CN115160742A - PBAT composite material and preparation method thereof - Google Patents
PBAT composite material and preparation method thereof Download PDFInfo
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- CN115160742A CN115160742A CN202210816853.7A CN202210816853A CN115160742A CN 115160742 A CN115160742 A CN 115160742A CN 202210816853 A CN202210816853 A CN 202210816853A CN 115160742 A CN115160742 A CN 115160742A
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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
- 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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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Abstract
The invention discloses a PBAT composite material and a preparation method thereof, wherein the PBAT composite material comprises the following raw materials in parts by weight: 70-100 parts of PBAT, 10-20 parts of polyglycolide, 7-30 parts of modified aliphatic polyester, 0.5-4 parts of compatibilizer, 1-3 parts of heat-resistant agent and 0.8-2 parts of antibacterial agent. According to the invention, the PBAT is taken as a main raw material to endow the composite material with excellent biodegradability, the viscosity, the elongation at break and the spinnability of the composite material are improved by adding polyglycolide, the compatibility, the heat-resistant stability and the processability of the composite material can be improved by modifying aliphatic polyester, the heat-resistant performance and the antibacterial performance of the composite material are improved by adding a heat-resistant agent and an antibacterial agent, and the interface adhesion is improved by adding a compatilizer, so that the PBAT composite material which has the advantages of good processability, high mechanical property, strong stability, bacteria resistance and environmental protection is obtained.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a PBAT composite material and a preparation method thereof.
Background
In recent years, the development of environmentally friendly biodegradable polymers has attracted much attention due to the demand for reducing the amount of accumulated plastic waste in the environment. Aliphatic polyester is a common biodegradable material, has good biodegradability in natural environment, but has defects in performance, processing and the like, such as lower thermal stability and mechanical property. The aromatic polyester has higher mechanical strength and thermal stability due to the existence of a rigid group of benzene ring, but the biodegradation performance is poor. Among them, poly adipic acid/butylene terephthalate (PBAT) is considered as an ideal substitute for non-degradable high molecular materials such as polyethylene due to its good molecular flexibility and biodegradability, and a biodegradable composite material developed by using PBAT as a substrate has become one of effective ways to solve white pollution, but PBAT at the present stage also generally has the defects of poor barrier property, poor processability, high viscosity, poor weather resistance and the like. Thus, in order to enable rapid penetration of the degradable material into various application areas. The composite material obtained by compounding two or more high molecular polyesters with different characteristics makes up respective defects to balance the performance and has good degradation performance, so that the composite material with degradability replaces the traditional non-degradable raw material. The method has great practical significance for improving the environment, saving mineral resources and realizing eco-friendly green sustainable development.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provide a PBAT composite material and a preparation method thereof, wherein the PBAT composite material has the characteristics of good processability, high mechanical property, strong heat-resistant stability, antibiosis and environmental protection.
The purpose of the invention is realized by the following technical scheme: a PBAT composite material comprises the following raw materials in parts by weight:
in the invention, the PBAT is adopted as a main raw material, and the PBAT composite material is prepared by adding polyglycolide, modified aliphatic polyester, a compatibilizer, a heat-resistant agent and an antibacterial agent, has good mechanical property, high elongation at break, good heat resistance and antibacterial property, and has a wider hot processing window and good spinnability. Wherein, the viscosity, the elongation at break and the spinnability of a reaction system are improved by adding polyglycolide, and the heat resistance stability and the degradability of the PBAT composite material are effectively improved; the compatibility and the processing performance of the composite material can be improved by modifying the aliphatic polyester; the compatibility among PBAT, polyglycolide and modified aliphatic polyester can be effectively improved by adding the compatibilizer, and the interface adhesion is improved; the heat-resistant stability and the processing performance of the composite material are improved by adding the heat-resistant agent; the composite material has certain antibacterial effect by adding the antibacterial agent.
Further, the compatibilizer is at least one of 4,4 '-diphenylmethane diisocyanate, 2' - (1, 3-phenylene) -bisoxazoline (PBO), 2-1, 3-phenylene-Bisoxazoline (BOZ), polyvinyl acetate, or epoxy cage polysilsesquioxane.
