CN111499844A - Medical polylactic acid and preparation method thereof - Google Patents
Medical polylactic acid and preparation method thereof Download PDFInfo
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- CN111499844A CN111499844A CN202010409375.9A CN202010409375A CN111499844A CN 111499844 A CN111499844 A CN 111499844A CN 202010409375 A CN202010409375 A CN 202010409375A CN 111499844 A CN111499844 A CN 111499844A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/06—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from hydroxycarboxylic acids
- C08G63/08—Lactones or lactides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/823—Preparation processes characterised by the catalyst used for the preparation of polylactones or polylactides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/87—Non-metals or inter-compounds thereof
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Abstract
The present disclosure provides a method for preparing medical polylactic acid, which comprises: preparing lactide monomer, catalyst and initiator, and mixing in a polymerization reaction container to obtain a mixture; heating the mixture to cause the lactide monomer to undergo polymerization under the action of the catalyst and the initiator, and obtaining a polymer; and drying the crude product of the polylactic acid to obtain the medical polylactic acid, wherein the weight average molecular weight of the medical polylactic acid is greater than or equal to 400KDa, the molar ratio of lactide monomer to catalyst in the mixture is 8000: 1 to 60000: 1, the molar ratio of lactide monomer to initiator in the mixture is 4000: 1 to 30000: 1, and the purity of the lactide monomer is 95% to 100%. According to the present disclosure, a medical polylactic acid capable of improving reaction efficiency and reducing cost and a preparation method thereof can be provided.
Description
The application is filed as3, 8 months in 2018Application No. is201810188924.7The invention is named asSuper-high-energy-consumption energy-saving device Preparation method of medical polylactic acid with high molecular weightDivisional application of the patent application.
Technical Field
The present disclosure relates to a medical polylactic acid and a preparation method thereof.
Background
Polylactic acid is a chemically synthesized biodegradable polymer material, has very good biocompatibility and good mechanical properties, and the degradation products of the polylactic acid are carbon dioxide and water, so the polylactic acid is safe, environment-friendly, non-toxic and harmless and has wide application in medical fields such as surgical operation sutures, surgical suturing nails, bone fixing materials, medical anti-adhesion membranes, drug release, tissue engineering scaffolds and the like. The high molecular weight polylactic acid is needed in the fields of surgical operation suture lines, surgical suturing nails and bone fixing materials, so that the excellent thermodynamic property of the materials can be ensured, and the polylactic acid can be applied to medical treatment as a high-strength high-performance material.
There are two main methods for synthesizing polylactic acid, the first is direct polycondensation of lactic acid to obtain polylactic acid, and the other is ring-opening polymerization of lactide to obtain polylactic acid. The first method has harsh reaction conditions, long reaction time, high temperature and high vacuum degree, and water in the product is difficult to remove due to the increase of the later reaction viscosity, so that the obtained polylactic acid has lower molecular weight. At present, the second method, namely, the medical polylactic acid is obtained by lactide monomer ring-opening polymerization, is generally adopted at home and abroad. However, in the ring-opening polymerization process of lactide, because the purity of monomers, the anhydrous oxygen-free degree and the reaction vacuum degree are not high enough, the polymerization reaction generally cannot obtain polylactic acid with ultrahigh molecular weight (weight average molecular weight ≧ 400 KDa).
In order to solve the problem of preparing the polylactic acid with the ultrahigh molecular weight, Chinese patent CN106279643A discloses a method for preparing the polylactic acid with the weight-average molecular weight of 350 KDa-410 KDa by dehydrating and polycondensing lactic acid to obtain a lactic acid oligomer, mixing the lactic acid oligomer with a catalyst, heating and reacting under a vacuum condition to obtain a polylactic acid intermediate product, continuously adding a chain extender HDI, and continuously heating and reacting under a vacuum condition.
Chinese patent CN104448261A discloses a method for preparing polylactic acid with weight-average molecular weight of 400-550 KDa by two-stage decompression high-temperature lactide ring-opening polymerization with bio-organic guanidine compound and nontoxic acid salt as catalyst, wherein the first stage is decompressed and polymerized to obtain polylactic acid with medium molecular weight, and the second stage is continuously heated and decompressed to obtain polylactic acid with weight-average molecular weight of 400-550 KDa.
