CN115746796A - Preparation method of flexible flame-retardant shape-stabilized phase-change material - Google Patents
Preparation method of flexible flame-retardant shape-stabilized phase-change material Download PDFInfo
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Abstract
The invention relates to a preparation method of a flexible flame-retardant shape-stabilized phase-change material, belonging to the technical field of phase-change materials. The operation steps are as follows: preparing a flexible shape-stabilized phase-change material; (2) Preparing flexible flame-retardant coating by using a flame retardant, room-temperature vulcanized silicone rubber, a curing agent, a catalyst and a silane coupling agent; (3) Uniformly coating the flexible flame-retardant coating on the surface of the flexible phase-change material, wherein the thickness of the coating of the flame-retardant coating is 0.3-1mm; curing to obtain a flexible flame-retardant shape-stabilized phase change material; the flexible flame retardant shape-stabilized phase change material achieves the V0 grade by the vertical burning test (UL-94) and the oxygen index test (LOI) is more than 27 vol.%. The flexible shape-stabilized phase change material prepared in the step (1) does not contain a flame retardant, and the flame-retardant coating has high flexibility and has no influence on the mechanical property and the energy storage property of the flame-retardant shape-stabilized phase change material; the material prepared by the invention has low surface hardness and good flexibility, can adapt to various equipment shapes, and reduces the contact thermal resistance.
Description
Technical Field
The invention belongs to the technical field of phase-change materials, and particularly relates to a preparation method of a flexible flame-retardant shape-stabilized phase-change material.
Background
As a phase change material thermal management system with application potential in a passive thermal management system, additional components and electric energy supply are not needed, the complexity of equipment integration can be effectively reduced, and the reliability of a device is improved. However, the phase change matrix used in the phase change material thermal management system is flammable, and thus is limited by safety in thermal management applications with high fire safety requirements, such as battery packs for electric vehicles or building energy conservation. In order to realize the nonflammable characteristic of the phase change material, researchers add a flame retardant to the phase change matrix to suppress the flammability of the phase change material. In the current research on flame retardant shaping phase change materials, in order to obtain a better flame retardant effect, more than 20 wt% of flame retardants, such as halogen flame retardants (chlorinated paraffin, tetrachlorobisphenol, decabromodiphenyl ether, and the like), metal hydroxide flame retardants (magnesium hydroxide, aluminum hydroxide, and the like), intumescent flame retardants (ammonium polyphosphate, pentaerythritol, melamine, and the like), phosphorus flame retardants (red phosphorus, ammonium polyphosphate, phosphate, and the like), and nitrogen flame retardants (melamine, melamine phosphate, trioxypurine acid, and the like), are often added to a phase change matrix. However, the addition of a large amount of flame retardant can greatly reduce the specific gravity of the phase-change matrix, which leads to the reduction of the heat storage capacity of the material and has a great influence on the mechanical properties of the material.
In order to reduce the dosage of the flame retardant, a scholars manufactures the flame-retardant phase-change material based on the flame retardance of the coating, but researches on that the coating mainly takes epoxy resin and acrylic resin as binders, the epoxy resin and the acrylic resin are low in flexibility and high in hardness after being cured, and particularly after a large amount of additives are added, the hardness is further improved. Such a coating would reduce the mechanical properties of the flexible shape-stabilized phase change material.
Disclosure of Invention
In order to solve the problems of mechanical property change and energy storage performance reduction of the traditional flame-retardant phase-change material after a flame retardant is added in a physical blending mode, the invention provides a preparation method of a flexible flame-retardant phase-change material.
The preparation operation steps of the flexible flame-retardant shape-stabilized phase-change material are as follows:
(1) Preparing a flexible composite phase change material by adopting a phase change matrix, a support material and a heat conduction reinforcing material, and carrying out hot press molding on the flexible composite phase change material to obtain a flexible shaping phase change material;
(2) Adding 10-42 parts by mass of flame retardant into 87-56 parts by mass of room-temperature vulcanized silicone rubber, mechanically stirring until uniform mixing, adding 0.5-2 parts by mass of curing agent, 0.25-0.5 part by mass of catalyst and 0.25-0.5 part by mass of silane coupling agent, and fully stirring for five minutes to obtain a flexible flame-retardant coating;
(3) Uniformly coating the flexible flame-retardant coating on the surface of the flexible shape-stabilized phase change material, wherein the thickness of the coating of the flexible flame-retardant coating is 0.3-1mm; curing for more than 30min to obtain the flexible flame-retardant shape-stabilized phase change material;
the flexible flame-retardant shape-stabilized phase change material achieves the result of a vertical burning test (UL-94) of V0 grade, and the result of an oxygen index test (LOI) is more than 27 vol.%.
