CN114163793A - Chitosan antibacterial outer surface modified polylactic acid extrusion wire and preparation method thereof - Google Patents
Chitosan antibacterial outer surface modified polylactic acid extrusion wire and preparation method thereof Download PDFInfo
- Publication number
- CN114163793A CN114163793A CN202111428453.0A CN202111428453A CN114163793A CN 114163793 A CN114163793 A CN 114163793A CN 202111428453 A CN202111428453 A CN 202111428453A CN 114163793 A CN114163793 A CN 114163793A
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- CN
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- polylactic acid
- chitosan
- screw extruder
- wire
- surface modified
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- Pending
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- 229920000747 poly(lactic acid) Polymers 0.000 title claims abstract description 44
- 239000004626 polylactic acid Substances 0.000 title claims abstract description 44
- 229920001661 Chitosan Polymers 0.000 title claims abstract description 43
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 25
- 238000001125 extrusion Methods 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 239000004970 Chain extender Substances 0.000 claims abstract description 13
- 239000000945 filler Substances 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 229920002101 Chitin Polymers 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 230000006196 deacetylation Effects 0.000 claims description 2
- 238000003381 deacetylation reaction Methods 0.000 claims description 2
- -1 small molecule diol Chemical class 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 230000000845 anti-microbial effect Effects 0.000 claims 3
- 239000000454 talc Substances 0.000 claims 1
- 229910052623 talc Inorganic materials 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 19
- 241000894006 Bacteria Species 0.000 abstract description 6
- 241000222122 Candida albicans Species 0.000 abstract description 6
- 241000588724 Escherichia coli Species 0.000 abstract description 6
- 241000191967 Staphylococcus aureus Species 0.000 abstract description 6
- 229940095731 candida albicans Drugs 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 4
- 235000013305 food Nutrition 0.000 abstract description 3
- 150000004676 glycans Chemical class 0.000 description 8
- 229920001282 polysaccharide Polymers 0.000 description 8
- 239000005017 polysaccharide Substances 0.000 description 8
- 230000004048 modification Effects 0.000 description 6
- 238000012986 modification Methods 0.000 description 6
- 230000020176 deacylation Effects 0.000 description 4
- 238000005947 deacylation reaction Methods 0.000 description 4
- 239000002861 polymer material Substances 0.000 description 3
- 239000011258 core-shell material Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 2
- ACCCMOQWYVYDOT-UHFFFAOYSA-N hexane-1,1-diol Chemical group CCCCCC(O)O ACCCMOQWYVYDOT-UHFFFAOYSA-N 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical group CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/04—Polyesters derived from hydroxycarboxylic acids, e.g. lactones
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/05—Filamentary, e.g. strands
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/285—Feeding the extrusion material to the extruder
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Extrusion Moulding Of Plastics Or The Like (AREA)
Abstract
The invention discloses a chitosan antibacterial outer surface modified polylactic acid extrusion wire and a preparation method thereof, wherein the wire comprises the following components in parts by mass: 70-95% of polylactic acid, 0-20% of powder filler, 0-5% of chain extender and 5-10% of chitosan, wherein the polylactic acid extrusion wire is subjected to blending extrusion processing by adopting a co-rotating double-screw extruder or a single-screw extruder, and the chitosan antibacterial component is mainly accumulated on the outer surface of the wire by using 2/3 sections of tail end screw side feeding technology, so that the outer surface has excellent antibacterial property and biocompatibility, and meanwhile, the excellent mechanical property of the polylactic acid material of the wire body is not influenced, and the polylactic acid extrusion molding characteristics such as good processing flowability and suitability are realized; the obtained product has good biocompatibility, has the bacteriostasis rate of more than 70 percent on three typical bacteria such as candida albicans, escherichia coli, staphylococcus aureus and the like, and can be widely used in various food, health and medical scenes.
Description
Technical Field
The invention relates to a chitosan antibacterial outer surface modified polylactic acid extruded wire and a preparation method thereof, belonging to the field of medical polymer materials and products.
Background
Polylactic acid materials have gradually replaced traditional plastics such as PE, PVC, etc. to become one of the mainstream materials in daily use chemicals, packaging, and hygiene fields due to its excellent biocompatibility and environmental protection and degradability. However, aiming at some special performance requirements of the extruded wire material, the modification and processing technology, the formula and the like of the polylactic acid material are still not as mature and reliable as the traditional high polymer material, and especially the important antibacterial performance in food, medical materials and products has great development space for the modification technical means of the polylactic acid material.
