Phase-change temperature-controlled closed-cell foam insulation material and preparation method thereof

By using the high-closed-cell polyurethane wall phase-change microcapsule foaming structure and phase-change material to store heat in polyurethane foaming materials, the problems of poor insulation effect and insufficient compression rebound rate of traditional materials are solved, and more efficient insulation effect and material stability are achieved.

CN119775912APending Publication Date: 2025-04-08苏州环明新材料科技有限公司
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Patent Information

Application Number
CN202411903419.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-23
Publication Date
2025-04-08

AI Technical Summary

Technical Problem

The insufficient closed cell ratio of traditional polyurethane foaming materials leads to a reduced thermal insulation effect and insufficient compression rebound rate. The thickness decreases after long-term use, which cannot meet the high-power thermal insulation requirements.

Method used

The foamed structure of polyurethane wall material phase change microcapsules has a closed cell ratio of 93% to 98%, and the heat is stored through the phase change material to improve the heat insulation effect.

Benefits of technology

It significantly enhances the buffering and thermal insulation characteristics of the material by more than 20%, ensures the permanent compression rebound rate, improves the thermal insulation effect, and maintains the stability of the material.

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Abstract

The invention discloses a preparation method of a phase-change temperature-controlled closed-cell foaming thermal insulation material, comprising: removing water from polyester polyol and dissolving it in a dimethylformamide solvent, adding molten paraffin, dropping isocyanate, stirring and dispersing, adding a catalyst dibutyltin dilaurate, the polyol and the isocyanate form a polyurethane shell on the surface of the paraffin, emulsifying and dispersing polymerization to obtain a phase-change microcapsule emulsion of a polyurethane wall material, purifying the phase-change microcapsules of the polyurethane wall material; adding the phase-change microcapsules of the polyurethane wall material to a polyether polyol, adding a catalyst, silicone oil, and deionized water to obtain a foaming agent component A; using isocyanate as a B component; fully mixing the A and B components until the solution is milky white, and then pouring them into a mold of a copper foil substrate for foaming to obtain a phase-change temperature-controlled closed-cell foaming thermal insulation material. The closed-cell foaming of the invention improves the thermal insulation effect and compression resilience; the high-H value phase-change microcapsule structure improves the heat storage capacity and the overall thermal insulation effect.
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Description

Technical Field

[0001] The invention relates to the technical field of polymer material preparation, and in particular to a phase-change temperature-controlled closed-cell foaming thermal insulation material and a preparation method thereof. Background Art

[0002] The traditional technical solution is to use polyurethane foaming technology on the surface of copper foil, to evenly distribute heat through the horizontal heat dissipation performance of copper foil, and to use polyurethane foaming for insulation, so as to achieve the uniform insulation function of the product; however, the closed-pore rate of the traditional polyurethane foam surface is 43% to 65%, and because of the insufficient closed-pore rate, air is easily expelled under pressure, and the insulation effect is greatly reduced. In addition, when the closed-pore rate is insufficient, the compression rebound rate of the material is insufficient. After long-term use, the thickness will be reduced due to compression, and the insulation effect will gradually deteriorate; when the heat source power is high, the product generates a large amount of heat, and the heat source temperature and the shell (or safety temperature) are quite different. Simple pore insulation cannot meet the insulation requirements, and the heat will also be transferred to the shell through the insulation layer, and as the heat increases, the insulation effect will be further reduced. Under the stable working state of the heat source, high-power insulation effect cannot be achieved.

[0003] Therefore, the present invention provides a phase-change temperature-controlled closed-cell foamed insulation material and a preparation method thereof, which adopts a special polymer aerogel microcapsule foaming structure with a closed-cell rate of 93% to 98%. A small foaming support structure is formed in the foaming hole, which can effectively enhance the buffering and thermal insulation properties by more than 20%. Heat is stored inside the microcapsule through a phase change material with a certain phase change point and a high heat value, thereby greatly increasing the uniform thermal insulation effect of the material. Summary of the invention

[0004] The purpose of the present invention is to provide a phase-change temperature-controlled closed-cell foamed thermal insulation material and a preparation method thereof, so as to fill the gap in the current technology.

