Environment-friendly building energy-saving sound insulation material and preparation method thereof
By combining modified polyether polyol with isocyanate and modified hollow glass microbeads, combined with triazine flame retardant intercalation to modify sericite, the problem of insufficient flammability and flame retardant properties of rigid polyurethane foam is solved. , realizes excellent heat insulation and flame retardant properties of the material, while improving mechanical properties.
Patent Information
- Application Number
- CN202411363347.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-27
- Publication Date
- 2025-01-10
- Estimated Expiration
- 2044-09-27
AI Technical Summary
The existing rigid polyurethane foam insulation materials have problems such as flammability, insufficient flame retardant performance and great impact on physical properties, making it difficult to take into account both flame retardant performance and mechanical properties.
Use modified polyether polyol and isocyanate to prepare hard foamed polyurethane materials, add modified hollow glass microbeads, modified sericite and ammonium polyphosphate, and modify the treatment through chemical grafting and composite coupling agent, combined with triazine The flame retardant interlayer is modified with sericite to form a material with excellent heat insulation and flame retardant properties.
It achieves excellent heat insulation and flame retardant properties of the material, while improving mechanical properties, ensuring safety and thermal insulation effects.
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Abstract
Description
Technical Field
[0001] The invention belongs to the field of building materials, and in particular relates to an environmentally friendly building energy-saving sound-insulating material and a preparation method thereof. Background Art
[0002] With the development of urbanization, the building area is growing rapidly every year, while the area of energy-saving buildings only accounts for 5%, and the building energy consumption accounts for 30% of the total energy consumption. Building energy conservation is an important aspect of solving the energy consumption problem. Phase change material is a substance that can store or release latent heat in a nearly isothermal manner and has a high energy storage density. People classify phase change materials with high energy storage density as latent heat energy storage materials, which are suitable for thermal energy storage applications. In addition to storing thermal energy, phase change materials can also produce thermal regulation effects on the building components in which they are located by releasing a large amount of latent heat during the phase change process. At present, the most commonly used insulation material in building envelope structures is rigid polyurethane foam to ensure the internal insulation of the building.
[0003] Rigid polyurethane foam is inherently flammable, and its limiting oxygen index is 19.0%. During the combustion process, rigid polyurethane foam will burn violently and produce a large amount of toxic smoke and gas, resulting in serious casualties and economic losses. Therefore, researchers continue to modify rigid polyurethane insulation materials to make them flame retardant, and improve the flame retardant properties of rigid polyurethane insulation materials by adding flame retardants with various functions, and prepare new rigid polyurethane insulation materials with low cost, low thermal conductivity, good thermal insulation performance, and good flame retardant properties, thereby effectively flame retardant, ensuring safety, and heat insulation. Flame retardant rigid polyurethane foam has the disadvantages of large addition amount, poor dispersibility, and great influence on the physical properties of the material. Therefore, it is necessary to develop new building energy-saving materials that take into account both flame retardant properties and mechanical properties. Summary of the invention
[0004] In order to solve the deficiencies mentioned in the above background technology, the purpose of the present invention is to provide an environmentally friendly building energy-saving sound insulation material and a preparation method thereof, wherein a rigid foamed polyurethane material is prepared by using modified polyether polyol and isocyanate, and modified hollow glass microspheres, modified sericite and ammonium polyphosphate are added, so that the material has excellent thermal insulation and flame retardant properties, as well as good mechanical properties.
[0005] The purpose of the present invention can be achieved through the following technical solutions:
[0006] An environmentally friendly building energy-saving sound-insulating material comprises the following raw materials in parts by weight: 100-120 parts of modified polyether polyol, 140-150 parts of isocyanate, 8-12 parts of modified hollow glass microspheres, 5-8 parts of modified sericite, 3-5 parts of ammonium polyphosphate, 2-4 parts of foaming agent, 1-3 parts of stabilizer, and 0.1-0.5 parts of catalyst;
[0007] The modified polyether polyol is a polyether polyol containing phosphorus and phase change energy storage segments, the modified hollow glass microspheres are hollow glass microspheres surface-modified by a composite coupling agent, the modified sericite is sericite intercalated with a triazine flame retardant, and the triazine flame retardant is a triazine derivative containing a siloxane structure and a DOPO structure, and its structural formula is as follows:
[0008]
[0009] Further preferably, the catalyst is selected from one or more of pentamethyldiethylenetriamine, dimethylcyclohexylamine, 2-hydroxy-N,N,N-trimethyl-1-propylamine formate, potassium acetate and bis(dimethylaminoethyl) ether.
