, 5-20 parts of dimethyl methyl phosphate, 2-8 parts of graphene oxide, 10-20 parts of ferrite, 1-5 parts of zirconium oxide, 2-8 parts of zinc borate, 0.02-0.4 part of stannous octoate, 0.03-0.6 part of triethylene diamine, 0.2-3 parts of organic silicon surfactant and 2-8 parts of sodium bicarbonate.
Wherein the hydroxyl value of the polyether polyol is 30-60 mgKOH/g. The isocyanate index of the toluene diisocyanate is 0.60-1.15.
Based on the above, the flame-retardant, aging-resistant and failure-resistant polyurethane composite wave-absorbing material is obtained by carrying out polymerization reaction on the following components in parts by mass: 100 parts of polyether polyol, 40-50 parts of toluene diisocyanate, 0.15-0.25 part of nano carbon sol, 0.3-0.4 part of nano white carbon black, 13-17 parts of deionized water, 10-15 parts of dimethyl methyl phosphate, 4-6 parts of graphene oxide, 13-17 parts of ferrite, 2-4 parts of zirconium oxide, 4-6 parts of zinc borate, 0.08-0.3 part of stannous octoate, 0.12-0.45 part of triethylene diamine, 1-2 parts of organic silicon surfactant and 4-6 parts of sodium bicarbonate.
The invention also provides a preparation method of the flame-retardant aging-resistant ineffective polyurethane composite wave-absorbing material, which comprises the following steps:
mixing raw materials: uniformly stirring polyether polyol, dimethyl methyl phosphate, nano carbon sol, nano white carbon black, ferrite, zirconium oxide, zinc borate, stannous octoate, triethylene diamine and deionized water with an organic silicon surfactant at room temperature, and then performing ultrasonic dispersion treatment to obtain a primary mixture;
reaction foaming: adding toluene diisocyanate into the primary mixture, carrying out ultrasonic stirring for 5-10 minutes, adding the carboxyl carbon nano tube and sodium bicarbonate, and then quickly pouring into a mould for foaming at room temperature for 30-90 minutes to obtain wave-absorbing material gel;
and (3) freeze drying: and freeze-drying the wave-absorbing material gel to obtain the flame-retardant aging-resistant ineffective polyurethane composite wave-absorbing material.
Based on the above, the step of reactive foaming comprises: under the action of ultrasonic stirring, firstly, adding toluene diisocyanate into the primary mixture for 5-10 minutes under the condition of heating and stirring, and then adding graphene oxide and sodium bicarbonate; and then quickly pouring the mixture into a mould to foam for 30-90 minutes at room temperature to obtain the wave-absorbing material gel.
In view of the above, in the step of mixing the raw materials, the ultrasonic dispersion treatment is performed in a water bath.
Based on the above, the step of freeze-drying comprises: freezing the wave-absorbing material gel for 10-70 hours at the freezing temperature of 5-50 ℃ below the freezing point temperature of the mixed solution; then further drying the frozen mixed solution at a low temperature of-10 to-100 ℃ for 24 to 96 hours under low pressure, wherein the pressure is 0.1 to 1 kPa; and finally, curing the mixed solution dried at low temperature and low pressure for 4-12 hours at the temperature of 60-100 ℃.
Compared with the prior art, the flame-retardant aging-resistant ineffectiveness polyurethane composite wave-absorbing material provided by the invention has the advantages that dimethyl methyl phosphate and zinc borate are combined to play a flame-retardant synergistic effect, so that the flame-retardant aging-resistant ineffectiveness polyurethane composite wave-absorbing material has the characteristics of low smoke, low toxicity, difficult combustion and the like, and the flame-retardant property of the material reaches HF-1 level; sodium bicarbonate reacts with graphene oxide to generate bubbles, and meanwhile, deionized water in the wave-absorbing material gel is removed by matching with a freeze drying technology, so that the prepared flame-retardant aging-resistant invalid polyurethane composite wave-absorbing material has a porous structure and a large specific surface area. In addition, the nano carbon sol and the carbon nano tubes have better conductivity, are uniformly dispersed in the polyurethane matrix and form a good conductive network, so that the prepared polyurethane composite material has improved and stable electrical property and low percolation value. The flame-retardant aging-resistant ineffective polyurethane composite wave-absorbing material is prepared by combining a chemical foaming technology and a directional freeze-drying technology, and has the advantages of simple preparation process, low investment, high production efficiency and environmental friendliness.