In combination with the development of molecular antibacterial technology in recent years, the modified polymer materials with excellent antibacterial property by utilizing natural polysaccharides such as chitosan and cellulose have become important schemes for antibacterial modification technology and formula, so the natural polysaccharide modified polylactic acid material naturally becomes a technical means which is easy to be thought by the skilled person: for example, chinese patent CN201110113519.7 discloses a method for preparing a composite material added with chitosan modified polylactic acid.
However, natural polysaccharides are basically water-soluble polymers, and have very poor compatibility with polylactic acid materials, and the mechanical properties and the processability of the polylactic acid materials are seriously influenced by directly adding a material matrix and uniformly dispersing, and in addition, the antibacterial components of the polysaccharides can play an antibacterial role only by being distributed on the surface of the materials, but the antibacterial components are not significant by being uniformly distributed in the matrix materials, so that the performance is influenced, the antibacterial effect cannot be effectively played, and the cost is increased.
Disclosure of Invention
The invention aims to solve the technical problems of performance reduction and insufficient antibacterial effect caused by the chitosan modified polylactic acid.
In order to achieve the above object, in a first aspect, the present invention provides a chitosan antibacterial outer surface modified polylactic acid extruded wire, comprising the following components by mass: 70-95% of polylactic acid, 0-20% of powder filler, 0-5% of chain extender and 5-10% of chitosan.
Further, the powder filler is one or more of talcum powder, calcium carbonate powder and plasticized starch.
Further, the chain extender is a small molecule diol containing 2 to 10 carbon atoms.
Further, the chitosan is a chitin derivative with a degree of deacetylation in the range of 80-100%.
Further, the chitosan is mainly distributed on the outer surface of the wire rod.
Further, the content of the chitosan in the range of 0.3mm of the outer layer of the wire rod accounts for more than 70% of the total weight of the wire rod.
In a second aspect, the invention provides a preparation method of a chitosan antibacterial outer surface modified polylactic acid extruded wire, which comprises the following steps: (1) adding corresponding parts of polylactic acid and chain extender into a reaction kettle, stirring for 30-60 minutes at 85-105 ℃, and injecting into a screw extruder through a mixing and batching system; (2) simultaneously adding powder filler with corresponding weight at a feeding port of the single-screw extruder through a metering pump; (3) adding a side-feed sleeve at section 2/3 of the number of sections of the sleeve combination of the screw extruder, said section 2/3 being rounded to the value of the whole; (4) a corresponding portion of the chitosan component was fed through the side-feed feeder sleeve.
According to theoretical analysis and a large number of earlier experiments, when materials are fed in a side face mode, the materials in a cylinder are fully plasticized, the flowability is good, the materials which are just fed need to be plasticized for a certain time, when the flowability is poor, the materials are concentrated on the outer side of a cylinder cavity due to the low propelling speed, the materials and main materials form layering of a core-shell structure, after about 1/3 strokes, side feeding is fully plasticized, products which are good in plastic forming are extruded from a die head, early feeding can lead to full blending, the core-shell structure disappears, late feeding can lead to insufficient plasticizing of auxiliary materials, and extruded sections are poor.
Specifically, if the number of segments combined in the single screw extruder or co-rotating twin screw extruder barrel is 8, then 8 × 2/3 ≈ 5.33, rounded to an integer of 5, i.e. the side-feeding barrel is provided at the 5 th barrel of the single screw extruder or co-rotating twin screw extruder.
Further, the number of the combined sections of the screw extruder sleeve in the step (3) is 6, and the side-feeding sleeve is arranged at the 4 th section of the screw extruder sleeve.
Further, the screw extruder in the step (2) is a co-rotating twin-screw extruder or a single-screw extruder.
Compared with the prior art, the invention has the beneficial effects that:
the antibacterial component chitosan is mainly accumulated on the outer surface of the wire rod, so that the outer surface in contact with human tissues has excellent antibacterial property and biocompatibility, does not influence the excellent mechanical property of the polylactic acid material of the wire rod main body, has good processing fluidity, is suitable for extrusion molding and the like; the wire rod has good biocompatibility, the bacteriostasis rate of the outer surface of the wire rod to three typical bacteria such as candida albicans, escherichia coli, staphylococcus aureus and the like is more than or equal to 70%, and the wire rod can be widely used in various food, health and medical scenes.
Detailed Description
The present invention will now be described in further detail with reference to examples, but the present invention is not limited to the following examples, and any modifications made thereto will fall within the scope of the present invention.
Example 1:
a chitosan outer surface modified polylactic acid extrusion wire comprises the following components: 70% of polylactic acid, 18% of talcum powder filler, 2% of hexanediol chain extender and 10% of chitosan with the deacylation degree of 80%.
