CN117511159B - Cosmetic dry-wet separation packaging bag - Google Patents
Cosmetic dry-wet separation packaging bag Download PDFInfo
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- CN117511159B CN117511159B CN202410016325.2A CN202410016325A CN117511159B CN 117511159 B CN117511159 B CN 117511159B CN 202410016325 A CN202410016325 A CN 202410016325A CN 117511159 B CN117511159 B CN 117511159B
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- wet separation
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- 239000002537 cosmetic Substances 0.000 title claims abstract description 76
- 238000000926 separation method Methods 0.000 title claims abstract description 44
- 238000004806 packaging method and process Methods 0.000 title claims abstract description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 33
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229920000219 Ethylene vinyl alcohol Polymers 0.000 claims abstract description 23
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- 239000000661 sodium alginate Substances 0.000 claims abstract description 23
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- 239000005022 packaging material Substances 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 22
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 12
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- 238000007731 hot pressing Methods 0.000 claims abstract description 10
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- UFRKOOWSQGXVKV-UHFFFAOYSA-N ethene;ethenol Chemical compound C=C.OC=C UFRKOOWSQGXVKV-UHFFFAOYSA-N 0.000 claims abstract 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 29
- 239000004408 titanium dioxide Substances 0.000 claims description 14
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 10
- 239000011787 zinc oxide Substances 0.000 claims description 5
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 33
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- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
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- 230000000052 comparative effect Effects 0.000 description 41
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- 238000012360 testing method Methods 0.000 description 14
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- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 210000002421 cell wall Anatomy 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
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- 239000002861 polymer material Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
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- 229910002699 Ag–S Inorganic materials 0.000 description 1
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- 238000012512 characterization method Methods 0.000 description 1
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- RZXDTJIXPSCHCI-UHFFFAOYSA-N hexa-1,5-diene-2,5-diol Chemical compound OC(=C)CCC(O)=C RZXDTJIXPSCHCI-UHFFFAOYSA-N 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
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- 229920000642 polymer Polymers 0.000 description 1
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- 102000004169 proteins and genes Human genes 0.000 description 1
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- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000004580 weight loss Effects 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
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D31/00—Bags or like containers made of paper and having structural provision for thickness of contents
-
- 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
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
-
- 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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/14—Gas barrier composition
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses a dry-wet separation packaging bag for cosmetics, which belongs to the technical field of cosmetic packaging materials, and is prepared from a dry-wet separation packaging material for cosmetics, and the preparation method of the material comprises the following steps: PLA is dissolved in CHCl 3 Adding sodium alginate solution, adding NaOH solution to adjust pH, adding silver nitrate solution, dispersing uniformly, performing ultraviolet irradiation, filtering out solvent, washing and drying to obtain PLA-Ag powder; dry-treated EVOH, light shielding agent and nano SiO 2 And after being uniformly mixed with PLA-Ag powder, the mixture is subjected to melt blending, hot pressing and quenching to room temperature. The dry and wet separation packaging bag for the cosmetics is safe in components, is difficult to migrate into the components of the cosmetics in the long-term use process, has excellent barrier property and antibacterial property, is nontoxic and non-irritating, can be biodegraded, does not cause environmental pollution, and has good application prospect.
Description
Technical Field
The invention belongs to the technical field of cosmetic packaging materials, and particularly relates to a dry-wet separation packaging bag for cosmetics.
Background
With the rapid development of the cosmetic industry, cosmetic packaging is becoming more attractive as the last step in the modern cosmetic industry. The packaging material for cosmetics, besides glass, ceramic and metal materials with good barrier property, also plastic products such as plastic bottles, injection molding cans, hoses, film flexible packages and the like are made of high polymer materials such as PE, PP, PET, EVOH, or the high polymer materials are physically or chemically modified. These plastic products are relatively cheap but difficult to degrade, and can produce toxic and harmful gas by incineration, thus severely polluting the environment; in microscopic view, the plastic is not 'airtight', and the surface morphology of the PP and PE materials is observed under a high-power electron microscope, so that a plurality of holes are formed in the surface of the materials, which indicates that the plastic has certain permeability. PLA is a biodegradable, environmentally friendly aliphatic polyester, and is also a bio-based sustainable plastic that produces only CO when burned 2 And water. In addition, PLA has better barrier properties against oxygen and carbon dioxide than PE and PP and transparency and gloss over other biodegradable materials, but PLA has a relatively slow crystallization rate, and conventional technical means are to improve the crystallinity of PLA by optimizing annealing conditions or adding a nucleating agent, further improving barrier properties.
