CN108841152A - A kind of graphene-foaming lactic acid composite material and preparation method thereof - Google Patents
A kind of graphene-foaming lactic acid composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of graphene-foaming lactic acid composite materials and preparation method thereof, it is added in polylactic acid 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 polylactic acid, 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 foaming poly-lactic acid material of porous graphene filling.Graphene is filled in polylactic acid hole, plays the role of support, greatly enhances the intensity and elasticity of foamed material, and can improve the corona-resistance property of material, obtains differentiation foamed material.This method is simple and easy, and the addition of graphene oxide without influence, can assign material new function original preparation process after promoting material foundation performance, has broad prospect of application.
Description
Technical field
The invention belongs to field of compound material more particularly to a kind of graphene-foaming lactic acid composite material and its preparations
Method.
Background technique
Polylactic acid is to be exchanged with glycol ester by dimethyl terephthalate (DMT) or be esterified first with terephthalic acid (TPA) and ethylene glycol
Bishydroxyethyl terephthalate is synthesized, polycondensation reaction is then carried out again and is made, be widely used in dacron polyester fiber, image base
Piece, polyester bottles, electric components etc. also show that broad application prospect in foamed material field in recent years.Polylactic acid
It is milky or light yellow, highly crystalline polymer, smooth surface is glossy, creep resistance, fatigue durability, rub resistance,
Dimensional stability is all fine.There is excellent physical mechanical property in wider temperature range, long-term use temperature is up to 120
DEG C, electrical insulating property is excellent, or even under high-temperature high-frequency, electrical property is still preferable, but corona resistance is poor, hot water resistance and resistance to
Alkalinity is also poor, thus will have a direct impact on the service life of product.
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 polylactic acid and other auxiliary agents.In first segment foaming, foaming agent first decomposites gas in poly- cream
Hole is formed in acid, 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 the hole of polylactic acid, 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-foaming lactic acid 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-foaming lactic acid composite material, includes 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 polylactic acid 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 110~135 DEG C, is warming up to 136
~190 DEG C are foamed 5~15 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 foaming polylactic acid 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 foaming polylactic acid can not only be promoted
And hardness, while can be promoted its to light, electricity, heat stability.
To sum up, the foaming polylactic acid 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-foaming lactic acid 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 polylactic acid 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), 110
It foams 3~10 minutes at~135 DEG C, is warming up to 135~190 DEG C and foams 5~15 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 polylactic acid 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 110 DEG C, is warming up to 136 DEG C of foaming 15
Minute.
Through above step, graphene-foaming lactic acid 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 135 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 polylactic acid 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 8 minutes at 125 DEG C, is warming up to 150 DEG C and foams 15 points
Clock.
Through above step, graphene-foaming lactic acid 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 140 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 polylactic acid and 0.6 part of stearic acid, 0.6 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 7 minutes at 130 DEG C, is warming up to 175 DEG C and foams 12 points
Clock.
Through above step, graphene-foaming lactic acid 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 polylactic acid 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 8 minutes at 130 DEG C, is warming up to 185 DEG C and foams 7 points
Clock.
Through above step, graphene-foaming lactic acid 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 180 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 polylactic acid 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 190 DEG C and foams 5 points
Clock.
Through above step, graphene-foaming lactic acid composite material is obtained, specific performance is as shown in table 1.
Comparative example 1：Graphene oxide microballoon preparation foaming polylactic acid is not added.
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 polylactic acid 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 polylactic acid 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 polylactic acid 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-foaming lactic acid 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 polylactic acid 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-foaming lactic acid 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 foaming polylactic acid 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 lactic acid 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 foaming polylactic acid are close.
Claims (5)
1. a kind of graphene-foaming polylactic acid preparation method, which is characterized in that include the following steps：
(1) by atomization drying method that single-layer graphene oxide dispersion liquid is dry, graphene oxide microballoon is obtained, carbon-to-oxygen ratio is
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 polylactic acid 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 110~135 DEG C, is warming up to 136~190
DEG C foaming 5~15 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-foaming lactic acid composite material, which is characterized in that graphene film is overlapped to form porous network and is filled in hair
Among the hole for steeping polylactic acid.
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| WO2010089241A1 (en) * | 2009-02-04 | 2010-08-12 | Basf Se | Black, uv-stable thermoplastic moulding compounds |
| CN107513162A (en) * | 2017-08-21 | 2017-12-26 | 杭州高烯科技有限公司 | A kind of preparation method of graphene/nylon 6 nano-composite |
| CN107603179A (en) * | 2017-10-26 | 2018-01-19 | 山东圣泉新材料股份有限公司 | Polylactic acid foam material that a kind of graphene is modified and its preparation method and application |
| CN108164939A (en) * | 2017-12-30 | 2018-06-15 | 杭州高烯科技有限公司 | A kind of preparation method of the heat-resisting degradable graphene-poly butylene succinate composite foam material of high resiliency |
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