CN105907062B - High intensity low density natural plant fibre enhancing polycaprolactone composite material and preparation method thereof - Google Patents
High intensity low density natural plant fibre enhancing polycaprolactone composite material and preparation method thereof Download PDFInfo
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- CN105907062B CN105907062B CN201610305218.7A CN201610305218A CN105907062B CN 105907062 B CN105907062 B CN 105907062B CN 201610305218 A CN201610305218 A CN 201610305218A CN 105907062 B CN105907062 B CN 105907062B
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- C—CHEMISTRY; METALLURGY
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- 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
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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
- C08L97/00—Compositions of lignin-containing materials
- C08L97/02—Lignocellulosic material, e.g. wood, straw or bagasse
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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
- C08L2203/00—Applications
- C08L2203/30—Applications used for thermoforming
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- 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
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- C—CHEMISTRY; METALLURGY
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- 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
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
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Abstract
The invention discloses a kind of high intensity low density natural plant fibre to strengthen polycaprolactone composite material, the sandwich construction being alternately compounded to form successively by 2N+1 layer natural plant fibre layers and N layer pine needle curtains layer, N=1,2,3 or 4, the bottom of the composite and the superiors are natural plant fibre layer.The preparation method of the present invention, including：(1) natural plant fibre layer is prepared, (2) pine needle curtain layer is prepared in natural fiber layer, (3) natural plant fibre layer is prepared on pine needle curtain layer, (4) (2) and (3) are repeated several times, until forming the slab of three layers, five layers, seven layers or nine Rotating fields；(5) it is slab is hot-forming, complete the preparation of the low-density natural plant fibre enhancing polycaprolactone composite material.Its tensile strength of the composite of the present invention reaches more than 20MPa, and bending strength reaches more than 40MPa, while the density of the composite is in 1.0g/cm3Below.
Description
Technical field
The invention belongs to wood plastic composite preparation field, more particularly to a kind of high intensity low density natural plant fibre to strengthen
Polycaprolactone composite material and preparation method thereof.
Background technology
Natural plant fibre enhancing polycaprolactone composite material is passed through with the natural plant fibres such as wood, bamboo and polycaprolactone
A kind of wood plastic composite prepared by the methods of certain shaping, such material have easy processing, easy-formation, mechanical strength it is high,
The advantages that water-fast, inexpensive, renewable, it is widely used as the fields such as indoor and outdoor furniture material, automobile interior material.It is but conventional
Natural plant fibre enhancing polycaprolactone composite material molding mode be first by polyphosphazene polymer caprolactone and natural plant fibre
It is kneaded under high temperature or high speed, mixture through passing through thermoforming the methods of compression molding, extrusion forming and injection moulding, system again
A certain degree of thermal degradation occurs because of high-temperature mixing (mixing) and thermoforming in polyphosphazene polymer caprolactone during standby, so as to influence
The mechanical strength of composite.Meanwhile limited by forming method, it also is difficult to add the enhancement layer of view picture, system in composite
Standby composite bending strength is low；And because briquetting pressure is big (face pressure is in more than 5MPa), the composite density of preparation is big
(it is typically larger than 1.2g/cm3), application field is by a definite limitation.Therefore, a kind of natural plant fibre of high intensity low density is developed
Strengthen polycaprolactone composite material, it is great to expanding its application value.
The content of the invention
The technical problems to be solved by the invention are to overcome the shortcomings of to mention in background above technology and defect, there is provided one
Kind high intensity low density natural plant fibre enhancing polycaprolactone composite material and preparation method thereof.
In order to solve the above technical problems, technical scheme proposed by the present invention is：
A kind of high intensity low density natural plant fibre strengthens polycaprolactone composite material, is by 2N+1 layer natural plant fibres
The sandwich construction that layer and N layer pine needle curtains layer are alternately compounded to form successively, wherein N=1,2,3 or 4, the composite is most
Bottom and the superiors are natural plant fibre layer.
Above-mentioned composite, it is preferred that the thickness of the natural plants layer is 2-4mm.
