CN105907062A - High-strength low-density natural plant fibre strengthened polycaprolactone composite material and preparation method thereof - Google Patents

High-strength low-density natural plant fibre strengthened polycaprolactone composite material and preparation method thereof Download PDF

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CN105907062A
CN105907062A CN201610305218.7A CN201610305218A CN105907062A CN 105907062 A CN105907062 A CN 105907062A CN 201610305218 A CN201610305218 A CN 201610305218A CN 105907062 A CN105907062 A CN 105907062A
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natural plant
plant fibre
preparation
polycaprolactone
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CN105907062B (en
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李新功
郑霞
卢立
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Central South University of Forestry and Technology
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Central South University of Forestry and Technology
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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
    • C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
    • C08L67/04—Polyesters derived from hydroxycarboxylic acids, e.g. lactones
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L97/00—Compositions of lignin-containing materials
    • C08L97/02—Lignocellulosic material, e.g. wood, straw or bagasse
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/30—Applications used for thermoforming
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
    • C08L2205/16—Fibres; Fibrils

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Wood Science & Technology (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical And Physical Treatments For Wood And The Like (AREA)
  • Laminated Bodies (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention discloses a high-strength low-density natural plant fibre strengthened polycaprolactone composite material. The high-strength low-density natural plant fibre strengthened polycaprolactone composite material is of a multilayer structure which is formed by alternately compounding 2N+1 layers of natural plant fibre layers and N layers of pine needle curtain sub-layers in sequence, wherein N=1, 2, 3 or 4; both the bottommost layer and the topmost layer of the composite material are the natural plant fibre layers. A preparation method of the high-strength low-density natural plant fibre strengthened polycaprolactone composite material comprises the following steps: (1) preparing a natural plant fibre layer; (2) preparing a pine needle curtain sub-layer on the natural plant fibre layer; (3) preparing another natural plant fibre layer on the pine needle curtain sub-layer; (4) repeating the steps (2) and (3) over and over again until a plate blank with a three-layer structure, a five-layer structure, a seven-layer structure or a nine-layer structure is formed; (5) performing hot-press moulding on the plate blank to complete the preparation of the high-strength low-density natural plant fibre strengthened polycaprolactone composite material. According to the composite material disclosed by the invention, the tensile strength reaches 20 MPa or more, the bending strength reaches 40 MPa or more, and meanwhile, the density of the composite material is 1.0 g/cm<3> or less.

Description

High intensity low density natural plant fibre strengthens polycaprolactone composite material and preparation method thereof
Technical field
The invention belongs to wood plastic composite preparation field, particularly relate to a kind of high intensity low density natural plant fibre and strengthen poly-own interior Ester composite and preparation method thereof.
Background technology
Natural plant fibre strengthens polycaprolactone composite material and passes through certain with natural plant fibres such as wood, bamboos with polycaprolactone A kind of wood plastic composite prepared by the methods such as shaping, such material have easily processing, easy-formation, mechanical strength high, water-fast, The advantage such as inexpensive, renewable, is widely used as the field such as indoor and outdoor furniture material, automobile interior material.But, conventional sky So string strengthen polycaprolactone composite material molding mode be first by polyphosphazene polymer caprolactone and natural plant fibre at high temperature or Under Gao Su mixing, mixing thing is through again by method thermoformings such as compression molding, extruded and injection mouldings, in preparation process Polyphosphazene polymer caprolactone there will be a certain degree of thermal degradation because of high-temperature mixing (mixing) and thermoforming, thus affects composite Mechanical strength., limited by forming method meanwhile, composite also is difficult to add the enhancement layer of view picture, being combined of preparation Material bending intensity is low；And owing to briquetting pressure is big (face is pressed in more than 5MPa), the composite density of preparation is (the biggest In 1.2g/cm3), application is by a definite limitation.Therefore, the natural plant fibre developing a kind of high intensity low density strengthens poly-own Lactone composite, to expanding, its application value is great.
Summary of the invention
The technical problem to be solved is, overcomes the deficiency and defect mentioned in background above technology, it is provided that a kind of high-strength Low-density natural plant fibre strengthens polycaprolactone composite material and preparation method thereof.
