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WO2020088214A1 - Pha-modified tps/pbat biodegradable resin and preparation method therefor - Google Patents

Pha-modified tps/pbat biodegradable resin and preparation method therefor Download PDF

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Publication number
WO2020088214A1
WO2020088214A1 PCT/CN2019/110721 CN2019110721W WO2020088214A1 WO 2020088214 A1 WO2020088214 A1 WO 2020088214A1 CN 2019110721 W CN2019110721 W CN 2019110721W WO 2020088214 A1 WO2020088214 A1 WO 2020088214A1
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Prior art keywords
tps
pha
pbat
biodegradable resin
modified
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Chinese (zh)
Inventor
王庭慰
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Nanjing Wurui Biodegradable New Material Research Institute Co Ltd
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Nanjing Wurui Biodegradable New Material Research Institute Co Ltd
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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
    • 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
    • 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
    • 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
    • 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

Definitions

  • the invention relates to a PHA modified TPS / PBAT biodegradable resin and a preparation method thereof, belonging to the field of degradable plastics.
  • Starch is a commonly used biodegradable material.
  • the starch undergoes chemical modification steps such as esterification, grafting, etc., which can transform the original starch into a thermoplastic starch resin (TPS).
  • TPS thermoplastic starch resin
  • PBAT is a copolymer of butanediol adipate and butylene terephthalate, which has the characteristics of PBA and PBT, and has both good ductility and elongation at break, as well as good heat resistance And impact performance; in addition, it also has excellent biodegradability, is currently very active in the research of biodegradable plastics and one of the best degradable materials in the market.
  • Blending TPS and PBAT can be used to prepare biodegradable membrane products.
  • the purpose of the present invention is to provide a PHA modified TPS / PBAT biodegradable resin, which can greatly improve the mechanical properties of the resin.
  • a PHA modified TPS / PBAT biodegradable resin prepared from the following parts by weight of raw materials:
  • it is prepared from the following parts by weight of raw materials: TPS 25 parts, PBAT 50 parts, PHA 25 parts.
  • the TPS is a granular material modified by thermoplastic starch, and the starch is modified to give it plasticity, that is, it has a certain fluidity (plasticity) when heated, and the starch is grafted on the starch during the modification. Intermediate so that it can be compatible with more materials and blended together. Its flow rate is 1-3g / 10min, melt index 190 °C / 2.16kg, density: 1.2g / cm 3 , and volatile matter ⁇ 0.3%.
  • the PBAT is a copolymer of butanediol adipate and butylene terephthalate, which is an aliphatic resin, which has the thermoplasticity of petrochemical plastic resin, and can be bio-processed in nature after being molded and used. Degradation, especially under composting conditions, its biodegradability is more obvious.
  • Typical products include BASF's Ecoflex, domestic Guangzhou Jinfa 1024, Zhejiang Xinfu 2003F, etc. The flow rate is 2-5g / 10min, the melt index is 190 °C / 2.16kg, and the density is 1.25g / cm 3
  • the PHA is a polyhydroxy fatty acid ester, which is an intracellular fat synthesized by many microorganisms, that is, materials are produced by changing biomass, fermentation and other processes through biomass materials.
  • Degradability and thermoplasticity of plastics can play a blending and compatibility role for TPS and PBAT. Colleagues can improve the mechanical properties of compatible materials.
  • Domestic manufacturers include Beijing Lanjing Technology Co., Ltd. and Ningbo Tianan Company in Zhejiang.
  • the invention also discloses a preparation method of the PHA modified TPS / PBAT biodegradable resin, and the steps include:
  • the co-rotating 1 48 twin screw with a diameter of 75mm can be used.
  • the processing temperature is 120-150 ° C
  • r is 200-220r / min
  • in zone 11 is Vacuum port, vacuum degree -0.08, die port pressure 3.5-4Mpa
  • the exit strip of the mixer is sent to the pelletizer with a conveyor belt, and air-cooled
  • the flow rate of the pelletized resin is 1-3g / 10min, 190 °C /2.16kg, density 1.23-1.25g / cm 3 , volatile matter ⁇ 0.3%.
  • TPS and PBAT when TPS and PBAT are blended and granulated, a certain amount of PHA is added for modification.
  • the starch in PHA and TPS and the ester in PBAT have good compatibility. Under the action of twin screw shearing, it can Uniformly combined with TPS and PBAT.
  • the mechanical properties of TPS / PBAT biodegradable resin can be greatly improved by more than 20%.
  • PHA is also a material produced by using natural plants as raw materials and using biological fermentation engineering technology, so it can greatly increase the biomass content in the blend and is easier to degrade.
  • PHA has very good thermal insulation and water barrier properties. When added to TPS / PBAT biodegradable resin, the water resistance of the film made is enhanced, and it can be applied to more products (such as sanitary products).
  • the PHA modified TPS / PBAT biodegradable resin is prepared from the following parts by weight of raw materials:
  • the resin is formed into a film by a blown film machine with a film thickness of 0.03mm. Its performance is tested according to GB / T1040.3, and the performance parameters are shown in Table 1.
  • the PHA modified TPS / PBAT biodegradable resin is prepared from the following parts by weight of raw materials:
  • the resin is formed into a film by a film blowing machine.
  • the thickness of the film is 0.03mm. Its performance is tested according to GB / T1040.3. See Table 2 for performance parameters.
  • the PHA modified TPS / PBAT biodegradable resin is prepared from the following parts by weight of raw materials:
  • the resin is formed into a film by a blown film machine with a film thickness of 0.03mm. Its performance is tested according to GB / T1040.3. See Table 3 for performance parameters.
  • TPS / PBAT biodegradable resin is prepared from the following parts by weight of raw materials:
  • the resin is formed into a film by a blown film machine with a film thickness of 0.03mm. Its performance is tested according to GB / T1040.3, and the performance parameters are shown in Table 1.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Biological Depolymerization Polymers (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

