CN104194131A - High-density polyethylene/graphene/polyaniline composite material and synthetic method thereof - Google Patents
High-density polyethylene/graphene/polyaniline composite material and synthetic method thereof Download PDFInfo
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- CN104194131A CN104194131A CN201410475407.XA CN201410475407A CN104194131A CN 104194131 A CN104194131 A CN 104194131A CN 201410475407 A CN201410475407 A CN 201410475407A CN 104194131 A CN104194131 A CN 104194131A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
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Abstract
The invention discloses a high-density polyethylene/graphene/polyaniline composite material and a synthetic method thereof. According to the high-density polyethylene/graphene/polyaniline composite material, the surface of graphene is coated with polyaniline to form a polyaniline/graphene blend, and the polyaniline/graphene blend is dispersed in a high-density polyethylene substrate. As the polyaniline (PANI) coats the graphene (CB) to be blended with the high-density polyethylene (HDPE) substrate, the dispersity of the graphene is improved, the degree of crystallinity of the high-density polyethylene is reduced, therefore, the PTC intensity and the stability of the polyethylene/graphene/polyaniline composite material are improved.
Description
Technical field
The present invention relates to self temperature limiting electrical conducting functional materials and preparation method thereof, particularly a kind of high density polyethylene(HDPE)/grapheme/polyaniline composite material and synthetic method thereof.
Background technology
In recent decades, the research of conductive polymer composite has obtained major progress.Graphene is the major ingredient of conducing composite material, and it directly affects specific conductivity and the switching characteristic of ptc material.It is the novel conducting polymer composite of a class that the conducting particless such as Graphene or metal are dispersed in to the matrix material forming in polymeric matrix.Conducting particles is filled into the electroconductibility that not only can improve matrix material in polymeric matrix, and can improves resistance value in very wide temperature range (room temperature is to the temperature of fusion of body material).High molecular PTC material has broad application prospects at aspects such as current limiter, electromagnetic wave shielding, temp auto-controlled heating and high temperature protections, is a kind of rising new function material.
Due to the specific physical character of Graphene, between Graphene particle autohemagglutination effect large, be difficult to be uniformly dispersed in organic and inorganic and polymeric matrix.And the mechanical property of dosing the polymer composite of Graphene not only depends on the mechanical property of polymer matrix, also relevant with the high molecular interface performance of matrix with Graphene.Therefore, at Graphene surface grafting or to be coated with organic polymer be to address this problem a kind of effective ways.In the last few years, by grafting or coating graphite alkene, had very large development with mechanical property and stable appearance that superpolymer blend improves material again.In the prior art, Low Density Polyethylene (LDPE) performance is improved on the surface that the method by letex polymerization is coated to Graphene by acrylate (ACM).Polyaniline has the features such as structure diversification, resistance to oxidation and good heat resistance.Polyaniline and its derivative not only can obtain by the doping of protonic acid good electroconductibility, and can be by adding oxygenant or reductive agent that the electronic migration in its skeleton is changed, i.e. " redox doping ".After doping, the electric conductivity of Polyaniline and its derivative can improve 10 more than the order of magnitude, and can improve its solvability and processing characteristics in solvent.
In actual use, the less stable of conductive polymer functional composite material PTC behavior.Conventionally adopt the means such as matrix is crosslinked, conducting particles surface treatment, mixture thermal treatment to improve the stability of PTC behavior.But these methods are all relative to the stabilization of PTC effect, rather than absolute.
Summary of the invention
For above-mentioned problems of the prior art, the object of the present invention is to provide a kind of high density polyethylene(HDPE)/grapheme/polyaniline composite material and synthetic method thereof, with polyaniline (PANI) coating graphite alkene (CB) and with the blend of high density polyethylene(HDPE) (HDPE) matrix, improve the dispersiveness of Graphene, reduce the degree of crystallinity of high density polyethylene(HDPE), thereby increase the PTC intensity of polyethylene/graphene/polyaniline composite material and improve its stability.
In order to realize foregoing invention object, the technical solution used in the present invention is as follows:
High density polyethylene(HDPE)/grapheme/polyaniline composite material, wherein, polyaniline-coated, on Graphene surface, form polyaniline/Graphene blend, and polyaniline/Graphene blend is dispersed in high density polyethylene(HDPE) matrix.