For solving above-mentioned technical problem, the technical scheme that the present invention proposes is:
A kind of high intensity low density natural plant fibre strengthens polycaprolactone composite material, is by 2N+1 layer natural plant fibre layer and N The sandwich construction that layer pine needle curtain layer is the most alternately compounded to form, wherein N=1,2,3 or 4, the bottom of described composite It is natural plant fibre layer with the superiors.
Above-mentioned composite, it is preferred that the thickness of described natural plants layer is 2-4mm.
Above-mentioned composite, it is preferred that described pine needle curtain layer is crossed through microwave heating treatment.
As a total inventive concept, the present invention also provides for a kind of high intensity low density natural plant fibre enhancing polycaprolactone and is combined The preparation method of material, comprises the following steps:
(1) paraffin wax emulsions is spread upon on billet, then natural plant fibre is uniformly dissipated the steel pad being layered on coated paraffin wax emulsions The thick natural plant fibre layer of 2-4mm is made on plate；
(2) by spray gun, the dimethyl formamide solution of polycaprolactone is uniformly sprayed onto on natural plant fibre layer, is dried, so After pine needle curtain is laid on natural plant fibre layer formation pine needle curtain layer；
(3) natural plant fibre uniformly scattered being layered on pine nut curtain layer is made the thick natural plant fibre layer of 2-4mm, obtain Slab；
(4) billet scribbling paraffin wax emulsions is covered on slab prepared by step (3)；It is then fed in heat pressing forming machines entering Row is hot-forming, completes described low-density natural plant fibre and strengthens the preparation of polycaprolactone composite material.
Above-mentioned preparation method, it is preferred that be additionally included on the natural plant fibre layer after step (3) and step (2) is repeated several times Operate with step (3), until forming five layers, seven layers or the composite slab of nine Rotating fields.
Above-mentioned preparation method, it is preferred that during hot-forming, hot pressing temperature is 100-120 DEG C, and pressing time is 15-30min, Pressure is 1.0-2.0Mpa.
Above-mentioned preparation method, it is preferred that polycaprolactone and dimethyl formyl in the dimethyl formamide solution of described polycaprolactone The mass ratio of amine is 1:4.
Above-mentioned preparation method, it is preferred that the preparation method of described pine needle curtain is: it is 500-700W that pine needle is first sent into power Microwave-oven-heating 1-2min, be seamed into the pine needle curtain of individual layer after cooling, use the PVC suturing with thread management of a diameter of 0.2mm.Use Heating using microwave can destroy its surface wax coat in the case of not destroying pine needle intensity, adds the active group quantity on pine needle surface. After pine needle is microwaved, its surface-active base increases by more than 120%.
Above-mentioned preparation method, it is preferred that in described step (2), the dimethyl formamide solution of polycaprolactone and natural plants Fibrage mass ratio is (30-40): 1；Described dry employing hot blast blows 5-10min, makes dimethylformamide volatilize as early as possible totally.
Above-mentioned preparation method, it is preferred that the particle diameter of described natural plant fibre is 30～60 mesh；Described paraffin wax emulsions spreads upon Coated weight on billet is 2g/m2。
Compared with prior art, it is an advantage of the current invention that:
(1) the high intensity low density natural plant fibre of the present invention strengthens polycaprolactone composite material by selecting the natural of alternating structure Plant fiber layer and pine needle curtain layer, polycaprolactone can uniformly vulcanize to pine needle curtain layer, form good enhancement layer so that The hot strength of this composite reaches more than 20MPa, and bending strength reaches more than 40MPa, and this composite is close simultaneously Degree is at 1.0g/cm3Below.
(2), compared with the preparation method of the present invention and the injection moulding of prior art, the method such as extruded, the present invention can be multiple Condensation material adds pine needle curtain layer, and microwaved its surface-active base rear of pine needle increases by more than 120%, can significantly improve Pine needle and polycaprolactone compatibility, the natural plant fibre of preparation strengthens polycaprolactone composite material under ensureing low-density situation, High intensity can also be obtained.