Further, the heat-resistant agent is at least one of lanthanum phenylphosphonate, cerium phenylphosphonate or magnesium phosphate.
Further, the antibacterial agent is at least one of chitosan, rutin or curcumin.
Further, the preparation method of the polyglycolide comprises the following steps: adding glycolide, 1, 4-butanediol, pentaerythritol and stannous octoate into a reaction kettle, inflating nitrogen, raising the temperature of the reaction kettle to 100-120 ℃, maintaining for 20-30min, raising the temperature to 170-180 ℃, and reacting for 2-4h to obtain the polyglycolide.
Further, the inherent viscosity of the polyglycolide is 0.65 to 0.75 eta/(dg/L).
In the invention, the polyglycolide prepared by the preparation method has good mechanical property and thermal stability, the intrinsic viscosity of the polyglycolide can be in the range of 0.65-0.75 eta/(dg/L), and the composite polyglycolide and PBAT can obviously improve the problems of high viscosity, mechanical property and heat resistance of the PBAT. Meanwhile, the compatibility and the degradation rate of the PBAT composite material are obviously improved by adding polyglycolide.
Further, the preparation of the modified aliphatic polyester comprises the following steps:
s1, adding a small amount of glycol into a reaction kettle, then adding terephthalic acid, glycol, glycolide and a catalyst in parts by weight, stirring for a period of time, and introducing nitrogen;
s2, raising the temperature to 160-190 ℃ for reaction for 1-4h, raising the temperature to 220-240 ℃ for esterification for 2-4h, then continuing raising the temperature to 240-260 ℃, adjusting the pressure to 80-100kPa and keeping for 40-60min, adjusting the pressure to-100 kPa and the temperature to 260-270 ℃ for continuous reaction until the reaction is finished, and obtaining the modified aliphatic polyester.
Further, in the step S1, the mass ratio of terephthalic acid, ethylene glycol, glycolide and the catalyst is 30-50:35-70:15-30:1-5.
Further, in step S1, the catalyst is at least one of stannous 2-ethyl hexanoate, stannous octoate or stannic lactate.
Further, the modified aliphatic polyester has a number average molecular weight of 7000 to 20000g/mol.
The preparation reaction mode of the modified aliphatic polyester is as follows:
the modified aliphatic polyester prepared by the preparation steps has good compatibility and processability, and the processing window of the composite material is effectively widened by adding the modified aliphatic polyester.
The invention provides a preparation method of a PBAT composite material, which comprises the following steps:
drying the obtained PBAT, polyglycolide and modified aliphatic polyester in an oven at 70-80 ℃ for 8-12h;
weighing the dried PBAT, polyglycolide, modified aliphatic polyester, compatibilizer, heat-resistant agent and antibacterial agent in proportion, and uniformly mixing in a high-speed mixer;
transferring the material obtained in the step (2) to a double-screw extruder for injection molding and extrusion, cooling and then slicing to obtain the PBAT composite material.
The invention has the beneficial effects that: the PBAT composite material is prepared by taking PBAT as a main raw material and adding polyglycolide, modified aliphatic polyester, a compatibilizer, a heat-resistant agent and an antibacterial agent. Wherein, the viscosity, the elongation at break and the spinnability of a reaction system are improved by adding polyglycolide, and the heat resistance stability and the degradability of the PBAT composite material are effectively improved; the compatibility and the processing performance of the composite material can be improved by modifying the aliphatic polyester. The PBAT composite material disclosed by the invention has good processing performance, heat-resistant stability and antibacterial property when being used for melt spinning, and the obtained fiber has excellent mechanical property.
Detailed Description
The present invention will be further described with reference to the following examples, which are not intended to limit the scope of the present invention.
Example 1
The PBAT composite material of this example comprises the following raw materials in parts by weight:
further, the compatibilizer is 4, 4' -diphenylmethane diisocyanate.
Further, the heat-resistant agent is magnesium phosphate.
Further, the antibacterial agent is chitosan.
Further, the preparation method of the polyglycolide comprises the following steps: adding glycolide, 1, 4-butanediol, pentaerythritol and stannous octoate into a reaction kettle, inflating nitrogen, raising the temperature of the reaction kettle to 100 ℃, maintaining for 20min, raising the temperature to 170 ℃, and reacting for 3h to obtain the polyglycolide.