[0010] Further preferably, the preparation method of the modified polyether polyol comprises the following steps:
[0011] (1) adding polyethylene glycol to tetrahydrofuran and stirring to dissolve to obtain solution A, adding phosphorus oxychloride to n-hexane and dissolving to obtain solution B, slowly dropping solution B into solution A, stirring evenly and then standing for 1 to 2 hours;
[0012] (2) slowly heating the reaction system to 90-100° C., slowly adding the polyether polyol while stirring, and keeping the temperature to react for 1-2 hours after the addition is completed to obtain a modified polyether polyol.
[0013] More preferably, the molar ratio of polyethylene glycol, phosphorus oxychloride and polyether polyol is 2:1:1.
[0014] Further preferably, the method for preparing the modified hollow glass microspheres comprises the following steps:
[0015] a. Mix silane coupling agents γ-aminopropyltriethoxysilane and γ-mercaptopropyltrimethoxysilane in a mass ratio of 3:2, and then add them into an ethanol aqueous solution in a volume ratio of 9:1;
[0016] b. Add the hollow glass microspheres into the hydrolyzed silane aqueous solution and stir the reaction at 60°C for 3 to 5 hours;
[0017] c. After the reaction is completed, the modified hollow glass microspheres are obtained by repeatedly washing with deionized water and ethanol for 3 to 5 times, and then filtering under reduced pressure, and then filtering under reduced pressure and drying.
[0018] Further preferably, the preparation method of modified sericite comprises the following steps:
[0019] A. Add p-hydroxybenzaldehyde and sodium carbonate to acetone, stir to mix thoroughly, then add cyanuric chloride, slowly heat to 50-60°C, reflux for 4-6 hours, cool to room temperature after the reaction, filter under reduced pressure, wash with water 3-5 times, and dry to obtain a white powder product A;
[0020] B. Add 3-aminopropyltriethoxysilane, triethylamine and tetrahydrofuran into a reactor, stir to fully mix, then add product A, slowly raise the temperature to 50-60°C, reflux for 4-6 hours, evaporate and filter to remove tetrahydrofuran and triethylamine hydrochloride, add ethyl acetate to the separated organic phase, dry and filter, and distill the filtrate under reduced pressure to obtain product B;
[0021] C. Add DOPO to 1,2-dichloroethane, stir and heat to 85°C. After DOPO is completely dissolved, slowly add product B, keep the system temperature at 85°C, and reflux for 4 to 6 hours. After the reaction is completed, reduce pressure and filter, then wash with 1,2-dichloroethane 3 to 5 times to remove excess DOPO. After washing, dry and dry to obtain a triazine flame retardant;
[0022] D. Add sericite to a mixture of anhydrous ethanol and distilled water, and disperse by ultrasonication for 10 to 15 minutes. Adjust the pH value of the solution to 4 with aqueous hydrochloric acid solution. Then slowly add triazine flame retardant to the sericite dispersion, and disperse by ultrasonication for 5 to 10 minutes. Heat to 60 to 80°C and keep the temperature for reaction for 3 to 5 hours. After cooling, filter, wash and dry to obtain modified sericite.
[0023] More preferably, the molar ratio of cyanuric chloride, p-hydroxybenzaldehyde, 3-aminopropyltriethoxysilane and DOPO is 1:2:1:2.