At present, when the cosmetic packaging material is developed, only the sealing property of the packaging is often emphasized, but the barrier properties such as oxygen resistance, water resistance and the like caused by the permeability of the material are ignored, so that the main components of the cosmetic are deactivated and even deteriorated and cannot be used, and the product is wasted. Meanwhile, in order to improve the processing and using performance of the plastic product, additives such as a stabilizer, an antistatic property, a plasticizer and the like are added in the production process of the cosmetic package, and the additives are degraded under certain conditions (such as illumination, high temperature and the like) so as to be separated out from materials and migrate into the cosmetic to pollute the cosmetic, thereby endangering the health of users. Therefore, the cosmetic packaging materials need to have good barrier properties and safety to avoid these problems.
Disclosure of Invention
The invention aims to provide a dry-wet separation packaging bag for cosmetics, which is prepared from a dry-wet separation packaging material for cosmetics, so as to solve the problems that the additive material of the cosmetic packaging bag is easy to cause deterioration of the cosmetics and pollute the cosmetics.
The aim of the invention can be achieved by the following technical scheme:
the cosmetic dry-wet separation packaging bag is prepared from a cosmetic dry-wet separation packaging material, and the cosmetic dry-wet separation packaging material is prepared by the following steps:
s1, PLA modification: polylactic acid (PLA) is dissolved in CHCl 3 Adding sodium alginate solution at room temperature (25-30deg.C), adding NaOH solution to adjust pH to 9-10, adding silver nitrate solution under stirring, stirring for 3-4 hr to obtain PLA-Ag mixed solution, irradiating at 254nm wavelength in ultraviolet crosslinking instrument for 4-6 hr, filtering with suction filter to remove solvent, washing, and vacuum drying to obtain PLA-Ag powder;
s2, eutectic film pressing: ethylene vinyl alcohol polymer (EVOH), light shielding agent and nano SiO 2 Drying, mixing with PLA-Ag powder, stirring, mixing with molten mixture of 150 deg.C, 155 deg.C, 160 deg.C, 170 deg.C, 180 deg.C, 160 deg.C, 155 deg.C, 150 deg.C, and hot pressing at 15-25MPa to obtain film with thickness of 0.025-0.5mm, and quenching with circulating water to room temperature.
Further, the concentration of the sodium alginate solution is 0.45-0.6%, and the concentration of the silver nitrate is 0.1M.
Further, the dosage ratio of the polylactic acid to the sodium alginate solution to the silver nitrate solution is 15-20g:2mL, 3-6mL.
Further, the concentration of the NaOH solution was 0.1M.
Further, the light shielding agent is any one of zinc oxide and titanium dioxide.
Further, the EVOH, the light shielding agent and the nano SiO 2 The weight percentage of PLA-Ag is 18-40wt%, 2-4wt%, 3-8wt% and 50-75wt%.
Further, the method comprises the steps of,the EVOH, the light shielding agent and the nano SiO 2 The drying treatment is carried out under vacuum condition of 75-90deg.C for 3-5 hr.
Further, the rotational speed of the extruder is 90-120rpm.
The invention has the beneficial effects that:
1. the invention prepares a cosmetic dry-wet separation packaging bag, which is prepared from a cosmetic dry-wet separation packaging material, and the cosmetic dry-wet separation packaging bag prepared from the material has safe components and is difficult to migrate into cosmetic components in the long-term use process, so that the cosmetic is protected from deterioration; in addition, the anti-bacterial coating has excellent barrier property and antibacterial property, can effectively prevent the problems of cosmetic pollution and the like caused by the permeation of water vapor, oxygen and the like, is nontoxic and non-irritating, can be biodegraded, does not cause environmental pollution, and has good application prospect.
