CN114805697A - Compatibilizer for improving PLA/PBAT compatibility and high-filling full-biodegradable composite material - Google Patents
Compatibilizer for improving PLA/PBAT compatibility and high-filling full-biodegradable composite material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 16
- 238000011049 filling Methods 0.000 title claims abstract description 16
- 229920001896 polybutyrate Polymers 0.000 title claims abstract 11
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 67
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 23
- 208000034530 PLAA-associated neurodevelopmental disease Diseases 0.000 claims abstract description 12
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- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 12
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- 238000002360 preparation method Methods 0.000 claims description 4
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- AGXUVMPSUKZYDT-UHFFFAOYSA-L barium(2+);octadecanoate Chemical compound [Ba+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AGXUVMPSUKZYDT-UHFFFAOYSA-L 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
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- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 2
- FATBGEAMYMYZAF-KTKRTIGZSA-N oleamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(N)=O FATBGEAMYMYZAF-KTKRTIGZSA-N 0.000 claims description 2
- FATBGEAMYMYZAF-UHFFFAOYSA-N oleicacidamide-heptaglycolether Natural products CCCCCCCCC=CCCCCCCCC(N)=O FATBGEAMYMYZAF-UHFFFAOYSA-N 0.000 claims description 2
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- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims description 2
- 239000008117 stearic acid Substances 0.000 claims description 2
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 2
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- UAUDZVJPLUQNMU-UHFFFAOYSA-N Erucasaeureamid Natural products CCCCCCCCC=CCCCCCCCCCCCC(N)=O UAUDZVJPLUQNMU-UHFFFAOYSA-N 0.000 claims 1
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- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 2
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- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/02—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polycarbonates or saturated polyesters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2403/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2403/02—Starch; Degradation products thereof, e.g. dextrin
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2451/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2451/08—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/04—Polyesters derived from hydroxy carboxylic acids, e.g. lactones
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08K2003/265—Calcium, strontium or barium carbonate
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Abstract
The invention provides a compatibilizer for improving the compatibility of PLA and PBAT and a high-filling full-biodegradable composite material, which are used for enhancing the compatibility between the PLA and the PBAT and improving the filling amount of calcium carbonate. The fully biodegradable composite material prepared by using the compatibilizer has high filling amount, has the advantages of high tensile and tearing strength, good elongation at break, good barrier property, good degradation performance, strong water resistance and moisture resistance and the like, completely meets the requirements of packaging materials, can be widely applied to commercial supersource bags, garbage bags, rolling bags, agricultural films and the like, can be completely degraded under natural conditions, greatly reduces the production cost, does not generate harmful substances such as waste gas, waste water and the like, and protects the environment.
Description
Technical Field
The invention belongs to the technical field of biodegradable composite materials, and particularly relates to a compatibilizer for improving the compatibility of PLA and PBAT and a high-filling full-biodegradable composite material.
Background
With the development of the traditional plastic industry, plastic products are widely used in various fields and become an essential part of life. Because the traditional plastics have higher and higher consumption of petroleum resources and are difficult to degrade in natural environment, and the incineration treatment can generate a lot of harmful gases, the traditional plastics bring great convenience to people for living, and simultaneously, the problem of white pollution also causes great damage to the living environment of people. Therefore, replacing petroleum-based plastics with biodegradable plastics is one of the important ways to solve the problem of white pollution, among which polylactic acid (PLA) and polybutylene terephthalate-CO-adipate (PBAT) are the most used biodegradable plastics among many biodegradable plastics.
Polylactic acid (PLA) and polybutylene terephthalate-CO-adipate (PBAT), although excellent biodegradable materials, have certain drawbacks in their own right. For example, polylactic acid (PLA) has low elongation at break, high brittleness, poor toughness, high requirements on temperature and humidity, poor crystallinity control, difficult processing, and the like; polybutylene terephthalate-CO-adipate butylene glycol (PBAT) has low strength, defective processability, and the like. Therefore, the polylactic acid (PL A) and the polybutylene terephthalate-CO-adipate (PBAT) are blended, so that the advantages of the polylactic acid (PL A) and the polybutylene terephthalate-CO-adipate (PBAT) are complementary, and the production cost can be reduced by adding calcium carbonate, but the polylactic acid (PLA) and the polybutylene terephthalate-CO-adipate (PBAT) have poor compatibility and limited calcium carbonate filling amount, so that a compatilizer which can improve the compatibility between the PLA and the PBAT and can also improve the calcium carbonate filling content is hopefully used.
