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A multistage polymerization method for the preparation of polylactic acid by ring-opening polymerization of lactide

A polymerization method, ring-opening polymerization technology, applied in the field of polymer material synthesis, can solve the problems of air tightness or uneven mass and heat transfer, difficult to control the stability of conditions, unstable quality of final products, etc., and achieve short reaction time , easy to control, good sealing effect

Active Publication Date: 2017-07-04
杭州聚丰新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

If it contains a dynamic stirring device, it is very easy to cause the problems of air tightness or uneven mass and heat transfer as mentioned above; Too many transfer pumps and pipelines are required between each reactor, which further increases energy consumption and investment. In addition, more reactors and auxiliary equipment are more difficult to control the stability of conditions, and long reaction time will easily lead to unstable quality of final products. , is not an economical choice in industry

Method used

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  • A multistage polymerization method for the preparation of polylactic acid by ring-opening polymerization of lactide
  • A multistage polymerization method for the preparation of polylactic acid by ring-opening polymerization of lactide

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Experimental program
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Embodiment 1

[0057] In this embodiment, the ring type static mixing reaction device such as figure 1 As shown, it is a reaction device composed of two static mixers. In the figure, 1 is a plunger metering pump, 2 is a check valve, 3 is a pressure gauge, 4 is a melt delivery pump, 5 is a static mixer, and 6 is a sampling The number of valves and discharge ports, the number of corrugated plate type mixing units in the static mixer is 30, and the corrugated plates have 9 layers in total. The radial direction between the corrugated plates and the mixer is 70°, and the angle between the top angle of the corrugated plates is 30°. The static mixers are all 500mm in length and 14mm in inner diameter. Be that the mass fraction is 95%, optical purity is 98% L-lactide and composite catalyst (composite catalyst quality is 0.05% of L-lactide, catalyst zinc powder and cocatalyst ethylene glycol molar ratio are 1:0.1 ) into the ring-type static mixing reaction device, the antioxidant is antioxidant-24, ...

Embodiment 2

[0059] In this embodiment, a ring-type static mixing reaction device consisting of 3 static mixers is used. The number of corrugated plate-type mixing units in the static mixer is 10, and the corrugated plates have 4 layers. The radial direction of the corrugated plates and the mixer is 5°, the included angle of corrugated plate top angle is 170°. The static mixers are all 500mm in length and 16mm in inner diameter. Be that 96% by mass fraction, optical purity be 98% L-lactide and composite catalyst (composite catalyst quality is 0.5% of L-lactide, catalyst tin powder and cocatalyst dodecanol mol ratio are 1: 3) Adding to the ring type static mixing reaction device, the antioxidant is Antioxidant-24, and the added amount is 0.03% of the mass of L-lactide. The mixing temperature in the first stage is 100°C, the flow rate of the reaction system is 1mm / s, and the shear rate is 1s -1 , the number of cycles in the reaction device is 5. In the second stage, the polymerization tem...

Embodiment 3

[0061] In this embodiment, a ring-type static mixing reaction device consisting of 4 static mixers is used. The number of corrugated plate-type mixing units in the static mixer is 15, and the corrugated plates have 7 layers. The radial direction of the corrugated plates and the mixer is 45°, the included angle of corrugated plate top angle is 30°. The static mixers are all 500mm in length and 18mm in inner diameter. Be that 97% by mass fraction, optical purity be 98% L-lactide and composite catalyst (composite catalyst quality is 0.7% of L-lactide, catalyst zinc oxide and cocatalyst tridecyl alcohol mol ratio are 1: 3) Adding to the ring type static mixing reaction device, the antioxidant is antioxidant-24, and the added amount is 0.05% of the mass of lactide. The mixing temperature in the first stage is 100°C, the flow rate of the reaction system is 5mm / s, and the shear rate is 40s -1 , the number of cycles in the reaction device is 8. In the second stage, the polymerizati...

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Abstract

The present invention discloses a multi-stage polymerization method for polylactic acid preparation by ring-opening polymerization of lactide, the method is as follows: molten L-lactide and a composite catalyst system are fully mixed in a ring-type static mixing reaction device comprising a corrugated plate type static mixer, the reaction device temperature is raised for initial ring-opening polymerization, then the reaction device temperature is further raised for L-polylactic acid preparation. According to the multi-stage polymerization method, by adjusting of temperature and reaction time of different stages and adjusting of reaction system flow rate and shear rate, high optical purity and molecular weight polylactic acid with the distribution meeting the requirements of spinning can be obtained. Compared with the conventional polymerization method, the multi-stage polymerization method has the advantages of simple polymerization equipment, low energy consumption, low investment, short reaction time, controllable product properties, high production magnification degree and the like.

Description

technical field [0001] The invention belongs to the technical field of polymer material synthesis, and relates to a synthesis method of biodegradable polylactic acid, in particular to a multistage polymerization method for preparing spinning-grade polylactic acid through ring-opening polymerization of lactide. Background technique [0002] As people pay more and more attention to energy consumption and environmental protection, polylactic acid has received more and more attention. Polylactic acid or polylactide (PLA) is a biodegradable polyester, which has important applications in textiles, food packaging, drug release, tissue engineering, etc., and its composite materials are used in automotive interiors, building materials, etc. It also has broad application prospects. Generally, PLA is mainly prepared by direct polycondensation of lactic acid or ring-opening polymerization of lactide. In contrast, the synthesis of high relative molecular weight polylactic acid generall...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/78C08G63/08
Inventor 邵惠丽刘鹏杨革生吴剑波胡学超
Owner 杭州聚丰新材料有限公司
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