CN109096524A - A kind of graphene-foaming polyethylene terephthalate composite material and preparation method - Google Patents
A kind of graphene-foaming polyethylene terephthalate composite material and preparation method Download PDFInfo
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- 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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- 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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- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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Abstract
The invention discloses a kind of graphene-foaming polyethylene terephthalate composite material and preparation methods, it is added in polyethylene terephthalate 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 polyethylene terephthalate, 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 obtain the foaming pet material of porous graphene filling.Graphene is filled in polyethylene terephthalate 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 polyethylene terephthalate are multiple
Condensation material and preparation method thereof.
Background technique
Polyethylene terephthalate is exchanged by dimethyl terephthalate (DMT) with glycol ester or with terephthalic acid (TPA)
Bishydroxyethyl terephthalate is first synthesized with ethylene glycol esterification, polycondensation reaction is then carried out again and is made, it is poly- to be widely used in terylene
Ester fiber, image substrate, polyester bottles, electric components etc. also show that in foamed material field widely answer in recent years
Use prospect.Polyethylene terephthalate is milky or light yellow, highly crystalline polymer, and smooth surface is glossy,
Creep resistance, fatigue durability, rub resistance, dimensional stability are all fine.There is excellent physics in wider temperature range
Mechanical performance, for long-term use temperature 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 alkali resistance are 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 polyethylene terephthalate and other auxiliary agents.In first segment foaming, foaming agent first divides
It solves gas and forms hole in polyethylene terephthalate, and graphene oxide microballoon then stays in these holes.?
After temperature is further promoted, one side foaming agent decomposes completely, promotes hole growth to expand, another aspect graphene oxide sheet table
The oxygen-containing group in face decomposes, so that volume expansion occurs for graphene oxide microballoon, to gradually be filled into poly terephthalic acid second
In the hole of diol ester, supporting network structure is formed, melt strength is improved, prevents cell collapse.Finally make composite material
Mechanical property is obviously improved, and due to the presence of graphene, so that composite foam obtains to a certain extent the stability of light, heat
Promotion.
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 poly terephthalic acid second two
Alcohol ester 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 polyethylene terephthalate 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 polyethylene terephthalates and 0.2~0.6 part of stearic acid, 0.3~1 part of peroxidating two
Isopropylbenzene, 0.6~1 part of 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
~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 the technique of two steps foaming, graphene film is overlapped to form porous network and is filled in foaming poly terephthalic acid second
Among the hole of diol ester.Wherein, primary hole configurations is formed in the first foaming stages, graphene oxide microballoon selectively exists
Among these holes.Make graphene oxide also in the oxygen-containing functional group fast eliminating of the second foaming stages surface of graphene oxide
It originally is graphene, graphene oxide microballoon occurs volume expansion and is full of hole, while foaming agent further decomposes, and forms support
Network structure improves melt 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, foaming poly terephthalic acid second two can not only be promoted
The tensile strength and hardness of alcohol ester, at the same can be promoted its to light, electricity, heat stability.
To sum up, the foaming polyethylene terephthalate obtained using this method not only has in mechanical property excellent
Performance also has broad prospect of application in the multifunctionality such as light, electricity, heat, is suitable for modern multi-functional, mass production, simple and easy
Requirement.
Specific embodiment
Graphene-foaming polyethylene terephthalate 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 polyethylene terephthalates and 0.2~0.6 part of stearic acid, 0.3~1 part
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 step
(3) mixer is added together with the product of step (2) in product, in 100~110 DEG C of mixings.(5) production for obtaining step (4)
Mold is added in object, foams 3~10 minutes at 110~135 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 polyethylene terephthalates and 0.2 part of stearic acid, 0.3 part of cumyl peroxide,
0.6 part of zinc oxide, which is added in mixer, carries out mixing, and 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 20
Minute.
Through above step, graphene-foaming polyethylene terephthalate composite material, specific performance such as table 1 are obtained
It is shown.
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 155 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 polyethylene terephthalates and 0.3 part of stearic acid, 0.5 part of cumyl peroxide,
0.7 part of zinc oxide, which is added in mixer, carries out mixing, and 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 5 minutes at 125 DEG C, is warming up to 160 DEG C and foams 10 points
Clock.
