An environment-friendly building energy-saving sound insulation material and its preparation method
Through the combination of modified polyether polyol, modified hollow glass microbeads and triazine flame retardant interlayer modified sericite, the problems of insufficient flame retardant performance and poor mechanical properties of rigid polyurethane foam insulation materials are solved, and high-efficiency heat insulation, flame retardant and mechanical properties are improved.
Patent Information
- Application Number
- CN202411363347.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-27
- Publication Date
- 2025-07-11
- Estimated Expiration
- 2044-09-27
AI Technical Summary
The existing rigid polyurethane foam insulation materials have the disadvantages of insufficient flame retardant performance, poor dispersion, and great impact on the physical properties of the materials. The traditional flame retardant modification methods are cheap but have limited effects, making it difficult to take into account both flame retardant performance and mechanical properties.
The rigid foamed polyurethane material is prepared by using modified polyether polyols and isocyanate. Modified hollow glass microbeads, modified sericite and ammonium polyphosphate are added. Modified by chemical grafting and coupling agent, and modified sericite is combined with triazine flame retardant intercalation to form a stable three-dimensional crosslinking network to improve the flame retardant and mechanical properties of the material.
It achieves excellent heat insulation and flame retardant properties of the material, and also has good mechanical properties, reducing the thermal conductivity and improving the dispersion and flame retardant effect of the material.
Smart Images

Figure QLYQS_1 
Figure BDA0005065469590000021 
Figure BDA0005065469590000101
Abstract
Description
Technical Field
[0001] The present invention belongs to the field of building materials, and particularly relates to an environment-friendly building energy-saving sound insulation material and a preparation method thereof. Background Technique
[0002] With the development of urbanization construction, the building area increases at a high speed 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 to solve the energy consumption problem. A phase change material is a substance that can store or release latent heat in an almost isothermal manner and has a very high energy storage density. People classify the phase change material with a very high energy storage density as a latent heat thermal energy storage material, which is suitable for thermal energy storage applications. In addition to storing thermal energy, the phase change material can also generate a heat regulation effect on the building components where it is located by releasing a large amount of latent heat during the phase change process. Currently, the most commonly used thermal insulation material in building envelopes is rigid polyurethane foam to ensure the internal insulation of buildings.
[0003] Rigid polyurethane foam has inherent flammability, 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 gases, resulting in serious casualties and economic losses. Therefore, researchers have continuously carried out flame retardant modification on rigid polyurethane thermal insulation materials. By adding various functional flame retardants, the flame retardant performance of rigid polyurethane thermal insulation materials is improved, and a new type of rigid polyurethane thermal insulation material with low cost, small thermal conductivity, good thermal insulation performance and excellent flame retardant performance is prepared, so as to effectively prevent fire, ensure safety, and have heat insulation. Flame retardant rigid polyurethane foam has disadvantages such as a large addition amount, poor dispersion, and a great influence on the physical properties of the material. Therefore, it is necessary to develop a new type of building energy-saving material that takes into account both flame retardant performance and mechanical properties. Summary of the Invention
[0004] To solve the deficiencies mentioned in the above background technique, the purpose of the present invention is to provide an environment-friendly building energy-saving sound insulation material and a preparation method thereof. Rigid foamed polyurethane material is prepared with modified polyether polyol and isocyanate, and modified hollow glass microspheres, modified sericite and ammonium polyphosphate are added to make the material have excellent heat insulation and flame retardant properties, and at the same time have good mechanical properties.
[0005] The purpose of the present invention can be achieved through the following technical solutions:
[0006] An environment-friendly building energy-saving sound insulation material, comprising 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, 0.1-0.5 part 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, 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 mix them thoroughly, then add product A, slowly heat up to 50 - 60 °C, and reflux for 4 - 6 h. Evaporate and filter to remove tetrahydrofuran and triethylamine hydrochloride. Add ethyl acetate to the separated organic phase, dry and then filter. After distilling the filtrate under reduced pressure, product B is obtained.
[0021] C. Add DOPO into 1,2-dichloroethane, stir and heat up to 85 °C. After DOPO is completely dissolved, slowly add product B, keep the system temperature at 85 °C, and reflux for 4 - 6 h. After the reaction is completed, filter under reduced pressure, and then wash with 1,2-dichloroethane for 3 - 5 times to remove the excessive DOPO. After washing, dry to obtain the triazine flame retardant.
[0022] D. Add sericite into the mixed solution of absolute ethanol and distilled water, ultrasonically disperse for 10 - 15 min, adjust the pH of the solution to 4 with hydrochloric acid aqueous solution, then slowly add the triazine flame retardant into the sericite dispersion, ultrasonically disperse for 5 - 10 min, heat to 60 - 80 °C and keep the temperature for reaction for 3 - 5 h. After cooling, filter, wash, and dry to obtain the modified sericite.
