Multistage reaction continuous polymerization unit for synthesizing polylactic acid material with lactides monomer

A technology for synthesizing polylactic acid and polymerization equipment, which is applied in the field of multi-stage continuous polymerization process and equipment, which can solve the problems of low product molecular weight, difficult operation control, low lactide conversion rate, etc., to increase molecular weight, reduce load, and disperse equipment load effect

Inactive Publication Date: 2009-01-28
四川琢新生物材料研究有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The purpose of the present invention is to improve the continuous polymerization of polylactic acid by adopting a single twin-screw reaction extrusion process and device, which is difficult to control in operation, the conversion rate of lactide is low, and the disadvantages of low molecular weight of the product

Method used

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  • Multistage reaction continuous polymerization unit for synthesizing polylactic acid material with lactides monomer
  • Multistage reaction continuous polymerization unit for synthesizing polylactic acid material with lactides monomer
  • Multistage reaction continuous polymerization unit for synthesizing polylactic acid material with lactides monomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add the refined L-lactide to one of the pre-polymerization tanks. The volume of the pre-polymerization tank is 800L. Remove the original air in the tank and flush it with nitrogen repeatedly. After melting, start the agitator to add catalyst (the amount is 0.1% of the monomer), heat up to 160°C to start polymerization, open the discharge valve when the lactide conversion rate reaches 30%, and prepolymer and remaining lactide are mixed in a certain amount. The speed is put into a twin-screw reaction extruder rotating in the same direction. The diameter of the extruder screw is φ65mm, and the ratio of length to diameter is L / D=45. Wait. The lactide conversion rate of the twin-screw reaction extruder reaches about 90%. A melt pump is installed at the outlet of the extruder to control the extrusion rate. About 50-70kg / h of the material passes through the static mixer to make the pre-heated Polymer, lactide, catalyst, etc. are evenly mixed. The static mixer is equipped with...

Embodiment 2

[0022]Add the refined DL-lactide to one of the pre-polymerization tanks. The volume of the pre-polymerization tank is 800L. Remove the original air in the tank and flush it with nitrogen repeatedly. After melting, start the agitator to add the catalyst (the amount is 1% of the monomer), heat up to 180°C to start polymerization, and open the discharge valve when the lactide conversion rate reaches 10%, and the prepolymer and the remaining lactide are mixed in a certain amount. The speed is put into a twin-screw reaction extruder rotating in the same direction. The diameter of the extruder screw is φ65mm, and the ratio of length to diameter is L / D=45. Wait. Through the twin-screw reaction extruder until the conversion rate of lactide reaches about 80%, a melt pump is installed at the exit of the extruder to control the extrusion rate, and about 50-70kg / h of the material passes through the static mixer to make it The prepolymer, lactide, catalyst, etc. are evenly mixed. The stat...

Embodiment 3

[0024] Add the mixture of refined DL-lactide and glycolide (the mixing ratio can be determined according to the needs of the product, the ratio in this example is 75:25) into one of the prepolymerization tanks, the volume of the prepolymerization tank is 800L, and the The original air in the kettle was repeatedly flushed with nitrogen, and the temperature was raised to 120-140°C after evacuating and filling several times. After the monomers were completely melted, the agitator was started to add the catalyst (0.01% of the monomer), the molecular weight regulator ethylene glycol (the amount 0.1% of the monomer) to 180 ° C to start polymerization, when the monomer conversion rate reaches 40%, open the discharge valve, put the prepolymer and the remaining monomer into the co-rotating twin-screw reaction extrusion at a certain rate extruder, extruder screw diameter φ65mm, length-to-diameter ratio L / D=45, equipped with forward conveying screw element, kneading block, toothed dispers...

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Abstract

The invention provides a multi-grade continuous polyplant of polylactic acid materials, which is synthesized by the ring-opening polymerization of a lactide monomer. The multi-grade continuous polyplant consists of a polyplant device and a feed device with different characteristics, including a prepolymer reaction kettle set, a double-screw reaction squeezer, a fused mass feed pump, a static mixer and a tubular reactor. Compared with the plant for adopting a single double-screw reaction squeezer to synthesize the polylactic acid materials, the multi-grade continuous polyplant disperses and lightens the load of the reaction devices of each grade as a multi-grade plant is used for replacing a single-grade reaction plant, thus leading the control on the conversion rate of the lactide monomer to be easier and more stable; as the fused mass feed pump is connected in series in the middle, the floating speed of the materials and the pressure of the squeezer and a subsequence device can be stabilized, the reaction condition can be better controlled; as the back section of the plant is provided with the static mixer and the tubular reactor, the final conversion rate of the lactide monomer can be further improved, thus being beneficial to improving and adjusting the molecular weight and the molecular weight distribution of the polylactic acid materials.

Description

technical field [0001] The multi-stage continuous polymerization process and device described in the present invention are used for ring-opening polymerization of lactide monomers to synthesize biodegradable polylactic acid materials. The polymer polymerization method and equipment involve polymer chemistry and polymer physics. , using multi-level equipment segmented control, can achieve the effect of dispersing equipment load, facilitating operation, improving product conversion rate, adjusting molecular weight and stabilizing quality. Background technique [0002] The synthesis of polylactic acid materials is usually to synthesize lactide from lactic acid, and then ring-opening polymerization of lactide to generate polylactic acid, that is, a two-step method, which can synthesize products with higher molecular weight. In the two-step method, lactide is opened There are many methods of ring polymerization. The simplest polymerization method is batch polymerization in ampoul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/08B29C47/40B29C48/57B29C48/535B29C48/54B29C48/55B29C48/565
CPCB29C47/6031B29C47/6056B29C47/6025B29C47/605B29C47/6037B29C48/535B29C48/54B29C48/55B29C48/565B29C48/57
Inventor 袁明龙申开智袁明伟王贵恒邓先模
Owner 四川琢新生物材料研究有限公司
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