(3) preparation method of the present invention is not related to high-temperature mixing (mixing) process, can avoid because high-temperature mixing (mixing) carries The polycaprolactone thermal degradation problems come, also reduces preparation energy consumption simultaneously.
(4) preparation process of the present invention need not add coupling agent, i.e. saves energy environmental protection again.
Accompanying drawing explanation
Fig. 1 is the structural representation of the high intensity low density natural plant fibre enhancing polycaprolactone composite material of three-decker of the present invention Figure.
Fig. 2 is the structural representation of the high intensity low density natural plant fibre enhancing polycaprolactone composite material of five-layer structure of the present invention Figure.
Marginal data: 1, natural plant fibre layer；2, pine needle curtain layer.
Detailed description of the invention
For the ease of understanding the present invention, below in conjunction with Figure of description and preferred embodiment, invention herein is done more comprehensively, carefully Cause ground to describe, but protection scope of the present invention is not limited to specific embodiment.
Unless otherwise defined, with those skilled in the art, all technical terms used hereinafter are generally understood that implication is identical.This Technical term used in literary composition is intended merely to describe the purpose of specific embodiment, is not intended to limit the scope of the invention.
Unless otherwise specified, the various raw material used in the present invention, reagent, instrument and equipment etc. all can be purchased by market Can buy or can be prepared by existing method.
Embodiment 1:
A kind of high intensity low density natural wood fiber reinforced polycaprolactone composite of the present invention, structural representation as it is shown in figure 1, The sandwich being the most alternately compounded to form by two-layer natural plant fibre layer 1 (natural wood fibrage) and one layer of pine needle curtain layer 2 Structure, wherein the bottom and the superiors of this composite are natural wood fibrage (thickness is 2mm), and intermediate layer is pine needle Curtain layer.
The preparation method of the high intensity low density natural wood fiber reinforced polycaprolactone composite of the present embodiment, comprises the following steps:
(1) paraffin wax emulsions is spread upon on billet that (paraffin wax emulsions applying amount is 2g/m as anti-adhesion agent2), then by 40 mesh Natural wood fiber uniformly dissipate to be layered on the billet of coated paraffin wax emulsions and make the thick natural wood fibrage of 2mm；
Pine needle is sent into the microwave-oven-heating 2min that power is 500W, with the PVC linear slit Cheng Dan of a diameter of 0.2mm after cooling The pine needle curtain of layer, standby；
(2) by spray gun by the dimethyl formamide solution of the polycaprolactone (matter of polycaprolactone and dimethylformamide in this solution Amount ratio is 1:4) uniformly it is sprayed onto on natural wood fibrage (dimethyl formamide solution of polycaprolactone and natural wood fibrage quality Ratio is 30:1), then use the hair-dryer natural wood fibrage blowing hot-air to the dimethyl formamide solution spraying polycaprolactone 5min, makes dimethylformamide volatilization clean；Then pine needle curtain is laid on natural wood fibrage formation pine needle curtain layer；
(3) again the natural wood fiber of 40 mesh uniformly scattered being layered on pine nut curtain layer is made the thick natural wood fibrage of 2mm, To three-decker slab；
(4) by the billet that scribbles paraffin wax emulsions, (applying amount of paraffin wax emulsions is 2g/m2) cover the slab prepared in step (3) On；Being then fed in heat pressing forming machines carrying out hot-forming, hot pressing temperature is 120 DEG C, and pressing time is 15min, and pressure is 1.0Mpa, completes the preparation of low-density natural wood fiber reinforced polycaprolactone composite.
High intensity low density natural wood fiber reinforced polycaprolactone composite hot strength prepared by the present embodiment reaches 22MPa, curved Qu Qiangdu reaches 45MPa, and density only has 0.90g/cm3。
Embodiment 2:
The high intensity low density natural bamboo fibres of a kind of present invention strengthens polycaprolactone composite material, structural representation as in figure 2 it is shown, The five layers of knot being the most alternately compounded to form by three layers of natural plant fibre layer 1 (natural bamboo fibres layer) and two-layer pine needle curtain layer 2 Structure, wherein the bottom and the superiors of this composite are natural bamboo fibres layer (thickness is 3mm).