[0005] The purpose of the present invention is achieved through the following technical solutions:

[0006] A method for preparing a phase-change temperature-controlled closed-cell foam insulation material comprises the following steps:

[0007] S1. Preparation of polyurethane wall material phase change microcapsules:

[0008] a. After drying and removing water, the polyester polyol is dissolved in dimethylformamide (DMF) solvent, stirred at high speed, and molten paraffin is added thereto, and the paraffin is wrapped by the polyol to form microsphere suspension droplets;

[0009] b. Control the temperature and stirring speed, add isocyanate dropwise, stir and disperse for 2 to 3 hours after complete addition; add catalyst dibutyltin dilaurate (DBTDL), slowly dropwise for 1 to 1.5 hours, under the action of the catalyst, polyol and isocyanate form a polyurethane shell on the surface of paraffin, emulsify and disperse polymerize for 12 to 16 hours to obtain a phase change microcapsule emulsion of polyurethane wall material;

[0010] c. filtering, separating and purifying the phase-change microcapsule emulsion of the polyurethane wall material obtained by polymerization to obtain the phase-change microcapsules of the polyurethane wall material;

[0011] S2. Preparation of phase-change temperature-controlled closed-cell foam insulation material:

[0012] d. Add the purified polyurethane wall material phase change microcapsules to polyether polyol, and add a catalyst, silicone oil, and deionized water, and stir and mix thoroughly to obtain a foaming agent component A;

[0013] e. Using isocyanate as component B;

[0014] f. Component A and component B are fully mixed and stirred until the solution becomes milky white, and then poured into a copper foil substrate mold for foaming. After the foaming is completed, the phase-change temperature-controlled closed-cell foamed insulation material can be obtained.

[0015] Preferably, in step a, the paraffin is encapsulated by polyol to form microsphere suspension droplets with a particle size of 10 to 20 microns.

[0016] Preferably, in step b, the controlled temperature is 80-100° C., and the stirring speed is 1000-1200 r / min; the isocyanate is selected from one of toluene diisocyanate (TDI), diphenylmethane diisocyanate (MDI) or isophorone diisocyanate (IPDI).

[0017] Preferably, in step c, the particle size of the phase change microcapsules of the obtained polyurethane wall material is 20 to 30 microns.

[0018] Preferably, in step d, the catalyst is selected from one of dibutyltin dilaurate (DBTDL) and triethylenediamine A33 (TEDA).

[0019] Preferably, in step e, the isocyanate is selected from one of diphenylmethane diisocyanate (MDI) and toluene diisocyanate (TDI) as component B.

[0020] The present application also claims protection for a phase-change temperature-controlled closed-cell foamed thermal insulation material, which is prepared by the preparation method of the phase-change temperature-controlled closed-cell foamed thermal insulation material.

[0021] Preferably, the phase-change temperature-controlled closed-cell foamed thermal insulation material comprises, from top to bottom, a first acrylic pressure-sensitive adhesive layer, a substrate layer (copper foil), a foamed thermal insulation layer, and a second acrylic pressure-sensitive adhesive layer.

[0022] Working mechanism of the present invention:

[0023] The invention adopts the method of polyurethane emulsion polymerization, a molten phase change material (paraffin) is added to a polyol solution for emulsification, the liquid paraffin is emulsified into suspended droplets with a particle size of 10 to 20 microns by high-speed stirring, a curing agent (TDI / MDI, etc.) and a catalyst (DBTDL) are added, and emulsion polymerization is carried out at 80 to 100° C. After the polymerization is completed, phase change microcapsules of polyurethane wall materials with a particle size of 20 to 30 microns are purified by filtering, purification and other processes; the phase change microcapsules of polyurethane wall materials are added to the polyurethane foam system by pure water foaming, and the microcapsule shell is consistent with the foam matrix, so the microcapsule has very good dispersibility; the polyurethane foam is foamed by mixing two components A and B, wherein the A component is a mixture of polyol, catalyst, silicone oil and water, and the B component is isocyanate, and a phase change temperature-controlled closed-cell foaming insulation material product is obtained after foaming.

[0024] Due to the application of the above technical solution, the present invention has the following beneficial effects compared with the prior art:

[0025] 1. The present invention adopts closed-cell polyurethane with microcapsule foaming structure, with a closed-cell rate of 93% to 98%. A small foaming support structure is formed in the foaming pores, which can effectively enhance the cushioning and heat insulation properties by more than 20%. In addition, the closed-cell structure can ensure permanent compression rebound rate, is not prone to thickness changes, and can ensure stability;

[0026] 2. The high enthalpy value of the phase change material can absorb and store most of the heat from the heat source. Based on the characteristics of the phase change material, the present invention adopts a phase change material with an enthalpy value of 35 to 50°C phase change point. During the heat absorption process, the temperature does not rise, which can reduce the temperature of the heat source to a greater extent, thereby improving the thermal insulation effect. The coating structure of the microcapsule not only improves the compatibility with the foaming matrix resin, but also ensures the seepage of the phase change material, thereby improving the stability of the overall material. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] In order to more clearly illustrate the specific implementation methods of the present invention or the technical solutions in the prior art, the drawings required for use in the specific implementation methods or the description of the prior art will be briefly introduced below. Obviously, some of the drawings described below are some implementation methods of the present invention. For ordinary technicians in this field, other drawings can be made based on these drawings without paying any creative work.

