CN113881230A - Ceramic silicone rubber for heat insulation of power battery and preparation method thereof - Google Patents
Ceramic silicone rubber for heat insulation of power battery and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 88
- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 79
- 238000009413 insulation Methods 0.000 title claims abstract description 43
- 239000004945 silicone rubber Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 65
- 239000000463 material Substances 0.000 claims abstract description 48
- 239000011521 glass Substances 0.000 claims abstract description 44
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000000741 silica gel Substances 0.000 claims abstract description 30
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 30
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 9
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 9
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 9
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 9
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000010445 mica Substances 0.000 claims abstract description 9
- 229910052618 mica group Inorganic materials 0.000 claims abstract description 9
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000006229 carbon black Substances 0.000 claims abstract description 8
- 239000000835 fiber Substances 0.000 claims abstract description 8
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229920002545 silicone oil Polymers 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims description 23
- 238000003756 stirring Methods 0.000 claims description 21
- 238000012360 testing method Methods 0.000 claims description 20
- 239000003795 chemical substances by application Substances 0.000 claims description 19
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- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910052717 sulfur Inorganic materials 0.000 claims description 6
- 239000011593 sulfur Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 238000003801 milling Methods 0.000 claims description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 7
- 239000003063 flame retardant Substances 0.000 abstract description 7
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- 239000000047 product Substances 0.000 description 19
- 239000002131 composite material Substances 0.000 description 9
- 238000002679 ablation Methods 0.000 description 6
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- 230000000694 effects Effects 0.000 description 5
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 229910052744 lithium Inorganic materials 0.000 description 4
- 238000002468 ceramisation Methods 0.000 description 3
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000000635 electron micrograph Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
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- 239000012466 permeate Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
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- 229910052604 silicate mineral Inorganic materials 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
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Images
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention particularly relates to ceramic silicone rubber for heat insulation of a power battery and a preparation method thereof. The ceramic silicon rubber comprises the following raw materials in parts by weight: 100 parts of silica gel, 5-20 parts of zinc borate, 6-15 parts of aluminum oxide, 5-10 parts of mica powder, 3-5 parts of kaolin, 10-25 parts of glass powder, 0.1-0.4 part of silane coupling agent, 5-20 parts of silicone oil, 20-30 parts of white carbon black, 4-10 parts of magnesium oxide and 10-20 parts of ceramic fiber. The ceramic silicon rubber has good mechanical property, flame retardant property and electrical conductivity, and is used for assembling power battery modules with aerogel or other materials to form heat insulation modules or displaying good impact resistance, heat insulation and flame retardant property when being independently assembled to form the heat insulation modules.
Description
Technical Field
The invention relates to the technical field of organic high molecular compounds, in particular to ceramic silicone rubber for heat insulation of a power battery and a preparation method thereof.
Background
With the rapid development of new energy automobiles and energy storage, lithium battery fires frequently occur, and because the lithium battery fires at a high speed and is harmful, the requirements on thermal protection materials are higher and higher. At present, ceramic silicon rubber is mostly used as a frame in heat insulation of lithium ion batteries of new energy automobiles, aerogel is used as a main heat insulation material, and the silicon rubber has the functions of heat insulation and vibration resistance among the batteries. The ceramic silicon rubber composite material combines the basic characteristics of the silicon rubber phase at normal temperature and the advantages of the ceramic phase at high temperature, so that the ceramic silicon rubber composite material can play different roles under different service working conditions, plays heat insulation and anti-vibration roles at normal temperature, can play a role in heat insulation and promotion of structure maintenance under the condition of high-temperature ignition, is often used for replacing the traditional ceramic silicon rubber of common silicon rubber, and is mainly used for insulating and temperature-resistant cables, the temperature-resistant cables pay attention to insulation, flame retardance and ceramic formation, and the coating layers of the cables, such as the shielding layer and the cross-linked polyethylene layer of the cables, are also taken into consideration, the structure is more complex for the ceramic silicon rubber for heat insulation of power batteries, and the production process is complex and difficult to automate. In addition, the lithium ion battery has the requirement of reducing the cost in new energy automobiles and energy storage, and a low-cost ceramic polymer composite material is adopted for the requirement.