CN 113773558A discloses PLA and PBAT and ST degradation composite material and its production process. According to the mass percentage, 20-30 parts of PLA resin, 20-30 parts of PBAT resin, 0.3-1 part of ST, 60-80 parts of edible corn starch, 0.5-2 parts of starch composite modifier, 0.5-1.5 parts of lubricant, 0.3-0.8 part of coupling agent and 0.3-0.8 part of antioxidant. The method needs to modify the starch to prepare modified starch, and then the modified starch is mixed with other materials to be granulated according to a proportion, and finally the biodegradable film material is prepared.
CN 113736223A provides an inorganic filled PBAT/PLA material composition and a method for preparing particles and films thereof. According to the weight portion, 50-80 portions of PBAT, 3-10 portions of PLA, 1-5 portions of PVA, 0.5-1 portion of water, 10-30 portions of talcum powder, 1-5 portions of plasticizer, 0.1-1 portion of lubricant, 0.1-1 portion of compatilizer and 0.1-1 portion of chain extender.
CN 113773617A provides a PBAT-based material and a preparation method and application thereof, and comprises, by weight, 30-40 parts of PBAT, 10-20 parts of PLA, 5-15 parts of corn starch, 5-10 parts of PMMA, 25-35 parts of talcum powder, 1-5 parts of ethylene glycol, and 0.1-1 part of PTW (reactive elastomer ethylene-butyl acrylate-glycidyl methacrylate copolymer). The method has complicated processing process, and the used compatibilizer can not be biodegraded.
Although the biodegradable film material is prepared by the method, the filler content is low, the process is complicated, the energy consumption is high, the degradation rate is low, and the prepared film material has weak mechanical capacity, is easy to break and has high cost, so that the application range is limited.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a compatibilizer used for enhancing the compatibility between PLA and PBAT full-biodegradable composite materials. Also provides a preparation method of the high calcium carbonate filled PLA/PBAT particles. The fully biodegradable composite material prepared by using the compatibilizer has low production cost, has certain mechanical strength and temperature resistance, completely meets the requirements of packaging materials, can be widely applied to commercial supersource bags, garbage bags, rolling bags, agricultural films and the like, can be completely degraded under natural conditions, does not generate harmful substances such as waste gas, waste water and the like, protects the environment and saves petroleum resources.
In order to achieve the technical purpose, the invention is solved by the following technical scheme:
the invention provides a compatibilizer for improving the compatibility of PLA and PBAT, which comprises the following components in parts by weight: 75-98 parts of polylactic acid (PLA), 1-10 parts of Maleic Anhydride (MAH), 0.1-1 part of dibenzoyl peroxide (BPO), 0.1-1 part of main antioxidant and 0.1-1 part of auxiliary antioxidant, and the preparation method comprises the following steps:
the method comprises the following steps: weighing BPO and MAH by an electronic balance according to a certain proportion, adding the BPO and the MAH into a beaker filled with 500mL of acetone, and then placing the beaker in an ultrasonic cleaning machine for shaking dissolution for 30 min;
step two: adding pure PLA particles into the mixed solution in the step one, uniformly mixing, and drying;
step three: and finally, carrying out melt extrusion in a double-screw extruder to prepare the compatibilizer graft A used by the invention, granulating and drying for later use, wherein the temperature of each temperature zone of the extruder is set to be 165,175,185,185,185,175 ℃ respectively, and the rotating speed of a screw is set to be 100 r/min.
