CN109161092A - A kind of graphene-expanded polypropylene composite material and preparation method - Google Patents
A kind of graphene-expanded polypropylene composite material and preparation method Download PDFInfo
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- CN109161092A CN109161092A CN201810702715.XA CN201810702715A CN109161092A CN 109161092 A CN109161092 A CN 109161092A CN 201810702715 A CN201810702715 A CN 201810702715A CN 109161092 A CN109161092 A CN 109161092A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/102—Azo-compounds
- C08J9/103—Azodicarbonamide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
Abstract
The invention discloses a kind of graphene-expanded polypropylene composite material and preparation methods, it is added in polypropylene and is uniformly mixed by the foaming agent and graphene oxide microballoon that will premix, after first step low-temp foaming, hole is formed inside polypropylene, graphene oxide microballoon is distributed in inside hole, again after second step foams, foaming agent further decomposes so that hole is able to continued growth, and the graphene oxide microballoon in hole is expanded and is restored, it is gradually filled with hole, finally obtains the expanded polypropylene material of porous graphene filling.Graphene is filled in polypropylene hole, plays the role of support, greatly enhances the intensity and elasticity of foamed material, and can improve other mechanical properties of material.
Description
Technical field
The invention belongs to field of compound material more particularly to a kind of graphene-expanded polypropylene composite material and its preparations
Method.
Background technique
Polypropylene is a kind of thermoplastic resin as prepared by propylene polymerization, usually translucent colorless solid, odorless nothing
Poison.The highly crystallized due to compound with regular structure, PP foam material have excellent heat resistance, corrosion resistance, and product is available
Moise-heat sterilization is its outstanding advantages；Its environmental-friendly performance is outstanding, releases when burning, is easily recycled without poison gas.Polypropylene plastics
Density is small, is most light general-purpose plastics, is widely used in the fields such as packaging, automobile, aerospace, but the disadvantage is that low temperature resistant punching
Hitting property is poor, easy to aging, has to be overcome.
Graphene is a kind of two-dimentional carbon material with monoatomic layer thickness, has low-density, high mechanical strength, heat
Conductance and conductivity and excellent corrosion resistance, and it is good with the compatibility of high molecular material, it can be used as the increasing of high molecular material
Strong body uses.The performance indexes of material can be obviously improved by (being lower than 1%) under extremely low additive amount, have wide city
Field prospect.
The present invention utilizes the thermal instability of graphene oxide microballoon, and graphene oxide microballoon and foaming agent is total in advance
It is mixed, it adds in the mixed system of polypropylene and other auxiliary agents.In first segment foaming, foaming agent first decomposites gas poly- third
Hole is formed in alkene, and graphene oxide microballoon then stays in these holes.After temperature is further promoted, one side foaming agent
It decomposes completely, hole growth is promoted to expand, the oxygen-containing group on another aspect graphene oxide sheet surface decomposes, so that graphite oxide
Volume expansion occurs for alkene microballoon, to gradually be filled into polyacrylic hole, forms supporting network structure, it is strong to improve melt
Degree, prevents cell collapse.Finally the mechanical property of composite material is obviously improved, and due to the presence of graphene, so that
Composite foam obtains a degree of promotion to the stability of light, heat.
Summary of the invention
The purpose of the present invention is aiming at the shortcomings of the prior art, provide a kind of graphene-expanded polypropylene composite material and
Preparation method.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of preparation method of graphene-expanded polypropylene composite material, comprising the following steps:
(1) will be dry having a size of 1~50 micron of single-layer graphene oxide dispersion liquid by atomization drying method, it is aoxidized
Graphene microballoon, carbon-to-oxygen ratio are 3~6.
(2) 1~10 mass parts graphene oxide microballoon for obtaining step (1) mixes with 2~4 mass parts foaming agents
It is even.
(3) by 100 mass parts polypropylene and 0.2~0.6 part of stearic acid, 0.3~1 part of cumyl peroxide, 0.6~1
Part zinc oxide, which is added in mixer, carries out mixing, and temperature is 150~200 DEG C.
