CN110079020A - A kind of new energy vehicle battery pack upper cover anti-flaming polypropylene material and preparation method thereof - Google Patents
A kind of new energy vehicle battery pack upper cover anti-flaming polypropylene material and preparation method thereof Download PDFInfo
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- CN110079020A CN110079020A CN201910444521.9A CN201910444521A CN110079020A CN 110079020 A CN110079020 A CN 110079020A CN 201910444521 A CN201910444521 A CN 201910444521A CN 110079020 A CN110079020 A CN 110079020A
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Abstract
The present invention provides a kind of new energy vehicle battery pack upper cover anti-flaming polypropylene materials and preparation method thereof, it is that will foam after polypropylene and the first additive, the second additive melting mixing, the introducing of foam process meets the lightweight requirements of new energy vehicle battery pack upper cover so that product density substantially reduces.First additive is made of with carbon fiber powder, wollastonite in powder, hollow glass micropearl, hexa etc. for raw material, second additive is made of with sodium carboxymethyl cellulose solution, polyvinyl alcohol, aluminium dihydrogen phosphate, sodium polyphosphate, poly (hexamethylene) hydrochloride, oxidation modification graphite etc. for raw material, the introducing of said components effectively increases mechanical property, the flame retardant property of product, meets the high standards of new energy vehicle battery pack upper cover.
Description
Technical field
The present invention relates to technical field of new energy, particularly, are related to a kind of new energy vehicle battery pack upper cover with fire-retardant
Polypropylene material and preparation method thereof.
Background technique
New-energy automobile, which refers to, uses unconventional vehicle fuel as a source of power, the dynamic Control and drive of comprehensive vehicle
The advanced technology of dynamic aspect, the advanced automobile with new technology, new construction of the technical principle of formation.Currently, with people's environmental protection
The enhancing of consciousness, the market proportion sustainable growth of new-energy automobile, consequent are material markets for new-energy automobile week
The materials demand on side is also gradually increased.
New-energy automobile is compared with conventional fuel oil car, and battery portion has particularity, to the part when battery pack designs
Security requirement it is high, either its mechanical property or flame retardant property are required very high.Battery pack upper cover is as new energy
The upper housing of source automobile batteries packet is combined into battery pack object with lower case, the work for playing sealing and being isolated with automotive interior
With not being subjected to the non-structural part of external force.Most current new energy vehicle battery pack upper cover using Metal Material Welding, casting or
Person is stamped to form, and the density of metal material is big, is unfavorable for the lightweight of battery pack upper cover, and complex forming technology is time-consuming.For
Loss of weight has document report to form using sheet molding compound material is hot-forming, is thermosetting plastics, cannot recycle,
Toxic gas can be also generated when solidification, leads to environmental pollution, is detrimental to health, and density is still not small enough, cannot achieve light
Quantization requires.
Therefore, it is badly in need of a kind of new material used suitable for new energy vehicle battery pack upper cover now, power should be met
Performance, the high standards of flame retardant property are learned, and should lightweight as far as possible.
Summary of the invention
It is an object of that present invention to provide a kind of new energy vehicle battery pack upper cover anti-flaming polypropylene material and preparation method thereof,
The mechanical property, flame retardant property and lightweight requirements technology of new energy vehicle battery pack upper cover are unable to satisfy to solve current material to ask
Topic.
To achieve the above object, the present invention provides a kind of systems of new energy vehicle battery pack upper cover anti-flaming polypropylene material
Preparation Method, the specific steps are as follows:
(1) first carbon fiber powder, wollastonite in powder, hollow glass micropearl, hexa and coupling agent mixed grinding are obtained
It is spare to the first additive；
(2) polyvinyl alcohol, aluminium dihydrogen phosphate, sodium polyphosphate are then added into sodium carboxymethyl cellulose solution and gathers
Hexa-methylene guanidine hydrochloride, stirring and dissolving are subsequently added into oxidation modification graphite, supersonic oscillations 30~40 minutes, are suspended
Liquid, drying recycle torque rheometer to be kneaded, obtain the second additive, spare；
(3) the second additive obtained by the first additive obtained by polypropylene, step (1), step (2) is finally utilized into twin-screw
Extruder melting mixing, injects foaming agent, and underwater cutpellet obtains the granular polypropylene material.
Preferably, in step (1), carbon fiber powder, wollastonite in powder, hollow glass micropearl, hexa and coupling agent
Mass ratio be 1:15~20:5~6:2~3:15~20.
Preferably, the specific method of step (1) is: first by carbon fiber powder, wollastonite in powder, hollow glass micropearl mixed grinding
20~30 minutes, 900~1000 DEG C are then heated to, keeps the temperature 30~40 minutes, cooled to room temperature (25 DEG C) adds six
Methenamine and coupling agent, mixed grinding 50~60 minutes up to first additive.
