CN108084896A - Acrylate structural adhesive that a kind of flame retardant type power battery aluminum shell bonds and preparation method thereof - Google Patents
Acrylate structural adhesive that a kind of flame retardant type power battery aluminum shell bonds and preparation method thereof Download PDFInfo
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- CN108084896A CN108084896A CN201711341293.XA CN201711341293A CN108084896A CN 108084896 A CN108084896 A CN 108084896A CN 201711341293 A CN201711341293 A CN 201711341293A CN 108084896 A CN108084896 A CN 108084896A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
- C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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Abstract
The invention discloses the acrylate structural adhesives that a kind of flame retardant type power battery aluminum shell bonds, and including oxidant constituents and reducing agent component, oxidant constituents and reducing agent volume components ratio are 1:1；Oxidant constituents include isobornyl methacrylate, 2 phenoxyethyl acrylates, 3,3,5 trimethyl cyclohexane methacrylates, nitrile rubber, methyl methacrylate butyl acrylate diblock copolymer, fire retardant, peroxide and stabilizer；Reducing agent component includes methacrylic acid tetrahydrofurfuryl alcohol ester, isooctyl methacrylate, 2 hydroxyethyl methacrylate phosphates, end carboxyl modified chloroprene rubber, methyl methacrylate butyl acrylate diblock copolymer, fire retardant, substituting thioureido, cobalt naphthenate, auxiliary agent and stabilizer.The invention also discloses preparation methods.Thermal discharge is low when the present invention uses, and film surface is not in stomata and lines, can also play fire retardation, effectively increases the security reliability of battery.
Description
Technical field
The present invention relates to acrylate structural adhesive technical fields, and in particular to a kind of flame retardant type power battery aluminum shell bonds
Acrylate structural adhesive and preparation method thereof.
Background technology
Power battery not only needs higher as the power supply that power resources are provided for electric vehicle, electric train etc.
Energy and power, it is also necessary to higher energy density and security reliability.
Currently, square power battery aluminum hull encapsulation and aluminum hull and battery pack between structure the bonding generally use second generation
Acrylate structural adhesive is realized.Main cause is that second generation acrylate structural adhesive is a kind of bi-component third reacted completely
Olefin(e) acid ester structure glue, has many advantages, such as, if room temperature curing is quick and curing rate is adjustable, can pasta bond, need not be tight
The surface treatment of lattice and binding material is extensive.
However, existing acrylate structural adhesive is when in use, fever is unable to control, and a large amount of mix (more than 10g) can be sent out
Raw violent exothermic reaction, causes film surface substantial amounts of stomata and lines occur；The power battery completed is bonded to use
Cheng Zhong if vibration or variation of ambient temperature occur for vehicle, can cause inside battery structure to change, battery safety
Reduce, than it is relatively hazardous in addition be present with combustion phenomena cause car crash accident occur.
The content of the invention
For defect in the prior art, it is an object of the invention to provide a kind of flame retardant type power battery aluminum shells
Cohesive acrylate structural adhesive, thermal discharge is low during use, and film surface is not in stomata and lines, can also be played fire-retardant
Effect effectively increases the security reliability of battery.
To achieve the above objectives, the present invention adopts the technical scheme that：What a kind of flame retardant type power battery aluminum shell bonded
Acrylate structural adhesive, including oxidant constituents and reducing agent component；
The oxidant constituents and the reducing agent volume components ratio are 1:1；
According to the mass fraction, every 100 parts of oxidant constituents include 10~40 parts of isobornyl methacrylates, 1
~20 parts of 2- phenoxyethyl acrylates, 5~15 parts of 3,3,5- trimethyl cyclohexanes methacrylates, 1~15 part of butyronitrile
Rubber, 1~10 part of methyl methacrylate-butyl acrylate diblock copolymer, 10~30 parts of fire retardants, 1~6 part of peroxidating
Object and 1~4 part of stabilizer；
According to the mass fraction, the every 100 parts reducing agent components include 10~40 parts of methacrylic acid tetrahydrofurfuryl alcohol esters,
1~10 part of isooctyl methacrylate, 1~10 part of 2- hydroxyethyl methacrylate phosphate, 1~15 part of end carboxyl are modified
Neoprene, 1~10 part of methyl methacrylate-butyl acrylate diblock copolymer, 10~30 parts of fire retardants, 0.5~2 part
Substituting thioureido, 1~4 part of cobalt naphthenate, 0.5~5 part of auxiliary agent and 1~4 part of stabilizer.
Further, the oxidant constituents and the reducing agent volume components ratio are 1:1；
According to the mass fraction, every 100 parts of oxidant constituents include 25~35 parts of isobornyl methacrylates, 5
~15 parts of 2- phenoxyethyl acrylates, 8~12 parts of 3,3,5- trimethyl cyclohexanes methacrylates, 5~12 parts of butyronitrile
Rubber, 3~8 parts of methyl methacrylate-butyl acrylate diblock copolymers, 15~25 parts of fire retardants, 2~5 parts of peroxidating
Object and 2~3 parts of stabilizers；
According to the mass fraction, the every 100 parts reducing agent components include 28~35 parts of methacrylic acid tetrahydrofurfuryl alcohol esters,
5~8 parts of isooctyl methacrylate, 3~8 parts of 2- hydroxyethyl methacrylate phosphates, 5~10 parts of end carboxyls are modified chlorine
Buna, 3~9 parts of methyl methacrylate-butyl acrylate diblock copolymers, 25~30 parts of fire retardants, 1~1.5 part take
For thiocarbamide, 1.5~3 parts of cobalt naphthenates, 1~3 part of auxiliary agent and 1.5~2 parts of stabilizers.