[0024] A method for preparing an environmentally friendly building energy-saving sound-insulating material comprises the following steps:
[0025] S1. According to the formula ratio, weigh the modified polyether polyol, catalyst, stabilizer and water, mix them, stir them at high speed for 10 to 15 minutes, mix the modified hollow glass microspheres, modified sericite and ammonium polyphosphate together, pour them into the mixture, and stir them at high speed for 10 minutes;
[0026] S2. Add a foaming agent, stir at high speed for 1 to 2 minutes, then add isocyanate, stir at high speed for 8 to 10 seconds, quickly pour the resulting mixture into a prepared mold, mature at 100 to 120° C. for 4 to 6 hours, and foam to obtain an environmentally friendly building energy-saving sound insulation material.
[0027] Beneficial effects of the present invention:
[0028] The environmentally friendly building energy-saving sound insulation material of the present invention uses modified polyether polyol and isocyanate to prepare rigid foamed polyurethane material, and adds modified hollow glass microspheres, modified sericite and ammonium polyphosphate, so that the material has excellent heat insulation and flame retardant properties, and also has good mechanical properties. The modified polyether polyol uses phosphorus oxychloride as a coupling agent, and by chemical grafting, the phase change energy storage material polyethylene glycol is embedded in the polyether polyol in a block manner, so that the polyether polyol has a good phase change energy storage function, and the foaming material prepared by combining it with isocyanate has the effect of energy storage and thermal insulation, and the introduction of flame retardant element phosphorus improves the flame retardant properties of the polyether polyol. The modified hollow glass microspheres improve the interface bonding between the hollow glass microspheres and the polymer matrix by a composite coupling agent, one end of the coupling agent molecule is connected to the hollow glass microspheres by chemical reaction, and the lipophilic group at the other end is cured and cross-linked with the active group of the polymer matrix to form a stable three-dimensional cross-linked network, thereby improving the tensile strength of the material to a certain extent. On the other hand, hollow glass microspheres are an inorganic non-metallic material, and the hollow part is a spherical particle filled with an inert gas. It has the characteristics of light weight, low density, and low thermal conductivity. The hollow glass microspheres are evenly dispersed in the polymer matrix, which can further reduce the thermal insulation effect of the material. The sericite is modified by intercalation of triazine flame retardant, wherein the triazine flame retardant is a triazine derivative containing a siloxane structure and a DOPO structure, rich in N, P, and Si elements, which promotes the dehydration and carbonization of the polymer during thermal cracking, and forms a carbonaceous protective layer of Si-O and Si-C. At the same time, the DOPO group also has a good gas phase flame retardant effect. The modified sericite is then compounded with ammonium polyphosphate for flame retardancy. Several effects promote each other and can give the material good flame retardant properties. In addition, through the intercalation modification of the triazine flame retardant, the interlayer spacing of the sericite can be increased, and at the same time, organic groups are given, which improves the dispersibility of the sericite in the material. DETAILED DESCRIPTION
[0029] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0030] Example 1
[0031] A modified polyether polyol, wherein the modified polyether polyol is a polyether polyol containing phosphorus and a phase change energy storage segment, and the preparation method thereof comprises the following steps:
[0032] (1) Add 0.2 mol of polyethylene glycol 800 to 30 ml of tetrahydrofuran and stir to dissolve to obtain solution A, add 0.1 mol of phosphorus oxychloride to 20 ml of n-hexane and dissolve to obtain solution B, slowly dropwise add solution B to solution A, stir evenly and let stand for 2 hours;
[0033] (2) The reaction system was slowly heated to 95° C., and 0.1 mol of polyether polyol 4110 was slowly added while stirring. After the addition was completed, the reaction was kept warm for 2 h to obtain a modified polyether polyol.
[0034] Example 2
[0035] A modified hollow glass microsphere, wherein the modified hollow glass microsphere is a hollow glass microsphere surface-modified by a composite coupling agent, and the preparation method thereof comprises the following steps:
[0036] a. Mix 3.1 g of silane coupling agent γ-aminopropyltriethoxysilane and 2.0 g of γ-mercaptopropyltrimethoxysilane, and then add them into 100 ml of ethanol aqueous solution with a volume ratio of 9:1;
[0037] b. Add 10.5 g of hollow glass microspheres into the hydrolyzed silane aqueous solution and stir the reaction at 60°C for 4 h;
[0038] c. After the reaction is completed, the modified hollow glass microspheres are obtained by repeatedly washing with deionized water and ethanol for 3 to 5 times, and then filtering under reduced pressure, and then filtering under reduced pressure and drying.
