Preparation method of biodegradable polyester amide modified polylactic acid

A polyester amide and biodegradation technology, applied in the field of polylactic acid, can solve the problems of polylactic acid racemization, poor polylactic acid crystallinity, low melting point, etc., and achieve the effects of mild conditions, cheap raw materials, and easy availability of raw materials

Active Publication Date: 2017-05-10
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the current polycondensation-chain extension method can obtain high-molecular-weight polylactic acid, it is easy to cause racemization of polylactic acid due to long-term high-temperature polycondensation and chain extension. Even if L-lactic acid or D-lactic acid is used as raw material, the obtained polylactic acid The crystallinity is generally poor and the melting point is low, which affects the thermal and mechanical properties of the material; at the same time, the brittleness of polylactic acid still cannot be improved

Method used

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  • Preparation method of biodegradable polyester amide modified polylactic acid
  • Preparation method of biodegradable polyester amide modified polylactic acid
  • Preparation method of biodegradable polyester amide modified polylactic acid

Examples

Experimental program
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Embodiment 1

[0045] 1) Preparation of short polyamide diacid: Weigh 50.00 parts of nylon 610 salt, 31.77 parts of sebacic acid, and 0.20 parts of phosphorous acid in parts by weight, and react at 200°C under normal pressure for 1 hour under nitrogen protection, and then heat up to 210° C. and react under normal pressure for 3 hours to obtain a short polyamide diacid with an acid value of 202.86 mgKOH / g and a hydroxyl value of 1.14 mgKOH / g.

[0046] 2) Preparation of polyester amide prepolymer: Weigh 57.89 parts of short polyamide diacid prepared in step 1), 42.07 parts of polyethylene glycol (M=400g / mol), 0.20 parts of phosphorous acid, chlorine 0.10 parts of stannous chloride, 0.10 parts of p-toluenesulfonic acid, under the protection of nitrogen, the temperature was raised to 200 ° C under normal pressure for 1 hour, and then a decompression device was used, the temperature was raised to 210 ° C, and the reaction was gradually reduced by a water pump for 2 hours. Then use an oil pump to ...

Embodiment 2

[0051] 1) Preparation of polyester amide prepolymer: Weigh 57.89 parts of short polyamide diacid prepared in step 1) of Example 1), 42.07 parts of polyethylene glycol (M=600g / mol), phosphorous acid in parts by weight 0.20 parts, 0.10 parts of stannous chloride, 0.10 parts of p-toluenesulfonic acid, under the protection of nitrogen, the temperature was raised to 200 ° C under normal pressure for 1 hour, and then a decompression device was used, the temperature was raised to 210 ° C, and the water pump was used to depressurize gradually React for 2 hours, then depressurize with an oil pump, and react for 3 hours in a 3 mmHg decompression system to obtain a polyester amide prepolymer with an acid value of 35.02 mgKOH / g and a hydroxyl value of 20.034 mgKOH / g.

[0052] 2) Preparation of polylactic acid-b-polyesteramide: Weigh 20.00 parts of polylactic acid in Step 3) of Example 1, 13.22 parts of polyester amide prepolymer prepared in Step 1) of Example 2, and sub 0.20 parts of phos...

Embodiment 3

[0055] 1) Preparation of polyester amide prepolymer: Weigh 35.50 parts of short polyamide diacid prepared in step 1) of Example 1), 65.10 parts of polyethylene glycol (M=1000g / mol), phosphorous acid 0.20 parts, 0.10 parts of stannous chloride, 0.10 parts of p-toluenesulfonic acid, under the protection of nitrogen, the temperature was raised to 200 ° C under normal pressure for 1 hour, and then a decompression device was used, and the temperature was raised to 210 ° C. React for 2 hours, and then use an oil pump to reduce the pressure to 3 mmHg and react for 3 hours to obtain a polyester amide prepolymer with an acid value of 22.22 mgKOH / g and a hydroxyl value of 15.31 mgKOH / g.

[0056] 2) Preparation of polylactic acid-b-polyesteramide prepolymer: Weigh 20.00 parts of polylactic acid prepolymer in Step 3) of Example 1, and polyester amide prepolymer prepared in Step 1) of Example 3 in parts by weight. 17.12 parts of polymer, 0.20 parts of phosphorous acid, 0.10 parts of stanno...

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Abstract

A preparation method of biodegradable polyesteramide modified polylactic acid belongs to the technical field of polylactic acid. The method adopting a polycondensation-chain extension technology to prepare aliphatic polyesteramide modified polylactic acid comprises the following steps: carrying out melt polycondensation on aliphatic short-chain polyamide diacid and polyether diol to prepare a polyesteramide prepolymer, polycondensing the polyesteramide prepolymer, and a polylactic acid prepolymer, and carrying out chain extension by using diacylbislactame and bisoxazoline chain extender to prepare the biodegradable polyesteramide modified polylactic acid product with the molecular weight of 90290-111820. The method has the advantages of mild conditions, cheap and easily available raw materials, and environmental protection.

Description

technical field [0001] The invention relates to a preparation method of polylactic acid modified with biodegradable polyester amide, in particular to the preparation of polyester amide prepolymer by polycondensation of aliphatic polyether diol and short polyamide diacid. Further polycondensation and chain extension are used to prepare polyesteramide-modified polylactic acid with a molecular weight of 90,290 to 111,820, which belongs to the technical field of polylactic acid. [0002] technical background [0003] Polylactic acid (PLA) is a transparent polymer with good strength and biocompatibility. It is completely biodegradable and its raw materials are renewable. It is very friendly to the environment and the human body. Degradable plastic. At present, high-molecular-weight polylactic acid is mainly prepared by ring-opening polymerization of lactide. This method is complex and makes the production cost of polylactic acid relatively high. At the same time, polylactic acid ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G81/00C08G63/91C08G69/44
Inventor 赵京波赵艳平张军营杨万泰
Owner BEIJING UNIV OF CHEM TECH
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