A PLA/PBAT high-filling full-biodegradable composite material comprises, by weight, 5-20 parts of polylactic acid (PLA), 40-60 parts of polybutylene terephthalate-co-butylene adipate (PBAT), 30-45 parts of calcium carbonate, 1-10 parts of a compatibilizer A, 0.5-2 parts of a coupling agent, 0.1-1 part of a lubricant and 0.1-1 part of an antioxidant, and the method for preparing the PLA/PBAT full-biodegradable composite material comprises the following steps:
s1, placing PLA and PBAT into a blast oven or a vacuum oven according to the formula proportion for drying treatment, and drying at 75-85 ℃ for 4-12h to ensure that the water content of each component is less than or equal to 1000ppm for later use;
s2, putting the compatibilizer into a blast oven or a vacuum oven according to the formula proportion for drying treatment, and drying for 1-2h at 50-70 ℃ for later use;
s3, adding calcium carbonate into the drying and stirring machine according to the formula proportion, heating and dehydrating for 1-2h, measuring the water content, controlling the water content below 0.3%, setting the temperature at 110 ℃ and setting the rotating speed at 50 r/min. Then stirring for 10-20min at 50-60 ℃ under the condition of 15r/min, then sequentially adding a coupling agent, an antioxidant and a lubricant, and continuously stirring for 30min to prepare modified calcium carbonate;
s4, adding the dried PLA, PBAT and compatibilizer into the modified calcium carbonate prepared in the step S3, adding a lubricant, and continuously stirring for 30min to obtain a PLA/PBAT and calcium carbonate blend;
and S5, carrying out twin-screw extrusion granulation on the blend to obtain the calcium carbonate filled PLA/PBAT particles.
Wherein the compatibilizer adopts the compatibilizer A for increasing the compatibility of PLA/PBAT.
Preferably, the polylactic acid used above has a melt index of 5 to 7 g/min.
Preferably, the polybutylene terephthalate-CO-adipate used as described above has a melt index of 2.7 to 4.9 g/min.
Preferably, the fineness of the calcium carbonate used is 1000-2000 mesh.
Preferably, the coupling agent used is one or more of aluminate, titanate, gamma-mercaptopropyltrimethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane or gamma-glycidoxypropyltrimethoxysilane.
Preferably, the lubricant used is one or more of stearic acid, calcium stearate, sodium stearate, zinc stearate, barium stearate, erucyl amide, oleamide, paraffin wax or polyethylene wax.
Preferably, the primary antioxidant used is one or more of hindered phenol antioxidant (2, 2-bis [ [3[3, 5-bis (1, 1-dimethylethyl) -4-hydroxyphenyl ] -1-oxopropoxy ] methyl ] -1, 3-propanediyl-3, 5-bis (1, 1-dimethylethyl) -4-hydroxyphenylpropionate) (1010), β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid octadecanol ester (1076) and 2-methylenebis (4-methyl-6-tert-butylphenol) (2246).
Preferably, the auxiliary antioxidant is one or more of phosphite ester antioxidant tris (2, 4-di-tert-butyl phenyl) phosphite (168), didodecanediol thiodipropionate (DLTDP) and distearyl thiodipropionate (DSTDP).
The invention can bring the following beneficial effects:
1. the compatibilizer can be prepared by grafting PLA by Maleic Anhydride (MAH) and Benzoyl Peroxide (BPO), has simple operation and low cost, and can improve the compatibility between the PLA and the PBAT.
2. One end of the aluminate ester can react with the chemical groups on the surface of the calcium carbonate, and the other end can react with the maleic anhydride, so that the calcium carbonate is better compatible with the PLA/PBAT blend after modification, thereby improving the filling amount in the PLA/PBAT, achieving the effect of reducing the cost, and also enhancing the mechanical property of the fully biodegradable composite material.
3. The invention has simple operation process and short operation time, is beneficial to reducing the cost in all aspects, and is suitable for large-scale industrial production and large-batch continuous production.
Drawings
FIG. 1 shows the results of the comprehensive mechanical property tests of the examples;
fig. 2 shows an SEM image of an embodiment.
Detailed Description
The technical solutions of the present invention will be described clearly and completely below, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
First, experiment raw materials
PLA (polylactic acid): NatureWorks LLC product, USA, 4032D, melt index 5-7g/10min (190 ℃, 2.16 kg).
