CN113350179A - Freezing low-temperature ball milling preparation method of polylactic acid soft tissue filling micron particles - Google Patents
Freezing low-temperature ball milling preparation method of polylactic acid soft tissue filling micron particles Download PDFInfo
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- CN113350179A CN113350179A CN202110636437.4A CN202110636437A CN113350179A CN 113350179 A CN113350179 A CN 113350179A CN 202110636437 A CN202110636437 A CN 202110636437A CN 113350179 A CN113350179 A CN 113350179A
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- ball milling
- freezing
- polylactic acid
- soft tissue
- liquid nitrogen
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61J—CONTAINERS SPECIALLY ADAPTED FOR MEDICAL OR PHARMACEUTICAL PURPOSES; DEVICES OR METHODS SPECIALLY ADAPTED FOR BRINGING PHARMACEUTICAL PRODUCTS INTO PARTICULAR PHYSICAL OR ADMINISTERING FORMS; DEVICES FOR ADMINISTERING FOOD OR MEDICINES ORALLY; BABY COMFORTERS; DEVICES FOR RECEIVING SPITTLE
- A61J3/00—Devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms
- A61J3/02—Devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms into the form of powders
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/10—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with one or a few disintegrating members arranged in the container
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- Engineering & Computer Science (AREA)
- Animal Behavior & Ethology (AREA)
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Abstract
The invention discloses a freezing low-temperature ball milling preparation method of polylactic acid soft tissue filling micron particles, which comprises the following steps: step a), subpackaging; step b) freezing; step c) grinding; step d), sorting; step e) preparing a solution; step f), mixing; step g) freeze drying; step a) subpackaging: weighing a certain amount of polylactic acid raw material particles, placing the materials in a ball milling tank, adding a grinding ball, sealing a cover, and freezing in the step b): the canister containing the resin particles is placed in a liquid nitrogen tank, and the liquid nitrogen tank is placed in a refrigerator. According to the invention, polylactic acid raw material particles are subjected to sub-packaging, grinding and sorting, and then the treated polylactic acid is improved by freezing and mixing, so that the refinement of polylactic acid production steps can be improved, the production difficulty is reduced, and the problems that the existing polylactic acid preparation method is complicated, is inconvenient to popularize and cannot meet the use requirements of the existing beauty and plastic industry are solved.
Description
Technical Field
The invention relates to the technical field of beauty medicines, in particular to a method for preparing polylactic acid soft tissue filling micron particles by freezing and low-temperature ball milling.
Background
Hyaluronic acid and the like are mostly used in the existing beauty and plastic industry, but the hyaluronic acid has the defect of short maintenance time and can be absorbed by a human body usually in 6-12 months after injection, so that a part of the plastic industry selects polylactic acid injection to stimulate the regeneration of facial deep bone collagen, but the existing polylactic acid preparation method is complicated, is inconvenient to popularize and cannot meet the use requirements of the existing beauty and plastic industry.
Disclosure of Invention
In order to solve the problems in the background art, the invention aims to provide a method for preparing polylactic acid soft tissue filling micron particle freezing low-temperature ball milling, which has the advantage of simple preparation method and solves the problems that the existing polylactic acid preparation method is complicated, is inconvenient to popularize and cannot meet the use requirements of the existing beauty and plastic industry.
In order to achieve the purpose, the invention provides the following technical scheme: a method for preparing polylactic acid soft tissue filling micron particle freezing low temperature ball milling comprises the following steps: step a), subpackaging; step b) freezing; step c) grinding; step d), sorting; step e) preparing a solution; step f), mixing; step g) freeze drying;
step a) subpackaging: weighing a certain amount of polylactic acid raw material particles, placing the materials in a ball milling tank, adding a grinding ball, and sealing a cover;
step b) freezing: placing the ball tank containing the resin particles in a liquid nitrogen tank, and placing the liquid nitrogen tank in a refrigerator;
step c) grinding: assembling the two ball milling tanks into the ball mill and starting the ball mill for ball milling;
step d), sorting: taking a proper amount of distilled water, washing the materials in the ball milling tank into a beaker, and selecting a proper filter sieve to filter the solution into another beaker to obtain a filtrate;
step e) preparing a solution: dissolving 2-4% of mannitol, 0.2-0.4% of sodium carboxymethyl cellulose solution and 0.05-0.25% of triple hyaluronic acid to generate a required solution;
step f) mixing: filtering the filtrate in vacuum to obtain a filter cake, and then putting the filter cake into a prepared solution for mixing to obtain a suspension;
step g) freeze drying: and (4) freeze-drying the suspension to obtain a final product.
Preferably, in the step a), the ball milling jar is divided, and the weight of the ball milling jar after the division is weighed before assembly, wherein the weight of the ball milling jar needs to be approximately balanced.