Further, the oxidant constituents and the reducing agent volume components ratio are 1:1；
According to the mass fraction, every 100 parts of oxidant constituents include 30 parts of isobornyl methacrylates, 12 parts of 2-
Phenoxyethyl acrylate, 8 parts of 3,3,5- trimethyl cyclohexanes methacrylates, 10 parts of nitrile rubbers, 8 parts of metering systems
Sour methyl esters-butyl acrylate diblock copolymer, 25 parts of fire retardants, 5 parts of peroxide and 2 parts of stabilizers；
According to the mass fraction, the every 100 parts reducing agent components include 35 parts of methacrylic acid tetrahydrofurfuryl alcohol esters, 8 parts
Isooctyl methacrylate, 6 parts of 2- hydroxyethyl methacrylate phosphates, 8 parts of end carboxyl modified chloroprene rubbers, 8 parts of first
Base methyl acrylate-acrylic acid butyl ester diblock copolymer, 28 parts of fire retardants, 1.5 parts of substituting thioureidos, 2 parts of cobalt naphthenates, 2 parts
Auxiliary agent and 1.5 parts of stabilizers.
Further, the stabilizer for hydroquinone, naphthoquinones, 2,6- di-t-butyls to (dimethyl aminomethyl) phenol,
At least two in EDETATE DISODIUM and p methoxy phenol.
Further, the peroxide is isopropyl benzene hydroperoxide, benzoyl peroxide, methyl ethyl ketone peroxide and ring
One or both of hexanone peroxide.
Further, the fire retardant for ammonium polyphosphate, Melamine Polyphosphate, melamine aminuria cyanate,
At least two in tricresyl phosphate (2- chloroethyls) ester, triaryl phosphate and tricresyl phosphate (2- chloropropyls) ester.
Further, the auxiliary agent is at least one of paraffin, methacrylic acid, maleic acid and maleic acid.
The present invention also provides the acrylate structurals that a kind of as above any flame retardant type power battery aluminum shell bonds
The preparation method of glue, includes the following steps：
The oxidant constituents and the reducing agent component are prepared, prepare the oxidant constituents and the reducing agent component
Sequencing it is unlimited；
The preparation method of the oxidant constituents is：By isobornyl methacrylate, 2- phenoxyethyl acrylates,
3,3,5- trimethyl cyclohexane methacrylates and nitrile rubber are added in dynamic mixed machine, and high-speed stirred is until nitrile rubber is complete
Dissolving adds in methyl methacrylate-butyl acrylate diblock copolymer, fire retardant and stabilizer, high-speed stirred 0.5~1
Hour, peroxide is added, when stirring at low speed 0.5~1 is small, obtains the oxidant constituents；
The preparation method of the reducing agent component is：By methacrylic acid tetrahydrofurfuryl alcohol ester, isooctyl methacrylate, 2-
Hydroxyethyl methacrylate phosphate and end carboxyl modified chloroprene rubber are added in dynamic mixed machine, and high-speed stirred is until end carboxyl
Modified chloroprene rubber is completely dissolved, add in methyl methacrylate-butyl acrylate diblock copolymer, fire retardant, auxiliary agent and
Stabilizer when high-speed stirred 0.5~1 is small, adds in substituting thioureido and cobalt naphthenate, when stirring at low speed 0.5~1 is small, obtains described
Reducing agent component；
The oxidant constituents and the reducing agent component are packed respectively, by oxidant constituents and described during use
Reducing agent component by volume 1:1 mixing, obtains the acrylate structural adhesive of flame retardant type power battery aluminum shell bonding.
Compared with prior art, the advantage of the invention is that：
(1) after the oxidant constituents in the present invention and reducing agent component mix, while enough reaction speeds are ensured, greatly
Width reduces the heat of reaction, can avoid reacting too fast and cause largely to concentrate heat release, can control the exothermic peak of product
Below 80 DEG C, heat build-up is avoided to cause danger, can also prevent temperature is excessively high to cause acrylate structural adhesive when in use due to heat
Rise spilling, and prevent acrylate structural adhesive glue-line generate bubble and lines and cooling after volume change it is excessive, in this implementation
In example, the volume contraction of product is less than 1% after curing.
(2) in the present invention, isobornyl methacrylate, methacrylic acid tetrahydrofurfuryl alcohol ester and methacrylic acid are used
Different monooctyl ester replaces methyl methacrylate, can effectively reduce the temperature of product, while ensure product intensity after cooling.
(3) in the present invention, using mixed type organophosphor nitrogen based flame retardant, it is no more than 30% premise in fire retardant usage amount
Under, can reach V1 grades it is fire-retardant, while product cure after more than 16MPa can be reached to the adhesive strength of aluminium.
Specific embodiment
The present invention is described in further detail with reference to embodiments.
Inventive embodiments provide the acrylate structural adhesive that a kind of flame retardant type power battery aluminum shell bonds, including oxidation
Agent component and reducing agent component, wherein：
Oxidant constituents and reducing agent volume components ratio are 1:1；
According to the mass fraction, every 100 parts of oxidant constituents include 10~40 parts of isobornyl methacrylates, 1~20
Part 2- phenoxyethyl acrylate, 5~15 parts of 3,3,5- trimethyl cyclohexanes methacrylates, 1~15 part of nitrile rubber,
1~10 part of methyl methacrylate-butyl acrylate diblock copolymer, 10~30 parts of fire retardants, 1~6 part of peroxide and 1
~4 parts of stabilizers；
According to the mass fraction, every 100 parts of reducing agent components include 10~40 parts of methacrylic acid tetrahydrofurfuryl alcohol esters, 1~
10 parts of isooctyl methacrylate, 1~10 part of 2- hydroxyethyl methacrylate phosphate, 1~15 part of end carboxyl are modified chlorine
Buna, 1~10 part of methyl methacrylate-butyl acrylate diblock copolymer, 10~30 parts of fire retardants, 0.5~2 part take
For thiocarbamide, 1~4 part of cobalt naphthenate, 0.5~5 part of auxiliary agent and 1~4 part of stabilizer.
