WO2022213498A1 - Preparation method for biodegradable polyester chip - Google Patents

Preparation method for biodegradable polyester chip Download PDF

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Publication number
WO2022213498A1
WO2022213498A1 PCT/CN2021/104216 CN2021104216W WO2022213498A1 WO 2022213498 A1 WO2022213498 A1 WO 2022213498A1 CN 2021104216 W CN2021104216 W CN 2021104216W WO 2022213498 A1 WO2022213498 A1 WO 2022213498A1
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pressure
temperature
preparation
reactor
degrees celsius
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PCT/CN2021/104216
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French (fr)
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张新峰
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苏州楷儒新材料科技有限公司
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L67/00Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
    • C08L67/02Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G81/00Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L87/00Compositions of unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
    • C08L87/005Block or graft polymers not provided for in groups C08L1/00 - C08L85/04
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/06Biodegradable

Definitions

  • the invention relates to the technical field of polyester chips, in particular to a preparation method of biodegradable polyester chips.
  • the present invention proposes a preparation method of biodegradable polyester chips.
  • the preparation method of a kind of biodegradable polyester chips proposed by the present invention comprises the following steps:
  • Preliminary preparation two reactors with stirring function, temperature adjustment mechanism, pressure adjustment mechanism, data acquisition equipment, succinic acid, butanediol, polylactic acid, aliphatic-aromatic copolyester, inert gas inflation equipment , catalyst, the two reactors are connected by connecting pipes;
  • S2 Auxiliary mechanism connection: Next, connect the inert gas inflating equipment, the temperature regulating mechanism and the pressure regulating mechanism to the two reactors through the regulating pipe, and set the control mechanism to control the opening and closing of the regulating pipe. After the connection, check the gas of the relevant equipment. tightness;
  • S3 reactant preparation: add succinic acid and butanediol to one of the reaction kettles, the ratio of succinic acid and butanediol is 17:23, and the temperature adjustment mechanism is used to heat up the reaction kettle to make it at 180-220 Stir for 1.5-2.5 hours at degrees Celsius, then flush the inert gas into the reactor through the inert gas inflating device, raise the temperature in the reactor to 220-270 degrees Celsius, add catalyst, and increase the pressure in the reactor through the pressure regulating mechanism. Up to 800Pa, continue to stir for 3 hours, slowly reduce the pressure in the reactor until 300Pa, make succinic acid and 1.4 butanediol fully react;
  • the data collection device includes a temperature sensor, a pressure sensor, a computer and a data collector.
  • the biodegradable polyester chips formed by fully reacting and mixing succinic acid, butanediol, polylactic acid and aliphatic-aromatic copolyester have high degradation efficiency and no pollution after degradation.
  • Traditional polyester chips can greatly shorten the degradation time, relieve the pressure of polyester on the soil during the degradation process, and the degraded components will not pollute the soil, which is environmentally friendly and convenient, and has strong practicability.
  • Data acquisition equipment will prepare data, etc. Record and analyze, so as to obtain the most ideal preparation data, which is conducive to saving production resources and reducing production costs.
  • FIG. 1 is a schematic diagram of a preparation process of a preparation method of a biodegradable polyester chip proposed by the present invention.
  • Preliminary preparation two reactors with stirring function, temperature adjustment mechanism, pressure adjustment mechanism, data acquisition equipment, succinic acid, butanediol, polylactic acid, aliphatic-aromatic copolyester, inert gas inflation equipment , catalyst, the two reactors are connected by connecting pipes, and the connecting pipes should be equipped with control valves to open or close the connecting pipes;
  • S2 Auxiliary mechanism connection: Next, connect the inert gas inflating equipment, the temperature regulating mechanism and the pressure regulating mechanism to the two reactors through the regulating pipe, and set the control mechanism to control the opening and closing of the regulating pipe. After the connection, check the gas of the relevant equipment. tightness, to avoid equipment leakage during the preparation process affecting the preparation of polyester chips;
  • S3 reactant preparation: add succinic acid and butanediol to one of the reaction kettles, the ratio of succinic acid and butanediol is 17:23, and the temperature adjustment mechanism is used to heat up the reaction kettle to make it at 180-220 Stir for 1.5-2.5 hours at degrees Celsius, then flush the inert gas into the reactor through the inert gas inflating device, raise the temperature in the reactor to 220-270 degrees Celsius, add catalyst, and increase the pressure in the reactor through the pressure regulating mechanism. Up to 800Pa, continue to stir for 3 hours, slowly reduce the pressure in the reactor until 300Pa, make succinic acid and 1.4 butanediol fully react;
  • the data acquisition equipment includes a temperature sensor, a pressure sensor, a computer and a data collector.
