CN101790454A - Poly-(lactic acid) Biocomposite material of making a kind of flow process of poly-(lactic acid) Biocomposite material and utilizing this flow process made - Google Patents

Poly-(lactic acid) Biocomposite material of making a kind of flow process of poly-(lactic acid) Biocomposite material and utilizing this flow process made Download PDF

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CN101790454A
CN101790454A CN200880101691A CN200880101691A CN101790454A CN 101790454 A CN101790454 A CN 101790454A CN 200880101691 A CN200880101691 A CN 200880101691A CN 200880101691 A CN200880101691 A CN 200880101691A CN 101790454 A CN101790454 A CN 101790454A
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biocomposite material
fiber
pla
flow process
lactic acid
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CN200880101691A
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金显中
李秉浩
金熙壽
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Seoul National University Industry Foundation
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Seoul National University Industry Foundation
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
    • B29C70/06—Fibrous reinforcements only
    • B29C70/10—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres
    • B29C70/12—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres using fibres of short length, e.g. in the form of a mat
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/02—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
    • B29C70/06—Fibrous reinforcements only
    • B29C70/10—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
    • B29C70/28—Shaping operations therefor
    • B29C70/40—Shaping or impregnating by compression not applied
    • B29C70/42—Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles
    • B29C70/46—Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles using matched moulds, e.g. for deforming sheet moulding compounds [SMC] or prepregs
    • B29C70/465—Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles using matched moulds, e.g. for deforming sheet moulding compounds [SMC] or prepregs and impregnating by melting a solid material, e.g. sheets, powders of fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2995/00—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds
    • B29K2995/0037—Other properties
    • B29K2995/0059—Degradable
    • B29K2995/006—Bio-degradable, e.g. bioabsorbable, bioresorbable or bioerodible

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Composite Materials (AREA)
  • Textile Engineering (AREA)
  • Reinforced Plastic Materials (AREA)
  • Biological Depolymerization Polymers (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Injection Moulding Of Plastics Or The Like (AREA)
  • Materials For Medical Uses (AREA)

Abstract

The present invention illustrates a kind of method of making Biocomposite material, this method is utilized a combing flow process, with biodegradable (lactic acid) (PLA) selected universal polypropylene fiber of fiber mixing that gathers, and compression molding is a Biocomposite material, can overcome problem, and explanation is with this PLA Biocomposite material of this method made with this PLA Biocomposite material of injection molding made.