Further, wherein the mass ratio of polyaniline and Graphene is 100:2-100:20, and the mass ratio of polyaniline/Graphene blend and high density polyethylene(HDPE) is 1:1-1:8.
Further, wherein the mass ratio of polyaniline and Graphene is 35:1, and the mass ratio of polyaniline/Graphene blend and high density polyethylene(HDPE) is 1:3.
A synthetic method for high density polyethylene(HDPE)/grapheme/polyaniline composite material, comprises following steps:
Step 1: the blend of high density polyethylene(HDPE) and polyaniline/Graphene is placed in to high mixed device and is dry mixed evenly;
Step 2: plastify the formed mixture of step 1 in Banbury mixer;
Step 3: discharging, lower, pelletizing, make sheet material;
Step 4: by sheet material compression moulding on vulcanizing press.
Aforesaid method further comprises the preparation process of graphene/polyaniline blend: the aniline that takes 1.0g joins in hydrochloric acid soln, after ultrasonic dispersion, add a certain amount of Graphene, ultrasonic dispersion also slowly drips quantitative ammonium persulphate hydrochloric acid soln under mechanical stirring, after reaction 3-6h, by deionized water repetitive scrubbing suction filtration for product, to filtrate, be neutral; Filter cake is vacuum-drying 8-20h at 60 ℃, and grinding packs in sealing bag and keeps in Dark Place after sieving, and obtains graphene/polyaniline blend.
Further, in described step 2, banburying temperature is 150-180 ℃, fusion time 8-15 minute.
Further, in described step 2, banburying temperature is 160 ℃, fusion time 10 minutes.
Further, in described step 4, the condition of compression moulding is, preheating 5-10 minute, hot pressing 2-5 minute, pressure 18 megapascal (MPa)s, temperature 150-250 ℃.
Further, in described step 4, the condition of compression moulding is, preheating 8 minutes, hot pressing 3 minutes, pressure 18 megapascal (MPa)s, 200 ℃ of temperature.
Adopt technique scheme, beneficial effect of the present invention has:
1. in the present invention, by processing after Graphene with polyaniline, owing to introducing polar group, in polymkeric substance, can play preferably sterically hindered barrier action, stop reassociating of Graphene particle, segregation degree declines, and has improved the dispersiveness of Graphene.
2. the blend of polyaniline/Graphene is dispersed in high density polyethylene matrix, has effectively destroyed the crystallization of HDPE.
3. after polyaniline is processed, the introducing of polyaniline has destroyed the chain-like structure of Graphene, particle surface is with segment polarity group,-NH group and-polar group of Cl group and CB particle surface easily forms hydrogen bond action, make CB particle surface form stronger physical chemistry bonding force, the interaction between particle and matrix strengthens to some extent.Therefore strengthened the stability of matrix material.
Accompanying drawing explanation
Fig. 1 is the synthetic method schematic diagram of high density polyethylene(HDPE)/grapheme/polyaniline composite material.
Fig. 2 is high density polyethylene(HDPE) when different from graphene/polyaniline blend mass ratio, the comparison diagram of the room temperature resistivity of high density polyethylene(HDPE)/grapheme/polyaniline composite material and Graphene massfraction relation.
Fig. 3 is high density polyethylene(HDPE) when different from graphene/polyaniline blend mass ratio, the scanning electron microscope (SEM) photograph that polyethylene distributes in high density polyethylene(HDPE)/grapheme/polyaniline composite material.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment and accompanying drawing, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
The invention provides a kind of high density polyethylene(HDPE)/grapheme/polyaniline composite material, wherein, polyaniline-coated, on Graphene surface, form polyaniline/Graphene blend, and polyaniline/Graphene blend is dispersed in high density polyethylene(HDPE) matrix.
The present embodiment provides the synthetic method of high density polyethylene(HDPE)/grapheme/polyaniline composite material, as shown in Figure 1, comprises following steps:
Step 1: the blend of high density polyethylene(HDPE) and polyaniline/Graphene is placed in to high mixed device and is dry mixed evenly;
Step 2: plastify the formed mixture of step 1 in Banbury mixer;
Step 3: discharging, lower, pelletizing, make sheet material;
Step 4: by sheet material compression moulding on vulcanizing press.