(4) mixer is added together with the product of step (2) in the product of step (3), in 100~110 DEG C of mixings.
(5) mold is added in the product for obtaining step (4), foams 3~10 minutes at 115~135 DEG C, is warming up to 136
~200 DEG C are foamed 5~20 minutes.
Further, the atomization drying temperature of the step (1) is 130~200 DEG C.
Further, the foaming agent of the step (2) is AC foaming agent, and decomposition temperature is 130~140 DEG C.
The beneficial effects of the present invention are:
(1) using two steps foaming technique, graphene film be overlapped to form porous network be filled in expanded polypropylene hole it
In.Wherein, form primary hole configurations in the first foaming stages, graphene oxide microballoon be selectively present in these holes it
In.Graphene oxide is set to be reduced to graphene in the oxygen-containing functional group fast eliminating of the second foaming stages surface of graphene oxide,
Graphene oxide microballoon occurs volume expansion and is full of hole, while foaming agent further decomposes, and forms supporting network structure, mentions
High fondant-strength prevents cell collapse.
(2) graphene film is mutually lapped to form network structure in hole, since direction has height to graphene film in face
Strong high mould performance has excellent flexibility in normal direction, thus after forming network, the tensile strength of expanded polypropylene can not only be promoted
Etc. mechanical properties, while can be promoted its to light, electricity, heat stability.
To sum up, the expanded polypropylene obtained using this method not only in mechanical property have outstanding representation, light, electricity,
Also there is broad prospect of application in the multifunctionality such as heat, suitable for modern multi-functional, mass production, simple and easy requirement.
Specific embodiment
Graphene-expanded polypropylene composite material method is prepared to include the following steps:
(1) will be dry having a size of 1~50 micron of single-layer graphene oxide dispersion liquid by atomization drying method, it is aoxidized
Graphene microballoon, carbon-to-oxygen ratio are 3~6.The atomization drying temperature is 130~200 DEG C.(2) by step (1) obtain 1~
10 mass parts graphene oxide microballoons are uniformly mixed with 2~4 mass parts foaming agents.The foaming agent is AC foaming agent, decomposes temperature
Degree is 130~140 DEG C.(3) by 100 mass parts polypropylene and 0.2~0.6 part of stearic acid, 0.3~1 part of cumyl peroxide,
0.6~1 part of zinc oxide, which is added in mixer, carries out mixing, and temperature is 150~200 DEG C.(4) by the product and step of step (3)
(2) mixer is added in product together, in 100~110 DEG C of mixings.(5) mold is added in the product for obtaining step (4), 115
It foams 3~10 minutes at~135 DEG C, is warming up to 136~200 DEG C and foams 5~20 minutes.
The present invention is specifically described below by embodiment, the present embodiment is served only for doing further the present invention
It is bright, it should not be understood as limiting the scope of the invention, those skilled in the art makes one according to the content of foregoing invention
A little nonessential changes and adjustment belong to protection scope of the present invention.
Embodiment 1:
(1) will be dry having a size of 1~10 micron of single-layer graphene oxide dispersion liquid by atomization drying method, it is aoxidized
Graphene microballoon, carbon-to-oxygen ratio 3.Atomization drying temperature is 130 DEG C.
(2) the 1 mass parts graphene oxide microballoon that step (1) obtains is uniformly mixed with 2 mass parts AC foaming agents.
(3) by 100 mass parts polypropylene and 0.2 part of stearic acid, 0.3 part of cumyl peroxide, 0.6 part of zinc oxide addition
Mixing is carried out in mixer, temperature is 150 DEG C.
(4) mixer is added together with the product of step (2) in the product of step (3), in 100 DEG C of mixings.
(5) mold is added in the product for obtaining step (4), foams 10 minutes at 115 DEG C, is warming up to 136 DEG C of foaming 20
Minute.
Through above step, graphene-expanded polypropylene composite material is obtained, specific performance is as shown in table 1.