Description

Poly-(lactic acid) Biocomposite material of making a kind of flow process of poly-(lactic acid) Biocomposite material and utilizing this flow process made
[technical field]
The present invention is relevant with a kind of method of making Biocomposite material substantially, especially with utilizing a combing flow process mixed biologic degraded poly-(lactic acid) (PLA) a kind of method of fiber and selected universal polypropylene fiber is relevant, and the compressible problem that can overcome that is configured as with this PLA Biocomposite material of injection molding method made.The present invention simultaneously is relevant with this PLA Biocomposite material of the method made that utilizes the present invention.
[prior art]
Owing to pay attention to global environmental problem gradually, the influence of for example processing of waste plastic, climate change pact and new environmental specification or the like have more been deepened the concern to the novel environment friendly material that comprises Biocomposite material.Biocomposite material generally is made up of the strengthening material that natural fiber powder (for example wood powder, rice husk powder, bamboo powder or the like) and natural fiber (for example wood fibre, linen thread, fiber crops or the like) are made.So just can utilize Biocomposite material and as the substitute of the traditional polymer composite of being formed with inorganic material (carbon fiber that for example utilizes glass fibre to make) as strengthening material.Compared to this inorganic filler, Biocomposite material has the advantage of biodegradation and environmental protection.
[disclosure]
[technical matters]
Use at present or study more than several Biocomposite materials all based on polyene hydroxyl (PP, PE, PS), can be widely used in this polymer industry, and with environmental protection and natural fiber that can biodegradation or powder as reinforcing agent.Develop the material that this class Biocomposite material can be used and offer base plate construction material, structural material, filler and be applied to automotive interior.Yet, although polyene hydroxyl composite has the feature of environmental protection of part, because the nondegradation of this polyene hydroxyl makes polyene hydroxyl composite not assert that the feature of environmental protection is arranged.Therefore, be desirably in the following application that various industrial aspect can be provided based on all biodegradable Biocomposite materials of biological degradation polyalcohol.The physical characteristic that the research institute that is carrying out at present gives Biocomposite material can reach the equally gratifying physical characteristic of universal resin of present use.
In many such biodegradable polymer, PLA (poly-(lactic acid)) has caused special attention.Because when such biodegradable polymers was embedded in a landfill, this polymer can be degraded to the avirulence material, so utilize such biodegradable PLA as a kind of base polymer of Biocomposite material its advantage to be arranged.In addition, PLA is a kind of indissolubility living resources, can replace exhaustive petroleum resources.Yet when via injection molding the PLA fiber production being Biocomposite material, the high fragility of this PLA fiber when room temperature can cause problem.That is to say that forming the PLA that mixes pattern with the natural stuffing with a higher young's modulus is with injection molding mode made, so this final Biocomposite material breaks easily.Except this fragility factor, the problem of this natural material is that injection molding needs this powder processing.
The problem that is taken place when preparing this PLA fiber base Biocomposite material in order to overcome with injection molding, the present invention advises a kind of compression forming method of use one combing flow process.In addition, all well and good by this Biocomposite material that PLA is prepared in conjunction with evaluating with every physical index of prepared this universal polymer P P of compression molding, and can overcome the fragility of this PLA.
[technical solution]
Purpose of the present invention is: penetrating via the compression that utilizes a combing flow process provides the method for making a kind of Biocomposite material, and wherein this physical characteristic can overcome the fragility of this PLA by this.
Another object of the present invention is: a kind of method is provided, penetrates via the compression that utilizes a combing flow process, make a biological composite by the PLA fiber, the universal polymer P P of itself and this is combined and improve physical characteristic.
Another purpose of the present invention is: the Biocomposite material that can use in all types of industries field that requires mechanical strength (comprising electronic equipment and automotive interior case) is provided.
[favourable effect]
Utilize this Biocomposite material of this method made to comprise: to mix via a combing flow process as (PLA) fiber and of a base polymer poly-(lactic acid), and obtain desmachyme as the natural fiber of a strengthening material; Under the pressure of a decision in advance, this desmachyme is processed as a liner; And this liner carried out compression molding and become thing composite material sheet in all one's life, can overcome the high fragility problem of this PLA and meet needed physical characteristic, comprise tensile strength, bending strength and impact strength.
In addition, even if utilize the PLA fiber in conjunction with the PP fiber, method of the present invention still guarantees the intensity and the biological degradability of this Biocomposite material.Biocomposite material of the present invention has mechanical and physical property to a certain degree, and the application in all types of industries field that requires mechanical strength (case that comprises electronic equipment and automotive interior) can be provided.
[illustrating]
The 1st figure: be the block flow diagram of making the Biocomposite material flow process according to the present invention;
The 2nd figure: be the schematic diagram of measuring the bending strength method of Biocomposite material according to the present invention;
The 3rd figure: be schematic diagram according to the Biocomposite material tensile strength of base polymer type and this natural fiber content;
The 4th figure: be schematic diagram according to the Biocomposite material tensile strength of base polymer type;
The 5th figure: be schematic diagram according to the Biocomposite material bending strength of base polymer type;
The 6th figure: be schematic diagram according to the Biocomposite material impact strength of base polymer type and this natural fiber content; And
The 7th figure: be schematic diagram according to the Biocomposite material impact strength of base polymer type.
[optimal mode]
The method that proposes a kind of making one biological composite in order to reach above purpose comprises: in a combing flow process, mix as (PLA) fiber and as the natural fiber of a strengthening material of a base polymer poly-(lactic acid), and produce desmachyme; Under the pressure of a decision in advance, this desmachyme is processed as a liner; And this liner carried out compression molding and obtain a biological composite material sheet.
Provide a kind of method of making one biological composite to comprise simultaneously: in a combing flow process, mixing as a base polymer poly-(lactic acid) (PLA) fiber and in conjunction with polypropylene fibre on function as the natural fiber of a strengthening material, produce desmachyme; Under the pressure of a decision in advance, this desmachyme is processed as a liner; And this liner carried out compression molding and obtain a biological composite material sheet.
This Biocomposite material can overcome PLA to have the problem of high fragility and meets desired physical characteristic, comprises tensile strength, bending strength and impact strength.
In addition, even if utilize the PLA fiber to come in conjunction with the PP fiber, method of the present invention still can guarantee the intensity and the biological degradability of this Biocomposite material.Biocomposite material of the present invention has mechanical and physical property to a certain degree, and the application in all types of industries field can be provided, and wherein comprises electronic equipment and automotive interior material.
Via the following graphic explanation that proposes but shall not be construed as and limit example of the present invention, just can further understand the present invention.