The extruded strand was processed as follows: (1) adding polylactic acid and a chain extender into a reaction kettle, stirring for 30 minutes at the temperature of 85 ℃, and injecting into a co-rotating double-screw extruder through a mixing and batching system; (2) simultaneously adding powder filler into a feeding port of the co-rotating double-screw extruder through a metering pump; (3) a6-sleeve co-rotating double-screw extruder is selected, a side feeding sleeve is adopted at the fourth sleeve, and the corresponding amount of chitosan component is fed.
The final extrusion molding wire rod is measured, the content of polysaccharide in the outer layer of the wire rod within the thickness range of 0.3mm accounts for 92 +/-2% of the total weight of the wire rod, and the bacteriostasis rate of the wire rod on three typical bacteria such as candida albicans, escherichia coli, staphylococcus aureus and the like reaches 85 +/-2%.
Example 2:
a chitosan outer surface modified polylactic acid extrusion wire comprises the following components: 80% of polylactic acid, 10% of calcium carbonate filler, 2% of hexanediol chain extender and 8% of chitosan with the deacylation degree of 80%.
The extruded strand was processed as follows: the extruded strand was processed as follows: (1) adding polylactic acid and a chain extender into a reaction kettle, stirring for 30 minutes at the temperature of 105 ℃, and injecting into a single-screw extruder through a mixing and batching system; (2) simultaneously adding powder filler into a feeding port of the single-screw extruder through a metering pump; (3) an 8-sleeve single-screw extruder is selected, a side-feeding sleeve is adopted at the fifth sleeve, and the chitosan component with the corresponding weight is fed.
The final extrusion molding wire rod is measured, the polysaccharide content in the outer layer of the wire rod within the thickness range of 0.3mm accounts for 90 +/-2 percent of the total weight of the wire rod, and the bacteriostasis rate of the wire rod on three typical bacteria such as candida albicans, escherichia coli, staphylococcus aureus and the like reaches 77 +/-2 percent.
Example 3:
a chitosan outer surface modified polylactic acid extrusion wire comprises the following components: 85% of polylactic acid, 5% of butanediol chain extender and 10% of chitosan with the deacylation degree of 90%.
The extruded strand was processed as follows: the extruded strand was processed as follows: (1) adding polylactic acid and a chain extender into a reaction kettle, stirring for 50 minutes at the temperature of 85 ℃, and injecting into a single-screw extruder through a mixing and batching system; (2) a12-sleeve single-screw extruder is selected, a side-feeding sleeve is adopted at the eighth sleeve, and the corresponding amount of chitosan component is fed.
The final extrusion molding wire rod is measured, the polysaccharide content in the outer layer of the wire rod within the thickness range of 0.3mm accounts for 82 +/-2 percent of the total weight of the wire rod, and the bacteriostasis rate of the wire rod on three typical bacteria such as candida albicans, escherichia coli, staphylococcus aureus and the like reaches 75 +/-2 percent.
Example 4:
a chitosan outer surface modified polylactic acid extrusion wire comprises the following components: 90% of polylactic acid and 10% of chitosan with the deacylation degree of 100%.
The extruded strand was processed as follows: the extruded strand was processed as follows: (1) adding polylactic acid into a co-rotating double-screw extruder; (2) a6-sleeve co-rotating double-screw extruder is selected, a side feeding sleeve is adopted at the fourth sleeve, and the corresponding amount of chitosan component is fed.
Finally, the extruded wire is measured, the content of polysaccharide in the outer layer of the wire within the thickness range of 0.3mm accounts for 72 +/-2 percent of the total weight of the extruded wire, and the bacteriostasis rate of the extruded wire to three typical bacteria such as candida albicans, escherichia coli, staphylococcus aureus and the like reaches 73 +/-2 percent.
The foregoing is considered as illustrative of the principles of the invention and is not intended to limit the invention in any way. The undescribed parts are by no means to be considered as employing the solutions known in the art, and any simple modification, equivalent change and modification made to the above embodiments in accordance with the technical spirit of the present invention are still within the scope of the technical solution of the present invention.
Claims (9)
1. The chitosan antibacterial outer surface modified polylactic acid extrusion wire is characterized by comprising the following components in parts by mass: 70-95% of polylactic acid, 0-20% of powder filler, 0-5% of chain extender and 5-10% of chitosan.
2. The chitosan antimicrobial outer surface modified polylactic acid extruded strand according to claim 1, wherein the powder filler is one or more of talc, calcium carbonate powder and plasticized starch.
3. The chitosan antimicrobial outer surface modified polylactic acid extruded strand according to claim 1, wherein the chain extender is a small molecule diol having 2 to 10 carbon atoms.
