CN117624534B - Sound-insulation noise-reduction modified plastic and preparation method thereof - Google Patents
Sound-insulation noise-reduction modified plastic and preparation method thereof Download PDFInfo
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- CN117624534B CN117624534B CN202410090371.7A CN202410090371A CN117624534B CN 117624534 B CN117624534 B CN 117624534B CN 202410090371 A CN202410090371 A CN 202410090371A CN 117624534 B CN117624534 B CN 117624534B
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- 238000002156 mixing Methods 0.000 claims abstract description 75
- 239000011148 porous material Substances 0.000 claims abstract description 67
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- 238000001035 drying Methods 0.000 claims description 47
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- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 30
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 30
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 27
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 27
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 21
- 238000011068 loading method Methods 0.000 claims description 21
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- 229920001296 polysiloxane Polymers 0.000 claims description 14
- 229920002545 silicone oil Polymers 0.000 claims description 14
- MPKQTNAUFAZSIJ-UHFFFAOYSA-N thiophene-3,4-diol Chemical compound OC1=CSC=C1O MPKQTNAUFAZSIJ-UHFFFAOYSA-N 0.000 claims description 14
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 10
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 10
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 10
- OAKJQQAXSVQMHS-UHFFFAOYSA-N hydrazine Substances NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 10
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 10
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- 230000000694 effects Effects 0.000 abstract description 15
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 8
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- 239000011737 fluorine Substances 0.000 description 6
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- FCCRGBVYSYHQRQ-UHFFFAOYSA-N [ethenyl(dimethyl)silyl]oxy-dimethylsilicon Chemical compound C[Si](C)O[Si](C)(C)C=C FCCRGBVYSYHQRQ-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses a sound-insulating and noise-reducing modified plastic and a preparation method thereof, and relates to the technical field of high polymer materials. In the preparation of the sound-insulating and noise-reducing modified plastic, silica sol is prepared into porous silica microspheres; carrying 4,4' -oxo-bis-benzenesulfonyl hydrazide on the porous silica microspheres after silane coupling modification to prepare loaded modified porous silica microspheres; reacting diphenoxyphosphoryl chloride with 1-aminopyrrole to obtain N-diphenoxyphosphoryl aminopyrrole; mixing the polyol mixed solution, the pore opening agent, the foaming agent, the loaded modified porous silica microspheres and the isocyanate prepolymer, foaming and curing to form a polyurethane porous material; and then oxidizing and polymerizing pyrrole and N-diphenoxyphosphoryl amino pyrrole on the surfaces of pore channels and air cavities of the polyurethane porous material to prepare the sound-insulating and noise-reducing modified plastic. The sound-insulating and noise-reducing modified plastic prepared by the invention has good antistatic performance, flame retardant property and sound-insulating and noise-reducing effects.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a sound-insulation noise-reduction modified plastic and a preparation method thereof.
Background
Noise pollution is a kind of global non-negligible hazard which has serious influence on the production and life of people, and the pollution of the noise pollution and water and the pollution of the atmosphere are called as three important worldwide pollution. Since such potentially harmful noise is a serious source of environmental pollution, various studies on acoustic performance have been conducted. Noise control industry has been eager for porous media sound absorption research including automotive silencers, air conditioning accessories, overhead roads, and the like. Nowadays, sound absorbing materials are being studied more and more deeply, and the application range of the sound absorbing materials is also more and more wide, and the sound absorbing materials comprise noise in various aspects such as highway tunnels, movie theatres, buildings and the like.
The porous material is very popular in noise control, and wood fiber board, microperforated panel and the like have good noise reduction effect, but the low rigidity and strength affect the application field: the porous metal sound absorbing material has high strength and rigidity and good corrosion resistance, but has wide selectivity in sound absorption and relatively high cost in preparation; cellular foam is therefore a more suitable choice, with polyurethane foam being the most widespread.
Polyurethane foam plastic has the advantages of light weight, high specific strength, shock absorption, sound absorption and the like, is widely applied to various fields of construction, traffic, life and the like, but has more combustible carbon-hydrogen molecules in a main chain, low density and larger specific surface area, so that the polyurethane foam plastic is extremely easy to burn in air, generates a plurality of smoke and toxic gas in a burning reaction, and brings great harm to lives and property of people. Therefore, polyurethane foam with good flame retardant effect is studied, so that the polyurethane foam has good sound absorption and compression performance and excellent flame retardant performance, and is better applied to various fields in people's life.
Disclosure of Invention
The invention aims to provide sound-insulating and noise-reducing modified plastic and a preparation method thereof, which are used for solving the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
The sound-insulating and noise-reducing modified plastic is prepared by mixing polyol mixed liquid, a pore opening agent, a foaming agent, loaded modified porous silica microspheres and isocyanate prepolymer, foaming and curing to obtain a polyurethane porous material; and then oxidizing and polymerizing pyrrole and N-diphenoxyphosphoryl amino pyrrole on the surfaces of pore channels and air cavities of the polyurethane porous material to prepare the sound-insulating and noise-reducing modified plastic. Preferably, the modified polypropylene is prepared by grafting vinyl tetramethyl disiloxane on polypropylene.
The polyol mixture is prepared by mixing alpha, omega-hydroxypropyl polysiloxane silicone oil MY 1203M, 3, 4-dihydroxythiophene and triethanolamine as optimization.
As optimization, the modified porous silica microsphere after loading is prepared by modifying the porous silica microsphere with a silane coupling agent KH-550 and loading 4,4' -oxo-bis-benzenesulfonyl hydrazide.
Preferably, the N-diphenoxyphosphoryl aminopyrrole is prepared by reacting diphenoxyphosphoryl chloride and 1-aminopyrrole.
A preparation method of sound-insulating and noise-reducing modified plastic comprises the following preparation steps:
(1) Uniformly mixing silica sol, urea and pure water according to a mass ratio of 1:1:140-160, regulating the PH to 1.2-1.3 by using hydrochloric acid with a mass fraction of 10%, adding sodium dodecyl benzene sulfonate with a mass of 0.2-0.3 times that of the silica sol, stirring for 10-12 min at 50-60 ℃ and 200-300 r/min, adding formaldehyde with a urea molar mass of 0.7-0.8 times, continuing stirring for 4-6 h, centrifugally separating, washing for 3-5 times by using pure water, drying for 10-12 h at 60-70 ℃, placing in a muffle furnace for programmed temperature calcination, and naturally cooling to room temperature to obtain porous silica microspheres;
(2) Uniformly mixing a silane coupling agent, pure water and absolute ethyl alcohol according to a mass ratio of 1:2-3:8-10, stirring at 20-30 ℃ for 20-25 min at 600-800 r/min, adding porous silica microspheres with the mass of 0.8-1 times that of a silane coupling agent KH-550, stirring at 20-30 ℃ for 1-2 h at 200-300 r/min, centrifugally separating to obtain solid, washing with absolute ethyl alcohol for 3-5 times, and drying at 60-70 ℃ for 6-8 h to obtain modified porous silica microspheres; uniformly mixing 4,4' -oxo-bis-benzenesulfonyl hydrazine and diethyl ether according to the mass ratio of 1:10-12 to prepare a loading solution, immersing the modified porous silica microspheres in the loading solution, standing for 3-5 min at 10-15 ℃, taking out and drying for 4-6 h at 30-40 ℃, and repeating the immersed drying process for 3-5 times to obtain the loaded modified porous silica microspheres;
(3) Weighing 50-60 parts of polyol mixed solution, 1 part of pore opening agent, 4-6 parts of foaming agent and 15-20 parts of loaded modified porous silica microspheres according to the mass parts, and weighing isocyanate prepolymer according to the molar weight of hydroxyl in the polyol mixed solution and the molar weight of isocyanate groups in the isocyanate prepolymer of 1:1.1-1.2; adding the polyol mixed solution and the pore opening agent into N, N-dimethylformamide which is 2-3 times of the mass of the polyol mixed solution in a nitrogen atmosphere, uniformly mixing, adding the loaded modified porous silica microspheres, stirring for 3-5 min at 20-30 ℃ at 200-300 r/min, adding the isocyanate prepolymer, stirring for reacting for 20-30 min at 50-60 ℃ at 200-300 r/min, heating to 70-80 ℃ for continuously stirring for reacting for 10-15 min, stopping stirring and preserving heat for 10-12 h, taking out and washing with pure water for 3-5 times, and standing for 6-8 h at 20-30 ℃ at 1-2 kPa to obtain the polyurethane porous material;
(4) Uniformly mixing pyrrole, N-diphenoxyphosphoryl aminopyrrole and absolute ethyl alcohol according to the mass ratio of 1:0.2-0.3:10-15 to prepare pyrrole solution; dissolving ferric chloride in 6mol/L hydrochloric acid aqueous solution at 20 ℃ until saturation is reached, so as to obtain saturated ferric chloride solution; at room temperature, immersing the polyurethane porous material in pyrrole solution for 80-100 s, taking out, standing for 6-8 h at 10-20 ℃ under 1-2 kPa, immersing in saturated ferric chloride solution for 80-100 s until no liquid drips in 20s, standing for 6-8 h at 0-4 ℃, placing in absolute ethyl alcohol for washing for 3-5 min, taking out, and drying for 6-8 h at 30-40 ℃ under 1-2 kPa to obtain the sound-insulation and noise-reduction modified plastic.