The silicon rubber is a linear high molecular polymer with a main chain of Si-O-Si bond, SiO2The content is very high, and a large amount of SiO is generated in the ablation process2Can participate in the ceramic reaction of other components in the composite material, and is an ideal ceramic polymer matrix material. And the high-temperature vulcanized silicone rubber has excellent heat resistance, lower density and smaller heat conductivity coefficient, and can be widely used in the field of thermal protection. Various ceramic fillers, such as various metal and non-metal oxides such as: silicide, carbide, nitride, various silicate minerals and the like can be prepared into the silicon rubber composite material with excellent performance, which is suitable for the heat insulation of the lithium battery and can be used for ceramic according to the basic requirements of the heat insulation of the lithium battery. Wherein, Chinese patent CN 104629374A discloses a silicon rubber-based ablation-resistant heat-insulating composite material and a preparation method thereof; chinese patent CN 109206919A discloses a silicon rubber heat-insulating material and a preparation method thereof; chinese patent CN106433148A discloses a carbon fiber cloth reinforced/heat vulcanized rubber ablation-resistant composite material and a preparation method thereof; in the published patent documents, the provided ceramifiable silicon rubber composite material has the problem of high cost, is mainly used in the aerospace field, cannot realize large-scale machine production, is poor in industrial application, and is difficult to use in civil automobiles. Therefore, the ceramic silicone rubber material which is flame retardant at normal temperature, simple in high-temperature ceramic preparation process, low in cost and applicable to large-scale application is urgently needed to be developed, so that the ceramic silicone rubber material can be applicable to industrial implementation of new energy automobiles.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provide ceramic silicone rubber for heat insulation of a power battery, which has good mechanical property, flame retardance and electrical conductivity.
The invention also aims to provide ceramic silicone rubber for heat insulation of a power battery and a preparation method thereof.
The purpose of the invention is realized by the following technical scheme: the ceramic silicone rubber for heat insulation of the power battery comprises the following raw materials in parts by weight: 100 parts of silica gel, 5-20 parts of zinc borate, 6-15 parts of aluminum oxide, 5-10 parts of mica powder, 3-5 parts of kaolin, 10-25 parts of glass powder, 0.1-0.4 part of silane coupling agent, 5-20 parts of silicone oil, 20-30 parts of white carbon black, 4-10 parts of magnesium oxide and 10-20 parts of ceramic fiber.
According to the invention, silica gel is used as a matrix, and the ceramic silicone rubber with good mechanical property, strong ablation resistance and strong flame retardance is prepared by mixing and compounding the components. The mica powder, kaolin and ceramic fiber are used as ceramic forming fillers, so that the strength and the ceramic property of a ceramic body can be effectively improved, the addition of zinc borate, aluminum oxide and magnesium oxide is beneficial to improving the thermal stability and the flame retardance of silicon rubber, the white carbon black is also used as a reinforcing agent for improving the strength of the ceramic silicon rubber, and the addition of the silicon oil and the silane coupling agent enables materials in the preparation process to keep good processing performance, and improves the crosslinking density and the bonding strength among the components. When the ceramic silicon rubber is burnt in fire or high temperature, the ceramic silicon rubber can be converted into a multi-component composite phase ceramic body with self-supporting property, the effect of isolating oxygen and heat is enhanced, the further burning of a matrix is prevented, and a good flame-retardant effect is achieved.
Preferably, the glass powder is at least one of high-temperature glass powder, medium-temperature glass powder and low-temperature glass powder. Specifically, the low-temperature glass powder refers to glass powder with a softening point of less than 400 ℃, the medium-temperature glass powder refers to glass powder with a softening point of between 400 ℃ and 650 ℃, and the high-temperature glass powder refers to glass powder with a softening point of more than 650 ℃.
Preferably, the weight ratio of the glass powder to the silane coupling agent is 100: 1-2.
Preferably, the amount of the silane coupling agent is 0.3-1.5% of the amount of the glass powder.
