CN114672170A - Heat insulation material and lithium battery heat insulation protection pad - Google Patents
Heat insulation material and lithium battery heat insulation protection pad Download PDFInfo
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Abstract
The invention discloses a heat insulation material, which comprises the following components: 107 silicon rubber, vinyl silicone oil, heat conducting powder, reinforcing filler, a halogen-free flame retardant, a cross-linking agent, a catalyst, an antioxidant and an inhibitor, wherein the bentonite modified by polydopamine and triisopropylphenyl phosphate is added, so that the high free energy of the surface of the bentonite is reduced, the hydrophobicity is improved, the polarity is reduced, and the uniform dispersion of the bentonite in a silicon rubber matrix is improved, thereby improving the mechanical property of the material.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a heat insulation material and a lithium battery heat insulation protection pad.
Background
The performance of the power battery determines the performance of the electric automobile to a great extent, and compared with the traditional rechargeable battery, the lithium battery has the advantages of high working voltage, large specific energy, long cycle life, low self-discharge rate, no memory effect and the like, so the lithium battery becomes the most widely applied power battery of the electric automobile in recent years.
As a power source of an electric vehicle, the performance and life of a battery pack are regarded as important. The battery pack is formed by serially connecting single batteries, the interval between the single batteries is small, and the heat dissipation is easy to be uneven during charging and discharging, so that the temperature among the batteries is uneven, and the problems of poor overall discharging performance, short service life and the like of the battery pack are caused. Meanwhile, under the conditions of high-rate discharge such as acceleration of the electric automobile, if heat dissipation is not timely, a large amount of heat can be accumulated in a short time, so that the temperature of the lithium battery pack rises sharply, and even serious accidents such as explosion caused by thermal runaway can occur.
In the safety requirement of the power storage battery for the electric vehicle, the battery pack or the system needs to provide an alarm signal 5min before danger occurs in a passenger cabin due to thermal runaway of the battery and thermal diffusion of the air, so as to remind people to evacuate, and the higher requirement is provided for thermal safety protection of the power battery. The power battery has complex use working conditions, the thermal runaway phenomenon of the power battery cannot be completely avoided, the spread of the thermal runaway of the battery monomer in the module is inhibited or even blocked, and the power battery is an important means for ensuring the life and property safety of vehicle passengers.
In recent years, scholars at home and abroad make a lot of improvement work on the aspect of battery thermal runaway suppression, such as: the battery pack is stored and used at a proper temperature through the box body coated with the heat insulation layer module, and the balance of the battery module environment is improved; the propagation of thermal runaway of the power battery is inhibited through the water mist, but the design for inhibiting the thermal runaway by adopting the water mist is complex, and a fire extinguishing system is difficult to integrate on a pure electric vehicle; asbestos cloth is also selected as a heat insulation layer between batteries to successfully block the spread of thermal runaway, but the asbestos cloth has great harm to human bodies and cannot be applied to blocking the thermal spread. Therefore, there is a need for a heat insulating material that can effectively insulate heat and is harmless to the human body.
CN107141808A discloses a heat-conducting temperature-resistant silicon foam material and a preparation method thereof, wherein 20-45 parts of silicon rubber, 10-25 parts of silicon resin and 5-15 parts of reinforcing agent are milled in an open mill for 10-30 minutes at normal temperature, then 0-1 part of pigment, 2-5 parts of heat-conducting filler, 3-10 parts of curing agent and 5-15 parts of foaming agent are added, and the milling is continued until the mixture is uniform. Pressing the milled material into a sheet with a certain thickness by using hot-pressing equipment, heating the sheet in a drying tunnel at 180 ℃ for 3-5 minutes to completely foam the sheet, and then performing molding press polishing treatment in press polishing equipment to obtain the 0.3-5 MM silicon foam. The silicon foam prepared by the method has good thermal conductivity and buffer resistance, can resist the temperature of-60-260 ℃, and can be applied to hot pressing occasions with higher buffer requirements. Although the silicon foam prepared by the method has good heat conduction and temperature resistance, the silicon foam still has the defect of easy combustion when being applied to a high-temperature environment.
Disclosure of Invention
In view of the above defects in the prior art, the technical problem to be solved by the present invention is to provide a thermal insulation material which is harmless to human body, can delay thermal runaway of a lithium battery pack, and is flame retardant.
In order to achieve the purpose of the invention, the invention adopts the following technical scheme:
a heat insulation material is a silicon rubber foam material and comprises the following components: 107 silicon rubber, vinyl silicone oil, heat-conducting powder, reinforcing filler, halogen-free flame retardant, crosslinking agent, catalyst, antioxidant and inhibitor.