At first to propose the composition explanation of this Biocomposite material according to the present invention, propose the explanation of this Biocomposite material and experiment then according to the present invention.This noun that present application for patent is used " combing flow process " expression is after removing unwanted material or removing unwanted shorter length, crude fibre in the small-sized aggregation can be separated into indivedual yarns by a flow process, indivedual then yarns can the position on position parallel to each other and be prepared as carding.Can use a carding machine to carry out this combing flow process.
The present invention's fiber poly-(lactic acid) (PLA) is intended for a biological degradation polymer.The length of this fiber poly-(lactic acid) is 30mm, the scope of melt index 10 to 30g/10min (190 ℃/2,160g) between, density is 1.22g/cm 3Following Chemical formula 1 can be represented PLA.
Chemical formula 1
Be used in conjunction with one of PLA non-biodegradable material is polypropylene (PP) fiber of Korea S Kolon system.The density of this PP fiber is 0.91g/cm 3, MFI is that (230 ℃/2,160g), length is 30mm to 12g/10min.
According to the present invention, can select PLA fiber and PP fiber to use, with a kind of strengthening material as Biocomposite material of the present invention together with this natural fiber kenaf and jute (by the import of institute of Korea S Soo trading company).In addition, can utilize the natural fiber of length 50～70mm as a kind of strengthening material.
The making of example 1:PLA Biocomposite material
Utilize following compression molding flow process to make the PLA Biocomposite material.At first, utilize a carding machine to mix this biodegradation PLA fiber and non-biodegradation PP fiber and this kenaf or jute fiber.After with a needle point method this mixing desmachyme being embroidered, keep temperature under the pressure of a decision in advance be 120 ℃, and resulting this mixing desmachyme is processed as a liner, carries out compression molding then.In order to finish compression molding, be 70kgf/cm at pressure 2This temperature is set at 200 ℃ down.Through after this flow process, just can construction Biocomposite material sheet.This Biocomposite material sheet will be stored in the Polythene Bag with the prevention penetration of moisture.Fig. 1 shows the making flow process of this PLA Biocomposite material that comprises a combing flow process.Table 1 has been put the composition with this Biocomposite material of this flow process made in order.The mixed proportion of representing this composition fiber with wt%.
The composition of table 1. Biocomposite material (wt%)
Figure GPA00001013586000041
Experiment example 1: the preparation of sample
Take out sample by dried this Biocomposite material sheet, utilize a pressing, under 5MPa, use sample to carry out tensile strength and bending strength test.Test will be 23 ± 2 ℃ in temperature, and RH carried out 40 hours for 50 ± 5% times.
Experiment example 2: the tensile strength of measuring Biocomposite material
Measure the tensile strength of this sample so that check effect and lip-deep this polymeric material of this Biocomposite material of this combing flow process.Measure tensile strength according to ASTM D638-03, at room temperature use a general-purpose test machine (Zwick Co.), setting a drift speed is 5mm/min.Obtain a mean value of five measurement results of this tensile strength.
Experiment example 3: the bending strength of measuring Biocomposite material
Measure the bending strength of this sample so that check effect and lip-deep this polymeric material of this Biocomposite material of this combing flow process.Measure bending strength according to ASTM D790-03, at room temperature use a general-purpose test machine (Zwick Co.), setting a compression speed is 5mm/min.Obtain a mean value of five measurement results of this bending strength.Fig. 2 illustrates a three-point bending test.
Experiment example 4: the impact strength of measuring Biocomposite material
Impact strength is that a sample is subjected to impact load and breaks needed unit are or unit length energy.According to ASTM D256, impact the unit width energy of side and can represent impact strength.Generally carry out measurement in three kinds of modes: a unfilled corner operation, finish one-shot measurement with this operation at this equidirectional of a unfilled corner; One no unfilled corner operation is finished one-shot measurement with this operation at this rightabout of a unfilled corner; And a final operation, wherein on a sample that stands vertically, add one-shot.This example uses unfilled corner operation test impact strength.
1. according to the tensile strength of polymeric material
Fig. 3 demonstration adds that by PP natural fiber or PLA add the tensile strength of the Biocomposite material that the jute fiber is formed.As shown in the drawing, when increasing the content of this natural fiber, can descend by the tensile strength of natural fiber and this Biocomposite material that PP formed.When the content of this natural fiber is lower than 30%, this drops to gradually and forms, but when using more content, this descends just very rapid, show when adding the volume natural fiber as a strengthening material, the connection between PP and this natural fiber will be weakened, and the tensile strength of this Biocomposite material can be reduced greatly.In addition, as the explanation of following table 2, the high more voidage that will increase in this Biocomposite material of the content of natural fiber causes the decline of tensile strength.When increasing the content of natural fiber, finding to increase voidage.Voidage can be disturbed the connection of this PP to the jute fiber, and hinders the transmission of this stress, therefore causes the decline of tensile strength.The content of this space interface can form the space between the natural fiber and within the natural fiber.When the preparation of the natural fiber of one low content is entered sample, because the cause of this PLA fragility, be easy to break at this sample surfaces based on this Biocomposite material of PLA.Therefore can in this Biocomposite material, obtain intensity on the low side.On the other hand, can measure that to contain a natural fiber content be that 50% or 70% Biocomposite material has quite high intensity.And the intensity of this Biocomposite material only can be higher than the intensity based on this Biocomposite material of PP.These results explain and select a PLA polymer as one of reason of a base polymer of Biocomposite material.
Table 2. is according to the void content of natural fiber content in the Jute/PP compound
Figure GPA00001013586000061
Fig. 4 shows according to the tensile strength of using as the base polymer of Biocomposite material.Adopt the mixture of PP, PP and PLA and PLA as base polymer (Class1: PP fiber 50%+Jute fiber 50% respectively, type 2:PP fiber 35%+PLA fiber 15%+Jute fiber 50%, type 3:PP fiber 25%+PLA fiber 25%+Jute fiber 50%, type 4:PP fiber 15%+PLA fiber 35%+Jute fiber 50%, type 5:PP fiber 50%+Jute fiber 50%).Only in using the type 5 of PLA as a kind of unique base polymer, can measure this tensile strength descends, but show that other this Biocomposite material all has similar numerical value and can obviously not descend, expression PLA can partly replace PP, and tensile strength is descended significantly.That is to say, demonstrate the tensile strength that is similar to based on the compound of PP based on the Biocomposite material of PLA and PP, but more biological degradability is arranged, therefore can utilize as the material of environmental protection more.
Simultaneously, The above results also proves: can overcome the fragility problem that this Biocomposite material suffered via the injection molding made via this PLA Biocomposite material of the compression molding made that uses a combing flow process.In addition, although replace this a part of PP fiber with PLA, this Biocomposite material shows enough physical characteristics.
2. according to the bending strength of polymeric material
Fig. 5 measures and draws the bending strength of this Biocomposite material of example 1 made.As shown in the figure, compared to this Biocomposite material so that PP and PLA were formed, even if using the content of this Jute fiber in the Biocomposite material that PP and PLA formed is 50%, its intensity and no significant difference hint the combination of a kind of PP and PLA and use PLA can both be used as the base polymer of Biocomposite material separately.
3. according to the impact strength of polymeric material
With reference to Fig. 6, when increasing the content of this natural fiber, the impact strength of this Biocomposite material will increase.The improvement of this impact strength may be interpreted as the fragility that this Biocomposite material of expression can overcome this base polymer.Fig. 7 shows the impact strength of this Biocomposite material of being made up of the mixed base polymer.This diagram data obviously shows: find to add that by various PP and PLA this Biocomposite material that the mixture of jute fiber is formed has enough impact strengths.