In the invention, the addition of the glass powder is beneficial to improving the bonding effect among particles and increasing the strength of the obtained ceramic silicon rubber. In addition, the addition of the glass powder with different melting points can adjust the ceramic transition temperature of the ceramic silicon rubber, so that the bonding effect among the component particles is more obvious, and the compactness and the strength of the ceramic body are favorably enhanced. However, the dosage of the glass powder is not suitable to be too high, and the addition of the glass powder with high dosage is easy to cause the reduction of the thermal stability of the silicon rubber, so that the ablation performance of the material is not improved. Therefore, the weight ratio of the glass frit to the silane coupling agent is strictly defined in the present invention to be 100: 1-2.
The other purpose of the invention is realized by the following technical scheme: a preparation method of ceramic silicon rubber for power battery heat insulation comprises the following steps:
s1, powder proportioning: weighing and mixing the powder in corresponding parts by weight according to the proportion;
s2, banburying and stirring: adding silica gel and the powder obtained in the step S1 into an internal mixer, cooling with cooling water, cooling, stirring, and stirring under pressure for 300 seconds to uniformly mix the materials;
s3, cooling and aging: placing the material obtained in the step S2 in a normal temperature environment for cooling, and storing for at least one week to ensure that the material is fully permeated;
s4, adding sulfur and remilling: adding a vulcanizing agent and the material obtained in the step S3 into an open mill for remilling for 10-15min to prepare ceramic silica gel;
s5, tabletting: pressing the ceramic silica gel material obtained in the step S4 on a three-roll calender to form a formed product with the required thickness;
s6, vulcanization molding: and (5) putting the molded product obtained in the step S5 into a mold or an oven, heating, hot-pressing and vulcanizing to obtain the silicon rubber test piece.
Preferably, in step S2, the internal mixer is stirred at 50-60 deg.C and 80-300 r/min. More preferably, the stirring speed of the internal mixer is 150-200 r/min.
Preferably, in step S4, the vulcanizing agent is DBTB, and the material temperature of the open mill is 40-50 ℃.
Preferably, the adding amount of the vulcanizing agent is 9-15 per mill of the adding weight of the material obtained in the step S3.
Preferably, the sheeting is performed in step S5, the thickness of the molded product is adjusted according to the thickness of the product, and the linear speed of the three-roll calender is 0.8-1.5 m/min.
Preferably, the step S6 is carried out for molding vulcanization molding, wherein the molding temperature is 155-165 ℃, and the molding time is 3-5 min.
Preferably, in step S6, an oven vulcanization molding is performed, wherein the oven temperature is 160-170 ℃, and the baking time is 7-10 min.
The preparation method is simple and controllable, mild in condition, safe and environment-friendly and low in production cost, the silica gel and the powder raw materials are fully mixed through the step S2, the components are completely permeated through cooling and aging for more than one week, the processability and compatibility of the mixed material are obviously improved, a vulcanizing agent is added for open milling, the crosslinking density of the silica gel is improved, a formed product with the required thickness is pressed through a three-roll calender, and finally the formed product is heated and vulcanized to form the ceramic silica gel.
The invention has the beneficial effects that: the ceramic silicon rubber for heat insulation of the power battery has good mechanical property, flame retardance and electrical conductivity, is used for being combined with aerogel or other materials among battery modules to form a heat insulation module, or is independently assembled to form the heat insulation module, can bear stronger impact on a battery pack box body, has good pressure resistance and high thermal stability, and is beneficial to heat insulation of the battery modules. Moreover, the silicone rubber provided by the invention is simple in preparation process, low in production cost, safe and environment-friendly, and suitable for large-scale industrial implementation.
Drawings
FIG. 1 is an electron micrograph of a ceramicized silicone rubber prepared in example 2 of the present invention.
Fig. 2 is a partially enlarged view of fig. 1.
FIG. 3 is a TGA profile of a ceramic silicone rubber prepared according to example 2 of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples for facilitating understanding of those skilled in the art, and the description of the embodiments is not intended to limit the present invention.