Preferably, the heat insulation material comprises the following components in parts by weight: 80-120 parts of 107 silicon rubber, 5-10 parts of vinyl silicone oil, 10-30 parts of heat-conducting powder, 20-40 parts of reinforcing filler, 30-80 parts of halogen-free flame retardant, 8-15 parts of cross-linking agent, 0.2-1 part of catalyst, 0.3-0.8 part of antioxidant and 0.1-0.3 part of inhibitor.
Preferably, the heat-conducting powder is one or a mixture of two or more of aluminum oxide, magnesium oxide, zinc oxide, aluminum nitride, boron nitride, silicon carbide and heat-conducting carbon powder; further preferably, the heat conductive powder is silicon carbide.
Preferably, the reinforcing filler is one of fumed silica, rutile titanium dioxide and acetylene-based carbon black; further preferably, the reinforcing filler is fumed silica; most preferably, the fumed silica modified by the silane coupling agent; the silane coupling agent modified fumed silica can be better dispersed in a silicon rubber matrix and can be crosslinked with Si-O-Si bonds of silicon rubber, and when the silicon rubber foam is subjected to an external force, the silicone rubber foam can be used as a stress point to disperse stress, so that the tear strength and the elongation of the material are improved; the preparation method of the silane coupling agent modified fumed silica comprises the following steps:
(1) 0.05-1 part of sodium dodecyl sulfate and 2-3 parts of gas phase SiO2Adding into 10-30 parts of 50-75 wt% ethanol water solution, stirring, performing ultrasonic treatment for 0.5-1 hr, heating to 60-80 deg.C, adding 0.5-1 part of gamma-methacryloxypropyltrimethoxysilane dropwise, reacting at constant temperature for 2-3 hr, washing with ethanol, and centrifuging to obtain KH570-SiO2；
(2) Mixing KH570-SiO2Adding into 30-50 parts of 50-75 wt% ethanol water solution, dripping 0.1-0.3 part of hydroxy silicone oil and 1-2 parts of dibutyltin dilaurate, and stirring at 25-35 deg.CAnd after 3-5 hours, washing with absolute ethyl alcohol, and centrifuging to obtain the silane coupling agent modified fumed silica.
The foam material can play a role in sealing and protecting the battery pack, is a compressible high-molecular foam material with organic and inorganic properties, porous and low-density, and has the advantages of light weight, heat insulation, sound insulation and the like. Compared with polyurethane foam, the general silicone rubber foam has better high-low temperature service performance, can not become brittle after being used at high temperature for a long time, has certain flame retardant performance due to unique silicon-oxygen bonds, but has a large number of unstable organic groups on side chains, and the foamed foam holes increase the contact area with oxygen, can burn at high temperature and can not meet the use requirement of a lithium battery pack; in order to increase the flame retardant property of the silicon rubber foam, a flame retardant is generally added into the silicon rubber foam, but the flame retardant containing halogen can release harmful gas during combustion to influence the health of people and pollute the environment; and the tearing resistance and the pressure change performance of the silicon rubber foam are poor, so that the silicon rubber foam is not beneficial to sealing and can be used as a buffer piece for a long time.
Preferably, the halogen-free flame retardant is modified bentonite, and the preparation method comprises the following steps:
1) adding bentonite into a dilute sulfuric acid solution for reaction, filtering, washing and drying to obtain pretreated bentonite;
2) preparing a dopamine hydrochloride aqueous solution, adding a Tris buffer solution, heating, centrifuging, filtering and drying after the reaction is finished to obtain poly-dopamine;
3) adding the pretreated bentonite into absolute ethyl alcohol, stirring uniformly, adding polydopamine and triisopropylphenyl phosphate, heating for reaction, cooling, filtering and drying to obtain modified bentonite;
further preferably, the preparation method of the modified bentonite is as follows:
1) roasting bentonite at the temperature of 200-300 ℃ for 2-4h, cooling to 20-40 ℃, grinding, sieving with a 500-mesh sieve with 600 meshes, adding the obtained product into 10-20 wt% dilute sulfuric acid solution, heating to 80-90 ℃ for reaction for 2-4h, filtering, collecting filter cakes, washing the filter cakes with water until the pH value is 6.5-7.5, and drying in a drying box at the temperature of 60-80 ℃ for 6-8h to obtain pretreated bentonite;
2) preparing 20-30 wt% dopamine hydrochloride aqueous solution, adjusting the pH value to 8-9, adding Tris buffer solution, uniformly mixing, heating to 30-50 ℃, reacting for 1-2h, centrifuging, filtering and collecting filter residue, washing the filter residue with water for 2-3 times, and freeze-drying at-40 to-45 ℃ for 24-48 h to obtain polydopamine;
3) adding the pretreated bentonite into absolute ethyl alcohol, stirring uniformly, adding polydopamine and triisopropylphenyl phosphate, heating to 80-100 ℃, carrying out reflux reaction for 20-24h, cooling to 20-40 ℃, filtering, collecting a filter cake, and drying at 60-80 ℃ for 6-8h to obtain the modified bentonite.