As optimization, the preparation method of the silica sol in the step (1) comprises the following steps: uniformly mixing tetraethoxysilane, ammonia water with the mass fraction of 25%, pure water and absolute ethyl alcohol according to the volume ratio of 1:1:1.9-2.1:18-22, stirring for 3-4 hours at the temperature of 40-50 ℃ at the speed of 200-300 r/min, centrifugally separating to obtain solid, and standing for 3-4 hours at the temperature of 20-30 ℃ at the speed of 1-2 kPa.
As optimization, the temperature programming calcination method in the step (1) comprises the following steps: sequentially heating from room temperature to 200 ℃ at a heating rate of 7 ℃/min and preserving heat for 2 hours, heating to 270 ℃ at a heating rate of 1 ℃/min and preserving heat for 2 hours, heating to 350 ℃ at a heating rate of 2 ℃/min and preserving heat for 2 hours, and heating to 450 ℃ at a heating rate of 5 ℃/min and preserving heat for 2 hours.
As optimization, the polyol mixed solution in the step (3) is prepared by uniformly mixing alpha, omega-hydroxypropyl polysiloxane silicone oil MY 1203M, 3, 4-dihydroxythiophene and triethanolamine according to a mass ratio of 8-10:1:1.
As optimization, the model of the pore opening agent in the step (3) is G501; the model of the foaming agent is 141B; the type of the isocyanate prepolymer is HDI-N3390.
As optimization, the preparation method of the N-diphenoxyphosphoryl aminopyrrole in the step (4) comprises the following steps: adding diphenoxyphosphoryl chloride and 1-aminopyrrole into N, N-dimethylformamide with the mass of 6-8 times of diphenoxyphosphoryl chloride according to the molar ratio of 1:1, adding triethylamine with the mass of 0.8-1.2 times of diphenoxyphosphoryl chloride, stirring and reacting for 2-3 h at the temperature of 0-5 ℃ and the speed of 200-300 r/min in a nitrogen atmosphere, and standing for 6-8 h at the temperature of 20-30 ℃ and the speed of 1-2 kPa.
Compared with the prior art, the invention has the following beneficial effects:
When the modified plastic with sound insulation and noise reduction is prepared, diphenoxyphosphoryl chloride and 1-aminopyrrole are reacted to prepare N-diphenoxyphosphoryl aminopyrrole; mixing the polyol mixed solution, the pore opening agent, the foaming agent, the loaded modified porous silica microspheres and the isocyanate prepolymer, foaming and curing to form a polyurethane porous material; and then oxidizing and polymerizing pyrrole and N-diphenoxyphosphoryl amino pyrrole on the surfaces of pore channels and air cavities of the polyurethane porous material to prepare the sound-insulating and noise-reducing modified plastic.
Firstly, preparing silica sol into porous silica microspheres; the porous silica microspheres are modified by a silane coupling agent KH-550 and then loaded with 4,4' -oxo-bis-benzenesulfonyl hydrazine to prepare loaded modified porous silica microspheres, the porous structure has good sound absorption effect, the porous silica microspheres are modified, the dispersibility of the porous silica microspheres is improved, the sound insulation and noise reduction performance and the flame retardance are improved, and the surface is provided with amino groups, so that the porous silica microspheres have good combination effect with a main body; the modified porous silica microspheres are loaded, and the loaded 4,4' -oxo-bis-benzenesulfonyl hydrazide has the foaming effect, and directly starts from the inside of the modified porous silica microspheres, so that the interface bonding state of the modified porous silica microspheres and the polymer is improved, the pore diameter is kept communicated, the better sound absorption effect is achieved, and the sound insulation and noise reduction performance is improved.
And secondly, mixing alpha, omega-hydroxypropyl polysiloxane silicone oil MY 1203M, 3, 4-dihydroxythiophene and triethanolamine to prepare a polyol mixed solution, wherein the alpha, omega-hydroxypropyl polysiloxane silicone oil can be used for preparing a polysiloxane chain segment in a polyurethane porous material, has a good flame retardant effect, and the 3, 4-dihydroxythiophene can be used for participating in the polymerization of pyrrole in the preparation process of the polyurethane porous material, so that polypyrrole is combined on the surfaces of pores and air cavities, is not easy to fall off and rolls to cause pore canal blockage, and therefore, the sound insulation and noise reduction performance is improved.
Finally, pyrrole and N-diphenoxyphosphoryl amino pyrrole are oxidized and polymerized on the pore canal and the air cavity surface of the polyurethane porous material, the N-diphenoxyphosphoryl amino pyrrole participates in the polymerization of pyrrole, and the formed polypyrrole contains a large amount of diphenoxyphosphoryl amino structures and has good char-forming protection effect on the main body of the polyurethane porous material, so that the flame retardance is improved, the polypyrrole has good electric conductivity, the sound-insulation noise-reduction modified plastic is not easy to generate static electricity, the reduction of the sound-insulation noise-reduction performance of blocking pores by static electricity attraction dust can be avoided, and the potential safety hazard of fire disaster caused by static electricity can also be avoided.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The method provided by the present invention is described in detail by the following examples for more clarity of illustration.