Above-mentioned composite, it is preferred that the pine needle curtain layer is crossed by microwave heating treatment.
The inventive concept total as one, the present invention also provide a kind of high intensity low density natural plant fibre enhancing and gathered in oneself
The preparation method of ester composite, comprises the following steps：
(1) paraffin wax emulsions are applied on billet, then natural plant fibre is uniformly dissipated and is layered on coated paraffin wax emulsions
Billet on the thick natural plant fibre layers of 2-4mm are made；
(2) dimethyl formamide solution of polycaprolactone is uniformly sprayed onto on natural plant fibre layer by spray gun, done
It is dry, then pine needle curtain is laid on natural plant fibre layer and forms pine needle curtain layer；
(3) natural plant fibre is uniformly dissipated to be layered on and the thick natural plant fibre layers of 2-4mm is made on pine nut curtain layer, obtained
To slab；
(4) billet for scribbling paraffin wax emulsions is covered on the slab prepared in step (3)；It is then fed into heat pressing forming machines
Carry out hot-forming, complete the preparation of low-density natural plant fibre enhancing 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 is repeated several times
(2) operated with step (3), until forming the composite slab of five layers, seven layers or 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 1.0-2.0Mpa.
Above-mentioned preparation method, it is preferred that polycaprolactone and diformazan in the dimethyl formamide solution of the polycaprolactone
The mass ratio of base formamide is 1:4.
Above-mentioned preparation method, it is preferred that the preparation method of the pine needle curtain is：It is first 500- by pine needle feeding power
700W microwave stove heat 1-2min, the pine needle curtain of individual layer is seamed into after cooling, is closed using a diameter of 0.2mm PVC linear slits.Using
Microwave heating can destroy its surface wax coat in the case where not destroying pine needle intensity, add the active radix on pine needle surface
Amount.Its surface-active base increase by more than 120% after pine needle is microwaved.
Above-mentioned preparation method, it is preferred that in the step (2), the dimethyl formamide solution of polycaprolactone with it is natural
Plant fiber layer mass ratio is (30-40):1；The drying blows 5-10min using hot blast, dimethylformamide is volatilized as early as possible
Totally.
Above-mentioned preparation method, it is preferred that the particle diameter of the natural plant fibre is 30~60 mesh；The paraffin wax emulsions apply
The coated weight being put on billet is 2g/m2。
Compared with prior art, the advantage of the invention is that：
(1) high intensity low density natural plant fibre of the invention strengthens polycaprolactone composite material by selecting alternating structure
Natural plant fibre layer and pine needle curtain layer, polycaprolactone can uniformly vulcanize to pine needle curtain layer, form enhancing well
Layer so that the tensile strength of the composite reaches more than 20MPa, and bending strength reaches more than 40MPa, while the composite
Density in 1.0g/cm3Below.
(2) preparation method of the invention is compared with the methods of injection moulding, extrusion forming of prior art, and the present invention can be with
Pine needle curtain layer is added in the composite, and its microwaved rear surface-active base of pine needle increases by more than 120%, Ke Yixian
Writing improves pine needle and polycaprolactone compatibility, and the natural plant fibre enhancing polycaprolactone composite material of preparation is ensureing low-density
Situation under, high intensity can also be obtained.
(3) preparation method of the invention is not related to high-temperature mixing (mixing) process, can avoid because of high-temperature mixing (mixing)
The polycaprolactone thermal degradation problems brought, while also reduce preparation energy consumption.
(4) preparation process of the invention need not add coupling agent, that is, save energy environmental protection again.
Brief description of the drawings
Fig. 1 is the structure of the high intensity low density natural plant fibre enhancing polycaprolactone composite material of three-decker of the present invention
Schematic diagram.
Fig. 2 is the structure of the high intensity low density natural plant fibre enhancing polycaprolactone composite material of five-layer structure of the present invention
Schematic diagram.
Marginal data：1st, natural plant fibre layer；2nd, pine needle curtain layer.
