CN106893288A - A kind of preparation method of high-strength degradable lactic acid composite material - Google Patents

A kind of preparation method of high-strength degradable lactic acid composite material Download PDF

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Publication number
CN106893288A
CN106893288A CN201510949307.0A CN201510949307A CN106893288A CN 106893288 A CN106893288 A CN 106893288A CN 201510949307 A CN201510949307 A CN 201510949307A CN 106893288 A CN106893288 A CN 106893288A
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CN
China
Prior art keywords
coupling agent
pla
lactic acid
composite material
preparation
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Pending
Application number
CN201510949307.0A
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Chinese (zh)
Inventor
马海清
刘刚
杨鑫
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Sichuan Xinda Enterprise Group Co Ltd
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Sichuan Xinda Enterprise Group Co Ltd
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Priority to CN201510949307.0A priority Critical patent/CN106893288A/en
Publication of CN106893288A publication Critical patent/CN106893288A/en
Pending legal-status Critical Current

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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
    • C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
    • 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
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/92—Measuring, controlling or regulating
    • 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
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/92704—Temperature
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/06—Biodegradable
    • 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
    • C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers

Abstract

The present invention relates to a kind of preparation method of high-strength degradable lactic acid composite material, the ratio of its raw material components PLA/PC is 20:80, glass fibre, coupling agent, bulking agent.Production method is after a kind of hydrolysate with treated coupling agent is well mixed with the composite of PLA/PC and compatilizer, with glass fibre（GF）Blending carries out melting extrusion, forms the PLA composites of glass fiber reinforcement, the transmission of material strip communicated band, air cold cut, pelletizing, the packaging that will be extruded.The present invention directly extrudes high intensity biodegradable lactic acid composite material, and simple production process, product strength is good, environmentally safe using rear biodegradable, can effectively alleviate environmental problem and energy crisis.