Detailed Description
The technical solution of the present invention is further described in detail by the following embodiments.
Example 1
The embodiment of the invention provides a flame-retardant aging-resistant invalid polyurethane composite wave-absorbing material which is prepared by carrying out polymerization reaction on the following components in parts by mass: 100 parts of polyether polyol, 30 parts of toluene diisocyanate, 0.05 part of nano carbon sol, 0.2 part of nano white carbon black, 10 parts of deionized water, 5 parts of methyl dimethyl phosphate, 2 parts of graphene oxide, 10 parts of ferrite, 1 part of zirconium oxide, 2 parts of zinc borate, 0.02 part of stannous octoate, 0.03 part of triethylene diamine, 0.2 part of an organic silicon surfactant and 2 parts of sodium bicarbonate.
The embodiment of the invention also provides a preparation method of the flame-retardant aging-resistant ineffective polyurethane composite wave-absorbing material, which comprises the following steps:
mixing raw materials: according to the mass parts, polyether polyol, dimethyl methyl phosphate, nano carbon sol, nano white carbon black, ferrite, zirconium oxide, zinc borate, stannous octoate, triethylene diamine, deionized water and an organic silicon surfactant are uniformly stirred at room temperature, and then subjected to ultrasonic dispersion treatment to obtain a primary mixture;
reaction foaming: under the action of ultrasonic stirring, firstly, adding toluene diisocyanate into the primary mixture for 5-10 minutes under the condition of heating and stirring, and then adding graphene oxide and sodium bicarbonate; then quickly pouring the mixture into a mould to foam for 30 minutes at room temperature to obtain wave-absorbing material gel;
and (3) freeze drying: freezing the wave-absorbing material gel for 10 hours at the freezing temperature of 5 ℃ below the freezing point temperature of the mixed solution; then further drying the frozen mixed solution at the low temperature of-10 ℃ for 24 hours under low pressure, wherein the pressure is 0.1 kPa; and finally, curing the mixed solution dried at low temperature and low pressure at 60 ℃ for 12 hours to obtain the flame-retardant, aging-resistant and invalid polyurethane composite wave-absorbing material.
Performance testing
The method for detecting the wave absorbing performance comprises the following steps: the flame-retardant aging-resistant invalid polyurethane composite wave-absorbing material is cut into a rectangular sheet sample with the area of 3cm multiplied by 3cm and the thickness of 4 mm, a layer of aluminum foil with a very smooth surface is attached to the surface of one side of the sample, and a microwave reflectivity curve of the sample in a frequency band of 4-20 GHz is tested by a digital vector network analyzer (8722ET type). And detecting that the wave absorbing performance is less than-39 db in the frequency range of 4 GHz-20 GHz.
The flame retardant property detection method comprises the following steps: the above were tested according to GB/T8332-2008 foam Combustion Performance test method horizontal Combustion method. Through detection, the flame retardant property of the flame-retardant aging-resistant invalid polyurethane composite wave-absorbing material reaches HF-1 level.
Example 2
The embodiment of the invention provides a flame-retardant aging-resistant ineffective polyurethane composite wave-absorbing material which is prepared by carrying out polymerization reaction on the following components in parts by mass: 100 parts of polyether polyol, 40 parts of toluene diisocyanate, 0.15 part of nano carbon sol, 0.3 part of nano white carbon black, 13 parts of deionized water, 10 parts of dimethyl methyl phosphate, 4 parts of graphene oxide, 13 parts of ferrite, 2 parts of zirconium oxide, 4 parts of zinc borate, 0.08 part of stannous octoate, 0.12 part of triethylene diamine, 1 part of organic silicon surfactant and 4 parts of sodium bicarbonate.
The embodiment of the invention also provides a preparation method of the flame-retardant aging-resistant ineffective polyurethane composite wave-absorbing material, which is basically the same as the preparation method provided by the embodiment 1, and the difference is that:
reaction foaming: the room temperature foaming time in this step was 60 minutes;
and (3) freeze drying: the steps comprise freezing the wave-absorbing material gel for 30 hours at the freezing temperature of 15 ℃ below the freezing point temperature of the mixed solution; then further drying the frozen mixed solution at the low temperature of-30 ℃ for 48 hours under low pressure, wherein the pressure is 0.3 kPa; and finally, curing the mixed solution dried at low temperature and low pressure at 70 ℃ for 10 hours to obtain the flame-retardant, aging-resistant and invalid polyurethane composite wave-absorbing material.