As a typical embodiment of the invention, the ceramic silicone rubber for heat insulation of the power battery comprises the following raw materials in parts by weight: 100 parts of silica gel, 5-20 parts of zinc borate, 6-15 parts of aluminum oxide, 5-10 parts of mica powder, 3-5 parts of kaolin, 10-25 parts of glass powder, 0.1-0.4 part of silane coupling agent, 5-20 parts of silicone oil, 20-30 parts of white carbon black, 4-10 parts of magnesium oxide and 10-20 parts of ceramic fiber.
In a typical embodiment of the present invention, the glass frit is at least one of a high-temperature glass frit, a medium-temperature glass frit, and a low-temperature glass frit.
In a typical embodiment of the present invention, the weight ratio of the glass frit to the silane coupling agent is 100: 1-2. More preferably, the amount of the silane coupling agent is 0.3 to 1.5% of the amount of the glass frit.
The preparation method of the ceramic silicon rubber for heat insulation of the power battery comprises the following steps:
s1, powder proportioning: weighing and mixing the powder in corresponding parts by weight according to the proportion;
s2, banburying and stirring: adding silica gel and the powder obtained in the step S1 into an internal mixer, cooling with cooling water, cooling, stirring, and stirring under pressure for 300 seconds to uniformly mix the materials;
s3, cooling and aging: placing the material obtained in the step S2 in a normal temperature environment for cooling, and storing for at least one week to ensure that the material is fully permeated;
s4, adding sulfur and remilling: adding a vulcanizing agent and the material obtained in the step S3 into an open mill for remilling for 10-15min to prepare ceramic silica gel;
s5, tabletting: pressing the ceramic silica gel material obtained in the step S4 on a three-roll calender to form a formed product with the required thickness;
s6, vulcanization molding: and (5) putting the molded product obtained in the step S5 into a mold or an oven, heating, hot-pressing and vulcanizing to obtain the silicon rubber test piece.
In step S2, the internal mixer is stirred at 50-60 deg.C and at 80-300 rpm. More preferably, the stirring speed of the internal mixer is 150-200 r/min.
In a typical embodiment of the present invention, in step S4, the vulcanizing agent is DBTB, and the batch temperature of the open mill is 40 to 50 ℃.
In a typical embodiment of the present invention, the vulcanizing agent is added in an amount of 9 to 15 per mill of the weight of the material obtained in step S3.
As a typical embodiment of the present invention, sheeting is performed in step S5, the thickness of the molded product is adjusted according to the product thickness, and the line speed of the three-roll calender is 0.8 to 1.5 m/min.
As a typical embodiment of the present invention, the step S6 is a step of molding vulcanization molding, wherein the molding temperature is 155-165 ℃, and the molding time is 3-5 min.
As a typical embodiment of the present invention, the oven vulcanization molding is performed in step S6, the oven temperature is 160-170 ℃, and the baking time is 7-10 min.
Example 1
The ceramic silicone rubber for heat insulation of the power battery comprises the following raw materials in parts by weight: 100 parts of silica gel, 5 parts of zinc borate, 6 parts of aluminum oxide, 5 parts of mica powder, 3 parts of kaolin, 10 parts of glass powder, 0.15 part of silane coupling agent, 6 parts of silicone oil, 20 parts of white carbon black, 4 parts of magnesium oxide and 10 parts of ceramic fiber.
Preferably, the glass powder is a mixture of medium-temperature glass powder and low-temperature glass powder in a mass ratio of 1: 2.5.
The preparation method of the ceramic silicon rubber for heat insulation of the power battery comprises the following steps:
s1, powder proportioning: weighing and mixing the powder in corresponding parts by weight according to the proportion;
s2, banburying and stirring: adding silica gel and the powder obtained in the step S1 into an internal mixer, cooling with cooling water, cooling, stirring, and stirring under pressure for 300 seconds to uniformly mix the materials;
s3, cooling and aging: placing the material obtained in the step S2 in a normal temperature environment for cooling, and storing for one week to fully permeate the material;
s4, adding sulfur and remilling: adding a vulcanizing agent and the material obtained in the step S3 into an open mill for remilling for 10min to prepare ceramic silica gel;
s5, tabletting: pressing the ceramic silica gel material obtained in the step S4 on a three-roll calender to form a formed product with the required thickness;
s6, vulcanization molding: and (5) putting the molded product obtained in the step S5 into an oven, heating, hot-pressing and vulcanizing to obtain the silicon rubber test piece.
