CN112322049A - Low-thermal-conductivity-coefficient organic silicon foam material and preparation method thereof - Google Patents
Low-thermal-conductivity-coefficient organic silicon foam material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an organosilicon foam material with low thermal conductivity and a preparation method thereof, wherein the organosilicon foam material consists of A, B components, and the A component comprises the following raw materials in parts by weight: 70-90 parts of vinyl silicone oil, 0.1-10 parts of assistant foaming agent, 5-20 parts of modified hollow microspheres, 0.1-1 part of catalyst and 0.01-0.05 part of inhibitor, wherein the component B comprises the following raw materials in parts by weight: 60-90 parts of vinyl silicone oil, 10-30 parts of hydrogen-containing silicone oil and 10-20 parts of modified hollow microspheres. The invention solves the problems that the organic silicon foam heat insulation needs to add a large amount of filler and the heat insulation efficiency is low. The prepared organosilicon foam has low thermal conductivity coefficient, the thermal conductivity coefficient is less than 0.02W/(m × K), the mechanical property is good, the tensile strength is more than 280kPa, and the elongation at break is more than 90%.
Description
Technical Field
The invention belongs to the technical field of organic silicon foam materials, and particularly relates to an organic silicon foam material with a low thermal conductivity coefficient and a preparation method thereof.
Background
The organic silicon material is a high molecular material which takes a silicon-oxygen bond as a main body and an organic group as a side chain, and has excellent high and low temperature resistance, aging resistance, ozone resistance, electric insulation and chemical reaction resistance. The organic silicon foam material has excellent performance of the organic silicon material, light weight, high elasticity and good damping and noise reduction performance. The composite material can be widely applied to the fields of aerospace, rail transit, electronic and electric components, various sealing materials and the like.
In some professional application fields, such as the fields with high-efficiency heat insulation requirements in rail transit and aerospace, higher requirements are put on the heat resistance and heat insulation performance of the organic silicon foam.
Hollow glass beads or ceramic beads can be used as heat insulation filler due to low thermal conductivity, and are often applied to organic silicon foam to reduce the thermal conductivity of the material. For example: patent CN201110387002.7 discloses a double-group low-thermal-conductivity silicone rubber foam material and a preparation method thereof, the material mainly comprises a silicone rubber binder, hollow microspheres and aerogel, and has the characteristics of uniform structure, low thermal conductivity and the like. Patent CN201210321307.2 discloses a preparation method of a foaming silicone rubber material with low thermal conductivity coefficient, and the invention adopts hollow glass beads as a silicone rubber material reinforcing agent, so that the mechanical property of silicone rubber is improved without losing the characteristics of softness and heat insulation. However, the hollow microspheres therein generally only have the function of insulating heat conduction, cannot effectively shield the radiation electromagnetic waves generated by a heat source, cannot block heat from being transferred to the interior of the material through radiation, and have low heat insulation efficiency.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and shortcomings mentioned in the background art, and provide a low-thermal conductivity silicone foam material and a preparation method thereof, so as to improve the heat insulation efficiency.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a low-thermal-conductivity silicone foam material is composed of A, B components, wherein the A component comprises the following raw materials in parts by weight:
the component B comprises the following raw materials in parts by weight:
60-90 parts of vinyl silicone oil
10-30 parts of hydrogen-containing silicone oil
10-20 parts of modified hollow microspheres
Wherein the modified hollow microspheres are obtained by mixing tourmaline and hollow microspheres at the temperature of 80-120 ℃ for 2-4 h.
Further, the hollow microspheres are one or a mixture of two of glass microspheres or ceramic microspheres.
Furthermore, the particle size of the tourmaline is 120-180 μm, and the particle size of the hollow micro-beads is 20-30 μm.
Further, the mass ratio of the tourmaline to the hollow microspheres is (0.8-1.2): 1.
Further, the vinyl silicone oil is a polydimethylsiloxane containing at least two vinyl groups per molecule, and has a viscosity of 10 to 1,000,000 mPas at 25 ℃.
Further, the hydrogen content of the hydrogen-containing silicone oil is 0.1-1.5%.
Further, the auxiliary foaming agent is one or a composition of more than two of ethanol, ethylene glycol, propanol or butanediol.
