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Sulfonic acid compound-containing and tin compound-containing polylactic acid composition and preparation method thereof

A technology of sulfonic acid compound and tin compound is applied in the field of preparing polylactic acid, which can solve the problems of poor heat resistance and hydrolysis resistance of polylactic acid.

Active Publication Date: 2013-03-13
萘琪沃克有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0033] Aiming at the problem of poor heat resistance and hydrolysis resistance of polylactic acid, the present invention provides a polylactic acid composition containing sulfonic acid compound and tin compound, which has the advantages of high hydrolysis resistance, excellent color and high melting point, etc.

Method used

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  • Sulfonic acid compound-containing and tin compound-containing polylactic acid composition and preparation method thereof
  • Sulfonic acid compound-containing and tin compound-containing polylactic acid composition and preparation method thereof
  • Sulfonic acid compound-containing and tin compound-containing polylactic acid composition and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0113] After pouring 200 g of 90 wt % L-lactic acid aqueous solution into a 500 mL four-necked flask, the flask was placed in an oil bath. Install a stirrer on the four-neck flask, insert a thermocouple thermometer, connect the vacuum pipeline and the nitrogen pipeline and replace with nitrogen for 3 times, then raise the temperature of the oil bath to 120°C for dehydration. The system pressure gradually decreased from normal pressure to 5KPa within 60 minutes from the start of dehydration; then continued dehydration at 5KPa for 1.5 hours (total dehydration 2.5 hours); at this time, after returning the system pressure to normal pressure with nitrogen, add 4952mg of tin (the addition amount is 27513ppm relative to the mass of lactic acid in terms of metal elements, the same below), 3964mg of methanedisulfonic acid (the addition amount is based on sulfonate-SO 3 The sulfur element mass in H is 8000ppm relative to the lactic acid mass, the same below). Then the temperature of th...

Embodiment 2

[0116] After pouring 200 g of 90 wt % L-lactic acid aqueous solution into a 500 mL four-necked flask, the flask was placed in an oil bath. Install a stirrer on the four-neck flask, insert a thermocouple thermometer, connect the vacuum pipeline and the nitrogen pipeline and replace with nitrogen for 3 times, then raise the temperature of the oil bath to 120°C for dehydration. The system pressure gradually decreased from normal pressure to 5KPa within 60 minutes from the start of dehydration; then continued dehydration at 5KPa for 1.5 hours (total dehydration 2.5 hours); at this time, after returning the system pressure to normal pressure with nitrogen, add Stannous acetate 9mg (25ppm), ethanedisulfonic acid 338mg (632ppm). Then the temperature of the system was raised to 160°C, the pressure was gradually reduced from normal pressure to 0.3KPa within 2 hours, and the pressure was kept at 0.3KPa for 4 hours (6 hours in total) after melt polymerization, poured out, and cooled to o...

Embodiment 3

[0119] After pouring 200 g of 90 wt % L-lactic acid aqueous solution into a 500 mL four-necked flask, the flask was placed in an oil bath. Install a stirrer on the four-neck flask, insert a thermocouple thermometer, connect the vacuum pipeline and the nitrogen pipeline and replace with nitrogen for 3 times, then raise the temperature of the oil bath to 120°C for dehydration. The system pressure gradually decreased from normal pressure to 5KPa within 60 minutes from the start of dehydration; then continued dehydration at 5KPa for 1.5 hours (total dehydration 2.5 hours); at this time, after returning the system pressure to normal pressure with nitrogen, add Stannous acetate 107.7mg (300ppm), propanedisulfonic acid 765mg (1333ppm). Then the temperature of the system was raised to 160°C, the pressure was gradually reduced from normal pressure to 0.3KPa within 2 hours, and the pressure was kept at 0.3KPa for 4 hours (6 hours in total) after melt polymerization, poured out, and cool...

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Abstract

The invention discloses a sulfonic acid compound-containing and tin compound-containing polylactic acid composition and a preparation method thereof. The composition comprises polylactic acid, a sulfonic acid compound and a tin compound, wherein the sulfonic acid compound is one or more of dibasic sulfonic acid, polybasic sulfonic acid, a bibasic stannous sulfonate compound or a polybasic stannous sulfonate compound. The method for preparing the polylactic acid in the invention comprises the following steps of: performing dehydration treatment on lactic acid (or lactic acid prepolymer) serving as a raw material, and then performing melt polycondensation in the presence of a composite catalyst consisting of the dibasic sulfonic acid and / or the polybasic sulfonic acid and the tin compound to obtain the polylactic acid product; and the method also can comprise the following step of: further performing solid-phase polyreaction on the product of the melt polycondensation to finally obtain high molecular weight polylactic acid. Due to the adoption of the method, the reaction period is shortened by using a direct condensation method, and the polylactic acid having high molecular weight, high melting point and high thermal stability is obtained. For the polylactic acid prepared by the method, the process is simple and stable, the condensation time is shot, and the cost is relatively low.

Description

technical field [0001] The invention belongs to the field of polymer materials, in particular to a polylactic acid composition containing a sulfonic acid compound and a tin compound and a polylactic acid composition using one or more of dibasic sulfonic acid or polybasic sulfonic acid together with a tin compound as a compound Catalyst preparation method of polylactic acid. Background technique [0002] In the 21st century, environmental pollution and resource shortages have become global problems, and they are getting more and more attention. Synthetic polymer materials using petroleum as raw materials are widely used and have made important contributions to the development of human civilization. However, such materials are difficult to recycle after use, causing serious "white pollution" problems; on the other hand, petroleum is a non-renewable resource, and the increasing consumption of petroleum has caused human beings to face serious resource shortages. It is expected...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L67/04C08K5/42C08K3/08C08K3/38C08K3/24C08K5/098C08G63/06C08G63/87C08G63/85C08G63/80
Inventor 左璞晶何勇魏小花於向宁
Owner 萘琪沃克有限责任公司
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