PBAT (polybutylene terephthalate-co-adipate): a product of polyester Limited at Tungtun of Xinjiang blue mountain, No. TH801T, having a melt index of 2.7-4.9g/10min (190 ℃, 2.16 kg).
BPO (benzoyl peroxide): shanghai Michelin Biochemical technology, Inc.; MAH (maleic anhydride): shanghai Teng quasi-Biotechnology Limited; antioxidant IRGAFOS 168 tris (2, 4-di-tert-butylphenyl) phosphite and antioxidant IRGAFOS 1010(2, 2-bis [ [3[3, 5-bis (1, 1-dimethylethyl) -4-hydroxyphenyl ] -1-oxopropoxy ] methyl ] -1, 3-propanediyl-3, 5-bis (1, 1-dimethylethyl) -4-hydroxyphenylpropionate): BASF new materials, inc; calcium stearate: weikang Biotechnology Ltd. Other raw materials and reagents were obtained from commercial sources unless otherwise specified.
Second, performance test parameters and test method
(1) The samples of examples 1 to 10 were each subjected to tensile strength testing according to the method of GB/T1040.1-2006.
(2) The samples of examples 1 to 10 were each subjected to an elongation at break test according to the method of GB/T1040.1-2006.
(3) The samples of examples 1 to 10 were each subjected to micron-scale electron scanning electron microscopy measurements according to the method of GB/T1659.4-2008.
Third, specific embodiments
Example 1
And S1, placing PLA and PBAT into a blast oven or a vacuum oven for drying treatment, and drying for 4 hours at 80 ℃.
S2, preparing the compatibilizer A by melt blending of a double-screw extruder, wherein the adding parts of MAH and BPO are respectively 2% and 0.35% of the total part of PLA. Putting MAH and BPO into 500mL of acetone, putting the acetone into an ultrasonic cleaning machine, vibrating and dissolving the acetone for 30min, uniformly mixing the acetone with 95 parts of PLA, and drying; and then carrying out melt extrusion, granulation and drying in a double-screw extruder to prepare the compatibilizer A. The temperature of each section of the extruder (from the mouth mold to the feeding port) is set to be 165,175,185,185,185,175 ℃ respectively, and the screw rotating speed is set to be 100 r/min.
S3, modification of calcium carbonate: adding calcium carbonate into a drying and stirring machine according to the formula proportion, heating and dehydrating for 1-2h, measuring the water content, controlling the water content to be below 0.3%, setting the temperature to be 110 ℃, and setting the rotating speed to be 50 r/min. Then stirring for 10-20min at 50-60 ℃ under the condition of 15r/min, then sequentially adding the coupling agent, the antioxidant and the lubricant, and continuously stirring for 30min to prepare the modified calcium carbonate.
S4, mixing 10 parts by weight of PLA, 50 parts by weight of PBAT, 5 parts by weight of compatibilizer A, 0.2 part by weight of antioxidant 168, 0.4 part by weight of antioxidant 1010 and 0.4 part by weight of lubricant with 30 parts by weight of modified calcium carbonate in a high-speed mixer, wherein the mixing speed is 50rpm, and the mixing time is 10 minutes; then adding the mixture into a double-screw extruder to extrude and granulate. The extrusion conditions were: the screw rotating speed is 200rpm, and the screw temperature is set from the feed opening to the machine head in a segmented mode as follows: the modified full-biodegradable material is prepared by air cooling, granulating and drying at 155 ℃, 160 ℃, 165 ℃ and 160 ℃.
S5, placing the modified full-biodegradable composite material into a film blowing machine for film blowing processing, setting the temperature of each temperature zone of the film blowing machine to be 145-165 ℃, and finally obtaining the high-filling full-degradable film.