  • the biodegradable polyester chips formed by fully reacting and mixing succinic acid, butanediol, polylactic acid and aliphatic-aromatic copolyester have high degradation efficiency and no pollution after degradation.
  • Traditional polyester chips can greatly shorten the degradation time, relieve the pressure of polyester on the soil during the degradation process, and the degraded components will not pollute the soil, which is environmentally friendly and convenient, and has strong practicability.
  • Data acquisition equipment will prepare data, etc. Record and analyze, so as to obtain the most ideal preparation data, which is conducive to saving production resources and reducing production costs.

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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)
  • Polyesters Or Polycarbonates (AREA)

Abstract

Disclosed is a preparation method for a biodegradable polyester chip, comprising the following steps: S1, preliminary preparation: two reactors having a stirring function, a temperature adjustment mechanism, a pressure adjustment mechanism, a data acquisition device, succinic acid, butanediol, polylactic acid, an aliphatic-aromatic copolyester, an inert gas inflating device, and a catalyst, the two reactors being connected by means of a connecting pipe; and S2, auxiliary mechanism connection: next, the inert gas inflating device, the temperature adjustment mechanism and the pressure adjustment mechanism are respectively connected to the two reactors by means of adjustment pipes. In the present invention, the biodegradable polyester chip is formed by fully reacting and mixing succinic acid, butanediol, polylactic acid and an aliphatic-aromatic copolyester. The degradation efficiency thereof is high, and no pollution is created after degradation, which can greatly shorten the degradation time and relieve the pressure of polyester on soil during degradation; in addition, the components after degradation do not pollute the soil, which environmentally friendly and convenient.

Description

一种生物可降解聚酯切片的制备方法A kind of preparation method of biodegradable polyester chips 技术领域technical field
本发明涉及聚酯切片技术领域,尤其涉及一种生物可降解聚酯切片的制备方法。 The invention relates to the technical field of polyester chips, in particular to a preparation method of biodegradable polyester chips.
背景技术Background technique
随着经济的发展和人民生活水平的不断提高,人口不断增加,生活垃圾的产量也日益增加,生活垃圾中的塑料,特别是一次性塑料包装材料、日用品和地膜废弃物等对环境的污染日益加重。对可生物降解塑料的研发迫在眉睫。With the development of the economy and the continuous improvement of people's living standards, the population continues to increase, and the output of domestic garbage is also increasing. The plastics in the domestic garbage, especially the disposable plastic packaging materials, daily necessities and plastic film waste, are increasingly polluting the environment. aggravated. The research and development of biodegradable plastics is imminent.
现有的绝大部分聚酯塑料材料均无法高效降解,当其被丢弃掩埋后,自然降解时间长,降解效率低,对土壤以及周围环境造成负担,同时无法降解的塑料凳占用大量土地,造成用地紧张。Most of the existing polyester plastic materials cannot be efficiently degraded. When they are discarded and buried, the natural degradation time is long, the degradation efficiency is low, and it is a burden to the soil and the surrounding environment. Tension in use.
技术解决方案technical solutions
基于背景技术存在的技术问题,本发明提出了一种生物可降解聚酯切片的制备方法。Based on the technical problems existing in the background art, the present invention proposes a preparation method of biodegradable polyester chips.