Disclosed is a PHA-modified TPS/PBAT biodegradable resin, comprising the following raw materials in parts by weight: TPS 10-30%; PBAT 20-50%; and PHA 1-30%. Also disclosed is a preparation method of the biodegradable resin. The method involves adding a certain amount of PHA to achieve modification during blending and pelleting TPS and PBAT. PHB is highly compatible with the starch in TPS and the ester in PBAT and can evenly combine with TPS and PBAT under the shearing action of a twin screw. With the addition of PHA, the resulting TPS/PBAT biodegradable resin improves substantially in mechanical properties, with an improvement of more than 20%. Further, as a material produced from natural plant materials by biofermentation processes, PHA can substantially increase the biomass content of the blend, allowing the blend to be more easily degradable. Moreover, as PHA has excellent thermal insulation and waterproof performance, increased water resistance is effected in a film prepared from the TPS/PBAT biodegradable resin added with PHA.

Description

PHA改性的TPS/PBAT可生物降解树脂及其制备方法PHA modified TPS / PBAT biodegradable resin and preparation method thereof 技术领域Technical field

本发明涉及一种PHA改性的TPS/PBAT可生物降解树脂及其制备方法，属于可降解塑料领域。The invention relates to a PHA modified TPS / PBAT biodegradable resin and a preparation method thereof, belonging to the field of degradable plastics.

背景技术Background technique

淀粉是常用的生物可降解材料，将淀粉经过酯化、接枝、等化学改性步骤，可使原淀粉转变成热塑性淀粉树脂(TPS)。Starch is a commonly used biodegradable material. The starch undergoes chemical modification steps such as esterification, grafting, etc., which can transform the original starch into a thermoplastic starch resin (TPS).

PBAT是己二酸丁二醇酯和对苯二甲酸丁二醇酯的共聚物，兼具PBA和PBT的特性，既有较好的延展性和断裂伸长率，也有较好的耐热性和冲击性能；此外，还具有优良的生物降解性，是目前生物降解塑料研究中非常活跃和市场应用最好降解材料之一。PBAT is a copolymer of butanediol adipate and butylene terephthalate, which has the characteristics of PBA and PBT, and has both good ductility and elongation at break, as well as good heat resistance And impact performance; in addition, it also has excellent biodegradability, is currently very active in the research of biodegradable plastics and one of the best degradable materials in the market.

将TPS和PBAT共混，可用于制备生物可降解的膜类制品。Blending TPS and PBAT can be used to prepare biodegradable membrane products.

发明内容Summary of the invention

本发明的目的在于提供一种PHA改性的TPS/PBAT可生物降解树脂，可大幅提高树脂的力学性能。The purpose of the present invention is to provide a PHA modified TPS / PBAT biodegradable resin, which can greatly improve the mechanical properties of the resin.

本发明的目的通过以下技术方案实现：The object of the present invention is achieved by the following technical solutions:

一种PHA改性的TPS/PBAT可生物降解树脂，由以下重量份的原料制备而成：A PHA modified TPS / PBAT biodegradable resin, prepared from the following parts by weight of raw materials:

TPS   10-30％TPS 10-30%

PBAT  20-50％PBAT 20-50%

PHA   1-30％。PHA 1-30%.

