CN103571158A - High interfacial compatibility PLA/PBAT blend and preparation method - Google Patents
High interfacial compatibility PLA/PBAT blend and preparation method Download PDFInfo
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Abstract
The present invention discloses a high interfacial compatibility PLA/PBAT blend preparation method, which comprises: uniformly mixing pre-dried polylactic acid (PLA) and pre-dried poly(butyleneadipate-co-terephthalate) (PBAT) according to any mass ratios; adding the mixture to a HAAKE mixer to mix, wherein the mixing temperature is 150-180 DEG C, and the rotation speed of the rotor is 40-70 rpm; and after the blend is melted, adding a chain extender A and a chain extender B, and continuously mixing for 5-10 min to obtain the high interfacial compatibility PLA/PBAT blend. The invention further provides the high interfacial compatibility PLA/PBAT blend prepared through the preparation method. According to the present invention, different reaction activities of the two chain extenders on different terminal groups of the polyester are adopted, the PLA and PBAT block copolymer is formed in the blend is formed, the process steps are simplified, and the high interfacial compatibility PLA/PBAT blend is obtained.
Description
Technical field
The present invention relates to technical field of polymer materials, relate in particular to the aliphatic polyester of high interface compatibility and aliphatic-aromatic copolyester blend and preparation method thereof, be specially polylactic acid PLA/poly-(terephthalic acid butyleneglycol-CO-hexanodioic acid butyleneglycol) ester PBAT blend of a kind of high interface compatibility and preparation method thereof.
Background technology
Poly-(terephthalic acid butyleneglycol-co-hexanodioic acid butyleneglycol) ester (PBAT) is a kind of aliphatic-aromatic copolyester, has both had good ductility and toughness, has again good thermotolerance and impact property; Simultaneously, this copolyesters also has good biodegradability, is a kind of environmentally friendly macromolecular material, can be widely used in the wrapping material fields such as film, substitute traditional non-degradable plastics film, the problem of environmental pollution that the use of minimizing conventional films brings.But the tensile strength of this aliphatic-aromatic copolyester of PBAT low (22Mpa left and right); In addition, PBAT is that to take terephthalic acid (PTA) or dimethyl terephthalate (DMT) (DMT), BDO (BG) and hexanodioic acid (AA) be raw material, under catalyst action, by direct esterification or ester-interchange method, is polymerized.The expensive raw material price of preparing this copolyesters.Therefore, on cost, adopt full-biodegradable film prepared by PBAT to compare and there is very large weak tendency with not biodegradable films such as traditional polypropylene (PP), polyethylene (PE).So in order to reduce the cost of PBAT Biodegradable film, a kind of method is by PBAT and starch blending.But film strength prepared by the blend obtaining by this method will be lower, be unsuitable for some the higher occasion of requirement of strength is used.
Poly(lactic acid) (PLA) is that the starch being extracted by renewable plant resourceses such as corn, potatos is converted into glucose, and glucose becomes lactic acid by fermentation, the aliphatic polyester being further polymerized.The glass transition temperature Tg of PLA is approximately 55 ℃, and fusing point Tm is approximately 180 ℃, has good biocompatibility, and can complete biodegradable, and the final product after degraded is water and carbonic acid gas, thereby PLA is nontoxic, can not cause environmental pollution.Meanwhile, the tensile strength of PLA high (>60MPa), modulus of compression is high, and the transparency is good, and forming process is convenient, and price is cheap compared with PBAT.Therefore, film prepared by PLA and PBAT blend not only can complete biodegradable, can also utilize the high strength of PLA to improve the tensile strength of blend simultaneously, makes the film of preparation be applicable to the occasion higher to requirement of strength.
But interface compatibility when PLA and PBAT blend is poor, in order to make blend there is better tensile strength, must improve the interface compatibility of PLA and PBAT.Document (Bioresource Technology 101,2010:8406-8415) etc. reported and used the compound of epoxies as both expanding materials, the epoxide group that utilizes expanding material and-OH or-COOH effect, make to connect on expanding material molecular chain PLA and PBAT molecular chain, thereby improve both interface compatibilities; Patent CN101245178 first makes PLA and carry out-OH of PBAT end-blocking, then in the molten system of PLA and PBAT, add vulcabond to carry out the segmented copolymer that chain extension is prepared PLA and PBAT, then with this segmented copolymer, as expanding material, join and in the co-mixing system of PLA and PBAT, improve both interface compatibilities.
Because the reactive behavior of epoxide group and the p-OH of isocyanate groups is higher, p-COOH shows as larger inertia, so adopt this compounds to need first just can obtain reasonable compatibilization effect to carry out-OH of polyester termination process as expanding material, this is complicated operation in actual industrial production.
