CN104559099B - Polylactic acid-based flax fiber composite material and preparation process thereof - Google Patents
Polylactic acid-based flax fiber composite material and preparation process thereof Download PDFInfo
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- CN104559099B CN104559099B CN201510007542.6A CN201510007542A CN104559099B CN 104559099 B CN104559099 B CN 104559099B CN 201510007542 A CN201510007542 A CN 201510007542A CN 104559099 B CN104559099 B CN 104559099B
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- flax fiber
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- 239000000835 fiber Substances 0.000 title claims abstract description 37
- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 241000208202 Linaceae Species 0.000 title claims abstract description 29
- 235000004431 Linum usitatissimum Nutrition 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000004626 polylactic acid Substances 0.000 title abstract description 32
- 229920000747 poly(lactic acid) Polymers 0.000 title abstract description 31
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000001125 extrusion Methods 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 239000008187 granular material Substances 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 15
- 150000001875 compounds Chemical class 0.000 claims description 12
- 238000005469 granulation Methods 0.000 claims description 10
- 230000003179 granulation Effects 0.000 claims description 10
- -1 lactyl Chemical group 0.000 claims description 9
- 238000002347 injection Methods 0.000 claims description 8
- 239000007924 injection Substances 0.000 claims description 8
- 238000005516 engineering process Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 5
- 239000007822 coupling agent Substances 0.000 abstract description 3
- 238000001746 injection moulding Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000012545 processing Methods 0.000 abstract description 3
- 208000034530 PLAA-associated neurodevelopmental disease Diseases 0.000 abstract 1
- 238000011160 research Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- VQKFNUFAXTZWDK-UHFFFAOYSA-N alpha-methylfuran Natural products CC1=CC=CO1 VQKFNUFAXTZWDK-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
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- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a high-performance polylactic acid-based flax fiber composite material and a preparation process thereof. The composite material comprises the following components: 80 wt% of PLA and 20 wt% of flax fiber. The preparation method of the composite material comprises the following steps: drying PLA granules and short flax fibers by using a drying box, putting the dried raw materials into a co-rotating double-screw extrusion system according to the components of the composite material for hot mixing extrusion, cooling by using a cooling pipeline, and finally granulating, drying and injection molding. Wherein the screw speed is 150tr/min and the total feed rate is 4kg/h or 2 kg/h. Compared with the existing preparation method, the material does not need a coupling agent in the mixing process, so that the cleanness and complete degradability of the composite material are ensured; expensive hot processing equipment is not needed, the cost is reduced, and the preparation method has high efficiency. Can be applied to mass production, and expands the application range of the polylactic acid-based flax fiber composite material.
Description
Technical field
The present invention relates to a kind of mechanical property height, the polylactic acid base flax fiber composite of mix homogeneously and preparation work thereof
Skill.Being specifically related to a kind of energy-conserving and environment-protective, the high-performance poly lactyl have completely biodegradable, being independent of oil is sub-
The heat of mixing expressing technique of flaxen fiber, has wide range of applications.
Background technology
Polylactic acid (PLA) has a fully biodegradable as a kind of macromolecular material, and its preparation process be with
Reproducible plant resources is raw material.Therefore, the development and application of PLA can alleviate dependence oil to a certain extent
Conventional polymer material non-degradable pressure that environment is caused and shortage of resources problem.
But the toughness of polylactic acid is low, high in cost of production shortcoming greatly limit its range of application.
Meanwhile, flax fiber (Linen) is that in Plant fiber, mechanical property is a kind of, cheap and easy to get also
And biodegradable and regeneration.Therefore by polylactic acid as basic phase, Caulis et Folium Lini is prepared using flax fiber as reinforcement fine
Dimension/polylactic acid (PLA-Linen) composite improves material property and the method reducing cost, by greatly as a kind of
Amount experimental fact proves effectively.
The development within initial a period of time of the polylactic acid base flax fiber composite is more slow, and its reason is that it mixes
Closing extrusion to be difficult to control, often, and easily there is the blocking of fiber in broken string.The seminar of SYLVAN was once
Through preferably controlling the parameters in extrusion, however obtained compound particles the injection mo(u)lding stage by
In viscosity excessive and can not the demoulding smoothly.
In the mixing extrusion of polylactic acid and flax fiber, in process temperature control, feeding degree of accuracy and
The requirement of tooth shape of screw and screw speed is higher, hole easily occurs, causes that sample fragility is big, defect is many.
, there is following drawback in traditional heat of mixing expressing technique, and first, processing step is more and energy loss is big；The
Two, coupling agent need to be used to increase mixing homogeneity, destroy the complete biodegradability of composite；3rd,
Preparing sample yields low, defect is many；4th, twin-screw system has kneading disk device more, easily causes blocking
Phenomenon.
Summary of the invention
It is an object of the invention to provide a kind of energy-conserving and environment-protective, stability is high, has high Young's modulus, high-tensile
Preparation method with the polylactic acid base flax fiber composite of high impact toughness.
The technical solution realizing the object of the invention is:
A kind of lactyl flax fiber composite, composition is as follows: PLA 80%wt, flax fiber 20%wt.
