CN112680177A - Low-density high-temperature-resistant pouring sealant and preparation method thereof - Google Patents
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Abstract
The invention discloses a low-density high-temperature-resistant pouring sealant, which comprises the following components in parts by weight: 100 parts of vinyl silicone oil, 10 to 20 parts of a cross-linking agent, 10 to 30 parts of a metal-organic framework material, 30 to 60 parts of a heat-conducting filler, 1 to 3 parts of a platinum catalyst and 0.01 to 0.1 part of an inhibitor. The metal-organic framework material is a porous material, and is a crystalline porous material with a periodic network structure formed by self-assembly of transition metal ions and organic ligands. The organic ligand in the metal-organic framework material has stronger interaction with the polymer chain segment and can be uniformly dispersed in the polymer matrix. In addition, the metal-organic framework material has the advantages of high porosity, low density, large specific surface area, high temperature resistance and the like, wherein UiO-66-Br and UiO-66 can be kept stable at 450 ℃, and UiO-66-NH2 and UiO-66-NO2 can be kept stable at 350 ℃.
Description
Technical Field
The invention relates to the technical field of pouring sealants, in particular to a low-density high-temperature-resistant pouring sealant and a preparation method thereof.
Background
New energy automobiles have become the trend of future automobile development. The development of the light weight of the automobile is the key for saving electric energy and increasing the endurance mileage. The battery of the new energy automobile is a battery panel consisting of a plurality of battery packs, and the encapsulation of the battery is a key technology applied to the new energy automobile. During the driving process of the automobile, the battery can generate a large amount of heat, so that the temperature of the battery is increased, and the consumption, the service life and the use safety of the battery are increased. Development of light, heat-conducting, flame-retardant and high-temperature-resistant pouring sealant is always the key point of new energy automobiles. Organic silicon is gradually applied to the field of new energy battery pouring sealant due to the properties of insulation, flame retardance, high temperature resistance, aging resistance and the like, and the heat-conducting property of the organic silicon pouring sealant usually needs to be added with a large amount of filler, so that the weight of a battery is increased. The preparation of the low-density pouring sealant usually adopts hollow fillers, such as hollow glass beads, hollow coal cinder micro powder, hollow silica micro powder and the like, but the hollow fillers are easy to delaminate in the storage process.
Disclosure of Invention
The invention aims to provide a low-density high-temperature-resistant pouring sealant and a preparation method thereof, which solve one or more of the problems in the prior art.
On one hand, the invention provides a low-density high-temperature-resistant pouring sealant, which comprises the following components in parts by weight: 100 parts of vinyl silicone oil, 10 to 20 parts of a cross-linking agent, 10 to 30 parts of a metal-organic framework material, 30 to 60 parts of a heat-conducting filler, 1 to 3 parts of a platinum catalyst and 0.01 to 0.1 part of an inhibitor.
In some embodiments, the vinyl silicone oil has a viscosity of 2000 to 30000 mPa-s and a vinyl content of 0.1% to 3.0%.
In some embodiments, the crosslinking agent is a hydrogen-containing silicone oil having a viscosity of 500 to 3000 mPa-s.
In some embodiments, the metal-organic framework material is UiO-66, UiO-66-Br, UiO-66-NH2Or UiO-66-NO2One or more of (a).
In some embodiments, the thermally conductive filler is one or more of graphene, silica micropowder, alumina, magnesia, boron nitride.
In some embodiments, the platinum catalyst is one of chloroplatinic acid-isopropanol or chloroplatinic acid-divinyltetramethyldisiloxane, wherein the platinum content is 3% o to 1% by mass.
In some embodiments, the inhibitor is one or more of 2-methyl-3-butyn-2-ol, 3-methyl-1-hexyn-3-ol, 1-ethynylcyclohexanol, methyltris (methylbutynoxy) silane, phenyltri (methylbutynoxy) silane, vinyltri (methylbutynoxy) silane, polyvinyl polysiloxane.