    本发明提出的一种生物可降解聚酯切片的制备方法,包括以下步骤:The preparation method of a kind of biodegradable polyester chips proposed by the present invention comprises the following steps:
S1:前期准备:两个具有搅拌功能的反应釜、温度调节机构、压力调节机构、数据采集设备、丁二酸、丁二醇、聚乳酸、脂肪族-芳香族共聚酯、惰性气体充气设备、催化剂,两个反应釜之间通过连接管道进行连接;S1: Preliminary preparation: two reactors with stirring function, temperature adjustment mechanism, pressure adjustment mechanism, data acquisition equipment, succinic acid, butanediol, polylactic acid, aliphatic-aromatic copolyester, inert gas inflation equipment , catalyst, the two reactors are connected by connecting pipes;
S2:辅助机构连接:接着将惰性气体充气设备、温度调节机构与压力调节机构分别与两个反应釜通过调节管道进行连接,并设置控制机构控制调节管道的开启与关闭,连接后检查相关设备气密性;S2: Auxiliary mechanism connection: Next, connect the inert gas inflating equipment, the temperature regulating mechanism and the pressure regulating mechanism to the two reactors through the regulating pipe, and set the control mechanism to control the opening and closing of the regulating pipe. After the connection, check the gas of the relevant equipment. tightness;
S3:反应物制备:将丁二酸与丁二醇加入其中一个反应釜中,丁二酸与丁二醇比例为17:23,通过温度调节机构对反应釜进行升温,使其在180-220摄氏度下搅拌1.5-2.5小时,接着通过惰性气体充气设备将惰性气体冲入反应釜中,将反应釜中温度升高至220-270摄氏度,并加入催化剂,通过压力调节机构将反应釜中压力升高至800Pa,继续搅拌3小时,缓慢降低反应釜内压力直至300Pa,使丁二酸与1.4丁二醇充分反应;S3: reactant preparation: add succinic acid and butanediol to one of the reaction kettles, the ratio of succinic acid and butanediol is 17:23, and the temperature adjustment mechanism is used to heat up the reaction kettle to make it at 180-220 Stir for 1.5-2.5 hours at degrees Celsius, then flush the inert gas into the reactor through the inert gas inflating device, raise the temperature in the reactor to 220-270 degrees Celsius, add catalyst, and increase the pressure in the reactor through the pressure regulating mechanism. Up to 800Pa, continue to stir for 3 hours, slowly reduce the pressure in the reactor until 300Pa, make succinic acid and 1.4 butanediol fully react;
S4:反应物制备:将聚乳酸、脂肪族-芳香族共聚酯加入另外一个反应釜中,聚乳酸、脂肪族-芳香族共聚酯比例为3:1.1,通过温度调节机构缓慢对反应釜进行升温,同时通过压力调节机构将反应釜内部压力提升至300Pa,使其在50-80摄氏度下搅拌1-1.5小时,接着同样通过惰性气体充气设备将惰性气体冲入反应釜中,将反应釜中温度降低至40-60摄氏度,并加入催化剂,继续搅拌3小时,搅拌过程中将反应釜中压力缓慢降低至100Pa,使聚乳酸、脂肪族-芳香族共聚酯充分反应;S4: Preparation of reactants: add polylactic acid and aliphatic-aromatic copolyester to another reaction kettle, and the ratio of polylactic acid and aliphatic-aromatic copolyester is 3:1.1. The temperature is raised, and the internal pressure of the reactor is raised to 300Pa through the pressure regulating mechanism, and it is stirred at 50-80 degrees Celsius for 1-1.5 hours. The medium temperature is lowered to 40-60 degrees Celsius, and a catalyst is added, and stirring is continued for 3 hours. During the stirring process, the pressure in the reactor is slowly reduced to 100 Pa, so that the polylactic acid and the aliphatic-aromatic copolyester are fully reacted;