优选的，由以下重量份的原料制备而成：TPS 25份、PBAT 50份、PHA25份。Preferably, it is prepared from the following parts by weight of raw materials: TPS 25 parts, PBAT 50 parts, PHA 25 parts.

优选的，所述TPS是为热塑性淀粉改性后的颗粒状物质，将淀粉经过改性赋予它塑性，即在加热时它具有一定流动性(塑性)，在改性中给淀粉接枝上一定中间体，使之能与更多材料相容，共混一体。其流动速率在1-3g/10min，融熔指数190℃/2.16kg,密度：1.2g/cm 3，可挥发物<0.3％。 Preferably, the TPS is a granular material modified by thermoplastic starch, and the starch is modified to give it plasticity, that is, it has a certain fluidity (plasticity) when heated, and the starch is grafted on the starch during the modification. Intermediate so that it can be compatible with more materials and blended together. Its flow rate is 1-3g / 10min, melt index 190 ℃ / 2.16kg, density: 1.2g / cm 3 , and volatile matter <0.3%.

优选的，所述PBAT是己二酸丁二醇酯和对苯二甲酸丁二醇酯的共聚物，属脂肪族树脂，它即具备石化塑料树脂的热塑性，同时在成型使用后能在自然界生物降解，尤其在堆肥条件下，其生物降解性更明显。典型产品有BASF的Ecoflex和国产广州金发1024，浙江鑫富2003F等，其流动速率在2-5g/10min，融熔指数190℃/2.16kg，密度：1.25g/cm 3。 Preferably, the PBAT is a copolymer of butanediol adipate and butylene terephthalate, which is an aliphatic resin, which has the thermoplasticity of petrochemical plastic resin, and can be bio-processed in nature after being molded and used. Degradation, especially under composting conditions, its biodegradability is more obvious. Typical products include BASF's Ecoflex, domestic Guangzhou Jinfa 1024, Zhejiang Xinfu 2003F, etc. The flow rate is 2-5g / 10min, the melt index is 190 ℃ / 2.16kg, and the density is 1.25g / cm 3

所述PHA是聚羟基脂肪酸酯，是很多微生物合成的细胞内脂，即通过生物质材料改变菌种、发酵等过程生产材料，它的多样性表现在具有很好的生物相容性，生物可降解性和塑料的热塑性，对TPS和PBAT它能起到共混相容作用，同事能提高相容性材料力学性能，国内厂家有北京蓝晶科技有限公司，浙江宁波天安公司。The PHA is a polyhydroxy fatty acid ester, which is an intracellular fat synthesized by many microorganisms, that is, materials are produced by changing biomass, fermentation and other processes through biomass materials. Degradability and thermoplasticity of plastics can play a blending and compatibility role for TPS and PBAT. Colleagues can improve the mechanical properties of compatible materials. Domestic manufacturers include Beijing Lanjing Technology Co., Ltd. and Ningbo Tianan Company in Zhejiang.

本发明还公开了上述PHA改性的TPS/PBAT可生物降解树脂的制备方法，其步骤包括：The invention also discloses a preparation method of the PHA modified TPS / PBAT biodegradable resin, and the steps include:

将TPS、PHA和PBAT均匀混合后进入同向双螺杆中，可选用直径为75mm同向平行1:48双螺杆，加工℃为120-150℃，r为200-220r/min,在11区为真空口,真空度-0.08，模口压力3.5-4Mpa,混合机出模口拉条用传送带送至切粒机，并加以风冷，切粒树脂其流动速率在1-3g/10min,190℃/2.16kg,密度在1.23-1.25g/cm 3，可挥发物<0.3％。 Mix TPS, PHA and PBAT uniformly into the co-rotating twin screw. The co-rotating 1: 48 twin screw with a diameter of 75mm can be used. The processing temperature is 120-150 ° C, r is 200-220r / min, and in zone 11 is Vacuum port, vacuum degree -0.08, die port pressure 3.5-4Mpa, the exit strip of the mixer is sent to the pelletizer with a conveyor belt, and air-cooled, the flow rate of the pelletized resin is 1-3g / 10min, 190 ℃ /2.16kg, density 1.23-1.25g / cm 3 , volatile matter <0.3%.