The further technical scheme is as follows:
in the step (1), 60-85 parts by mass of phase change matrix and 13-30 parts by mass of supporting material are added into a high-temperature reaction kettle at the temperature of 160-190 ℃, and are stirred and co-melted until the phase change matrix and the supporting material are uniformly mixed; adding 3-10 parts by mass of heat conduction reinforcing material, and continuously stirring until the mixture is uniform; vacuumizing, and continuously stirring for 30-60min to obtain a flexible composite phase change material; taking out the flexible composite phase change material, putting the flexible composite phase change material into a mould, and performing hot press molding at the temperature of 80-110 ℃ to obtain a flexible shape-stabilized phase change material;
the phase change matrix is a conventional phase change matrix material and comprises more than one of alkane phase change materials (paraffin, eicosane, octadecane and the like), alcohol phase change materials (octadecanol, polyethylene glycol and the like) and fatty acid phase change materials (lauric acid, myristic acid and the like);
the support material is a conventional polymer support material and comprises one of Olefin Block Copolymer (OBC), hydrogenated styrene-butadiene-styrene block copolymer (SEBS) and ethylene-octene high Polymer (POE);
the heat conduction reinforcing material is a conventional heat conduction reinforcing material and comprises more than one of expanded graphite, carbon fiber, multilayer graphene oxide and graphene powder.
In the step (2), the flame retardant is a conventional flame retardant, and comprises more than one of expandable graphite, chlorinated paraffin, antimony trioxide, ammonium polyphosphate, white carbon black and titanium dioxide.
In the step (2), the curing agent is a conventional silicon rubber curing agent and comprises methyl triethoxysilane or methyl tributyrinoxime silane.
In the step (2), the catalyst is a conventional silicon rubber curing catalyst and comprises dibutyltin dilaurate or stannous octoate.
In the step (2), the silane coupling agent comprises a silane coupling agent KH550 or a silane coupling agent KH570.
The beneficial technical effects of the invention are embodied in the following aspects:
the invention solves the problems of mechanical property change and energy storage performance reduction of the traditional flame-retardant phase-change material after the flame retardant is added in a physical blending mode. In order to obtain a better flame-retardant effect, more than 20% of flame retardant is usually added into a phase-change material matrix, so that the energy storage performance of the phase-change material is greatly reduced, and the flexibility of the phase-change material is also reduced. According to the flexible flame-retardant shaping phase-change material based on the flame-retardant coating, the flame retardant is only contained in the flexible flame-retardant coating on the outer surface, the flexible shaping phase-change material wrapped inside is not added with the flame retardant, and the flexible flame-retardant coating is positioned at the place where oxygen and heat are most effectively isolated, so that the flexible flame-retardant shaping phase-change material prepared in the manner not only can play a good flame-retardant role with less flame retardant, but also does not influence the mechanical property of the phase-change material, and the coating is thinner, so that the influence on the energy storage property of the phase-change material is smaller, when the latent heat reduction is 14.7%, the vertical combustion test result of the material can reach UL-94 V0 level, the oxygen index LOI is 29.5 vol%, and the peak value of the heat release rate is reduced by 77.6%.
The phase-change material adopted by the invention has normal-temperature flexibility, the flexibility of the phase-change material after being changed into the flame-retardant phase-change material is mainly kept by the flexible flame-retardant coating, and common coating binders such as epoxy resin and acrylic resin have weaker flexibility after being cured, mainly because the C-C bond has larger internal rotation steric hindrance and shorter bond length so that the flexibility of the phase-change material after being cured is weaker, thereby influencing the overall mechanical property of the material; the main chain of the room temperature vulcanized silicone rubber adopted by the invention is Si-O-Si, and the room temperature vulcanized silicone rubber has the advantages of long bond length, large bond angle, small internal rotation resistance and good flexibility.
Referring to fig. 1, a structure diagram of a flexible flame-retardant shape-stabilized phase-change material is shown, wherein the middle part is the flexible shape-stabilized phase-change material, and the outer coating part is a flexible flame-retardant coating.