Example 2
Using the modified calcium carbonate and the compatibilizer A prepared in example 1 as raw materials, fully mixing 9 parts by weight of PLA, 48 parts by weight of PBAT, 35 parts by weight of plasticized modified starch, 5 parts by weight of compatibilizer, 0.2 part by weight of antioxidant 168, 0.4 part by weight of antioxidant 1010 and 0.4 part by weight of lubricant in a high-speed mixer at a mixing speed of 50rpm for 10 minutes; then adding the mixture into a double-screw extruder to extrude and granulate. The extrusion conditions were: the screw rotating speed is 200rpm, and the screw temperature is set from the feed opening to the machine head in a segmented mode as follows: the modified full-biodegradable material is prepared by air cooling, granulating and drying at the temperature of 155 ℃, 160 ℃, 165 ℃ and 160 ℃. And carrying out film blowing processing to obtain the high-filling full-degradable film.
Example 3
Taking the modified calcium carbonate and the compatibilizer A prepared in the example 1 as raw materials, and fully mixing 8 parts by weight of PLA, 45 parts by weight of PBAT, 40 parts by weight of plasticized modified starch, 5 parts by weight of compatibilizer, 0.2 part by weight of antioxidant 168, 0.4 part by weight of antioxidant 1010 and 0.4 part by weight of lubricant in a high-speed mixer at the mixing speed of 50rpm for 10 minutes; then adding the mixture into a double-screw extruder to extrude and granulate. The extrusion conditions were: the screw rotating speed is 200rpm, and the screw temperature is set from the feed opening to the machine head in a segmented mode as follows: the modified full-biodegradable material is prepared by air cooling, granulating and drying at the temperature of 155 ℃, 160 ℃, 165 ℃ and 160 ℃. And carrying out film blowing processing to obtain the high-filling full-degradable film.
Example 4
Taking the modified calcium carbonate and the compatibilizer A prepared in the example 1 as raw materials, and fully mixing 7 parts by weight of PLA, 42 parts by weight of PBAT, 45 parts by weight of modified calcium carbonate, 5 parts by weight of compatibilizer, 0.2 part by weight of antioxidant 168, 0.4 part by weight of antioxidant 1010 and 0.4 part by weight of lubricant in a high-speed mixer at a mixing speed of 50rpm for 10 minutes; then adding the mixture into a double-screw extruder to extrude and granulate. The extrusion conditions were: the screw rotating speed is 200rpm, and the screw temperature is set from the feed opening to the machine head in a segmented mode as follows: the modified full-biodegradable material is prepared by air cooling, granulating and drying at the temperature of 155 ℃, 160 ℃, 165 ℃ and 160 ℃. And carrying out film blowing processing to obtain the high-filling full-degradable film.
Example 5
Taking the modified calcium carbonate prepared in the example 1 as a raw material, fully mixing 10 parts by weight of PLA, 50 parts by weight of PBAT, 30 parts by weight of calcium carbonate, 0.2 part by weight of antioxidant 168, 0.4 part by weight of antioxidant 1010 and 0.4 part by weight of lubricant in a high-speed mixer at the mixing speed of 50rpm for 10 minutes; then adding the mixture into a double-screw extruder to extrude and granulate. The extrusion conditions were: the screw rotating speed is 200rpm, and the screw temperature is set from the feed opening to the machine head in a segmented mode as follows: air cooling, granulating, drying at 155 deg.C, 160 deg.C, 165 deg.C, 160 deg.C, and blowing to obtain film.
Example 6
Using the modified calcium carbonate prepared in example 1 as a raw material, fully mixing 9 parts by weight of PLA, 48 parts by weight of PBAT, 35 parts by weight of calcium carbonate, 0.2 part by weight of antioxidant 168, 0.4 part by weight of antioxidant 1010 and 0.4 part by weight of lubricant in a high-speed mixer at a mixing speed of 50rpm for 10 minutes; then adding the mixture into a double-screw extruder to extrude and granulate. The extrusion conditions were: the screw rotating speed is 200rpm, and the screw temperature is set from the feed opening to the machine head in a segmented mode as follows: air cooling, granulating, drying at 155 deg.C, 160 deg.C, 165 deg.C, 160 deg.C, and blowing to obtain film.