Embodiment
For the ease of understanding the present invention, below in conjunction with Figure of description and preferred embodiment to invent herein do it is more complete
Face, meticulously describe, but protection scope of the present invention is not limited to specific embodiment.
Unless otherwise defined, all technical terms used hereinafter are generally understood that implication phase with those skilled in the art
Together.Technical term used herein is intended merely to describe the purpose of specific embodiment, is not intended to the limitation present invention's
Protection domain.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1：
A kind of high intensity low density natural wood fiber reinforced polycaprolactone composite of the invention, structural representation such as Fig. 1
Shown, being alternately compounded to form successively by two layers of natural plant fibre layer 1 (natural wood fibrous layer) and one layer of pine needle curtain layer 2 three
The bottom of Mingzhi's structure, the wherein composite and the superiors are natural wood fibrous layer (thickness 2mm), and intermediate layer is pine
Pin curtain sublayer.
The preparation method of the high intensity low density natural wood fiber reinforced polycaprolactone composite of the present embodiment, including it is following
Step：
(1) it is applied on billet that (paraffin wax emulsions applying amount is 2g/m using paraffin wax emulsions as anti-adhesion agent2), then by 40
The natural wood-fibred of purpose, which uniformly dissipates to be layered on, is made the thick natural wood fibrous layers of 2mm on the billet of coated paraffin wax emulsions；
Pine needle is sent into the microwave stove heat 2min that power is 500W, with a diameter of 0.2mm PVC linear slits Cheng Dan after cooling
The pine needle curtain of layer, it is standby；
(2) by spray gun by the dimethyl formamide solution of polycaprolactone (polycaprolactone and dimethyl formyl in the solution
The mass ratio of amine is 1:4) (dimethyl formamide solution of polycaprolactone and natural wood fibre are uniformly sprayed onto on natural wood fibrous layer
It is 30 to tie up layer mass ratio:1) natural wood, then using hair-dryer to the dimethyl formamide solution for spraying polycaprolactone is fine
Layer blowing hot-air 5min is tieed up, makes dimethylformamide volatilization clean；Then pine needle curtain is laid on natural wood fibrous layer and forms pine
Pin curtain sublayer；
(3) again the natural wood-fibred of 40 purposes is uniformly dissipated to be layered on and the thick natural wood fibrous layers of 2mm is made on pine nut curtain layer,
Obtain three-decker slab；
(4) by the billet for scribbling paraffin wax emulsions, (applying amount of paraffin wax emulsions is 2g/m2) cover the plate prepared in step (3)
On base；It is then fed into heat pressing forming machines and carries out hot-forming, hot pressing temperature is 120 DEG C, pressing time 15min, and pressure is
1.0Mpa, complete the preparation of low-density natural wood fiber reinforced polycaprolactone composite.
High intensity low density natural wood fiber reinforced polycaprolactone composite tensile strength manufactured in the present embodiment reaches
22MPa, bending strength reach 45MPa, and density only has 0.90g/cm3。
Embodiment 2：
A kind of high intensity low density natural bamboo fibres enhancing polycaprolactone composite material of the invention, structural representation such as Fig. 2
Shown, being alternately compounded to form successively by three layers of natural plant fibre layer 1 (natural bamboo fibres layer) and two layers of pine needle curtain layer 2 five
The bottom of Rotating fields, the wherein composite and the superiors are natural bamboo fibres layer (thickness 3mm).