The high intensity low density natural bamboo fibres of the present embodiment strengthens the preparation method of polycaprolactone composite material, comprises the following steps:
(1) paraffin wax emulsions is spread upon on billet that (paraffin wax emulsions applying amount is 2g/m as anti-adhesion agent2), then by 50 mesh Natural bamboo fibres uniformly dissipate to be layered on the billet of coated paraffin wax emulsions and make the thick ground floor natural bamboo fibres layer of 3mm；
Pine needle is sent into the microwave-oven-heating 1min that power is 700W, with the PVC linear slit Cheng Dan of a diameter of 0.2mm after cooling The pine needle curtain of layer, standby；
(2) by spray gun by the dimethyl formamide solution of the polycaprolactone (matter of polycaprolactone and dimethylformamide in this solution Amount ratio is 1:4) uniformly it is sprayed onto on natural bamboo fibres layer (dimethyl formamide solution of polycaprolactone and natural bamboo fibres layer quality Ratio is 38:1), then use the hair-dryer natural bamboo fibres layer blowing hot-air to the dimethyl formamide solution spraying polycaprolactone 10min, makes dimethylformamide volatilization clean；Then pine needle curtain is laid on natural bamboo fibres layer formation ground floor pine needle curtain Layer；
(3) natural bamboo fibres of 50 mesh is uniformly dissipated be layered on ground floor pine nut curtain layer that to make the second layer thick for 3mm natural again Bamboo fibre layer；
(4) use the method identical with step (2) that the pine needle curtain handled well is laid in the dimethyl formyl being jetted through polycaprolactone On the second layer natural bamboo fibres layer of amine organic solution, make second layer pine needle curtain layer；
(5) method identical with step (3) is used the natural bamboo fibres of 50 mesh uniformly scattered being layered on pine needle curtain layer to be made The third layer natural bamboo fibres layer that 3mm is thick, i.e. forms the slab of a five-layer structure；
(6) by the billet that scribbles paraffin wax emulsions, (applying amount of paraffin wax emulsions is 2g/m2) cover the slab prepared in step (5) On；Being then fed in heat pressing forming machines carrying out hot-forming, hot pressing temperature is 110 DEG C, and pressing time is 20min, and pressure is 1.5Mpa, completes low-density natural bamboo fibres and strengthens the preparation of polycaprolactone composite material.
High intensity low density natural wood fiber reinforced polycaprolactone composite hot strength prepared by the present embodiment reaches 24MPa, curved Qu Qiangdu reaches 48MPa, and density only has 0.96g/cm3。
Embodiment 3:
A kind of high intensity low density natural straw fiber reinforced polycaprolactone composite of the present invention, structural representation as it is shown in figure 1, The Sanming City being the most alternately compounded to form by two-layer natural plant fibre layer 1 (natural straw fibrage) and one layer of pine needle curtain layer 2 Controlling structure, wherein the bottom and the superiors of this composite are natural straw fibrage (thickness is 2mm), and intermediate layer is Pine needle curtain layer.
The preparation method of the high intensity low density natural straw fiber reinforced polycaprolactone composite of the present embodiment, comprises the following steps:
(1) paraffin wax emulsions is spread upon on billet that (paraffin wax emulsions applying amount is 2g/m as anti-adhesion agent2), then by 60 mesh Natural straw fiber uniformly dissipate to be layered on the billet of coated paraffin wax emulsions and make the thick natural straw fibrage of 2mm；
Pine needle is sent into the microwave-oven-heating 2min that power is 500W, with the PVC linear slit Cheng Dan of a diameter of 0.2mm after cooling The pine needle curtain of layer, standby；
(2) by spray gun by the dimethyl formamide solution of the polycaprolactone (matter of polycaprolactone and dimethylformamide in this solution Amount ratio is 1:4) uniformly it is sprayed onto on natural straw fibrage (dimethyl formamide solution of polycaprolactone and natural straw fibrage Mass ratio is 40:1), then use hair-dryer to blow to the natural straw fibrage of the dimethyl formamide solution spraying polycaprolactone Hot blast 8min, makes dimethylformamide volatilization clean；Then the pine needle curtain handled well is laid on natural straw fibrage formation Pine needle curtain layer；
(3) again the natural straw fiber of 60 mesh uniformly scattered being layered on pine nut curtain layer is made the thick natural straw fibrage of 2mm, Obtain three-decker slab；
(4) by the billet that scribbles paraffin wax emulsions, (applying amount of paraffin wax emulsions is 2g/m2) cover the slab prepared in step (3) On；Being then fed in heat pressing forming machines carrying out hot-forming, hot pressing temperature is 100 DEG C, and pressing time is 25min, and pressure is 2.0Mpa, completes the preparation of low-density natural straw fiber reinforced polycaprolactone composite.