On the other hand, the invention provides a preparation method of the low-density high-temperature-resistant pouring sealant, which comprises the following steps:
the pouring sealant A comprises the following components: adding 50 parts of vinyl silicone oil, 10 to 20 parts of cross-linking agent, 10 to 30 parts of metal-organic framework material, 15 to 30 parts of heat-conducting filler and 0.01 to 0.1 part of inhibitor into a kneader, stirring for 1 to 3 hours in vacuum at 120 to 180 ℃, adding hydrogen-containing silicone oil and inhibitor after the temperature is reduced to 50 to 80 ℃, and continuing stirring for 1 to 3 hours to obtain a component A;
and (3) pouring sealant B component: adding 50 parts of vinyl silicone oil, 15-30 parts of heat-conducting filler and 1-3 parts of platinum catalyst into a kneader, and stirring for 1-3 hours in vacuum at 120-180 ℃ to obtain a component B;
preparing a pouring sealant: mixing A, B components according to a mass ratio of 1: 1, uniformly mixing, defoaming in vacuum, and curing at 80-120 ℃ for 2-12 h to obtain the low-density high-temperature-resistant pouring sealant.
Compared with the prior art, the invention has the following advantages:
1. the metal-organic framework material is a porous material, and is a crystalline porous material with a periodic network structure formed by self-assembly of transition metal ions and organic ligands. The organic ligand in the metal-organic framework material has stronger interaction with the polymer chain segment and can be uniformly dispersed in the polymer matrix. In addition, the metal-organic framework material has the advantages of high porosity, low density, large specific surface area, high temperature resistance and the like, wherein UiO-66-Br and UiO-66 can be kept stable at 450 ℃, and UiO-66-NH2 and UiO-66-NO2 can be kept stable at 350 ℃.
2. The metal-organic framework material is used as a filler to be added into the pouring sealant, so that the density of the pouring sealant can be reduced, and the temperature resistance of the pouring sealant can be improved.
Detailed Description
The present invention will be further described with reference to the following examples. The following examples are only for illustrating the performance of the present invention more clearly and are not limited to the following examples.
Example 1:
the preparation method of the low-density high-temperature-resistant pouring sealant comprises the following steps:
the pouring sealant A comprises the following components: adding 50g of vinyl silicone oil, 5g of cross-linking agent hydrogen-containing silicone oil, 10g of metal-organic framework material UiO-66, 15g of heat-conducting filler graphene and 0.005g of inhibitor 2-methyl-3-butynyl-2 alcohol into a kneader, stirring for 3 hours in vacuum at 120 ℃, adding 5g of hydrogen-containing silicone oil and 0.005g of inhibitor 2-methyl-3-butynyl-2 alcohol after the temperature is reduced to 50 ℃, and continuing stirring for 1 hour to obtain a component A;
and (3) pouring sealant B component: adding 50g of vinyl silicone oil, 15g of heat-conducting filler graphene and 1g of platinum catalyst chloroplatinic acid-isopropanol into a kneader, and stirring for 3 hours in vacuum at 120 ℃ to obtain a component B;
preparing a pouring sealant: mixing A, B components according to a mass ratio of 1: 1, uniformly mixing, defoaming in vacuum, and curing at 80 ℃ for 12 hours to obtain the low-density high-temperature-resistant pouring sealant.
Example 2:
the preparation method of the low-density high-temperature-resistant pouring sealant comprises the following steps:
the pouring sealant A comprises the following components: adding 50g of vinyl silicone oil, 10g of cross-linking agent hydrogen-containing silicone oil, 30g of metal-organic framework material UiO-66-Br, 30g of heat-conducting filler silicon micropowder and 0.05g of inhibitor 3-methyl-1-hexynyl-3-alcohol into a kneader, stirring for 1h in vacuum at 180 ℃, adding 10g of hydrogen-containing silicone oil and 0.05g of inhibitor 3-methyl-1-hexynyl-3-alcohol after the temperature is reduced to 80 ℃, and continuing stirring for 3h to obtain a component A;
and (3) pouring sealant B component: adding 50g of vinyl silicone oil, 30g of heat-conducting filler silicon powder and 3g of platinic acid catalyst chloroplatinic acid-divinyl tetramethyl disiloxane into a kneader, and stirring for 1h in vacuum at 180 ℃ to obtain a component B;
preparing a pouring sealant: mixing A, B components according to a mass ratio of 1: 1, uniformly mixing, defoaming in vacuum, and curing at 120 ℃ for 2 hours to obtain the low-density high-temperature-resistant pouring sealant.