Referring to fig. 2, when a fire source is close to the flexible flame-retardant phase-change material, the flexible flame-retardant coating contacts with flame first, the flame retardant in the coating degrades to release non-combustible gas to reduce the oxygen content on the surface of the material, and simultaneously, the generated non-volatile substances cover the surface of the phase-change material to form a compact carbon layer, so that the oxygen is isolated from contacting with the flexible shaping phase-change material, and heat is isolated from being transmitted into the flexible shaping phase-change material, so that the flame is extinguished, and the material is prevented from continuing to burn.
As shown in fig. 3, the flexible shape-stabilized phase change material is comparative example 1, the example 1 is obtained after the flexible flame-retardant coating is coated on the surface of the flexible shape-stabilized phase change material, the comparative example 2 is obtained after the flame retardant with the same proportion of the coating is added into the phase change material, and it can be found from fig. 3 that after the flame retardant is directly added into the phase change material, cracks occur in bending and twisting of the material, and the flexible flame-retardant coating has little influence on the mechanical properties of the material.
The preparation method is simple, and the flexible flame-retardant shape-stabilized phase change material has low surface hardness and good flexibility, can adapt to the shape of equipment and reduces the contact thermal resistance.
Drawings
FIG. 1 is a structural diagram of a flexible flame-retardant shape-stabilized phase-change material.
FIG. 2 is a flame-retardant principle diagram of a flexible flame-retardant shape-stabilized phase-change material.
Fig. 3 is a mechanical property test chart of the material.
FIG. 4 is a heat release rate graph of a cone calorimetry experiment of a flexible flame retardant shaped phase change material.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
The preparation operation steps of the flexible flame-retardant shape-stabilized phase change material are as follows:
(1) 80g of No. 40 paraffin and 15g of Olefin Block Copolymer (OBC) are added into a high-temperature reaction kettle with the temperature of 170 ℃ for melt mixing, and the mixture is stirred and melted until the mixture is uniformly mixed. 3g of expanded graphite was added thereto, and stirring was continued until homogeneous. And (3) carrying out vacuum pumping operation on the high-temperature reaction kettle, and continuously stirring for 30-60min to obtain the flexible composite phase change material. And stopping stirring, opening the high-temperature reaction kettle, taking out the flexible composite phase change material, putting the flexible composite phase change material into a mold, and performing hot press molding at 80 ℃ to obtain the flexible shaping phase change material.
(2) Adding 8g of expandable graphite and 4g of ammonium polyphosphate (mass ratio is 2; and adding 1g of methyl triethoxysilane, 0.5g of dibutyltin dilaurate and 0.5g of silane coupling agent KH570, and fully stirring for five minutes to obtain the flexible flame-retardant coating.
(3) Uniformly coating the flexible flame-retardant coating on the surface of the flexible phase-change material, wherein the thickness of the coating of the flexible flame-retardant coating is 0.4mm; and curing for 1h to obtain the flexible flame-retardant shape-stabilized phase change material.
The material is subjected to a heat conductivity coefficient test by a Hot Disk method, the heat conductivity is 0.8W/(m.K), and the latent heat is 135.6J/g as measured by a differential scanning calorimeter. The result of a vertical burning test (UL-94) is V0, the material has no drop phenomenon, and the flame is extinguished within 30 s; oxygen index measurement (LOI) result 29.5vol.%; the result of the cone calorimetry test is that the peak value of the heat release rate is 228kW/m 2 The average heat release rate was 67kW/m 2 。
Comparative example 1
A flexible phase change material was prepared according to the step (1) of example 1 without application of a flame retardant coating.
The material was tested for thermal conductivity by the Hot Disk method and had a thermal conductivity of 0.9W/(m.K) and a latent heat of 159.1J/g as measured by differential scanning calorimetry. The result of the vertical burning test (UL-94) is NC (not reaching the UL-94 classification grade standard), the material burns violently, and the phenomenon of falling is generated. Oxygen index measurement (LOI) result 19.5vol.%. The result of the cone calorimetry test is that the peak value of the heat release rate is 1016kW/m 2 The average heat release rate was 229kW/m 2 。
Comparative example 2
The preparation operation steps of the conventional flexible flame-retardant phase-change material are as follows:
(1) Adding 80g of No. 40 paraffin and 15g of OBC into a high-temperature reaction kettle at the temperature of 170 ℃ for melt mixing, stirring and eutectic melting until the mixture is uniformly mixed, adding 3g of expanded graphite, 12g of expandable graphite and ammonium polyphosphate (mass ratio is 2. And after the uniform stirring, carrying out vacuum pumping operation on the high-temperature reaction kettle, and continuously stirring for 30-60min to obtain the flexible composite phase change material.
