WO2022127120A1 - Nouveau pbat hautement chargé en amidon et procédé de préparation associé - Google Patents

Nouveau pbat hautement chargé en amidon et procédé de préparation associé Download PDF

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WO2022127120A1
WO2022127120A1 PCT/CN2021/109213 CN2021109213W WO2022127120A1 WO 2022127120 A1 WO2022127120 A1 WO 2022127120A1 CN 2021109213 W CN2021109213 W CN 2021109213W WO 2022127120 A1 WO2022127120 A1 WO 2022127120A1
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parts
starch
pbat
novel high
filled
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PCT/CN2021/109213
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English (en)
Chinese (zh)
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涂丹
陈敏
王加浙
陈思松
陈思汕
蔡盛赢
陈盛介
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浙江世博新材料股份有限公司
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Publication of WO2022127120A1 publication Critical patent/WO2022127120A1/fr

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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
    • C08L3/00—Compositions of starch, amylose or amylopectin or of their derivatives or degradation products
    • C08L3/04—Starch derivatives, e.g. crosslinked derivatives
    • C08L3/06—Esters
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • 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
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/262—Alkali metal carbonates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
    • C08K2003/3045—Sulfates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • 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
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
    • Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics

Definitions

  • the invention belongs to the technical field of PBAT material preparation, and in particular relates to a novel high-starch filled PBAT and a preparation method thereof.
  • PBAT is a thermoplastic biodegradable plastic, which is a copolymer of butylene adipate and butylene terephthalate. It has both the characteristics of PBA and PBT, and has good ductility and elongation at break. Good heat resistance and impact performance; in addition, it also has excellent biodegradability, which is very active in the research of biodegradable plastics and one of the best biodegradable materials in the market.
  • the existing PBAT material has the problems of low tensile strength and Vicat softening temperature, high preparation cost, and cannot be blown alone.
  • Starch is an important natural biodegradable material polymer. As a renewable natural resource, it has the advantages of low cost and extensive sources. However, there are a large number of intramolecular and intermolecular invitations in the starch, the structure is complex, and most of them exist in the state of granules, which cannot be directly thermoplastically processed. Therefore, it is necessary to improve the process so that the modified starch can be thermoplastically processed, which has become a new research trend.
  • the invention provides a novel high-starch-filled PBAT and a preparation method thereof.
  • the starch is made into gel to solve the problems of dispersion and compatibility of the starch, and the proportion of starch can be greatly increased, while the consumption of the base material PBAT can be reduced. Reduce the cost of materials, accelerate biodegradation, protect the ecological environment, and save energy.
  • a new type of high starch filled PBAT including the following raw materials: PBAT, starch gel, silane coupling agent KH550, cross-linking agent, compatibilizer, starch modifier, antioxidant, erucamide, PE wax, polytetrafluoroethylene Vinyl fluoride micropowder, nucleating agent, nano barium sulfate;
  • the weight ratio of the PBAT, starch gel, silane coupling agent KH550, crosslinking agent and compatibilizer is (30-45): (50-60): (1-3): (2-4): ( 4-10).
  • the weight ratio of the PBAT, starch gel, silane coupling agent KH550, crosslinking agent, and compatibilizer is 40:55:2:3:8.
  • novel high starch filling PBAT in parts by weight, includes the following raw materials: 30-45 parts of PBAT, 50-60 parts of starch gel, 1-3 parts of silane coupling agent KH550, 2-3 parts of cross-linking agent 4 parts, 4-10 parts of compatibilizer, 5-10 parts of starch modifier, 1-2 parts of antioxidant, 2-5 parts of erucamide, 2-5 parts of PE wax, 5- 10 parts, 2-5 parts of nucleating agent, 5-10 parts of nano barium sulfate.
  • the novel high starch filling PBAT in parts by weight, includes the following raw materials: 40 parts of PBAT, 55 parts of starch gel, 2 parts of silane coupling agent KH550, 3 parts of crosslinking agent, 8 parts of compatibilizer , 8 parts of starch modifier, 1.6 parts of antioxidant, 4 parts of erucamide, 3 parts of PE wax, 7 parts of polytetrafluoroethylene micropowder, 3 parts of nucleating agent, and 8 parts of nano barium sulfate.