Further, the catalyst is chloroplatinic acid, and the inhibitor is 1-alkynyl cyclohexanol.
Further, the silicone foam thermal conductivity is <0.02W/(m × K).
The preparation method of the low-thermal conductivity silicone foam material provided by the invention comprises the following steps:
a, B components are uniformly mixed, and the organosilicon foam material is prepared by temperature programming and foaming, wherein the temperature programming comprises the following steps: the foaming temperature is 50-60 ℃, the foaming time is 10-30 min, the heat treatment temperature is 150-160 ℃, and the heat treatment time is 2-3 h.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the hollow microspheres subjected to heating modification treatment are added into the organic silicon foam, and a large number of ions with the same charge exist in the hollow interiors of the hollow microspheres, so that heat energy electromagnetic waves can be effectively shielded; under the condition of low addition amount, the heat conduction of the material is reduced and the surface radiation resistance is improved, and the heat conductivity coefficient of the foam material is reduced by the two modes in a synergistic manner. And a proper process route is optimized, so that high mechanical property of the foam is ensured, and meanwhile, more efficient foam heat insulation capability is provided.
The invention solves the problems that the organic silicon foam heat insulation needs to add a large amount of filler and the heat insulation efficiency is low. The prepared organosilicon foam has low thermal conductivity coefficient, the thermal conductivity coefficient is less than 0.02W/(m × K), the mechanical property is good, the tensile strength is more than 280kPa, and the elongation at break is more than 90%.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
The modified hollow microspheres are one or a mixture of two of modified glass microspheres or modified ceramic microspheres. The modification is mainly carried out by the following method: common hollow microbeads are modified by blending tourmaline master batches under heating, and then are screened and separated. In a specific embodiment, tourmaline with the particle size of 120-180 μm is added into common hollow microspheres with the same mass and the particle size of 20-30 μm, the mixture is uniformly mixed in a high-speed mixer at the temperature of 80-120 ℃ for 2-4 h, and the modified hollow microspheres are obtained after standing, cooling and screening separation. A large amount of ions with the same charge exist in the hollow interior of the modified hollow microsphere, and the electromagnetic waves generated by the ions with the same charge can effectively shield heat electromagnetic waves and improve the heat insulation efficiency.
Mix at the temperature of 80 ~ 120 ℃, under heating and mechanical friction, arouse the difference in electric heat and voltage between the tourmaline crystal, this energy is changeed and is made the air ionization take place, makes the air molecule ionization that closes on turn into the air anion, because heating temperature is high, impels to produce more air anions, reaches better effect.
If tourmaline is directly added as the raw material of the organic silicon foam, no benefit is brought to the mechanical property of the foam, and the hollow microspheres can be used as the reinforcing filler of the organic silicon foam, which is beneficial to the foam to simultaneously keep low density and high strength. In order to avoid the influence of tourmaline on the mechanical strength of the organic silicon foam, the modified hollow microspheres are used as negative ion carriers and added into the organic silicon foam, so that the scheme is better.
The organosilicon is a macromolecule taking siloxane as a main chain, the hollow microspheres can be used as a reinforcing filler of the organosilicon, the bulk density of the hollow microspheres is small, and the hollow microspheres are applied to organosilicon foam, so that the foam has good mechanical properties at the same time of low density, and can realize various effects.
The low thermal conductivity silicone foam of one embodiment of the present invention is comprised of A, B components, wherein:
the component A comprises the following raw materials in parts by weight:
the component B comprises the following raw materials in parts by weight:
60-90 parts of vinyl silicone oil
10-30 parts of hydrogen-containing silicone oil
10-20 parts of modified hollow microspheres
Preferably, the vinyl silicone oil is a polydimethylsiloxane containing at least two vinyl groups per molecule, and has a viscosity of 10 to 1,000,000 mPas at 25 ℃, preferably 5000 to 100,000 mPas.
Preferably, the hydrogen content of the hydrogen-containing silicone oil is 0.1-1.5% by mass. The hydrogen content has an influence on both foam curing and foaming, too low a crosslinking degree, the foam cannot be cured completely, too high a reaction speed, and the quality of the foam cells is influenced.
Preferably, the auxiliary foaming agent is one or a combination of any two or more of ethanol, ethylene glycol, propanol and butanediol. The catalyst is chloroplatinic acid. The inhibitor is 1-alkynyl cyclohexanol.