[0028] Figure 1This is a structural diagram of a phase-change temperature-controlled closed-cell foam insulation material according to Example 1 of the present invention;

[0029] Figure 2 Schematic diagram of closed-cell foaming of the thermal insulation layer of the phase-change temperature-controlled closed-cell foaming thermal insulation material of Example 1 of the present invention;

[0030] Figure 3 It is a comparison diagram of the closed-cell foaming technology of Example 1 of the present invention and the open-cell foaming technology of Comparative Example 1;

[0031] Figure 4 This is a diagram showing the thermal insulation effect of the phase-change temperature-controlled uniform thermal insulation material of Example 1 of the present invention;

[0032] Figure 5 This is a heat insulation effect diagram of the common heat insulation material of Comparative Example 1 of the present invention;

[0033] in, Figure 1 Middle: 1. Acrylic pressure-sensitive adhesive layer 1; 2. Base material layer; 3. Foam insulation layer; 4. Acrylic pressure-sensitive adhesive layer 2; Figure 4 Middle: The left picture is Comparative Example 1, and the right picture is Example 1. DETAILED DESCRIPTION

[0034] In order to have a clearer understanding of the technical features, purposes and effects of the present invention, a specific implementation scheme is now described in detail.

[0035] The present invention is further described below in conjunction with the embodiments, but the present invention is not limited to the following embodiments. The implementation conditions used in the embodiments can be further adjusted according to the different requirements of specific use, and the implementation conditions not indicated are conventional conditions in the industry. The technical features involved in each embodiment of the present invention can be combined with each other as long as they do not conflict with each other.

[0036] Example 1

[0037] See attached Figure 1-4 This embodiment provides a method for preparing a phase-change temperature-controlled closed-cell foam insulation material, comprising the following steps:

[0038] S1. Preparation of polyurethane wall material phase change microcapsules:

[0039] a. After drying and removing water, the polyester polyol is dissolved in dimethylformamide (DMF) solvent, stirred at high speed, and molten paraffin is added thereto. The paraffin is wrapped by the polyol to form microsphere suspension droplets of 10 to 20 microns;

[0040] b. Control the temperature to 80°C and the stirring speed to 1000r / min, add toluene diisocyanate (TDI) dropwise, stir and disperse for 2h after complete addition; add catalyst dibutyltin dilaurate (DBTDL), slowly dropwise within 1h, under the action of the catalyst, polyol and isocyanate form a polyurethane shell on the surface of paraffin, emulsify and disperse polymerize for 12h to obtain a phase change microcapsule emulsion of polyurethane wall material;

[0041] c. The phase-change microcapsule emulsion of the polyurethane wall material obtained by polymerization is filtered, separated and purified to obtain the phase-change microcapsules of the polyurethane wall material, wherein the particle size of the phase-change microcapsules of the polyurethane wall material is 20 to 30 microns;

[0042] S2. Preparation of phase-change temperature-controlled closed-cell foam insulation material:

[0043] d. Add the purified polyurethane wall material phase change microcapsules to polyether polyol, and add catalyst dibutyltin dilaurate (DBTDL), silicone oil, and deionized water, and stir and mix thoroughly to obtain a foaming agent component A;

[0044] e. using diphenylmethane diisocyanate (MDI) as component B;

[0045] f. Mix component A and component B thoroughly and stir until the solution is milky white, then pour into a copper foil substrate mold for foaming. After the foaming is completed, the phase-change temperature-controlled closed-cell foamed thermal insulation material can be obtained;

[0046] The phase-change temperature-controlled closed-cell foamed heat-insulating material comprises, from top to bottom, an acrylic pressure-sensitive adhesive layer one (1), a substrate layer (2) (copper foil), a foamed heat-insulating layer (3), and an acrylic pressure-sensitive adhesive layer two (4).

[0047] Comparative Example 1

[0048] See attached Figure 5 , this comparative example is the open-cell foaming technology in the prior art.

[0049] according to Figure 4 From the foaming technology comparison diagram of Example 1 of the present invention and the comparative example of the prior art, it can be seen that after the present invention is compressed by external force, the air is squeezed to both sides of the foaming layer (no air overflows), and its buffering and heat-insulating properties are better; while after the comparative example is compressed by external force, the air overflows outward, the air becomes less, and the heat-insulating effect is poor.