本发明在TPS与PBAT共混造粒时，加入一定量的PHA改性，PHA与TPS中的淀粉以及PBAT中的酯类均有很好的相容性，在双螺杆剪切作用下，能与TPS和PBAT均匀结合。添加PHA后，TPS/PBAT可生物降解树脂的力学性能可大幅提高，提高幅度在20％以上。同时PHA也是以天然植物为原料，利用生物发酵工程技术生产出来的材料，故可以大幅提高共混物中生物质含量，更易于降解。而且PHA具有很好的保温和隔水性能，添加到TPS/PBAT可生物降解树脂后，制成的薄膜防水性增强，可适用更多产品采用(如卫生制品等)。In the present invention, when TPS and PBAT are blended and granulated, a certain amount of PHA is added for modification. The starch in PHA and TPS and the ester in PBAT have good compatibility. Under the action of twin screw shearing, it can Uniformly combined with TPS and PBAT. After the addition of PHA, the mechanical properties of TPS / PBAT biodegradable resin can be greatly improved by more than 20%. At the same time, PHA is also a material produced by using natural plants as raw materials and using biological fermentation engineering technology, so it can greatly increase the biomass content in the blend and is easier to degrade. Moreover, PHA has very good thermal insulation and water barrier properties. When added to TPS / PBAT biodegradable resin, the water resistance of the film made is enhanced, and it can be applied to more products (such as sanitary products).

具体实施方式detailed description

实施例1Example 1

本PHA改性的TPS/PBAT可生物降解树脂，由以下重量份的原料制备而成：The PHA modified TPS / PBAT biodegradable resin is prepared from the following parts by weight of raw materials:

TPS   24份TPS 24 copies

PBAT  56份PBAT 56 copies

PHA   20份。20 copies of PHA.

树脂经吹膜机成膜，膜厚度为0.03mm，按GB/T1040.3检测其性能，性能参数见表1。The resin is formed into a film by a blown film machine with a film thickness of 0.03mm. Its performance is tested according to GB / T1040.3, and the performance parameters are shown in Table 1.

表1：Table 1:

拉伸强度纵横平均Tensile strength vertical and horizontal average 断裂伸长率纵横平均Elongation at break 撕裂强度纵横平均Tear strength vertical and horizontal average 30Mpa30Mpa 400％400% 110N/15min110N / 15min

实施例2Example 2

本PHA改性的TPS/PBAT可生物降解树脂，由以下重量份的原料制备而成：The PHA modified TPS / PBAT biodegradable resin is prepared from the following parts by weight of raw materials:

TPS   18份TPS 18 copies

PBAT  42份42 copies of PBAT

PHA   40份。40 copies of PHA.

树脂经吹膜机成膜，膜厚度为:0.03mm，按GB/T1040.3检测其性能，性能参数见表2。The resin is formed into a film by a film blowing machine. The thickness of the film is 0.03mm. Its performance is tested according to GB / T1040.3. See Table 2 for performance parameters.

表2：Table 2:

拉伸强度纵横平均Tensile strength vertical and horizontal average 断裂伸长率纵横平均Elongation at break 撕裂强度纵横平均Tear strength vertical and horizontal average 35Mpa35Mpa 400％400% 120N/15min120N / 15min

实施例3Example 3

本PHA改性的TPS/PBAT可生物降解树脂，由以下重量份的原料制备而成：The PHA modified TPS / PBAT biodegradable resin is prepared from the following parts by weight of raw materials:

TPS   30份TPS 30 copies

PBAT  60份60 copies of PBAT

PHA   10份。10 copies of PHA.

树脂经吹膜机成膜，膜厚度为0.03mm，按GB/T1040.3检测其性能，性能参数见表3。The resin is formed into a film by a blown film machine with a film thickness of 0.03mm. Its performance is tested according to GB / T1040.3. See Table 3 for performance parameters.

表3：table 3:

拉伸强度纵横平均Tensile strength vertical and horizontal average 断裂伸长率纵横平均Elongation at break 撕裂强度纵横平均Tear strength vertical and horizontal average 27Mpa27Mpa 300％300% 95N/15min95N / 15min

对比例1Comparative Example 1

TPS/PBAT可生物降解树脂，由以下重量份的原料制备而成：TPS / PBAT biodegradable resin is prepared from the following parts by weight of raw materials:

TPS   30份TPS 30 copies

PBAT  70份70 copies of PBAT

树脂经吹膜机成膜，膜厚度为0.03mm，按GB/T1040.3检测其性能，性能参数见对比表1。The resin is formed into a film by a blown film machine with a film thickness of 0.03mm. Its performance is tested according to GB / T1040.3, and the performance parameters are shown in Table 1.