The preparation method of the high intensity low density natural bamboo fibres enhancing polycaprolactone composite material of the present embodiment, including it is following
Step：
(1) it is applied on billet that (paraffin wax emulsions applying amount is 2g/m using paraffin wax emulsions as anti-adhesion agent2), then by 50
Purpose natural bamboo fibres, which uniformly dissipate to be layered on, is made the thick first layer natural bamboo fibres layers of 3mm on the billet of coated paraffin wax emulsions；
Pine needle is sent into the microwave stove heat 1min that power is 700W, with a diameter of 0.2mm PVC linear slits Cheng Dan after cooling
The pine needle curtain of layer, it is standby；
(2) by spray gun by the dimethyl formamide solution of polycaprolactone (polycaprolactone and dimethyl formyl in the solution
The mass ratio of amine is 1:4) (dimethyl formamide solution of polycaprolactone and natural bamboo fibre are uniformly sprayed onto on natural bamboo fibres layer
It is 38 to tie up layer mass ratio:1) the natural bamboo, then using hair-dryer to the dimethyl formamide solution for spraying polycaprolactone is fine
Layer blowing hot-air 10min is tieed up, makes dimethylformamide volatilization clean；Then pine needle curtain is laid on natural bamboo fibres layer and forms
One layer of pine needle curtain layer；
(3) again the natural bamboo fibres of 50 mesh are uniformly dissipated to be layered on and the thick second layers of 3mm is made on first layer pine nut curtain layer
Natural bamboo fibres layer；
(4) dimethyl for being jetted through polycaprolactone using the pine needle curtain handled well is laid in step (2) identical method
On the second layer natural bamboo fibres layer of formamide organic solution, second layer pine needle curtain layer is made；
(5) using with step (3) identical method, by the natural bamboo fibres of 50 mesh, uniformly scattered be layered on pine needle curtain layer is made
The third layer natural bamboo fibres layer thick into 3mm, that is, form the slab of a five-layer structure；
(6) by the billet for scribbling paraffin wax emulsions, (applying amount of paraffin wax emulsions is 2g/m2) cover the plate prepared in step (5)
On base；It is then fed into heat pressing forming machines and carries out hot-forming, hot pressing temperature is 110 DEG C, pressing time 20min, and pressure is
1.5Mpa, complete the preparation of low-density natural bamboo fibres enhancing polycaprolactone composite material.
High intensity low density natural wood fiber reinforced polycaprolactone composite tensile strength manufactured in the present embodiment reaches
24MPa, bending strength reach 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 invention, structural representation is as schemed
Shown in 1, alternately it is compounded to form successively by two layers of natural plant fibre layer 1 (natural straw fibrous layer) and one layer of pine needle curtain layer 2
Sandwich structure, the wherein bottom of the composite and the superiors are natural straw fibrous layer (thickness 2mm), middle
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, including with
Lower step：
(1) it is applied on billet that (paraffin wax emulsions applying amount is 2g/m using paraffin wax emulsions as anti-adhesion agent2), then by 60
Purpose natural straw fiber, which uniformly dissipates to be layered on, is made the thick natural straw fibrous layers of 2mm on the billet of coated paraffin wax emulsions；
Pine needle is sent into the microwave stove heat 2min that power is 500W, with a diameter of 0.2mm PVC linear slits Cheng Dan after cooling
The pine needle curtain of layer, it is standby；
(2) by spray gun by the dimethyl formamide solution of polycaprolactone (polycaprolactone and dimethyl formyl in the solution
The mass ratio of amine is 1:4) (dimethyl formamide solution of polycaprolactone and natural rice are uniformly sprayed onto on natural straw fibrous layer
Grass fiber layer mass ratio is 40:1), then using hair-dryer to the natural of the dimethyl formamide solution for spraying polycaprolactone
Rice-straw fibre layer blowing hot-air 8min, make dimethylformamide volatilization clean；Then the pine needle curtain handled well is laid in natural rice
Pine needle curtain layer is formed on grass fiber layer；
(3) again the natural straw fiber of 60 mesh is uniformly dissipated to be layered on and the thick natural straw fibres of 2mm is made on pine nut curtain layer
Layer is tieed up, obtains three-decker slab；
(4) by the billet for scribbling paraffin wax emulsions, (applying amount of paraffin wax emulsions is 2g/m2) cover the plate prepared in step (3)
On base；It is then fed into heat pressing forming machines and carries out hot-forming, hot pressing temperature is 100 DEG C, pressing time 25min, and pressure is
2.0Mpa, complete the preparation of low-density natural straw fiber reinforced polycaprolactone composite.
