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Method for preparing biodegradable poly(malic acid) material

A technology of polymalic acid and malic acid, which is applied in the field of preparation of polymalic acid materials, can solve the problems of time-consuming, difficult separation and purification of intermediate products, and many steps, and achieve the effect of an economical preparation method

Inactive Publication Date: 2011-04-06
ZHANGJIAGANG CHAINENG BIOLOGICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method route is more complicated, and the step of forming lactone is more, uneconomical or yield is too low, and this has just restricted the development of this method
[0005] To sum up, the current manufacturing methods of polymalic acid have these advantages and disadvantages: (1) The direct polymerization method is a one-step reaction, which is straightforward and simple, and the separation and purification of the product is easy. High yield; economical; but the obtained polymalic acid has low molecular weight and high reaction temperature
(2) The molecular weight of polymalic acid obtained by the ring-opening polymerization method is high, and the product is mainly β-type PMLA, but there are many steps, time-consuming, low yield, difficult separation and purification of intermediate products, and high cost
(3) The molecular weight of polymalic acid obtained by the biological fermentation method is high, the product is relatively pure, and the synthesis conditions are mild; but the yield is low and the process is long, so far only β-type PMLA can be synthesized

Method used

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  • Method for preparing biodegradable poly(malic acid) material
  • Method for preparing biodegradable poly(malic acid) material
  • Method for preparing biodegradable poly(malic acid) material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] This example provides a preparation method of polymalic acid, the specific process is as follows: first check the vacuum degree of the system; accurately weigh 5.0011g D,L-mixed malic acid on an analytical balance, and add it to the flask; accurately weigh 0.0478 g tin protochloride, join in the distillation flask; Measure 100ml diphenyl ether and join in the flask, start to react; Vacuumize first, start heating when the degree of vacuum reaches about 0.07MPa; Regulate the temperature to make it rise steadily, When the reaction temperature reaches 110°C, it stabilizes to allow the reaction to proceed normally, and the vacuum degree of the reaction is stabilized at 1 mmHg; after about 22 hours of reaction, stop heating first, and then stop vacuuming; when the temperature of the flask drops, take it out and quickly Scrape out the product in the retort and put it on the Petri dish, and seal it well; the product in the retort becomes a block with high hardness due to the r...

Embodiment 2

[0023] This example provides a preparation method of polymalic acid, the specific process is as follows: first check the vacuum degree of the system; accurately weigh 5.0011g D,L-mixed malic acid on an analytical balance, and add it to the flask; accurately weigh 0.0478 g tin protochloride, join in the distillation flask; Measure 100ml diphenyl ether and join in the flask, start to react; Vacuumize first, start heating when the degree of vacuum reaches about 0.07MPa; Regulate the temperature to make it rise steadily, When the reaction temperature reaches 120°C, it stabilizes to allow the reaction to proceed normally, and the vacuum degree of the reaction is stable at 1 mmHg; after about 23 hours of reaction, stop heating first, and then stop vacuuming; when the temperature of the flask drops, take it out and use a medicine spoon Scrape out the product in the retort and put it on the Petri dish, and seal it well; the product in the retort becomes a block with high hardness due...

Embodiment 3

[0025] This embodiment provides a preparation method of polymalic acid, which is basically the same as Example 1, except that the reaction time is extended to 31 hours.

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Abstract

The invention relates to a method for preparing a biodegradable poly(malic acid) material. The method comprises the following steps of: (1) establishing a reaction system for vacuumizing, heating and removing water; (2) adding D,L-malic acid, a catalyst and a solvent into a reactor; vacuumizing and starting heating after the vacuum degree reaches 0.07 MPa or higher; adjusting a temperature to be risen to 110 to 120 DEG C steadily; preserving heat and reacting for 22 to 32 hours; and stopping heating as well as vacuumizing, wherein the vacuum degree of the reaction system needs to be stabilized over 1 mmHg in the process; and (3) dissolving a reaction product with tetrahydrofuran; adding the dissolved reaction product into cyclohexane, methylbenzene or a mixed solvent of the cyclohexane and the methylbenzene in an amount which is 20 to 50 times the volume of the tetrahydrofuran; and precipitating and drying a precipitate to obtain the poly(malic acid) material. In the method, the shortcoming that only the poly(malic acid) with relatively low molecular weight can be obtained by a conventional direct polymerization method is overcome; therefore, a rapid and economic preparation method is provided for obtaining the poly(malic acid) with relatively high molecular weight.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, in particular to a preparation method of a polymalic acid material. Background technique [0002] Biodegradable materials refer to polymer materials that degrade through the action of microorganisms in nature. Since it is biodegradable, it will not pollute the environment, and can be widely used in the fields of environment, medicine, health care products and the like. Polymalic acid (PMLA) is a class of biodegradable materials similar to polylactic acid. PMLA can be first degraded into oligomers by some microorganisms, then into monomers such as malic acid, and finally degraded into carbon dioxide and water. The degradation efficiency of PMLA is very fast, and it can be completely degraded into monomers after a few hours in the bacteria. PMLA is used as a drug carrier, and its carboxyl side group can be combined with the active group of the drug molecule. PMLA with a larger mole...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/06C08G63/78
Inventor 董坚卞忠华
Owner ZHANGJIAGANG CHAINENG BIOLOGICAL TECH