(2) And stopping stirring, opening the high-temperature reaction kettle, taking out the flexible composite phase change material, putting the flexible composite phase change material into a mold, and performing hot press molding at 80 ℃ to obtain the flexible shaping phase change material.
The material is subjected to a heat conductivity coefficient test by a Hot Disk method, the heat conductivity is 1.8W/(m.K), and the latent heat is 136.9J/g as measured by a differential scanning calorimeter. The result of the vertical burning test (UL-94) is NC (not reaching the UL-94 classification grade standard), the material burns violently, and the phenomenon of falling is caused. Oxygen index measurement (LOI) results 21.1vol.%. The result of the cone calorimetry test is that the peak value of the heat release rate is 316kW/m 2 The average heat release rate is 99kW/m 2 。
The mechanical property test chart and the heat release rate chart of example 1, comparative example 1 and comparative example 2 are shown in fig. 3 and fig. 4, respectively. The mechanical property test result of the material shows that the comparative example 2 obtained by adding the flame retardant with the same proportion of the coating into the phase-change material has cracks in bending and twisting, the mechanical property is reduced, and the flexible flame-retardant coating has little influence on the overall mechanical property of the material. From the cone calorimeter test results, it can be known that: the flame-retardant coating is used for flame retarding the flexible shape-stabilized phase change material, so that a better flame-retardant effect is achieved, the peak value of the heat release rate is reduced by 77.6%, and the average heat release rate is reduced by 70.7%.
The latent heat of the example 1 and the comparative example 2 is respectively reduced by 14.7 percent and 13.9 percent compared with the latent heat of the comparative example 1 (in the subsequent examples, the flexible shape-stabilized phase change material which is not coated with the flame-retardant coating is called as a pure sample), and the latent heat reduction degree of the two is equivalent, but the flame-retardant effect of the example 1 is obviously better.
Example 2
The preparation operation steps of the flexible flame-retardant shape-stabilized phase-change material are as follows:
(1) 74g of eicosane, 10g of hydrogenated styrene-butadiene-styrene block copolymer (SEBS) and 10g of ethylene-octene copolymer (POE) were added into a high-temperature reaction kettle at 190 ℃ for melt mixing, stirred and co-melted until uniform mixing was achieved, 4g of expanded graphite and 2g of carbon fibers were added thereto, and stirring was continued until uniform mixing was achieved. And (3) carrying out vacuum pumping operation on the high-temperature reaction kettle, and continuously stirring for 30-60min to obtain the flexible composite phase change material. Stopping stirring, opening the high-temperature reaction kettle, taking out the flexible composite phase change material, putting the flexible composite phase change material into a mold, and carrying out hot press molding at 80-110 ℃ to obtain the flexible shaping phase change material.
(2) Adding 30g of chlorinated paraffin and 12g of antimony trioxide (mass ratio is 5; adding 1g of methyl tributyl ketoxime silane, 0.5g of stannous octoate and 0.5g of silane coupling agent KH570, and fully stirring for five minutes to obtain the flexible flame-retardant coating.
(3) Uniformly coating the flexible flame-retardant coating on the surface of the flexible phase change material, wherein the thickness of the coating of the flexible flame-retardant coating is 0.3mm; and curing for 1.5h to obtain the flexible flame-retardant shape-stabilized phase change material.
The material was tested for thermal conductivity by Hot Disk method and had a thermal conductivity of 1.3W/(m.k) and a latent heat of 125.5J/g (19.2% lower than that of pure sample). The result of the vertical burning test (UL-94) is V0, the material has no sagging phenomenon, the flame is extinguished within 3s, and the result of the oxygen index measurement (LOI) is 36vol.%. The result of the cone calorimetry test is that the peak value of the heat release rate is 167kW/m 2 The average heat release rate was 64kW/m 2 。
Example 3
The preparation operation steps of the flexible flame-retardant shape-stabilized phase-change material are as follows:
(1) Adding 70g of octadecanol, 8g of Olefin Block Copolymer (OBC) and 8g of hydrogenated styrene-butadiene-styrene block copolymer (SEBS) into a high-temperature reaction kettle at the temperature of 180 ℃ for melt mixing, stirring and co-melting until uniform mixing is achieved, adding 5g of expanded graphite and 5g of graphene, and continuing stirring until uniform mixing is achieved. And (3) carrying out vacuum pumping operation on the high-temperature reaction kettle, and continuously stirring for 30-60min to obtain the flexible composite phase change material. Stopping stirring, opening the high-temperature reaction kettle, taking out the flexible composite phase change material, putting the flexible composite phase change material into a mold, and performing hot press molding at 110 ℃ to obtain the flexible shaping phase change material.