4. The chitosan antibacterial outer surface modified polylactic acid extruded wire according to claim 1, wherein the chitosan is a chitin derivative having a degree of deacetylation in the range of 80-100%.
5. The chitosan antimicrobial outer surface modified polylactic acid extruded wire according to any one of claims 1 to 4, wherein the chitosan is mainly distributed on the outer surface of the wire.
6. The chitosan antibacterial outer surface modified polylactic acid extruded wire rod according to claim 5, wherein the content of chitosan in the outer layer of the wire rod within the thickness range of 0.3mm is more than 70% of the total weight of the wire rod.
7. A preparation method of a chitosan antibacterial outer surface modified polylactic acid extrusion wire is characterized by comprising the following steps: adding corresponding parts of polylactic acid and chain extender into a reaction kettle, stirring for 30-60 minutes at 85-105 ℃, and injecting into a screw extruder through a mixing and batching system; (2) simultaneously adding powder filler with corresponding weight at a feeding port of the single-screw extruder through a metering pump; (3) adding a side-feed sleeve at section 2/3 of the number of sections of the sleeve combination of the screw extruder, said section 2/3 being rounded to the value of the whole; (4) a corresponding portion of the chitosan component was fed through the side-feed feeder sleeve.
8. The method for preparing the chitosan antibacterial outer surface modified polylactic acid extruded wire rod according to claim 7, wherein the number of the combined sections of the screw extruder sleeve in the step (3) is 6, and the side-feeding sleeve is arranged at the 4 th section of the screw extruder sleeve.
9. The method for preparing the chitosan antibacterial outer surface modified polylactic acid extruded wire rod according to claim 7, wherein the screw extruder in the step (2) is a co-rotating twin-screw extruder or a single-screw extruder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111428453.0A CN114163793A (en) | 2021-11-29 | 2021-11-29 | Chitosan antibacterial outer surface modified polylactic acid extrusion wire and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111428453.0A CN114163793A (en) | 2021-11-29 | 2021-11-29 | Chitosan antibacterial outer surface modified polylactic acid extrusion wire and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114163793A true CN114163793A (en) | 2022-03-11 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111428453.0A Pending CN114163793A (en) | 2021-11-29 | 2021-11-29 | Chitosan antibacterial outer surface modified polylactic acid extrusion wire and preparation method thereof |
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| Country | Link |
|---|---|
| CN (1) | CN114163793A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101935440A (en) * | 2010-09-26 | 2011-01-05 | 华南理工大学 | Starch/polylactic acid antibacterial activity packaging material as well as preparation method and application thereof |
| CN102757626A (en) * | 2011-04-29 | 2012-10-31 | 李文涛 | Preparation method of chitosan and polylactic acid composite material |
| CN108570224A (en) * | 2018-05-24 | 2018-09-25 | 天津科技大学 | A kind of antibacterial high barrier degradation plastic and its preparation |
| CN109705557A (en) * | 2019-01-22 | 2019-05-03 | 上海九意日用品有限公司 | A kind of long-acting biological antibacterial polylactic acid plastics and preparation method thereof |
| CN109735073A (en) * | 2019-01-08 | 2019-05-10 | 福建师范大学 | A kind of high-content chitosan filling 3D printing consumptive material and preparation method thereof |
| CN110204890A (en) * | 2019-06-27 | 2019-09-06 | 金旸（厦门）新材料科技有限公司 | A kind of aperture noise reduction heat-resistant polyamide material and its preparation method and application |
-
2021
- 2021-11-29 CN CN202111428453.0A patent/CN114163793A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101935440A (en) * | 2010-09-26 | 2011-01-05 | 华南理工大学 | Starch/polylactic acid antibacterial activity packaging material as well as preparation method and application thereof |
| CN102757626A (en) * | 2011-04-29 | 2012-10-31 | 李文涛 | Preparation method of chitosan and polylactic acid composite material |
| CN108570224A (en) * | 2018-05-24 | 2018-09-25 | 天津科技大学 | A kind of antibacterial high barrier degradation plastic and its preparation |
| CN109735073A (en) * | 2019-01-08 | 2019-05-10 | 福建师范大学 | A kind of high-content chitosan filling 3D printing consumptive material and preparation method thereof |
| CN109705557A (en) * | 2019-01-22 | 2019-05-03 | 上海九意日用品有限公司 | A kind of long-acting biological antibacterial polylactic acid plastics and preparation method thereof |
| CN110204890A (en) * | 2019-06-27 | 2019-09-06 | 金旸（厦门）新材料科技有限公司 | A kind of aperture noise reduction heat-resistant polyamide material and its preparation method and application |
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Application publication date: 20220311 |
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