[0039] Example 3
[0040] A modified sericite mica, wherein the modified sericite mica is a triazine flame retardant intercalated modified sericite mica, wherein the triazine flame retardant is a triazine derivative containing a siloxane structure and a DOPO structure, and a preparation method of the modified sericite mica comprises the following steps:
[0041] A. Add 4.8g of p-hydroxybenzaldehyde and 0.5g of sodium carbonate into 50ml of acetone, stir to mix thoroughly, then add 3.6g of cyanuric chloride, slowly heat to 55°C, reflux for 5h, cool to room temperature after the reaction, filter under reduced pressure, wash with water 3-5 times, and dry to obtain a white powder product A;
[0042] B. Add 4.4 g of 3-aminopropyltriethoxysilane, 20 ml of triethylamine and 40 ml of tetrahydrofuran into a reactor, stir to mix thoroughly, then add product A, slowly raise the temperature to 55° C., reflux for 5 h, evaporate and filter to remove tetrahydrofuran and triethylamine hydrochloride, add ethyl acetate to the separated organic phase, dry and filter, and distill the filtrate under reduced pressure to obtain product B;
[0043] C. Add 8.6 g of DOPO to 80 ml of 1,2-dichloroethane, stir and heat to 85° C. After DOPO is completely dissolved, slowly add product B, keep the system temperature at 85° C., and reflux for 5 hours. After the reaction is completed, reduce the pressure and filter, then wash with 1,2-dichloroethane for 3 to 5 times to remove excess DOPO. After washing, dry and dry to obtain the triazine flame retardant;
[0044] D. Add 5.1 g of sericite to a mixture of 55 ml of anhydrous ethanol and 5 ml of distilled water, and disperse by ultrasonication for 12 min. Adjust the pH value of the solution to 4 with aqueous hydrochloric acid solution. Then slowly add 3.2 g of triazine flame retardant to the sericite dispersion, and disperse by ultrasonication for 8 min. Heat to 70 °C and keep the reaction for 4 h. After cooling, filter, wash, and dry to obtain the modified sericite.
[0045] Example 4
[0046] An environmentally friendly building energy-saving sound-insulating material comprises the following raw materials in parts by weight: 100 parts of modified polyether polyol, 150 parts of isocyanate, 8 parts of modified hollow glass microspheres, 8 parts of modified sericite, 3 parts of ammonium polyphosphate, 4 parts of blowing agent HFC 245fa, 1 part of stabilizer L6900, 0.2 parts of pentamethyldiethylenetriamine, and 0.3 parts of dimethylcyclohexylamine; the modified polyether polyol is the polyether polyol containing phosphorus and phase change energy storage segments prepared in Example 1, the modified hollow glass microspheres are the composite coupling agent surface-modified hollow glass microspheres prepared in Example 2, and the modified sericite is the triazine flame retardant intercalated modified sericite prepared in Example 3. Modified sericite
[0047] The preparation method of the environmentally friendly building energy-saving sound insulation material comprises the following steps:
[0048] S1. According to the formula ratio, weigh the modified polyether polyol, pentamethyldiethylenetriamine, dimethylcyclohexylamine, stabilizer L6900 and water, mix them, stir them at high speed for 12 minutes, then mix the modified hollow glass microspheres, modified sericite and ammonium polyphosphate together, pour them into the mixture, and stir them at high speed for 10 minutes;
[0049] S2, adding blowing agent HFC 245fa, stirring at high speed for 1.5 minutes, then adding isocyanate, stirring at high speed for 8-10 seconds, quickly pouring the obtained mixture into the prepared mold, ripening at 110° C. for 5 hours, and foaming to obtain the environmentally friendly building energy-saving sound insulation material.