Further preferably, the dosage ratio of the bentonite to the dilute sulfuric acid solution in the step 1) is 1-2g:30-40 mL.
Further preferably, the dosage ratio of the dopamine hydrochloride aqueous solution to the Tris buffer solution in the step 2) is 2-4: 1-3.
Further preferably, the dosage ratio of the pretreated bentonite, the absolute ethyl alcohol, the polydopamine and the triisopropylphenyl phosphate in the step 3) is 6-10 g: 50-80 mL: 1-2g: 2-3 g.
The bentonite is an aqueous clay mineral mainly containing montmorillonite, has good thermal stability and chemical stability, can play a role in enhancing and improving adhesion force and can also improve the functions of flame retardance, insulation, wear resistance, corrosion resistance and the like of a product, but the surface of the bentonite is hydrophilic and oleophobic, is strong in polarity, has a large specific surface area and a high surface free energy, is easy to agglomerate in a silicon rubber system and difficult to uniformly disperse, influences the flame retardance synergistic effect, and is poor in binding force with a silicon rubber matrix, so that the performance of the material is easily reduced. The inventor treats bentonite by polydopamine and triisopropylphenyl phosphate, so that the high free energy of the surface of the bentonite is reduced, the hydrophobicity of the bentonite is improved, the polarity of the bentonite is reduced, the uniform dispersion of the bentonite in a silicon rubber matrix is improved, the mechanical property of the material is improved, meanwhile, the polydopamine and the triisopropylphenyl phosphate can form nitrogen-phosphorus synergistic flame retardance, the triisopropylphenyl phosphate plays a role in a condensed phase to promote the matrix to form carbon, the polydopamine generates non-combustible gas in a gas phase to achieve the synergistic flame retardance effect, and in addition, a rigid benzene ring structure in the triisopropylphenyl phosphate enables the flame retardance and the thermal stability of the bentonite to be more excellent.
Preferably, the cross-linking agent is polymethylhydrosiloxane.
Preferably, the catalyst is a platinum catalyst; the platinum catalyst can promote the crosslinking reaction of the silicon rubber and increase the crosslinking density, thereby improving the mechanical property of the material and simultaneously improving the flame retardant property of the material.
Preferably, the antioxidant is 2, 8-di-tert-butyl-4-methylphenol.
Preferably, the inhibitor is alkynylcyclohexanol.
The invention also provides a preparation method of the heat insulation material, which comprises the following steps:
s1, weighing the raw materials according to the formula, mixing 107 silicon rubber, vinyl silicone oil, heat-conducting powder, reinforcing filler, halogen-free flame retardant, antioxidant and inhibitor, heating and stirring uniformly, and then vacuumizing to obtain a mixture 1;
s2, adding a cross-linking agent and a catalyst into the mixture 1 to obtain a mixture 2;
s3, coating the mixture 2 on the surface of a release film, placing the release film in the air for foaming, and drying and separating the release film to obtain the heat insulation material.
Preferably, the preparation method of the heat insulation material comprises the following steps:
s1, mixing 80-120 parts of 107 silicone rubber, 5-10 parts of vinyl silicone oil, 10-30 parts of heat-conducting powder, 20-40 parts of reinforcing filler, 30-80 parts of halogen-free flame retardant, 8-15 parts of antioxidant and 0.2-1 part of inhibitor, heating to 60-90 ℃, stirring for 60-90min at the stirring speed of 50-80 r/min, vacuumizing, and continuously stirring for 20-30min to obtain a mixture 1;
s2, adding 8-15 parts of cross-linking agent and 0.2-1 part of catalyst into the mixture 1, and stirring for 10-30min at the stirring speed of 40-60 r/min to obtain a mixture 2;
s3, coating the mixture 2 on the surface of a PET release film, placing the PET release film in the air, soaking the PET release film for 3-5min at 20-40 ℃, placing the PET release film in an oven at 60-80 ℃ for drying for 5-10min, cooling to 20-40 ℃, and separating the PET release film to obtain the heat insulation material.