Performance testing
The same method as that provided in the embodiment 1 is adopted to detect the wave absorption performance and the flame retardant performance of the flame-retardant aging-resistant ineffective polyurethane composite wave-absorbing material provided in the embodiment, and the detection result is as follows: the wave-absorbing performance is less than-43 db in the frequency range of 4 GHz-20 GHz, and the flame-retardant performance of the flame-retardant aging-resistant invalid polyurethane composite wave-absorbing material reaches HF-1 level.
Example 3
The embodiment of the invention provides a flame-retardant aging-resistant invalid polyurethane composite wave-absorbing material which is prepared by carrying out polymerization reaction on the following components in parts by mass: 100 parts of polyether polyol, 45 parts of toluene diisocyanate, 0.2 part of nano carbon sol, 0.35 part of nano white carbon black, 15 parts of deionized water, 13 parts of methyl dimethyl phosphate, 5 parts of graphene oxide, 15 parts of ferrite, 3 parts of zirconium oxide, 5 parts of zinc borate, 0.2 part of stannous octoate, 0.3 part of triethylene diamine, 1.6 parts of an organic silicon surfactant and 5 parts of sodium bicarbonate.
The embodiment of the invention also provides a preparation method of the flame-retardant aging-resistant ineffective polyurethane composite wave-absorbing material, which is basically the same as the preparation method provided by the embodiment 1, and the difference is that:
reaction foaming: the room temperature foaming time in this step was 60 minutes;
and (3) freeze drying: the steps comprise freezing the wave-absorbing material gel for 40 hours at the freezing temperature of 30 ℃ below the freezing point of the mixed solution; then further drying the frozen mixed solution at the low temperature of 50 ℃ below zero for 60 hours under low pressure, wherein the pressure is 0.6 kPa; and finally, curing the mixed solution dried at low temperature and low pressure at 80 ℃ for 8 hours to obtain the flame-retardant, aging-resistant and invalid polyurethane composite wave-absorbing material.
Performance testing
The same method as that provided in the embodiment 1 is adopted to detect the wave absorption performance and the flame retardant performance of the flame-retardant aging-resistant ineffective polyurethane composite wave-absorbing material provided in the embodiment, and the detection result is as follows: the wave-absorbing performance is less than-47 db in the frequency range of 4 GHz-20 GHz, and the flame retardant performance of the flame-retardant aging-resistant invalid polyurethane composite wave-absorbing material reaches HF-1 level.
Example 4
The embodiment of the invention provides a flame-retardant aging-resistant ineffective polyurethane composite wave-absorbing material which is prepared by carrying out polymerization reaction on the following components in parts by mass: 100 parts of polyether polyol, 50 parts of toluene diisocyanate, 0.25 part of nano carbon sol, 0.4 part of nano white carbon black, 17 parts of deionized water, 15 parts of dimethyl methyl phosphate, 6 parts of graphene oxide, 17 parts of ferrite, 4 parts of zirconium oxide, 6 parts of zinc borate, 0.3 part of stannous octoate, 0.45 part of triethylene diamine, 2 parts of an organic silicon surfactant and 6 parts of sodium bicarbonate.
The embodiment of the invention also provides a preparation method of the flame-retardant aging-resistant ineffective polyurethane composite wave-absorbing material, which is basically the same as the preparation method provided by the embodiment 1, and the difference is that:
reaction foaming: the room temperature foaming time in this step was 90 minutes;
and (3) freeze drying: the steps comprise freezing the wave-absorbing material gel for 60 hours at the freezing temperature of 40 ℃ below the freezing point temperature of the mixed solution; then further drying the frozen mixed solution at the low temperature of minus 80 ℃ for 72 hours under low pressure, wherein the pressure is 0.8 kPa; and finally, curing the mixed solution dried at low temperature and low pressure at 90 ℃ for 6 hours to obtain the flame-retardant, aging-resistant and invalid polyurethane composite wave-absorbing material.
Performance testing
The same method as that provided in the embodiment 1 is adopted to detect the wave absorption performance and the flame retardant performance of the flame-retardant aging-resistant ineffective polyurethane composite wave-absorbing material provided in the embodiment, and the detection result is as follows: the wave-absorbing performance is less than-46 db in the frequency range of 4 GHz-20 GHz, and the flame-retardant performance of the flame-retardant aging-resistant invalid polyurethane composite wave-absorbing material reaches HF-1 level.