The two preparation methods of the ultra-high molecular weight polylactic acid both need multi-step reaction, have complex process, huge energy consumption and higher production cost, and reaction reagents are not easy to obtain, such as the chain extender HDI mentioned in patent CN106279643A and the bio-organic guanidine compound catalyst mentioned in patent CN104448261A, which all need specific synthesis.
Disclosure of Invention
The present disclosure has been made in view of the above-described state of the art, and an object thereof is to provide a medical polylactic acid capable of improving reaction efficiency and reducing cost, and a method for producing the same.
To this end, an aspect of the present disclosure provides a method for preparing medical polylactic acid, which includes: preparing lactide monomer, catalyst and initiator, and mixing in a polymerization reaction container to obtain a mixture; heating the mixture to cause the lactide monomer to undergo polymerization under the action of the catalyst and the initiator, and obtaining a polymer; dissolving the polymer, and adding a poor solvent to precipitate a crude polylactic acid product; and drying the crude product of the polylactic acid to obtain the medical polylactic acid, wherein the weight average molecular weight of the medical polylactic acid is greater than or equal to 400KDa, the molar ratio of the lactide monomer to the catalyst in the mixture is 8000: 1 to 60000: 1, the molar ratio of the lactide monomer to the initiator is 4000: 1 to 30000: 1, and the purity of the lactide monomer is 95% to 100%. In one aspect of the present disclosure, a medical polylactic acid is synthesized using a lactide monomer, whereby it is possible to facilitate an improvement in production efficiency and a reduction in production cost, and the molecular weight of the synthesized medical polylactic acid is increased by selecting the purity of the lactide monomer and controlling the amounts of a catalyst and an initiator, so that a medical polylactic acid of a predetermined weight average molecular weight can be obtained.
In the preparation method related to one aspect of the present disclosure, optionally, the lactide monomer is a levorotatory lactide monomer or a dextrorotatory lactide monomer, the catalyst is a tin compound, and the initiator is an alcohol compound. In this case, the lactide monomer can be polymerized to form the medical polylactic acid, and the catalyst and the initiator can contribute to the polymerization reaction of the lactide monomer.
In the production method according to an aspect of the present disclosure, the polymer is optionally dissolved using dichloromethane or chloroform, and the poor solvent is ethanol, methanol, or isopropanol. This can dissolve the polymer and precipitate a crude polylactic acid product.
In the preparation method related to one aspect of the present disclosure, optionally, the catalyst is at least one of stannous octoate, stannous acetate, and stannous chloride, and the initiator is at least one of dodecanol, 1, 4-butanediol, and cyclohexanehexol.
In the preparation method related to one aspect of the present disclosure, optionally, the polymerization reaction is performed under anhydrous and oxygen-free conditions, and the polymerization reaction is performed in a vacuum atmosphere having a vacuum degree of 1 to 1000Pa, and the polymerization reaction is performed at 100 ℃ to 180 ℃ for 6 to 120 hours. This can increase the molecular weight of the medical polylactic acid obtained by the production.
In the production method according to an aspect of the present disclosure, optionally, a stirring treatment is maintained during the reaction of the polymerization reaction, and the stirring treatment is magnetic stirring. This enables the mixture to be sufficiently mixed and uniformly heated.
In the production method according to an aspect of the present disclosure, optionally, the polymerization reaction vessel is subjected to a tube sealing treatment using a high-temperature spray gun before the polymerization reaction occurs. This can increase the degree of vacuum in the polymerization reaction vessel, thereby ensuring that the polymerization reaction system is carried out in a sufficiently high vacuum environment.
In the production method according to an aspect of the present disclosure, optionally, before the polymerization reaction occurs, the polymerization reaction vessel is subjected to a vacuum-pumping water-removing oxygen-removing treatment. Thereby, the polymerization reaction can be carried out under anhydrous and oxygen-free conditions.
In the production method related to one aspect of the present disclosure, optionally, the polymerization reaction is performed in a vacuum atmosphere having a vacuum degree of 1 to 20Pa, and the polymerization reaction is performed at a temperature of 130 ℃ to 150 ℃ for 12 to 72 hours. This can further increase the molecular weight of the medical polylactic acid obtained by the production.
Another aspect of the present disclosure provides a medical polylactic acid prepared by the method for preparing any one of the above medical polylactic acids. In another aspect of the present disclosure, the medical polylactic acid is prepared by the above-described method for preparing medical polylactic acid, so that an ultra-high molecular weight medical polylactic acid can be obtained.