Further, the preparation of the modified aliphatic polyester comprises the following steps:
s1, coating a small amount of glycol in a reaction kettle, then adding terephthalic acid, glycol, glycolide and a catalyst in parts by weight, stirring for a period of time, and introducing nitrogen;
and S2, raising the temperature to 160 ℃ for reaction for 2h, raising the temperature to 220 ℃ for esterification for 2h, then continuing raising the temperature to 240 ℃, adjusting the pressure to be 80kPa for 40min, and adjusting the pressure to be-100 kPa and the temperature to be 260 ℃ for continuous reaction until the reaction is finished, thus obtaining the modified aliphatic polyester.
Further, in step S1, the mass ratio of terephthalic acid, ethylene glycol, glycolide, and the catalyst is 30:40:15:0.2.
further, in step S1, the catalyst is stannous octoate.
The preparation method of the PBAT composite material of this embodiment includes the following steps:
(1) Drying the obtained PBAT, polyglycolide and modified aliphatic polyester in an oven pool at 70 ℃ for 8h;
(2) Weighing the dried PBAT, polyglycolide, modified aliphatic polyester, compatibilizer, heat-resistant agent and antibacterial agent in proportion, placing the mixture into a high-speed stirrer, and uniformly mixing;
(3) Transferring the material obtained in the step (2) to a double-screw extruder for injection molding and extrusion, cooling and then slicing to obtain the PBAT composite material.
Example 2
The PBAT composite material of this example comprises the following raw materials in parts by weight:
further, the compatibilizer is 2, 2-bis (1, 3-phenylene) bisoxazoline.
Further, the heat-resistant agent is cerium phenylphosphonate.
Further, the antibacterial agent is curcumin.
Further, the preparation method of the polyglycolide comprises the following steps: adding glycolide, 1, 4-butanediol, pentaerythritol and stannous octoate into a reaction kettle, inflating nitrogen, raising the temperature of the reaction kettle to 110 ℃, maintaining for 20min, raising the temperature to 170 ℃, and reacting for 3h to obtain the polyglycolide.
Further, the preparation of the modified aliphatic polyester comprises the following steps:
s1, coating a small amount of glycol in a reaction kettle, then adding terephthalic acid, glycol, glycolide and a catalyst in parts by weight, stirring for a period of time, and introducing nitrogen;
and S2, raising the temperature to 170 ℃ for reaction for 3h, raising the temperature to 230 ℃ for esterification for 3h, then continuing raising the temperature to 250 ℃, adjusting the pressure to 80kPa for 50min, and adjusting the pressure to-100 kPa and the temperature to 260 ℃ for continuous reaction until the reaction is finished, thus obtaining the modified aliphatic polyester.
Further, in step S1, the mass ratio of terephthalic acid, ethylene glycol, glycolide, and the catalyst is 40:50:20:0.4.
further, in step S1, the catalyst is tin lactate.
The preparation method of the PBAT composite material of this embodiment includes the following steps:
(1) Drying the PBAT, the polyglycolide and the modified aliphatic polyester in an oven pool at 80 ℃ for 10 hours;
(2) Weighing the dried PBAT, polyglycolide, modified aliphatic polyester, compatibilizer, heat-resistant agent and antibacterial agent in proportion, and uniformly mixing in a high-speed mixer;
(3) Transferring the material obtained in the step (2) to a double-screw extruder for injection molding and extrusion, cooling and then slicing to obtain the PBAT composite material.
Example 3
The PBAT composite material of this example comprises the following raw materials in parts by weight:
further, the compatibilizer is 2,2' - (1, 3-phenylene) -bisoxazoline.
Further, the heat-resistant agent is lanthanum phenylphosphonate.
Further, the antibacterial agent is rutin.
Further, the preparation method of the polyglycolide comprises the following steps: adding glycolide, 1, 4-butanediol, pentaerythritol and stannous octoate into a reaction kettle, inflating nitrogen, raising the temperature of the reaction kettle to 115 ℃, maintaining for 30min, raising the temperature to 175 ℃, and reacting for 3h to obtain the polyglycolide.