It is further preferred that the coupling agent is vinyltrimethoxysilane or vinyl three ('beta '-methoxy ethyoxyl)
Any one of silane.
It is further preferred that the partial size of the hollow glass micropearl is 100~120 μm.
Preferably, in step (2), sodium carboxymethyl cellulose solution, polyvinyl alcohol, aluminium dihydrogen phosphate, sodium polyphosphate,
Poly (hexamethylene) hydrochloride, oxidation modification graphite mass ratio be 1000:2~3:0.3~0.5:1~2:0.8~1:0.5~
0.8, the mass concentration of the sodium carboxymethyl cellulose solution is 3 ‰.
It is further preferred that the preparation method of the sodium carboxymethyl cellulose solution are as follows: while stirring carboxymethyl fibre
It ties up plain sodium to be poured slowly into water, 60~70 DEG C are stirred 18~24 hours to get the sodium carboxymethyl cellulose solution.
Preferably, in step (2), the oxidation modification graphite is to carry out oxidation processes to graphite using Hummer method to obtain
It arrives.
It is further preferred that the oxidation modification graphite specific in four-hole bottle the preparation method is as follows: be added graphite, dense
Potassium permanganate is added under condition of ice bath for sulfuric acid, sodium nitrate, and 35 DEG C are reacted 30 minutes, and deionized water is added, and 98 DEG C are reacted 30 points
Clock, filtration washing immediately is dry, supersonic oscillations handle 20~30 minutes to get；Wherein, graphite, the concentrated sulfuric acid, sodium nitrate, height
Potassium manganate and the mass ratio of deionized water are 1:20:0.5:3:50.
Preferably, in step (2), the process conditions of mixing are as follows: 150~180 DEG C are kneaded 20~30 minutes.
Preferably, in step (3), the polypropylene is copolymer polypropylene or homopolypropylene, in 230 DEG C, 2.16kg
Under test condition, melt index is 60~100g/10min.
Preferably, in step (3), polypropylene, the first additive, the second additive, foaming agent mass ratio be 100:1~
2:0.8~1:0.9~1.1.
Preferably, it in step (3), is mixed 2~3 minutes before double screw extruder melting mixing first with high-speed mixer.
Preferably, in step (3), the foaming agent is selected from the double benzene sulfonyls of diisopropyl azodiformate, 4,4'- oxo
The mixture of any one of hydrazine, chloroform or pentane or their arbitrary proportions.
Preferably, in step (3), the screw diameter of the extruder is 30~40mm, and draw ratio L/D is 30~40, machine
Cylinder is divided into 7 heating regions, their operating temperature is followed successively by 210 DEG C, 210 DEG C, 205 DEG C, 205 DEG C, 200 DEG C, 200 DEG C, 195
DEG C, engine speed is controlled at 300~500 revs/min.
Preferably, in step (3), underwater cutpellet, concrete technology condition are realized using underwater pelletizer are as follows: solution pump is given
The melt pressure of the form stable of underwater pelletizer, the pressure of solution pump are 10~15MPa, blow valve temperature is 190~
200 DEG C, die plate temperature be 180~190 DEG C, recirculated water water temperature be 75~85 DEG C, recirculated water work when hydraulic pressure be 0.5~
0.8MPa。
The present invention also provides a kind of new energy vehicle battery pack upper cover flame-retardant polypropylenes obtained using above-mentioned preparation method
Alkene material.
The invention has the following advantages:
The present invention will foam after polypropylene and the first additive, the second additive melting mixing, and foam process draws
Enter so that product density substantially reduces, meets the lightweight requirements of new energy vehicle battery pack upper cover.First additive is with carbon fiber
Dimension powder, wollastonite in powder, hollow glass micropearl, hexa etc. are made of raw material, and the second additive is with carboxymethyl cellulose
Plain sodium water solution, polyvinyl alcohol, aluminium dihydrogen phosphate, sodium polyphosphate, poly (hexamethylene) hydrochloride, oxidation modification graphite etc. are
Raw material is made, and the introducing of said components effectively increases mechanical property, the flame retardant property of product, meets in new energy vehicle battery pack
The high standards of lid.
Hollow glass micropearl makes product lightweight, effectively reduces product density in conjunction with subsequent foaming step, meets new
The lightweight requirements of energy vehicle battery pack upper cover.
Oxidation modification graphite, carbon fiber powder cooperate with the mechanical property for improving product with wollastonite in powder, this is because: carbon fiber
Powder and the microcosmic tool fibre morphology of wollastonite in powder, in the preparation process of the first additive, the length of wollastonite in powder and carbon fiber powder
It builds to form size, different hole between the different, fiber that differs in size, the mixed and disorderly nothing of hole outside fiber extending direction
Chapter, it is mutually interspersed, external forces are helped to disperse, high-intensitive load are born, so that humidification is played, in twin-screw extrusion
In melting process, oxidation modification is graphite-filled into hole, to good filling effect is formed between polypropylene chains, to improve
The mechanical property of product.It can also be first heat-treated in the preparation, carry out heavy carbon, further increase the mechanical property of product.