Example 1
The preparation method of the sound-insulating and noise-reducing modified plastic mainly comprises the following preparation steps:
(1) Uniformly mixing tetraethoxysilane, ammonia water with the mass fraction of 25%, pure water and absolute ethyl alcohol according to the volume ratio of 1:1:1.9:18, stirring for 4 hours at 40 ℃ and 200r/min, centrifugally separating to obtain solid, and standing for 4 hours at 20 ℃ and 1kPa to obtain silica sol; uniformly mixing silica sol, urea and pure water according to a mass ratio of 1:1:140, regulating the pH to 1.2 by using hydrochloric acid with a mass fraction of 10%, adding sodium dodecyl benzene sulfonate with a mass of 0.2 times that of the silica sol, stirring for 12min at 50 ℃ and 200r/min, adding formaldehyde with a molar quantity of 0.7 times that of the urea, continuously stirring for 6h, centrifugally separating, washing 3 times by using pure water, drying for 12h at 60 ℃, placing in a muffle furnace, sequentially heating from room temperature to 200 ℃ at a heating rate of 7 ℃/min and preserving heat for 2h, heating to 270 ℃ at a heating rate of 1 ℃/min and preserving heat for 2h, heating to 350 ℃ at a heating rate of 2 ℃/min and preserving heat for 2h, heating to 450 ℃ at a heating rate of 5 ℃/min and preserving heat for 2h, and naturally cooling to room temperature to obtain porous silica microspheres;
(2) Uniformly mixing a silane coupling agent KH-550, pure water and absolute ethyl alcohol according to a mass ratio of 1:2:8, stirring at 20 ℃ for 25min at 600r/min, adding porous silica microspheres with the mass 0.8 times that of the silane coupling agent KH-550, stirring at 20 ℃ for 2h at 200r/min, centrifugally separating to obtain a solid, washing with absolute ethyl alcohol for 3 times, and drying at 60 ℃ for 8h to obtain modified porous silica microspheres; uniformly mixing 4,4' -oxo-bis-benzenesulfonyl hydrazine and diethyl ether according to a mass ratio of 1:10 to prepare a loading solution, immersing the modified porous silica microspheres in the loading solution, standing at 10 ℃ for 5min, taking out and drying at 30 ℃ for 6h, and repeating the immersing and drying process for 3 times to obtain the loaded modified porous silica microspheres;
(3) Uniformly mixing alpha, omega-hydroxypropyl polysiloxane silicone oil MY 1203M, 3, 4-dihydroxythiophene and triethanolamine according to a mass ratio of 8:1:1 to obtain a polyol mixed solution; weighing 50 parts of polyol mixed solution, 1 part of G501 pore-forming agent, 4 parts of 141B foaming agent and 15 parts of loaded modified porous silica microspheres according to the parts by weight, and weighing the HDI-N3390 isocyanate prepolymer according to the molar quantity of hydroxyl in the polyol mixed solution and the molar quantity of isocyanate groups in the HDI-N3390 isocyanate prepolymer of 1:1.1; in nitrogen atmosphere, adding the polyol mixed solution and the pore opening agent into N, N-dimethylformamide which is 2 times of the mass of the polyol mixed solution, uniformly mixing, adding the loaded modified porous silica microspheres, stirring for 5min at 20 ℃ and 200r/min, adding the HDI-N3390 isocyanate prepolymer, stirring for reaction for 30min at 50 ℃ and 200r/min, heating to 70 ℃ and continuing stirring for reaction for 10min, stopping stirring and preserving heat for 12h, taking out and washing with pure water for 3 times, and standing for 8h at 20 ℃ and 1kPa to obtain a polyurethane porous material;
(4) Adding diphenoxyphosphoryl chloride and 1-aminopyrrole into N, N-dimethylformamide with 6 times of diphenoxyphosphoryl chloride according to a molar ratio of 1:1, adding triethylamine with 0.8 times of diphenoxyphosphoryl chloride, stirring and reacting for 3h at 200r/min at 0 ℃ in a nitrogen atmosphere, and standing for 8h at 20 ℃ at 1kPa to obtain N-diphenoxyphosphoryl aminopyrrole; uniformly mixing pyrrole, N-diphenoxyphosphoryl aminopyrrole and absolute ethyl alcohol according to the mass ratio of 1:0.2:10 to prepare pyrrole solution; dissolving ferric chloride in 6mol/L hydrochloric acid aqueous solution at 20 ℃ until saturation is reached, so as to obtain saturated ferric chloride solution; at room temperature, immersing the polyurethane porous material in pyrrole solution for 80s, taking out, standing for 8h at 10 ℃ under 1kPa, immersing in saturated ferric chloride solution for 100s until no liquid drips in 20s, standing for 8h at 0 ℃, placing in absolute ethyl alcohol for washing for 3min, taking out, and drying for 8h at 30 ℃ under 1kPa to obtain the sound-insulation noise-reduction modified plastic.
Example 2
The preparation method of the sound-insulating and noise-reducing modified plastic mainly comprises the following preparation steps:
(1) Uniformly mixing tetraethoxysilane, ammonia water with the mass fraction of 25%, pure water and absolute ethyl alcohol according to the volume ratio of 1:1:2:20, stirring at 45 ℃ for 3.5 hours at 250r/min, centrifugally separating to obtain solid, and standing at 25 ℃ for 3.5 hours at 1.5kPa to obtain silica sol; uniformly mixing silica sol, urea and pure water according to a mass ratio of 1:1:150, regulating the pH to 1.25 by using hydrochloric acid with a mass fraction of 10%, adding sodium dodecyl benzene sulfonate with a mass of 0.25 times that of the silica sol, stirring for 11min at 55 ℃ and 250r/min, adding formaldehyde with a molar quantity of 0.75 times that of the urea, continuously stirring for 5h, centrifugally separating, washing for 4 times by using pure water, drying for 10-12 h at 65 ℃, placing in a horse fluorine furnace, sequentially heating from room temperature to 200 ℃ at a heating rate of 7 ℃/min and keeping the temperature for 2h, heating to 270 ℃ at a heating rate of 1 ℃/min and keeping the temperature for 2h, heating to 350 ℃ at a heating rate of 2 ℃/min and keeping the temperature for 2h, heating to 450 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 2h, and naturally cooling to room temperature to obtain porous silica microspheres;
(2) Uniformly mixing a silane coupling agent KH-550, pure water and absolute ethyl alcohol according to a mass ratio of 1:2.5:9, stirring at 25 ℃ for 22min at 700r/min, adding porous silica microspheres with the mass 0.9 times that of the silane coupling agent KH-550, stirring at 25 ℃ for 1.5h at 250r/min, centrifugally separating to obtain a solid, washing with absolute ethyl alcohol for 4 times, and drying at 65 ℃ for 7h to obtain modified porous silica microspheres; uniformly mixing 4,4' -oxo-bis-benzenesulfonyl hydrazine and diethyl ether according to a mass ratio of 1:11 to prepare a loading solution, immersing the modified porous silica microspheres in the loading solution, standing at 12 ℃ for 4min, taking out and drying at 35 ℃ for 5h, and repeating the immersing and drying process for 4 times to obtain the loaded modified porous silica microspheres;
(3) Uniformly mixing alpha, omega-hydroxypropyl polysiloxane silicone oil MY 1203M, 3, 4-dihydroxythiophene and triethanolamine according to a mass ratio of 9:1:1 to obtain a polyol mixed solution; weighing 55 parts of polyol mixed solution, 1 part of G501 pore-forming agent, 5 parts of 141B foaming agent and 18 parts of loaded modified porous silica microspheres according to the parts by weight, and weighing the HDI-N3390 isocyanate prepolymer according to the molar quantity of hydroxyl in the polyol mixed solution and the molar quantity of isocyanate groups in the HDI-N3390 isocyanate prepolymer of 1:1.15; in nitrogen atmosphere, adding the polyol mixed solution and the pore opening agent into N, N-dimethylformamide with the mass of 2.5 times of that of the polyol mixed solution, uniformly mixing, adding the loaded modified porous silica microspheres, stirring at 25 ℃ for 3.5min at 250r/min, adding the HDI-N3390 isocyanate prepolymer, stirring at 55 ℃ for reaction at 250r/min for 25min, heating to 75 ℃ for continuous stirring for reaction for 12min, stopping stirring and preserving heat for 11h, taking out, washing with pure water for 4 times, and standing at 25 ℃ for 7h at 1.5kPa to obtain the polyurethane porous material;
(4) Adding diphenoxyphosphoryl chloride and 1-aminopyrrole into N, N-dimethylformamide with the mass being 7 times that of diphenoxyphosphoryl chloride according to the molar ratio of 1:1, adding triethylamine with the mass being 1 time that of diphenoxyphosphoryl chloride, stirring and reacting for 2.5h at the temperature of 250r/min in a nitrogen atmosphere, and standing for 7h at the temperature of 25 ℃ and the pressure of 1.5kPa to prepare the N-diphenoxyphosphoryl aminopyrrole; uniformly mixing pyrrole, N-diphenoxyphosphoryl aminopyrrole and absolute ethyl alcohol according to the mass ratio of 1:0.25:12 to prepare pyrrole solution; dissolving ferric chloride in 6mol/L hydrochloric acid aqueous solution at 20 ℃ until saturation is reached, so as to obtain saturated ferric chloride solution; at room temperature, immersing the polyurethane porous material in pyrrole solution for 90s, taking out, standing for 7h at 15 ℃ and 1.5kPa, immersing in saturated ferric chloride solution for 90s until no liquid drips in 20s, standing for 7h at 2 ℃, placing in absolute ethyl alcohol for washing for 4min, taking out, and drying for 7h at 35 ℃ and 1.5kPa to obtain the sound-insulation noise-reduction modified plastic.