The invention also discloses a lithium battery heat-preservation protection pad which is formed by cutting the heat-insulation material according to the processing size or cutting the heat-insulation material and the aluminizer after being bonded in a glue hot-pressing mode according to the processing size.
Compared with the prior art, the invention has the beneficial effects that:
the halogen-free flame retardant prepared by the invention does not contain halogen elements, is an environment-friendly flame retardant material, improves the dispersibility of the bentonite in a silicon rubber matrix material and improves the mechanical property of the material by modifying the bentonite with polydopamine and triisopropylphenyl phosphate, and the triisopropylphenyl phosphate can form nitrogen-phosphorus synergistic flame retardant, and the rigid benzene ring structure in the triisopropylphenyl phosphate molecule ensures that the flame retardant property and the thermal stability are more excellent.
Detailed Description
The present invention will be described in further detail with reference to the following specific examples. The procedures, conditions, experimental methods and the like for carrying out the present invention are common knowledge and common general knowledge in the art except for the contents specifically mentioned below, and the present invention is not particularly limited.
For the sake of brevity, the articles used in the following examples are all commercially available products unless otherwise specified, and the methods used are conventional methods unless otherwise specified.
The invention uses part of raw materials with the following sources:
107 silicone rubber, CAS No.: 63148-60-7, viscosity of 20000 mPas, metal ion content not more than 20ppm, Shenzhen Jipeng silicon fluoride materials Limited.
Polymethylhydrosiloxane, CAS number 63148-57-2, boiling point 142 ℃, hydrogen content 1.6-1.62%, Shandong PolyChemicals, Inc.
SiO2Aerogel, cabot chemical limited.
Bentonite with whiteness of 90 and density of 60g/cm3The apparent viscosity is 50 mPas, the hardness is 3, the expansion factor is 12, and the processing plant for the mineral products is transported in Lingshou county.
Dopamine hydrochloride with CAS number of 62-31-7, ignition residue of less than or equal to 0.05 percent and melting point of 248-250 ℃, Shanghai Haosheng industry Co., Ltd.
Triisopropylphenyl phosphate with CAS number 68937-41-7, flash point 263.1 deg.C, boiling point 480 deg.C, Guangzhou Toyoda New materials Co.
Platinum catalyst, containing 3000ppm platinum, Shanghai silicon friend New Material science and technology company.
PET release film, thickness 0.05mm, jujube Qiang county country strong glass steel preferred company.
Example 1
A preparation method of a heat insulation material comprises the following steps:
s1, mixing 100g of 107 silicon rubber, 8g of vinyl silicone oil, 20g of silicon carbide, 30g of silane coupling agent modified fumed silica, 50g of modified bentonite, 0.6g of 2, 8-di-tert-butyl-4-methylphenol and 0.2g of alkynyl cyclohexanol, heating to 85 ℃, stirring for 90min at the stirring speed of 70 revolutions per minute, vacuumizing, and continuing stirring for 30min to obtain a mixture 1;
s2, adding 10g of polymethylhydrosiloxane and 0.8g of platinum catalyst into the mixture 1, and stirring for 20min at a stirring speed of 50 revolutions per minute to obtain a mixture 2;
s3, coating the mixture 2 on the surface of a PET release film, placing the PET release film in the air, soaking for 5min at 30 ℃, then placing the PET release film in a 75 ℃ oven, drying for 5min, cooling to 30 ℃, and separating the PET release film to obtain the heat insulation material.
The preparation method of the silane coupling agent modified fumed silica comprises the following steps:
(1) 0.08g of sodium dodecyl sulfate and 2g of gas phase SiO2Adding into 30g of 50 wt% ethanol water solution, stirring uniformly, performing ultrasonic treatment for 0.5 hour, heating to 70 ℃, then dropwise adding 0.8g of gamma-methacryloxypropyltrimethoxysilane, reacting for 3 hours at constant temperature, washing with ethanol, and centrifuging to obtain KH570-SiO2；
(2) Mixing KH570-SiO2Placed in 50g of a 75% by weight aqueous ethanol solution, 0.2g of a hydroxy silicone oil and 1g of dibutyltin dilaurate were added dropwise thereto, and after stirring at 25 ℃ for 5 hours, the mixture was dried with anhydrousWashing and centrifuging by using ethanol to obtain the silane coupling agent modified fumed silica.