Present invention introduces sodium carboxymethylcellulose, polyvinyl alcohol as carbon source, and sodium polyphosphate is as acid source, hexa-methylene
As foaming agent, said components constitute P-N collaboration Intumescent Retardant System for tetramine, poly (hexamethylene) hydrochloride, greatly improve
The anti-flammability of product, at a lower temperature, sodium polyphosphate generate can esterification polyol and acid as dehydrating agent, slightly higher
At a temperature of release acid, with carbon source (sodium carboxymethylcellulose, polyvinyl alcohol) esterification occurs for acid, six methylenes in system
Urotropine, poly (hexamethylene) hydrochloride accelerate reaction to carry out as catalyst；The vapor that is generated in reaction process and non-ignitable
Property gas make system in a molten state expanded foamed, formed fireprotection layer；Aluminium dihydrogen phosphate is and upper as phosphorus flame retardant
It states P-N collaboration Intumescent Retardant System collocation to use, phosphorous flame-retardant effect can be strengthened, generated in thermal degradation process more inclined
Phosphoric acid and poly-metaphosphoric acid so that comburant dehydration carbonization, when heated between the hydroxyl of aluminium dihydrogen phosphate dehydration formed it is stable more
Polyacetylene compound further strengthens above-mentioned fireprotection layer, forms fine and close layer of charcoal, effectively interruption heat exchange, and prevents imflammable gas
Diffusion and evolution, while oxygen being prevented to spread to bottom, flame retardant effect is further increased, in addition, oxidation modification graphite can be with
Physical barrier effect is played, heat exchange is further interrupted, and oxygen is prevented to spread to bottom, each component collaboration improves the resistance of product
Combustion property.
Since hexa heating easily distils and decomposes, and unavoidably there is high temperature ring when the preparation of the second additive
Border, therefore it is introduced in the first additive, directly progress grinding operation, which is realized, is modified, and avoids significant loss.
Other than objects, features and advantages described above, there are also other objects, features and advantages by the present invention.
The present invention is further detailed explanation below.
Specific embodiment
The embodiment of the present invention is described in detail below, but the present invention can be limited and be covered according to claim
Multitude of different ways implement.
Embodiment 1:
A kind of preparation method of new energy vehicle battery pack upper cover anti-flaming polypropylene material, the specific steps are as follows:
(1) first carbon fiber powder, wollastonite in powder, hollow glass micropearl, hexa and coupling agent mixed grinding are obtained
It is spare to the first additive；
(2) polyvinyl alcohol, aluminium dihydrogen phosphate, sodium polyphosphate are then added into sodium carboxymethyl cellulose solution and gathers
Hexa-methylene guanidine hydrochloride, stirring and dissolving are subsequently added into oxidation modification graphite, supersonic oscillations 30 minutes, obtain suspension, dry
It is dry, it recycles torque rheometer to be kneaded, obtains the second additive, it is spare；
(3) the second additive obtained by the first additive obtained by polypropylene, step (1), step (2) is finally utilized into twin-screw
Extruder melting mixing, injects foaming agent, and underwater cutpellet obtains the granular polypropylene material.
In step (1), carbon fiber powder, wollastonite in powder, hollow glass micropearl, hexa and coupling agent mass ratio
For 1:15:5:2:15.
The specific method of step (1) is: first by carbon fiber powder, wollastonite in powder, hollow glass micropearl mixed grinding 20 minutes,
900 DEG C are then heated to, keeps the temperature 30 minutes, cooled to room temperature (25 DEG C) adds hexa and coupling agent, mixes
Grinding is closed 50 minutes up to first additive.Coupling agent is vinyltrimethoxysilane.The partial size of hollow glass micropearl
It is 100 μm.
In step (2), sodium carboxymethyl cellulose solution, polyvinyl alcohol, aluminium dihydrogen phosphate, sodium polyphosphate, poly- six Asia
Methylguanidine hydrochloride, oxidation modification graphite mass ratio be 1000:2:0.3:1:0.8:0.5, the sodium carboxymethylcellulose water
The mass concentration of solution is 3 ‰.The preparation method of the sodium carboxymethyl cellulose solution are as follows: while stirring carboxymethyl cellulose
Plain sodium is poured slowly into water, and 60 DEG C are stirred 18 hours to get the sodium carboxymethyl cellulose solution.
In step (2), the oxidation modification graphite is to carry out oxidation processes to graphite using Hummer method to obtain, specific to make
Preparation Method is as follows: graphite, the concentrated sulfuric acid, sodium nitrate being added in four-hole bottle, potassium permanganate, 35 DEG C of reactions 30 are added under condition of ice bath
Minute, deionized water is added, 98 DEG C are reacted 30 minutes, and filtration washing immediately is dry, supersonic oscillations handle 20 minutes to get；
Wherein, the mass ratio of graphite, the concentrated sulfuric acid, sodium nitrate, potassium permanganate and deionized water is 1:20:0.5:3:50.