Summary of the invention
Object of the present invention is just to provide PLA/PBAT blend of a kind of high interface compatibility and preparation method thereof, with solve that above-mentioned prior art exists for obtaining good compatibilization effect, need first to carry out-OH of polyester termination process, the problem of the method complicated operation of existing increase-volume PLA and PBAT blend.
Object of the present invention is achieved through the following technical solutions:
The preparation method of PLA/PBAT blend, comprise the following steps:
After dried in advance polylactic acid PLA and poly-(terephthalic acid butyleneglycol-CO-hexanodioic acid butyleneglycol) ester PBAT resin are mixed with any mass ratio, add and in Haake Banbury mixer, carry out banburying, banburying temperature is 150-180 ℃, rotor speed is 40-70rpm, after blend melting, add chainextender A and chainextender B, continue banburying 5-10min, obtain polylactic acid PLA and poly-(terephthalic acid butyleneglycol-CO-hexanodioic acid butyleneglycol) ester PBAT blend of high interface compatibility.
Preferably, described polylactic acid PLA polyester is to be obtained by D-ALPHA-Hydroxypropionic acid, Pfansteihl, D-, Pfansteihl or DL-LACTIC ACID polymerization, and preferable weight-average molecular weight is 40000-200000.
Preferably, described poly-(terephthalic acid butyleneglycol-CO-hexanodioic acid butyleneglycol) ester PBAT copolyesters is with terephthalic acid PTA or dimethyl terephthalate (DMT) DMT, 1,4-butyleneglycol BG and hexanodioic acid AA are that polymerizable raw material obtains, and preferable weight-average molecular weight is 20000-130000.
Preferably, the preferred 1:9-9:1 of mass ratio of described polylactic acid PLA and poly-(terephthalic acid butyleneglycol-CO-hexanodioic acid butyleneglycol) ester PBAT.
Preferably, described chainextender A is bisoxazoline class chainextender, is selected from one or more in 2,2 '-bis-(2-oxazolines) or 1,3-penylene-bis-(2-oxazolines).
Preferably, the isocyanates chainextender that described chainextender B is functionality >=2, is selected from one or more in hexamethylene diisocyanate, tolylene diisocyanate, diphenylmethanediisocyanate, an xylylene diisocyanate, PPDI, dimethyl diphenyl vulcabond, isophorone diisocyanate, lysinediisocyanate or polymethylene multi-phenenyl isocyanate.
Preferably, the add-on of described chainextender A and chainextender B accounts for the 0.04-1.8% of polylactic acid PLA and poly-(terephthalic acid butyleneglycol-CO-hexanodioic acid butyleneglycol) ester PBAT total mass.
Preferably, the mass ratio of described chainextender A and chainextender B is 0.4-2.5:1.
Preferably, the mode that adds of described chainextender can be that chainextender A and chainextender B add simultaneously, also can first add chainextender A, then add chainextender B.
The present invention also comprises polylactic acid PLA/poly-(terephthalic acid butyleneglycol-CO-hexanodioic acid butyleneglycol) ester PBAT blend of a kind of high interface compatibility being prepared by above-mentioned preparation method.
Compared with prior art, the present invention has following beneficial effect:
Due to bisoxazoline class chainextender, p-COOH shows as higher activity, and p-OH is shown as inertia; And the p-OH of isocyanates chainextender shows as higher activity, p-COOH is shown as inertia.The present invention adopts this two kinds of chainextender actings in conjunction, utilize two kinds of chainextenders active to the differential responses of polyester different end group, thereby be more conducive to form the segmented copolymer of PLA and PBAT in PLA and PBAT blend, reach the object that improves two-phase interface consistency, also without to carry out-OH of polyester or-COOH termination process, simplify processing step, obtained having the PLA/PBAT blend of high interface compatibility.
Embodiment
Below in conjunction with each embodiment, describe the present invention in detail, but be to be understood that lifted embodiment is just in order to explain the present invention, and be not intended to limit protection scope of the present invention.
The PLA resin using in embodiment is the production of Natureworks company, and the trade mark is 4032D; PBAT resin is that BASF Aktiengesellschaft produces, and the trade mark is Ecoflex C1200.
Tensile property testing standard is ASTM D638, dumbbell shaped batten, and thick 1mm, draw speed is 10mm/min, surveys 5 samples, gets its mean value for every group; Socle girder notched Izod impact strength testing standard is ASTM D256, the thick 3mm of batten, and bob velocity 3.5m/s, the heavy 0.816kg of pendulum, surveys 5 samples, gets its mean value for every group.