Further, the preparation of the modified aliphatic polyester comprises the following steps:
s1, coating a small amount of glycol in a reaction kettle, then adding terephthalic acid, glycol, glycolide and a catalyst in parts by weight, stirring for a period of time, and introducing nitrogen;
and S2, raising the temperature to 180 ℃ for reaction for 3h, raising the temperature to 230 ℃ for esterification for 3h, then continuing raising the temperature to 250 ℃, adjusting the pressure to be 90kPa for 50min, and adjusting the pressure to be-100 kPa and the temperature to be 265 ℃ for continuing reaction until the end, thus obtaining the modified aliphatic polyester.
Further, in step S1, the mass ratio of terephthalic acid, ethylene glycol, glycolide, and the catalyst is 40:60:25:0.3.
further, in step S1, the catalyst is at least one of stannous 2-ethyl hexanoate, stannous octoate or stannic lactate.
The preparation method of the PBAT composite material of the embodiment includes the following steps:
(1) Drying the obtained PBAT, polyglycolide and modified aliphatic polyester in an oven pool at 80 ℃ for 10h;
(2) Weighing the dried PBAT, polyglycolide, modified aliphatic polyester, compatibilizer, heat-resistant agent and antibacterial agent in proportion, and uniformly mixing in a high-speed mixer;
(3) Transferring the material obtained in the step (2) to a double-screw extruder for injection molding and extrusion, cooling and then slicing to obtain the PBAT composite material.
Example 4
The PBAT composite material of this example comprises the following raw materials in parts by weight:
further, the compatibilizer is polyvinyl acetate.
Further, the heat-resistant agent is phenylphosphonic acid.
Further, the antibacterial agent is chitosan.
Further, the preparation method of the polyglycolide comprises the following steps: adding glycolide, 1, 4-butanediol, pentaerythritol and stannous octoate into a reaction kettle, inflating nitrogen, raising the temperature of the reaction kettle to 120 ℃, maintaining for 30min, raising the temperature to 180 ℃, and reacting for 4h to obtain the polyglycolide.
Further, the preparation of the modified aliphatic polyester comprises the following steps:
s1, coating a small amount of glycol in a reaction kettle, then adding terephthalic acid, glycol, glycolide and a catalyst in parts by weight, stirring for a period of time, and introducing nitrogen;
and S2, raising the temperature to 190 ℃ for reaction for 3h, raising the temperature to 240 ℃ for esterification for 3h, then continuing raising the temperature to 260 ℃, adjusting the pressure to be 100kPa for 40min, and adjusting the pressure to be-100 kPa and the temperature to be 270 ℃ for continuing reaction until the reaction is finished, thus obtaining the modified aliphatic polyester.
Further, in step S1, the mass ratio of terephthalic acid, ethylene glycol, glycolide, and the catalyst is 50:68:22:0.4.
further, in step S1, the catalyst is stannous 2-ethylhexanoate.
The preparation method of the PBAT composite material of the embodiment includes the following steps:
(1) Drying the obtained PBAT, polyglycolide and modified aliphatic polyester in an oven at 70-80 ℃ for 8-12h;
(2) Weighing the dried PBAT, polyglycolide, modified aliphatic polyester, compatibilizer, heat-resistant agent and antibacterial agent in proportion, placing the mixture into a high-speed stirrer, and uniformly mixing;
(3) Transferring the material obtained in the step (2) to a double-screw extruder for injection molding and extrusion, cooling and slicing to obtain the PBAT composite material.
Comparative example 1
The comparative example differs from example 2 in that: the raw materials of the PBAT composite material described in this comparative example do not contain modified aliphatic polyester.
The remainder of this comparative example was the same as example 2 and will not be described in detail here.
Comparative example 2
This comparative example differs from example 2 in that: the raw materials of the PBAT composite material described in this comparative example did not contain polyglycolide.
The remainder of this comparative example was the same as example 2 and will not be described in detail here.
Comparative example 3
This comparative example differs from example 2 in that: the raw materials of the PBAT composite material described in this comparative example do not contain polyglycolide and modified aliphatic polyester.
The remainder of this comparative example was the same as example 2 and will not be described again here.