2. Firstly, carrying out grafting modification on PLA, introducing carboxyl and hydroxyl on the surface of PLA through NaOH alkaline hydrolysis, grafting sodium alginate on the surface of PLA through coupling reaction, and promoting the hydroxyl in the sodium alginate to promote Ag by utilizing ultraviolet irradiation + Reduction to Ag 0 The silver nanoparticles penetrate through the cell wall to enter cells when the silver nanoparticles perform antibacterial action, and react with sulfhydryl groups to form Ag-S so as to coagulate proteins, destroy the activity of cell synthetase, and the cells lose division proliferation capacity and die. On the other hand, sodium alginate is not only used as a reducing agent for reducing Ag 0 At the same time, due to its carboxyl group, with Ag + The combination of the components to form a net structure plays a role of a stabilizer to prevent Ag 0 Further agglomerating along with the increase of sunlight time so as to lose part of antibacterial performance and ensure long-acting antibacterial effect; then, the PLA and the EVOH modified with silver nano particles are melt blended, in the hot pressing process of a hot press at different temperatures, the EVOH is taken as a base material of a packaging material, and simultaneously taken as a carrier for PLA barrier modification, a nucleating agent is not required to be added, the potential toxicity brought by the nucleating agent is avoided, and the mechanical property and the microorganism resistance of a polymeric material are effectively improvedThe ability to invade, thereby expanding the range of applications for PLA.
3. In the invention, zinc oxide and titanium oxide have strong and wide ultraviolet absorption spectrum in the use of the light shielding agent, but have poor dispersibility, and through being co-dissolved with nano silicon dioxide, the dispersibility of the light shielding agent in plastic products is improved, and meanwhile, the light shielding agent has the synergistic effect of resisting the photo-aging effect, so that the material is ensured to have long-acting antibacterial property.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a plot of the results of a moisture loss test for cosmetics according to the present invention;
FIG. 2 is a plot showing the results of the long-acting antimicrobial property of the cosmetic packaging bag material of the present invention;
FIG. 3 is a Transmission Electron Microscope (TEM) image of PLA-Ag of example 4 of the present invention;
fig. 4 is a TEM image of PLA in comparative example 7 of the present invention.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The cosmetic dry-wet separation packaging bag is prepared from a cosmetic dry-wet separation packaging material, and the cosmetic dry-wet separation packaging material is prepared by the following steps:
s1, PLA modification: 17g PLA was dissolved in 48mL CHCl 3 Obtaining uniform and transparent solution, adding 2mL of 0.6% sodium alginate solution at room temperature, adding 0.1M NaOH solution to adjust pH to 9.5, adding 0.1M 4mL silver nitrate solution at 200rpm, continuously stirring for 4 hours to obtain PLA-Ag mixed solution, placing in an ultraviolet crosslinking instrument, irradiating for 4 hours at 254nm wavelength, filtering out solvent by a suction filter, washing for 3 times, vacuum drying at 60 ℃,obtaining PLA-Ag powder;
s2, eutectic film pressing: EVOH, titanium dioxide and nano SiO 2 Drying for 4h at 85 ℃ under vacuum respectively; 26wt% of EVOH,4wt% of titanium dioxide and 4.5wt% of nano SiO 2 Placing the mixture and 65.5wt% PLA-Ag powder into a high-speed mixer, mixing for 60S, transferring the mixture into an extruder for melt blending, wherein the rotation speed of the extruder is 120rpm, the temperature from a feeding section to a die head is 150 ℃, 155 ℃, 160 ℃, 170 ℃, 180 ℃, 170 ℃, 160 ℃, 155 ℃, 150 ℃ and 24MPa, hot-pressing the mixture into a film with the thickness of 0.1mm, and quenching the film to room temperature by using circulating water.
Example 2
The cosmetic dry-wet separation packaging bag is prepared from a cosmetic dry-wet separation packaging material, and the cosmetic dry-wet separation packaging material is prepared by the following steps:
s1, PLA modification: 20g PLA was dissolved in 48mL CHCl 3 Adding 2mL of 0.5% sodium alginate solution at room temperature, adding 0.1M NaOH solution to adjust the pH value to 9.5, adding 0.1M 5.5mL of silver nitrate solution at 200rpm, continuously stirring for 3.8h to obtain PLA-Ag mixed solution, placing the PLA-Ag mixed solution in an ultraviolet cross-linking instrument, irradiating for 5h at 254nm wavelength, filtering out solvent by a suction filter, washing for 3 times, and vacuum drying at 60 ℃ to obtain PLA-Ag powder;
s2, eutectic film pressing: EVOH, titanium dioxide and nano SiO 2 Drying at 80deg.C under vacuum for 4.5 hr; 38wt% of EVOH,3.5wt% of titanium dioxide and 7.2wt% of nano SiO 2 Placing the mixture and 51.3wt% PLA-Ag powder into a high-speed mixer, mixing for 60S, transferring the mixture into an extruder for melt blending, wherein the rotation speed of the extruder is 110rpm, the temperature from a feeding section to a die head is 150 ℃, 155 ℃, 160 ℃, 170 ℃, 180 ℃, 170 ℃, 160 ℃, 155 ℃, 150 ℃ and 20MPa, hot-pressing the mixture into a film with the thickness of 0.1mm, and quenching the film to room temperature by using circulating water.