[0050] Example 5
[0051] An environmentally friendly building energy-saving sound-insulating material comprises the following raw materials in parts by weight: 120 parts of modified polyether polyol, 140 parts of isocyanate, 12 parts of modified hollow glass microspheres, 5 parts of modified sericite, 5 parts of ammonium polyphosphate, 2 parts of blowing agent HFC365 / 227, 2 parts of stabilizer L6100, 1 part of stabilizer DC193, and 0.1 part of 2-hydroxy-N,N,N-trimethyl-1-propylamine formate; the modified polyether polyol is the polyether polyol containing phosphorus and phase change energy storage segments prepared in Example 1, the modified hollow glass microspheres are the composite coupling agent surface-modified hollow glass microspheres prepared in Example 2, and the modified sericite is the triazine flame retardant intercalated modified sericite prepared in Example 3.
[0052] The preparation method of the environmentally friendly building energy-saving sound insulation material comprises the following steps:
[0053] S1. According to the formula ratio, weigh the modified polyether polyol, 2-hydroxy-N,N,N-trimethyl-1-propylamine formate, stabilizer L6100, stabilizer DC193 and water, stir at high speed for 10 minutes, then mix the modified hollow glass microspheres, modified sericite and ammonium polyphosphate together, pour into the mixture, and stir at high speed for 10 minutes;
[0054] S2, adding blowing agent HFC365 / 227, stirring at high speed for 1 minute, then adding isocyanate, stirring at high speed for 8 seconds, quickly pouring the obtained mixture into the prepared mold, ripening at 20° C. for 4 hours, and foaming to obtain the environmentally friendly building energy-saving sound insulation material.
[0055] Example 6
[0056] An environmentally friendly building energy-saving sound-insulating material comprises the following raw materials in parts by weight: 110 parts of modified polyether polyol, 145 parts of isocyanate, 10 parts of modified hollow glass microspheres, 6 parts of modified sericite, 4 parts of ammonium polyphosphate, 1 part of blowing agent HFO 1233zd, 2 parts of blowing agent HFO 1336mzz, 2 parts of stabilizer B8462, and 0.3 parts of bis(dimethylaminoethyl) ether; the modified polyether polyol is the polyether polyol containing phosphorus and phase change energy storage segments prepared in Example 1, the modified hollow glass microspheres are the composite coupling agent surface-modified hollow glass microspheres prepared in Example 2, and the modified sericite is the triazine flame retardant intercalated modified sericite prepared in Example 3.
[0057] The preparation method of the environmentally friendly building energy-saving sound insulation material comprises the following steps:
[0058] S1. According to the formula ratio, weigh the modified polyether polyol, potassium acetate and bis(dimethylaminoethyl) ether, stabilizer B8462 and water, mix them, stir them at high speed for 10 minutes, then mix the modified hollow glass microspheres, modified sericite and ammonium polyphosphate together, pour them into the mixture, and stir them at high speed for 10 minutes;
[0059] S2, adding blowing agent HFO 1233zd and blowing agent HFO 1336mzz, stirring at high speed for 2 minutes, then adding isocyanate, stirring at high speed for 10 seconds, quickly pouring the obtained mixture into the prepared mold, ripening at 100° C. for 6 hours, and foaming to obtain the environmentally friendly building energy-saving sound insulation material.
[0060] Comparative Example 1
[0061] An environmentally friendly building energy-saving sound-insulating material comprises the following raw materials in parts by weight: 110 parts of polyether polyol, 145 parts of isocyanate, 10 parts of modified hollow glass microspheres, 6 parts of modified sericite, 4 parts of ammonium polyphosphate, 1 part of blowing agent HFO 1233zd, 2 parts of blowing agent HFO 1336mzz, 2 parts of stabilizer B8462, and 0.3 parts of bis(dimethylaminoethyl) ether; the polyether polyol is the unmodified polyether polyol added in step (2) of Example 1, the modified hollow glass microspheres are the composite coupling agent surface-modified hollow glass microspheres prepared in Example 2, and the modified sericite is the triazine flame retardant intercalated modified sericite prepared in Example 3.