Embodiment 1
After being mixed according to both mass ratioes 90/10, dried in advance PLA and PBAT add in Haake Banbury mixer, at 170 ℃, and banburying under the rotor speed of 50rpm.After blend melting, add chainextender A and chainextender B simultaneously, the add-on of chainextender A and chainextender B is 1.8% of total polymer mass (PLA and PBAT total mass), the mass ratio of chainextender A and chainextender B is 1:1; Wherein chainextender A be 2,2 '-bis-(2-oxazolines), chainextender B is hexamethylene diisocyanate; Chainextender adds rear continuation banburying 10min, obtains PLA and the PBAT blend of high interface compatibility.
By the good blend compressing tablet on vulcanizing press of banburying, 170 ℃ of molding temperatures, after blend melting under 15MPa hot pressing 5min, the 15min that colds pressing, obtains respectively the thick and thick print of 3mm of 1mm, makes and stretches and impact batten and carry out Mechanics Performance Testing.
Embodiment 2
After being mixed according to both mass ratioes 10/90, dried in advance PLA and PBAT add in Haake Banbury mixer, at 180 ℃, and banburying under the rotor speed of 40rpm.After blend melting, add chainextender A and chainextender B simultaneously, the add-on of chainextender A and chainextender B is 0.04% of total polymer mass (PLA and PBAT total mass), the mass ratio of chainextender A and chainextender B is 2.5:1; Wherein chainextender A is 1,3-penylene-bis-(2-oxazolines), and chainextender B is tolylene diisocyanate; Chainextender adds rear continuation banburying 5min, obtains PLA and the PBAT blend of high interface compatibility.
By the good blend compressing tablet on vulcanizing press of banburying, 170 ℃ of molding temperatures, after blend melting under 15MPa hot pressing 5min, the 15min that colds pressing, obtains respectively the thick and thick print of 3mm of 1mm, makes and stretches and impact batten and carry out Mechanics Performance Testing.
Embodiment 3
After being mixed according to both mass ratioes 60/40, dried in advance PLA and PBAT add in Haake Banbury mixer, at 150 ℃, and banburying under the rotor speed of 70rpm.After blend melting, first add chainextender A2,2 '-bis-(2-oxazolines), after banburying 2min, add again chainextender B lysinediisocyanate, continue banburying 5min, obtain PLA and the PBAT blend of high interface compatibility.The add-on of chainextender A and chainextender B is 0.5% of total polymer mass (PLA and PBAT total mass), and the mass ratio of chainextender A and chainextender B is 0.4:1.
By the good blend compressing tablet on vulcanizing press of banburying, 170 ℃ of molding temperatures, after blend melting under 15MPa hot pressing 5min, the 15min that colds pressing, obtains respectively the thick and thick print of 3mm of 1mm, makes and stretches and impact batten and carry out Mechanics Performance Testing.
Embodiment 4
After being mixed according to both mass ratioes 50/50, dried in advance PLA and PBAT add in Haake Banbury mixer, at 180 ℃, and banburying under the rotor speed of 50rpm.After blend melting, add chainextender A and chainextender B simultaneously, the add-on of chainextender A and chainextender B is 0.8% of total polymer mass (PLA and PBAT total mass), the mass ratio of chainextender A and chainextender B is 2.5:1; Wherein chainextender A is 1,3-penylene-bis-(2-oxazolines), and chainextender B is polymethylene multi-phenenyl isocyanate; Chainextender adds rear continuation banburying 5min, obtains PLA and the PBAT blend of high interface compatibility.
By the good blend compressing tablet on vulcanizing press of banburying, 170 ℃ of molding temperatures, after blend melting under 15MPa hot pressing 5min, the 15min that colds pressing, obtains respectively the thick and thick print of 3mm of 1mm, makes and stretches and impact batten and carry out Mechanics Performance Testing.
Embodiment 5
After being mixed according to both mass ratioes 50/50, dried in advance PLA and PBAT add in Haake Banbury mixer, at 180 ℃, and banburying under the rotor speed of 50rpm.After blend melting, add chainextender A and chainextender B simultaneously, the add-on of chainextender A and chainextender B is 1.1% of total polymer mass (PLA and PBAT total mass), the mass ratio of chainextender A and chainextender B is 0.7:1; Wherein chainextender A is 1,3-penylene-bis-(2-oxazolines), and chainextender B is diphenylmethanediisocyanate; Chainextender adds rear continuation banburying 5min, obtains PLA and the PBAT blend of high interface compatibility.
By the good blend compressing tablet on vulcanizing press of banburying, 170 ℃ of molding temperatures, after blend melting under 15MPa hot pressing 5min, the 15min that colds pressing, obtains respectively the thick and thick print of 3mm of 1mm, makes and stretches and impact batten and carry out Mechanics Performance Testing.
Comparative example 1
After dried in advance PLA and PBAT are mixed according to both mass ratioes 60/40, add in Haake Banbury mixer, at 170 ℃, banburying 10min under the rotor speed of 50rpm, obtains PLA and PBAT blend.