The preparation method of the modified bentonite comprises the following steps:
1) roasting 20g of bentonite at 280 ℃ for 3h, cooling to 30 ℃, grinding, sieving with a 550-mesh sieve, adding into 350mL of 10 wt% dilute sulfuric acid solution, heating to 90 ℃ for reaction for 3h, filtering, collecting a filter cake, washing the filter cake with water until the pH value is 7, and drying in a 80 ℃ drying oven for 7h to obtain pretreated bentonite;
2) preparing 300mL of 30 wt% dopamine hydrochloride aqueous solution, adjusting the pH value to 8, adding 200mL of Tris buffer solution, uniformly mixing, heating to 40 ℃, reacting for 2 hours, centrifuging, filtering and collecting filter residues, washing the filter residues with water for 3 times, and freeze-drying at-40 ℃ for 40 hours to obtain polydopamine;
3) adding 8g of pretreated bentonite into 80mL of absolute ethanol, stirring uniformly, adding 1g of polydopamine and 2g of triisopropylphenyl phosphate, heating to 90 ℃, carrying out reflux reaction for 24 hours, cooling to 30 ℃, filtering, collecting a filter cake, and drying in a 70 ℃ drying oven for 8 hours to obtain the modified bentonite.
The preparation method of the lithium battery heat preservation protection pad comprises the following steps: and cutting the heat-insulating material into a sample with the thickness of 10mm to obtain the lithium battery heat-insulating protection pad.
Example 2
A preparation method of a heat insulation material comprises the following steps:
s1, mixing 100g of 107 silicon rubber, 8g of vinyl silicone oil, 20g of silicon carbide, 30g of silane coupling agent modified fumed silica, 50g of modified bentonite, 0.6g of 2, 8-di-tert-butyl-4-methylphenol and 0.2g of alkynyl cyclohexanol, heating to 85 ℃, stirring for 90min at the stirring speed of 70 revolutions per minute, vacuumizing, and continuing stirring for 30min to obtain a mixture 1;
s2, adding 10g of polymethylhydrosiloxane and 0.8g of platinum catalyst into the mixture 1, and stirring for 20min at a stirring speed of 50 revolutions per minute to obtain a mixture 2;
s3, coating the mixture 2 on the surface of a PET release film, placing the PET release film in the air, soaking for 5min at 30 ℃, then placing the PET release film in a 75 ℃ oven, drying for 5min, cooling to 30 ℃, and separating the PET release film to obtain the heat insulation material.
The preparation method of the silane coupling agent modified fumed silica comprises the following steps:
(1) 0.08g of sodium dodecyl sulfate and 2g of gas phase SiO2Adding into 30g of 50 wt% ethanol water solution, stirring uniformly, performing ultrasonic treatment for 0.5 hour, heating to 70 ℃, then dropwise adding 0.8g of gamma-methacryloxypropyltrimethoxysilane, reacting for 3 hours at constant temperature, washing with ethanol, and centrifuging to obtain KH570-SiO2；
(2) Mixing KH570-SiO2And (3) placing the mixture into 50g of 75 wt% ethanol aqueous solution, dropwise adding 0.2g of hydroxyl silicone oil and 1g of dibutyltin dilaurate into the mixture, stirring the mixture at 25 ℃ for 5 hours, washing the mixture by using absolute ethanol, and centrifuging the mixture to obtain the silane coupling agent modified fumed silica.
The preparation method of the modified bentonite comprises the following steps:
1) roasting 20g of bentonite at 280 ℃ for 3h, cooling to 30 ℃, grinding, sieving with a 550-mesh sieve, adding into 350mL of 10 wt% dilute sulfuric acid solution, heating to 90 ℃ for reaction for 3h, filtering, collecting a filter cake, washing the filter cake with water until the pH value is 7, and drying in a 80 ℃ drying oven for 7h to obtain pretreated bentonite;
2) preparing 300mL of 30 wt% dopamine hydrochloride aqueous solution, adjusting the pH value to 8, adding 200mL of Tris buffer solution, uniformly mixing, heating to 40 ℃, reacting for 2 hours, centrifuging, filtering and collecting filter residues, washing the filter residues with water for 3 times, and freeze-drying at-40 ℃ for 40 hours to obtain polydopamine;
3) adding 8g of pretreated bentonite into 80mL of absolute ethyl alcohol, stirring uniformly, adding 3g of polydopamine, heating to 90 ℃, carrying out reflux reaction for 24h, cooling to 30 ℃, filtering, collecting a filter cake, and drying in a drying oven at 70 ℃ for 8h to obtain the modified bentonite.
The preparation method of the lithium battery heat-preservation protection pad comprises the following steps: and cutting the heat-insulating material into a sample with the thickness of 10mm to obtain the lithium battery heat-insulating protection pad.