Description

A kind of preparation method of high-strength degradable lactic acid composite material
Technical field
The invention belongs to PLA biological plastics field, it is related to a kind of preparation method of high-strength degradable lactic acid composite material.
Background technology
PLA has the advantages that excellent biological degradability, easy processing are molded because of it, in recent years the extremely favor of macromolecular material industry.But the defect such as itself more crisp, hot property is poor, degradation speed is whard to control, limits using effect, therefore need to be modified treatment.It preferably, is improved its machinery and heat resistance by the toughness and heat resistance of makrolon with polylactic acid blend, while adding compatilizer to improve both compatibilities.As most general reinforcing fiber because of its high intensity, high-modulus and high-fire resistance, the enhancing for being widely used in various general-purpose plastics and engineering plastics is modified glass fibre.
Fiber reinforcement PLA composites, especially glass fibre have 80% or so to apply in terms of various forms of macromolecular material enhancings.As reinforcing material, it is widely used, but because glass fibre and resin-based compatibility are bad, although and traditional silane coupler etc. can be obviously improved the compatibility of glass fibre and numerical value, but its temperature classification is low, differ larger with PLA in structure, it is impossible to significantly play a part of increase-volume, so the not enough problem of glass fiber reinforcement utilization rate can be caused, i.e. enhancing effect is undesirable.Therefore we obtain its hydrolysate and treatment are modified to glass fibre with treated coupling agent, strengthen its surface-active, improve the enhancing utilization rate of glass fibre.
The content of the invention
It is an object of the invention to provide a kind of preparation method of high-strength degradable lactic acid composite material, after being well mixed with the composite of PLA/PC and compatilizer with the hydrolysate of treated coupling agent, it is blended with glass fibre, by extrusion by melting, the PLA composites of glass fiber reinforcement are formed.Comprise the following steps that：
1st, the surface treatment of glass fibre
Coupling agent KH560 is diluted in water, is 7 with vinegar acid for adjusting pH value, be made into the coupling agent solution of 10 wt%.After coupling agent is fully hydrolyzed, solution is placed at 60 DEG C of vacuum and dries 4 h, just obtain the hydrolysate of coupling agent.Coupling agent after hydrolysis is well mixed with PLA, PC and E-MA-GMA material grain.Well mixed material is finally carried out into melting extrusion blending with GF.
2nd, the preparation of PLA/PC/E-MA-GMA/GF composites
First by PC at 120 DEG C the h of forced air drying 12,60 DEG C of h of drying 12 of PLA vacuum, PLA/PC/E-MA-GMA, coupling agent, GF are separately added into first, second, third Weightlessness balance, PLA/PC/E-MA-GMA is added from main spout, coupling agent is added from the second side spout, by the content of Weightlessness balance accurate adjustment each component, processing temperature is between 250-270 DEG C.It is to obtain high intensity PLA composites of the present invention by the transmission of the material strip of extrusion communicated band, air cold cut, pelletizing.
Specific embodiment
Example 1
Coupling agent KH560 is diluted in water, is 7 with vinegar acid for adjusting pH value, is made into the coupling agent solution of 10wt%.After coupling agent is fully hydrolyzed, solution is placed at 60 DEG C of vacuum and dries 4h, obtain the hydrolysate of coupling agent.It is 265 DEG C to set each process section temperature of double screw extruder, 270 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 250 DEG C, after temperature reaches setting value, first open the first Weightlessness balance, PLA/PC/E-MA-GMA mixtures are added from main spout with the rate of feeding of 20kg/h, after after die extrusion PLA, open the second Weightlessness balance, GF is added with the speed of 10kg/h, after machine to be extruded operates steadily, opening side feeding and the 3rd Weightlessness balance, coupling agent is added with the speed of 0.2kg/h, control screw speed is between 180-200rad/min, 80% of moment of torsion no more than machine utilization, head melt temperature is no more than 180 DEG C.
Tensile strength（MPa）79.5th, stretch modulus（MPa）1500th, bending strength（MPa）119.2nd, bending modulus（MPa）3230.
Embodiment 2
Coupling agent KH560 is diluted in water, is 7 with vinegar acid for adjusting pH value, is made into the coupling agent solution of 10wt%.After coupling agent is fully hydrolyzed, solution is placed at 60 DEG C of vacuum and dries 4h, obtain the hydrolysate of coupling agent.It is 265 DEG C to set each process section temperature of double screw extruder, 270 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 250 DEG C, after temperature reaches setting value, first open the first Weightlessness balance, PLA/PC/E-MA-GMA mixtures are added from main spout with the rate of feeding of 20kg/h, after after die extrusion PLA, open the second Weightlessness balance, GF is added with the speed of 10kg/h, after machine to be extruded operates steadily, opening side feeding and the 3rd Weightlessness balance, coupling agent is added with the speed of 0.3kg/h, control screw speed is between 180-200rad/min, 80% of moment of torsion no more than machine utilization, head melt temperature is no more than 180 DEG C.
Tensile strength（MPa）80.2nd, stretch modulus（MPa）1570th, bending strength（MPa）120.9th, bending modulus（MPa）3264.
Embodiment 3
Coupling agent KH560 is diluted in water, is 7 with vinegar acid for adjusting pH value, is made into the coupling agent solution of 10wt%.After coupling agent is fully hydrolyzed, solution is placed at 60 DEG C of vacuum and dries 4h, obtain the hydrolysate of coupling agent.It is 265 DEG C to set each process section temperature of double screw extruder, 270 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 250 DEG C, after temperature reaches setting value, first open the first Weightlessness balance, PLA/PC/E-MA-GMA mixtures are added from main spout with the rate of feeding of 20kg/h, after after die extrusion PLA, open the second Weightlessness balance, GF is added with the speed of 10kg/h, after machine to be extruded operates steadily, opening side feeding and the 3rd Weightlessness balance, coupling agent is added with the speed of 0.4kg/h, control screw speed is between 180-200rad/min, 80% of moment of torsion no more than machine utilization, head melt temperature is no more than 180 DEG C.
Tensile strength（MPa）82.8th, stretch modulus（MPa）1640th, bending strength（MPa）123.1st, bending modulus（MPa）3322.
Embodiment 4
Coupling agent KH560 is diluted in water, is 7 with vinegar acid for adjusting pH value, is made into the coupling agent solution of 10wt%.After coupling agent is fully hydrolyzed, solution is placed at 60 DEG C of vacuum and dries 4h, obtain the hydrolysate of coupling agent.It is 265 DEG C to set each process section temperature of double screw extruder, 270 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 250 DEG C, after temperature reaches setting value, first open the first Weightlessness balance, PLA/PC/E-MA-GMA mixtures are added from main spout with the rate of feeding of 20kg/h, after after die extrusion PLA, open the second Weightlessness balance, GF is added with the speed of 20kg/h, after machine to be extruded operates steadily, opening side feeding and the 3rd Weightlessness balance, coupling agent is added with the speed of 0.4kg/h, control screw speed is between 180-200rad/min, 80% of moment of torsion no more than machine utilization, head melt temperature is no more than 180 DEG C.
Tensile strength（MPa）102.2nd, stretch modulus（MPa）2045th, bending strength（MPa）138.1st, bending modulus（MPa）4830.
Embodiment 5
Coupling agent KH560 is diluted in water, is 7 with vinegar acid for adjusting pH value, is made into the coupling agent solution of 10wt%.After coupling agent is fully hydrolyzed, solution is placed at 60 DEG C of vacuum and dries 4h, obtain the hydrolysate of coupling agent.It is 265 DEG C to set each process section temperature of double screw extruder, 270 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 250 DEG C, after temperature reaches setting value, first open the first Weightlessness balance, PLA/PC/E-MA-GMA mixtures are added from main spout with the rate of feeding of 20kg/h, after after die extrusion PLA, open the second Weightlessness balance, GF is added with the speed of 25kg/h, after machine to be extruded operates steadily, opening side feeding and the 3rd Weightlessness balance, coupling agent is added with the speed of 0.4kg/h, control screw speed is between 180-200rad/min, 80% of moment of torsion no more than machine utilization, head melt temperature is no more than 180 DEG C.
Tensile strength（MPa）113.9th, stretch modulus（MPa）2180th, bending strength（MPa）150.9th, bending modulus（MPa）5584.