High intensity low density natural wood fiber reinforced polycaprolactone composite hot strength prepared by the present embodiment reaches 26MPa, curved Qu Qiangdu reaches 50MPa, and density only has 0.99g/cm3。

Claims (10)

1. a high intensity low density natural plant fibre strengthens polycaprolactone composite material, it is characterised in that described composite is The sandwich construction being the most alternately compounded to form by 2N+1 layer natural plant fibre layer and N layer pine needle curtain layer, wherein N=1,2, 3 or 4, the bottom of described composite and the superiors are natural plant fibre layer.
2. composite as claimed in claim 1, it is characterised in that the thickness of described natural plants layer is 2-4mm.
3. composite as claimed in claim 1, it is characterised in that described pine needle curtain layer is through microwave heating treatment mistake 's.
4. the preparation method of a high intensity low density natural plant fibre enhancing polycaprolactone composite material, it is characterised in that include Following steps:
(1) paraffin wax emulsions is spread upon on billet, then natural plant fibre is uniformly dissipated the steel pad being layered on coated paraffin wax emulsions The thick natural plant fibre layer of 2-4mm is made on plate；
(2) by spray gun, the dimethyl formamide solution of polycaprolactone is uniformly sprayed onto on natural plant fibre layer, is dried, so After pine needle curtain is laid on natural plant fibre layer formation pine needle curtain layer；
(3) natural plant fibre uniformly scattered being layered on pine nut curtain layer is made the thick natural plant fibre layer of 2-4mm, obtain Slab；
(4) billet scribbling paraffin wax emulsions is covered on slab prepared by step (3)；It is then fed in heat pressing forming machines entering Row is hot-forming, completes described low-density natural plant fibre and strengthens the preparation of polycaprolactone composite material.
5. the preparation method stated such as claim 4, it is characterised in that be additionally included in the natural plant fibre layer after step (3) On be repeated several times step (2) and step (3) operation, until formed five layers, seven layers or the composite slab of nine Rotating fields.
6. the preparation method as described in claim 4 or 5, it is characterised in that during hot-forming, hot pressing temperature is 100-120 DEG C, pressing time is 15-30min, and pressure is 1.0-2.0Mpa.
7. the preparation method as described in claim 4 or 5, it is characterised in that the dimethyl formamide solution of described polycaprolactone Middle polycaprolactone is 1:4 with the mass ratio of dimethylformamide.
8. the preparation method as described in claim 4 or 5, it is characterised in that the preparation method of described pine needle curtain is: first by pine The microwave-oven-heating 1-2min that power is 500-700W sent into by pin, is seamed into the pine needle curtain of individual layer after cooling.
9. the preparation method as described in claim 4 or 5, it is characterised in that in described step (2), the two of polycaprolactone NMF solution and natural plant fibre layer mass ratio are (30-40): 1；Described dry employing hot blast blows 5-10min.
10. the preparation method as described in profit requires 4 or 5, it is characterised in that the particle diameter of described natural plant fibre is 30～60 Mesh；It is 2g/m that described paraffin wax emulsions spreads upon the coated weight on billet2。
CN201610305218.7A 2016-05-10 2016-05-10 High intensity low density natural plant fibre enhancing polycaprolactone composite material and preparation method thereof Expired - Fee Related CN105907062B (en)

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Publication number Priority date Publication date Assignee Title
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