Synthesis of molecular weight controllable polylactic acid without metal residual

A synthesis method and molecular weight technology, applied in the field of synthesis of organic polymer materials, can solve the problems of complex production process, large equipment investment, high technical requirements, etc., and achieve the effect of simple process, high product yield and narrow molecular weight distribution

Inactive Publication Date: 2009-05-13
HARBIN ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the production process is complicated, the process is long, it needs to be reacted unde...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Under normal temperature, normal pressure, and argon protection, in a reaction device equipped with a stirrer, add 10 g of L-lactide, add 69.4 mL of dichloromethane, stir well, and prepare L-lactide with a molar concentration of 1M. lactide solution. With 2-propyn-1 alcohol as the initiator, according to the molar ratio of L-lactide, 2-propyn-1 alcohol, 1,8-diazabicyclo[5.4.0]undec-7-ene The ratio is 8:1:0.08. Add 2-propyn-1 alcohol and 1,8-diazabicyclo[5.4.0]undec-7-ene sequentially under stirring, and react for 0.25h.

[0027] (2) According to the molar ratio of 2-propyn-1 alcohol to benzoic acid is 1:2, add benzoic acid under stirring and react for 20 minutes.

[0028] (3) Prepare methanol according to the volume ratio of the reaction solution to methanol at 1:20, drop the reaction solution into methanol, polylactic acid forms a precipitate, filter, and wash with methanol twice. Vacuum dry at 30°C for 24h.

[0029] (4) The product is poly-L-lactic acid whose e...

Embodiment 2

[0031] (1) The experimental device and experimental conditions were the same as in Example 1. Add 10 g of D-lactide and 100 mL of dichloromethane, and stir evenly to prepare a D-lactide solution with a molar concentration of 0.7 M. With 4-ethynyl benzyl alcohol as initiator, according to the molar ratio of D-lactide, 4-ethynyl benzyl alcohol, 1,8-diazabicyclo[5.4.0]undec-7-ene is 28 : 1: 0.28, add 4-ethynyl benzyl alcohol and 1,8-diazabicyclo[5.4.0]undec-7-ene sequentially under stirring, and react for 0.5h.

[0032] (2) According to the molar ratio of 4-ethynyl benzyl alcohol and benzoic acid as 1:3, add benzoic acid under stirring and react for 18 minutes.

[0033] (3) Prepare methanol according to the volume ratio of the reaction solution to methanol at 1:15, drop the reaction solution into methanol, polylactic acid forms a precipitate, filters, and washes twice with methanol. Dry in vacuum at 20°C for 48h.

[0034] (4) The product is poly-D-lactic acid whose end group is...

Embodiment 3

[0036] (1) The experimental device and experimental conditions were the same as in Example 1. Add 15 g of L-lactide and 150 mL of dichloromethane, stir evenly, and prepare an L-lactide solution with a molar concentration of 0.7 M. With 6-azido-1-hexanol as the initiator, according to L-lactide, 6-azido-1-hexanol, 1,8-diazabicyclo[5.4.0]undeca-7- The molar ratio of alkenes is 200:1:2, and 6-azido-1-hexanol and 1,8-diazabicyclo[5.4.0]undec-7-ene are added sequentially under stirring and reacted for 1.5h.

[0037] (2) According to the molar ratio of 6-azido-1-hexanol to benzoic acid of 1:2, add benzoic acid under stirring and react for 20 minutes.

[0038] (3) Prepare methanol according to the volume ratio of the reaction solution to methanol at 1:15, drop the reaction solution into methanol, polylactic acid forms a precipitate, filter, and wash with methanol three times. Vacuum dry at 25°C for 48h.

[0039](4) The product is poly-L-lactic acid whose end group is an azido group...

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PUM

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Abstract

The invention provides a method for synthesizing a polylactic acid which has no metallic residue and has controllable molecular weight. The method is as follows: a reaction solvent is added into lactide to prepare a lactide solution the mol concentration of which is between 0.5 and 1.5 M under the protection of inert gas, and an initiator and catalyst are added into the lactide solution in turn, and subjected to polymerization for 0.25 to 2 hours, wherein the mol ratio of the lactide to the initiator to the catalyst is 6-350 to 1 to 0.06-0.35; a terminator is added into the lactide solution, and subjected to termination reaction for 10 to 20 minutes, wherein the mol ratio of the initiator to the terminator is 1 to 1-5; and methanol is prepared, wherein the volume ratio of the reaction solution to the methanol is 1 to 10-20, the reaction solution is dripped into the methanol to form polylactic acid deposit, and the polylactic acid deposit is separated out, filtered, subjected to methanol washing for 2 to 3 times, and subjected to vacuum drying for 24 to 48 hours at a temperature of between 20 and 40 DEG C to obtain the product. The synthesis method can be performed under the condition of room temperature and normal pressure, has high product yield and simple technique, does not require the conditions of heating and decompression, is easy to operate, and can effectively control the molecular weight of the polylactic acid product; and the product has no metallic residue and can be used as a medical material.

Description

(1) Technical field [0001] The invention relates to a method for synthesizing organic polymer materials, in particular to a method for synthesizing polylactic acid which is non-toxic and can be used as a medical material. (2) Background technology [0002] Polylactic acid is a polymer material with good biocompatibility and biodegradability. It is widely used in drug sustained-release capsules and surgical sutures because of its non-toxic, non-accumulating, and degradation products that can participate in human metabolism. Wire, orthopedic internal fixation materials, etc. It can be completely decomposed under the action of microorganisms, water, acid, alkali, etc. in nature, and the final product is CO 2 and H 2 O, the intermediate product lactic acid is also a product of normal glucose metabolism in the body. It will not accumulate in important organs and cause adverse reactions, and it is also non-polluting to the environment. Therefore, it is used as an environmentally...

Claims

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Application Information

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IPC IPC(8): C08G63/87C08G63/08
Inventor 张春红刘飞刘方彬
Owner HARBIN ENG UNIV
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