Preferably, in the step b), during freezing, when liquid nitrogen is input into a liquid nitrogen tank, the liquid nitrogen discharging amount is taken into consideration, so that the liquid nitrogen is ensured to flow over the ball milling tank.
Preferably, in the step b), the freezing time of the liquid nitrogen tank is 30min-2h, and the freezing temperature is lower than zero.
Preferably, the step c) of grinding is repeated 1 to 2 times for 15 to 20 minutes.
Preferably, in the step d), the material which is not screened by the filter screen is subjected to vacuum drying and then is subjected to ball milling to reach a qualified size.
Preferably, in the step f), the filter paper has a pore size of 1-5 um.
Preferably, in the step g), the suspension is freeze-dried for 24 hours or more.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, polylactic acid raw material particles are subjected to sub-packaging, grinding and sorting, and then the processed polylactic acid is improved by freezing and mixing, so that the refinement of the polylactic acid production steps can be improved, the production difficulty is reduced, scientific and beneficial production steps are formed, and the problems that the existing polylactic acid preparation method is complicated, is inconvenient to popularize and cannot meet the use requirements of the existing beauty and plastic industry are solved.
Drawings
FIG. 1 is a schematic view of the preparation process of the present invention;
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1, the method for preparing polylactic acid soft tissue filling microparticles by freezing and low-temperature ball milling comprises the following steps: step a), subpackaging; step b) freezing; step c) grinding; step d), sorting; step e) preparing a solution; step f), mixing; step g) freeze drying;
step a) subpackaging: weighing a certain amount of polylactic acid raw material particles, placing the materials in a ball milling tank, adding a grinding ball, and sealing a cover;
step b) freezing: placing the ball tank containing the resin particles in a liquid nitrogen tank, and placing the liquid nitrogen tank in a refrigerator;
step c) grinding: assembling the two ball milling tanks into the ball mill and starting the ball mill for ball milling;
step d), sorting: taking a proper amount of distilled water, washing the materials in the ball milling tank into a beaker, and selecting a proper filter sieve to filter the solution into another beaker to obtain a filtrate;
step e) preparing a solution: dissolving 2-4% of mannitol, 0.2-0.4% of sodium carboxymethyl cellulose solution and 0.05-0.25% of triple hyaluronic acid to generate a required solution;
step f) mixing: filtering the filtrate in vacuum to obtain a filter cake, and then putting the filter cake into a prepared solution for mixing to obtain a suspension;
step g) freeze drying: and (4) freeze-drying the suspension to obtain a final product.
The invention is further arranged that step a) of sub-packaging, the weight of the ball milling jar after packaging is weighed before assembly, and the weight of the ball milling jar needs to be approximately balanced.
The invention is further set in the step b) for freezing, and when liquid nitrogen is input into the liquid nitrogen tank, the liquid nitrogen discharging amount is taken into consideration so as to ensure that the liquid nitrogen overflows the ball milling tank.
The invention is further set in that the step b) is freezing, the freezing time of the liquid nitrogen tank is 30min-2h, and the freezing temperature is lower than zero.
The invention is further configured that step c) is carried out for 15-20 minutes, and the process is repeated 1-2 times.
The invention is further set in that the materials which are not screened by the filter screen are subjected to ball milling after being subjected to vacuum drying in the step d) for sorting so as to reach the qualified size.
The invention is further configured that step f) mixing, the pore size of the filter paper is between 1-5 um.
The invention is further configured that step g) is freeze-dried and the suspension is freeze-dried for more than 24 hours.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A polylactic acid soft tissue filling micron particle freezing low-temperature ball milling preparation method is characterized in that: the method comprises the following steps: step a), subpackaging; step b) freezing; step c) grinding; step d), sorting; step e) preparing a solution; step f), mixing; step g) freeze drying;
step a) subpackaging: weighing a certain amount of polylactic acid raw material particles, placing the materials in a ball milling tank, adding a grinding ball, and sealing a cover;
step b) freezing: placing the ball tank containing the resin particles in a liquid nitrogen tank, and placing the liquid nitrogen tank in a refrigerator;
step c) grinding: assembling the two ball milling tanks into the ball mill and starting the ball mill for ball milling;
step d), sorting: taking a proper amount of distilled water, washing the materials in the ball milling tank into a beaker, and selecting a proper filter sieve to filter the solution into another beaker to obtain a filtrate;
step e) preparing a solution: dissolving 2-4% of mannitol, 0.2-0.4% of sodium carboxymethyl cellulose solution and 0.05-0.25% of triple hyaluronic acid to generate a required solution;
step f) mixing: filtering the filtrate in vacuum to obtain a filter cake, and then putting the filter cake into a prepared solution for mixing to obtain a suspension;
step g) freeze drying: and (4) freeze-drying the suspension to obtain a final product.