In step (2), the process conditions of mixing are as follows: 150 DEG C are kneaded 20 minutes.
In step (3), the polypropylene is copolymer polypropylene, and under 230 DEG C, the test condition of 2.16kg, melting refers to
Number is 60g/10min.
In step (3), polypropylene, the first additive, the second additive, foaming agent mass ratio be 100:1:0.8:0.9.
In step (3), mixed 2 minutes before double screw extruder melting mixing first with high-speed mixer.
In step (3), foaming agent is diisopropyl azodiformate.
In step (3), the screw diameter of extruder is 30mm, and draw ratio L/D is 30, and machine barrel is divided into 7 heating regions, it
Operating temperature be followed successively by 210 DEG C, 210 DEG C, 205 DEG C, 205 DEG C, 200 DEG C, 200 DEG C, 195 DEG C, engine speed is controlled 300
Rev/min.
In step (3), underwater cutpellet, concrete technology condition are realized using underwater pelletizer are as follows: solution pump is given to be cut under water
The pressure of the melt pressure of the form stable of grain machine, the solution pump is 10MPa, and blow valve temperature is 190 DEG C, and die plate temperature is
180 DEG C, recirculated water water temperature is 75 DEG C, and hydraulic pressure when recirculated water works is 0.5MPa.
A kind of new energy vehicle battery pack upper cover anti-flaming polypropylene material obtained using above-mentioned preparation method.
Embodiment 2:
A kind of preparation method of new energy vehicle battery pack upper cover anti-flaming polypropylene material, the specific steps are as follows:
(1) first carbon fiber powder, wollastonite in powder, hollow glass micropearl, hexa and coupling agent mixed grinding are obtained
It is spare to the first additive；
(2) polyvinyl alcohol, aluminium dihydrogen phosphate, sodium polyphosphate are then added into sodium carboxymethyl cellulose solution and gathers
Hexa-methylene guanidine hydrochloride, stirring and dissolving are subsequently added into oxidation modification graphite, supersonic oscillations 40 minutes, obtain suspension, dry
It is dry, it recycles torque rheometer to be kneaded, obtains the second additive, it is spare；
(3) the second additive obtained by the first additive obtained by polypropylene, step (1), step (2) is finally utilized into twin-screw
Extruder melting mixing, injects foaming agent, and underwater cutpellet obtains the granular polypropylene material.
In step (1), carbon fiber powder, wollastonite in powder, hollow glass micropearl, hexa and coupling agent mass ratio
For 1:20:6:3:20.
The specific method of step (1) is: first by carbon fiber powder, wollastonite in powder, hollow glass micropearl mixed grinding 30 minutes,
1000 DEG C are then heated to, keeps the temperature 40 minutes, cooled to room temperature (25 DEG C) adds hexa and coupling agent,
Mixed grinding 60 minutes up to first additive.Coupling agent is vinyl three ('beta '-methoxy ethyoxyl) silane.Hollow glass
The partial size of glass microballon is 120 μm.
In step (2), sodium carboxymethyl cellulose solution, polyvinyl alcohol, aluminium dihydrogen phosphate, sodium polyphosphate, poly- six Asia
Methylguanidine hydrochloride, oxidation modification graphite mass ratio be 1000:3:0.5:2:1:0.8, the sodium carboxymethylcellulose is water-soluble
The mass concentration of liquid is 3 ‰.The preparation method of the sodium carboxymethyl cellulose solution are as follows: while stirring carboxymethyl cellulose
Sodium is poured slowly into water, and 70 DEG C are stirred 24 hours to get the sodium carboxymethyl cellulose solution.
In step (2), the oxidation modification graphite is to carry out oxidation processes to graphite using Hummer method to obtain, specific to make
Preparation Method is as follows: graphite, the concentrated sulfuric acid, sodium nitrate being added in four-hole bottle, potassium permanganate, 35 DEG C of reactions 30 are added under condition of ice bath
Minute, deionized water is added, 98 DEG C are reacted 30 minutes, and filtration washing immediately is dry, supersonic oscillations handle 30 minutes to get；
Wherein, the mass ratio of graphite, the concentrated sulfuric acid, sodium nitrate, potassium permanganate and deionized water is 1:20:0.5:3:50.
In step (2), the process conditions of mixing are as follows: 180 DEG C are kneaded 30 minutes.
In step (3), the polypropylene is homopolypropylene, and under 230 DEG C, the test condition of 2.16kg, melting refers to
Number is 100g/10min.
In step (3), polypropylene, the first additive, the second additive, foaming agent mass ratio be 100:2:1:1.1.
In step (3), mixed 3 minutes before double screw extruder melting mixing first with high-speed mixer.