(2) Adding 7.14g of chlorinated paraffin, 2.86g of antimony trioxide (mass ratio is 5.
(3) Uniformly coating the flexible flame-retardant coating on the surface of the flexible phase change material, wherein the thickness of the coating of the flexible flame-retardant coating is 1.0mm; and curing for 3h to obtain the flexible flame-retardant shape-stabilized phase change material.
The material was tested for thermal conductivity by Hot Disk method and had a thermal conductivity of 1.8W/(m · K) and a latent heat of 118.8J/g (22.9% reduction compared to the latent heat of the pure sample). The result of the vertical burning test (UL-94) was V0, the material did not sag, the flame was extinguished within 3s, and the result of the oxygen index measurement (LOI) was 38.3vol.%. The result of the cone calorimetry test is that the peak value of the heat release rate is 162kW/m 2 The average heat release rate is 52kW/m 2 。
It will be readily understood by those skilled in the art that the above embodiments 1-3 are merely preferred embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included within the scope of the present invention.
Claims (6)
1. The preparation method of the flexible flame-retardant shape-stabilized phase change material is characterized by comprising the following operation steps of:
(1) Preparing a flexible composite phase change material by adopting a phase change matrix, a support material and a heat conduction reinforcing material, and carrying out hot press molding on the flexible composite phase change material to obtain a flexible shaping phase change material;
(2) Adding 10-42 parts by mass of flame retardant into 87-56 parts by mass of room temperature vulcanized silicone rubber, mechanically stirring until uniform mixing is achieved, adding 0.5-2 parts by mass of curing agent, 0.25-0.5 part by mass of catalyst and 0.25-0.5 part by mass of silane coupling agent, and fully stirring for five minutes to obtain the flexible flame retardant coating;
(3) Uniformly coating the flexible flame-retardant coating on the surface of the flexible shape-stabilized phase change material, wherein the thickness of the coating of the flexible flame-retardant coating is 0.3-1mm; curing for more than 30min to obtain the flexible flame-retardant shape-stabilized phase change material;
the flexible flame retardant shape-stabilized phase change material achieves UL-94 V0 grade in vertical burning test result, and the oxygen index test result (LOI) is more than 27 vol%; compared with the flexible shape-stabilized phase change material, the peak value of the heat release rate of the flexible flame-retardant shape-stabilized phase change material is reduced by more than 60%.
2. The preparation method of the flexible flame-retardant shape-stabilized phase change material as claimed in claim 1, characterized in that: in the step (1), 60-85 parts by mass of phase change matrix and 13-30 parts by mass of supporting material are added into a high-temperature reaction kettle at the temperature of 160-190 ℃, and are stirred and co-melted until the phase change matrix and the supporting material are uniformly mixed; adding 3-10 parts by mass of heat conduction reinforcing material, and continuously stirring until the mixture is uniform; vacuumizing, and continuously stirring for 30-60min to obtain the flexible composite phase-change material; taking out the flexible composite phase change material, putting the flexible composite phase change material into a mould, and performing hot press molding at the temperature of 80-110 ℃ to obtain a flexible shape-stabilized phase change material;
the phase change matrix comprises No. 40 paraffin or eicosane or octadecanol;
the support material comprises an Olefin Block Copolymer (OBC), a hydrogenated styrene-butadiene-styrene block copolymer (SEBS), an ethylene-octene high Polymer (POE);
the heat conduction reinforcing material comprises more than one of expanded graphite, carbon fiber, multilayer graphene oxide and graphene powder.
3. The preparation method of the flexible flame-retardant shape-stabilized phase-change material according to claim 1, characterized in that: in the step (2), the flame retardant comprises more than one of expandable graphite, chlorinated paraffin, antimony trioxide, ammonium polyphosphate, white carbon black and titanium dioxide.
4. The preparation method of the flexible flame-retardant shape-stabilized phase change material as claimed in claim 1, characterized in that: in the step (2), the curing agent comprises methyltriethoxysilane or methyltributanone oxime silane.
5. The preparation method of the flexible flame-retardant shape-stabilized phase change material as claimed in claim 1, characterized in that: in the step (2), the catalyst comprises dibutyltin dilaurate or stannous octoate.
6. The preparation method of the flexible flame-retardant shape-stabilized phase change material as claimed in claim 1, characterized in that: in the step (2), the silane coupling agent comprises a silane coupling agent KH550 or a silane coupling agent KH570.
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