CN109306160A - Polylactic acid graphene composite material and preparation method thereof - Google Patents

Polylactic acid graphene composite material and preparation method thereof Download PDF

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Publication number
CN109306160A
CN109306160A CN201710632763.1A CN201710632763A CN109306160A CN 109306160 A CN109306160 A CN 109306160A CN 201710632763 A CN201710632763 A CN 201710632763A CN 109306160 A CN109306160 A CN 109306160A
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China
Prior art keywords
polylactic acid
graphene
composite material
solution
preparation
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CN201710632763.1A
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Chinese (zh)
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陈伟
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Zhangjiagang City Fook New Mstar Technology Ltd
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Zhangjiagang City Fook New Mstar Technology Ltd
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Priority to CN201710632763.1A priority Critical patent/CN109306160A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/018Additives for biodegradable polymeric composition

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

This application discloses a kind of preparation methods of polylactic acid graphene composite material, comprising: (1), prepares graphene solution;(2), PLA solution is prepared;(3), above-mentioned PLA solution and graphene solution are mixed according to mass ratio for 50~200:1, stir 30~40min, obtain mixture, mixture is added dropwise in 10~15 times of ethylene glycol solution, centrifuge separation, sediment is collected, dry 10~12h under the conditions of 70~80 DEG C obtains composite material.Graphene in polylactic acid graphene composite material of the present invention can be preferably dispersed in polylactic acid matrix, by the thermal stability that graphene addition can be significantly improved to composite material in polylactic acid matrix.

Description

Polylactic acid graphene composite material and preparation method thereof
Technical field
The present invention relates to field of material technology, more particularly to a kind of polylactic acid graphene composite material and its preparation side Method.
Background technique
Polylactic acid is a kind of biodegradable polymers obtained by lactic acid condensation or lactide ring-opening polymerisation, in addition to tool Outside having the advantages that raw material sources are extensive and renewable, production process is pollution-free, polylactic acid has good biocompatibility, gloss Degree and the transparency, also have certain fungus resistance, anti-flammability and ultraviolet-resistent property, are widely used as packaging material, medical material, fibre Dimension, non-woven fabric etc. are applied to the fields such as clothes, papermaking, building, biomedicine.But the brittleness of polylactic acid is larger, notch punching Hit intensity is less than 3kJ/m2;Its heat resistance is also poor, and heat distortion temperature is only 60 DEG C or so, the two disadvantages limit poly- cream Application of the acid in terms of structural timber.
In order to expand the application range of polylactic acid, prior art discloses the sides of a variety of performances for improving poly-lactic acid material Method, wherein the method for improving its heat resistance mainly includes carrying out annealing to polylactic acid to improve its crystallinity, utilizes fiber It is enhanced or makes poly-lactic acid material crosslinking etc., the method for its toughness is improved mainly by the rubber of polylactic acid and high tenacity Glue is elastomer blended.But the heat resistance of the composite material is still poor, and its intensity and rigidity have it is a degree of Loss.
For this reason, it is necessary in view of the above-mentioned problems, propose a kind of polylactic acid graphene composite material and preparation method thereof, energy Enough solve the problems, such as that polylactic acid exists in the prior art.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of polylactic acid graphene composite material, to overcome the prior art In deficiency.
To achieve the above object, the invention provides the following technical scheme:
The present invention discloses a kind of preparation method of polylactic acid graphene composite material, comprising:
(1), graphene solution is prepared;
(2), PLA solution is prepared;
(3), above-mentioned PLA solution and graphene solution are mixed according to mass ratio for 50~200:1, stirring 30~ 40min obtains mixture, mixture is added dropwise in 10~15 times of ethylene glycol solution, is centrifugated, collection sediment, and 70 Dry 10~12h, obtains composite material under the conditions of~80 DEG C.
Preferably, in step (1), the preparation method of graphene solution include: by graphene dispersion in organic solvent A, 1~3h of ultrasound under the conditions of 20~25 DEG C obtains the graphene solution that mass concentration is 0.1~0.2mg/mL.
Preferably, in step (2), the preparation method of PLA solution includes: that polylactic acid is dissolved in organic solvent A, 20~30min is stirred, the PLA solution that mass concentration is 10~20mg/mL is obtained.
Preferably, the organic solvent A is one of tetrahydrofuran or chloroform.
Technical solution of the present invention also provides a kind of polylactic acid graphene composite wood obtained according to above-mentioned preparation method Material.
Compared with the prior art, the advantages of the present invention are as follows: the graphene in polylactic acid graphene composite material of the present invention It can preferably be dispersed in polylactic acid matrix, by the way that graphene addition can be significantly improved composite wood in polylactic acid matrix The thermal stability of material.
Specific embodiment
The present invention is described further by the following example: according to following embodiments, the present invention may be better understood. However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described in embodiment are only used In illustrating the present invention, without the present invention described in detail in claims should will not be limited.
Embodiment 1
By graphene dispersion in tetrahydrofuran or chloroform solvent, 1~3h of ultrasound under the conditions of 20~25 DEG C is obtained Mass concentration is the graphene solution of 0.1mg/mL.
Polylactic acid is dissolved in tetrahydrofuran or chloroform solvent, 20~30min is stirred, obtaining mass concentration is The PLA solution of 20mg/mL.
Above-mentioned PLA solution and graphene solution are mixed according to mass ratio for 200:1,30~40min is stirred, obtains Mixture is added dropwise in 10~15 times of ethylene glycol solution by mixture, centrifuge separation, is collected sediment, is done under the conditions of 75 DEG C Dry 11h obtains composite material.
Embodiment 2
By graphene dispersion in tetrahydrofuran or chloroform solvent, 1~3h of ultrasound under the conditions of 20~25 DEG C is obtained Mass concentration is the graphene solution of 0.2mg/mL.
Polylactic acid is dissolved in tetrahydrofuran or chloroform solvent, 20~30min is stirred, obtaining mass concentration is The PLA solution of 10mg/mL.
Above-mentioned PLA solution and graphene solution are mixed according to mass ratio for 50:1,30~40min is stirred, is mixed Object is closed, mixture is added dropwise in 10~15 times of ethylene glycol solution, is centrifugated, sediment, drying under the conditions of 70 DEG C are collected 10h obtains composite material.
Embodiment 3
By graphene dispersion in tetrahydrofuran or chloroform solvent, 1~3h of ultrasound under the conditions of 20~25 DEG C is obtained Mass concentration is the graphene solution of 0.15mg/mL.
Polylactic acid is dissolved in tetrahydrofuran or chloroform solvent, 20~30min is stirred, obtaining mass concentration is The PLA solution of 15mg/mL.
Above-mentioned PLA solution and graphene solution are mixed according to mass ratio for 100:1,30~40min is stirred, obtains Mixture is added dropwise in 10~15 times of ethylene glycol solution by mixture, centrifuge separation, is collected sediment, is done under the conditions of 80 DEG C Dry 12h obtains composite material.
Technical solution of the present invention also provides a kind of polylactic acid graphene composite wood obtained according to above-mentioned preparation method Material.In the polylactic acid graphene composite material that preparation method of the invention obtains, graphene can preferably be dispersed in polylactic acid In matrix, by the thermal stability that graphene addition can be significantly improved to composite material in polylactic acid matrix.
In order to preferably embody the thermal stability of polylactic acid graphene composite material in the present invention, below with reference to specific reality Data are tested to be illustrated.
5~10mg sample is weighed, N is tested with the heating rate of 10 DEG C/min2Polylactic acid and polylactic acid graphene under atmosphere Thermal stability, N2Flow is 50mL/min.Test result is as follows table:
Sample T5(℃) T50(℃)
Polylactic acid 239.0 271.8
Polylactic acid graphene composite material 261.8 284.6
Wherein, T5Temperature when for polylactic acid mass loss 5%, T50Temperature when for polylactic acid mass loss 50%.By Result in upper table it is found that polylactic acid graphene composite material T5Value is 261.8 DEG C, improves 22.8 DEG C than pure polylactic acid;It is poly- The T of lactic acid graphene composite material50Value is 284.6 DEG C, improves 12.8 DEG C than pure polylactic acid.Thus, it is indicated, that of the invention In technical solution, the thermal stability of poly-lactic acid material is can be improved in addition graphene, and the addition of graphene delays poly- significantly The thermal decomposition temperature of lactic acid matrix the reason of mainly there are two aspects: one be graphene nano lamella shielding action, it is another A is the diffusion for hindering volatile decomposition products.
Finally, it is to be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive Property include so that include a series of elements process, method, article or equipment not only include those elements, but also Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic Element.