Example 3
The preparation method of the sound-insulating and noise-reducing modified plastic mainly comprises the following preparation steps:
(1) Uniformly mixing tetraethoxysilane, ammonia water with the mass fraction of 25%, pure water and absolute ethyl alcohol according to the volume ratio of 1:1:2.1:22, stirring for 3 hours at 50 ℃ and 300r/min, centrifugally separating to obtain solid, and standing for 3 hours at 30 ℃ and 2kPa to obtain silica sol; uniformly mixing silica sol, urea and pure water according to a mass ratio of 1:1:160, regulating the pH to 1.3 by using hydrochloric acid with a mass fraction of 10%, adding sodium dodecyl benzene sulfonate with a mass of 0.3 times that of the silica sol, stirring for 10min at 60 ℃ and 300r/min, adding formaldehyde with a molar quantity of 0.8 times that of the urea, continuously stirring for 4h, centrifugally separating, washing for 5 times by using pure water, drying for 10h at 70 ℃, placing in a muffle furnace, sequentially heating from room temperature to 200 ℃ at a heating rate of 7 ℃/min and preserving heat for 2h, heating to 270 ℃ at a heating rate of 1 ℃/min and preserving heat for 2h, heating to 350 ℃ at a heating rate of 2 ℃/min and preserving heat for 2h, heating to 450 ℃ at a heating rate of 5 ℃/min and preserving heat for 2h, and naturally cooling to room temperature to obtain porous silica microspheres;
(2) Uniformly mixing a silane coupling agent KH-550, pure water and absolute ethyl alcohol according to a mass ratio of 1:3:10, stirring for 20min at 30 ℃ at 800r/min, adding porous silica microspheres with the mass 1 times that of the silane coupling agent KH-550, stirring for 1h at 30 ℃ at 300r/min, centrifugally separating to obtain a solid, washing with absolute ethyl alcohol for 5 times, and drying for 6h at 70 ℃ to obtain modified porous silica microspheres; uniformly mixing 4,4' -oxo-bis-benzenesulfonyl hydrazine and diethyl ether according to a mass ratio of 1:12 to prepare a loading solution, immersing the modified porous silica microspheres in the loading solution, standing at 15 ℃ for 3min, taking out and drying at 40 ℃ for 4h, and repeating the immersing and drying process for 5 times to obtain the loaded modified porous silica microspheres;
(3) Uniformly mixing alpha, omega-hydroxypropyl polysiloxane silicone oil MY 1203M, 3, 4-dihydroxythiophene and triethanolamine according to a mass ratio of 10:1:1 to obtain a polyol mixed solution; weighing 60 parts of polyol mixed solution, 1 part of G501 pore-forming agent, 6 parts of 141B foaming agent and 20 parts of loaded modified porous silica microspheres according to the parts by weight, and weighing the HDI-N3390 isocyanate prepolymer according to the molar quantity of hydroxyl in the polyol mixed solution and the molar quantity of isocyanate groups in the HDI-N3390 isocyanate prepolymer of 1:1.2; in a nitrogen atmosphere, adding a polyol mixed solution and a pore opening agent into N, N-dimethylformamide which is 3 times of the mass of the polyol mixed solution, uniformly mixing, adding the loaded modified porous silica microspheres, stirring for 5min at 30 ℃ and 200-300 r/min, adding an HDI-N3390 isocyanate prepolymer, stirring for reacting for 20min at 60 ℃ and 300r/min, heating to 80 ℃ for continuously stirring for reacting for 10min, stopping stirring and preserving heat for 12h, taking out and washing with pure water for 5 times, and standing for 6h at 20 ℃ and 2kPa to obtain a polyurethane porous material;
(4) Adding diphenoxyphosphoryl chloride and 1-aminopyrrole into N, N-dimethylformamide with 6-8 times of diphenoxyphosphoryl chloride according to a molar ratio of 1:1, adding triethylamine with 1.2 times of diphenoxyphosphoryl chloride, stirring and reacting for 2 hours at a temperature of 300r/min in a nitrogen atmosphere, and standing for 6 hours at a temperature of 30 ℃ under a pressure of 2kPa to obtain N-diphenoxyphosphoryl aminopyrrole; uniformly mixing pyrrole, N-diphenoxyphosphoryl aminopyrrole and absolute ethyl alcohol according to the mass ratio of 1:0.3:15 to prepare pyrrole solution; dissolving ferric chloride in 6mol/L hydrochloric acid aqueous solution at 20 ℃ until saturation is reached, so as to obtain saturated ferric chloride solution; at room temperature, immersing the polyurethane porous material in pyrrole solution for 100s, taking out, standing for 6h at 20 ℃ under 2kPa, immersing in saturated ferric chloride solution for 100s until no liquid drips in 20s, standing for 6h at 4 ℃, placing in absolute ethyl alcohol for washing for 5min, taking out, and drying for 6h at 40 ℃ under 2kPa to obtain the sound-insulation noise-reduction modified plastic.