The preparation technology of above-mentioned lactyl flax fiber composite, described preparation technology comprises the following steps:
The first step: the coarse tow of PLA granule and length no more than 3mm is dried；
Second step: according to composite material compositions proportioning, dried raw material is put into the feeding of parallel dual-screw extruder
Mouthful, the screw shaft sleeving temperature of parallel dual-screw extruder is set to 12 sections, its each section of temperature be followed successively by 50 DEG C, 100 DEG C,
110 DEG C, 115 DEG C, 130 DEG C, 135 DEG C, 135 DEG C, 145 DEG C, 145 DEG C, 145 DEG C, 155 DEG C, 155 DEG C, to former
Material carries out hot mixing extrusion, and controlling total feed rate is 4kg/h or 2kg/h, and screw speed is 150tr/min；
3rd step: cut granulation the most afterwards by water cooled for the mixing extrudate of previous step, the rotating speed of diced system is
1500tr/min；
In 4th step, the compound particles that cooling granulation obtains is dried, injection mo(u)lding.
In the first step, baking temperature is not more than 80 DEG C, drying time 2-4h.
In 4th step, baking temperature is not more than 80 DEG C, drying time 6-8h.
Compared with prior art, its remarkable advantage is the present invention: (1) is by accurately controlling particles of polylactic acid and short Caulis et Folium Lini
The rate of feeding of fiber, each section of temperature of twin-screw system length direction and the rotating speed of twin screw, so that mixing extrusion
Process stabilization, automatization, with the polylactic acid base flax fiber obtaining mix homogeneously, porosity is low, mechanical property is good
Composite.(2) present invention need not add any coupling agent, maintains the complete biodegradability of composite.
(3) present invention need not the equipment of costliness and complicated processing step, reduces preparation cost.(4) present invention is fine
Wesy's amount is big compared with on going result greatly, also improves the mechanical property of material while reducing cost.(5) present invention squeezes
Go out process simple, do not use kneading disk, it is easy to be applied in actual production.
Below in conjunction with the accompanying drawings the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is sample surface scan Electronic Speculum figure in the embodiment of the present invention 1.
Fig. 2 is sample surface scan Electronic Speculum figure in the embodiment of the present invention 2..
Detailed description of the invention
Embodiment 1
(1) composite material compositions design
Polylactic acid base flax fiber composite in the present invention, composition is as follows: PLA 80%wt, flax fiber 20%wt.
(2) raw material drying
Particles of polylactic acid and coarse tow being respectively put in drying baker, baking temperature is 80 DEG C, is dried 2h.
(3) mix homogeneously is prepared, the mixing expressing technique of the polylactic acid base flax fiber composite of high intensity
CLEXTRAL-BC21 double screw extruder is used to prepare mix homogeneously, polylactic acid-flax fiber that size is unified
Compound particles, concrete preparation method is as follows: according to composite material compositions proportioning, raw material is put into parallel dual-screw and extrudes
The spout of machine, raw material dried to the first step carries out hot mixing extrusion, sets total feed rate as 4kg/h, spiral shell
Bar rotating speed is 150tr/min.Set each section of temperature of twin screw length direction as:
To mix cutting granulation after the cooled tube-cooled of extrudate, the rotating speed of diced system is 1500tr/min.
(4) compound particles is dried
The compound particles that cooling granulation obtains is dried 6h, and baking temperature is 80 DEG C.
(5) injection mo(u)lding.
Use the injection moulding machine of Krauss Maffei 50t level, to dried compound particles injection mo(u)lding.It sets
Determining parameter is:
It can be seen from figure 1 that fiber size is relatively big, illustrating that its palliating degradation degree is low, reinforced effects is good.
Extrusion stage total feed rate is 4kg/h, screw speed is that the sample Young's modulus prepared under the conditions of 150tr/min is the highest,
Under this background, the assembly average of each sample is 6091Mpa, higher than pure polylactic acid sample 64%.Maximum is
6490Mpa is higher than pure polylactic acid 75.5%, and is better than the research test result of equidirectional before this problem.Its impact is tough
Property also optimal, the impact fracture energy assembly average of each sample is 20.3kJ/m2, higher than pure polylactic acid sample 14%.
Maximum is 20.9kJ/m2Higher than pure polylactic acid 17.8% simultaneously also superior to the research test knot of equidirectional before this problem
Really.
Embodiment 2
(1) composite material compositions design
Polylactic acid base flax fiber composite in the present invention, composition is as follows: PLA 80%wt, flax fiber 20%wt.
(2) raw material drying
Particles of polylactic acid and coarse tow being respectively put in drying baker, baking temperature is 80 DEG C, is dried 2h.