By the good blend compressing tablet on vulcanizing press of banburying, 170 ℃ of molding temperatures, after blend melting under 15MPa hot pressing 5min, the 15min that colds pressing, obtains respectively the thick and thick print of 3mm of 1mm, makes and stretches and impact batten and carry out Mechanics Performance Testing.
The sample mechanical experimental results of embodiment 1-5 and comparative example 1 is as following table 1.
Table 1
By to blend Mechanics Performance Testing find, adopt this chain extension method can improve significantly the interface compatibility of blend, the blend mechanical property after modification is improved.
Disclosed is above only several specific embodiments of the application, but the application is not limited thereto, and the changes that any person skilled in the art can think of, all should drop in the application's protection domain.
Claims (10)
1. a preparation method for the PLA/PBAT blend of high interface compatibility, is characterized in that, comprises the following steps:
After dried in advance polylactic acid PLA and poly-(terephthalic acid butyleneglycol-CO-hexanodioic acid butyleneglycol) ester PBAT resin are mixed with any mass ratio, add and in Haake Banbury mixer, carry out banburying, banburying temperature is 150-180 ℃, rotor speed is 40-70rpm, after blend melting, add chainextender A and chainextender B, continue banburying 5-10min, obtain polylactic acid PLA and poly-(terephthalic acid butyleneglycol-CO-hexanodioic acid butyleneglycol) ester PBAT blend of high interface compatibility.
2. the preparation method of the PLA/PBAT blend of high interface compatibility as claimed in claim 1, it is characterized in that, described polylactic acid PLA polyester is to be obtained by D-ALPHA-Hydroxypropionic acid, Pfansteihl, D-, Pfansteihl or DL-LACTIC ACID polymerization, and preferable weight-average molecular weight is 40000-200000.
3. the preparation method of the PLA/PBAT blend of high interface compatibility as claimed in claim 1, it is characterized in that, described poly-(terephthalic acid butyleneglycol-CO-hexanodioic acid butyleneglycol) ester PBAT copolyesters is with terephthalic acid or dimethyl terephthalate (DMT), 1,4-butyleneglycol and hexanodioic acid are that polymerizable raw material obtains, and preferable weight-average molecular weight is 20000-130000.
4. the preparation method of the PLA/PBAT blend of high interface compatibility as claimed in claim 1, is characterized in that, the preferred 1:9-9:1 of mass ratio of described polylactic acid PLA and poly-(terephthalic acid butyleneglycol-CO-hexanodioic acid butyleneglycol) ester PBAT.
5. the preparation method of the PLA/PBAT blend of high interface compatibility as claimed in claim 1, it is characterized in that, described chainextender A is bisoxazoline class chainextender, is selected from 2, one or more in 2 '-bis-(2-oxazolines) or 1,3-penylene-bis-(2-oxazolines).
6. the preparation method of the PLA/PBAT blend of high interface compatibility as claimed in claim 1, it is characterized in that, the isocyanates chainextender that described chainextender B is functionality >=2, is selected from one or more in hexamethylene diisocyanate, tolylene diisocyanate, diphenylmethanediisocyanate, an xylylene diisocyanate, PPDI, dimethyl diphenyl vulcabond, isophorone diisocyanate, lysinediisocyanate or polymethylene multi-phenenyl isocyanate.
7. the preparation method of the PLA/PBAT blend of high interface compatibility as claimed in claim 1, it is characterized in that, the add-on of described chainextender A and chainextender B accounts for the 0.04-1.8% of polylactic acid PLA and poly-(terephthalic acid butyleneglycol-CO-hexanodioic acid butyleneglycol) ester PBAT total mass.
8. the preparation method of the PLA/PBAT blend of high interface compatibility as claimed in claim 1, is characterized in that, the mass ratio of described chainextender A and chainextender B is 0.4-2.5:1.
9. the preparation method of the PLA/PBAT blend of high interface compatibility as claimed in claim 1, is characterized in that, the mode that adds of described chainextender can be that chainextender A and chainextender B add simultaneously, also can first add chainextender A, then add chainextender B.
10. the polylactic acid PLA of the high interface compatibility that the preparation method described in any one prepares in claim 1-9/poly-(terephthalic acid butyleneglycol-CO-hexanodioic acid butyleneglycol) ester PBAT blend.
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CN114381098A (en) * | 2020-10-19 | 2022-04-22 | 北京化工大学 | Bio-based random copolyester compatibilization modified PLA/PBAT composite material and preparation method thereof |
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CN114381098A (en) * | 2020-10-19 | 2022-04-22 | 北京化工大学 | Bio-based random copolyester compatibilization modified PLA/PBAT composite material and preparation method thereof |
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