  • the starch gel in parts by weight, includes the following raw materials: 70-80 parts of edible starch, 20-30 parts of edible glycerin, 10-15 parts of citric acid, and 20-30 parts of sodium carbonate.
  • starch gel is prepared according to the following process: 20-30 parts by weight of edible glycerin and 10-15 parts of citric acid are mixed uniformly at a temperature of 50-60 ° C, and then 70-80 parts of edible starch are added , stir for 1-1.5h to make it evenly dispersed, stir at 650-850r/min speed for 10-30min, then add 20-30 parts of sodium carbonate to adjust the pH to 6.0-7.0, then heat up to 80-100°C, keep the temperature for 0.5- After 1.0 h, it was taken out and cooled to room temperature to obtain starch gel.
  • the edible starch includes one or more of edible corn starch, sweet potato flour, and mung bean flour.
  • the antioxidant includes one or both of antioxidant 1010 and antioxidant 168.
  • the present invention also provides a kind of preparation method of novel high starch filling PBAT, comprises the following steps:
  • the starch gel, starch modifier and coupling agent KH550 are pretreated in a high-speed mixer, and then PBAT, compatibilizer, and nano-barium sulfate are added to mix evenly, and then cross-linking agent, nucleating agent, and antioxidant are added.
  • PBAT compatibilizer
  • nano-barium sulfate are added to mix evenly
  • cross-linking agent nucleating agent, and antioxidant are added.
  • the screw length-diameter ratio of the twin-screw extruder is 35-48:1, and the temperature of melt blending is 160-180°C.
  • Glycerol of the present invention and sodium carbonate play a synergistic role in the preparation of novel high starch filled PBAT, and synergistically improve the tensile strength and Vicat softening temperature of novel high starch filled PBAT, this is because: in the preparation of starch gel Among them, citric acid is a tricarboxylic acid, which can form acid anhydride under heating and then undergo an esterification reaction with the hydroxyl groups on starch molecules to generate citric acid starch ester, which is cross-linked, thereby improving the water resistance of starch; while a certain amount of glycerol It can increase the mobility of starch molecular chain and promote the esterification reaction. In addition, adding sodium carbonate to obtain good gelatinity of starch gel, and then cooperate with glycerin to improve the tensile strength and Vicat softening temperature of new high starch filled PBAT.
  • the present invention lacks starch gel in the raw material for preparing the novel high starch filling PBAT, which has a great impact on the performance of the novel high starch filling PBAT.
  • the gelatinized starch can form a certain elasticity and strength
  • the translucent gel of PBAT, starch gel is a multi-dimensional network structure formed by the interconnection of starch molecules, which can be better added and dispersed in the substrate of the material, thereby improving the tensile strength and Vicat softening temperature of PBAT;
  • the starch gel prepared by the invention has good compatibility with PBAT, no starch powder layer, extremely high filling ratio and no bridging phenomenon, which can greatly reduce the cost of materials, accelerate biodegradation, protect the ecological environment, and save energy. .
  • the tensile strength and Vicat softening temperature of the novel high starch-filled PBAT prepared by the present invention are significantly higher than those of the PBAT prepared by the prior art, and the novel The high starch-filled PBAT can be blown alone, but the PBAT prepared by the prior art cannot be blown alone.
  • the number of days required for the complete degradation of the novel high-starch-filled PBAT prepared by the present invention is no more than 90 days, which is far less than that of the prior art.
  • the number of days required for complete degradation of the obtained PBAT (180 days), and the cost of the novel high-starch-filled PBAT prepared by the present invention is far lower than the cost of the PBAT prepared by the prior art, and the economic benefit is good.
  • the novel high starch filled PBAT in parts by weight, includes the following raw materials: 30-45 parts of PBAT, 50-60 parts of starch gel, 1-3 parts of silane coupling agent KH550, cross-linking agent 2-4 parts, 4-10 parts of compatibilizer, 5-10 parts of starch modifier, 1-2 parts of antioxidant, 2-5 parts of erucamide, 2-5 parts of PE wax, PTFE powder 5-10 parts, 2-5 parts of nucleating agent, 5-10 parts of nano barium sulfate, and the antioxidant includes one or both of antioxidant 1010 and antioxidant 168;