[0062] The preparation method of the above-mentioned environmentally friendly building energy-saving sound insulation material is the same as that of Example 6.
[0063] Comparative Example 2
[0064] An environmentally friendly building energy-saving sound-insulating material comprises the following raw materials in parts by weight: 110 parts of modified polyether polyol, 145 parts of isocyanate, 6 parts of modified sericite, 4 parts of ammonium polyphosphate, 1 part of blowing agent HFO 1233zd, 2 parts of blowing agent HFO 1336mzz, 2 parts of stabilizer B8462, and 0.3 part of bis(dimethylaminoethyl) ether; the modified polyether polyol is the polyether polyol containing phosphorus and phase change energy storage segments prepared in Example 1, and the modified sericite is the triazine flame retardant intercalated modified sericite prepared in Example 3.
[0065] The preparation method of the above-mentioned environmentally friendly building energy-saving sound insulation material is the same as that of Example 6.
[0066] Comparative Example 3
[0067] An environmentally friendly building energy-saving sound-insulating material comprises the following raw materials in parts by weight: 110 parts of modified polyether polyol, 145 parts of isocyanate, 10 parts of modified hollow glass microspheres, 4 parts of ammonium polyphosphate, 1 part of blowing agent HFO 1233zd, 2 parts of blowing agent HFO1336mzz, 2 parts of stabilizer B8462, and 0.3 parts of bis(dimethylaminoethyl) ether; the modified polyether polyol is the polyether polyol containing phosphorus and phase change energy storage segments prepared in Example 1, and the modified hollow glass microspheres are the hollow glass microspheres surface-modified by a composite coupling agent prepared in Example 2.
[0068] The preparation method of the above-mentioned environmentally friendly building energy-saving sound insulation material is the same as that of Example 6.
[0069] Performance Testing
[0070] 1. Flame retardant performance test
[0071] The environmentally friendly building energy-saving sound insulation materials in Examples 4 to 6 and Comparative Examples 1 to 3 were tested for the limiting oxygen index of RPUF and RPUF / EG composite materials using an oxygen index meter according to ASTMD2863 standard, and the sample size was 127mm×10mm×10mm; the vertical combustion level was tested using a horizontal vertical combustion tester according to ASTM-D3801:2010 standard, and the sample size was 127mm×13mm×10mm. Combustion behavior: A micro combustion calorimeter was used to test the combustion performance of the composite material according to ASTM D7309:2007 standard, the sample mass was 5-10mg, the heating rate was 1℃ / s, and the temperature range was 100-650℃. The data obtained are shown in Table 1 below.
[0072] Table 1 Flame retardant properties of environmentally friendly building energy-saving sound insulation materials
[0073]
[0074] It can be seen from the data in Table 1 that due to the lack of modified sericite, the flame retardant performance of the environmentally friendly building energy-saving sound insulation material prepared in Comparative Example 3 is significantly worse than that of other groups. In Examples 4 to 6 of the present invention and Comparative Examples 1 to 2, triazine flame retardant intercalation modified sericite is added, wherein the triazine flame retardant is a triazine derivative containing a siloxane structure and a DOPO structure, rich in N, P, and Si elements, which promotes polymer dehydration and carbonization during thermal cracking, and forms a carbonaceous protective layer of Si-O and Si-C. At the same time, the DOPO group also has a good gas phase flame retardant effect, and then the modified sericite is compounded with ammonium polyphosphate for flame retardancy, and several effects promote each other, which can give the material good flame retardant performance. And through the intercalation modification of the triazine flame retardant, the interlayer spacing of the sericite can be increased, and at the same time, the organic group is given, which improves the dispersibility of the sericite in the material.