Preferably, in step S2, the internal mixer is stirred at 50 ℃ and 80 rpm.
Preferably, in step S4, the vulcanizing agent is DBTB, and the material temperature of the open mill is 40 ℃.
Preferably, the adding amount of the vulcanizing agent is 9 per mill of the adding amount of the material obtained in the step S3.
Preferably, the thickness of the molded product is 2mm, and the linear speed of the three-roll calender is 0.8 m/min.
Preferably, in step S6, the oven temperature is 160 ℃, and the baking time is 7 min.
Example 2
The ceramic silicone rubber for heat insulation of the power battery comprises the following raw materials in parts by weight: 100 parts of silica gel, 12 parts of zinc borate, 10 parts of aluminum oxide, 8 parts of mica powder, 3 parts of kaolin, 20 parts of glass powder, 0.3 part of silane coupling agent, 14 parts of silicone oil, 25 parts of white carbon black, 6 parts of magnesium oxide and 15 parts of ceramic fiber.
Preferably, the glass powder is a mixture of high-temperature glass powder and low-temperature glass powder in a mass ratio of 1:2.
The preparation method of the ceramic silicon rubber for heat insulation of the power battery comprises the following steps:
s1, powder proportioning: weighing and mixing the powder in corresponding parts by weight according to the proportion;
s2, banburying and stirring: adding silica gel and the powder obtained in the step S1 into an internal mixer, cooling with cooling water, cooling, stirring, and stirring under pressure for 300 seconds to uniformly mix the materials;
s3, cooling and aging: placing the material obtained in the step S2 in a normal temperature environment for cooling, and storing for one week to fully permeate the material;
s4, adding sulfur and remilling: adding a vulcanizing agent and the material obtained in the step S3 into an open mill for remilling for 12min to prepare ceramic silica gel;
s5, tabletting: pressing the ceramic silica gel material obtained in the step S4 on a three-roll calender to form a formed product with the required thickness;
s6, vulcanization molding: and (5) putting the molded product obtained in the step S5 into a mold, heating, hot-pressing and vulcanizing to obtain the silicon rubber test piece.
Preferably, in step S2, the internal mixer is stirred at a temperature of 60 ℃ and a stirring speed of 150 rpm.
Preferably, in step S4, the vulcanizing agent is DBTB, and the material temperature of the open mill is 45 ℃.
Preferably, the adding amount of the vulcanizing agent is 12 per mill of the adding amount of the material obtained in the step S3.
Preferably, the thickness of the formed product is 2.3mm, and the linear speed of the three-roller calender is 1.2 m/min.
Preferably, in step S6, the temperature of the mold is 160 ℃, and the pressing time of the mold is 4 min.
Example 3
The ceramic silicone rubber for heat insulation of the power battery comprises the following raw materials in parts by weight: 100 parts of silica gel, 20 parts of zinc borate, 13 parts of aluminum oxide, 9 parts of mica powder, 5 parts of kaolin, 22 parts of glass powder, 0.4 part of silane coupling agent, 20 parts of silicone oil, 28 parts of white carbon black, 10 parts of magnesium oxide and 20 parts of ceramic fiber.
Preferably, the glass powder is a mixture of high-temperature glass powder and low-temperature glass powder in a ratio of 1: 1.25.
The preparation method of the ceramic silicon rubber for heat insulation of the power battery comprises the following steps:
s1, powder proportioning: weighing and mixing the powder in corresponding parts by weight according to the proportion;
s2, banburying and stirring: adding silica gel and the powder obtained in the step S1 into an internal mixer, cooling with cooling water, cooling, stirring, and stirring under pressure for 300 seconds to uniformly mix the materials;
s3, cooling and aging: placing the material obtained in the step S2 in a normal temperature environment for cooling, and storing for at least one week to ensure that the material is fully permeated;
s4, adding sulfur and remilling: adding a vulcanizing agent and the material obtained in the step S3 into an open mill for remilling for 15min to prepare ceramic silica gel;
s5, tabletting: pressing the ceramic silica gel material obtained in the step S4 on a three-roll calender to form a formed product with the required thickness;
s6, vulcanization molding: and (5) putting the molded product obtained in the step S5 into an oven, heating, hot-pressing and vulcanizing to obtain the silicon rubber test piece.