S5:反应物混合:当两个反应釜中混合物完全融合后,打开两个反应釜之间的连接管道,两个反应釜中的混合物逐渐混合,当混合物全部汇聚到一个反应釜中后,通过温度了解机构将反应釜温度控制在160-200摄氏度之间,通过压力调节机构将反应釜中压力控制在400Pa,搅拌2-4小时,使混合物完全混合;S5: Mixing of reactants: When the mixtures in the two reaction kettles are completely fused, open the connecting pipeline between the two reaction kettles, and the mixtures in the two reaction kettles are gradually mixed. The temperature understanding mechanism controls the temperature of the reaction kettle between 160-200 degrees Celsius, and controls the pressure in the reaction kettle at 400Pa through the pressure regulating mechanism, and stirs for 2-4 hours to completely mix the mixture;
S6:聚酯物冷却成型:当混合物完全混合后,通过温度调节机构将反应釜中的温度缓慢降低至30摄氏度,使聚酯物冷却成型,成型后进行切片,数据采集设备将制备过程中的数据进行记录,通过研究分析从而得到可降解聚酯切片制备的最优方案,有利于节约生产资源,降低生产成本。S6: Cooling and molding of polyester material: When the mixture is completely mixed, the temperature in the reaction kettle is slowly lowered to 30 degrees Celsius by a temperature adjustment mechanism, so that the polyester material is cooled and formed, and sliced after forming. The data is recorded, and the optimal plan for the preparation of degradable polyester chips is obtained through research and analysis, which is conducive to saving production resources and reducing production costs.
优选地,所述数据采集设备包括温度传感器、压力传感器、计算机以及数据采集器。Preferably, the data collection device includes a temperature sensor, a pressure sensor, a computer and a data collector.
有益效果beneficial effect
本发明中,通过丁二酸、丁二醇、聚乳酸、脂肪族-芳香族共聚酯充分反应混合形成的生物可降解聚酯切片,其降解效率高,且降解后无污染,相比于传统聚酯切片,能大大缩短降解时间,缓解聚酯物对降解过程中对于土壤的压力,且降解后的成分不会对土壤造成污染,环保便捷,实用性强,数据采集设备将制备数据等进行记录并加以分析,从而得到最理想的制备数据,有利于节约生产资源,降低生产成本。In the present invention, the biodegradable polyester chips formed by fully reacting and mixing succinic acid, butanediol, polylactic acid and aliphatic-aromatic copolyester have high degradation efficiency and no pollution after degradation. Traditional polyester chips can greatly shorten the degradation time, relieve the pressure of polyester on the soil during the degradation process, and the degraded components will not pollute the soil, which is environmentally friendly and convenient, and has strong practicability. Data acquisition equipment will prepare data, etc. Record and analyze, so as to obtain the most ideal preparation data, which is conducive to saving production resources and reducing production costs.
附图说明Description of drawings
图1为本发明提出的一种生物可降解聚酯切片的制备方法的制备流程示意图。FIG. 1 is a schematic diagram of a preparation process of a preparation method of a biodegradable polyester chip proposed by the present invention.
本发明的实施方式Embodiments of the present invention
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, but not all of the embodiments.