After oxidant constituents and the mixing of reducing agent component in the present invention, while enough reaction speeds are ensured, significantly
The heat of reaction is reduced, can avoid reacting too fast and cause largely to concentrate heat release, the exothermic peak of product can be controlled and existed
Less than 80 DEG C, heat build-up is avoided to cause danger, can also prevent temperature is excessively high to cause acrylate structural adhesive when in use due to thermal expansion
Overflow, and prevent acrylate structural adhesive glue-line generate bubble and lines and cooling after volume change it is excessive, in the present embodiment
In, the volume contraction of product is less than 1% after curing.
It is different using isobornyl methacrylate, methacrylic acid tetrahydrofurfuryl alcohol ester and methacrylic acid in the present invention
Monooctyl ester replaces methyl methacrylate, can effectively reduce the temperature of product, while ensure product intensity after cooling.
In the present invention, using mixed type organophosphor nitrogen based flame retardant, on the premise of fire retardant usage amount is no more than 30%,
Can reach V1 grades it is fire-retardant, while product cure after more than 16MPa can be reached to the adhesive strength of aluminium.
The proportioning of acrylate structural adhesive in the present invention can select within the above range according to actual needs, this implementation
In example, proportioning can also be：
Oxidant constituents and reducing agent volume components ratio are 1:1；
According to the mass fraction, every 100 parts of oxidant constituents include 25~35 parts of isobornyl methacrylates, 5~15
Part 2- phenoxyethyl acrylate, 8~12 parts of 3,3,5- trimethyl cyclohexanes methacrylates, 5~12 parts of nitrile rubbers,
3~8 parts of methyl methacrylate-butyl acrylate diblock copolymers, 15~25 parts of fire retardants, 2~5 parts of peroxide and 2
~3 parts of stabilizers；
According to the mass fraction, every 100 parts of reducing agent components include 28~35 parts of methacrylic acid tetrahydrofurfuryl alcohol esters, 5~8
Part isooctyl methacrylate, 3~8 parts of 2- hydroxyethyl methacrylate phosphates, 5~10 parts of end carboxyl Modified Polychloroprene rubbers
Glue, 3~9 parts of methyl methacrylate-butyl acrylate diblock copolymers, 25~30 parts of fire retardants, 1~1.5 part of substitution sulphur
Urea, 1.5~3 parts of cobalt naphthenates, 1~3 part of auxiliary agent and 1.5~2 parts of stabilizers.
The present invention optimum proportioning be：
Oxidant constituents and reducing agent volume components ratio are 1:1；
According to the mass fraction, every 100 parts of oxidant constituents include 30 parts of isobornyl methacrylates, 12 parts of 2- benzene oxygen
Base ethyl propylene acid esters, 8 parts of 3,3,5- trimethyl cyclohexanes methacrylates, 10 parts of nitrile rubbers, 8 parts of methyl methacrylates
Ester-butyl acrylate diblock copolymer, 25 parts of fire retardants, 5 parts of peroxide and 2 parts of stabilizers；
According to the mass fraction, every 100 parts of reducing agent components include 35 parts of methacrylic acid tetrahydrofurfuryl alcohol esters, 8 parts of methyl
Isooctyl acrylate monomer, 6 parts of 2- hydroxyethyl methacrylate phosphates, 8 parts of end carboxyl modified chloroprene rubbers, 8 parts of methyl-props
E pioic acid methyl ester-butyl acrylate diblock copolymer, 28 parts of fire retardants, 1.5 parts of substituting thioureidos, 2 parts of cobalt naphthenates, 2 parts of auxiliary agents
With 1.5 parts of stabilizers.
Stabilizer is hydroquinone, naphthoquinones, 2,6- di-t-butyls are to (dimethyl aminomethyl) phenol, EDETATE DISODIUM and to first
At least two in oxygroup phenol.
Peroxide is isopropyl benzene hydroperoxide, benzoyl peroxide, methyl ethyl ketone peroxide and Cyclohexanone peroxides
One or both of.
Fire retardant is ammonium polyphosphate, Melamine Polyphosphate, melamine aminuria cyanate, tricresyl phosphate (2- chloroethenes
Base) in ester, triaryl phosphate and tricresyl phosphate (2- chloropropyls) ester at least two.It is fire-retardant using organic P-N type of mixed type
Agent, amount of flame-retardant agent be no more than 30% on the premise of can reach V1 grade it is fire-retardant, while product curing after it is strong to the bonding of aluminium
Degree can reach more than 16MPa.
Auxiliary agent is at least one of paraffin, methacrylic acid, maleic acid and maleic acid.