2. The method for preparing polylactic acid soft tissue filling micron particles by freezing and low-temperature ball milling according to claim 1, which is characterized in that: and b) subpackaging, namely weighing the weight of the ball milling tank after the subpackaging is finished before assembling, wherein the weight of the ball milling tank needs to be approximately balanced.
3. The method for preparing polylactic acid soft tissue filling micron particles by freezing and low-temperature ball milling according to claim 1, which is characterized in that: and c) freezing in the step b), and when liquid nitrogen is input into the liquid nitrogen tank, paying attention to the liquid discharge amount of the liquid nitrogen so as to ensure that the liquid nitrogen overflows the ball milling tank.
4. The method for preparing polylactic acid soft tissue filling micron particles by freezing and low-temperature ball milling according to claim 1, which is characterized in that: and c) freezing in the step b), wherein the freezing time of the liquid nitrogen tank is 30min-2h, and the freezing temperature is lower than zero.
5. The method for preparing polylactic acid soft tissue filling micron particles by freezing and low-temperature ball milling according to claim 1, which is characterized in that: the step c) of grinding is repeated for 1 to 2 times, wherein the ball time is 15 to 20 minutes.
6. The method for preparing polylactic acid soft tissue filling micron particles by freezing and low-temperature ball milling according to claim 1, which is characterized in that: and d) sorting, namely continuously performing ball milling on the materials which are not screened by the filter screen after vacuum drying to reach the qualified size.
7. The method for preparing polylactic acid soft tissue filling micron particles by freezing and low-temperature ball milling according to claim 1, which is characterized in that: and f) mixing, wherein the aperture of the filter paper is between 1 and 5 um.
8. The method for preparing polylactic acid soft tissue filling micron particles by freezing and low-temperature ball milling according to claim 1, which is characterized in that: step g) freeze drying, wherein the suspension is freeze dried for more than 24 h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110636437.4A CN113350179A (en) | 2021-06-08 | 2021-06-08 | Freezing low-temperature ball milling preparation method of polylactic acid soft tissue filling micron particles |
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| CN202110636437.4A CN113350179A (en) | 2021-06-08 | 2021-06-08 | Freezing low-temperature ball milling preparation method of polylactic acid soft tissue filling micron particles |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104147640A (en) * | 2013-05-16 | 2014-11-19 | 吴学森 | Poly-d-lactic acid micro-nano particle as cosmetic and plastic filler and preparation method thereof |
| CN104292476A (en) * | 2014-10-09 | 2015-01-21 | 嘉兴凯泰生物材料有限公司 | Preparation method of polylactic acid filling particles |
| CN105412990A (en) * | 2015-12-27 | 2016-03-23 | 常州亚环环保科技有限公司 | Preparation method for asperosaponin-chitosan-promoted bone meal-polylactic acid-integrated aggregate stent |
| CN110841108A (en) * | 2019-12-27 | 2020-02-28 | 南京思元医疗技术有限公司 | Preparation method of polylactic acid microparticles and injectable soft tissue filler |
| CN111249525A (en) * | 2020-03-25 | 2020-06-09 | 宁波赛缪斯生物科技有限公司 | Injectable facial filler composition gel for cosmetic and plastic surgery and preparation method thereof |
| CN111298196A (en) * | 2020-03-27 | 2020-06-19 | 常州药物研究所有限公司 | Polylactic acid porous microsphere, preparation method and application thereof |
-
2021
- 2021-06-08 CN CN202110636437.4A patent/CN113350179A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104147640A (en) * | 2013-05-16 | 2014-11-19 | 吴学森 | Poly-d-lactic acid micro-nano particle as cosmetic and plastic filler and preparation method thereof |
| CN104292476A (en) * | 2014-10-09 | 2015-01-21 | 嘉兴凯泰生物材料有限公司 | Preparation method of polylactic acid filling particles |
| CN105412990A (en) * | 2015-12-27 | 2016-03-23 | 常州亚环环保科技有限公司 | Preparation method for asperosaponin-chitosan-promoted bone meal-polylactic acid-integrated aggregate stent |
| CN110841108A (en) * | 2019-12-27 | 2020-02-28 | 南京思元医疗技术有限公司 | Preparation method of polylactic acid microparticles and injectable soft tissue filler |
| CN111249525A (en) * | 2020-03-25 | 2020-06-09 | 宁波赛缪斯生物科技有限公司 | Injectable facial filler composition gel for cosmetic and plastic surgery and preparation method thereof |
| CN111298196A (en) * | 2020-03-27 | 2020-06-19 | 常州药物研究所有限公司 | Polylactic acid porous microsphere, preparation method and application thereof |
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Application publication date: 20210907 |