According to the present disclosure, a medical polylactic acid capable of improving reaction efficiency and reducing cost and a preparation method thereof can be provided.
Detailed Description
In order to explain the technical content, the objects and the effects of the present invention in detail, the following description will be given with reference to the embodiments.
The most key concept of the invention is as follows: the whole polymerization reaction process is carried out in an oxygen-free and water-free environment; the proportion of the monomers, the catalyst and the initiator is suitable, and the reaction conditions such as temperature, time and the like are suitable for controlling.
A method for preparing medical polylactic acid with ultrahigh molecular weight,
step 1: putting a lactide monomer, a catalyst and an initiator into a polymerization reaction container in a certain proportion;
step 2: heating to make the mixture in the polymerization reaction vessel perform polymerization reaction to obtain a polymer;
and step 3: dissolving the obtained polymer by using dichloromethane or trichloromethane, and adding a poor solvent to precipitate a crude polylactic acid product;
and 4, step 4: vacuum drying the precipitated crude polylactic acid product to obtain the ultrahigh molecular weight medical polylactic acid;
wherein, the step 1 and the step 2 are both carried out under the oxygen-free and water-free conditions;
in the step 1, the molar ratio of the lactide monomer to the catalyst is 8000-60000: 1, the molar ratio of lactide monomer to initiator is 4000-30000: 1; the purity of the lactide monomer is 95-100 percent;
the catalyst is at least one of stannous octoate, stannous acetate and stannous chloride; the initiator is at least one of dodecanol, 1, 4-butanediol and inositol;
and (3) carrying out the polymerization reaction in the step 2 in a vacuum environment with the pressure of 1-1000 Pa.
From the above description, the beneficial effects of the present invention are: compared with the preparation method for synthesizing the ultra-high molecular weight polylactic acid step by step in the prior art, the preparation method has the advantages that the preparation method is synthesized in one step, the segmented reaction is not needed, the production efficiency is improved, and the production cost is reduced; the high-purity lactide is used as a raw material, so that the vacuum degree of a reaction system is improved, and the synthesis of the polylactic acid with the ultrahigh molecular weight is facilitated; the tin compound is used as a catalyst, the alcohol compound is used as an initiator, the catalyst and the initiator have rich sources, no specific synthesis is needed, and the method is suitable for large-scale industrial production.
Further, the lactide monomer is a levorotatory lactide monomer or a dextrorotatory lactide monomer.
Further, in the step 2, the polymerization reaction is carried out at a temperature of 100 to 180 ℃.
Further, the polymerization reaction is carried out at a temperature of 130-150 ℃.
Further, in the step 2, the reaction time of the polymerization reaction is 6-120 h.
Further, the reaction time of the polymerization reaction is 12-72 h.
Further, the polymerization reaction in the step 2 is carried out in a vacuum environment with the pressure of 1-20 Pa.
Further, in step 3, the poor solvent is ethanol, methanol or isopropanol.
Further, in step 2, a high-temperature spray gun is used for sealing the polymerization reaction vessel.
As is apparent from the above description, the pipe sealing treatment of the polymerization vessel using the high-temperature lance can increase the degree of vacuum in the polymerization vessel, thereby ensuring that the polymerization system is carried out in a sufficiently high vacuum environment.
The comparative examples of the present invention are:
(a) under the anhydrous and anaerobic condition, 5kg of levorotatory lactide (L-lactide) is added into a polymerization reaction container, the purity of L-lactide is 92.5 percent, 1.40ml of stannous octoate and 1.98ml of dodecanol, L-lactide, stannous octoate and dodecanol are continuously added, the molar ratio of the lauryl octoate to the stannous octoate is 8000: 1: 2, and the polymerization reaction container is vacuumized to remove water and oxygen.
(b) Dissolving the monomer at 130 ℃, reacting for 48 hours under the low vacuum condition of 1000-30000 Pa, and stirring with magnetons in the reaction process.
(c) Dissolving the polymerization product by trichloromethane, and separating out absolute ethyl alcohol to obtain the polylactic acid with the weight-average molecular weight of 210 KDa.