[0023] Further preferably, the molar ratio of cyanuric chloride, p-hydroxybenzaldehyde, 3-aminopropyltriethoxysilane, and DOPO is 1:2:1:2.
[0024] A preparation method of an environment-friendly building energy-saving sound insulation material includes the following steps:
[0025] S1. Weigh modified polyether polyol, catalyst, stabilizer, and water according to the formula ratio, mix them, and stir at high speed for 10 - 15 min. Then mix modified hollow glass microspheres, modified sericite, and ammonium polyphosphate together, pour them into the mixed solution, and stir at high speed for 10 min.
[0026] S2. Add a foaming agent, stir at high speed for 1 - 2 min, then add isocyanate, stir at high speed for 8 - 10 s, quickly pour the obtained mixture into a prepared mold, and cure at 100 - 120 °C for 4 - 6 h to foam and obtain the environment-friendly building energy-saving sound insulation material.
[0027] The beneficial effects of the present invention:
[0028] The environmentally friendly building energy-saving sound insulation material of the present invention prepares a rigid foamed polyurethane material from a modified polyether polyol and an isocyanate, and adds modified hollow glass microspheres, modified sericite and ammonium polyphosphate, so that the material has excellent heat insulation and flame retardant properties, and at the same time has good mechanical properties. Among them, the modified polyether polyol uses phosphorus oxychloride as a coupling agent, and through chemical grafting, the phase change energy storage substance 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. Preparing a foamed material with isocyanate has the effects of energy storage, heat preservation and heat insulation. At the same time, the introduction of the flame retardant element phosphorus improves the flame retardant performance of the polyether polyol. The modified hollow glass microspheres improve the interfacial bonding between the hollow glass microspheres and the polymer matrix through a composite coupling agent. 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 crosslinked with the active group of the polymer matrix to form a stable three-dimensional crosslinked 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, which are spherical particles filled with inert gas in the hollow part. They have the characteristics of light weight, low density and low thermal conductivity. When the hollow glass microspheres are uniformly dispersed in the polymer matrix, the heat insulation effect of the material can be further reduced. The sericite is modified by intercalation with a triazine flame retardant. The triazine flame retardant is a triazine derivative containing a siloxane structure and a DOPO structure. The rich N, P, and Si elements promote the dehydration and carbonization of the polymer during pyrolysis, and at the same time form 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. Then, the modified sericite is compounded with ammonium polyphosphate for flame retardancy, and several effects promote each other, which can endow the material with good flame retardant properties. And through the intercalation modification of the triazine flame retardant, the layer spacing of the sericite can be increased, and at the same time, organic groups are imparted, which improves the dispersibility of the sericite in the material. Detailed Embodiments
[0029] The following will combine 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 a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative work belong to the protection scope of the present invention.
[0030] Example 1
[0031] A modified polyether polyol, the modified polyether polyol is a polyether polyol containing phosphorus and a phase change energy storage chain segment, and its preparation method includes 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 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, 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 up to 85 °C. After DOPO is completely dissolved, slowly add product B, keep the system temperature at 85 °C, reflux for 5 h. After the reaction is completed, filter under reduced pressure, and then wash with 1,2-dichloroethane 3 - 5 times to remove the excessive DOPO. After washing, dry it to obtain the triazine flame retardant;
[0044] D. Add 5.1 g of sericite to a mixed solution of 55 ml of absolute ethanol and 5 ml of distilled water, ultrasonically disperse for 12 min, adjust the pH of the solution to 4 with hydrochloric acid aqueous solution, then slowly add 3.2 g of triazine flame retardant to the sericite dispersion, ultrasonically disperse for 8 min, heat to 70 °C and keep the reaction for 4 h. After cooling, filter, wash and dry to obtain modified sericite.
[0045] Example 4
[0046] An environmentally friendly building energy-saving sound insulation material, comprising 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 foaming agent HFC 245fa, 1 part of stabilizer L6900, 0.2 part of pentamethyldiethylenetriamine, 0.3 part 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 above-mentioned environmentally friendly building energy-saving sound insulation material comprises the following steps:
[0048] S1. Weigh the modified polyether polyol, pentamethyldiethylenetriamine, dimethylcyclohexylamine, stabilizer L6900 and water according to the formula ratio, mix them, and stir at high speed for 12 min. Then mix the modified hollow glass microspheres, modified sericite and ammonium polyphosphate together, pour them into the mixed solution, and stir at high speed for 10 min;
[0049] S2. Add the foaming agent HFC 245fa, stir at high speed for 1.5 min, then add the isocyanate, stir at high speed for 8 - 10 s, quickly pour the obtained mixture into the prepared mold, and cure at 110 °C for 5 h to foam to obtain the environmentally friendly building energy-saving sound insulation material.