Comparative example 1
The preparation method of the sound-insulating and noise-reducing modified plastic mainly comprises the following preparation steps:
(1) Uniformly mixing tetraethoxysilane, ammonia water with the mass fraction of 25%, pure water and absolute ethyl alcohol according to the volume ratio of 1:1:2:20, stirring at 45 ℃ for 3.5 hours at 250r/min, centrifugally separating to obtain solid, and standing at 25 ℃ for 3.5 hours at 1.5kPa to obtain silica sol; uniformly mixing silica sol, urea and pure water according to a mass ratio of 1:1:150, regulating the pH to 1.25 by using hydrochloric acid with a mass fraction of 10%, adding sodium dodecyl benzene sulfonate with a mass of 0.25 times that of the silica sol, stirring for 11min at 55 ℃ and 250r/min, adding formaldehyde with a molar quantity of 0.75 times that of the urea, continuously stirring for 5h, centrifugally separating, washing for 4 times by using pure water, drying for 10-12 h at 65 ℃, placing in a horse fluorine furnace, sequentially heating from room temperature to 200 ℃ at a heating rate of 7 ℃/min and keeping the temperature for 2h, heating to 270 ℃ at a heating rate of 1 ℃/min and keeping the temperature for 2h, heating to 350 ℃ at a heating rate of 2 ℃/min and keeping the temperature for 2h, heating to 450 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 2h, and naturally cooling to room temperature to obtain porous silica microspheres;
(2) Uniformly mixing 4,4' -oxo-bis-benzenesulfonyl hydrazine and diethyl ether according to a mass ratio of 1:11 to prepare a loading solution, immersing porous silica microspheres in the loading solution, standing at 12 ℃ for 4min, taking out and drying at 35 ℃ for 5h, and repeating the immersing and drying process for 4 times to obtain the loaded porous silica microspheres;
(3) Uniformly mixing alpha, omega-hydroxypropyl polysiloxane silicone oil MY 1203M, 3, 4-dihydroxythiophene and triethanolamine according to a mass ratio of 9:1:1 to obtain a polyol mixed solution; weighing 55 parts of a polyol mixed solution, 1 part of a G501 pore opening agent, 5 parts of a 141B foaming agent and 18 parts of loaded porous silica microspheres according to the parts by weight, and weighing the HDI-N3390 isocyanate prepolymer according to the molar quantity of hydroxyl in the polyol mixed solution and the molar quantity of isocyanate groups in the HDI-N3390 isocyanate prepolymer of 1:1.15; in nitrogen atmosphere, adding the polyol mixed solution and the pore opening agent into N, N-dimethylformamide with the mass of 2.5 times of that of the polyol mixed solution, uniformly mixing, adding the loaded porous silica microspheres, stirring at 25 ℃ for 3.5min at 250r/min, adding the HDI-N3390 isocyanate prepolymer, stirring at 55 ℃ for reaction for 25min at 250r/min, heating to 75 ℃ for continuous stirring for reaction for 12min, stopping stirring and preserving heat for 11h, taking out, washing with pure water for 4 times, and standing at 25 ℃ for 7h at 1.5kPa to obtain the polyurethane porous material;
(4) Adding diphenoxyphosphoryl chloride and 1-aminopyrrole into N, N-dimethylformamide with the mass being 7 times that of diphenoxyphosphoryl chloride according to the molar ratio of 1:1, adding triethylamine with the mass being 1 time that of diphenoxyphosphoryl chloride, stirring and reacting for 2.5h at the temperature of 250r/min in a nitrogen atmosphere, and standing for 7h at the temperature of 25 ℃ and the pressure of 1.5kPa to prepare the N-diphenoxyphosphoryl aminopyrrole; uniformly mixing pyrrole, N-diphenoxyphosphoryl aminopyrrole and absolute ethyl alcohol according to the mass ratio of 1:0.25:12 to prepare pyrrole solution; dissolving ferric chloride in 6mol/L hydrochloric acid aqueous solution at 20 ℃ until saturation is reached, so as to obtain saturated ferric chloride solution; at room temperature, immersing the polyurethane porous material in pyrrole solution for 90s, taking out, standing for 7h at 15 ℃ and 1.5kPa, immersing in saturated ferric chloride solution for 90s until no liquid drips in 20s, standing for 7h at 2 ℃, placing in absolute ethyl alcohol for washing for 4min, taking out, and drying for 7h at 35 ℃ and 1.5kPa to obtain the sound-insulation noise-reduction modified plastic.
Comparative example 2
The preparation method of the sound-insulating and noise-reducing modified plastic mainly comprises the following preparation steps:
(1) Uniformly mixing tetraethoxysilane, ammonia water with the mass fraction of 25%, pure water and absolute ethyl alcohol according to the volume ratio of 1:1:2:20, stirring at 45 ℃ for 3.5 hours at 250r/min, centrifugally separating to obtain solid, and standing at 25 ℃ for 3.5 hours at 1.5kPa to obtain silica sol; uniformly mixing silica sol, urea and pure water according to a mass ratio of 1:1:150, regulating the pH to 1.25 by using hydrochloric acid with a mass fraction of 10%, adding sodium dodecyl benzene sulfonate with a mass of 0.25 times that of the silica sol, stirring for 11min at 55 ℃ and 250r/min, adding formaldehyde with a molar quantity of 0.75 times that of the urea, continuously stirring for 5h, centrifugally separating, washing for 4 times by using pure water, drying for 10-12 h at 65 ℃, placing in a horse fluorine furnace, sequentially heating from room temperature to 200 ℃ at a heating rate of 7 ℃/min and keeping the temperature for 2h, heating to 270 ℃ at a heating rate of 1 ℃/min and keeping the temperature for 2h, heating to 350 ℃ at a heating rate of 2 ℃/min and keeping the temperature for 2h, heating to 450 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 2h, and naturally cooling to room temperature to obtain porous silica microspheres;
(2) Uniformly mixing a silane coupling agent KH-550, pure water and absolute ethyl alcohol according to a mass ratio of 1:2.5:9, stirring at 25 ℃ for 22min at 700r/min, adding porous silica microspheres with the mass 0.9 times that of the silane coupling agent KH-550, stirring at 25 ℃ for 1.5h at 250r/min, centrifugally separating to obtain a solid, washing with absolute ethyl alcohol for 4 times, and drying at 65 ℃ for 7h to obtain modified porous silica microspheres;
(3) Uniformly mixing alpha, omega-hydroxypropyl polysiloxane silicone oil MY 1203M, 3, 4-dihydroxythiophene and triethanolamine according to a mass ratio of 9:1:1 to obtain a polyol mixed solution; weighing 55 parts of polyol mixed solution, 1 part of G501 pore-forming agent, 5 parts of 141B foaming agent and 18 parts of modified porous silica microspheres according to the parts by weight, and weighing the HDI-N3390 isocyanate prepolymer according to the molar quantity of hydroxyl in the polyol mixed solution and the molar quantity of isocyanate groups in the HDI-N3390 isocyanate prepolymer of 1:1.15; in nitrogen atmosphere, adding the polyol mixed solution and the pore opening agent into N, N-dimethylformamide with the mass of 2.5 times of that of the polyol mixed solution, uniformly mixing, adding modified porous silica microspheres, stirring at 25 ℃ and 250r/min for 3.5min, adding HDI-N3390 isocyanate prepolymer, stirring at 55 ℃ and 250r/min for reaction for 25min, heating to 75 ℃ for continuous stirring reaction for 12min, stopping stirring and preserving heat for 11h, taking out, washing with pure water for 4 times, and standing at 25 ℃ and 1.5kPa for 7h to obtain a polyurethane porous material;
(4) Adding diphenoxyphosphoryl chloride and 1-aminopyrrole into N, N-dimethylformamide with the mass being 7 times that of diphenoxyphosphoryl chloride according to the molar ratio of 1:1, adding triethylamine with the mass being 1 time that of diphenoxyphosphoryl chloride, stirring and reacting for 2.5h at the temperature of 250r/min in a nitrogen atmosphere, and standing for 7h at the temperature of 25 ℃ and the pressure of 1.5kPa to prepare the N-diphenoxyphosphoryl aminopyrrole; uniformly mixing pyrrole, N-diphenoxyphosphoryl aminopyrrole and absolute ethyl alcohol according to the mass ratio of 1:0.25:12 to prepare pyrrole solution; dissolving ferric chloride in 6mol/L hydrochloric acid aqueous solution at 20 ℃ until saturation is reached, so as to obtain saturated ferric chloride solution; at room temperature, immersing the polyurethane porous material in pyrrole solution for 90s, taking out, standing for 7h at 15 ℃ and 1.5kPa, immersing in saturated ferric chloride solution for 90s until no liquid drips in 20s, standing for 7h at 2 ℃, placing in absolute ethyl alcohol for washing for 4min, taking out, and drying for 7h at 35 ℃ and 1.5kPa to obtain the sound-insulation noise-reduction modified plastic.