Example 1
A preparation method of medical polylactic acid with ultrahigh molecular weight comprises the following specific steps:
(1) under the anhydrous and anaerobic condition, 5kg of levorotatory lactide (L-lactide) is added into a polymerization reaction bottle, the purity of L-lactide is 99.8 percent, 1.40ml of stannous octoate and 1.98ml of dodecanol, L-lactide, stannous octoate and dodecanol are continuously added, the molar ratio of the lauryl octoate to the stannous octoate is 8000: 1: 2, and the vacuum pumping is carried out to remove water and remove oxygen.
(2) Dissolving a monomer at 130 ℃, sealing a pipe by using a high-temperature spray gun under the high vacuum of 500-1000 Pa, ensuring the vacuum degree of a system, reacting for 48 hours, and stirring along with magnetons in the reaction process.
(3) The chloroform dissolves the polymerization product, and methanol is separated out to obtain the ultra-high molecular weight polylactic acid with the weight average molecular weight of 410 KDa.
Example 2
A preparation method of medical polylactic acid with ultrahigh molecular weight comprises the following specific steps:
(1) under the anhydrous and anaerobic condition, 5kg of levorotatory lactide (L-lactide) is added into a polymerization reaction bottle, the purity of L-lactide is 99.8 percent, 1.40ml of stannous octoate and 1.98ml of dodecanol, L-lactide, stannous octoate and dodecanol are continuously added, the molar ratio of the lauryl octoate to the stannous octoate is 8000: 1: 2, and the vacuum pumping is carried out to remove water and remove oxygen.
(2) Dissolving a monomer at 130 ℃, sealing a tube by using a high-temperature spray gun under high vacuum of 1-20 Pa, ensuring the vacuum degree of a system, reacting for 48 hours, and stirring along with magnetons in the reaction process.
(3) The chloroform dissolves the polymerization product, and the isopropanol is separated out to obtain the ultra-high molecular weight polylactic acid with the weight-average molecular weight of 490 KDa.
Example 3
A preparation method of medical polylactic acid with ultrahigh molecular weight comprises the following specific steps:
(1) under the anhydrous and anaerobic condition, 5kg of levorotatory lactide (L-lactide) is added into a polymerization reaction bottle, the purity of L-lactide is 99.8 percent, 1.40ml of stannous octoate and 1.98ml of dodecanol, L-lactide, stannous octoate and dodecanol are continuously added, the molar ratio of the lauryl octoate to the stannous octoate is 8000: 1: 2, and the vacuum pumping is carried out to remove water and remove oxygen.
(2) Dissolving a monomer at 130 ℃, sealing a tube by using a high-temperature spray gun under high vacuum of 1-20 Pa, ensuring the vacuum degree of a system, reacting for 72 hours, and stirring along with magnetons in the reaction process.
(3) Dissolving the polymerization product by the trichloromethane, and separating out absolute ethyl alcohol to obtain the ultra-high molecular weight polylactic acid with the weight-average molecular weight of 510 KDa.
Example 4
A preparation method of medical polylactic acid with ultrahigh molecular weight comprises the following specific steps:
(1) under the anhydrous and anaerobic condition, 5kg of D-lactide (D-lactide) with the purity of 96.5 percent is added into a polymerization reaction bottle. Adding 0.33ml stannous octoate and 0.46ml dodecanol, D-lactide, stannous chloride and 1, 4-butanediol at molar ratio of 34000: 1: 2. Vacuumizing to remove water and oxygen.
(2) Dissolving a monomer at 130 ℃, sealing a pipe by using a high-temperature spray gun under the high vacuum of 500-1000 Pa, ensuring the vacuum degree of a system, reacting for 48 hours, and stirring along with magnetons in the reaction process.
(3) Dissolving the polymerization product by the trichloromethane, and separating out absolute ethanol to obtain the ultra-high molecular weight polylactic acid with the weight-average molecular weight of 850 KDa.
Example 5
A preparation method of medical polylactic acid with ultrahigh molecular weight comprises the following specific steps:
(4) under the anhydrous and anaerobic condition, 5kg of D-lactide (D-lactide) with the purity of 99.9 percent is added into a polymerization reaction bottle. Adding 0.33ml stannous octoate and 0.46ml dodecanol, D-lactide, stannous chloride and 1, 4-butanediol at molar ratio of 34000: 1: 2. Vacuumizing to remove water and oxygen.