[0075] 2. Mechanical properties and thermal insulation performance test
[0076] The environmentally friendly building energy-saving sound insulation materials prepared in Examples 3 to 5 and Comparative Examples 1 to 2 were cut into test specimens and subjected to mechanical property tests using a universal testing machine. Referring to GB / T 528-2009, the molded specimens were cut into 25 mm × 4 mm dumbbell-shaped tensile specimens with a tensile rate of 20 mm / min. The thermal conductivity of the samples was tested using a thermal conductivity tester. The data obtained are shown in Table 2.
[0077] Table 2 Mechanical properties of environmentally friendly building energy-saving sound insulation materials
[0078]
[0079] It can be seen from the data in Table 2 that the mechanical properties of the materials in Comparative Examples 2 and 3 are worse than those in other groups. In Comparative Example 2, no modified hollow glass microspheres are added, and in Comparative Example 3, no modified sericite is added. Both hollow glass microspheres and sericite have a toughening effect. After modification, they can be evenly dispersed in the polymer matrix to better play a toughening role. The thermal insulation effect of the materials in Comparative Examples 1 and 2 is reduced. In Comparative Example 1, no modified polyether polyol is added. The modified polyether polyol of the present invention uses phosphorus oxychloride as a coupling agent, and embeds the phase change energy storage material polyethylene glycol into polyether polyol 4110 by chemical grafting, so that the polyether polyol has a good phase change energy storage function, and the prepared material has the effect of energy storage and thermal insulation, so the thermal insulation effect in Comparative Example 1 is reduced; at the same time, the introduction of the flame retardant element phosphorus improves the flame retardant properties of the polyether polyol, so in the flame retardant performance test, the flame retardant properties of Comparative Example 1 are reduced compared with Examples 4 to 6. In Comparative Example 2, no modified hollow glass is added. The present invention uses a composite coupling agent to improve the interface bonding between the hollow glass microspheres and the polymer matrix. One end of the coupling agent molecule is connected to the hollow glass microspheres through a chemical reaction, and the lipophilic group at the other end is cured and cross-linked with the active group of the polymer matrix to form a stable three-dimensional cross-linked network, thereby improving the tensile strength of the material to a certain extent. On the other hand, the hollow glass microspheres are an inorganic non-metallic material, and the hollow part has spherical particles filled with inert gas, which has the characteristics of light weight, low density, low thermal conductivity, etc. The hollow glass microspheres are evenly dispersed in the polymer matrix, which can further reduce the thermal insulation effect of the material.
[0080] The above shows and describes the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments, and the above embodiments and descriptions are only for explaining the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, and these changes and improvements all fall within the scope of the present invention to be protected.
Claims
1. An environmentally friendly building energy-saving sound insulation material, characterized in that: The invention comprises the following raw materials in parts by weight: 100-120 parts of modified polyether polyol, 140-150 parts of isocyanate, 8-12 parts of modified hollow glass microspheres, 5-8 parts of modified sericite, 3-5 parts of ammonium polyphosphate, 2-4 parts of foaming agent, 1-3 parts of stabilizer and 0.1-0.5 parts of catalyst; The modified polyether polyol is a polyether polyol containing phosphorus and phase change energy storage segments, the modified hollow glass microspheres are hollow glass microspheres surface-modified by a composite coupling agent, the modified sericite is a triazine flame retardant intercalated modified sericite, and the triazine flame retardant is a triazine derivative containing a siloxane structure and a DOPO structure, and its structural formula is as follows:
2. The environmentally friendly building energy-saving sound insulation material according to claim 1, characterized in that: The catalyst is selected from one or more of pentamethyldiethylenetriamine, dimethylcyclohexylamine, 2-hydroxy-N,N,N-trimethyl-1-propylamine formate, potassium acetate and bis(dimethylaminoethyl) ether.
3. The environmentally friendly building energy-saving sound insulation material according to claim 1, characterized in that: The preparation method of the modified polyether polyol comprises the following steps: (1) adding polyethylene glycol to tetrahydrofuran and stirring to dissolve to obtain solution A, adding phosphorus oxychloride to n-hexane and dissolving to obtain solution B, slowly dropping solution B into solution A, stirring evenly and then standing for 1 to 2 hours; (2) slowly heating the reaction system to 90-100° C., slowly adding the polyether polyol while stirring, and keeping the temperature to react for 1-2 hours after the addition is completed to obtain a modified polyether polyol.