In step (3), foaming agent 4,4'- oxobenzenesulfonyl hydrazide.
In step (3), the screw diameter of extruder is 40mm, and draw ratio L/D is 40, and machine barrel is divided into 7 heating regions, it
Operating temperature be followed successively by 210 DEG C, 210 DEG C, 205 DEG C, 205 DEG C, 200 DEG C, 200 DEG C, 195 DEG C, engine speed is controlled 500
Rev/min.
In step (3), underwater cutpellet, concrete technology condition are realized using underwater pelletizer are as follows: solution pump is given to be cut under water
The pressure of the melt pressure of the form stable of grain machine, the solution pump is 15MPa, and blow valve temperature is 200 DEG C, and die plate temperature is
190 DEG C, recirculated water water temperature is 85 DEG C, and hydraulic pressure when recirculated water works is 0.8MPa.
A kind of new energy vehicle battery pack upper cover anti-flaming polypropylene material obtained using above-mentioned preparation method.
Embodiment 3:
A kind of preparation method of new energy vehicle battery pack upper cover anti-flaming polypropylene material, the specific steps are as follows:
(1) first carbon fiber powder, wollastonite in powder, hollow glass micropearl, hexa and coupling agent mixed grinding are obtained
It is spare to the first additive；
(2) polyvinyl alcohol, aluminium dihydrogen phosphate, sodium polyphosphate are then added into sodium carboxymethyl cellulose solution and gathers
Hexa-methylene guanidine hydrochloride, stirring and dissolving are subsequently added into oxidation modification graphite, supersonic oscillations 30 minutes, obtain suspension, dry
It is dry, it recycles torque rheometer to be kneaded, obtains the second additive, it is spare；
(3) the second additive obtained by the first additive obtained by polypropylene, step (1), step (2) is finally utilized into twin-screw
Extruder melting mixing, injects foaming agent, and underwater cutpellet obtains the granular polypropylene material.
In step (1), carbon fiber powder, wollastonite in powder, hollow glass micropearl, hexa and coupling agent mass ratio
For 1:20:5:3:15.
The specific method of step (1) is: first by carbon fiber powder, wollastonite in powder, hollow glass micropearl mixed grinding 30 minutes,
900 DEG C are then heated to, keeps the temperature 40 minutes, cooled to room temperature (25 DEG C) adds hexa and coupling agent, mixes
Grinding is closed 50 minutes up to first additive.Coupling agent is vinyltrimethoxysilane.The partial size of hollow glass micropearl
It is 120 μm.
In step (2), sodium carboxymethyl cellulose solution, polyvinyl alcohol, aluminium dihydrogen phosphate, sodium polyphosphate, poly- six Asia
Methylguanidine hydrochloride, oxidation modification graphite mass ratio be 1000:2:0.5:1:1:0.5, the sodium carboxymethylcellulose is water-soluble
The mass concentration of liquid is 3 ‰.The preparation method of the sodium carboxymethyl cellulose solution are as follows: while stirring carboxymethyl cellulose
Sodium is poured slowly into water, and 70 DEG C are stirred 18 hours to get the sodium carboxymethyl cellulose solution.
In step (2), the oxidation modification graphite is to carry out oxidation processes to graphite using Hummer method to obtain, specific to make
Preparation Method is as follows: graphite, the concentrated sulfuric acid, sodium nitrate being added in four-hole bottle, potassium permanganate, 35 DEG C of reactions 30 are added under condition of ice bath
Minute, deionized water is added, 98 DEG C are reacted 30 minutes, and filtration washing immediately is dry, supersonic oscillations handle 30 minutes to get；
Wherein, the mass ratio of graphite, the concentrated sulfuric acid, sodium nitrate, potassium permanganate and deionized water is 1:20:0.5:3:50.
In step (2), the process conditions of mixing are as follows: 150 DEG C are kneaded 30 minutes.
In step (3), the polypropylene is copolymer polypropylene, and under 230 DEG C, the test condition of 2.16kg, melting refers to
Number is 60g/10min.
In step (3), polypropylene, the first additive, the second additive, foaming agent mass ratio be 100:2:0.8:1.1.
In step (3), mixed 2 minutes before double screw extruder melting mixing first with high-speed mixer.
In step (3), foaming agent is chloroform.
In step (3), the screw diameter of extruder is 40mm, and draw ratio L/D is 30, and machine barrel is divided into 7 heating regions, it
Operating temperature be followed successively by 210 DEG C, 210 DEG C, 205 DEG C, 205 DEG C, 200 DEG C, 200 DEG C, 195 DEG C, engine speed is controlled 500
Rev/min.
In step (3), underwater cutpellet, concrete technology condition are realized using underwater pelletizer are as follows: solution pump is given to be cut under water
The pressure of the melt pressure of the form stable of grain machine, the solution pump is 10MPa, and blow valve temperature is 200 DEG C, and die plate temperature is
180 DEG C, recirculated water water temperature is 85 DEG C, and hydraulic pressure when recirculated water works is 0.5MPa.