  • the starch gel is prepared according to the following process: 20-30 parts by weight of edible glycerin and 10-15 parts of citric acid are mixed uniformly at a temperature of 50-60° C., and then 70-80 parts of edible starch are added.
  • Edible starch includes one or more of edible corn starch, sweet potato powder, mung bean powder, stir for 1-1.5h to make it evenly dispersed, stir at 650-850r/min speed for 10-30min, and then add 20-30 parts of sodium carbonate Adjust pH to 6.0-7.0, then heat up to 80-100°C, keep warm for 0.5-1.0h, take out, and cool to room temperature to obtain starch gel;
  • the preparation method of described novel high starch filling PBAT comprises the following steps:
  • the starch gel, starch modifier and coupling agent KH550 are pretreated in a high-speed mixer at 80 °C, and then PBAT, compatibilizer, and nano-barium sulfate are added to mix evenly, and then cross-linking agent, nucleating agent, Antioxidant, erucamide, PE wax, polytetrafluoroethylene micropowder, and finally melt extruded, stretched, air-cooled and granulated by a twin-screw extruder to obtain a new type of high-starch filled PBAT.
  • the twin-screw extruder The length-diameter ratio of the screw coming out of the machine is 35-48:1, and the temperature of melt blending is 160-180°C.
  • a novel high starch-filled PBAT in parts by weight, includes the following raw materials: 32 parts of PBAT, 50 parts of starch gel, 5501 parts of silane coupling agent, 2 parts of cross-linking agent, 5 parts of compatibilizer, and starch modifier 6 parts, 10101 parts of antioxidant, 2 parts of erucamide, 2 parts of PE wax, 5 parts of polytetrafluoroethylene micropowder, 2 parts of nucleating agent, 6 parts of nano barium sulfate;
  • the starch gel was prepared according to the following process: 22 parts by weight of edible glycerin and 11 parts of citric acid were mixed uniformly at a temperature of 50° C., then 70 parts of corn starch were added, and stirred for 1.5 hours to make it uniformly dispersed, Stir at 650r/min for 30min, then add 20 parts of sodium carbonate to adjust pH to 6.9, then heat up to 83°C, keep warm for 0.9h, take out, cool to room temperature to obtain starch gel;
  • the preparation method of described novel high starch filling PBAT comprises the following steps:
  • the starch gel, starch modifier and coupling agent KH550 are pretreated in a high-speed mixer at 80 °C, and then PBAT, compatibilizer, and nano-barium sulfate are added to mix evenly, and then cross-linking agent, nucleating agent, Antioxidant, erucamide, PE wax, polytetrafluoroethylene micropowder, and finally melt extruded, stretched, air-cooled and granulated by a twin-screw extruder to obtain a new type of high-starch filled PBAT.
  • the twin-screw extruder The length-diameter ratio of the screw exiting the machine was 37:1, and the temperature of melt blending was 164°C.
  • a novel high starch-filled PBAT in parts by weight, includes the following raw materials: 40 parts of PBAT, 55 parts of starch gel, 5502 parts of silane coupling agent, 3 parts of cross-linking agent, 8 parts of compatibilizer, and starch modifier 8 parts, 1681.6 parts of antioxidant, 4 parts of erucamide, 3 parts of PE wax, 7 parts of polytetrafluoroethylene micropowder, 3 parts of nucleating agent, 8 parts of nano barium sulfate;
  • the starch gel is prepared according to the following process: 26 parts by weight of edible glycerin and 13 parts of citric acid are mixed uniformly at a temperature of 54° C., then 75 parts of sweet potato powder are added, and stirred for 1.3 hours to make it evenly dispersed, and then the starch gel is uniformly dispersed. Stir at 800r/min for 13min, then add 26 parts of sodium carbonate to adjust pH to 6.4, then heat up to 92°C, keep warm for 0.7h, take out, cool to room temperature to obtain starch gel;
  • the preparation method of described novel high starch filling PBAT comprises the following steps:
  • the starch gel, starch modifier and coupling agent KH550 are pretreated in a high-speed mixer at 80 °C, and then PBAT, compatibilizer, and nano-barium sulfate are added to mix evenly, and then cross-linking agent, nucleating agent, Antioxidant, erucamide, PE wax, polytetrafluoroethylene micropowder, and finally melt extruded, stretched, air-cooled and granulated by a twin-screw extruder to obtain a new type of high-starch filled PBAT.
  • the twin-screw extruder The length-diameter ratio of the screw exiting the machine was 42:1, and the melt-blending temperature was 175°C.