[0050] Example 5
[0051] An environmentally friendly building energy-saving sound insulation material, comprising 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-propanamine formate; the modified polyether polyol is a polyether polyol containing phosphorus and phase change energy storage segments prepared in Example 1, the modified hollow glass microspheres are hollow glass microspheres surface-modified with a composite coupling agent prepared in Example 2, and the modified sericite is sericite intercalation-modified with a triazine flame retardant prepared in Example 3.
[0052] The preparation method of the above-mentioned 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-propanamine formate, stabilizer L6100, stabilizer DC193 and water and mix them. After high-speed stirring for 10 min, mix the modified hollow glass microspheres, modified sericite and ammonium polyphosphate together, pour them into the mixed solution, and stir at high speed for 10 min;
[0054] S2. Add the blowing agent HFC365 / 227, stir at high speed for 1 min, then add isocyanate, stir at high speed for 8 s, quickly pour the obtained mixture into a prepared mold, and cure at 20 °C for 4 h to foam the environmentally friendly building energy-saving sound insulation material.
[0055] Example 6
[0056] An environmentally friendly building energy-saving sound insulation material, comprising 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 part of bis(dimethylaminoethyl)ether; the modified polyether polyol is a polyether polyol containing phosphorus and phase change energy storage segments prepared in Example 1, the modified hollow glass microspheres are hollow glass microspheres surface-modified with a composite coupling agent prepared in Example 2, and the modified sericite is sericite intercalation-modified with a triazine flame retardant prepared in Example 3.
[0057] The preparation method of the above-mentioned 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 and mix them. After high-speed stirring for 10 min, mix the modified hollow glass microspheres, modified sericite and ammonium polyphosphate together, pour them into the mixed solution, and stir at high speed for 10 min;
[0059] S2. Add blowing agent HFO 1233zd and blowing agent HFO 1336mzz, stir at high speed for 2 min, then add isocyanate and stir at high speed for 10 s. Pour the obtained mixture quickly into the prepared mold and cure at 100 °C for 6 h to foam the environmentally friendly building energy-saving sound insulation material.
[0060] Comparative Example 1
[0061] An environmentally friendly building energy-saving sound insulation material, comprising 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, 0.3 part 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 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 insulation material, comprising 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, 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 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 insulation material, comprising 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 HFO 1336mzz, 2 parts of stabilizer B8462, 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 hollow glass microspheres are the composite coupling agent surface-modified hollow glass microspheres prepared in Example 2.
[0068] The preparation method of the above-mentioned environment-friendly building energy-saving sound insulation material is the same as that in Example 6.
[0069] Performance testing
[0070] I. Flame retardancy performance test
[0071] The limiting oxygen index of RPUF and RPUF / EG composites of the environment-friendly building energy-saving sound insulation materials in Examples 4-6 and Comparative Examples 1-3 was tested by an oxygen index meter according to the ASTM D2863 standard, and the sample size was 127 mm × 10 mm × 10 mm; the vertical burning level was tested by a horizontal and vertical burning tester according to the ASTM-D3801:2010 standard, and the sample size was 127 mm × 13 mm × 10 mm. Combustion behavior: The combustion performance of the composite material was tested by a micro combustion calorimeter according to the ASTM D7309:2007 standard, the sample mass was 5-10 mg, the heating rate was 1 °C / s, and the temperature range was 100-650 °C. The obtained data are shown in Table 1 below.
[0072] Table 1 Flame retardancy performance of environment-friendly building energy-saving sound insulation materials
[0073]
[0074] It can be seen from the data in Table 1 that due to the absence of modified sericite, the flame retardancy performance of the environment-friendly building energy-saving sound insulation material prepared in Comparative Example 3 is significantly worse than that of other groups. In Examples 4-6 of the present invention and Comparative Examples 1-2, triazine flame retardant intercalated modified sericite was added. The triazine flame retardant is a triazine derivative containing a siloxane structure and a DOPO structure. The rich N, P, and Si elements promote the dehydration and carbonization of the polymer during pyrolysis, and at the same time form 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. Then, the modified sericite is compounded with ammonium polyphosphate for flame retardancy, and several effects promote each other, which can endow the material with good flame retardancy performance. And through the intercalation modification of the triazine flame retardant, the layer spacing of sericite can be increased, and at the same time, organic groups are endowed, improving the dispersibility of sericite in the material.