High intensity low density natural wood fiber reinforced polycaprolactone composite tensile strength manufactured in the present embodiment reaches
26MPa, bending strength reach 50MPa, and density only has 0.99g/cm3。
Claims (9)
- A kind of 1. preparation method of high intensity low density natural plant fibre enhancing polycaprolactone composite material, it is characterised in that institute It is the sandwich construction being alternately compounded to form successively by N+1 layer natural plant fibre layers and N layer pine needle curtains layer to state composite, its Middle N=1,2,3 or 4, the bottom of the composite and the superiors are natural plant fibre layer, the system of the composite Preparation Method comprises the following steps：(1) paraffin wax emulsions are applied on billet, then natural plant fibre is uniformly dissipated to the steel for being layered on coated paraffin wax emulsions The thick natural plant fibre layers of 2-4mm are made on backing plate；(2) dimethyl formamide solution of polycaprolactone is uniformly sprayed onto on natural plant fibre layer by spray gun, dried, so Pine needle curtain is laid on natural plant fibre layer afterwards and forms pine needle curtain layer；(3) natural plant fibre is uniformly dissipated to be layered on and the thick natural plant fibre layers of 2-4mm is made on pine nut curtain layer, obtain plate Base；(4) billet for scribbling paraffin wax emulsions is covered on the slab prepared in step (3)；It is then fed into heat pressing forming machines and carries out It is hot-forming, complete the preparation of the low-density natural plant fibre enhancing polycaprolactone composite material.
- 2. preparation method as claimed in claim 1, it is characterised in that the thickness of the natural plant fibre layer is 2-4mm.
- 3. preparation method as claimed in claim 1, it is characterised in that the pine needle curtain layer is by microwave heating treatment mistake 's.
- 4. the preparation method stated such as claim 1, it is characterised in that be additionally included on the natural plant fibre layer after step (3) Step (2) and step (3) operation is repeated several times, until forming the composite slab of five layers, seven layers or nine Rotating fields.
- 5. the preparation method as described in claim 1 or 4, it is characterised in that during hot-forming, hot pressing temperature 100- 120 DEG C, pressing time 15-30min, pressure 1.0-2.0Mpa.
- 6. the preparation method as described in claim 1 or 4, it is characterised in that the dimethyl formamide solution of the polycaprolactone The mass ratio of middle polycaprolactone and dimethylformamide is 1:4.
- 7. the preparation method as described in claim 1 or 4, it is characterised in that the preparation method of the pine needle curtain is：First by pine needle The microwave stove heat 1-2min that power is 500-700W is sent into, the pine needle curtain of individual layer is seamed into after cooling.
- 8. the preparation method as described in claim 1 or 4, it is characterised in that in the step (2), the dimethyl of polycaprolactone Formamide solution and natural plant fibre layer mass ratio are (30-40):1；The drying blows 5-10min using hot blast.
- 9. the preparation method as described in claim 1 or 4, it is characterised in that the particle diameter of the natural plant fibre is 30~60 Mesh；The coated weight that the paraffin wax emulsions are applied on billet is 2g/m2。
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| CN103429371A (en) * | 2011-03-30 | 2013-12-04 | 东丽株式会社 | Prepreg, fiber reinforced composite material, and manufacturing method for fiber reinforced composite material |
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2016
- 2016-05-10 CN CN201610305218.7A patent/CN105907062B/en not_active Expired - Fee Related
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| CN1242396A (en) * | 1999-07-16 | 2000-01-26 | 中山大学 | Method for preparing natural composite material |
| CN103429371A (en) * | 2011-03-30 | 2013-12-04 | 东丽株式会社 | Prepreg, fiber reinforced composite material, and manufacturing method for fiber reinforced composite material |
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| CN104118018A (en) * | 2014-07-23 | 2014-10-29 | 连云港保丽森实业有限公司 | Inorganic flame retarding bamboo and wood composite ecological plant fiber board and production method thereof |
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