The preparation method of the silicone foam material comprises the following steps:
(1) a, B components are prepared, and A, B components are respectively and uniformly mixed;
(2) a, B components are mixed evenly and put into a mould cavity, and then the mixture is foamed into the required low-thermal conductivity silicone foam material by a certain temperature programming. Preferably, the programmed temperature is specifically: the foaming temperature is 50-60 ℃, the foaming time is 10-30 min, the heat treatment temperature is 150-160 ℃, and the heat treatment time is 2-3 h.
The tensile strength and elongation at break of the silicone foams in the following examples and comparative examples were tested in accordance with the GB/T6344 standard; the thermal conductivity was tested according to the GB/T10295 standard.
Example 1:
the low-thermal-conductivity-coefficient organosilicon foam material comprises a component A and a component B, wherein the component A is mainly prepared from the following raw materials in parts by weight: 60g of vinyl silicone oil with the viscosity of 50Pa.s and the vinyl mass fraction of 0.2 percent, 1000mPa.s of viscosity, 15g of vinyl silicone oil with the vinyl mass fraction of 4 percent, 5g of ethylene glycol, 15g of modified hollow glass microsphere, 0.2g of chloroplatinic acid and 0.02g of 1-alkynyl cyclohexanol; the component B is mainly prepared from the following raw materials in parts by weight: 60g of vinyl silicone oil with the viscosity of 50Pa.s and the vinyl mass fraction of 0.2 percent, 25g of hydrogen-containing silicone oil with the hydrogen content of 0.75 percent and 15g of modified hollow glass beads.
The preparation method of the low-thermal-conductivity-coefficient silicone foam material comprises the following steps:
(1) adding tourmaline with the particle size of 150 microns into hollow glass beads with the same mass and the particle size of 20-30 microns, mixing for 3 hours in a high-speed mixer at 100 ℃ to uniformly mix, standing, cooling, and screening and separating to obtain modified hollow glass beads;
(2) taking 60g of vinyl silicone oil with the viscosity of 50Pa.s and the vinyl mass fraction of 0.2%, 15g of vinyl silicone oil with the viscosity of 1000mPa.s and the vinyl mass fraction of 4%, 5g of ethylene glycol, 15g of modified hollow glass microsphere, 0.2g of chloroplatinic acid and 0.02g of 1-alkynyl cyclohexanol, and fully and uniformly mixing through mechanical stirring to obtain a component A;
(3) taking 60g of vinyl silicone oil with the viscosity of 50Pa.s and the vinyl mass fraction of 0.2%, 25g of hydrogen-containing silicone oil with the hydrogen content of 0.75% and 15g of modified hollow glass beads, and fully and uniformly mixing by mechanical stirring to obtain a component B;
(4) a, B components are mechanically stirred uniformly according to the ratio of 1:1, and are foamed and cured for 15min at 50 ℃ and then are treated for 3h at 150 ℃ to obtain the low-thermal-conductivity-coefficient organic silicon foam sample 1.
The performance test result of the sample 1 has the tensile strength of 295kPa, the breaking elongation of 95 percent and the thermal conductivity of 0.19W/(m × K).
Example 2:
the low-thermal-conductivity-coefficient organosilicon foam material comprises a component A and a component B, wherein the component A is mainly prepared from the following raw materials in parts by weight: 65g of vinyl silicone oil with the viscosity of 10Pa.s and the vinyl mass fraction of 0.5 percent, 1500mPa.s of viscosity, 15g of vinyl silicone oil with the vinyl mass fraction of 3 percent, 8g of ethylene glycol, 12g of modified hollow ceramic microspheres, 0.2g of chloroplatinic acid and 0.02g of 1-alkynyl cyclohexanol; the component B is mainly prepared from the following raw materials in parts by weight: 65g of vinyl silicone oil with the viscosity of 10Pa.s and the vinyl mass fraction of 0.5 percent, 25g of hydrogen-containing silicone oil with the hydrogen content of 0.75 percent and modified hollow ceramic microspheres.