Comparative example 3
The preparation method of the sound-insulating and noise-reducing modified plastic mainly comprises the following preparation steps:
(1) Uniformly mixing tetraethoxysilane, ammonia water with the mass fraction of 25%, pure water and absolute ethyl alcohol according to the volume ratio of 1:1:2:20, stirring at 45 ℃ for 3.5 hours at 250r/min, centrifugally separating to obtain solid, and standing at 25 ℃ for 3.5 hours at 1.5kPa to obtain silica sol; uniformly mixing silica sol, urea and pure water according to a mass ratio of 1:1:150, regulating the pH to 1.25 by using hydrochloric acid with a mass fraction of 10%, adding sodium dodecyl benzene sulfonate with a mass of 0.25 times that of the silica sol, stirring for 11min at 55 ℃ and 250r/min, adding formaldehyde with a molar quantity of 0.75 times that of the urea, continuously stirring for 5h, centrifugally separating, washing for 4 times by using pure water, drying for 10-12 h at 65 ℃, placing in a horse fluorine furnace, sequentially heating from room temperature to 200 ℃ at a heating rate of 7 ℃/min and keeping the temperature for 2h, heating to 270 ℃ at a heating rate of 1 ℃/min and keeping the temperature for 2h, heating to 350 ℃ at a heating rate of 2 ℃/min and keeping the temperature for 2h, heating to 450 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 2h, and naturally cooling to room temperature to obtain porous silica microspheres;
(2) Uniformly mixing a silane coupling agent KH-550, pure water and absolute ethyl alcohol according to a mass ratio of 1:2.5:9, stirring at 25 ℃ for 22min at 700r/min, adding porous silica microspheres with the mass 0.9 times that of the silane coupling agent KH-550, stirring at 25 ℃ for 1.5h at 250r/min, centrifugally separating to obtain a solid, washing with absolute ethyl alcohol for 4 times, and drying at 65 ℃ for 7h to obtain modified porous silica microspheres; uniformly mixing 4,4' -oxo-bis-benzenesulfonyl hydrazine and diethyl ether according to a mass ratio of 1:11 to prepare a loading solution, immersing the modified porous silica microspheres in the loading solution, standing at 12 ℃ for 4min, taking out and drying at 35 ℃ for 5h, and repeating the immersing and drying process for 4 times to obtain the loaded modified porous silica microspheres;
(3) Uniformly mixing 1, 3-propanediol, 3, 4-dihydroxythiophene and triethanolamine according to a mass ratio of 9:1:1 to obtain a polyol mixed solution; weighing 55 parts of polyol mixed solution, 1 part of G501 pore-forming agent, 5 parts of 141B foaming agent and 18 parts of loaded modified porous silica microspheres according to the parts by weight, and weighing the HDI-N3390 isocyanate prepolymer according to the molar quantity of hydroxyl in the polyol mixed solution and the molar quantity of isocyanate groups in the HDI-N3390 isocyanate prepolymer of 1:1.15; in nitrogen atmosphere, adding the polyol mixed solution and the pore opening agent into N, N-dimethylformamide with the mass of 2.5 times of that of the polyol mixed solution, uniformly mixing, adding the loaded modified porous silica microspheres, stirring at 25 ℃ for 3.5min at 250r/min, adding the HDI-N3390 isocyanate prepolymer, stirring at 55 ℃ for reaction at 250r/min for 25min, heating to 75 ℃ for continuous stirring for reaction for 12min, stopping stirring and preserving heat for 11h, taking out, washing with pure water for 4 times, and standing at 25 ℃ for 7h at 1.5kPa to obtain the polyurethane porous material;
(4) Adding diphenoxyphosphoryl chloride and 1-aminopyrrole into N, N-dimethylformamide with the mass being 7 times that of diphenoxyphosphoryl chloride according to the molar ratio of 1:1, adding triethylamine with the mass being 1 time that of diphenoxyphosphoryl chloride, stirring and reacting for 2.5h at the temperature of 250r/min in a nitrogen atmosphere, and standing for 7h at the temperature of 25 ℃ and the pressure of 1.5kPa to prepare the N-diphenoxyphosphoryl aminopyrrole; uniformly mixing pyrrole, N-diphenoxyphosphoryl aminopyrrole and absolute ethyl alcohol according to the mass ratio of 1:0.25:12 to prepare pyrrole solution; dissolving ferric chloride in 6mol/L hydrochloric acid aqueous solution at 20 ℃ until saturation is reached, so as to obtain saturated ferric chloride solution; at room temperature, immersing the polyurethane porous material in pyrrole solution for 90s, taking out, standing for 7h at 15 ℃ and 1.5kPa, immersing in saturated ferric chloride solution for 90s until no liquid drips in 20s, standing for 7h at 2 ℃, placing in absolute ethyl alcohol for washing for 4min, taking out, and drying for 7h at 35 ℃ and 1.5kPa to obtain the sound-insulation noise-reduction modified plastic.
Comparative example 4
The preparation method of the sound-insulating and noise-reducing modified plastic mainly comprises the following preparation steps:
(1) Uniformly mixing tetraethoxysilane, ammonia water with the mass fraction of 25%, pure water and absolute ethyl alcohol according to the volume ratio of 1:1:2:20, stirring at 45 ℃ for 3.5 hours at 250r/min, centrifugally separating to obtain solid, and standing at 25 ℃ for 3.5 hours at 1.5kPa to obtain silica sol; uniformly mixing silica sol, urea and pure water according to a mass ratio of 1:1:150, regulating the pH to 1.25 by using hydrochloric acid with a mass fraction of 10%, adding sodium dodecyl benzene sulfonate with a mass of 0.25 times that of the silica sol, stirring for 11min at 55 ℃ and 250r/min, adding formaldehyde with a molar quantity of 0.75 times that of the urea, continuously stirring for 5h, centrifugally separating, washing for 4 times by using pure water, drying for 10-12 h at 65 ℃, placing in a horse fluorine furnace, sequentially heating from room temperature to 200 ℃ at a heating rate of 7 ℃/min and keeping the temperature for 2h, heating to 270 ℃ at a heating rate of 1 ℃/min and keeping the temperature for 2h, heating to 350 ℃ at a heating rate of 2 ℃/min and keeping the temperature for 2h, heating to 450 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 2h, and naturally cooling to room temperature to obtain porous silica microspheres;
(2) Uniformly mixing a silane coupling agent KH-550, pure water and absolute ethyl alcohol according to a mass ratio of 1:2.5:9, stirring at 25 ℃ for 22min at 700r/min, adding porous silica microspheres with the mass 0.9 times that of the silane coupling agent KH-550, stirring at 25 ℃ for 1.5h at 250r/min, centrifugally separating to obtain a solid, washing with absolute ethyl alcohol for 4 times, and drying at 65 ℃ for 7h to obtain modified porous silica microspheres; uniformly mixing 4,4' -oxo-bis-benzenesulfonyl hydrazine and diethyl ether according to a mass ratio of 1:11 to prepare a loading solution, immersing the modified porous silica microspheres in the loading solution, standing at 12 ℃ for 4min, taking out and drying at 35 ℃ for 5h, and repeating the immersing and drying process for 4 times to obtain the loaded modified porous silica microspheres;
(3) Uniformly mixing alpha, omega-hydroxypropyl polysiloxane silicone oil MY 1203M and triethanolamine according to a mass ratio of 9:1 to obtain a polyol mixed solution; weighing 55 parts of polyol mixed solution, 1 part of G501 pore-forming agent, 5 parts of 141B foaming agent and 18 parts of loaded modified porous silica microspheres according to the parts by weight, and weighing the HDI-N3390 isocyanate prepolymer according to the molar quantity of hydroxyl in the polyol mixed solution and the molar quantity of isocyanate groups in the HDI-N3390 isocyanate prepolymer of 1:1.15; in nitrogen atmosphere, adding the polyol mixed solution and the pore opening agent into N, N-dimethylformamide with the mass of 2.5 times of that of the polyol mixed solution, uniformly mixing, adding the loaded modified porous silica microspheres, stirring at 25 ℃ for 3.5min at 250r/min, adding the HDI-N3390 isocyanate prepolymer, stirring at 55 ℃ for reaction at 250r/min for 25min, heating to 75 ℃ for continuous stirring for reaction for 12min, stopping stirring and preserving heat for 11h, taking out, washing with pure water for 4 times, and standing at 25 ℃ for 7h at 1.5kPa to obtain the polyurethane porous material;
(4) Adding diphenoxyphosphoryl chloride and 1-aminopyrrole into N, N-dimethylformamide with the mass being 7 times that of diphenoxyphosphoryl chloride according to the molar ratio of 1:1, adding triethylamine with the mass being 1 time that of diphenoxyphosphoryl chloride, stirring and reacting for 2.5h at the temperature of 250r/min in a nitrogen atmosphere, and standing for 7h at the temperature of 25 ℃ and the pressure of 1.5kPa to prepare the N-diphenoxyphosphoryl aminopyrrole; uniformly mixing pyrrole, N-diphenoxyphosphoryl aminopyrrole and absolute ethyl alcohol according to the mass ratio of 1:0.25:12 to prepare pyrrole solution; dissolving ferric chloride in 6mol/L hydrochloric acid aqueous solution at 20 ℃ until saturation is reached, so as to obtain saturated ferric chloride solution; at room temperature, immersing the polyurethane porous material in pyrrole solution for 90s, taking out, standing for 7h at 15 ℃ and 1.5kPa, immersing in saturated ferric chloride solution for 90s until no liquid drips in 20s, standing for 7h at 2 ℃, placing in absolute ethyl alcohol for washing for 4min, taking out, and drying for 7h at 35 ℃ and 1.5kPa to obtain the sound-insulation noise-reduction modified plastic.