The present invention also provides the acrylate structurals that a kind of as above any flame retardant type power battery aluminum shell bonds
The preparation method of glue, includes the following steps：
Oxidant constituents and reducing agent component are prepared, the sequencing for preparing oxidant constituents and reducing agent component is unlimited；
The preparation method of oxidant constituents is：By isobornyl methacrylate, 2- phenoxyethyl acrylates, 3,3,
5- trimethyl cyclohexane methacrylates and nitrile rubber are added in dynamic mixed machine, and high-speed stirred is until nitrile rubber is completely molten
It is small to add in methyl methacrylate-butyl acrylate diblock copolymer, fire retardant and stabilizer, high-speed stirred 0.5~1 for solution
When, peroxide is added, when stirring at low speed 0.5~1 is small, obtains oxidant constituents；
The preparation method of reducing agent component is：By methacrylic acid tetrahydrofurfuryl alcohol ester, isooctyl methacrylate, 2- hydroxyls
Ethylmethyl acrylate phosphate and end carboxyl modified chloroprene rubber are added in dynamic mixed machine, and high-speed stirred is until end carboxyl is modified
Neoprene is completely dissolved, and adds in methyl methacrylate-butyl acrylate diblock copolymer, fire retardant, auxiliary agent and stabilization
Agent when high-speed stirred 0.5~1 is small, adds in substituting thioureido and cobalt naphthenate, when stirring at low speed 0.5~1 is small, obtains reducing agent group
Point；
Oxidant constituents and reducing agent component are packed respectively, oxidant constituents and reducing agent component are pressed into volume during use
Than 1:1 mixing, obtains the acrylate structural adhesive of flame retardant type power battery aluminum shell bonding.
Wherein, stabilizer, peroxide, fire retardant and auxiliary agent within the above range specific are selected and with comparing acrylic acid
The final strength and flame retardant property of ester structure glue have no substantial effect, and therefore, do not carry out considered critical to its specific proportioning.
Below by way of 11 embodiments and 1 comparative example, the present invention is described in detail.
Embodiment 1：
By 30 parts of isobornyl methacrylates, 12 parts of 2- phenoxyethyl acrylates, 8 parts of 3,3,5- front three basic ring second
Alkane methacrylate and 10 parts of nitrile rubbers are added in dynamic mixed machine, and high-speed stirred is completely dissolved up to nitrile rubber, adds in 8 parts
Methyl methacrylate-butyl acrylate diblock copolymer, 25 parts of fire retardants and 2 parts of stabilizers, high-speed stirred 0.5~1 are small
When, 5 parts of peroxide are added, when stirring at low speed 0.5~1 is small, obtain oxidant constituents；
By 35 methacrylic acid tetrahydrofurfuryl alcohol esters, 8 parts of isooctyl methacrylate, 6 parts of 2- hydroxy ethyl methyl acrylic acid
Ester phosphate and 8 parts of end carboxyl modified chloroprene rubbers are added in dynamic mixed machine, and high-speed stirred is until end carboxyl modified chloroprene rubber is complete
Fully dissolved, 8 parts of methyl methacrylate-butyl acrylate diblock copolymers of addition, 28 parts of fire retardants, 2 parts of auxiliary agents and 1.5 parts
Stabilizer when high-speed stirred 0.5~1 is small, adds in 1.5 parts of substituting thioureidos and 2 parts of cobalt naphthenates, when stirring at low speed 0.5~1 is small,
Obtain reducing agent component；
By oxidant constituents and reducing agent component by volume 1:1 mixing obtains flame retardant type power battery aluminum shell bonding
Acrylate structural adhesive.
Embodiment 2：
By 40 parts of isobornyl methacrylates, 15 parts of 2- phenoxyethyl acrylates, 5 parts of 3,3,5- front three basic ring second
Alkane methacrylate and 5 parts of nitrile rubbers are added in dynamic mixed machine, and high-speed stirred is completely dissolved up to nitrile rubber, adds in 10 parts
Methyl methacrylate-butyl acrylate diblock copolymer, 15 parts of fire retardants and 4 parts of stabilizers, high-speed stirred 0.5~1 are small
When, 6 parts of peroxide are added, when stirring at low speed 0.5~1 is small, obtain oxidant constituents；
By 40 parts of methacrylic acid tetrahydrofurfuryl alcohol esters, 5 parts of isooctyl methacrylate, 8 parts of 2- hydroxy ethyl methyl propylene
Acid esters phosphate and 5 parts of end carboxyl modified chloroprene rubbers are added in dynamic mixed machine, and high-speed stirred is until end carboxyl modified chloroprene rubber
It is completely dissolved, adds in 10 parts of methyl methacrylate-butyl acrylate diblock copolymers, 20 parts of fire retardants, 5 parts of auxiliary agents and 2
Part stabilizer when high-speed stirred 0.5~1 is small, adds in 2 parts of substituting thioureidos and 3 parts of cobalt naphthenates, when stirring at low speed 0.5~1 is small,
Obtain reducing agent component；
By oxidant constituents and reducing agent component by volume 1:1 mixing obtains flame retardant type power battery aluminum shell bonding
Acrylate structural adhesive.
Embodiment 3：
By 35 parts of isobornyl methacrylates, 20 parts of 2- phenoxyethyl acrylates, 15 parts of 3,3,5- front three basic rings
Ethane methacrylate and 15 parts of nitrile rubbers are added in dynamic mixed machine, and high-speed stirred is completely dissolved up to nitrile rubber, adds in 3
Part methyl methacrylate-butyl acrylate diblock copolymer, 10 parts of fire retardants and 1 part of stabilizer, high-speed stirred 0.5~1
Hour, 1 part of peroxide is added, when stirring at low speed 0.5~1 is small, obtains oxidant constituents；
By 28 parts of methacrylic acid tetrahydrofurfuryl alcohol esters, 9 parts of isooctyl methacrylate, 5 parts of 2- hydroxy ethyl methyl propylene
Acid esters phosphate and 10 parts of end carboxyl modified chloroprene rubbers are added in dynamic mixed machine, and high-speed stirred is until end carboxyl modified chloroprene rubber
It is completely dissolved, 9 parts of methyl methacrylate-butyl acrylate diblock copolymers of addition, 30 parts of fire retardants, 1 part of auxiliary agent and 3 parts
Stabilizer when high-speed stirred 0.5~1 is small, adds in 1 part of substituting thioureido and 4 parts of cobalt naphthenates, when stirring at low speed 0.5~1 is small, obtains
To reducing agent component；
By oxidant constituents and reducing agent component by volume 1:1 mixing obtains flame retardant type power battery aluminum shell bonding
Acrylate structural adhesive.