Example 3
A preparation method of a heat insulation material comprises the following steps:
s1, mixing 100g of 107 silicon rubber, 8g of vinyl silicone oil, 20g of silicon carbide, 30g of silane coupling agent modified fumed silica, 50g of modified bentonite, 0.6g of 2, 8-di-tert-butyl-4-methylphenol and 0.2g of alkynyl cyclohexanol, heating to 85 ℃, stirring for 90min at the stirring speed of 70 revolutions per minute, vacuumizing, and continuing stirring for 30min to obtain a mixture 1;
s2, adding 10g of polymethylhydrosiloxane and 0.8g of platinum catalyst into the mixture 1, and stirring for 20min at a stirring speed of 50 revolutions per minute to obtain a mixture 2;
s3, coating the mixture 2 on the surface of a PET release film, placing the PET release film in the air, soaking for 5min at 30 ℃, then placing the PET release film in a 75 ℃ oven, drying for 5min, cooling to 30 ℃, and separating the PET release film to obtain the heat insulation material.
The preparation method of the silane coupling agent modified fumed silica comprises the following steps:
(1) 0.08g of sodium dodecyl sulfate and 2g of gas phase SiO2Adding into 30g of 50 wt% ethanol water solution, stirring uniformly, performing ultrasonic treatment for 0.5 hour, heating to 70 ℃, then dropwise adding 0.8g of gamma-methacryloxypropyltrimethoxysilane, reacting for 3 hours at constant temperature, washing with ethanol, and centrifuging to obtain KH570-SiO2；
(2) Mixing KH570-SiO2And (3) putting the mixture into 50g of 75 wt% ethanol aqueous solution, dropwise adding 0.2g of hydroxyl silicone oil and 1g of dibutyltin dilaurate into the ethanol aqueous solution, stirring the mixture at 25 ℃ for 5 hours, washing the mixture with absolute ethanol, and centrifuging the mixture to obtain the silane coupling agent modified fumed silica.
The preparation method of the modified bentonite comprises the following steps:
1) roasting 20g of bentonite at 280 ℃ for 3h, cooling to 30 ℃, grinding, sieving with a 550-mesh sieve, adding into 350mL of 10 wt% dilute sulfuric acid solution, heating to 90 ℃ for reaction for 3h, filtering, collecting a filter cake, washing the filter cake with water until the pH value is 7, and drying in a 80 ℃ drying oven for 7h to obtain pretreated bentonite;
2) adding 8g of pretreated bentonite into 80mL of absolute ethyl alcohol, stirring uniformly, adding 3g of triisopropylphenyl phosphate, heating to 90 ℃, carrying out reflux reaction for 24h, cooling to 30 ℃, filtering, collecting a filter cake, and drying in a drying oven at 70 ℃ for 8h to obtain the modified bentonite.
The preparation method of the lithium battery heat preservation protection pad comprises the following steps: and cutting the heat-insulating material into a sample with the thickness of 10mm to obtain the lithium battery heat-insulating protection pad.
Comparative example 1
A preparation method of a heat insulation material comprises the following steps:
s1, mixing 100g of 107 silicon rubber, 8g of vinyl silicone oil, 20g of silicon carbide, 30g of silane coupling agent modified fumed silica, 50g of bentonite, 0.6g of 2, 8-di-tert-butyl-4-methylphenol and 0.2g of alkynyl cyclohexanol, heating to 85 ℃, stirring for 90min at the stirring speed of 70 r/min, vacuumizing, and continuing stirring for 30min to obtain a mixture 1;
s2, adding 10g of polymethylhydrosiloxane and 0.8g of platinum catalyst into the mixture 1, and stirring for 20min at a stirring speed of 50 revolutions per minute to obtain a mixture 2;
s3, coating the mixture 2 on the surface of a PET release film, placing the PET release film in the air, soaking for 5min at 30 ℃, then placing the PET release film in a 75 ℃ oven, drying for 5min, cooling to 30 ℃, and separating the PET release film to obtain the heat insulation material.
The preparation method of the silane coupling agent modified fumed silica comprises the following steps:
(1) 0.08g of sodium dodecyl sulfate and 2g of gas phase SiO2Adding into 30g of 50 wt% ethanol water solution, stirring uniformly, performing ultrasonic treatment for 0.5 hour, heating to 70 ℃, then dropwise adding 0.8g of gamma-methacryloxypropyltrimethoxysilane, reacting for 3 hours at constant temperature, washing with ethanol, and centrifuging to obtain KH570-SiO2；
(2) Mixing KH570-SiO2And (3) putting the mixture into 50g of 75 wt% ethanol aqueous solution, dropwise adding 0.2g of hydroxyl silicone oil and 1g of dibutyltin dilaurate into the ethanol aqueous solution, stirring the mixture at 25 ℃ for 5 hours, washing the mixture with absolute ethanol, and centrifuging the mixture to obtain the silane coupling agent modified fumed silica.