Example 7
Taking the modified calcium carbonate prepared in the example 1 as a raw material, fully mixing 8 parts by weight of PLA, 45 parts by weight of PBAT, 40 parts by weight of calcium carbonate, 0.2 part by weight of antioxidant 168, 0.4 part by weight of antioxidant 1010 and 0.4 part by weight of lubricant in a high-speed mixer at the mixing speed of 50rpm for 10 minutes; then adding the mixture into a double-screw extruder to extrude and granulate. The extrusion conditions were: the screw rotating speed is 200rpm, and the screw temperature is set from the feed opening to the machine head in a segmented mode as follows: at 155 ℃, 160 ℃, 165 ℃, 160 ℃ and air cooling, granulating, drying and blowing to obtain the film.
Example 8
Taking the modified calcium carbonate prepared in the example 1 as a raw material, fully mixing 7 parts by weight of PLA, 42 parts by weight of PBAT, 45 parts by weight of calcium carbonate, 0.2 part by weight of antioxidant 168, 0.4 part by weight of antioxidant 1010 and 0.4 part by weight of lubricant in a high-speed mixer at the mixing speed of 50rpm for 10 minutes; then adding the mixture into a double-screw extruder to extrude and granulate. The extrusion conditions were: the screw rotating speed is 200rpm, and the screw temperature is set from the feed opening to the machine head in a segmented mode as follows: air cooling, granulating, drying at 155 deg.C, 160 deg.C, 165 deg.C, 160 deg.C, and blowing to obtain film.
Fourth, Performance analysis
(1) Analysis of mechanical Properties
Referring to FIG. 1 and Table 1, by comparing examples 1 and 5, examples 2 and 6, examples 3 and 7, and examples 4 and 8, it can be concluded that the addition of compatibilizer A and modified calcium carbonate results in a significant improvement in the interfacial compatibility between PBAT/PLA and the modified calcium carbonate, and thus in a significant increase in the tensile strength and elongation at break of the article; examples 1-4 with the same amount of compatibilizer a added, the tensile strength of the article increased and then decreased with increasing amount of modified calcium carbonate, and the elongation at break gradually decreased. Therefore, the products of the examples 1 and 2 have the best comprehensive mechanical properties.
TABLE 1 mechanical property test results of the product
| Examples | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 |
| Tensile Strength (MPa) | 21.38 | 22.25 | 23.29 | 18.56 | 16.46 | 17.44 | 18.55 | 16.51 |
| Elongation at Break (%) | 498.83 | 458.23 | 380.96 | 191.48 | 430.16 | 414.25 | 352.71 | 179.58 |
(2) Influence of micro-morphology
FIG. 2 reflects the effect of examples 1-8 on the microtopography of PBAT/PLA blends of the addition of compatibilizer A and modified calcium carbonate to PBAT/PLA blends. Comparing FIGS. 2(a) and (e), (b) and (f), (c) and (g), (d) and (h), it can be seen that the compatibilizer A is not added, the boundary between the modified calcium carbonate particles and the PLA/PBAT blend is very distinct, indicating that the two have serious dispersion phase and extremely poor compatibility; the compatibilizer A is added, so that the compatibility of two phases is obvious, the holes left by the modified calcium carbonate and the PLA/PBAT are greatly reduced, and the interface is smooth. In FIGS. 2(a), (b), (c) and (d), when the same proportion of the compatibilizer A is added, the gradual deterioration of the microscopic appearance can be observed as the content of the modified calcium carbonate is increased. Therefore, the products of the example 1 and the example 2 have the best comprehensive performance.
The effects of the embodiment 1 and the embodiment 2 are optimal by integrating mechanical property analysis, micro-morphology influence and cost factors.
The present invention is illustrated by way of example and not by way of limitation. It will be apparent to those skilled in the art that other variations and modifications may be made in the foregoing disclosure without departing from the spirit or essential characteristics of all embodiments, and that all changes and modifications apparent from the above teachings are within the scope of the invention.