Embodiment 4：
By 25 parts of isobornyl methacrylates, 5 parts of 2- phenoxyethyl acrylates, 10 parts of 3,3,5- front three basic ring second
Alkane methacrylate and 12 parts of nitrile rubbers are added in dynamic mixed machine, and high-speed stirred is completely dissolved up to nitrile rubber, adds in 9 parts
Methyl methacrylate-butyl acrylate diblock copolymer, 30 parts of fire retardants and 4 parts of stabilizers, high-speed stirred 0.5~1 are small
When, 5 parts of peroxide are added, when stirring at low speed 0.5~1 is small, obtain oxidant constituents；
By 31 parts of methacrylic acid tetrahydrofurfuryl alcohol esters, 10 parts of isooctyl methacrylate, 10 parts of 2- hydroxy ethyl methyls third
Olefin(e) acid ester phosphate and 15 parts of end carboxyl modified chloroprene rubbers are added in dynamic mixed machine, and high-speed stirred is until end carboxyl Modified Polychloroprene rubber
Glue is completely dissolved, and adds in 3 parts of methyl methacrylate-butyl acrylate diblock copolymers, 25 parts of fire retardants, 3 parts of auxiliary agents and 1
Part stabilizer when high-speed stirred 0.5~1 is small, adds in 0.5 part of substituting thioureido and 1.5 parts of cobalt naphthenates, stirring at low speed 0.5~1 is small
When, obtain reducing agent component；
By oxidant constituents and reducing agent component by volume 1:1 mixing obtains flame retardant type power battery aluminum shell bonding
Acrylate structural adhesive.
Embodiment 5：
By 34 parts of isobornyl methacrylates, 18 parts of 2- phenoxyethyl acrylates, 13 parts of 3,3,5- front three basic rings
Ethane methacrylate and 8 parts of nitrile rubbers are added in dynamic mixed machine, and high-speed stirred is completely dissolved up to nitrile rubber, adds in 1
Part methyl methacrylate-butyl acrylate diblock copolymer, 21 parts of fire retardants and 3 parts of stabilizers, high-speed stirred 0.5~1
Hour, 2 parts of peroxide are added, when stirring at low speed 0.5~1 is small, obtain oxidant constituents；
By 28 parts of methacrylic acid tetrahydrofurfuryl alcohol esters, 10 parts of isooctyl methacrylate, 9 parts of 2- hydroxy ethyl methyl propylene
Acid esters phosphate and 14 parts of end carboxyl modified chloroprene rubbers are added in dynamic mixed machine, and high-speed stirred is until end carboxyl modified chloroprene rubber
It is completely dissolved, adds in 1 part of methyl methacrylate-butyl acrylate diblock copolymer, 26 parts of fire retardants, 4 parts of auxiliary agents and 2.5
Part stabilizer when high-speed stirred 0.5~1 is small, adds in 2 parts of substituting thioureidos and 3.5 parts of cobalt naphthenates, stirring at low speed 0.5~1 is small
When, obtain reducing agent component；
By oxidant constituents and reducing agent component by volume 1:1 mixing obtains flame retardant type power battery aluminum shell bonding
Acrylate structural adhesive.
Embodiment 6：
By 10 parts of isobornyl methacrylates, 18 parts of 2- phenoxyethyl acrylates, 11 parts of 3,3,5- front three basic rings
Ethane methacrylate and 14 parts of nitrile rubbers are added in dynamic mixed machine, and high-speed stirred is completely dissolved up to nitrile rubber, is added in
10 parts of methyl methacrylate-butyl acrylate diblock copolymers, 28 parts of fire retardants and 4 parts of stabilizers, high-speed stirred 0.5~
1 it is small when, add 5 parts of peroxide, when stirring at low speed 0.5~1 is small, obtain oxidant constituents；
By 40 parts of methacrylic acid tetrahydrofurfuryl alcohol esters, 10 parts of isooctyl methacrylate, 3 parts of 2- hydroxy ethyl methyl propylene
Acid esters phosphate and 15 parts of end carboxyl modified chloroprene rubbers are added in dynamic mixed machine, and high-speed stirred is until end carboxyl modified chloroprene rubber
Be completely dissolved, add in 10 parts of methyl methacrylate-butyl acrylate diblock copolymers, 13 parts of fire retardants, 3.5 auxiliary agents and
2.5 parts of stabilizers when high-speed stirred 0.5~1 is small, adds in 2 parts of substituting thioureidos and 1 part of cobalt naphthenate, stirring at low speed 0.5~1 are small
When, obtain reducing agent component；
By oxidant constituents and reducing agent component by volume 1:1 mixing obtains flame retardant type power battery aluminum shell bonding
Acrylate structural adhesive.