Example 3
The cosmetic dry-wet separation packaging bag is prepared from a cosmetic dry-wet separation packaging material, and the cosmetic dry-wet separation packaging material is prepared by the following steps:
s1, PLA modification: 15g PLA was dissolved in 48mL CHCl 3 Adding 2mL of 0.45% sodium alginate solution at room temperature, adding 0.1M NaOH solution to adjust the pH value to 9.5, adding 0.1M 3mL of silver nitrate solution at 200rpm, continuously stirring for 4 hours to obtain PLA-Ag mixed solution, placing the PLA-Ag mixed solution in an ultraviolet crosslinking instrument, irradiating for 4.5 hours at 254nm wavelength, filtering the solvent by a suction filter, washing for 3 times, and vacuum drying the rest materials at 60 ℃ to obtain PLA-Ag powder;
s2, eutectic film pressing: EVOH, zinc oxide and nano SiO 2 Drying at 90deg.C under vacuum for 3.5 hr; 18wt% of EVOH,2wt% of titanium dioxide and 5wt% of nano SiO 2 Placing the mixture and 75wt% PLA-Ag powder into a high-speed mixer, mixing for 60S, transferring the mixture into an extruder for melt blending, wherein the rotation speed of the extruder is 90rpm, the temperature from a feeding section to a die head is 150 ℃, 155 ℃, 160 ℃, 170 ℃, 180 ℃, 170 ℃, 160 ℃, 155 ℃, 150 ℃ and 18MPa, hot-pressing the mixture into a film with the thickness of 0.1mm, and quenching the film to room temperature by using circulating water.
Comparative example 1
The cosmetic dry-wet separation packaging bag is prepared from a cosmetic dry-wet separation packaging material, and the cosmetic dry-wet separation packaging material is prepared by the following steps:
EVOH, titanium dioxide and nano SiO 2 Drying for 4h at 85 ℃ under vacuum respectively; 26wt% of EVOH,4wt% of titanium dioxide and 4.5wt% of nano SiO 2 Placing the mixture and 65.5wt% PLA powder into a high-speed mixer, mixing for 60S, transferring the mixture into an extruder for melt blending, wherein the rotation speed of the extruder is 120rpm, the temperature from a feeding section to a die head is 150 ℃, 155 ℃, 160 ℃, 170 ℃, 180 ℃, 170 ℃, 160 ℃, 155 ℃, 150 ℃ and 24MPa, hot-pressing the mixture into a film with the thickness of 0.1mm, and quenching the film to room temperature by using circulating water.
Comparative example 2
A cosmetic dry-wet separation packaging bag is prepared by the same method as in example 1, except that no nanometer is addedSiO 2 。
Comparative example 3
A cosmetic dry-wet separation packaging bag is prepared by the same method as in example 1, except that titanium dioxide or zinc oxide is not added.
Comparative example 4
The cosmetic dry-wet separation packaging bag is prepared from a cosmetic dry-wet separation packaging material, and the cosmetic dry-wet separation packaging material is prepared by the following steps:
s1, PLA modification: 17g PLA was dissolved in 48mL CHCl 3 Obtaining a uniform and transparent solution, adding 2mL of 0.6% sodium alginate solution at room temperature, adding 0.1M NaOH solution to adjust the pH to 9.5, stirring for 4 hours at 200rpm to obtain PLA-Ag mixed solution, filtering the solvent by a suction filter, washing 3 times, and vacuum drying the rest substances at 60 ℃ to obtain PLA powder;
s2, eutectic film pressing: EVOH, titanium dioxide and nano SiO 2 Drying for 4h at 85 ℃ under vacuum respectively; 26wt% of EVOH,4wt% of titanium dioxide and 4.5wt% of nano SiO 2 Placing the mixture and 65.5wt% PLA powder into a high-speed mixer, mixing for 60S, transferring the mixture into an extruder for melt blending, wherein the rotation speed of the extruder is 120rpm, the temperature from a feeding section to a die head is 150 ℃, 155 ℃, 160 ℃, 170 ℃, 180 ℃, 170 ℃, 160 ℃, 155 ℃, 150 ℃ and 24MPa, hot-pressing the mixture into a film with the thickness of 0.1mm, and quenching the film to room temperature by using circulating water.