Example 3:
the preparation method of the low-density high-temperature-resistant pouring sealant comprises the following steps:
the pouring sealant A comprises the following components: 50g of vinyl silicone oil, 7.5g of crosslinking agent hydrogen-containing silicone oil and 20g of metal-organic framework material UiO-66-NH2Adding 20g of heat-conducting filler alumina and 0.0025g of inhibitor 1-ethynylcyclohexanol into a kneader, stirring for 2h under vacuum at 160 ℃, adding 7.5g of hydrogen-containing silicone oil and 0.0025g of inhibitor 1-ethynylcyclohexanol after the temperature is reduced to 60 ℃, and continuing stirring for 2h to obtain a component A;
and (3) pouring sealant B component: adding 50g of vinyl silicone oil, 20g of heat-conducting filler alumina and 2g of platinum catalyst chloroplatinic acid-isopropanol into a kneader, and stirring for 2 hours in vacuum at 160 ℃ to obtain a component B;
preparing a pouring sealant: mixing A, B components according to a mass ratio of 1: 1, uniformly mixing, defoaming in vacuum, and curing at 100 ℃ for 6 hours to obtain the low-density high-temperature-resistant pouring sealant.
Example 4:
the preparation method of the low-density high-temperature-resistant pouring sealant comprises the following steps:
the pouring sealant A comprises the following components: 50g of vinyl silicone oil, 6g of cross-linking agent hydrogen-containing silicone oil and 15g of metal-organic framework material UiO-66-NO218g of heat-conducting filler magnesium oxide and 0.01g of inhibitor methyl tri (methyl butynyloxy) silane are added into a kneader, vacuum stirring is carried out for 1.5h at 140 ℃, 6g of hydrogen-containing silicone oil and 0.01g of inhibitor methyl tri (methyl butynyloxy) silane are added after the temperature is reduced to 55 ℃, and stirring is continued for 1.5h, thus obtaining a component A;
and (3) pouring sealant B component: adding 50g of vinyl silicone oil, 18g of heat-conducting filler magnesium oxide and 1.5g of platinum catalyst chloroplatinic acid-isopropanol into a kneader, and stirring for 1.5h in vacuum at 140 ℃ to obtain a component B;
preparing a pouring sealant: mixing A, B components according to a mass ratio of 1: 1, uniformly mixing, defoaming in vacuum, and curing at 90 ℃ for 10 hours to obtain the low-density high-temperature-resistant pouring sealant.
Comparative example 1:
this comparative example differs from example 1 only in that no metal organic framework material is added.
And (3) performance testing: GB/T533-1991 'determination of vulcanized rubber Density' is adopted to test the density (g/cm) of the organosilicon potting adhesive after curing3) (ii) a And testing the heat-conducting property of the cured organic silicon potting adhesive by using a heat-conducting coefficient tester. The temperature of 5% of thermal weight loss after curing of the organic silicon potting adhesive is measured by TGA, and the temperature resistance of the potting adhesive is represented.
The performance test results are shown in table 1:
TABLE 1
As can be seen from Table 1, the higher the content of the metal-organic framework material in examples 1-4, the lower the density; the more the content of the heat-conducting filler is, the higher the heat conductivity is; and the high temperature resistance of the organic silicon pouring sealant added with the metal organic framework material is obviously superior to that of the organic silicon pouring sealant not added with the metal organic framework material.
Compared with the prior art, the invention has the following advantages:
1. the metal-organic framework material is a porous material, and is a crystalline porous material with a periodic network structure formed by self-assembly of transition metal ions and organic ligands. The organic ligand in the metal-organic framework material has stronger interaction with the polymer chain segment and can be uniformly dispersed in the polymer matrix. In addition, the metal-organic framework material has the advantages of high porosity, low density, large specific surface area, high temperature resistance and the like, wherein UiO-66-Br and UiO-66 can be kept stable at 450 ℃, and UiO-66-NH2 and UiO-66-NO2 can be kept stable at 350 ℃.
2. The metal-organic framework material is used as a filler to be added into the pouring sealant, so that the density of the pouring sealant can be reduced, and the temperature resistance of the pouring sealant can be improved.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept of the present invention, and these should also be construed as being within the scope of the present invention.
Claims (8)
1. The low-density high-temperature-resistant pouring sealant is characterized by comprising the following components in parts by weight: 100 parts of vinyl silicone oil, 10 to 20 parts of a cross-linking agent, 10 to 30 parts of a metal-organic framework material, 30 to 60 parts of a heat-conducting filler, 1 to 3 parts of a platinum catalyst and 0.01 to 0.1 part of an inhibitor.