Embodiment 7：
By 38 parts of isobornyl methacrylates, 1 part of 2- phenoxyethyl acrylate, 10 parts of 3,3,5- front three basic ring second
Alkane methacrylate and 7 parts of nitrile rubbers are added in dynamic mixed machine, and high-speed stirred is completely dissolved up to nitrile rubber, adds in 10 parts
Methyl methacrylate-butyl acrylate diblock copolymer, 26 parts of fire retardants and 3.5 parts of stabilizers, high-speed stirred 0.5~1
Hour, 4.5 parts of peroxide are added, when stirring at low speed 0.5~1 is small, obtain oxidant constituents；
By 40 parts of methacrylic acid tetrahydrofurfuryl alcohol esters, 10 parts of isooctyl methacrylate, 10 parts of 2- hydroxy ethyl methyls third
Olefin(e) acid ester phosphate and 10.5 parts of end carboxyl modified chloroprene rubbers are added in dynamic mixed machine, and high-speed stirred is until end carboxyl Modified Polychloroprene
Rubber is completely dissolved, add in 10 parts of methyl methacrylate-butyl acrylate diblock copolymers, 10 parts of fire retardants, 0.5 part help
Agent and 3 parts of stabilizers when high-speed stirred 0.5~1 is small, add in 2 parts of substituting thioureidos and 4 parts of cobalt naphthenates, stirring at low speed 0.5~1
Hour, obtain reducing agent component；
By oxidant constituents and reducing agent component by volume 1:1 mixing obtains flame retardant type power battery aluminum shell bonding
Acrylate structural adhesive.
Embodiment 8：
By 30 parts of isobornyl methacrylates, 4 parts of 2- phenoxyethyl acrylates, 12 parts of 3,3,5- front three basic ring second
Alkane methacrylate, 9 parts of nitrile rubbers are added in dynamic mixed machine, and high-speed stirred is completely dissolved up to nitrile rubber, adds in 9 parts of first
Base methyl acrylate-acrylic acid butyl ester diblock copolymer, 28 parts of fire retardants and 4 parts of stabilizers, when high-speed stirred 0.5~1 is small,
4 parts of peroxide are added, when stirring at low speed 0.5~1 is small, obtain oxidant constituents；
By 25 parts of methacrylic acid tetrahydrofurfuryl alcohol esters, 10 parts of isooctyl methacrylate, 10 parts of 2- hydroxy ethyl methyls third
Olefin(e) acid ester phosphate, 1 part of end carboxyl modified chloroprene rubber are added in dynamic mixed machine, and high-speed stirred is until end carboxyl modified chloroprene rubber
It is completely dissolved, adds in 10 parts of methyl methacrylate-butyl acrylate diblock copolymers, 30 parts of fire retardants, 5 parts of auxiliary agents and 3
Part stabilizer when high-speed stirred 0.5~1 is small, adds in 2 parts of substituting thioureidos, 4 parts of cobalt naphthenates, when stirring at low speed 0.5~1 is small, obtains
To reducing agent component；
By oxidant constituents and reducing agent component by volume 1:1 mixing obtains flame retardant type power battery aluminum shell bonding
Acrylate structural adhesive.
Embodiment 9：
By 38 parts of isobornyl methacrylates, 9 parts of 2- phenoxyethyl acrylates, 10 parts of 3,3,5- front three basic ring second
Alkane methacrylate, 10 parts of nitrile rubbers are added in dynamic mixed machine, and high-speed stirred is completely dissolved up to nitrile rubber, adds in 7 parts
Methyl methacrylate-butyl acrylate diblock copolymer, 20 parts of fire retardants and 2.5 parts of stabilizers, high-speed stirred 0.5~1
Hour, 3.5 parts of peroxide are added, when stirring at low speed 0.5~1 is small, obtain oxidant constituents；
By 10 parts of methacrylic acid tetrahydrofurfuryl alcohol esters, 10 parts of isooctyl methacrylate, 10 parts of 2- hydroxy ethyl methyls third
Olefin(e) acid ester phosphate, 15 parts of end carboxyl modified chloroprene rubbers are added in dynamic mixed machine, and high-speed stirred is until end carboxyl Modified Polychloroprene rubber
Glue is completely dissolved, add in 10 parts of methyl methacrylate-butyl acrylate diblock copolymers, 30 parts of fire retardants, 5 parts of auxiliary agents and
4 parts of stabilizers when high-speed stirred 0.5~1 is small, add in 2 parts of substituting thioureidos, 4 parts of cobalt naphthenates, when stirring at low speed 0.5~1 is small,
Obtain reducing agent component；
By oxidant constituents and reducing agent component by volume 1:1 mixing obtains flame retardant type power battery aluminum shell bonding
Acrylate structural adhesive.
Embodiment 10：
By 34 parts of isobornyl methacrylates, 10 parts of 2- phenoxyethyl acrylates, 13 parts of 3,3,5- front three basic rings
Ethane methacrylate, 7 parts of nitrile rubbers are added in dynamic mixed machine, and high-speed stirred is completely dissolved up to nitrile rubber, adds in 10
Part methyl methacrylate-butyl acrylate diblock copolymer, 21 parts of fire retardants, 2 parts of stabilizers, high-speed stirred 0.5~1 are small
When, 3 parts of peroxide are added, when stirring at low speed 0.5~1 is small, obtain oxidant constituents；
By 20 parts of methacrylic acid tetrahydrofurfuryl alcohol esters, 1 part of isooctyl methacrylate, 10 parts of 2- hydroxy ethyl methyl propylene
Acid esters phosphate, 15 parts of end carboxyl modified chloroprene rubbers are added in dynamic mixed machine, and high-speed stirred is until end carboxyl modified chloroprene rubber
Be completely dissolved, add in 10 parts of methyl methacrylate-butyl acrylate diblock copolymers, 30 parts of fire retardants, 4.5 parts of auxiliary agents and
3.5 parts of stabilizers when high-speed stirred 0.5~1 is small, add in 2 parts of substituting thioureidos, 4 parts of cobalt naphthenates, and stirring at low speed 0.5~1 is small
When, obtain reducing agent component；
By oxidant constituents and reducing agent component by volume 1:1 mixing obtains flame retardant type power battery aluminum shell bonding
Acrylate structural adhesive.