Claims (4)

1., with PLA/PC and compatilizer be well mixed treated coupling agent hydrolysate first by a kind of preparation method of high-strength degradable lactic acid composite material, it is characterised in that the PLA composites of described glass fiber reinforcement, then again with glass fibre（GF）Blended melting is extruded and is obtained；PLA and PC are with 20:80 mass ratioes are E-MA-GMA as matrix, solubilizer used（Ethylene-methyl acrylate-glyceryl methacrylate）Its formula is as follows：20 parts of PLA, 80 parts, bulking agent 4-7 parts, coupling agent 0.2-0.4 parts, glass fibre 15-30 parts of makrolon.
2. the preparation method of a kind of high-strength degradable lactic acid composite material according to claim 1, it is characterised in that described coupling agent is KH560, is 7 with vinegar acid for adjusting pH value first by its dilute with water, is made into the coupling agent solution of 10wt%；After coupling agent is fully hydrolyzed, solution is placed on 60 DEG C of vacuum, dries 4 h, obtain the hydrolysate of coupling agent.
3. the preparation method of a kind of high-strength degradable lactic acid composite material according to claim 1, it is characterised in that described PLA will first under vacuo 60 DEG C dry 12h, PC will dry 12h at 120 DEG C.
4. the preparation method of a kind of high-strength degradable lactic acid composite material according to claim 1, it is characterised in that it is comprised the following steps that：
By metering by PLA, makrolon, compatilizer mixture, coupling agent, glass fibre is separately added into first, second, third Weightlessness balance, mixture is added from main spout, side spout adds coupling agent, glass fibre is added in head, and extrusion blending is carried out by double screw extruder, and extruder processing temperature is between 250-270 DEG C；
The transmission of material strip communicated band, air cold cut, pelletizing, the packaging that will be extruded.
CN201510949307.0A 2015-12-18 2015-12-18 A kind of preparation method of high-strength degradable lactic acid composite material Pending CN106893288A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109206874A (en) * 2017-07-04 2019-01-15 四川鑫达企业集团有限公司 A kind of preparation method of the fire-retardant PLA/PC alloy material of high tenacity

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102108201A (en) * 2011-03-22 2011-06-29 东莞劲胜精密组件股份有限公司 High-property degradable plastic and preparation method thereof
CN102653627A (en) * 2011-03-04 2012-09-05 深圳市富恒塑胶新材料有限公司 Degradable PC (Poly Carbonate)/PLA (Poly Lactic Acid) alloy and preparation method thereof
CN102690507A (en) * 2011-03-23 2012-09-26 苏州汉扬精密电子有限公司 Glass fiber reinforced polylactic acid composite material
CN105086398A (en) * 2014-05-16 2015-11-25 四川鑫达企业集团有限公司 High-toughness flame-retarded PLA/PC alloy
CN106674947A (en) * 2015-08-20 2017-05-17 黑龙江鑫达企业集团有限公司 Method for producing PLA composite material having higher strength

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102653627A (en) * 2011-03-04 2012-09-05 深圳市富恒塑胶新材料有限公司 Degradable PC (Poly Carbonate)/PLA (Poly Lactic Acid) alloy and preparation method thereof
CN102108201A (en) * 2011-03-22 2011-06-29 东莞劲胜精密组件股份有限公司 High-property degradable plastic and preparation method thereof
CN102690507A (en) * 2011-03-23 2012-09-26 苏州汉扬精密电子有限公司 Glass fiber reinforced polylactic acid composite material
CN105086398A (en) * 2014-05-16 2015-11-25 四川鑫达企业集团有限公司 High-toughness flame-retarded PLA/PC alloy
CN106674947A (en) * 2015-08-20 2017-05-17 黑龙江鑫达企业集团有限公司 Method for producing PLA composite material having higher strength

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109206874A (en) * 2017-07-04 2019-01-15 四川鑫达企业集团有限公司 A kind of preparation method of the fire-retardant PLA/PC alloy material of high tenacity

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