Comparative example 5
The preparation method of the sound-insulating and noise-reducing modified plastic mainly comprises the following preparation steps:
(1) Uniformly mixing tetraethoxysilane, ammonia water with the mass fraction of 25%, pure water and absolute ethyl alcohol according to the volume ratio of 1:1:2:20, stirring at 45 ℃ for 3.5 hours at 250r/min, centrifugally separating to obtain solid, and standing at 25 ℃ for 3.5 hours at 1.5kPa to obtain silica sol; uniformly mixing silica sol, urea and pure water according to a mass ratio of 1:1:150, regulating the pH to 1.25 by using hydrochloric acid with a mass fraction of 10%, adding sodium dodecyl benzene sulfonate with a mass of 0.25 times that of the silica sol, stirring for 11min at 55 ℃ and 250r/min, adding formaldehyde with a molar quantity of 0.75 times that of the urea, continuously stirring for 5h, centrifugally separating, washing for 4 times by using pure water, drying for 10-12 h at 65 ℃, placing in a horse fluorine furnace, sequentially heating from room temperature to 200 ℃ at a heating rate of 7 ℃/min and keeping the temperature for 2h, heating to 270 ℃ at a heating rate of 1 ℃/min and keeping the temperature for 2h, heating to 350 ℃ at a heating rate of 2 ℃/min and keeping the temperature for 2h, heating to 450 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 2h, and naturally cooling to room temperature to obtain porous silica microspheres;
(2) Uniformly mixing a silane coupling agent KH-550, pure water and absolute ethyl alcohol according to a mass ratio of 1:2.5:9, stirring at 25 ℃ for 22min at 700r/min, adding porous silica microspheres with the mass 0.9 times that of the silane coupling agent KH-550, stirring at 25 ℃ for 1.5h at 250r/min, centrifugally separating to obtain a solid, washing with absolute ethyl alcohol for 4 times, and drying at 65 ℃ for 7h to obtain modified porous silica microspheres; uniformly mixing 4,4' -oxo-bis-benzenesulfonyl hydrazine and diethyl ether according to a mass ratio of 1:11 to prepare a loading solution, immersing the modified porous silica microspheres in the loading solution, standing at 12 ℃ for 4min, taking out and drying at 35 ℃ for 5h, and repeating the immersing and drying process for 4 times to obtain the loaded modified porous silica microspheres;
(3) Uniformly mixing alpha, omega-hydroxypropyl polysiloxane silicone oil MY 1203M, 3, 4-dihydroxythiophene and triethanolamine according to a mass ratio of 9:1:1 to obtain a polyol mixed solution; weighing 55 parts of polyol mixed solution, 1 part of G501 pore-forming agent, 5 parts of 141B foaming agent and 18 parts of loaded modified porous silica microspheres according to the parts by weight, and weighing the HDI-N3390 isocyanate prepolymer according to the molar quantity of hydroxyl in the polyol mixed solution and the molar quantity of isocyanate groups in the HDI-N3390 isocyanate prepolymer of 1:1.15; in nitrogen atmosphere, adding the polyol mixed solution and the pore opening agent into N, N-dimethylformamide with the mass of 2.5 times of that of the polyol mixed solution, uniformly mixing, adding the loaded modified porous silica microspheres, stirring at 25 ℃ for 3.5min at 250r/min, adding the HDI-N3390 isocyanate prepolymer, stirring at 55 ℃ for reaction at 250r/min for 25min, heating to 75 ℃ for continuous stirring for reaction for 12min, stopping stirring and preserving heat for 11h, taking out, washing with pure water for 4 times, and standing at 25 ℃ for 7h at 1.5kPa to obtain the polyurethane porous material;
(4) Uniformly mixing pyrrole and absolute ethyl alcohol according to a mass ratio of 1:12 to prepare pyrrole solution; dissolving ferric chloride in 6mol/L hydrochloric acid aqueous solution at 20 ℃ until saturation is reached, so as to obtain saturated ferric chloride solution; at room temperature, immersing the polyurethane porous material in pyrrole solution for 90s, taking out, standing for 7h at 15 ℃ and 1.5kPa, immersing in saturated ferric chloride solution for 90s until no liquid drips in 20s, standing for 7h at 2 ℃, placing in absolute ethyl alcohol for washing for 4min, taking out, and drying for 7h at 35 ℃ and 1.5kPa to obtain the sound-insulation noise-reduction modified plastic.
Test example 1
Sound insulation and noise reduction performance
The testing method comprises the following steps: a sound absorption sample was prepared according to GB/T18696.2, the sample size was 29mm in diameter and 30mm in length, and the sound absorption coefficient of the sample was measured by using a transfer function method. The results are shown in Table 1.
As can be seen from comparison of experimental data of examples 1-3 and comparative examples 1-5 in Table 1, the modified plastic for sound insulation and noise reduction prepared by the invention has good sound insulation and noise reduction performance.
As can be seen from the comparison of the data of examples 1-3 and comparative example 1, the sound absorption coefficients of examples 1-3 are high, which means that the porous silica microspheres are modified, and the dispersibility of the porous silica microspheres is improved, so that the sound insulation and noise reduction performance is improved, and the surface is provided with amino groups, so that the sound insulation and noise reduction composite material has a good combination effect with a main body.
The comparison of the data of examples 1-3 and comparative example 2 shows that the sound absorption coefficient of examples 1-3 is high, which indicates that the modified porous silica microspheres are loaded, and the loaded 4,4' -oxo-bis-benzenesulfonyl hydrazide has a foaming effect, and directly starts from the inside of the modified porous silica microspheres, so that the interface bonding state of the modified porous silica microspheres and the polymer is improved, the pore diameter is kept communicated, the better sound absorption effect is achieved, and the sound insulation and noise reduction performance is improved.
The data comparison of examples 1-3 and comparative example 4 shows that the sound absorption coefficient of examples 1-3 is high, which indicates that 3, 4-dihydroxythiophene is used in the preparation process of the polyurethane porous material, and can participate in polymerization of pyrrole subsequently, so that polypyrrole is combined on the surfaces of pores and air cavities to prevent the pores from being blocked due to falling and rolling, and thus the sound insulation and noise reduction performance is improved.
Test example 2
The flame retardant performance test method comprises the following steps: according to GB/T10707 oxygen index test standard, the prepared sound-insulating noise-reducing modified plastic is processed into 10mm10mm/>The LOI value was measured by clamping a rectangular sample bar of 80mm with a test tube clamp in the combustion cylinder. The results are shown in Table 2.
From the comparison of the experimental data of examples 1-3 and comparative examples 1-5 in Table 2, it can be found that the modified plastic for sound insulation and noise reduction prepared by the invention has good flame retardant property.
As can be seen from the comparison of the data of examples 1-3 and comparative example 1, the high limiting oxygen index of examples 1-3 demonstrates that the modification of the porous silica microspheres improves the dispersibility of the porous silica microspheres, and the porous silica microspheres themselves have flame retardant effects, and the improvement of the dispersibility also improves the overall flame retardance.