(5) Dissolving a monomer at 130 ℃, sealing a pipe by using a high-temperature spray gun under the high vacuum of 500-1000 Pa, ensuring the vacuum degree of a system, reacting for 48 hours, and stirring along with magnetons in the reaction process.
(6) The chloroform dissolves the polymerization product, and methanol is separated out to obtain the ultra-high molecular weight polylactic acid with the weight average molecular weight of 1050 KDa.
Example 6
A preparation method of medical polylactic acid with ultrahigh molecular weight comprises the following specific steps:
(1) under the anhydrous and anaerobic condition, 5kg of D-lactide (D-lactide) with the purity of 99.9 percent is added into a polymerization reaction bottle. Adding 0.33ml stannous octoate and 0.46ml dodecanol, D-lactide, stannous chloride and 1, 4-butanediol at molar ratio of 34000: 1: 2. Vacuumizing to remove water and oxygen.
(2) Dissolving a monomer at 130 ℃, sealing a tube by using a high-temperature spray gun under high vacuum of 1-20 Pa, ensuring the vacuum degree of a system, reacting for 48 hours, and stirring along with magnetons in the reaction process.
(3) The chloroform dissolves the polymerization product, and the isopropanol is separated out to obtain the ultra-high molecular weight polylactic acid with the weight average molecular weight of 1650 KDa.
Example 7
A preparation method of medical polylactic acid with ultrahigh molecular weight comprises the following specific steps:
(1) under the anhydrous and anaerobic conditions, 5kg of levorotatory lactide (L-lactide) is added into a polymerization reaction bottle, the purity of L-lactide is 95.8%, 0.19ml of stannous octoate and 0.26ml of dodecanol, L-lactide, stannous acetate and inositol are continuously added, the molar ratio of the cyclohexanehexol is 60000: 1: 2, and the polymerization reaction bottle is vacuumized to remove water and oxygen.
(2) Dissolving a monomer at 130 ℃, sealing a pipe by using a high-temperature spray gun under the high vacuum of 500-1000 Pa, ensuring the vacuum degree of a system, reacting for 48 hours, and stirring along with magnetons in the reaction process.
(3) The chloroform dissolves the polymerization product and methanol is precipitated to obtain the ultra-high molecular weight polylactic acid with the weight-average molecular weight of 1125 KDa.
Example 8
A preparation method of medical polylactic acid with ultrahigh molecular weight comprises the following specific steps:
(1) under the anhydrous and anaerobic conditions, 5kg of levorotatory lactide (L-lactide) is added into a polymerization reaction bottle, the purity of L-lactide is 99.9%, 0.19ml of stannous octoate and 0.26ml of dodecanol, L-lactide, stannous acetate and inositol are continuously added, the molar ratio of the cyclohexanehexol is 60000: 1: 2, and the polymerization reaction bottle is vacuumized to remove water and oxygen.
(2) Dissolving a monomer at 130 ℃, sealing a pipe by using a high-temperature spray gun under the high vacuum of 500-1000 Pa, ensuring the vacuum degree of a system, reacting for 48 hours, and stirring along with magnetons in the reaction process.
(3) Dissolving the polymerization product by trichloromethane, and precipitating by isopropanol to obtain the ultra-high molecular weight polylactic acid with the weight-average molecular weight of 1670 KDa.
Example 9
A preparation method of medical polylactic acid with ultrahigh molecular weight comprises the following specific steps:
(1) under the anhydrous and anaerobic conditions, 5kg of levorotatory lactide (L-lactide) is added into a polymerization reaction bottle, the purity of L-lactide is 99.9%, 0.19ml of stannous octoate and 0.26ml of dodecanol, L-lactide, stannous acetate and inositol are continuously added, the molar ratio of the cyclohexanehexol is 60000: 1: 2, and the polymerization reaction bottle is vacuumized to remove water and oxygen.
(2) Dissolving a monomer at 130 ℃, sealing a tube by using a high-temperature spray gun under high vacuum of 1-20 Pa, ensuring the vacuum degree of a system, reacting for 48 hours, and stirring along with magnetons in the reaction process.
(3) Dissolving the polymerization product with trichloromethane, and precipitating with anhydrous ethanol to obtain the ultra-high molecular weight polylactic acid with weight average molecular weight of 2160 KDa.