Embodiment 11：
By 36 parts of isobornyl methacrylates, 15 parts of 2- phenoxyethyl acrylates, 7 parts of 3,3,5- front three basic ring second
Alkane methacrylate, 9 parts of nitrile rubbers are added in dynamic mixed machine, and high-speed stirred is completely dissolved up to nitrile rubber, adds in 7 parts of first
Base methyl acrylate-acrylic acid butyl ester diblock copolymer, 22 parts of fire retardants, 1.5 parts of stabilizers, high-speed stirred 0.5~1 are small
When, 2.5 parts of peroxide are added, when stirring at low speed 0.5~1 is small, obtain oxidant constituents；
By 30 parts of methacrylic acid tetrahydrofurfuryl alcohol esters, 7 parts of isooctyl methacrylate, 1 part of 2- hydroxy ethyl methyl propylene
Acid esters phosphate, 9 parts of end carboxyl modified chloroprene rubbers are added in dynamic mixed machine, and high-speed stirred is until end carboxyl modified chloroprene rubber is complete
Fully dissolved, 10 parts of methyl methacrylate-butyl acrylate diblock copolymers of addition, 28 parts of fire retardants, 5 parts of auxiliary agents and 4 parts
Stabilizer when high-speed stirred 0.5~1 is small, adds in 2 parts of substituting thioureidos, 4 parts of cobalt naphthenates, when stirring at low speed 0.5~1 is small, obtains
Reducing agent component；
By oxidant constituents and reducing agent component by volume 1:1 mixing obtains flame retardant type power battery aluminum shell bonding
Acrylate structural adhesive.
Comparative example 1：
40 parts of methyl methacrylates, 5 parts of methacrylic acids, 9 parts of nitrile rubbers are added in dynamic mixed machine, high-speed stirred is extremely
Nitrile rubber is completely dissolved, and adds in 7 parts of methyl methacrylate-butadiene-styrene terpolymers, 34 parts of fire retardants and 2
Part stabilizer, when high-speed stirred 1 is small, adds 2 parts of peroxide, when stirring at low speed 1 is small, obtains oxidant constituents；
30 parts of methyl methacrylates, 9 parts of cyclohexyl methacrylates, 8 parts of end carboxyl modified chloroprene rubbers are added in dynamic
In mixed machine, high-speed stirred to end carboxyl modified chloroprene rubber is completely dissolved, and adds in 10 parts of methyl methacrylate-butadiene-benzene
Ethylene-dien terpolymer, 30 parts of fire retardants, 5 parts of auxiliary agents and 3 parts of stabilizers when high-speed stirred 1 is small, add in 2 parts of N, N- dimethyl
Aniline, 3 parts of N, N- dimethyl-p-toluidines when stirring at low speed 1 is small, obtain reducing agent component；
By oxidant constituents and reducing agent component by volume 1:1 mixing, obtains acrylate structural adhesive.
The acrylate structural adhesive prepared below to above-mentioned 11 embodiments and 1 comparative example is tested for the property.
Referring to table 1, according to GB/T2791-1995 adhesive T peeling strength test methods, using flexible material to flexible material
Material, the T peel strengths of the embodiment of the present invention can reach 6.4N/mm, and failure mode is cohesional failure, illustrates that the present invention has
Good toughness.
It is tested according to the assay method of GB/T7124-2008 adhesive tensile shear strengths strong to the bonding of aluminium flake at room temperature
Degree, the adhesion strength of the embodiment of the present invention can reach 16.8MPa.
High and low temperature resistance is tested by thermocycling experiment, thermocycling experiment condition is：25 DEG C of 0.5h, 25 DEG C~
90 DEG C of 0.5h, 90 DEG C of 4h, 90 DEG C~-40 DEG C 1h, -40 DEG C of 4h, -40 DEG C~25 DEG C 0.5h, are cycled 14 times with this, are added up to
147h；The present invention is 17.2MPa to the adhesion strength of aluminium, and intensity does not decay after thermal shock aging；
According to UL94 standard testings, flame retardant property of the embodiment of the present invention can reach V1 grades.
The performance test results of table 1, embodiment 1~11 and comparative example 1
The present invention is not limited to the above-described embodiments, for those skilled in the art, is not departing from
On the premise of the principle of the invention, several improvements and modifications can also be made, these improvements and modifications are also considered as the protection of the present invention
Within the scope of.The content not being described in detail in this specification belongs to the prior art well known to professional and technical personnel in the field.
Claims (8)
1. a kind of acrylate structural adhesive that flame retardant type power battery aluminum shell bonds, including oxidant constituents and reducing agent group
Point, it is characterised in that：
The oxidant constituents and the reducing agent volume components ratio are 1:1；
According to the mass fraction, every 100 parts of oxidant constituents include 10~40 parts of isobornyl methacrylates, 1~20
Part 2- phenoxyethyl acrylate, 5~15 parts of 3,3,5- trimethyl cyclohexanes methacrylates, 1~15 part of nitrile rubber,
1~10 part of methyl methacrylate-butyl acrylate diblock copolymer, 10~30 parts of fire retardants, 1~6 part of peroxide and 1
~4 parts of stabilizers；
According to the mass fraction, the every 100 parts reducing agent components include 10~40 parts of methacrylic acid tetrahydrofurfuryl alcohol esters, 1~
10 parts of isooctyl methacrylate, 1~10 part of 2- hydroxyethyl methacrylate phosphate, 1~15 part of end carboxyl are modified chlorine
Buna, 1~10 part of methyl methacrylate-butyl acrylate diblock copolymer, 10~30 parts of fire retardants, 0.5~2 part take
For thiocarbamide, 1~4 part of cobalt naphthenate, 0.5~5 part of auxiliary agent and 1~4 part of stabilizer.