(3) mix homogeneously is prepared, the mixing expressing technique of the polylactic acid base flax fiber composite of high intensity
CLEXTRAL-BC21 double screw extruder is used to prepare mix homogeneously, polylactic acid-flax fiber that size is unified
Compound particles, concrete preparation method is as follows: according to composite material compositions proportioning, raw material is put into parallel dual-screw and extrudes
The spout of machine, raw material dried to the first step carries out hot mixing extrusion, sets total feed rate as 2kg/h, spiral shell
Bar rotating speed is 150tr/min.Set each section of temperature of twin screw length direction as:
To mix cutting granulation after the cooled tube-cooled of extrudate, the rotating speed of diced system is 1500tr/min.
(4) compound particles is dried
The compound particles that cooling granulation obtains is dried 6h, and baking temperature is 80 DEG C.
(5) injection mo(u)lding.
Use the injection moulding machine of Krauss Maffei 50t level, to dried compound particles injection mo(u)lding.It sets
Determining parameter is:
As can be seen from Figure 2, although fiber size is little compared with Fig. 1, but its porosity is prepared less than in embodiment 1
Sample, in terms of hot strength, the most therefore surmounted embodiment 1.
Total feed rate be 2kg/h, screw speed be 150tr/min under the conditions of prepare sample hot strength the highest,
Under this background, the assembly average of each sample is 63.3Mpa, higher than pure polylactic acid sample 33.2%.Maximum is
64.6Mpa is higher than pure polylactic acid 36%, and is better than existing research test result.
Claims (6)
1. a lactyl flax fiber composite, it is characterised in that being calculated in mass percent, described composite is composed of the following components: PLA 80%, flax fiber 20%, described composite prepared by following steps:
The first step: the coarse tow of PLA granule and length no more than 3mm is dried；
Second step: according to composite material compositions proportioning, dried raw material is put into the spout of parallel dual-screw extruder, the screw shaft sleeving temperature of parallel dual-screw extruder is set to 12 sections, its each section of temperature is followed successively by 50 DEG C, 100 DEG C, 110 DEG C, 115 DEG C, 130 DEG C, 135 DEG C, 135 DEG C, 145 DEG C, 145 DEG C, 145 DEG C, 155 DEG C, 155 DEG C, raw material is carried out hot mixing extrusion, controlling total feed rate is 4kg/h or 2kg/h, and screw speed is 150tr/min；
3rd step: cut granulation the most afterwards by water cooled for the mixing extrudate of previous step, the rotating speed of diced system is 1500tr/min；
In 4th step, the compound particles that cooling granulation obtains is dried, injection mo(u)lding.
2. lactyl flax fiber composite as claimed in claim 1, it is characterised in that in the first step, baking temperature is not more than 80 DEG C, drying time 2-4h.
3. lactyl flax fiber composite as claimed in claim 1, it is characterised in that in the 4th step, baking temperature is not more than 80 DEG C, drying time 6-8h.
4. the preparation technology of a lactyl flax fiber composite, it is characterised in that comprise the steps:
The first step: the coarse tow of PLA granule and length no more than 3mm is dried；
Second step: according to composite material compositions proportioning, dried raw material is put into the spout of parallel dual-screw extruder, the screw shaft sleeving temperature of parallel dual-screw extruder is set to 12 sections, its each section of temperature is followed successively by 50 DEG C, 100 DEG C, 110 DEG C, 115 DEG C, 130 DEG C, 135 DEG C, 135 DEG C, 145 DEG C, 145 DEG C, 145 DEG C, 155 DEG C, 155 DEG C, raw material is carried out hot mixing extrusion, controlling total feed rate is 4kg/h or 2kg/h, and screw speed is 150tr/min；
3rd step: cut granulation the most afterwards by water cooled for the mixing extrudate of previous step, the rotating speed of diced system is 1500tr/min；
In 4th step, the compound particles that cooling granulation obtains is dried, injection mo(u)lding.
5. the preparation technology of lactyl flax fiber composite as claimed in claim 4, it is characterised in that in the first step, baking temperature is not more than 80 DEG C, drying time 2-4h.
6. the preparation technology of lactyl flax fiber composite as claimed in claim 4, it is characterised in that in the 4th step, baking temperature is not more than 80 DEG C, drying time 6-8h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510007542.6A CN104559099B (en) | 2015-01-07 | 2015-01-07 | Polylactic acid-based flax fiber composite material and preparation process thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510007542.6A CN104559099B (en) | 2015-01-07 | 2015-01-07 | Polylactic acid-based flax fiber composite material and preparation process thereof |
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| CN104559099A CN104559099A (en) | 2015-04-29 |
| CN104559099B true CN104559099B (en) | 2016-09-21 |
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| DE102016009794A1 (en) | 2016-08-12 | 2018-02-15 | Fabian Schütz | Constructive hybrid laser composite made of bamboo or flax |
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| JP2005089535A (en) * | 2003-09-12 | 2005-04-07 | Agri Future Joetsu Co Ltd | Composite resin composition and method for producing the same |
| CN101003667A (en) * | 2006-01-20 | 2007-07-25 | 东丽纤维研究所（中国）有限公司 | Composite material of poly lactic acid / natural faric, and production method |
| CN101200579B (en) * | 2007-11-26 | 2011-05-25 | 同济大学 | Natural fibre reinforced polylactic acid composite material and method for making same |
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