Claims (8)
1. A compatibilizer to increase the compatibility of PLA and PBAT, the compatibilizer component comprising: PLA75-98 parts by weight, maleic anhydride 1-10 parts by weight, dibenzoyl peroxide 0.1-1 parts by weight, main antioxidant 0.1-1 parts by weight, and auxiliary antioxidant 0.1-1 parts by weight, and the preparation method comprises the following steps:
s1: weighing BPO and MAH by an electronic balance according to a certain proportion, adding the BPO and the MAH into a beaker filled with 500mL of acetone, then placing the beaker in an ultrasonic cleaning machine for vibration dissolution for 30min, adding pure PLA particles into the mixed solution in the first step, uniformly mixing and drying;
s2: the compatibilizer graft A used in the invention is prepared by melt extrusion in a double-screw extruder, and is granulated and dried for standby, the temperature of each temperature zone of the extruder is set to be 165,175,185,185,185,175 ℃ respectively, and the rotating speed of the screw is set to be 100 r/min.
2. The PLA/PBAT high-filling full-biodegradable composite material is characterized by comprising 5-20 parts by weight of PLA, 40-60 parts by weight of PBAT, 30-45 parts by weight of calcium carbonate, 1-10 parts by weight of compatibilizer A, 0.5-2 parts by weight of coupling agent, 0.1-1 part by weight of lubricant and 0.1-1 part by weight of antioxidant, and the method for preparing the PLA/PBAT high-filling full-biodegradable composite material comprises the following steps:
s1, putting the polylactic acid and the polybutylene terephthalate-co-adipate into a blast oven or a vacuum oven according to the formula proportion for drying treatment, and drying for 4-12h at 75-85 ℃ to ensure that the water content of each component is less than or equal to 1000ppm for later use;
s2, putting the compatilizer A into a blast oven or a vacuum oven according to the formula proportion for drying treatment, and drying for 1-2h at 50-70 ℃ for later use;
s3, adding calcium carbonate into the drying and stirring machine according to the formula proportion, heating and dehydrating for 1-2h, measuring the water content, controlling the water content below 0.3%, setting the temperature at 110 ℃ and setting the rotating speed at 50 r/min. Then stirring for 10-20min at 50-60 ℃ under the condition of 15r/min, then sequentially adding a coupling agent, an antioxidant and a lubricant, and continuously stirring for 30min to prepare modified calcium carbonate;
s4, putting the dried PLA, PBAT and the compatilizer A into the modified calcium carbonate prepared in the step S3, adding the lubricant, and continuously stirring for 30min to obtain a PLA/PBAT and calcium carbonate blend;
and S5, carrying out twin-screw extrusion granulation on the blend to obtain the calcium carbonate filled PLA/PBAT particles.
3. The method of claim 2, wherein the compatibilizer is the compatibilizer A for increasing the compatibility of PLA/PBAT in claim 1.
4. The process according to claim 2, wherein the polylactic acid used has a melt index of 5 to 7g/min and the polybutylene terephthalate-CO-adipate has a melt index of 2.7 to 4.9 g/min.
5. The method as claimed in claim 2, wherein the calcium carbonate used has a fineness of 1000-2000 mesh.
6. The method of claim 2, wherein the coupling agent is one of aluminate, titanate, gamma-mercaptopropyltrimethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, or gamma-glycidoxypropyltrimethoxysilane.
7. The method according to claim 2, wherein the lubricant is one or more of stearic acid, calcium stearate, sodium stearate, zinc stearate, barium stearate, erucamide, oleamide, paraffin wax or polyethylene wax.
8. The method according to claim 2, wherein the primary antioxidant is one of hindered phenol antioxidant (2, 2-bis [ [3[3, 5-bis (1, 1-dimethylethyl) -4-hydroxyphenyl ] -1-oxopropoxy ] methyl ] -1, 3-propanediyl-3, 5-bis (1, 1-dimethylethyl) -4-hydroxyphenylpropionate) (1010), octadecanol β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate (1076) and 2-methylenebis (4-methyl-6-tert-butylphenol) (2246). The auxiliary antioxidant is one of phosphite ester antioxidant tris (2, 4-di-tert-butyl phenyl) phosphite (168), didodecanediol thiodipropionate (DLTDP) and distearyl thiodipropionate DSTDP.
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