A kind of new energy vehicle battery pack upper cover anti-flaming polypropylene material obtained using above-mentioned preparation method.
Embodiment 4:
A kind of preparation method of new energy vehicle battery pack upper cover anti-flaming polypropylene material, the specific steps are as follows:
(1) first carbon fiber powder, wollastonite in powder, hollow glass micropearl, hexa and coupling agent mixed grinding are obtained
It is spare to the first additive；
(2) polyvinyl alcohol, aluminium dihydrogen phosphate, sodium polyphosphate are then added into sodium carboxymethyl cellulose solution and gathers
Hexa-methylene guanidine hydrochloride, stirring and dissolving are subsequently added into oxidation modification graphite, supersonic oscillations 40 minutes, obtain suspension, dry
It is dry, it recycles torque rheometer to be kneaded, obtains the second additive, it is spare；
(3) the second additive obtained by the first additive obtained by polypropylene, step (1), step (2) is finally utilized into twin-screw
Extruder melting mixing, injects foaming agent, and underwater cutpellet obtains the granular polypropylene material.
In step (1), carbon fiber powder, wollastonite in powder, hollow glass micropearl, hexa and coupling agent mass ratio
For 1:15:6:2:20.
The specific method of step (1) is: first by carbon fiber powder, wollastonite in powder, hollow glass micropearl mixed grinding 20 minutes,
1000 DEG C are then heated to, keeps the temperature 30 minutes, cooled to room temperature (25 DEG C) adds hexa and coupling agent,
Mixed grinding 60 minutes up to first additive.Coupling agent is vinyl three ('beta '-methoxy ethyoxyl) silane.Hollow glass
The partial size of glass microballon is 100 μm.
In step (2), sodium carboxymethyl cellulose solution, polyvinyl alcohol, aluminium dihydrogen phosphate, sodium polyphosphate, poly- six Asia
Methylguanidine hydrochloride, oxidation modification graphite mass ratio be 1000:3:0.3:2:0.8:0.8, the sodium carboxymethylcellulose water
The mass concentration of solution is 3 ‰.The preparation method of the sodium carboxymethyl cellulose solution are as follows: while stirring carboxymethyl cellulose
Plain sodium is poured slowly into water, and 60 DEG C are stirred 24 hours to get the sodium carboxymethyl cellulose solution.
In step (2), the oxidation modification graphite is to carry out oxidation processes to graphite using Hummer method to obtain, specific to make
Preparation Method is as follows: graphite, the concentrated sulfuric acid, sodium nitrate being added in four-hole bottle, potassium permanganate, 35 DEG C of reactions 30 are added under condition of ice bath
Minute, deionized water is added, 98 DEG C are reacted 30 minutes, and filtration washing immediately is dry, supersonic oscillations handle 20 minutes to get；
Wherein, the mass ratio of graphite, the concentrated sulfuric acid, sodium nitrate, potassium permanganate and deionized water is 1:20:0.5:3:50.
In step (2), the process conditions of mixing are as follows: 180 DEG C are kneaded 20 minutes.
In step (3), the polypropylene is homopolypropylene, and under 230 DEG C, the test condition of 2.16kg, melting refers to
Number is 100g/10min.
In step (3), polypropylene, the first additive, the second additive, foaming agent mass ratio be 100:1:1:0.9.
In step (3), mixed 3 minutes before double screw extruder melting mixing first with high-speed mixer.
In step (3), foaming agent is pentane.
In step (3), the screw diameter of extruder is 30mm, and draw ratio L/D is 40, and machine barrel is divided into 7 heating regions, it
Operating temperature be followed successively by 210 DEG C, 210 DEG C, 205 DEG C, 205 DEG C, 200 DEG C, 200 DEG C, 195 DEG C, engine speed is controlled 300
Rev/min.
In step (3), underwater cutpellet, concrete technology condition are realized using underwater pelletizer are as follows: solution pump is given to be cut under water
The pressure of the melt pressure of the form stable of grain machine, the solution pump is 15MPa, and blow valve temperature is 190 DEG C, and die plate temperature is
190 DEG C, recirculated water water temperature is 75 DEG C, and hydraulic pressure when recirculated water works is 0.8MPa.
A kind of new energy vehicle battery pack upper cover anti-flaming polypropylene material obtained using above-mentioned preparation method.