参照图1,一种生物可降解聚酯切片的制备方法,包括以下步骤:1, a preparation method of biodegradable polyester chips, comprising the following steps:
S1:前期准备:两个具有搅拌功能的反应釜、温度调节机构、压力调节机构、数据采集设备、丁二酸、丁二醇、聚乳酸、脂肪族-芳香族共聚酯、惰性气体充气设备、催化剂,两个反应釜之间通过连接管道进行连接,且连接管道应设置有控制阀用以开启或关闭连接管道;S1: Preliminary preparation: two reactors with stirring function, temperature adjustment mechanism, pressure adjustment mechanism, data acquisition equipment, succinic acid, butanediol, polylactic acid, aliphatic-aromatic copolyester, inert gas inflation equipment , catalyst, the two reactors are connected by connecting pipes, and the connecting pipes should be equipped with control valves to open or close the connecting pipes;
S2:辅助机构连接:接着将惰性气体充气设备、温度调节机构与压力调节机构分别与两个反应釜通过调节管道进行连接,并设置控制机构控制调节管道的开启与关闭,连接后检查相关设备气密性,避免制备过程中设备漏气影响聚酯切片的制备;S2: Auxiliary mechanism connection: Next, connect the inert gas inflating equipment, the temperature regulating mechanism and the pressure regulating mechanism to the two reactors through the regulating pipe, and set the control mechanism to control the opening and closing of the regulating pipe. After the connection, check the gas of the relevant equipment. tightness, to avoid equipment leakage during the preparation process affecting the preparation of polyester chips;
S3:反应物制备:将丁二酸与丁二醇加入其中一个反应釜中,丁二酸与丁二醇比例为17:23,通过温度调节机构对反应釜进行升温,使其在180-220摄氏度下搅拌1.5-2.5小时,接着通过惰性气体充气设备将惰性气体冲入反应釜中,将反应釜中温度升高至220-270摄氏度,并加入催化剂,通过压力调节机构将反应釜中压力升高至800Pa,继续搅拌3小时,缓慢降低反应釜内压力直至300Pa,使丁二酸与1.4丁二醇充分反应;S3: reactant preparation: add succinic acid and butanediol to one of the reaction kettles, the ratio of succinic acid and butanediol is 17:23, and the temperature adjustment mechanism is used to heat up the reaction kettle to make it at 180-220 Stir for 1.5-2.5 hours at degrees Celsius, then flush the inert gas into the reactor through the inert gas inflating device, raise the temperature in the reactor to 220-270 degrees Celsius, add catalyst, and increase the pressure in the reactor through the pressure regulating mechanism. Up to 800Pa, continue to stir for 3 hours, slowly reduce the pressure in the reactor until 300Pa, make succinic acid and 1.4 butanediol fully react;
S4:反应物制备:将聚乳酸、脂肪族-芳香族共聚酯加入另外一个反应釜中,聚乳酸、脂肪族-芳香族共聚酯比例为3:1.1,通过温度调节机构缓慢对反应釜进行升温,同时通过压力调节机构将反应釜内部压力提升至300Pa,使其在50-80摄氏度下搅拌1-1.5小时,接着同样通过惰性气体充气设备将惰性气体冲入反应釜中,将反应釜中温度降低至40-60摄氏度,并加入催化剂,继续搅拌3小时,搅拌过程中将反应釜中压力缓慢降低至100Pa,使聚乳酸、脂肪族-芳香族共聚酯充分反应;S4: Preparation of reactants: add polylactic acid and aliphatic-aromatic copolyester to another reaction kettle, and the ratio of polylactic acid and aliphatic-aromatic copolyester is 3:1.1. The temperature is raised, and the internal pressure of the reactor is raised to 300Pa through the pressure regulating mechanism, and it is stirred at 50-80 degrees Celsius for 1-1.5 hours. The medium temperature is lowered to 40-60 degrees Celsius, and a catalyst is added, and stirring is continued for 3 hours. During the stirring process, the pressure in the reactor is slowly reduced to 100 Pa, so that the polylactic acid and the aliphatic-aromatic copolyester are fully reacted;
S5:反应物混合:通过数据采集设备实时采集两个反应釜内部混合物状态变化,当两个反应釜中混合物完全融合后,打开两个反应釜之间的连接管道,两个反应釜中的混合物逐渐混合,当混合物全部汇聚到一个反应釜中后,关闭反应釜之间的连接管道,通过温度了解机构将反应釜温度控制在160-200摄氏度之间,通过压力调节机构将反应釜中压力控制在400Pa,搅拌2-4小时,使混合物完全混合;S5: Mixing of reactants: real-time acquisition of the state changes of the mixtures in the two reactors through the data acquisition device. When the mixtures in the two reactors are completely fused, open the connecting pipeline between the two reactors, and the mixture Gradually mix, when the mixture is all gathered into one reactor, close the connecting pipes between the reactors, control the temperature of the reactor between 160-200 degrees Celsius through the temperature understanding mechanism, and control the pressure in the reactor through the pressure regulating mechanism. At 400Pa, stir for 2-4 hours to fully mix the mixture;
S6:聚酯物冷却成型:当混合物完全混合后,通过温度调节机构将反应釜中的温度缓慢降低至30摄氏度,使聚酯物冷却成型,成型后进行切片,数据采集设备将制备过程中的数据进行记录,通过研究分析从而得到可降解聚酯切片制备的最优方案,有利于节约生产资源,降低生产成本,所述数据采集设备包括温度传感器、压力传感器、计算机以及数据采集器。S6: Cooling and molding of polyester material: When the mixture is completely mixed, the temperature in the reaction kettle is slowly lowered to 30 degrees Celsius by a temperature adjustment mechanism, so that the polyester material is cooled and formed, and sliced after forming. The data is recorded, and the optimal plan for the preparation of degradable polyester chips is obtained through research and analysis, which is conducive to saving production resources and reducing production costs. The data acquisition equipment includes a temperature sensor, a pressure sensor, a computer and a data collector.