4. The environmentally friendly building energy-saving sound insulation material according to claim 3, characterized in that: The molar ratio of the polyethylene glycol, phosphorus oxychloride and polyether polyol is 2:1:
1.
5. The environmentally friendly building energy-saving sound insulation material according to claim 1, characterized in that: The preparation method of the modified hollow glass microspheres comprises the following steps: a. Mix silane coupling agents γ-aminopropyltriethoxysilane and γ-mercaptopropyltrimethoxysilane in a mass ratio of 3:2, and then add them into an ethanol aqueous solution in a volume ratio of 9:1; b. Add the hollow glass microspheres into the hydrolyzed silane aqueous solution and stir the reaction at 60°C for 3 to 5 hours; c. After the reaction is completed, the modified hollow glass microspheres are obtained by repeatedly washing with deionized water and ethanol for 3 to 5 times, then filtering under reduced pressure, and then filtering under reduced pressure and drying.
6. The environmentally friendly building energy-saving sound insulation material according to claim 1, characterized in that: The preparation method of the modified sericite comprises the following steps: A. Add p-hydroxybenzaldehyde and sodium carbonate to acetone, stir to mix thoroughly, then add cyanuric chloride, slowly heat to 50-60°C, reflux for 4-6 hours, cool to room temperature after the reaction, filter under reduced pressure, wash with water 3-5 times, and dry to obtain a white powder product A; B. Add 3-aminopropyltriethoxysilane, triethylamine and tetrahydrofuran into a reactor, stir to fully mix, then add product A, slowly raise the temperature to 50-60°C, reflux for 4-6 hours, evaporate and filter to remove tetrahydrofuran and triethylamine hydrochloride, add ethyl acetate to the separated organic phase, dry and filter, and distill the filtrate under reduced pressure to obtain product B; C. Add DOPO to 1,2-dichloroethane, stir and heat to 85°C. After DOPO is completely dissolved, slowly add product B, keep the system temperature at 85°C, and reflux for 4 to 6 hours. After the reaction is completed, reduce pressure and filter, then wash with 1,2-dichloroethane 3 to 5 times to remove excess DOPO. After washing, dry and dry to obtain the triazine flame retardant; D. Add sericite to a mixture of anhydrous ethanol and distilled water, and disperse by ultrasonication for 10 to 15 minutes. Adjust the pH value of the solution to 4 with aqueous hydrochloric acid solution. Then slowly add triazine flame retardant to the sericite dispersion, and disperse by ultrasonication for 5 to 10 minutes. Heat to 60 to 80°C and keep the temperature for reaction for 3 to 5 hours. After cooling, filter, wash and dry to obtain modified sericite.
7. The environmentally friendly building energy-saving sound-insulating material according to claim 1, characterized in that: The molar ratio of cyanuric chloride, p-hydroxybenzaldehyde, 3-aminopropyltriethoxysilane and DOPO is 1:2:1:
2.
8. A method for preparing an environmentally friendly building energy-saving sound-insulating material, wherein the environmentally friendly building energy-saving sound-insulating material is as described in any one of claims 1 to 7, characterized in that: The following steps are involved: S1. According to the formula ratio, weigh the modified polyether polyol, catalyst, stabilizer and water, mix them, stir them at high speed for 10 to 15 minutes, mix the modified hollow glass microspheres, modified sericite and ammonium polyphosphate together, pour them into the mixture, and stir them at high speed for 10 minutes; S2, adding a foaming agent, stirring at high speed for 1 to 2 minutes, then adding isocyanate, stirring at high speed for 8 to 10 seconds, quickly pouring the obtained mixture into a prepared mold, and ripening at 100 to 120° C. for 4 to 6 hours to foam the environmentally friendly building energy-saving sound insulation material.
Citation Information
Patent Citations
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