  • a novel high-starch-filled PBAT in parts by weight, includes the following raw materials: 44 parts of PBAT, 58 parts of starch gel, 3 parts of silane coupling agent KH550, 4 parts of cross-linking agent, 9 parts of compatibilizer, starch modified 9 parts of antioxidants, 2 parts of antioxidants, 5 parts of erucamide, 4 parts of PE wax, 10 parts of polytetrafluoroethylene micropowder, 5 parts of nucleating agent, and 10 parts of nano barium sulfate;
  • the starch gel is prepared according to the following process: 28 parts by weight of edible glycerin and 14 parts of citric acid are mixed uniformly at a temperature of 58° C., then 79 parts of mung bean powder are added, and stirred for 1.1 h to make it uniformly dispersed, and then placed Stir at 700r/min for 18min, then add 30 parts of sodium carbonate to adjust pH to 6.2, then heat up to 87°C, keep warm for 0.8h, take out, cool to room temperature to obtain starch gel;
  • the preparation method of described novel high starch filling PBAT comprises the following steps:
  • the starch gel, starch modifier and coupling agent KH550 are pretreated in a high-speed mixer at 80 °C, and then PBAT, compatibilizer, and nano-barium sulfate are added to mix evenly, and then cross-linking agent, nucleating agent, Antioxidant, erucamide, PE wax, polytetrafluoroethylene micropowder, and finally melt extruded, stretched, air-cooled and granulated by a twin-screw extruder to obtain a new type of high-starch filled PBAT.
  • the twin-screw extruder The length-diameter ratio of the screw exiting the machine was 46:1, and the melt-blending temperature was 178°C.
  • the preparation process is basically the same as that of Example 2, the only difference is that starch gel is lacking in the raw material for preparing the novel high-starch-filled PBAT.
  • the preparation process is basically the same as that of Example 2, the only difference is that glycerin and sodium carbonate are lacking in the raw starch gel for preparing the novel high-starch-filled PBAT.
  • the preparation process is basically the same as that of Example 2, the only difference is that the raw starch gel for preparing the novel high-starch-filled PBAT lacks glycerin.
  • the preparation process is basically the same as that of Example 2, the only difference is that sodium carbonate is lacking in the raw starch gel for preparing the novel high-starch-filled PBAT.
  • the PBAT products of Examples 1-3 and Comparative Examples 1-5 were tested for various indicators, and whether the film could be blown alone was tested, and the cost was calculated.
  • the test results obtained were as follows, wherein the tensile strength was tested by GB/T 1040.1; Vicat softening point temperature was tested by ISO 306; degradation performance was tested by GB/T19277.1-2011.
  • the number of days required for the complete degradation of the new high-starch-filled PBAT prepared in Examples 1-3 is no more than 90 days, which is far less than the required number of days for the complete degradation of the PBAT prepared in Comparative Example 5 (prior art). Days (need 180 days), in addition the cost of the novel high starch filling PBAT that embodiment 1-3 makes is far lower than the PBAT cost that comparative example 5 (prior art) makes; It can be seen from the data of embodiment 1-3 simultaneously, Embodiment 2 is the best embodiment.
  • starch gel is lacking in the raw material for preparing novel high starch filling PBAT, which has a great influence on the performance of novel high starch filling PBAT, this is because: paste
  • the transformed starch can form a translucent gel with certain elasticity and strength.
  • Starch gel is a multi-dimensional network structure formed by the interconnection of starch molecules. Tensile strength of PBAT, Vicat softening temperature.
  • Example 1 From the data of Example 1 and Comparative Examples 2-4, it can be seen that glycerin and sodium carbonate play a synergistic role in the preparation of novel high starch filled PBAT, and synergistically improve the tensile strength and Vicat softening of novel high starch filled PBAT Temperature, this is because: in the preparation of starch gel, citric acid is a tricarboxylic acid, which can form acid anhydride under heating and then undergo esterification with the hydroxyl group on the starch molecule to generate citric acid starch ester, which is in a cross-linked state.
  • citric acid is a tricarboxylic acid, which can form acid anhydride under heating and then undergo esterification with the hydroxyl group on the starch molecule to generate citric acid starch ester, which is in a cross-linked state.
  • glycerol can increase the mobility of starch molecular chains, promote esterification, and add sodium carbonate to obtain good gelatinity of starch gel, and then synergize with glycerol to improve the new high starch filling PBAT. Tensile strength, Vicat softening temperature.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