2. the acrylate structural adhesive that flame retardant type power battery aluminum shell as described in claim 1 bonds, it is characterised in that：
The oxidant constituents and the reducing agent volume components ratio are 1:1；
According to the mass fraction, every 100 parts of oxidant constituents include 25~35 parts of isobornyl methacrylates, 5~15
Part 2- phenoxyethyl acrylate, 8~12 parts of 3,3,5- trimethyl cyclohexanes methacrylates, 5~12 parts of nitrile rubbers,
3~8 parts of methyl methacrylate-butyl acrylate diblock copolymers, 15~25 parts of fire retardants, 2~5 parts of peroxide and 2
~3 parts of stabilizers；
According to the mass fraction, the every 100 parts reducing agent components include 28~35 parts of methacrylic acid tetrahydrofurfuryl alcohol esters, 5~8
Part isooctyl methacrylate, 3~8 parts of 2- hydroxyethyl methacrylate phosphates, 5~10 parts of end carboxyl Modified Polychloroprene rubbers
Glue, 3~9 parts of methyl methacrylate-butyl acrylate diblock copolymers, 25~30 parts of fire retardants, 1~1.5 part of substitution sulphur
Urea, 1.5~3 parts of cobalt naphthenates, 1~3 part of auxiliary agent and 1.5~2 parts of stabilizers.
3. the acrylate structural adhesive that flame retardant type power battery aluminum shell as described in claim 1 bonds, it is characterised in that：
The oxidant constituents and the reducing agent volume components ratio are 1:1；
According to the mass fraction, every 100 parts of oxidant constituents include 30 parts of isobornyl methacrylates, 12 parts of 2- benzene oxygen
Base ethyl propylene acid esters, 8 parts of 3,3,5- trimethyl cyclohexanes methacrylates, 10 parts of nitrile rubbers, 8 parts of methyl methacrylates
Ester-butyl acrylate diblock copolymer, 25 parts of fire retardants, 5 parts of peroxide and 2 parts of stabilizers；
According to the mass fraction, the every 100 parts reducing agent components include 35 parts of methacrylic acid tetrahydrofurfuryl alcohol esters, 8 parts of methyl
Isooctyl acrylate monomer, 6 parts of 2- hydroxyethyl methacrylate phosphates, 8 parts of end carboxyl modified chloroprene rubbers, 8 parts of methyl-props
E pioic acid methyl ester-butyl acrylate diblock copolymer, 28 parts of fire retardants, 1.5 parts of substituting thioureidos, 2 parts of cobalt naphthenates, 2 parts of auxiliary agents
With 1.5 parts of stabilizers.
4. the acrylate structural adhesive that flame retardant type power battery aluminum shell as described in claim 1 bonds, it is characterised in that：Institute
Stabilizer is stated as hydroquinone, naphthoquinones, 2,6- di-t-butyls are to (dimethyl aminomethyl) phenol, EDETATE DISODIUM and to methoxybenzene
At least two in phenol.
5. the acrylate structural adhesive that flame retardant type power battery aluminum shell as described in claim 1 bonds, it is characterised in that：Institute
Peroxide is stated as one in isopropyl benzene hydroperoxide, benzoyl peroxide, methyl ethyl ketone peroxide and Cyclohexanone peroxides
Kind or two kinds.
6. the acrylate structural adhesive that flame retardant type power battery aluminum shell as described in claim 1 bonds, it is characterised in that：Institute
State fire retardant for ammonium polyphosphate, Melamine Polyphosphate, melamine aminuria cyanate, tricresyl phosphate (2- chloroethyls) ester,
At least two in triaryl phosphate and tricresyl phosphate (2- chloropropyls) ester.
7. the acrylate structural adhesive that flame retardant type power battery aluminum shell as described in claim 1 bonds, it is characterised in that：Institute
Auxiliary agent is stated as at least one of paraffin, methacrylic acid, maleic acid and maleic acid.
8. a kind of preparation for the acrylate structural adhesive that flame retardant type power battery aluminum shell as described in claim 1-7 is any bonds
Method, which is characterized in that it includes the following steps：
The oxidant constituents and the reducing agent component are prepared, prepare the elder generation of the oxidant constituents and the reducing agent component
Order is unlimited afterwards；
The preparation method of the oxidant constituents is：By isobornyl methacrylate, 2- phenoxyethyl acrylates, 3,3,
5- trimethyl cyclohexane methacrylates and nitrile rubber are added in dynamic mixed machine, and high-speed stirred is until nitrile rubber is completely molten
It is small to add in methyl methacrylate-butyl acrylate diblock copolymer, fire retardant and stabilizer, high-speed stirred 0.5~1 for solution
When, peroxide is added, when stirring at low speed 0.5~1 is small, obtains the oxidant constituents；
The preparation method of the reducing agent component is：By methacrylic acid tetrahydrofurfuryl alcohol ester, isooctyl methacrylate, 2- hydroxyls
Ethylmethyl acrylate phosphate and end carboxyl modified chloroprene rubber are added in dynamic mixed machine, and high-speed stirred is until end carboxyl is modified
Neoprene is completely dissolved, and adds in methyl methacrylate-butyl acrylate diblock copolymer, fire retardant, auxiliary agent and stabilization
Agent when high-speed stirred 0.5~1 is small, adds in substituting thioureido and cobalt naphthenate, when stirring at low speed 0.5~1 is small, obtains the reduction
Agent component；
The oxidant constituents and the reducing agent component are packed respectively, by the oxidant constituents and the reduction during use
Agent component by volume 1:1 mixing, obtains the acrylate structural adhesive of flame retardant type power battery aluminum shell bonding.
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