The preparation method of the lithium battery heat-preservation protection pad comprises the following steps: and cutting the heat-insulating material into a sample with the thickness of 10mm to obtain the lithium battery heat-insulating protection pad.
Test example 1
Measurement of thermal conductivity coefficient: the thermal conductivity of the lithium battery thermal insulation protection pad prepared in example 1 was measured by a thermal conductivity meter, the sample size was 50mm × 30mm × 10mm, the experimental voltage was 2V, each sample was measured 5 times, the time interval was 3min, the experimental results were averaged, and the experimental result was 0.196W · K (m · K)-1The lithium battery heat-insulating protection pad has a low heat conductivity coefficient, which shows that the material has good heat-insulating property.
Test example 2
Vertical burning test: the lithium battery heat preservation protection pad prepared in the embodiment 1-3 and the comparative example 1 is cut into strips with the size of 130mm × 13mm × 10mm, GB/T10707-2008 'determination of rubber burning performance' is taken as a test standard, each group of sample strips tests 5 samples, the flame is moved to the lower end of the sample to be tested to be ignited for 10s, the flame is removed, if the sample is extinguished within 30s, the sample is re-ignited, the burning condition of the sample is observed, the continuous burning time of the sample is recorded, and the vertical burning grade of the sample is judged according to the recorded test result. The vertical burning test mainly observes whether the sample is self-extinguished within 10s or 30s and whether dripping is generated in the burning process. Stopping combustion of the vertical sample within 10 s; no drop is generated, namely UL94-V0 level is reached; the sample is extinguished within 30s of combustion after being ignited, and no polymer molten drops are generated in the combustion process, so that the sample is UL94-V1 grade; the sample bars are extinguished within 30s of combustion after being ignited and molten drops are generated in the combustion process, and the sample bars belong to the UL94-V2 grades.
Limiting oxygen index test: the lithium battery insulation protection pads prepared in the examples 1-3 and the comparative example 1 are cut into strips with the size of 120mm × 6.5mm × 3mm, the limit oxygen index of the composite material is tested by using a limit oxygen index tester, the test method comprises the steps of marking a mark at a position of 50mm of the strip, then placing the strip into a combustion cylinder, igniting one end of the strip, recording the combustion time and the position of the strip, repeatedly operating the operation until the combustion time is just 50mm after 3min, recording the LOI value at the moment, and testing results are shown in the table 1:
TABLE 1 flame retardancy test results of the materials
| Vertical combustion class | LOI(％) | |
| Example 1 | V0 | 32.2 |
| Example 2 | V1 | 29.4 |
| Example 3 | V1 | 27.3 |
| Comparative example 1 | V1 | 22.3 |
The smaller the limiting oxygen index of the material, the more readily the material burns. It can be seen from the experimental results in table 1 that the thermal insulation material prepared in example 1 has the best flame retardant performance, while example 1 is different from other examples and comparative examples in that bentonite modified by polydopamine and triisopropylphenyl phosphate is added, and the probable reason is that the polydopamine and triisopropylphenyl phosphate on the surface of the modified bentonite can form nitrogen-phosphorus synergistic flame retardant at the same time, the triisopropylphenyl phosphate plays a role in promoting matrix char formation in a condensed phase, and the polydopamine forms incombustible gas in a gas phase to achieve the synergistic flame retardant effect, so that the flame retardant performance of the material is further improved.
Test example 3
And (3) testing mechanical properties:
testing tensile property: the testing standard is GB/T1040.1-2018, part 1 of determination of plastic tensile property, a CMT-4104 microcomputer controlled electronic universal tester of MTS system (China) company is adopted, materials prepared in each embodiment and comparative example are cut into the size of 150mm multiplied by 30mm multiplied by 10mm, the tensile property test is carried out on each sample, the tensile rate is 50mm/min, the experimental temperature is 25 ℃, the gauge length is 60mm, the thickness is 4mm, a group of samples is not less than 5, the temperature is 23 ℃, the adjustment is carried out for at least 24h under the environment with the relative humidity of 50%, and the average value of the test results is taken;
compression set test: the lithium battery insulating protection pads prepared in each example and comparative example were subjected to a compression set test (50% compression/100 ℃/22h) according to ISO37-2005, Standard test strips prepared according to ASTM D1056 Standard Specification for Flexible Cellular Materials-Sponge Expanded Rubber, wherein a set of test pieces is not less than 5, the test results are averaged, and the test results are shown in Table 2:
TABLE 2 test results of mechanical Properties of the materials
| Tensile Strength (KPa) | Compression set (%) | |
| Example 1 | 334 | 1.62 |
| Example 2 | 304 | 1.88 |
| Example 3 | 298 | 1.91 |
| Comparative example 1 | 225 | 4.32 |
The higher the tensile strength value and the lower the compression set value, the better the mechanical properties of the material are. As can be seen from the experimental results in Table 2, the mechanical properties of the material are not reduced by the addition of the halogen-free flame retardant, and the possible reasons are that the surface energy of the bentonite modified by the polydopamine and the triisopropylphenyl phosphate is reduced, the hydrophobicity is enhanced, and the uniform dispersion of the bentonite in a silicon rubber matrix is facilitated, so that the mechanical properties of the material are improved.