拉伸强度纵横平均Tensile strength vertical and horizontal average 断裂伸长率纵横平均Elongation at break 撕裂强度纵横平均Tear strength vertical and horizontal average 22Mpa22Mpa 350％350% 90N/15min90N / 15min

从以上实例1～3和对比例不难看出PHA加入TPS和PBAT中，对共混材料相容性有很大改善，突出表现在其力学性能随PHA加入和不加入比较以及PHA加入越多，其力学性能提高幅度越大，反映共混材料相容性越高，其他功能也有相应提高，不再一一叙述。It is not difficult to see from the above examples 1 to 3 and the comparative example that PHA is added to TPS and PBAT, which greatly improves the compatibility of the blended material. The greater the improvement of its mechanical properties, the higher the compatibility of the blended materials, and the corresponding improvement of other functions, which will not be described one by one.

Claims (5)

一种PHA改性的TPS/PBAT可生物降解树脂，由以下重量份的原料制备而成：A PHA modified TPS / PBAT biodegradable resin, prepared from the following parts by weight of raw materials: TPS   10-30％TPS 10-30% PBAT  20-50％PBAT 20-50% PHA   1-30％。PHA 1-30%. 根据权利要求1所述的PHA改性的TPS/PBAT可生物降解树脂，其特征在于：由以下重量份的原料制备而成：TPS 25份、PBAT 50份、PHA 25份。The PHA modified TPS / PBAT biodegradable resin according to claim 1, characterized in that it is prepared from the following parts by weight of raw materials: TPS 25 parts, PBAT 50 parts, PHA 25 parts. 根据权利要求2所述的PHA改性的TPS/PBAT可生物降解树脂，其特征在于：所述TPS为热塑性淀粉改性后颗粒状物质，其流动速率在1-3g/10min，融熔指数190℃/2.16kg,密度：1.2g/cm 3，可挥发物<0.3％。 The PHA modified TPS / PBAT biodegradable resin according to claim 2, characterized in that: the TPS is a granular material modified by thermoplastic starch, the flow rate is 1-3g / 10min, and the melt index is 190 ℃ / 2.16kg, density: 1.2g / cm 3 , volatile matter <0.3%. 根据权利要求3所述的PHA改性的TPS/PBAT可生物降解树脂，其特征在于：所述PBAT流动速率在2-5g/10min，融熔指数190℃,2.16kg，密度：1.25g/cm 3。 The PHA modified TPS / PBAT biodegradable resin according to claim 3, characterized in that the PBAT flow rate is 2-5g / 10min, the melt index is 190 ° C, 2.16kg, and the density is 1.25g / cm 3 . 一种PHA改性的TPS/PBAT可生物降解树脂的制备方法，其步骤包括：A preparation method of PHA modified TPS / PBAT biodegradable resin, the steps include: 将TPS、PHA和PBAT均匀混合后进入同向双螺杆中，可选用直径为75mm同向平行1:48双螺杆，加工℃为120-150℃，r为200-220r/min,在11区为真空口,真空度-0.08，模口压力3.5-4Mpa,混合机出模口拉条用传送带送至切粒机，并加以风冷，切粒树脂其流动速率在1-3g/10min,190℃/2.16kg,密度在1.23-1.25g/cm 3，可挥发物<0.3％。 Mix TPS, PHA and PBAT uniformly into the co-rotating twin screw. The co-rotating 1: 48 twin screw with a diameter of 75mm can be used. The processing temperature is 120-150 ° C, r is 200-220r / min, and in zone 11 is Vacuum port, vacuum degree -0.08, die port pressure 3.5-4Mpa, the exit strip of the mixer is sent to the pelletizer with a conveyor belt, and air-cooled, the flow rate of the pelletized resin is 1-3g / 10min, 190 ℃ /2.16kg, density 1.23-1.25g / cm 3 , volatile matter <0.3%.
PCT/CN2019/110721 2018-11-01 2019-10-12 Pha-modified tps/pbat biodegradable resin and preparation method therefor Ceased WO2020088214A1 (en)

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CN109504042A (en) * 2018-11-01 2019-03-22 南京五瑞生物降解新材料研究院有限公司 PHA modified TPS/PBAT biodegradable resin and preparation method thereof
CN111574815A (en) * 2020-05-25 2020-08-25 南京瑞鑫环保科技有限公司 PHA (polyhydroxyalkanoate) -modified PPC (polypropylene)/TPS (thermoplastic polystyrene) biodegradable resin and preparation method thereof
CN112812518A (en) * 2020-12-31 2021-05-18 重庆和泰润佳股份有限公司 Thermoplastic biodegradable plastic and preparation method thereof
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