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Method for preparing long chain branched polylactic resin by combining two-step functional group reaction

A technology of long-chain branched polylactic acid and polylactic acid resin, which is applied in the field of preparation of long-chain branched polylactic acid resin, and can solve problems such as difficulty in adjusting product branching degree, product molecular weight and branching degree, and difficulty in ensuring product performance. , to achieve the effect of large-scale continuous production, remarkable branching effect and high molecular weight

Active Publication Date: 2012-05-16
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method of obtaining long-chain branches by free radical reaction, that is, adding an organic peroxide-based free-radical initiator to the system, although the reaction is rapid and can introduce long-chain branched structures, due to the randomness of the initiator free radical hydrogen abstraction reaction, It is possible to cause branching of polylactic acid and to promote its degradation, which makes it very difficult to predict and control the molecular weight and branching degree of the product according to the needs, so that it is difficult to ensure the performance of the product; in contrast, the functional group reaction can Control the branching degree and molecular weight of long-chain branched products to a certain extent according to needs
After searching, the existing technical schemes about using epoxy compounds as functional group monomers to realize long-branched polylactic acid in the melt processing process have improved the melt strength of the product, but the disadvantage is that the reaction rate is too high. Slow, not conducive to continuous production
In addition, it is difficult to achieve the purpose of adjusting the degree of branching of products according to product needs only by controlling the dosage of epoxy compounds.

Method used

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  • Method for preparing long chain branched polylactic resin by combining two-step functional group reaction
  • Method for preparing long chain branched polylactic resin by combining two-step functional group reaction
  • Method for preparing long chain branched polylactic resin by combining two-step functional group reaction

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Experimental program
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Effect test

Embodiment 1

[0027] Synthesis of Long-chain Branched Polylactic Acid by Two-step Functional Group Reaction

[0028] Add 100 parts by weight of polylactic acid resin to an internal mixer with a rotation speed of 20 rpm at 210°C, and add 0.15 parts of 1,3,5-trimethyl-2,4,6-tri(3, 5-di-tert-butyl-4-hydroxybenzyl)benzene, 0.30 parts of pyromellitic dianhydride, 0.61 parts of triglycidyl isocyanuric acid, mixed for 2 minutes; then the internal mixer was raised to 60rpm , Melt blending until the end of the reaction, that is, stop after about 25 minutes, to obtain long-chain branched polylactic acid. Table 1 shows the melt index (190° C., 2.16 kg load) of the obtained reaction product material measured according to the ASTM D1238 standard. The torque and temperature curves in the internal mixer are shown in figure 1 , at 180°C and the strain is 5% under the condition of viscosity change curve with frequency see figure 2 , the morphological image of the supercritical carbon dioxide foamed prod...

Embodiment 2

[0030] Synthesis of Long-chain Branched Polylactic Acid by Two-step Functional Group Reaction

[0031] Add 100 parts of polylactic acid resin to an internal mixer with a rotation speed of 20 rpm at 210°C, and then add 0.15 parts of 1,3,5-trimethyl-2,4,6-tris(3, 5-di-tert-butyl-4-hydroxybenzyl) benzene, 0.46 parts of pyromellitic dianhydride, 0.61 parts of triglycidyl isocyanuric acid, mixed for 2 minutes; then internal mixer was raised to 60rpm, blend until the end of the reaction, stop after about 25 minutes, and make long-chain branched polylactic acid. The melt index test results are shown in Table 1.

Embodiment 3

[0033] Synthesis of Long-chain Branched Polylactic Acid by Two-step Functional Group Reaction

[0034] Add 100 parts of linear polylactic acid industrial materials into a internal mixer with a rotation speed of 20 rpm at 210 ° C, and add 0.15 parts of 1,3,5-trimethyl-2,4,6-trimethyl-2,4,6-tri( 3,5-di-tert-butyl-4-hydroxybenzyl)benzene, 0.60 parts of pyromellitic dianhydride, 0.61 parts of triglycidyl isocyanuric acid, mixed for 2 minutes; then internal mixer Increase to 60rpm, blend until the end of the reaction, stop after about 25 minutes, and make long-chain branched polylactic acid. The melt index test results are shown in Table 1.

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Abstract

The invention provides a method for preparing long chain branched polylactic resin by combining two-step functional group reaction, and relates to the technical field of polymer processing. The method for preparing the long chain branched polylactic resin by combining two-step functional group reaction comprises the following steps of: (1) melting polylactic resin; (2) adding an antioxidant, anhydride polyfunctional monomers and epoxy polyfunctional monomers, and mixing uniformly; and (3) melting and blending until the reaction is finished to obtain the long chain branched polylactic, whereinbased on 100 weight parts of linear polylactic resin, the antioxidant is 0.1 to 0.5 part, the anhydride polyfunctional monomers are 0.1 to 1 part; and the epoxy polyfunctional monomers are 0.1 to 1 part; and the epoxy polyfunctional monomers have the functionality of more than or equal to 3. By the method, the reaction rate is improved by 5 to 10 times; the obtained long chain branched polylacticproduct has an obvious branching effect, the melt strength and viscosity are greatly improved, and the product material meets the requirement of forming and can be easily subjected to film making, foaming and other processes according to product requirements; and the branching degree and the melt strength of the product can be controlled to a certain extent by regulating a monomer proportion and reaction temperature.

Description

technical field [0001] The invention relates to the technical field of polymer processing, in particular to a method for preparing long-chain branched polylactic acid resin. Background technique [0002] In recent years, biodegradable polymer materials have attracted widespread attention due to their significant advantages of not causing serious pollution to the environment after use. Among them, the polylactic acid resin material is more prominent. Not only can it be degraded and returned to nature after use, but its source does not depend on the exploitation of petroleum, and it is a completely renewable energy source, which makes the development and use of this material completely realize the natural cycle. , really meet the needs of low-carbon environmental protection. In addition, compared with similar polyester materials, polylactic acid has many advantages such as good mechanical properties and thermoplasticity, good resilience and curl durability, good oil resistanc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/91C08G63/06
Inventor 刘建叶乔金樑张师军郭梅芳王小兰王海波
Owner CHINA PETROLEUM & CHEM CORP
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