Comparative example 5
The cosmetic dry-wet separation packaging bag is prepared from a cosmetic dry-wet separation packaging material, and the cosmetic dry-wet separation packaging material is prepared by the following steps:
s1, weighing 99.5 parts of PLA powder and 0.5 part of Ag nano particles according to parts by weight, and mixing the PLA powder and the Ag nano particle mixture;
s2, eutectic film pressing: EVOH, titanium dioxide and nano SiO 2 Drying for 4h at 85 ℃ under vacuum respectively; 26wt% of EVOH,4wt% of titanium dioxide and 4.5wt% of nano SiO 2 Then with 65.5wt% PLA powder and Ag nano particlesPlacing the mixture into a high-speed mixer, mixing for 60S, transferring the mixture into an extruder for melt blending, wherein the rotation speed of the extruder is 120rpm, the temperature from a feeding section to a die head is 150 ℃, 155 ℃, 160 ℃, 170 ℃, 180 ℃, 170 ℃, 160 ℃, 155 ℃, 150 ℃, and hot-pressing into a film with the thickness of 0.1mm under the pressure of 24MPa, and quenching to room temperature by using circulating water.
Comparative example 6
A cosmetic dry-wet separation packaging bag is prepared by the same method as in example 1, except that no nano SiO is added 2 And a light shielding agent.
Performance tests were performed on examples 1-3 and comparative examples 1, 4 and 5:
antibacterial test
The film pasting method is adopted: according to the antibacterial property test method in QB/T2591-2003, the antibacterial effect is examined by the antibacterial rate after the antibacterial plastic is contacted with the test bacteria for 24 hours. The calculation formula of the antibacterial rate is as follows:
R＝(B-C)/B×100％
wherein R is antibacterial rate; b is average recovered bacteria number of a blank control sample; and C is the average recovered bacteria number of the antibacterial plastic.
In the invention, the average number of the recovered bacteria is 1.44cm 2 Average colonies on solid medium were calculated and the average of 3 parallel experiments was taken as the count result.
Test strain: coli, staphylococcus aureus, commercially available
The same size of the packages prepared in examples 1 to 3 and comparative examples 1, 4 and 5 were cut out, respectively, and antibacterial property test was performed using a film-sticking method. Culturing at 37deg.C for 36h according to 1.44cm 2 The number of colonies grown thereon was counted for antibacterial efficiency, and the results are shown in Table 1.
TABLE 1
| Coli (%) | Staphylococcus aureus (%) | |
| Example 1 | 96.83 | 98.42 |
| Example 2 | 96.21 | 99.09 |
| Example 3 | 96.44 | 98.78 |
| Comparative example 1 | 64.37 | 66.55 |
| Comparative example 4 | 84.64 | 85.21 |
| Comparative example 5 | 85.77 | 86.15 |
As can be seen from Table 1, the dry-wet separation package bag of the cosmetic prepared by the invention has remarkable antibacterial property, and the antibacterial effect is stronger than that of the silver nanoparticles (comparative example 5) mixed in the sodium alginate modified PLA (comparative example 4) and PLA powder, which is due to the Ag generated by reduction under the irradiation of ultraviolet light 0 Aggregate into clusters and load onThe nano silver on the surface of PLA has an influence on the surface charge of bacteria so as to generate antibacterial performance, and meanwhile, the nano silver and sodium alginate are synergistic to improve the surface area of PLA, so that the possibility that bacteria contact with cosmetic packaging bags is reduced; the bacteriostasis to E.coli and to Staphylococcus aureus is slightly different due to the different cell wall composition of the gram-positive and gram-negative bacteria.