本发明中,通过丁二酸、丁二醇、聚乳酸、脂肪族-芳香族共聚酯充分反应混合形成的生物可降解聚酯切片,其降解效率高,且降解后无污染,相比于传统聚酯切片,能大大缩短降解时间,缓解聚酯物对降解过程中对于土壤的压力,且降解后的成分不会对土壤造成污染,环保便捷,实用性强,数据采集设备将制备数据等进行记录并加以分析,从而得到最理想的制备数据,有利于节约生产资源,降低生产成本。In the present invention, the biodegradable polyester chips formed by fully reacting and mixing succinic acid, butanediol, polylactic acid and aliphatic-aromatic copolyester have high degradation efficiency and no pollution after degradation. Traditional polyester chips can greatly shorten the degradation time, relieve the pressure of polyester on the soil during the degradation process, and the degraded components will not pollute the soil, which is environmentally friendly and convenient, and has strong practicability. Data acquisition equipment will prepare data, etc. Record and analyze, so as to obtain the most ideal preparation data, which is conducive to saving production resources and reducing production costs.
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。The above description is only a preferred embodiment of the present invention, but the protection scope of the present invention is not limited to this. The equivalent replacement or change of the inventive concept thereof shall be included within the protection scope of the present invention.

Claims (2)

1、一种生物可降解聚酯切片的制备方法,其特征在于,包括以下步骤:1, a preparation method of biodegradable polyester chips, is characterized in that, comprises the following steps:
S1:前期准备:两个具有搅拌功能的反应釜、温度调节机构、压力调节机构、数据采集设备、丁二酸、丁二醇、聚乳酸、脂肪族-芳香族共聚酯、惰性气体充气设备、催化剂,两个反应釜之间通过连接管道进行连接;S1: Preliminary preparation: two reactors with stirring function, temperature adjustment mechanism, pressure adjustment mechanism, data acquisition equipment, succinic acid, butanediol, polylactic acid, aliphatic-aromatic copolyester, inert gas inflation equipment , catalyst, the two reactors are connected by connecting pipes;
S2:辅助机构连接:接着将惰性气体充气设备、温度调节机构与压力调节机构分别与两个反应釜通过调节管道进行连接,并设置控制机构控制调节管道的开启与关闭,连接后检查相关设备气密性;S2: Auxiliary mechanism connection: Next, connect the inert gas inflating equipment, the temperature regulating mechanism and the pressure regulating mechanism to the two reactors through the regulating pipe, and set the control mechanism to control the opening and closing of the regulating pipe. After the connection, check the gas of the relevant equipment. tightness;
S3:反应物制备:将丁二酸与丁二醇加入其中一个反应釜中,丁二酸与丁二醇比例为17:23,通过温度调节机构对反应釜进行升温,使其在180-220摄氏度下搅拌1.5-2.5小时,接着通过惰性气体充气设备将惰性气体冲入反应釜中,将反应釜中温度升高至220-270摄氏度,并加入催化剂,通过压力调节机构将反应釜中压力升高至800Pa,继续搅拌3小时,缓慢降低反应釜内压力直至300Pa,使丁二酸与1.4丁二醇充分反应;S3: reactant preparation: add succinic acid and butanediol to one of the reaction kettles, the ratio of succinic acid and butanediol is 17:23, and the temperature adjustment mechanism is used to heat up the reaction kettle to make it at 180-220 Stir for 1.5-2.5 hours at degrees Celsius, then flush the inert gas into the reactor through the inert gas inflating device, raise the temperature in the reactor to 220-270 degrees Celsius, add catalyst, and increase the pressure in the reactor through the pressure regulating mechanism. Up to 800Pa, continue to stir for 3 hours, slowly reduce the pressure in the reactor until 300Pa, make succinic acid and 1.4 butanediol fully react;