The preparation method of the low-thermal-conductivity-coefficient silicone foam material comprises the following steps:
(1) adding tourmaline with the particle size of 150 microns into hollow ceramic microbeads with the same mass and the particle size of 20-30 microns, mixing for 3 hours in a high-speed mixer at the temperature of 100 ℃ to uniformly mix, standing, cooling, and screening and separating to obtain modified hollow ceramic microbeads;
(2) taking 65g of vinyl silicone oil with the viscosity of 10Pa.s and the vinyl mass fraction of 0.5%, 15g of vinyl silicone oil with the viscosity of 1500mPa.s and the vinyl mass fraction of 3%, 8g of ethylene glycol, 12g of modified hollow ceramic microspheres, 0.2g of chloroplatinic acid and 0.02g of 1-alkynyl cyclohexanol, and fully and uniformly mixing by mechanical stirring to obtain a component A;
(3) taking 65g of vinyl silicone oil with the viscosity of 10Pa.s and the vinyl mass fraction of 0.5%, 25g of hydrogen-containing silicone oil with the hydrogen content of 0.75% and 10g of modified hollow ceramic microspheres, and fully and uniformly mixing by mechanical stirring to obtain a component B;
(4) a, B components are mechanically stirred uniformly according to the ratio of 1:1, and are foamed and cured for 20min at the temperature of 60 ℃ and then are treated for 2.5h at the temperature of 160 ℃ to obtain the low-thermal-conductivity-coefficient organic silicon foam sample 2.
The performance test result of the sample 2 has the tensile strength of 310kPa, the breaking elongation of 91 percent and the thermal conductivity of 0.18W/(m × K).
Comparative example 1:
the only difference between this comparative example and example 1 is that the modified hollow glass microspheres were replaced with ordinary hollow glass microspheres. Silicone foam sample 3 was obtained.
Sample 3 has the performance test results of 285kPa tensile strength, 85% elongation at break and 0.35W/(m K) thermal conductivity.
Comparative example 2
The only difference between this comparative example and example 1 is that the modification of the cenospheres with tourmaline is carried out at normal temperature: adding tourmaline with the particle size of 150 mu m into hollow glass microspheres with the same mass and the size of 20-30 mu m, mixing the mixture in a high-speed mixer at normal temperature for 3 hours to uniformly mix the mixture, standing the mixture, and screening and separating the mixture to obtain the modified hollow glass microspheres.
This example yielded silicone sample 4.
Sample 4 has 295kPa tensile strength, 94% elongation at break and 0.28W/(m × K) thermal conductivity.
Comparative example 3
The low-thermal-conductivity-coefficient organosilicon foam material comprises a component A and a component B, wherein the component A is mainly prepared from the following raw materials in parts by weight: 60g of vinyl silicone oil with the viscosity of 50Pa.s and the vinyl mass fraction of 0.2 percent, 1000mPa.s of viscosity, 15g of vinyl silicone oil with the vinyl mass fraction of 4 percent, 5g of glycol, 15g of hollow glass microsphere, 15g of tourmaline with the particle size of 150 mu m, 0.2g of chloroplatinic acid and 0.02g of 1-alkynyl cyclohexanol; the component B is mainly prepared from the following raw materials in parts by weight: 60g of vinyl silicone oil with the viscosity of 50Pa.s and the vinyl mass fraction of 0.2 percent, 25g of hydrogen-containing silicone oil with the hydrogen content of 0.75 percent, 15g of hollow glass beads and 15g of tourmaline with the grain diameter of 150 mu m.
The preparation method of the low-thermal-conductivity-coefficient silicone foam material comprises the following steps:
(1) taking 60g of vinyl silicone oil with the viscosity of 50Pa.s and the vinyl mass fraction of 0.2%, 15g of vinyl silicone oil with the viscosity of 1000mPa.s and the vinyl mass fraction of 4%, 5g of ethylene glycol, 15g of hollow glass microspheres, 15g of 150 mu m particle size tourmaline, 0.2g of chloroplatinic acid and 0.02g of 1-alkynyl cyclohexanol, and fully and uniformly mixing by mechanical stirring to obtain a component A;
(2) taking 60g of vinyl silicone oil with the viscosity of 50Pa.s and the vinyl mass fraction of 0.2%, 25g of hydrogen-containing silicone oil with the hydrogen content of 0.75%, 15g of hollow glass microspheres and 15g of tourmaline with the particle size of 150 mu m, and fully and uniformly mixing by mechanical stirring to obtain a component B;
(3) a, B components are mechanically stirred uniformly according to the ratio of 1:1, and are foamed and cured for 15min at 50 ℃ and then are treated for 3h at 150 ℃ to obtain the low-thermal-conductivity-coefficient organic silicon foam sample 5.