Cosmetic water loss rate test:
the cosmetics prepared in comparative examples 1 to 6 were packaged in dry and wet separation packages for cosmetic water loss rate, respectively, to test the long-acting antibacterial and barrier properties of the cosmetic packaging materials:
in m 1 Indicating the initial quality of the cosmetics on day 0, packaging the cosmetics by using a sample, sealing, and then placing the packaged cosmetics in a refrigerator for cold storage, wherein the temperature of the refrigerator is set to be 3-5 ℃. After refrigerating for n days, taking out the cosmetics, weighing the mass of the cosmetics by a balance, and taking the mass as m 2 And (3) representing. Using r= (m 1 -m 2 )/m 1 The water loss rate R of the cosmetic samples was determined by x 100% and the test results are shown in fig. 1.
As can be seen from fig. 1, the moisture loss of the cosmetics caused by the decomposition of microorganisms and enzymes and poor barrier property of the packaging material, etc., is 16.74% in the case of 10 months, the water loss rate of comparative example 1 is severe, 7.54% in the case of comparative example 4 (sodium alginate modified PLA), only 1.65% in the case of example 1, and 10.28% in the case of 10 months in the case of comparative example 5 (PLA powder and silver nanoparticle compounding), which means that the barrier property can be improved by sodium alginate treated PLA, and the antibacterial property of PLA can be synergistically improved by sodium alginate and silver nanoparticle; in the same case, the water loss rates of comparative example 2, comparative example 3 and comparative example 6 were 4.84%, 3.21% and 9.10%, respectively, indicating nano SiO 2 And a light shielding agent can improve the barrier properties of the material; therefore, the components in the packaging bag material are difficult to migrate into the cosmetics, and the product quality of the cosmetics is effectively ensured.
Degradation performance test: according to annex D in GB/T18006.2-1999 disposable degradable tableware degradation Performance test method: the method for testing the compostability of the biodegradable material tests and calculates the biodegradation rate R in units of;
water vapor and oxygen transmission rates: the gas permeation tester was used for measurement, the measurement was performed 5 times, the average value was taken, and the measurement results are shown in Table 2:
TABLE 2
| Oxygen transmission rate/g.m -2 ·d -1 | Water vapor transmission rate/g.m -2 ·d -1 | Percent of degradation weight loss | |
| Example 1 | 0.0019 | 1.046 | 81.2 |
| Example 2 | 0.020 | 1.051 | 81.0 |
| Example 3 | 0.021 | 1.048 | 81.7 |
| Comparative example 1 | 0.024 | 1.084 | 70.4 |
| Comparative example 2 | 0.031 | 1.177 | 79.8 |
| Comparative example 3 | 0.030 | 1.182 | 80.4 |
| Comparative example 4 | 0.026 | 1.123 | 78.4 |
| Comparative example 5 | 0.028 | 1.311 | 74.9 |
| Comparative example 6 | 0.045 | 2.234 | 64.3 |
As can be seen from Table 2, the dry and wet separation packaging bags for cosmetics prepared in examples 1-3 have excellent oxygen and water resistance and degradation properties.
Light transmittance test:
the cosmetic dry and wet separation packages prepared in example 1, comparative example 2, comparative example 3 and comparative example 6 were cut into films having a size of 5cm×5cm, and the light transmittance percentage of the packages at 500nm was measured using a UV-VIS scanning spectrophotometer, and the light transmittance results of the respective films were calculated as shown in table 3:
TABLE 3 Table 3
| Description of the preferred embodiments | Transmittance% |
| Example 1 | 0.24 |
| Comparative example 2 | 8.4 |
| Comparative example 3 | 12.7 |
| Comparative example 6 | 74.7 |
As can be seen from table 3, under the same light conditions, the comparative examples 2 and 3 have a certain function of blocking ultraviolet rays because the materials thereof do not contain nano silica or light shielding agent, whereas the nano silica or light shielding agent in example 1 cooperatively shields ultraviolet rays, further preventing deterioration of cosmetics.