Embodiment 2:
(1) will be dry having a size of 10~20 microns of single-layer graphene oxide dispersion liquid by atomization drying method, obtain oxygen
Graphite alkene microballoon, carbon-to-oxygen ratio 4.Atomization drying temperature is 145 DEG C.
(2) the 3 mass parts graphene oxide microballoons that step (1) obtains are uniformly mixed with 3 mass parts AC foaming agents.
(3) by 100 mass parts polypropylene and 0.3 part of stearic acid, 0.5 part of cumyl peroxide, 0.8 part of zinc oxide addition
Mixing is carried out in mixer, temperature is 160 DEG C.
(4) mixer is added together with the product of step (2) in the product of step (3), in 100 DEG C of mixings.
(5) mold is added in the product for obtaining step (4), foams 7 minutes at 125 DEG C, is warming up to 150 DEG C and foams 13 points
Clock.
Through above step, graphene-expanded polypropylene composite material is obtained, specific performance is as shown in table 1.
Embodiment 3:
(1) will be dry having a size of 20~30 microns of single-layer graphene oxide dispersion liquid by atomization drying method, obtain oxygen
Graphite alkene microballoon, carbon-to-oxygen ratio 5.Atomization drying temperature is 170 DEG C.
(2) the 5 mass parts graphene oxide microballoons that step (1) obtains are uniformly mixed with 4 mass parts AC foaming agents.
(3) by 100 mass parts polypropylene and 0.6 part of stearic acid, 0.7 part of cumyl peroxide, 1.0 parts of zinc oxide additions
Mixing is carried out in mixer, temperature is 170 DEG C.
(4) mixer is added together with the product of step (2) in the product of step (3), in 110 DEG C of mixings.
(5) mold is added in the product for obtaining step (4), foams 8 minutes at 130 DEG C, is warming up to 200 DEG C and foams 5 points
Clock.
Through above step, graphene-expanded polypropylene composite material is obtained, specific performance is as shown in table 1.
Embodiment 4:
(1) will be dry having a size of 40~50 microns of single-layer graphene oxide dispersion liquid by atomization drying method, obtain oxygen
Graphite alkene microballoon, carbon-to-oxygen ratio 6.Atomization drying temperature is 200 DEG C.
(2) the 1 mass parts graphene oxide microballoon that step (1) obtains is uniformly mixed with 2 mass parts AC foaming agents.
(3) by 100 mass parts polypropylene and 0.4 part of stearic acid, 0.9 part of cumyl peroxide, 0.7 part of zinc oxide addition
Mixing is carried out in mixer, temperature is 180 DEG C.
(4) mixer is added together with the product of step (2) in the product of step (3), in 107 DEG C of mixings.
(5) mold is added in the product for obtaining step (4), foams 10 minutes at 130 DEG C, is warming up to 195 DEG C and foams 5 points
Clock.
Through above step, graphene-expanded polypropylene composite material is obtained, specific performance is as shown in table 1.
Embodiment 5:
(1) will be dry having a size of 40~50 microns of single-layer graphene oxide dispersion liquid by atomization drying method, obtain oxygen
Graphite alkene microballoon, carbon-to-oxygen ratio 5.Atomization drying temperature is 190 DEG C.
(2) the 10 mass parts graphene oxide microballoons that step (1) obtains are uniformly mixed with 4 mass parts AC foaming agents.
(3) by 100 mass parts polypropylene and 0.5 part of stearic acid, 1.0 parts of cumyl peroxides, 0.9 part of zinc oxide addition
Mixing is carried out in mixer, temperature is 200 DEG C.
(4) mixer is added together with the product of step (2) in the product of step (3), in 110 DEG C of mixings.
(5) mold is added in the product for obtaining step (4), foams 3 minutes at 135 DEG C, is warming up to 200 DEG C and foams 5 points
Clock.
Through above step, graphene-expanded polypropylene composite material is obtained, specific performance is as shown in table 1.
Comparative example 1: graphene oxide microballoon is not added and prepares expanded polypropylene.