Embodiment 5:
A kind of preparation method of new energy vehicle battery pack upper cover anti-flaming polypropylene material, the specific steps are as follows:
(1) first carbon fiber powder, wollastonite in powder, hollow glass micropearl, hexa and coupling agent mixed grinding are obtained
It is spare to the first additive；
(2) polyvinyl alcohol, aluminium dihydrogen phosphate, sodium polyphosphate are then added into sodium carboxymethyl cellulose solution and gathers
Hexa-methylene guanidine hydrochloride, stirring and dissolving are subsequently added into oxidation modification graphite, supersonic oscillations 35 minutes, obtain suspension, dry
It is dry, it recycles torque rheometer to be kneaded, obtains the second additive, it is spare；
(3) the second additive obtained by the first additive obtained by polypropylene, step (1), step (2) is finally utilized into twin-screw
Extruder melting mixing, injects foaming agent, and underwater cutpellet obtains the granular polypropylene material.
In step (1), carbon fiber powder, wollastonite in powder, hollow glass micropearl, hexa and coupling agent mass ratio
For 1:18:5.5:2.5:18.
The specific method of step (1) is: first by carbon fiber powder, wollastonite in powder, hollow glass micropearl mixed grinding 25 minutes,
950 DEG C are then heated to, keeps the temperature 35 minutes, cooled to room temperature (25 DEG C) adds hexa and coupling agent, mixes
Grinding is closed 55 minutes up to first additive.Coupling agent is vinyl three ('beta '-methoxy ethyoxyl) silane.Hollow glass
The partial size of microballon is 110 μm.
In step (2), sodium carboxymethyl cellulose solution, polyvinyl alcohol, aluminium dihydrogen phosphate, sodium polyphosphate, poly- six Asia
Methylguanidine hydrochloride, oxidation modification graphite mass ratio be 1000:2.5:0.4:1.5:0.9:0.7, the carboxymethyl cellulose
The mass concentration of sodium water solution is 3 ‰.The preparation method of the sodium carboxymethyl cellulose solution are as follows: while stirring carboxymethyl
Sodium cellulosate is poured slowly into water, and 65 DEG C are stirred 20 hours to get the sodium carboxymethyl cellulose solution.
In step (2), the oxidation modification graphite is to carry out oxidation processes to graphite using Hummer method to obtain, specific to make
Preparation Method is as follows: graphite, the concentrated sulfuric acid, sodium nitrate being added in four-hole bottle, potassium permanganate, 35 DEG C of reactions 30 are added under condition of ice bath
Minute, deionized water is added, 98 DEG C are reacted 30 minutes, and filtration washing immediately is dry, supersonic oscillations handle 25 minutes to get；
Wherein, the mass ratio of graphite, the concentrated sulfuric acid, sodium nitrate, potassium permanganate and deionized water is 1:20:0.5:3:50.
In step (2), the process conditions of mixing are as follows: 170 DEG C are kneaded 25 minutes.
In step (3), the polypropylene is copolymer polypropylene, and under 230 DEG C, the test condition of 2.16kg, melting refers to
Number is 80g/10min.
In step (3), polypropylene, the first additive, the second additive, foaming agent mass ratio be 100:1.5:0.9:1.
In step (3), mixed 2 minutes before double screw extruder melting mixing first with high-speed mixer.
In step (3), foaming agent is diisopropyl azodiformate.
In step (3), the screw diameter of extruder is 35mm, and draw ratio L/D is 35, and machine barrel is divided into 7 heating regions, it
Operating temperature be followed successively by 210 DEG C, 210 DEG C, 205 DEG C, 205 DEG C, 200 DEG C, 200 DEG C, 195 DEG C, engine speed is controlled 400
Rev/min.
In step (3), underwater cutpellet, concrete technology condition are realized using underwater pelletizer are as follows: solution pump is given to be cut under water
The pressure of the melt pressure of the form stable of grain machine, the solution pump is 12MPa, and blow valve temperature is 195 DEG C, and die plate temperature is
185 DEG C, recirculated water water temperature is 80 DEG C, and hydraulic pressure when recirculated water works is 0.6MPa.
A kind of new energy vehicle battery pack upper cover anti-flaming polypropylene material obtained using above-mentioned preparation method.
Comparative example 1
Carbon fiber powder in omited steps (1), remaining is the same as embodiment 1.
Comparative example 2
Wollastonite in powder in omited steps (1), remaining is the same as embodiment 1.
Comparative example 3
Hollow glass micro-ball in omited steps (1), remaining is the same as embodiment 1.
Comparative example 4
Hexa in omited steps (1), remaining is the same as embodiment 1.
Comparative example 5
Sodium carboxymethyl cellulose solution in step (2) is replaced with into water, remaining is the same as embodiment 1.
Comparative example 6
Polyvinyl alcohol in omited steps (2), remaining is the same as embodiment 1.
Comparative example 7
Aluminium dihydrogen phosphate in omited steps (2), remaining is the same as embodiment 1.
Comparative example 8
Sodium polyphosphate in omited steps (2), remaining is the same as embodiment 1.
Comparative example 9
Poly (hexamethylene) hydrochloride in omited steps (2), remaining is the same as embodiment 1.
Comparative example 10
Oxidation modification graphite in omited steps (2), remaining is the same as embodiment 1.