Wherein, the preparation method of graphene/polyaniline blend is: the aniline that takes 1.0g joins in hydrochloric acid soln, after ultrasonic dispersion, add a certain amount of Graphene, ultrasonic dispersion also slowly drips quantitative ammonium persulphate hydrochloric acid soln under mechanical stirring, after reaction 4h, product is used to deionized water repetitive scrubbing suction filtration, to filtrate, being neutral. filter cake is vacuum-drying 12h at 60 ℃, and grinding packs in sealing bag and keeps in Dark Place after sieving, and obtains graphene/polyaniline blend.
With preferred embodiment, the present invention is further described below.
Embodiment mono-:
Step 1: high density polyethylene(HDPE) and Graphene/polyphenylene copolymerized amine are placed in to high mixed device and are dry mixed evenly, the mass ratio of polyaniline and Graphene is 100:2, and the mass ratio of polyaniline/Graphene blend and high density polyethylene(HDPE) is 1:1;
Step 2: plastify the mixture forming in step 1 in Banbury mixer, banburying temperature is 150 ℃, fusion time 15 minutes;
Step 3: discharging, lower, pelletizing, make sheet material;
Step 4: by sheet material compression moulding on vulcanizing press, the condition of compression moulding is, preheating 5 minutes, hot pressing 5 minutes, pressure 18 megapascal (MPa)s, 250 ℃ of temperature.
Embodiment bis-:
Step 1: high density polyethylene(HDPE) and graphene/polyaniline multipolymer are placed in to high mixed device and are dry mixed evenly, the mass ratio of polyaniline and Graphene is 100:20, and the mass ratio of polyaniline/Graphene blend and high density polyethylene(HDPE) is 1:3;
Step 2: plastify the mixture forming in step 1 in Banbury mixer, banburying temperature is 180 ℃, fusion time 8 minutes;
Step 3: discharging, lower, pelletizing, make sheet material;
Step 4: by sheet material compression moulding on vulcanizing press, the condition of compression moulding is, preheating 10 minutes, hot pressing 2 minutes, pressure 18 megapascal (MPa)s, 150 ℃ of temperature.
Embodiment tri-:
Step 1: high density polyethylene(HDPE) and graphene/polyaniline multipolymer are placed in to high mixed device and are dry mixed evenly, the mass ratio of polyaniline and Graphene is 100:2, and the mass ratio of polyaniline/Graphene blend and high density polyethylene(HDPE) is 1:5;
Step 2: plastify the mixture forming in step 1 in Banbury mixer, banburying temperature is 160 ℃, fusion time 10 minutes;
Step 3: discharging, lower, pelletizing, make sheet material;
Step 4: by sheet material compression moulding on vulcanizing press, the condition of compression moulding is, preheating 8 minutes, hot pressing 3 minutes, pressure 18 megapascal (MPa)s, 200 ℃ of temperature.
Embodiment tetra-:
Step 1: high density polyethylene(HDPE) and graphene/polyaniline multipolymer are placed in to high mixed device and are dry mixed evenly, the mass ratio of polyaniline and Graphene is 35:1, and the mass ratio of polyaniline/Graphene blend and high density polyethylene(HDPE) is 1:1;
Step 2: plastify the mixture forming in step 1 in Banbury mixer, banburying temperature is 150 ℃, fusion time 15 minutes;
Step 3: discharging, lower, pelletizing, make sheet material;
Step 4: by sheet material compression moulding on vulcanizing press, the condition of compression moulding is, preheating 5 minutes, hot pressing 5 minutes, pressure 18 megapascal (MPa)s, 250 ℃ of temperature.
Embodiment five:
Step 1: high density polyethylene(HDPE) and graphene/polyaniline multipolymer are placed in to high mixed device and are dry mixed evenly, the mass ratio of polyaniline and Graphene is 35:1, and the mass ratio of polyaniline/Graphene blend and high density polyethylene(HDPE) is 1:8;
Step 2: plastify the mixture forming in step 1 in Banbury mixer, banburying temperature is 160 ℃, fusion time 10 minutes;
Step 3: discharging, lower, pelletizing, make sheet material;
Step 4: by sheet material compression moulding on vulcanizing press, the condition of compression moulding is, preheating 8 minutes, hot pressing 3 minutes, pressure 18 megapascal (MPa)s, 200 ℃ of temperature.