Preferably, in step S2, the internal mixer is stirred at a temperature of 60 ℃ and a stirring speed of 300 rpm.
Preferably, in step S4, the vulcanizing agent is DBTB, and the material temperature of the open mill is 45 ℃.
Preferably, the adding amount of the vulcanizing agent is 15 per mill of the adding amount of the material obtained in the step S3.
Preferably, the thickness of the molded product is 3mm, and the linear speed of the three-roll calender is 1.5 m/min.
Preferably, in step S6, the oven temperature is 170 ℃, and the baking time is 10 min.
Comparative example 1
This comparative example differs from example 2 in that: the ceramic silicone rubber for heat insulation of the power battery comprises the following raw materials in parts by weight: 100 parts of silica gel, 12 parts of zinc borate, 10 parts of alumina, 8 parts of mica powder, 3 parts of kaolin, 0.3 part of silane coupling agent, 14 parts of silicone oil and 6 parts of magnesium oxide.
The preparation method of the ceramic silicon rubber for the heat insulation of the power battery in the comparative example is the same as that of the example 2.
The ceramic silicone rubber test piece obtained in example 2 was subjected to electron microscopy analysis and TGA test. Specifically, the test piece prepared in example 2 was placed in a muffle furnace, heated to 800 ℃ at a rate of 5 ℃/min and calcined for 40min, and the obtained test piece was observed for the porcelain formation on the surface with a microscope; the TGA test of the sample was carried out on the test piece obtained in example 2 by using a thermogravimetric analyzer TA Q550 (ASTM E1131-20), and the temperature was raised from 40 ℃ at an initial temperature of 10 ℃/min to 600 ℃ in a nitrogen atmosphere, and the temperature was further raised to 750 ℃ by switching nitrogen to air. The ceramic silicone rubber test pieces obtained in the above examples 1 to 3 and comparative example 1 were subjected to mechanical properties and flame retardancy. Specifically, a hardness meter is adopted to measure the Shore hardness of the test piece, and the test standard is GB/T531-2008; the flame retardant rating of the test was determined using the UL94HB standard test method.
Fig. 1-2 are electron micrographs of the test piece obtained in example 2, and it can be seen from fig. 1 that the surface of the ceramming silicone rubber test piece obtained in example 2 is a dense and porous continuous structure, and after amplification, no obvious particles are observed on the surface of fig. 2, the surface is dense and forms a continuous phase, which indicates that the ceramming filler and the cosolvent in the raw materials of the present invention are fully melted at 800 ℃, the components are completely penetrated and have high bonding strength, and a continuous, complete and dense ceramic body structure is formed, thereby indicating that the silicone rubber of the present invention realizes a high ceramming effect. FIG. 3 is a TGA graph of the ceramic silicone rubber obtained in example 2. from FIG. 3, it can be seen that the ceramic silicone rubber of example 2 of the present invention is divided into three stages in the temperature rising process, and at first, the weight of the ceramic silicone rubber is reduced by 4.201% below 325 ℃, which is mainly caused by the softening and melting of the flux component; the weight of the ceramic silicon rubber is reduced by 36.310% between 325 and 575 ℃, which is mainly caused by the cross-linking bond and main chain decomposition of the ceramic silicon rubber, and the melting is fully and gradually vitrified in the process; the ceramization transformation of the silicon rubber is formed between 575 and 750 ℃, and the residual quantity of the ceramization silicon rubber after 750 ℃ is 53.196%, thereby showing that the ceramization silicon rubber has high heat resistance stability and strong ablation resistance.