L'invention concerne un nouveau PBAT hautement charge en amidon et un procédé de préparation associé. Le PBAT comprend les matières premières suivantes : du PBAT, du gel d'amidon, un agent de couplage au silane KH550, un agent de réticulation, un agent de compatibilité, un modificateur d'amidon, un antioxydant, de l'érucamide, une cire de PE, une poudre de polytétrafluoroéthylène, un agent de nucléation et du sulfate de baryum nanométrique ; et le PBAT est formé au moyen de la préparation d'un matériau principal, de la préparation d'un matériau modifié, puis du mélange du matériau principal, du matériau modifié, de l'agent de compatibilité et du sulfate de baryum nanométrique, puis par chauffage, plastification, extrusion, calandrage et d'autres étapes. La résistance à la traction et la température de ramollissement Vicat du nouveau PBAT hautement chargé en amidon préparé sont respectivement significativement supérieures à la résistance à la traction et à la température de ramollissement Vicat du PBAT préparé selon l'état de la technique et le film peut être formé individuellement par soufflage. En outre, la vitesse de dégradation est rapide et les coûts sont faibles, ce qui présente d'excellents avantages économiques.
PCT/CN2021/109213 2020-12-16 2021-08-12 Nouveau pbat hautement chargé en amidon et procédé de préparation associé WO2022127120A1 (fr)

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CN202011487895.8A CN112625304B (zh) 2020-12-16 2020-12-16 一种高淀粉填充pbat材料及其制备方法

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GARCIA PATRÍCIA SALOMÃO, GROSSMANN MARIA VICTÓRIA EIRAS, SHIRAI MARIANNE AYUMI, LAZARETTI MARCELA MARTA, YAMASHITA FABIO, MULLER C: "Improving action of citric acid as compatibiliser in starch/polyester blown films", INDUSTRIAL CROPS AND PRODUCTS, vol. 52, 1 January 2014 (2014-01-01), NL , pages 305 - 312, XP055944433, ISSN: 0926-6690, DOI: 10.1016/j.indcrop.2013.11.001 *

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