Embodiment six:
Step 1: high density polyethylene(HDPE) and graphene/polyaniline multipolymer are placed in to high mixed device and are dry mixed evenly, the mass ratio of polyaniline and Graphene is 100:2, and the mass ratio of polyaniline/Graphene blend and high density polyethylene(HDPE) is 1:8;
Step 2: plastify the mixture forming in step 1 in Banbury mixer, banburying temperature is 160 ℃, fusion time 10 minutes;
Step 3: discharging, lower, pelletizing, make sheet material;
Step 4: by sheet material compression moulding on vulcanizing press, the condition of compression moulding is, preheating 8 minutes, hot pressing 3 minutes, pressure 18 megapascal (MPa)s, 200 ℃ of temperature.
Performance test:
Fig. 2 represents room temperature resistivity and the Graphene relation with contents curve of CB, HDPE/CB mixture, ACM/CB mixture and HDPE/PANI/CB mixture.Wherein a represents HDPE/PANI/CB mixture, and b represents HDPE/CB mixture, and c represents ACM/CB mixture, and d represents CB monomer.Can obviously find out that the percolation threshold of HDPE/PANI/CB mixture is much higher than HDPE/CB, this is because the interparticle interaction force of pure Graphene is strong, is easy to agglomeration, and segregation degree is high, and conductive network is easy to form, therefore critical Graphene concentration is lower; Polyaniline is processed after Graphene, owing to introducing polar group, in polymkeric substance, can play preferably sterically hindered barrier action, stoped reassociating of Graphene particle, segregation degree declines, and is difficult for forming conductive path, therefore critical Graphene concentration is higher under low concentration condition.
Fig. 3 is the scanning electron microscope (SEM) photograph of the HDPE/PANI/CB matrix material of PANI/CB mixture different content.As can be seen from the figure, polyaniline/graphene complex can reasonablely be dispersed in HDPE, and when the increase of content surpasses 15Phr, mixture can both be dispersed in the middle of " mesh " substantially equably.This may be that aniline is processed after Graphene, and moistened surface reduces interfacial free energy simultaneously; Owing to introducing polar group, in polymkeric substance, can play preferably sterically hindered barrier action, stoped reassociating of Graphene particle, make particle size distribution even, dispersion effect is very remarkable.
The above embodiment has only expressed embodiments of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (9)
1. high density polyethylene(HDPE)/grapheme/polyaniline composite material, is characterized in that, polyaniline-coated, on Graphene surface, form polyaniline/Graphene blend, and polyaniline/Graphene blend is dispersed in high density polyethylene(HDPE) matrix.
2. high density polyethylene(HDPE)/grapheme/polyaniline composite material according to claim 1, it is characterized in that, wherein the mass ratio of polyaniline and Graphene is 100:2-100:20, and the mass ratio of polyaniline/Graphene blend and high density polyethylene(HDPE) is 1:1-1:8.
3. high density polyethylene(HDPE)/grapheme/polyaniline composite material according to claim 2, is characterized in that, wherein the mass ratio of polyaniline and Graphene is 35:1, and the mass ratio of polyaniline/Graphene blend and high density polyethylene(HDPE) is 1:3.
4. a synthetic method for high density polyethylene(HDPE)/grapheme/polyaniline composite material according to claim 1, is characterized in that, comprises following steps:
Step 1: high density polyethylene(HDPE) and polyaniline/Graphene blend are placed in to high mixed device and are dry mixed evenly;
Step 2: plastify the formed mixture of step 1 in Banbury mixer;
Step 3: discharging, lower, pelletizing, make sheet material;
Step 4: by sheet material compression moulding on vulcanizing press.
5. the synthetic method of high density polyethylene(HDPE)/grapheme/polyaniline composite material according to claim 4, it is characterized in that, the preparation process that further comprises graphene/polyaniline blend: the aniline that takes 1.0g joins in hydrochloric acid soln, after ultrasonic dispersion, add a certain amount of Graphene, ultrasonic dispersion also slowly drips quantitative ammonium persulphate hydrochloric acid soln under mechanical stirring, after reaction 3-6h, by deionized water repetitive scrubbing suction filtration for product, to filtrate, be neutral; Filter cake is vacuum-drying 8-20h at 60 ℃, and grinding packs in sealing bag and keeps in Dark Place after sieving, and obtains graphene/polyaniline blend.