The PBAT composites prepared in examples 1-4 and comparative examples 1-3 described above were subjected to vicat softening temperature testing according to ASTM D648. In addition, the fiber fineness and the mechanical strength of the slices prepared in the examples and the comparative examples are tested after the melt spinning operation is carried out on the slices by using a composite spinning machine (6-hole spinneret plate, the diameter of a spinneret orifice is 1 mm), the fiber fineness is tested by using GB/T14343-1993 standard, and the fiber mechanical strength is tested by using GB/T14344-2008 standard. Each set of experiments was run in triplicate and the data averaged, and the results of the tests for examples 1-4 and comparative examples 1-3 are shown in the table below.
From the data in the table above, the vicat softening temperature of the PBAT composite materials prepared in examples 1 to 4 is much higher than that of comparative examples 1 to 3, which shows that the PBAT composite materials have good heat stability, and the tensile strength and elongation at break of the PBAT composite materials prepared in examples 1 to 4 are higher than those of comparative examples 1 to 3, which shows that the PBAT composite materials have good tensile strength and elongation at break. According to the PBAT composite material, the PBAT is used as a main raw material, and polyglycolide, modified aliphatic polyester, a compatibilizer, a heat-resistant agent and an antibacterial agent are added to prepare the PBAT composite material, and the PBAT composite material has the advantages of good mechanical property, high elongation at break, good heat-resistant property and antibacterial property, wide thermal processing window and good spinnability.
The above specific examples are further illustrative of the technical solutions and advantages of the present invention, and are not intended to limit the embodiments. It will be apparent to those skilled in the art that any obvious alternative is within the scope of the invention without departing from the inventive concept.
Claims (10)
1. A PBAT composite characterized by: the feed comprises the following raw materials in parts by weight:
2. the PBAT composite of claim 1, in which: the compatibilizer is at least one of 4,4 '-diphenylmethane diisocyanate, 2' - (1, 3-phenylene) -bisoxazoline (PBO), 2-oxazoline (BOZ) (1, 3-phenylene), polyvinyl acetate or epoxy cage polysilsesquioxane.
3. The PBAT composite of claim 1, in which: the heat-resistant agent is at least one of lanthanum phenylphosphonate, cerium phenylphosphonate or magnesium phosphate.
4. The PBAT composite of claim 1, in which: the antibacterial agent is at least one of chitosan, rutin or curcumin.
5. The PBAT composite of claim 1, in which: the inherent viscosity of the polyglycolide is 0.65-0.75 eta/(dg/L).
6. The PBAT composite of claim 1, in which: the preparation of the modified aliphatic polyester comprises the following steps:
s1, coating ethylene glycol in a reaction kettle, adding terephthalic acid, ethylene glycol, glycolide and a catalyst in parts by weight, stirring for a period of time, and introducing nitrogen;
s2, raising the temperature to 160-190 ℃ for reaction for 1-4h, raising the temperature to 220-240 ℃ for esterification for 2-4h, then continuing raising the temperature to 240-260 ℃, adjusting the pressure to 80-100kPa and keeping for 40-60min, adjusting the pressure to-100 kPa and the temperature to 260-270 ℃ for continuous reaction until the reaction is finished, and obtaining the modified aliphatic polyester.
7. The PBAT composite of claim 6, characterized in that: in step S1, the mass ratio of terephthalic acid, ethylene glycol, glycolide and the catalyst is 30-50:35-70:15-30:0.1-0.5.
8. The PBAT composite of claim 6, characterized in that: in step S1, the catalyst is at least one of stannous 2-ethyl hexanoate, stannous octoate or stannic lactate.
9. A PBAT composite material according to claim 6, characterized in that: the number average molecular weight of the modified aliphatic polyester is 7000-20000g/mol.
10. The method of preparing a PBAT composite material of any of claims 1-9, wherein: the method comprises the following steps:
(1) Drying the obtained PBAT, polyglycolide and modified aliphatic polyester in an oven at 70-80 ℃ for 8-12h;
(2) Weighing the dried PBAT, polyglycolide, modified aliphatic polyester, compatibilizer, heat-resistant agent and antibacterial agent in proportion, and uniformly mixing in a high-speed mixer;
(3) Transferring the material obtained in the step (2) to a double-screw extruder for injection molding and extrusion, cooling and slicing to obtain the PBAT composite material.
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2022
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