Modified polylactic acid preparation method and modified polylactic acid preparation device

A preparation device and technology of polylactic acid, applied in the field of preparation method of modified polylactic acid and its preparation device, can solve the problem of poor flexibility and impact resistance of polylactic acid, insignificant toughening effect of polylactic acid, and insufficient fluency of the preparation process and other problems, to achieve the effect of increasing hydrophilicity, increasing sustained release effect, and increasing fluency

Pending Publication Date: 2017-12-01
BENGBU COLLEGE
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  • Summary
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  • Claims
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Problems solved by technology

[0002] Polylactic acid is a polymer obtained by polymerization of lactic acid as the main raw material. It is widely used in the biomedical industry. Polylactic acid can be hydrolyzed and degreased in the body to generate lactic acid monomer, which is then oxidized to pyruvate by lactate dehydrogenase, and participates as an energy substance. The tricarboxylic acid cycle leads to CO 2 and H 2 O is excreted through the lungs, kidneys, and skin. It is highly safe to the human body and can be absorbed by human tissues. In addition to its excellent physical and mechanical properties, it has been obtained in long-acting controlled release systems of drugs (such as sustained release injections, oral drugs). Application, the preparation of polylactic acid includes direct method and indirect method. Due to the low molecular weight of the polylactic acid prepared by the direct synthesis method, most of the polylactic acid with higher molecular weight is required in the prior art, and the indirect method is mostly used for preparation. However, although polylactic acid It has relatively good degradation and absorption capacity, but the flexibility and impact resistance of polylactic acid are poor and the slow-release effect is not ideal. In order to make the drug exert the best drug effect, it is necessary to modify polylactic acid. In the prior art, polylactic acid is not only The preparation method is complicated, and the toughening effect on polylactic acid is not obvious
In addition, since there is no special preparation device in the preparation of polylactic acid, a three-necked flask is generally used for preparation in the preparation process, but the three-necked flask needs to be repeatedly installed and disassembled during use, resulting in insufficient fluency in the preparation process and affecting production efficiency

Method used

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  • Modified polylactic acid preparation method and modified polylactic acid preparation device
  • Modified polylactic acid preparation method and modified polylactic acid preparation device
  • Modified polylactic acid preparation method and modified polylactic acid preparation device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Embodiment 1: the preparation method of modified polylactic acid,

[0046] Step 1: Take an appropriate amount of L-lactic acid and put it in container I. After vacuumizing container I, distill at 25°C for 1 hour, then put molecular sieves into container I for later use. , adding molecular sieves to purify the L-lactic acid.

[0047] Step 2: Add the dehydrated L-lactic acid and 1,4-butanediol to container II in sequence, the mass ratio of L-lactic acid and 1,4-butanediol is n L-乳酸 :n 1,4-丁二醇 =40:1, the container II is heated to 70°C, and then stannous chloride is added, the mass ratio of L-lactic acid to 1,4-butanediol is n L-乳酸 :n 氯化亚锡 =100:1 Heating to 110°C for 30 minutes, using stannous chloride as a catalyst, and polymerizing L-lactic acid under the action of 1,4-butanediol.

[0048] Step 3: Vacuumize the container II, and then gradually increase the temperature in the container II at a heating rate of 7°C / 30min until the temperature reaches 160°C, continue the ...

Embodiment 2

[0056] Embodiment 2: the preparation method of modified polylactic acid,

[0057] Step 1: Take an appropriate amount of L-lactic acid and place it in container I, vacuumize container I, distill at 30°C for 1 hour, and then put molecular sieves into container I for later use;

[0058] Step 2: Pass N into container II 2 , and continue for a period of time to get rid of the original gas in the container 1;

[0059] Step 3: Add L-lactic acid and 1,4-butanediol after water removal to container II in sequence, the mass ratio of L-lactic acid and 1,4-butanediol is n L-乳酸 :n 1,4-丁二醇 =60:1, heat the container II to 75°C, then add stannous chloride, the mass ratio of L-lactic acid to 1,4-butanediol is n L-乳酸 :n 氯化亚锡 =150:1 heated to 120°C for 45 minutes;

[0060] Step 4: Vacuumize the container II, then gradually increase the temperature in the container II at a heating rate of 8°C / 30min until the temperature reaches 170°C, continue the reaction for 8h, stop heating, remove the vac...

Embodiment 3

[0068] Embodiment 3: the preparation method of modified polylactic acid,

[0069] Step 1: Take an appropriate amount of L-lactic acid and place it in container I, vacuumize container I, distill at 40°C for 1 hour, and then put molecular sieves into container I for later use;

[0070] Step 2: Add the dehydrated L-lactic acid and 1,4-butanediol to container II in sequence, the mass ratio of L-lactic acid and 1,4-butanediol is n L-乳酸 :n 1,4-丁二醇 =80:1, the container II is heated to 80°C, and then stannous chloride is added, the mass ratio of L-lactic acid to 1,4-butanediol is n L-乳酸 :n 氯化亚锡 =250:1 heated to 130°C for 70 minutes;

[0071] Step 3: Vacuumize container II, then gradually increase the temperature in container II at a heating rate of 10°C / 30min until the temperature reaches 180°C, continue the reaction for 15 hours, stop heating, remove the vacuum, and obtain product A;

[0072] Step 4: Add an appropriate amount of the product A synthesized in step 4 into the three-...

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Abstract

The invention discloses a modified polylactic acid preparation method. The method includes: adding an appropriate amount of L-lactic acid into a container I, dehydrating, and sequentially adding dehydrated L-lactic acid and 1,4-butanediol into a container II to obtain a product A through reaction under the catalytic reaction of stannous chloride; adding the product A and 2,4-toluene diisocynate into a container III; feeding N2 into the container III to obtain a product B; dissolving with chloroform, and adding methyl alcohol to obtain a precipitate; sequentially adding chitosan and 50% NaOH solution into a container IV to obtain a product C through reaction; adding the product C and solution A into the container IV, continuously stirring for reaction for 1-5h at 90 DEG C, adopting diethyl ether for precipitating a product D obtained in reaction, and drying solid obtained by precipitating for 10h under a vacuum condition to obtain modified polylactic acid. The modified polylactic acid preparation method has advantages that the reaction process is easy to control, hydrophilcity and flexibility of polylactic acid can be improved, and medicine diffusion can be effectively inhibited to improve slow-release effect owing to a chitosan macromolecular structure.

Description

technical field [0001] The invention mainly relates to the field of preparation of modified polylactic acid, in particular to a preparation method of modified polylactic acid and a preparation device thereof. Background technique [0002] Polylactic acid is a polymer obtained by polymerization of lactic acid as the main raw material. It is widely used in the biomedical industry. Polylactic acid can be hydrolyzed and degreased in the body to generate lactic acid monomer, which is then oxidized to pyruvate by lactate dehydrogenase, and participates as an energy substance. The tricarboxylic acid cycle leads to CO 2 and H 2 O is excreted through the lungs, kidneys, and skin. It is highly safe to the human body and can be absorbed by human tissues. In addition to its excellent physical and mechanical properties, it has been obtained in long-acting controlled release systems of drugs (such as sustained release injections, oral drugs). Application, the preparation of polylactic a...

Claims

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Application Information

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IPC IPC(8): C08G63/91C08G63/08C08G63/78C08G18/76C08G18/64C08G18/42
CPCC08G18/428C08G18/6484C08G18/7614C08G63/08C08G63/785C08G63/912
Inventor 吴景梅赵建军邰燕芳史宜望
Owner BENGBU COLLEGE
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