Comparative example 11
The unimplanted foaming agent in step (3).
Test example
Examples 1 to 5 and 1~11 gained polypropylene material of comparative example are tested for the property, the results are shown in Table 1.
1. the performance test results of table
As shown in Table 1, the polypropylene material of Examples 1 to 5 has excellent mechanical property and anti-flammability, and density is small, full
The lightweight requirements of sufficient new energy vehicle battery pack upper cover.Carbon fiber powder in 1 omited steps of comparative example (1), comparative example 2 omit step
Suddenly the wollastonite in powder in (1), the mechanical property of product are obviously deteriorated；Hollow glass micro-ball in 3 omited steps of comparative example (1),
Product density becomes larger；Hexa in 4 omited steps of comparative example (1), comparative example 5 are fine by the carboxymethyl in step (2)
It ties up plain sodium water solution and replaces with water, the polyvinyl alcohol in 6 omited steps of comparative example (2), the phosphorus in 7 omited steps of comparative example (2)
Acid dihydride aluminium, the sodium polyphosphate in 8 omited steps of comparative example (2), the polyhexamethylene guanide in 9 omited steps of comparative example (2)
The anti-flammability of hydrochloride, product is obviously deteriorated；Oxidation modification graphite in 10 omited steps of comparative example (2), the mechanical property of product
It can obviously be deteriorated with anti-flammability；Comparative example 11 unimplanted foaming agent, density of product in step (3) obviously become larger.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of new energy vehicle battery pack upper cover anti-flaming polypropylene material, which is characterized in that specific steps are such as
Under:
(1) carbon fiber powder, wollastonite in powder, hollow glass micropearl, hexa and coupling agent mixed grinding are first obtained
One additive, it is spare；
(2) polyvinyl alcohol, aluminium dihydrogen phosphate, sodium polyphosphate and poly- six Asia are then added into sodium carboxymethyl cellulose solution
Methylguanidine hydrochloride, stirring and dissolving are subsequently added into oxidation modification graphite, supersonic oscillations 30~40 minutes, obtain suspension, dry
It is dry, it recycles torque rheometer to be kneaded, obtains the second additive, it is spare；
(3) the second additive obtained by the first additive obtained by polypropylene, step (1), step (2) is finally utilized into twin-screw extrusion
Machine melting mixing, injects foaming agent, and underwater cutpellet obtains the granular polypropylene material.
2. preparation method according to claim 1, which is characterized in that carbon fiber powder, wollastonite in powder, hollow in step (1)
The mass ratio of glass microballoon, hexa and coupling agent is 1:15~20:5~6:2~3:15~20.
3. preparation method according to claim 1, which is characterized in that the specific method of step (1) is: first by carbon fiber
Powder, wollastonite in powder, hollow glass micropearl mixed grinding 20~30 minutes are then heated to 900~1000 DEG C, keep the temperature 30~40 points
Clock, cooled to room temperature add hexa and coupling agent, add up to described first within mixed grinding 50~60 minutes
Charging.
4. preparation method according to claim 3, which is characterized in that the coupling agent be vinyltrimethoxysilane or
Any one of vinyl three ('beta '-methoxy ethyoxyl) silane.
5. preparation method according to claim 1, which is characterized in that in step (2), sodium carboxymethyl cellulose solution,
Polyvinyl alcohol, aluminium dihydrogen phosphate, sodium polyphosphate, poly (hexamethylene) hydrochloride, oxidation modification graphite mass ratio be 1000:
2~3:0.3~0.5:1~2:0.8~1:0.5~0.8, the mass concentration of the sodium carboxymethyl cellulose solution are 3 ‰.
6. preparation method according to claim 1, which is characterized in that in step (2), the process conditions of mixing are as follows: 150~
180 DEG C are kneaded 20~30 minutes.
7. preparation method according to claim 1, which is characterized in that in step (3), the polypropylene is copolymer polypropylene
Or homopolypropylene, under 230 DEG C, the test condition of 2.16kg, melt index is 60~100g/10min.
8. preparation method according to claim 1, which is characterized in that in step (3), polypropylene, the first additive, second
Additive, foaming agent mass ratio be 100:1~2:0.8~1:0.9~1.1.
9. preparation method according to claim 1, which is characterized in that in step (3), realized using underwater pelletizer underwater
Pelletizing, concrete technology condition are as follows: solution pump gives the melt pressure of the form stable of underwater pelletizer, the pressure of the solution pump
For 10~15MPa, blow valve temperature is 190~200 DEG C, and die plate temperature is 180~190 DEG C, and recirculated water water temperature is 75~85 DEG C,
Hydraulic pressure when recirculated water works is 0.5~0.8MPa.
10. a kind of new energy vehicle battery pack upper cover obtained using preparation method described in any one of claim 1~9 is with fire-retardant
Polypropylene material.
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