Comparative example 2:
(1) by atomization drying method that 0.1~5 micron of size of single-layer graphene oxide dispersion liquid is dry, it is aoxidized
Graphene microballoon, carbon-to-oxygen ratio 3.Atomization drying temperature is 130 DEG C.
, with embodiment 1, specific performance is as shown in table 1 for remaining.
Comparative example 3:
(1) by atomization drying method that 100~300 microns of size of single-layer graphene oxide dispersion liquid is dry, obtain oxygen
Graphite alkene microballoon, carbon-to-oxygen ratio 3.Atomization drying temperature is 130 DEG C.
, with embodiment 1, specific performance is as shown in table 1 for remaining.
Comparative example 4:
(1) by atomization drying method that 40~50 microns of size of single-layer graphene oxide dispersion liquid is dry, it is aoxidized
Graphene microballoon, carbon-to-oxygen ratio 10.Atomization drying temperature is 250 DEG C.
, with embodiment 1, specific performance is as shown in table 1 for remaining.
Comparative example 5:
(1) by atomization drying method that 40~50 microns of size of single-layer graphene oxide dispersion liquid is dry, it is aoxidized
Graphene microballoon, carbon-to-oxygen ratio 3.Atomization drying temperature is 250 DEG C.
(2) the 0.5 mass parts graphene oxide microballoon that step (1) obtains is uniformly mixed with 2 mass parts AC foaming agents.
(3) by 100 mass parts polypropylene and 0.3 part of stearic acid, 0.5 part of cumyl peroxide, 0.7 part of zinc oxide addition
Mixing is carried out in mixer, temperature is 150 DEG C.
, with embodiment 1, specific performance is as shown in table 1 for remaining.
Comparative example 6:
(1) by atomization drying method that 40~50 microns of size of single-layer graphene oxide dispersion liquid is dry, it is aoxidized
Graphene microballoon, carbon-to-oxygen ratio 3.Atomization drying temperature is 250 DEG C.
(2) the 20 mass parts graphene oxide microballoons that step (1) obtains are uniformly mixed with 2 mass parts AC foaming agents.
(3) by 100 mass parts polypropylene and 0.3 part of stearic acid, 0.5 part of cumyl peroxide, 0.7 part of zinc oxide addition
Mixing is carried out in mixer, temperature is 150 DEG C.
, with embodiment 1, specific performance is as shown in table 1 for remaining.
Comparative example 7:
(1) being dried by air blast will be dry having a size of 1~5 micron of single-layer graphene oxide dispersion liquid, obtains oxidation stone
Black alkene dry powder, carbon-to-oxygen ratio 10.Drying temperature is 180 DEG C.
(2) the 5 mass parts graphene oxide dry powder that step (1) obtains are uniformly mixed with 2 mass parts AC foaming agents.
(3) by 100 mass parts polypropylene and 0.3 part of stearic acid, 0.5 part of cumyl peroxide, 0.7 part of zinc oxide addition
Mixing is carried out in mixer, temperature is 150 DEG C.
(4) mixer is added together with the product of step (2) in the product of step (3), in 100 DEG C of mixings.
(5) mold is added in the product for obtaining step (4), foams 3 minutes at 135 DEG C, is warming up to 150 DEG C and foams 5 points
Clock
Through above step, graphene-expanded polypropylene composite material is obtained, specific performance is as shown in table 1.
Comparative example 8:
(1) being dried by air blast will be dry having a size of 1~5 micron of single-layer graphene oxide dispersion liquid, obtains oxidation stone
Black alkene dry powder, carbon-to-oxygen ratio 3.Drying temperature is 180 DEG C.
(2) the 5 mass parts graphene oxide dry powder that step (1) obtains are uniformly mixed with 2 mass parts AC foaming agents.
(3) by 100 mass parts polypropylene and 0.3 part of stearic acid, 0.5 part of cumyl peroxide, 0.7 part of zinc oxide addition
Mixing is carried out in mixer, temperature is 150 DEG C.
(4) mixer is added together with the product of step (2) in the product of step (3), in 100 DEG C of mixings.
(5) mold is added in the product for obtaining step (4), foams 15 minutes at 170 DEG C.