Sample 5, the tensile strength 207kPa, the elongation at break 65%, and the thermal conductivity 0.23W/(m K) were measured.
The results of the samples 1 and 2 show that the addition of the modified hollow microspheres can enable the foam to obtain better mechanical property and lower heat conductivity coefficient, the heat conductivity coefficient of the material can be efficiently reduced due to the double-effect synergistic effect of the modified hollow microspheres, the sample 3 is close to the samples 1 and 2 in tensile property by adding the conventional hollow glass microspheres, and the heat insulation capability is much poorer than that of the samples 1 and 2, and the performance of reducing the heat conductivity coefficient of the organic silicon foam by the conventional hollow microspheres is proved to be inferior to that of the modified glass microspheres, so that the advantage of the organic silicon foam with low heat conductivity coefficient can be seen. Sample 4 shows that the effect of modifying glass beads by using a non-heating method is poor, the foam thermal conductivity coefficient does not achieve the effect of the invention, and sample 5 shows that the method of directly adding tourmaline into the foam body has a large influence on the foam strength and does not achieve the effect of the invention.
The foregoing is considered as illustrative of the preferred embodiments of the invention and is not to be construed as limiting the invention in any way. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention should fall within the protection scope of the technical scheme of the present invention, unless the technical spirit of the present invention departs from the content of the technical scheme of the present invention.
Claims (10)
1. The low-thermal-conductivity silicone foam material consists of A, B components, and is characterized in that the A component comprises the following raw materials in parts by weight:
the component B comprises the following raw materials in parts by weight:
60-90 parts of vinyl silicone oil
10-30 parts of hydrogen-containing silicone oil
10-20 parts of modified hollow microspheres
Wherein the modified hollow microspheres are obtained by mixing tourmaline and hollow microspheres at the temperature of 80-120 ℃ for 2-4 h.
2. The low thermal conductivity silicone foam according to claim 1, wherein the cenospheres are one or a mixture of glass or ceramic microbeads.
3. The low thermal conductivity silicone foam material according to claim 1 or 2, wherein the particle size of the tourmaline is 120 to 180 μm, and the particle size of the cenospheres is 20 to 30 μm.
4. The low-thermal-conductivity silicone foam material according to claim 1 or 2, wherein the mass ratio of the tourmaline to the cenospheres is (0.8-1.2): 1.
5. The low thermal conductivity silicone foam material according to claim 1 or 2, wherein the vinyl silicone oil is a polydimethylsiloxane having at least two vinyl groups per molecule, and has a viscosity of 10 to 1,000,000 mPas at 25 ℃.
6. The low thermal conductivity silicone foam according to claim 1 or 2, characterized in that the hydrogen content of the hydrogen-containing silicone oil is 0.1% to 1.5%.
7. The low thermal conductivity silicone foam according to claim 1 or 2, wherein the co-blowing agent is one or a combination of any two or more of ethanol, ethylene glycol, propanol or butanediol.
8. The low thermal conductivity silicone foam of claim 1 or 2, wherein the catalyst is chloroplatinic acid and the inhibitor is 1-alkynylcyclohexanol.
9. The low thermal conductivity silicone foam according to claim 1 or 2, characterized in that the silicone foam thermal conductivity is <0.02W/(m x K).
10. A method for preparing the low thermal conductivity silicone foam material according to any one of claims 1 to 9, comprising the steps of:
a, B components are uniformly mixed, and the organosilicon foam material is prepared by temperature programming and foaming, wherein the temperature programming comprises the following steps: the foaming temperature is 50-60 ℃, the foaming time is 10-30 min, the heat treatment temperature is 150-160 ℃, and the heat treatment time is 2-3 h.
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| CN116023787A (en) * | 2022-11-11 | 2023-04-28 | 武汉中科先进材料科技有限公司 | Organic silicon foam with double-peak cell structure and preparation method thereof |
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