S4:反应物制备:将聚乳酸、脂肪族-芳香族共聚酯加入另外一个反应釜中,聚乳酸、脂肪族-芳香族共聚酯比例为3:1.1,通过温度调节机构缓慢对反应釜进行升温,同时通过压力调节机构将反应釜内部压力提升至300Pa,使其在50-80摄氏度下搅拌1-1.5小时,接着同样通过惰性气体充气设备将惰性气体冲入反应釜中,将反应釜中温度降低至40-60摄氏度,并加入催化剂,继续搅拌3小时,搅拌过程中将反应釜中压力缓慢降低至100Pa,使聚乳酸、脂肪族-芳香族共聚酯充分反应;S4: Preparation of reactants: add polylactic acid and aliphatic-aromatic copolyester to another reaction kettle, and the ratio of polylactic acid and aliphatic-aromatic copolyester is 3:1.1. The temperature is raised, and the internal pressure of the reactor is raised to 300Pa through the pressure regulating mechanism, and it is stirred at 50-80 degrees Celsius for 1-1.5 hours. The medium temperature is lowered to 40-60 degrees Celsius, and a catalyst is added, and stirring is continued for 3 hours. During the stirring process, the pressure in the reactor is slowly reduced to 100 Pa, so that the polylactic acid and the aliphatic-aromatic copolyester are fully reacted;
S5:反应物混合:当两个反应釜中混合物完全融合后,打开两个反应釜之间的连接管道,两个反应釜中的混合物逐渐混合,当混合物全部汇聚到一个反应釜中后,通过温度了解机构将反应釜温度控制在160-200摄氏度之间,通过压力调节机构将反应釜中压力控制在400Pa,搅拌2-4小时,使混合物完全混合;S5: Mixing of reactants: When the mixtures in the two reaction kettles are completely fused, open the connecting pipeline between the two reaction kettles, and the mixtures in the two reaction kettles are gradually mixed. The temperature understanding mechanism controls the temperature of the reaction kettle between 160-200 degrees Celsius, and controls the pressure in the reaction kettle at 400Pa through the pressure regulating mechanism, and stirs for 2-4 hours to completely mix the mixture;
S6:聚酯物冷却成型:当混合物完全混合后,通过温度调节机构将反应釜中的温度缓慢降低至30摄氏度,使聚酯物冷却成型,成型后进行切片,数据采集设备将制备过程中的数据进行记录,通过研究分析从而得到可降解聚酯切片制备的最优方案,有利于节约生产资源,降低生产成本。S6: Cooling and molding of polyester material: When the mixture is completely mixed, the temperature in the reaction kettle is slowly lowered to 30 degrees Celsius by a temperature adjustment mechanism, so that the polyester material is cooled and formed, and sliced after forming. The data is recorded, and the optimal plan for the preparation of degradable polyester chips is obtained through research and analysis, which is conducive to saving production resources and reducing production costs.
根据权利要求1所述的一种生物可降解聚酯切片的制备方法,其特征在于,所述数据采集设备包括温度传感器、压力传感器、计算机以及数据采集器。The method for preparing a biodegradable polyester chip according to claim 1, wherein the data acquisition device comprises a temperature sensor, a pressure sensor, a computer and a data acquisition device.
PCT/CN2021/104216 2021-04-08 2021-07-02 Preparation method for biodegradable polyester chip WO2022213498A1 (en)

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