Long-acting antibacterial test:
the cosmetic packaging bag materials prepared in the example 1, the comparative example 4 and the comparative example 5 are placed in an ultraviolet crosslinking instrument to be irradiated under 254nm wavelength, and antibacterial properties of the materials are respectively tested in 0h, 24h, 48h and 96h, and escherichia coli is used as a test strain, and the test results are shown in figure 2; as can be seen from FIG. 2, the cosmetic packaging bag material prepared by the present invention has a certain increase in antibacterial ability with ultraviolet light irradiation, and has the following characteristicsDue to Ag during ultraviolet irradiation + Continuously reducing into Ag 0 The antibacterial performance of the composite material is always kept under the illumination condition; comparative example 1 has no antibacterial property in the material, and the antibacterial property is reduced with illumination; in the comparative example 4, the sodium alginate has a certain antibacterial property, and the antibacterial capability is stronger than that of the comparative example 1, but the material is further photolyzed along with illumination so as to lose efficacy; in comparative example 5, PLA powder was compounded with Ag nanoparticles, which have antibacterial properties and are stable, but since the amount thereof was stable, the antibacterial properties were limited by the amount of silver nanoparticles, and the silver nanoparticles could not be generated by themselves; in addition, sodium alginate was not added during the preparation process, and the antibacterial ability was inferior to that of example 1.
XRD (X-ray diffraction) characterization of PLA-Ag powder and PLA revealed that PLA-Ag had crystalline peaks at 38.0514 °,44.4371 ℃and 64.6145 ℃corresponding to (111), (200) and (220) crystal planes, respectively, whereas PLA had no such crystalline peaks.
Example 4
17g PLA was dissolved in 48mL CHCl 3 In the process, a uniform and transparent solution is obtained, 2mL of 0.6% sodium alginate solution is added at room temperature, then 0.1M NaOH solution is added to adjust the pH value to 9.5, 0.1M 4mL of silver nitrate solution is added at 200rpm, stirring is continued for 4 hours, PLA-Ag mixed solution is obtained, the PLA-Ag mixed solution is placed in an ultraviolet cross-linking instrument and irradiated for 4 hours at 254nm wavelength, then the PLA-Ag mixed solution is dripped on a copper mesh at room temperature, the loading condition is observed through a transmission electron microscope, and a TEM diagram of the PLA-Ag is shown as a graph in FIG. 3.
Comparative example 7
17g PLA was dissolved in 48mL CHCl 3 In the above, the polylactic acid was dropped onto a copper mesh at room temperature, and a TEM image of PLA was observed by a transmission electron microscope, as shown in FIG. 4.
As can be seen from FIGS. 3 and 4, ag produced by reduction under ultraviolet irradiation 0 The nano silver particles generated by agglomeration are loaded on PLA, the size of the nano silver particles is 5-7nm, and the nano silver particles and sodium alginate cooperate to improve the surface area of the PLA.
It is noted that relational terms such as first and second, and the like are 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. Moreover, 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 understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (3)
1. The cosmetic dry-wet separation packaging bag is characterized by being prepared from a cosmetic dry-wet separation packaging material, and the cosmetic dry-wet separation packaging material is prepared by the following steps:
s1.PLA was dissolved in CHCl 3 Adding sodium alginate solution, adding NaOH solution to adjust pH to 9-10, adding silver nitrate solution, dispersing uniformly, performing ultraviolet irradiation, filtering, washing with solvent, and drying to obtain PLA-Ag powder;
s2, drying EVOH, light shielding agent and nano SiO 2 Uniformly mixing with PLA-Ag powder, then carrying out melt blending, hot-pressing, and quenching to room temperature;
the concentration of the sodium alginate solution is 0.45-0.6%, the concentration of silver nitrate is 0.1M, and the concentration of NaOH is 0.1M; the dosage ratio of the PLA, the sodium alginate solution and the silver nitrate solution is 15-20g:2mL of 3-6mL; the ultraviolet irradiation wavelength is 254nm, and the ultraviolet irradiation time is 4-6h; the EVOH, the light shielding agent and the nano SiO 2 The weight percentage of PLA-Ag is 18-40wt%, 2-4wt%, 3-8wt% and 50-75wt%; the light shielding agent is any one of zinc oxide and titanium dioxide.
2. The cosmetic dry and wet separation packaging bag according to claim 1, wherein the EVOH, the light shielding agent, the nano SiO 2 The drying treatment is carried out under vacuum condition of 75-90deg.C for 3-5 hr.
3. The dry and wet separation pack for cosmetics according to claim 1, wherein the temperature of said melt blending feed section to said die is 150 ℃, 155 ℃, 160 ℃, 170 ℃, 180 ℃, 170 ℃, 160 ℃, 155 ℃, 150 ℃, respectively.
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