2. The low-density high-temperature-resistant pouring sealant as claimed in claim 1, wherein the viscosity of the vinyl silicone oil is 2000 to 30000 mPa-s, and the vinyl content is 0.1 to 3.0%.
3. The low-density high-temperature-resistant pouring sealant as claimed in claim 1, wherein the cross-linking agent is hydrogen-containing silicone oil, and the viscosity of the hydrogen-containing silicone oil is 500 to 3000 mPa-s.
4. The low-density high-temperature-resistant pouring sealant as claimed in claim 1, wherein the metal-organic framework material is UiO-66, UiO-66-Br, UiO-66-NH2Or UiO-66-NO2One or more of (a).
5. The low-density high-temperature-resistant pouring sealant as claimed in claim 1, wherein the heat-conducting filler is one or more of graphene, silica micropowder, alumina, magnesium oxide and boron nitride.
6. The low-density high-temperature-resistant pouring sealant as claimed in claim 1, wherein the platinum catalyst is one of chloroplatinic acid-isopropanol or chloroplatinic acid-divinyltetramethyldisiloxane, wherein the platinum content is 3% o to 1% by mass.
7. The low-density high-temperature-resistant pouring sealant as claimed in claim 1, wherein the inhibitor is one or more of 2-methyl-3-butyn-2-ol, 3-methyl-1-hexyn-3-ol, 1-ethynylcyclohexanol, methyltris (methylbutynoxy) silane, phenyltri (methylbutynoxy) silane, vinyltri (methylbutynoxy) silane and polyvinyl polysiloxane.
8. The preparation method of the low-density high-temperature-resistant pouring sealant is characterized by comprising the following steps of:
the pouring sealant A comprises the following components: adding 50 parts of vinyl silicone oil, 10 to 20 parts of cross-linking agent, 10 to 30 parts of metal-organic framework material, 15 to 30 parts of heat-conducting filler and 0.01 to 0.1 part of inhibitor into a kneader, stirring for 1 to 3 hours in vacuum at 120 to 180 ℃, adding hydrogen-containing silicone oil and inhibitor after the temperature is reduced to 50 to 80 ℃, and continuing stirring for 1 to 3 hours to obtain a component A;
and (3) pouring sealant B component: adding 50 parts of vinyl silicone oil, 15-30 parts of heat-conducting filler and 1-3 parts of platinum catalyst into a kneader, and stirring for 1-3 hours in vacuum at 120-180 ℃ to obtain a component B;
preparing a pouring sealant: mixing A, B components according to a mass ratio of 1: 1, uniformly mixing, defoaming in vacuum, and curing at 80-120 ℃ for 2-12 h to obtain the low-density high-temperature-resistant pouring sealant.
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| CN114836038A (en) * | 2022-03-01 | 2022-08-02 | 浙江师范大学 | High-temperature-resistant silicon rubber and preparation method thereof |
| CN115491042A (en) * | 2022-10-24 | 2022-12-20 | 苏州泰吉诺新材料科技有限公司 | Heat conduction gasket with low oil permeability and low volatilization characteristics and preparation method thereof |
| CN115612303A (en) * | 2022-10-21 | 2023-01-17 | 安徽壹石通材料科技股份有限公司 | Oil-seepage-prevention anti-aging heat-conducting gel and preparation method thereof |
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Cited By (6)
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| CN113817178A (en) * | 2021-10-18 | 2021-12-21 | 深圳市德镒盟电子有限公司 | Low-oil-permeability high-heat-conductivity heat-conducting gel and preparation method thereof |
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| CN115612303A (en) * | 2022-10-21 | 2023-01-17 | 安徽壹石通材料科技股份有限公司 | Oil-seepage-prevention anti-aging heat-conducting gel and preparation method thereof |
| CN115612303B (en) * | 2022-10-21 | 2023-08-18 | 安徽壹石通材料科技股份有限公司 | Oil-seepage-proofing aging-resistant heat-conducting gel and preparation method thereof |
| CN115491042A (en) * | 2022-10-24 | 2022-12-20 | 苏州泰吉诺新材料科技有限公司 | Heat conduction gasket with low oil permeability and low volatilization characteristics and preparation method thereof |
| CN115491042B (en) * | 2022-10-24 | 2023-11-28 | 苏州泰吉诺新材料科技有限公司 | Low-oil-seepage and low-volatility heat conduction gasket and preparation method thereof |
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Application publication date: 20210420 |