Example 5
The embodiment of the invention provides a flame-retardant aging-resistant invalid polyurethane composite wave-absorbing material which is prepared by carrying out polymerization reaction on the following components in parts by mass: 100 parts of polyether polyol, 60 parts of toluene diisocyanate, 0.4 part of nano carbon sol, 0.5 part of nano white carbon black, 20 parts of deionized water, 20 parts of dimethyl methyl phosphate, 8 parts of graphene oxide, 20 parts of ferrite, 5 parts of zirconium oxide, 8 parts of zinc borate, 0.4 part of stannous octoate, 0.6 part of triethylene diamine, 3 parts of an organic silicon surfactant and 8 parts of sodium bicarbonate.
The embodiment of the invention also provides a preparation method of the flame-retardant aging-resistant ineffective polyurethane composite wave-absorbing material, which is basically the same as the preparation method provided by the embodiment 1, and the difference is that:
reaction foaming: the room temperature foaming time in this step was 90 minutes;
and (3) freeze drying: the steps comprise freezing the wave-absorbing material gel for 70 hours at the freezing temperature of 50 ℃ below the freezing point temperature of the mixed solution; then further drying the frozen mixed solution at the low temperature of-100 ℃ for 96 hours under low pressure, wherein the pressure is 1 kPa; and finally, curing the mixed solution dried at low temperature and low pressure for 4 hours at 100 ℃ to obtain the flame-retardant aging-resistant invalid polyurethane composite wave-absorbing material.
Performance testing
The same method as that provided in the embodiment 1 is adopted to detect the wave absorption performance and the flame retardant performance of the flame-retardant aging-resistant ineffective polyurethane composite wave-absorbing material provided in the embodiment, and the detection result is as follows: the wave-absorbing performance is less than-41 db in the frequency range of 4 GHz-20 GHz, and the flame retardant performance of the flame-retardant aging-resistant invalid polyurethane composite wave-absorbing material reaches HF-1 level.
Claims (2)
1. The flame-retardant aging-resistant ineffective polyurethane composite wave-absorbing material is characterized by being prepared from the following components in parts by mass through polymerization reaction: 100 parts of polyether polyol, 30-60 parts of toluene diisocyanate, 0.05-0.4 part of nano carbon sol, 0.2-0.5 part of nano white carbon black, 10-20 parts of deionized water, 5-20 parts of dimethyl methyl phosphate, 2-8 parts of graphene oxide, 10-20 parts of ferrite, 1-5 parts of zirconium oxide, 2-8 parts of zinc borate, 0.02-0.4 part of stannous octoate, 0.03-0.6 part of triethylene diamine, 0.2-3 parts of an organic silicon surfactant and 2-8 parts of sodium bicarbonate, wherein the hydroxyl value of the polyether polyol is 30-60 mgKOH/g, and the isocyanate index of the toluene diisocyanate is 0.60-1.15.
2. The flame-retardant aging-resistant failure-resistant polyurethane composite wave-absorbing material according to claim 1, which is obtained by polymerization of the following components in parts by mass: 100 parts of polyether polyol, 40-50 parts of toluene diisocyanate, 0.15-0.25 part of nano carbon sol, 0.3-0.4 part of nano white carbon black, 13-17 parts of deionized water, 10-15 parts of dimethyl methyl phosphate, 4-6 parts of graphene oxide, 13-17 parts of ferrite, 2-4 parts of zirconium oxide, 4-6 parts of zinc borate, 0.08-0.3 part of stannous octoate, 0.12-0.45 part of triethylene diamine, 1-2 parts of organic silicon surfactant and 4-6 parts of sodium bicarbonate.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111621137A (en) * | 2020-06-22 | 2020-09-04 | 福州大学 | Low-smoke low-toxicity flame-retardant thermoplastic polyurethane composite material and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111621137A (en) * | 2020-06-22 | 2020-09-04 | 福州大学 | Low-smoke low-toxicity flame-retardant thermoplastic polyurethane composite material and preparation method thereof |
| CN111621137B (en) * | 2020-06-22 | 2021-12-21 | 福州大学 | Low-smoke low-toxicity flame-retardant thermoplastic polyurethane composite material and preparation method thereof |
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