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Lactide synthesis method

A synthesis method and lactide technology, applied in the direction of organic chemistry and the like, can solve the problems of low comprehensive yield, low primary yield and purity of lactide, etc., and achieve the effects of saving resources, reducing the number of purifications, and increasing the output.

Active Publication Date: 2022-08-02
珠海格力新材料有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In view of the prior art, in the current synthesis process for producing lactide, lactide is directly obtained by cracking lactic acid oligomers, the primary yield and purity of lactide are low, and the comprehensive yield of recrystallization is low problem, provide a lactide synthesis method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] like figure 1 As shown, in the 250ml there-necked bottle 2, add 42ml of 98.5% polymer-grade lactic acid and 1.6ml of stannous octoate, put in the zeolite and the magnet, place the there-necked bottle in the oil bath 1, and connect the splash-proof ball 4 to one mouth It is used to collect moisture, one port is connected to double row pipe 3, which is used to pass nitrogen or vacuum, and the other port is closed (as shown in the figure). figure 1 a); turn on the magnetic stirring, slowly evacuate and raise the temperature to 120°C, the solution is slightly boiled, rotate the double row pipe 3 double inclined tee, pass nitrogen, and keep the state to remove free water for 2h; after 2h, prevent splashing There is no more water to collect in the ball, the temperature is raised to 175 ° C, and the dehydration is continued for 2 h in the state to generate lactic acid oligomers; replace the receiving device 5 (such as figure 1 b), the temperature was quickly raised to 240 ° C...

Embodiment 2

[0039] like figure 2 As shown, in the 250ml single-necked bottle 2, add 42ml of polymerization grade D-lactic acid and 1.6ml of stannous octoate, put into the magnet, place the single-necked bottle in the oil bath 1, connect the distillation head 6, the condenser tube 9, The end pipe 10, the collection bottle 11, the distillation head 6, and the end pipe 10 are connected to the double-row pipe vacuum / nitrogen system 3 (such as figure 2 a); turn on the magnetic stirring, slowly evacuate and raise the temperature to 120°C, then keep the vacuum, and dehydrate by refluxing for 3h; after 3h, no more water is generated in the condenser tube, the temperature is raised to 175°C, and the dehydration is maintained in a slightly boiling state for 2h, Generate lactic acid oligomers; disconnect the vacuum connection and pass nitrogen from the distillation head 12 (such as figure 2 b), the temperature was raised to 240°C quickly, the lactide was evaporated, and collected by nitrogen, no...

Embodiment 3

[0041] like image 3As shown, in the 250ml single-necked bottle 2, add 42ml of 98.5% polymer-grade lactic acid and 1.6ml of stannous octoate, add zeolite and a magnet, place the single-necked bottle in an oil bath, connect distillation head 6, distillation head 7, The distillation head 7 is connected to the inverted conical flask 8, the condenser tube 9, the tail pipe 10, and the spherical flask 11 (as shown in the figure). image 3 a); turn on the magnetic stirring, slowly evacuate and raise the temperature to 120°C, keep the micro-boiling state to dehydrate the free water for 2h; after 2h, no more water is collected in the spherical flask 11, the temperature is raised to 175°C, and the dehydration is continued in the state 2h, lactic acid oligomers are generated; then the distillation head 7 is rotated 180° to make the conical flask 8 downward (such as image 3 b), vacuumize and depressurize, quickly heat up the temperature to 240 ° C, generate lactide vapor, collect in the...

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Abstract

The invention provides a method for synthesizing lactide, which takes polymer-grade lactic acid as a raw material, removes free water, dehydrates and condenses under the action of a catalyst to form lactic acid oligomers, depolymerizes the lactic acid oligomers to form lactide, and the lactide is in When it is generated, it is collected by vacuuming and decompressing or blowing out with inert gas. The advantages of the present invention are: while synthesizing lactide, it is separated from the reaction system, and the reaction is promoted in the direction of the formation of lactide, the content of impurities in the product is reduced while the output is increased, and white and transparent lactide is obtained, The number of purifications is reduced and resources are saved.

Description

technical field [0001] The invention belongs to the technical field of polymer chemical substance synthesis, in particular to a method for synthesizing lactide. Background technique [0002] Polylactic acid is a chemically synthesized macromolecule biodegradable plastic, which is non-toxic and has good biocompatibility. The final products after its degradation are water and carbon dioxide, which can alleviate or even eliminate the pollution of plastics to the environment. Recyclable biodegradable material. [0003] Under the implementation of the global "plastic restriction order" and "plastic ban order", the demand for polylactic acid has grown rapidly, and there is huge room for replacement in the future. The molecular weight of polylactic acid directly affects the application range of polylactic acid, and it is difficult to obtain high molecular weight polylactic acid at present. Lactide is an important intermediate in the process of preparing polylactic acid, and high ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D319/12
CPCC07D319/12
Inventor 李璞珺刘冬丽冯飞王琳唐梓健刘磊
Owner 珠海格力新材料有限公司
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