6. the synthetic method of high density polyethylene(HDPE)/grapheme/polyaniline composite material according to claim 4, is characterized in that, in described step 2, banburying temperature is 150-180 ℃, fusion time 8-15 minute.
7. the synthetic method of high density polyethylene(HDPE)/grapheme/polyaniline composite material according to claim 6, is characterized in that, in described step 2, banburying temperature is 160 ℃, fusion time 10 minutes.
8. the synthetic method of high density polyethylene(HDPE)/grapheme/polyaniline composite material according to claim 4, is characterized in that, in described step 4, the condition of compression moulding is, preheating 5-10 minute, hot pressing 2-5 minute, pressure 18 megapascal (MPa)s, temperature 150-250 ℃.
9. the synthetic method of high density polyethylene(HDPE)/grapheme/polyaniline composite material according to claim 8, is characterized in that, in described step 4, the condition of compression moulding is, preheating 8 minutes, hot pressing 3 minutes, pressure 18 megapascal (MPa)s, 200 ℃ of temperature.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104861276A (en) * | 2015-06-16 | 2015-08-26 | 中原工学院 | Method for preparing ethylene-vinyl acetate copolymer/polyaniline/ high density polyethylene (HDPE) composite conductive material |
| CN104910492A (en) * | 2015-06-16 | 2015-09-16 | 中原工学院 | Preparation method of ethylene propylene diene monomer/polyaniline/high density polyethylene composite conducting material |
| CN105960039A (en) * | 2016-06-13 | 2016-09-21 | 安徽和信科技发展有限责任公司 | Flame-retardant polymer automatic-temperature-controlling and heat-tracing cable |
| CN107011568A (en) * | 2017-04-19 | 2017-08-04 | 上海电气集团股份有限公司 | Composite graphite alkene/carbon black is the semi-conducting polymer and preparation method of conducting medium |
| CN113308047A (en) * | 2021-05-31 | 2021-08-27 | 常州优洁包装材料有限公司 | Impact-resistant antistatic sealing barrel and preparation method thereof |
| CN114989527A (en) * | 2022-06-10 | 2022-09-02 | 中化石化销售有限公司 | Graphene heat-conducting master batch and preparation method and application thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104861276A (en) * | 2015-06-16 | 2015-08-26 | 中原工学院 | Method for preparing ethylene-vinyl acetate copolymer/polyaniline/ high density polyethylene (HDPE) composite conductive material |
| CN104910492A (en) * | 2015-06-16 | 2015-09-16 | 中原工学院 | Preparation method of ethylene propylene diene monomer/polyaniline/high density polyethylene composite conducting material |
| CN104861276B (en) * | 2015-06-16 | 2017-11-24 | 中原工学院 | The preparation method of ethylene vinyl acetate copolymer/polyaniline/high density polyethylene (HDPE) composite conducting material |
| CN105960039A (en) * | 2016-06-13 | 2016-09-21 | 安徽和信科技发展有限责任公司 | Flame-retardant polymer automatic-temperature-controlling and heat-tracing cable |
| CN107011568A (en) * | 2017-04-19 | 2017-08-04 | 上海电气集团股份有限公司 | Composite graphite alkene/carbon black is the semi-conducting polymer and preparation method of conducting medium |
| CN107011568B (en) * | 2017-04-19 | 2019-12-20 | 上海电气集团股份有限公司 | Semiconductor polymer with composite graphene/carbon black as conductive medium and preparation method thereof |
| CN113308047A (en) * | 2021-05-31 | 2021-08-27 | 常州优洁包装材料有限公司 | Impact-resistant antistatic sealing barrel and preparation method thereof |
| CN114989527A (en) * | 2022-06-10 | 2022-09-02 | 中化石化销售有限公司 | Graphene heat-conducting master batch and preparation method and application thereof |
| CN114989527B (en) * | 2022-06-10 | 2024-03-29 | 中化石化销售有限公司 | Graphene heat conduction master batch and preparation method and application thereof |
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