[0050] In summary, the present invention adopts closed-cell polyurethane with a microcapsule foaming structure, with a closed-cell rate of 93% to 98%. A small foaming support structure is formed in the foaming hole, which can effectively enhance the buffering and heat insulation properties by more than 20%, and the closed-cell structure can ensure the permanent compression rebound rate, is not easy to produce thickness changes, and can ensure stability; the high H value of the phase change material can absorb and store most of the heat from the heat source, and based on the characteristics of the phase change material, the temperature does not rise during the heat absorption process, which can reduce the heat source temperature to a greater extent, thereby improving the heat insulation effect, and the coating structure of the microcapsule not only improves the compatibility with the foaming matrix resin, but also ensures the seepage of the phase change material, thereby improving the stability of the overall material.

[0051] The above-mentioned embodiment only expresses one implementation mode of the present invention, and its description is relatively specific and detailed, but it cannot be understood as limiting the scope of the invention patent. It should be pointed out that for ordinary technicians in this field, several modifications and improvements can be made without departing from the concept of the present invention, which all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be based on the attached claims.

Claims

1. A method for preparing a phase-change temperature-controlled closed-cell foam insulation material, characterized in that: The steps include: S1. Preparation of polyurethane wall material phase change microcapsules: a. After drying and removing water, the polyester polyol is dissolved in a dimethylformamide solvent, stirred at high speed, and molten paraffin is added thereto. The paraffin is wrapped by the polyol to form microsphere suspension droplets; b. Control the temperature and stirring speed, add isocyanate dropwise, stir and disperse for 2 to 3 hours after it is completely added; add dibutyltin dilaurate as a catalyst, slowly dropwise add within 1 to 1.5 hours, under the action of the catalyst, the polyol and isocyanate form a polyurethane shell on the surface of the paraffin, emulsify and disperse the polymer for 12 to 16 hours to obtain a phase change microcapsule emulsion of the polyurethane wall material; c. filtering, separating and purifying the phase-change microcapsule emulsion of the polyurethane wall material obtained by polymerization to obtain the phase-change microcapsules of the polyurethane wall material; S2. Preparation of phase-change temperature-controlled closed-cell foam insulation material: d. Add the purified polyurethane wall material phase change microcapsules to polyether polyol, and add a catalyst, silicone oil, and deionized water, and stir and mix thoroughly to obtain a foaming agent component A; e. Using isocyanate as component B; f. Component A and component B are fully mixed and stirred until the solution becomes milky white, and then poured into a copper foil substrate mold for foaming. After the foaming is completed, the phase-change temperature-controlled closed-cell foamed insulation material can be obtained.

2. The method for preparing a phase-change temperature-controlled closed-cell foam insulation material according to claim 1, characterized in that: In step a, the paraffin is wrapped by polyol to form microsphere suspension droplets with a particle size of 10 to 20 microns.

3. The method for preparing a phase-change temperature-controlled closed-cell foam insulation material according to claim 1, characterized in that: In step b, the controlled temperature is 80-100° C., and the stirring speed is 1000-1200 r / min; the isocyanate is selected from toluene diisocyanate, diphenylmethane diisocyanate or isophorone diisocyanate.

4. The method for preparing a phase-change temperature-controlled closed-cell foam insulation material according to claim 1, characterized in that: In step c, the particle size of the phase-change microcapsules of the obtained polyurethane wall material is 20 to 30 microns.

5. The method for preparing a phase-change temperature-controlled closed-cell foam insulation material according to claim 1, characterized in that: In step d, the catalyst is selected from one of dibutyltin dilaurate and triethylenediamine A33.

6. The method for preparing a phase-change temperature-controlled closed-cell foam insulation material according to claim 1, characterized in that: In step e, the isocyanate is selected from one of diphenylmethane diisocyanate and toluene diisocyanate as component B.

7. A phase-change temperature-controlled closed-cell foam insulation material, characterized in that: The material is prepared by the method for preparing a phase-change temperature-controlled closed-cell foamed thermal insulation material as described in any one of claims 1 to 6.

8. The phase-change temperature-controlled closed-cell foam insulation material according to claim 7, characterized in that: The phase-change temperature-controlled closed-cell foamed thermal insulation material comprises, from top to bottom, a first acrylic pressure-sensitive adhesive layer, a substrate layer, a foamed thermal insulation layer, and a second acrylic pressure-sensitive adhesive layer.