As can be seen from the comparison of the data of examples 1-3 and comparative example 3, the limiting oxygen index of examples 1-3 is high, which indicates that the use of alpha, omega-hydroxypropyl polysiloxane silicone oil in the preparation process of the polyurethane porous material can lead to polysiloxane chain segments in the polyurethane porous material and has good flame retardant effect.
As can be seen from the comparison of the data of examples 1-3 and comparative example 5, the limiting oxygen index of examples 1-3 is high, which indicates that N-diphenoxyphosphoryl amino pyrrole participates in the polymerization of pyrrole, and the formed polypyrrole contains a large amount of diphenoxyphosphoryl amino structure and has good char formation protection effect on the main body of the polyurethane porous material, thereby improving the flame retardance.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (6)
1. The sound-insulating and noise-reducing modified plastic is characterized by being prepared by mixing polyol mixed liquid, a pore opening agent, a foaming agent, loaded modified porous silica microspheres and isocyanate prepolymer, foaming and curing to obtain a polyurethane porous material; oxidizing and polymerizing pyrrole and N-diphenoxy phosphoryl amino pyrrole on the surfaces of pore channels and air cavities of the polyurethane porous material to prepare sound-insulating and noise-reducing modified plastic;
the polyol mixed solution is prepared by mixing alpha, omega-hydroxypropyl polysiloxane silicone oil, 3, 4-dihydroxythiophene and triethanolamine;
the modified porous silica microsphere is prepared by modifying porous silica microsphere with silane coupling agent and loading 4,4' -oxo-bis-benzenesulfonyl hydrazide;
The N-diphenoxyphosphoryl aminopyrrole is prepared by reacting diphenoxyphosphoryl chloride and 1-aminopyrrole.
2. The preparation method of the sound-insulating and noise-reducing modified plastic is characterized by comprising the following preparation steps:
(1) Uniformly mixing silica sol, urea and pure water according to a mass ratio of 1:1:140-160, regulating the pH value to 1.2-1.3 by using hydrochloric acid with a mass fraction of 10%, adding sodium dodecyl benzene sulfonate with a mass of 0.2-0.3 times that of the silica sol, stirring for 10-12 min at 50-60 ℃ at 200-300 r/min, adding formaldehyde with a urea molar amount of 0.7-0.8 times, continuing stirring for 4-6 h, centrifugally separating, washing for 3-5 times by pure water, drying for 10-12 h at 60-70 ℃, placing in a muffle furnace for programmed temperature calcination, and naturally cooling to room temperature to obtain porous silica microspheres;
(2) Uniformly mixing a silane coupling agent KH-550, pure water and absolute ethyl alcohol according to a mass ratio of 1:2-3:8-10, stirring for 20-25 min at 20-30 ℃ at 600-800 r/min, adding porous silica microspheres with the mass 0.8-1 times that of the silane coupling agent KH-550, stirring for 1-2 h at 20-30 ℃ at 200-300 r/min, centrifugally separating to obtain solid, washing 3-5 times with absolute ethyl alcohol, and drying for 6-8 h at 60-70 ℃ to obtain modified porous silica microspheres; uniformly mixing 4,4' -oxo-bis-benzenesulfonyl hydrazine and diethyl ether according to the mass ratio of 1:10-12 to prepare a loading solution, immersing the modified porous silica microspheres in the loading solution, standing for 3-5 min at 10-15 ℃, taking out and drying for 4-6 h at 30-40 ℃, and repeating the immersed drying process for 3-5 times to obtain the loaded modified porous silica microspheres;
(3) Uniformly mixing alpha, omega-hydroxypropyl polysiloxane silicone oil MY 1203M, 3, 4-dihydroxythiophene and triethanolamine according to a mass ratio of 8-10:1:1 to prepare a polyol mixed solution; weighing 50-60 parts of polyol mixed solution, 1 part of pore opening agent, 4-6 parts of foaming agent and 15-20 parts of loaded modified porous silica microspheres according to the mass parts, and weighing isocyanate prepolymer according to the molar weight of hydroxyl in the polyol mixed solution and the molar weight of isocyanate groups in the isocyanate prepolymer of 1:1.1-1.2; adding the polyol mixed solution and the pore opening agent into N, N-dimethylformamide which is 2-3 times of the mass of the polyol mixed solution in a nitrogen atmosphere, uniformly mixing, adding the loaded modified porous silica microspheres, stirring for 3-5 min at 20-30 ℃ at 200-300 r/min, adding the isocyanate prepolymer, stirring for reacting for 20-30 min at 50-60 ℃ at 200-300 r/min, heating to 70-80 ℃ for continuously stirring for reacting for 10-15 min, stopping stirring and preserving heat for 10-12 h, taking out and washing with pure water for 3-5 times, and standing for 6-8 h at 20-30 ℃ at 1-2 kPa to obtain the polyurethane porous material;
(4) Uniformly mixing pyrrole, N-diphenoxyphosphoryl aminopyrrole and absolute ethyl alcohol according to the mass ratio of 1:0.2-0.3:10-15 to prepare pyrrole solution; dissolving ferric chloride in 6mol/L hydrochloric acid aqueous solution at 20 ℃ until saturation is reached, so as to obtain saturated ferric chloride solution; at room temperature, immersing the polyurethane porous material in pyrrole solution for 80-100 s, taking out, standing for 6-8 h at 10-20 ℃ under 1-2 kPa, immersing in saturated ferric chloride solution for 80-100 s until no liquid drips in 20s, standing for 6-8 h at 0-4 ℃, placing in absolute ethyl alcohol for washing for 3-5 min, taking out, and drying for 6-8 h at 30-40 ℃ under 1-2 kPa to obtain the sound-insulation and noise-reduction modified plastic.
3. The method for preparing the modified plastic for sound insulation and noise reduction according to claim 2, wherein the method for preparing the silica sol in the step (1) is as follows: uniformly mixing tetraethoxysilane, ammonia water with the mass fraction of 25%, pure water and absolute ethyl alcohol according to the volume ratio of 1:1:1.9-2.1:18-22, stirring for 3-4 hours at the temperature of 40-50 ℃ at the speed of 200-300 r/min, centrifugally separating to obtain solid, and standing for 3-4 hours at the temperature of 20-30 ℃ at the speed of 1-2 kPa.
4. The method for preparing the modified plastic for sound insulation and noise reduction according to claim 2, wherein the method for temperature programming and calcining in the step (1) is as follows: sequentially heating from room temperature to 200 ℃ at a heating rate of 7 ℃/min and preserving heat for 2 hours, heating to 270 ℃ at a heating rate of 1 ℃/min and preserving heat for 2 hours, heating to 350 ℃ at a heating rate of 2 ℃/min and preserving heat for 2 hours, and heating to 450 ℃ at a heating rate of 5 ℃/min and preserving heat for 2 hours.
5. The method for producing a modified plastic for sound insulation and noise reduction according to claim 2, wherein the model of the tapping agent in the step (3) is G501; the model of the foaming agent is 141B; the type of the isocyanate prepolymer is HDI-N3390.
6. The method for preparing the modified plastic for sound insulation and noise reduction according to claim 2, wherein the preparation method of the N-diphenoxyphosphoryl aminopyrrole in the step (4) is as follows: adding diphenoxyphosphoryl chloride and 1-aminopyrrole into N, N-dimethylformamide with the mass of 6-8 times of diphenoxyphosphoryl chloride according to the molar ratio of 1:1, adding triethylamine with the mass of 0.8-1.2 times of diphenoxyphosphoryl chloride, stirring and reacting for 2-3 h at the temperature of 0-5 ℃ and the speed of 200-300 r/min in a nitrogen atmosphere, and standing for 6-8 h at the temperature of 20-30 ℃ and the speed of 1-2 kPa.
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