Claims (4)

1. method of making a biological composite comprises:
In a combing flow process, mix as poly-(lactic acid) of a base polymer (PLA) on fiber and the function as the natural fiber of a strengthening material, and produce desmachyme;
Under the pressure of a decision in advance, it is a liner that this desmachyme is processed; And
This liner is carried out compression molding and become thing composite material sheet in all one's life.
2. according to this method of patent claim 1, wherein can use the PLA fiber to become a desmachyme in conjunction with polypropylene fibre.
3. according to this method of patent claim 1 or 2, wherein this natural fiber is kenaf fiber or jute fiber.
4. poly-(lactic acid) Biocomposite material, and with wherein a kind of method made of patent claim 1 to 3.
CN200880101691A 2007-08-03 2008-07-31 Poly-(lactic acid) Biocomposite material of making a kind of flow process of poly-(lactic acid) Biocomposite material and utilizing this flow process made Pending CN101790454A (en)

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KR1020070078305A KR100870597B1 (en) 2007-08-03 2007-08-03 A process for manufacturing poly(latic acid) bio-composites and poly(latic acid) bio-composites thereby
KR10-2007-0078305 2007-08-03
PCT/KR2008/004465 WO2009020303A2 (en) 2007-08-03 2008-07-31 A process for manufacturing poly(latic acid) bio-composites and poly(latic acid) bio-composites thereby

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Application publication date: 20100728