Through above step, graphene-expanded polypropylene composite material is obtained, specific performance is as shown in table 1.
1 embodiment of table and comparative example relevant parameter and product property
It can be seen that the graphene oxide ruler at 1~50 micron from the comparison of embodiment 1,2,3 and comparative example 1,2,3
The excellent combination property of expanded polypropylene in very little range.When lamella size is too small, graphene film can not effectively play reinforcing effect
(comparative example 2), and it is oversized when, the contact area between graphene oxide sheet increases, and leads to the attraction between graphene oxide sheet
Power increases, and can not effectively expand in a heated state, and final product is still that spherical graphite alkene particle is present among hole, rises not
To reinforcing effect (comparative example 3).
As can be seen that the control of graphene oxide carbon-to-oxygen ratio is relatively more reasonable 3~6 from embodiment Isosorbide-5-Nitrae and comparative example 4, carbon
Oxygen than it is excessively high when, surface group quantity is few, it is difficult to make graphene oxide microsphere expansion (comparative example 4).Carbon-to-oxygen ratio is difficult lower than 3 comparisons
Large-sized graphene oxide is obtained, therefore is not discussed here.
From embodiment Isosorbide-5-Nitrae, 5 and comparative example 5,6 in as can be seen that graphene oxide additive amount between 1~10% most
It is reasonable.When additive amount is too low, it can not be effectively formed enhancing network, it is bad to the promotion of performance (comparative example 5).Adding too much
When, although can also effectively play humidification, performance has no compared with 10% and is obviously improved, therefore from cost performance isogonism
Degree considers to control additive amount lower than 10% (comparative example 6).
As can be seen that having by the graphene oxide powder that traditional stoving process obtains from embodiment 1 and comparative example 7
Higher carbon-to-oxygen ratio, this is because taking more time under forced air drying could sufficiently remove water.And this graphene oxide
Powder is existed with sheet stacking form, cannot effectively be expanded under heating condition, the performance of graphene is unable to give full play, to hair
Foam material performance contribution is little.
From embodiment 1 and comparative example 8 as can be seen that when being directly warming up to second stage when foaming, the performance of material
It is bad.This is because at relatively high temperatures, foaming agent and graphene oxide microballoon expand simultaneously, and graphene oxide microballoon is poly-
Compressed effect in polypropylene matrix, can not effectively expand, thus while foaming agent itself can be effectively formed hole, graphite oxide
The expansion effect of alkene is bad, and material overall performance and pure expanded polypropylene are close.
Claims (5)
1. a kind of preparation method of graphene-expanded polypropylene, which comprises the following steps:
(1) will be dry having a size of 1~50 micron of single-layer graphene oxide dispersion liquid by atomization drying method, obtain graphite oxide
Alkene microballoon, carbon-to-oxygen ratio are 3~6.
(2) 1~10 mass parts graphene oxide microballoon for obtaining step (1) is uniformly mixed with 2~4 mass parts foaming agents.
(3) by 100 mass parts polypropylene and 0.2~0.6 part of stearic acid, 0.3~1 part of cumyl peroxide, 0.6~1 part of oxygen
Change and carry out mixing in zinc addition mixer, temperature is 150~200 DEG C.
(4) mixer is added together with the product of step (2) in the product of step (3), in 100~110 DEG C of mixings.
(5) mold is added in the product for obtaining step (4), foams 3~10 minutes at 115~135 DEG C, is warming up to 136~200
DEG C foaming 5~20 minutes.
2. the method according to claim 1, wherein the atomization drying temperature of the step (1) is 130~200
℃。
3. decomposing temperature the method according to claim 1, wherein the foaming agent of the step (2) is AC foaming agent
Degree is 130~140 DEG C.
4. the method according to claim 1, wherein in the step 1 single-layer graphene oxide size be 1~
50 microns.
5. a kind of graphene-expanded polypropylene composite material, which is characterized in that graphene film is overlapped to form porous network and is filled in hair
Among the hole of foaming polypropylene.
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Application publication date: 20190108 |
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