Through above step, graphene-foaming polyethylene terephthalate composite material, specific performance such as table 1 are obtained
It is shown.
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 polyethylene terephthalates and 0.6 part of stearic acid, 1.0 parts of cumyl peroxides,
1.0 parts of zinc oxide, which are added in mixer, carries out mixing, and 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 3 minutes at 135 DEG C, is warming up to 175 DEG C and foams 10 points
Clock.
Through above step, graphene-foaming polyethylene terephthalate composite material, specific performance such as table 1 are obtained
It is shown.
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 polyethylene terephthalates and 0.4 part of stearic acid, 0.7 part of cumyl peroxide,
0.8 part of zinc oxide, which is added in mixer, carries out mixing, and 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 7 minutes at 130 DEG C, is warming up to 195 DEG C and foams 8 points
Clock.
Through above step, graphene-foaming polyethylene terephthalate composite material, specific performance such as table 1 are obtained
It is shown.
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 polyethylene terephthalates and 0.5 part of stearic acid, 0.9 part of cumyl peroxide,
0.9 part of zinc oxide, which is added in mixer, carries out mixing, and 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-foaming polyethylene terephthalate composite material, specific performance such as table 1 are obtained
It is shown.
Comparative example 1: graphene oxide microballoon preparation foaming polyethylene terephthalate 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 polyethylene terephthalates and 0.3 part of stearic acid, 0.5 part of cumyl peroxide,
0.7 part of zinc oxide, which is added in mixer, carries out mixing, and 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 polyethylene terephthalates and 0.3 part of stearic acid, 0.5 part of cumyl peroxide,
0.7 part of zinc oxide, which is added in mixer, carries out mixing, and temperature is 15 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 polyethylene terephthalates and 0.3 part of stearic acid, 0.5 part of cumyl peroxide,
0.7 part of zinc oxide, which is added in mixer, carries out mixing, and 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 15 points
Clock
Through above step, graphene-foaming polyethylene terephthalate composite material, specific performance such as table 1 are obtained
It is shown.
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 polyethylene terephthalates and 0.3 part of stearic acid, 0.5 part of cumyl peroxide,
0.7 part of zinc oxide, which is added in mixer, carries out mixing, and 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 20 minutes at 180 DEG C.
Through above step, graphene-foaming polyethylene terephthalate composite material, specific performance such as table 1 are obtained
It is shown.
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 polyethylene terephthalate in very little range.When lamella size is too small, graphene film can not have
Effect plays reinforcing effect (comparative example 2), and it is oversized when, the contact area between graphene oxide sheet increases, and causes to aoxidize stone
Attraction between black alkene piece increases, and can not effectively expand in a heated state, and final product is still that spherical graphite alkene particle exists
Among hole, reinforcing effect (comparative example 3) is not had.
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 ethylene glycol terephthalate matrix, can not effectively expand, thus while foaming agent itself can effective shape
At hole, the expansion effect of graphene oxide is bad, and material overall performance and pure foaming polyethylene terephthalate are close.
Claims (5)
1. a kind of graphene-foaming polyethylene terephthalate preparation method, which comprises 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 polyethylene terephthalates and 0.2~0.6 part of stearic acid, 0.3~1 part of peroxidating diisopropyl
Benzene, 0.6~1 part of 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 136~200
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-foaming polyethylene terephthalate composite material, which is characterized in that graphene film is overlapped to form more
Pore network is filled among the hole of foaming polyethylene terephthalate.
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| CN112574536A (en) * | 2020-12-10 | 2021-03-30 | 广东金榜塑料包装有限公司 | Preparation method of CPET sheet for blending modified high-temperature-resistant oven |
| CN116874894A (en) * | 2023-07-10 | 2023-10-13 | 昆山力普电子橡胶有限公司 | Automobile rubber shock pad and preparation method thereof |
| CN116874894B (en) * | 2023-07-10 | 2024-02-09 | 昆山力普电子橡胶有限公司 | Automobile rubber shock pad and preparation method thereof |
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Application publication date: 20181228 |