Claims (5)

1. a kind of preparation method of polylactic acid graphene composite material characterized by comprising
(1), graphene solution is prepared;
(2), PLA solution is prepared;
(3), above-mentioned PLA solution and graphene solution are mixed according to mass ratio for 50~200:1, stir 30~40min, Mixture is obtained, mixture is added dropwise in 10~15 times of ethylene glycol solution, is centrifugated, collection sediment, 70~80 DEG C Under the conditions of dry 10~12h, obtain composite material.
2. the preparation method of polylactic acid graphene composite material according to claim 1, it is characterised in that: in step (1), The preparation method of graphene solution includes: 1~3h of ultrasound under the conditions of 20~25 DEG C by graphene dispersion in organic solvent A, Obtain the graphene solution that mass concentration is 0.1~0.2mg/mL.
3. the preparation method of polylactic acid graphene composite material according to claim 1, it is characterised in that: in step (2), The preparation method of PLA solution includes: that polylactic acid is dissolved in organic solvent A, stirs 20~30min, obtains mass concentration For the PLA solution of 10~20mg/mL.
4. the preparation method of polylactic acid graphene composite material according to claim 2 or 3, it is characterised in that: described to have Solvent A is one of tetrahydrofuran or chloroform.
5. a kind of polylactic acid graphene composite material that preparation method according to claim 1 obtains.
CN201710632763.1A 2017-07-28 2017-07-28 Polylactic acid graphene composite material and preparation method thereof Pending CN109306160A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710632763.1A CN109306160A (en) 2017-07-28 2017-07-28 Polylactic acid graphene composite material and preparation method thereof

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Application Number Priority Date Filing Date Title
CN201710632763.1A CN109306160A (en) 2017-07-28 2017-07-28 Polylactic acid graphene composite material and preparation method thereof

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110922729A (en) * 2019-12-12 2020-03-27 安徽丰原乳酸聚酯材料有限公司 Heat-resistant polylactic acid material and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110922729A (en) * 2019-12-12 2020-03-27 安徽丰原乳酸聚酯材料有限公司 Heat-resistant polylactic acid material and preparation method thereof

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