In conclusion, the preparation method of the medical polylactic acid provided by the invention is different from the preparation method for synthesizing the ultra-high molecular weight polylactic acid step by step in the prior art, and the preparation method is synthesized in one step without sectional reaction, thereby being beneficial to improving the production efficiency and reducing the production cost; the high-purity lactide is used as a raw material, so that the vacuum degree of a reaction system is improved, and the synthesis of the polylactic acid with the ultrahigh molecular weight is facilitated; the tin compound is used as a catalyst, the alcohol compound is used as an initiator, the catalyst and the initiator have rich sources, no specific synthesis is needed, and the method is suitable for large-scale industrial production. The high-temperature spray gun is adopted to seal the polymerization reaction vessel, so that the vacuum degree in the polymerization reaction vessel can be improved, and the polymerization reaction system is ensured to be carried out in a high enough vacuum environment.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention in the specification or directly or indirectly applied to the related technical field are included in the scope of the present invention.
Claims (10)
1. A preparation method of medical polylactic acid is characterized in that,
the method comprises the following steps:
preparing lactide monomer, catalyst and initiator, and mixing in a polymerization reaction container to obtain a mixture;
heating the mixture to cause the lactide monomer to undergo polymerization under the action of the catalyst and the initiator, and obtaining a polymer;
dissolving the polymer, and adding a poor solvent to precipitate a crude polylactic acid product; and is
Drying the crude polylactic acid product to obtain the medical polylactic acid, wherein the weight average molecular weight of the medical polylactic acid is more than or equal to 400KDa,
wherein, in the mixture, the molar ratio of the lactide monomer to the catalyst is 8000: 1 to 60000: 1, the molar ratio of the lactide monomer to the initiator is 4000: 1 to 30000: 1, and the purity of the lactide monomer is 95% to 100%.
2. The production method according to claim 1,
the lactide monomer is a levorotatory lactide monomer or a dextrorotatory lactide monomer, the catalyst is a tin compound, and the initiator is an alcohol compound.
3. The production method according to claim 1,
the polymer is dissolved using dichloromethane or chloroform, and the poor solvent is ethanol, methanol or isopropanol.
4. The production method according to claim 1 or 2,
the catalyst is at least one of stannous octoate, stannous acetate and stannous chloride, and the initiator is at least one of dodecanol, 1, 4-butanediol and cyclohexanehexol.
5. The production method according to claim 1,
the polymerization reaction is carried out under anhydrous and oxygen-free conditions, and the polymerization reaction is carried out in a vacuum environment with a vacuum degree of 1 to 1000Pa, and the polymerization reaction is carried out under conditions of 100 ℃ to 180 ℃ for 6 to 120 hours.
6. The production method according to claim 1,
and maintaining stirring treatment during the reaction process of the polymerization reaction, wherein the stirring treatment is magneton stirring.
7. The production method according to claim 1,
and before the polymerization reaction occurs, performing pipe sealing treatment on the polymerization reaction container by using a high-temperature spray gun.
8. The production method according to claim 1 or 5,
before the polymerization reaction occurs, the polymerization reaction container is subjected to vacuumizing, water removing and oxygen removing treatment.
9. The production method according to claim 1 or 5,
the polymerization reaction is performed in a vacuum atmosphere having a degree of vacuum of 1 to 20Pa, and the polymerization reaction is performed at a temperature of 130 ℃ to 150 ℃ for 12 to 72 hours.
10. A medical polylactic acid is characterized in that,
prepared by the method for preparing the medical polylactic acid according to any one of the claims 1 to 9.
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| CN113512181A (en) * | 2021-08-09 | 2021-10-19 | 重庆大学 | Polylactic acid capable of being processed at low temperature and preparation method thereof |
| CN114773811A (en) * | 2022-06-27 | 2022-07-22 | 广东美联新材料股份有限公司 | Color master batch taking polylactic acid recovered waste material as carrier and preparation method thereof |
| CN115433349A (en) * | 2021-06-03 | 2022-12-06 | 中国科学技术大学 | Polylactic acid zwitterionic compound, synthetic method and application |
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| CN109762144B (en) * | 2018-12-19 | 2021-04-27 | 四川大学 | Ultraviolet-resistant polylactic acid material synthesized based on natural compound |
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| CN111499844B (en) | 2022-12-09 |
| CN108285528B (en) | 2020-06-12 |
| CN108285528A (en) | 2018-07-17 |
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