[0075] II. Mechanical properties and heat insulation performance test
[0076] The environment-friendly building energy-saving sound insulation materials prepared in Examples 3-5 and Comparative Examples 1-2 were cut into test specimens, and a universal testing machine was used for mechanical property testing. Referring to GB / T 528-2009, the molded specimens were cut into dumbbell-shaped tensile specimens of 25 mm × 4 mm, and the tensile rate was 20 mm / min. The thermal conductivity of the samples was tested by a thermal conductivity tester. The obtained data are shown in Table 2.
[0077] Table 2 Mechanical properties of environment-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 Example 2 and Comparative Example 3 are worse than those of other groups. In Comparative Example 2, modified hollow glass microspheres were not added, and in Comparative Example 3, modified sericite was not added. Both hollow glass microspheres and sericite have toughening effects. After modification, they can be evenly dispersed in the polymer matrix and better play the toughening role. The heat insulation effect of the materials in Comparative Example 1 and Comparative Example 2 decreased. In Comparative Example 1, modified polyether polyol was not added. In the present invention, the modified polyether polyol uses phosphorus oxychloride as a coupling agent, and by means of chemical grafting, the phase change energy storage substance polyethylene glycol is block-embedded into polyether polyol 4110, so that the polyether polyol has good phase change energy storage function, and the prepared material has energy storage and heat insulation effects. Therefore, the heat insulation effect decreased in Comparative Example 1. At the same time, the introduction of the flame retardant element phosphorus improved the flame retardant performance of the polyether polyol. Therefore, in the flame retardant performance test, the flame retardant performance of Comparative Example 1 was lower than that of Examples 4 to 6. Modified hollow glass was not added in Comparative Example 2. In the present invention, a composite coupling agent is used to improve the interfacial 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 crosslinked with the active group of the polymer matrix to form a stable three-dimensional crosslinked 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, which are spherical particles filled with inert gas in the hollow part. They have the characteristics of light weight, low density, and low thermal conductivity. When the hollow glass microspheres are evenly dispersed in the polymer matrix, the heat insulation effect of the material can be further reduced.
[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 by the above embodiments. What is described in the above embodiments and the specification only illustrates the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention will have various changes and improvements, and these changes and improvements all fall within the scope of the present invention claimed.
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, wherein 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) Add polyethylene glycol to tetrahydrofuran and stir to dissolve to obtain solution A, add phosphorus oxychloride to n-hexane and dissolve to obtain solution B, slowly drop solution B into solution A, stir evenly and let stand for 1 to 2 hours; (2) Slowly heat the reaction system to 90-100°C, slowly add the polyether polyol while stirring, and after the addition is completed, keep the temperature to react for 1-2 hours 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, wherein 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 3-5 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, and 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 heat 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 4-6 hours. After the reaction is completed, reduce pressure and filter, then wash with 1,2-dichloroethane 3-5 times to remove excess DOPO, and dry after washing to obtain the triazine flame retardant; D. Add sericite into the mixed solution of absolute ethanol and distilled water, ultrasonically disperse for 10 - 15 min, adjust the pH of the solution to 4 with hydrochloric acid aqueous solution, then slowly add the triazine flame retardant into the sericite dispersion, ultrasonically disperse for 5 - 10 min, heat to 60 - 80 °C and keep the reaction for 3 - 5 h, cool, filter, wash and dry to obtain the modified sericite.
7. The environmentally friendly building energy-saving sound insulation material according to claim 6, characterized in that The molar ratio of cyanuric chloride, p-hydroxybenzaldehyde, 3-aminopropyltriethoxysilane and DOPO is 1:2:1:
2.
8. A preparation method of an environment-friendly building energy-saving sound insulation material, wherein the environment-friendly building energy-saving sound insulation material is as described in any one of claims 1 to 7, characterized in that, It includes the following steps: S1. Weigh the modified polyether polyol, catalyst, stabilizer and water according to the formula ratio, mix them, and after high-speed stirring for 10 - 15 min, mix the modified hollow glass microspheres, modified sericite and ammonium polyphosphate together, pour them into the mixed solution, and stir at high speed for 10 min. S2. Add the foaming agent, stir at high speed for 1 - 2 min, then add the isocyanate, stir at high speed for 8 - 10 s, quickly pour the obtained mixture into the prepared mold, and cure at 100 - 120 °C for 4 - 6 h to foam and obtain the environmentally friendly building energy-saving sound insulation material.
Citation Information
Patent Citations
Phosphaphenanthrene flame-retardant compound containing s-triazine structure, and preparation and use thereof
CN101376665A
Anti-flaming phase-change energy storage, heat preservation and heat insulation material and preparation method thereof
CN106750174A