As can be seen from the data in the table, through the selection and combination of the raw material components and the optimization of the preparation method, the ceramic silicon rubber prepared in the examples 1-3 has good mechanical properties and flame retardant properties, and shows good compression resistance in a compression resistance test, the ceramic silicon rubber prepared in the examples 1-3 achieves the UL 94V 0 grade in the flame retardant test, and shows excellent flame resistance when the burning time is more than 3h under the continuous burning condition of the flame of a butane spray gun at the temperature of more than or equal to 1000 ℃, while the mechanical properties and the compression resistance of the ceramic silicon rubber prepared in the comparative example 1 are obviously reduced.
The above specific examples are further illustrative of the technical solutions and advantages of the present invention, and are not intended to limit the embodiments. It will be apparent to those skilled in the art that any obvious alternative is within the scope of the invention without departing from the inventive concept.
Claims (10)
1. The ceramic silicon rubber for heat insulation of the power battery is characterized in that: the feed comprises the following raw materials in parts by weight: 100 parts of silica gel, 5-20 parts of zinc borate, 6-15 parts of aluminum oxide, 5-10 parts of mica powder, 3-5 parts of kaolin, 10-25 parts of glass powder, 0.1-0.4 part of silane coupling agent, 5-20 parts of silicone oil, 20-30 parts of white carbon black, 4-10 parts of magnesium oxide and 10-20 parts of ceramic fiber.
2. The ceramicized silicone rubber for power battery insulation according to claim 1, wherein: the glass powder is at least one of high-temperature glass powder, medium-temperature glass powder and low-temperature glass powder.
3. The ceramicized silicone rubber for power battery insulation according to claim 2, wherein: the weight ratio of the glass powder to the silane coupling agent is 100: 1-2.
4. A method for producing a ceramicized silicone rubber for thermal insulation of a power battery according to any one of claims 1 to 3, characterized in that: the method comprises the following steps:
s1, powder proportioning: weighing and mixing the powder in corresponding parts by weight according to the proportion;
s2, banburying and stirring: adding silica gel and the powder obtained in the step S1 into an internal mixer, and pressurizing and stirring to uniformly mix the materials;
s3, cooling and aging: placing the material obtained in the step S2 in a normal temperature environment for cooling, and storing for at least one week;
s4, adding sulfur and remilling: adding a vulcanizing agent and the material obtained in the step S3 into an open mill for back-milling to obtain a ceramic silica gel;
s5, tabletting: pressing the ceramic silica gel material obtained in the step S4 on a three-roll calender to form a formed product with the required thickness;
s6, vulcanization molding: and (5) putting the formed product obtained in the step (S5) into a mold to carry out mold pressing or oven heating vulcanization, thus obtaining the silicon rubber test piece.
5. The preparation method of the ceramic silicone rubber for the thermal insulation of the power battery according to claim 4 is characterized by comprising the following steps: in step S2, the internal mixer is stirred at 50-60 deg.C and at 80-300 r/min.
6. The preparation method of the ceramic silicone rubber for the thermal insulation of the power battery according to claim 4 is characterized by comprising the following steps: in step S4, the vulcanizing agent is DBTB, and the material temperature of the open mill is 40-50 ℃.
7. The preparation method of the ceramic silicone rubber for the thermal insulation of the power battery according to claim 4 is characterized by comprising the following steps: in step S4, the addition amount of the vulcanizing agent is 9-15 per mill of the addition weight of the material obtained in step S3.
8. The preparation method of the ceramic silicone rubber for the thermal insulation of the power battery according to claim 4 is characterized by comprising the following steps: and (S5) tabletting, wherein the thickness of the formed product is adjusted according to the thickness of the product, and the linear speed of the three-roller calender is 0.8-1.5 m/min.
9. The preparation method of the ceramic silicone rubber for the thermal insulation of the power battery according to claim 4 is characterized by comprising the following steps: and (4) performing mould pressing vulcanization molding in step S6, wherein the mould pressing temperature is 155-165 ℃, and the mould pressing time is 3-5 min.
10. The preparation method of the ceramic silicone rubber for the thermal insulation of the power battery according to claim 4 is characterized by comprising the following steps: and S6, carrying out oven vulcanization molding, wherein the oven temperature is 160-170 ℃, and the baking time is 7-10 min.
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