Long-chain branched polylactic resin and preparation method and application thereof

A technology of polylactic acid resin and long-chain branching, which is applied in the field of long-chain branched polylactic acid resin and its preparation, can solve problems such as high cost, poor blow molding performance, and complicated operation, and achieve high crystallinity and crystallization speed, Effect of increasing melt strength and increasing crystallization rate

Active Publication Date: 2013-11-27
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to solve the problem that the existing linear polylactic acid has low melt strength, difficult foaming, and poor blow molding performance, and the preparation of long-chain branched or slightly cross-linked polylactic acid is not directly polymerized and requires post-modification. method, thus leading to the defects of high cost and complicated operation, and a long-chain branched polylactic acid resin and its preparation method and use are provided

Method used

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  • Long-chain branched polylactic resin and preparation method and application thereof
  • Long-chain branched polylactic resin and preparation method and application thereof
  • Long-chain branched polylactic resin and preparation method and application thereof

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preparation example Construction

[0055] A preparation method of long-chain branched polylactic acid resin, the preparation process of the polylactic acid resin whose coupling segment is the structure of formula 3 is as follows:

[0056] Step 1: Lactide undergoes ring-opening polymerization under the action of an initiator and a catalyst to obtain multi-arm polylactic acid; the initiator is a polyhydric alcohol, and the catalyst is stannous octoate, diethylzinc, tributylaluminum or bismuth (N,N-bis(trimethylsilyl)amino)zinc, the molar ratio of initiator alcoholic hydroxyl group to lactide is 1:50 to 1:100; the molar ratio of catalyst to lactide is 1:100 to 1 : 1000;

[0057] Step 2: Coupling multi-arm polylactic acid with diisocyanate obtained in step 1 to obtain long-chain branched polylactic acid; wherein the molar ratio of isocyanate groups to terminal hydroxyl groups of multi-arm polylactic acid is 0.8-1.5:1.

[0058] A preparation method of long-chain branched polylactic acid resin, the preparation proce...

Embodiment 1

[0086] Example 1: 3-Hydroxy Initiated-DP73-HDI Coupling

[0087] Under the protection of nitrogen, 1,1,1-trimethylolpropane (0.1789g, 4mmol OH), lactide (43.2g, 300mmol) were added to the flame-dried reaction flask, and the pumping-gassing was repeated three times , add 140ml of toluene and stannous octoate / toluene solution (3ml, 0.1mmol / ml), and react in an oil bath at 120°C for 24h to obtain three-arm polylactic acid. After the polymerization is completed, adjust the solution temperature to 110°C, under vigorous stirring , add 10ml HDI / toluene solution (0.2mmol / ml), keep at 110°C, stir and react for 0.5 hours, the product is precipitated with cold methanol, and vacuum dried at 60°C for 24h to obtain long-chain branched polylactic acid resin. The polymerization degree of gained long-chain branched polylactic acid resin is 72.5, and productive rate is 95%, and gel content is 0.2%, and absolute molecular weight Mw is 178,000, and polydispersity coefficient is 1.44, and zero-she...

Embodiment 2

[0088] Example 2: 3-Hydroxy Initiated-DP50-MDI Coupling

[0089]Under nitrogen protection, 1,1,1-trimethylolethane (0.160g, 4mmol OH), ethylene glycol (13mg, 0.4mmol), lactide (31.7g, 220mmol LA), were added to the reaction In the still, pump air-inflate repeatedly three times, add stannous octoate / toluene solution (2.2ml, 1.0mmol / ml), heat up to 110°C, stir and polymerize for 2 hours, then heat up to 170°C, continue polymerization for 8 hours, and obtain three-arm A mixture of polylactic acid and linear polylactic acid; after the polymerization is completed, keep the melt temperature at 170°C, under vigorous stirring, add 16.5ml of MDI / toluene solution (0.2mmol / ml) into the reactor, stir for 10 minutes, and the product is cooled Granulate and dry in a vacuum oven at 60°C to obtain long-chain branched polylactic acid resin. The degree of polymerization of the gained long-chain branched polylactic acid resin is 50, the productive rate is 98%, the gel content is 0.3%, the absol...

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Abstract

The invention discloses a long-chain branched polylactic resin and a preparation method and an application thereof, which belong to the technical field of high polymer materials and are used for overcoming the defects of low strength, difficulty in foaming, poor blow molding property and high cost existing in the conventional linear polylactic resin melt. The long-chain branched polylactic resin is formed by linearly connecting a multi-arm polylactic acid through a coupling chain segment or connecting a multi-arm polylactic acid with 3-8 multi-arm polylactic acids through a coupling segment; each arm of each multi-arm polylactic acid is of the same length; the polymerization degree of each arm is 50-100 counted by a lactide unit; the arm quantity N of the multi-arm polylactic resin is 3, 4, 6 or 8; and the coupling chain segment has a polyurethane structure. The invention further provides a long-chain branched polylactic resin and a preparation method and an application thereof. The long-chain branched polylactic resin can be directly used for foaming, can be blended with a linear polylactic acid, shows melt viscosity frequency dependency likewise, has remarkable shearing thinning behavior and tensile stress hardening phenomenon, and can be used for preparing a foaming material at a lower cost.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to a long-chain branched polylactic acid resin and its preparation method and application. Background technique [0002] Foam material is a kind of polymer / gas composite material with high polymer as the matrix. It generally has the characteristics of high specific strength, good impact resistance, good heat insulation and good electrical insulation. It has been widely used in packaging, aircraft, etc. And automotive parts, building materials, thermal insulation materials and medical fields. However, the current foam materials are all derived from non-biodegradable materials, and their application fields are increasingly subject to pressure and restrictions from environmental protection. With the increasing emphasis on environmental protection in today's society, degradable foam materials have been put on the agenda to replace existing foam plastics in some fields. Pol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/42C08G18/78C08G63/06C08L67/04C08L75/06C08J9/00
Inventor 景遐斌黄宇彬王亮燕谢志刚胡秀丽
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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