Claims (10)
1. The heat insulation material is characterized in that the preparation method of the heat insulation material comprises the following steps:
s1, weighing the raw materials according to the formula, mixing 107 silicon rubber, vinyl silicone oil, heat-conducting powder, reinforcing filler, halogen-free flame retardant, antioxidant and inhibitor, heating and stirring uniformly, and then vacuumizing to obtain a mixture 1;
s2, adding a cross-linking agent and a catalyst into the mixture 1 to obtain a mixture 2;
s3, coating the mixture 2 on the surface of a release film, placing the release film in the air for foaming, drying, and separating the release film to obtain the heat insulation material.
2. The thermal insulating material of claim 1, wherein: the heat-conducting powder is one or a mixture of two or more of aluminum oxide, magnesium oxide, zinc oxide, aluminum nitride, boron nitride, silicon carbide and heat-conducting carbon powder.
3. The thermal insulation material of claim 1, wherein: the reinforcing filler is one of fumed silica, rutile type titanium dioxide and acetylene based carbon black.
4. The heat-insulating material as claimed in claim 1, wherein the halogen-free flame retardant is modified bentonite, and the preparation method comprises the following steps:
1) adding bentonite into a dilute sulfuric acid solution for reaction, filtering, washing and drying to obtain pretreated bentonite;
2) preparing a dopamine hydrochloride aqueous solution, adding a Tris buffer solution, heating, centrifuging, filtering and drying after the reaction is finished to obtain poly-dopamine;
3) adding the pretreated bentonite into absolute ethyl alcohol, stirring uniformly, adding polydopamine and triisopropylphenyl phosphate, heating for reaction, cooling, filtering and drying to obtain the modified bentonite.
5. The thermal insulating material according to claim 4, wherein: the preparation method of the modified bentonite comprises the following steps:
1) roasting bentonite at the temperature of 200-300 ℃ for 2-4h, cooling to 20-40 ℃, grinding, sieving with a 500-mesh sieve with 600 meshes, adding the obtained product into 10-20 wt% dilute sulfuric acid solution, heating to 80-90 ℃ for reaction for 2-4h, filtering, collecting filter cakes, washing the filter cakes with water until the pH value is 6.5-7.5, and drying at 60-80 ℃ for 6-8h to obtain pretreated bentonite;
2) preparing 20-30 wt% dopamine hydrochloride aqueous solution, adjusting the pH value to 8-9, adding Tris buffer solution, uniformly mixing, heating to 30-50 ℃, reacting for 1-2h, centrifuging, filtering and collecting filter residue, washing the filter residue with water for 2-3 times, and freeze-drying at-40 to-45 ℃ for 24-48 h to obtain polydopamine;
3) adding the pretreated bentonite into absolute ethyl alcohol, stirring uniformly, adding polydopamine and triisopropylphenyl phosphate, heating to 80-100 ℃, carrying out reflux reaction for 20-24h, cooling to 20-40 ℃, filtering, collecting a filter cake, and drying at 60-80 ℃ for 6-8h to obtain the modified bentonite.
6. The thermal insulation material according to claim 4 or 5, wherein: the dosage ratio of the bentonite to the dilute sulfuric acid solution in the step 1) is 1-2g:30-40 mL.
7. The thermal insulation material according to claim 4 or 5, wherein: the dosage ratio of the dopamine hydrochloride aqueous solution to the Tris buffer solution in the step 2) is 2-4: 1-3.
8. The thermal insulating material of claim 1, wherein: the cross-linking agent is polymethylhydrosiloxane.
9. The thermal insulating material of claim 1, wherein: the catalyst is a platinum catalyst.
10. The utility model provides a lithium cell heat preservation protection pad which characterized in that: the heat insulating material according to any one of claims 1 to 9 is cut to a finished size or is cut to a finished size after the heat insulating material and the aluminized film are bonded by adhesive hot pressing.
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