CN112959740A - Antibacterial paper cup and preparation method thereof - Google Patents
Antibacterial paper cup and preparation method thereof Download PDFInfo
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- CN112959740A CN112959740A CN202110272815.5A CN202110272815A CN112959740A CN 112959740 A CN112959740 A CN 112959740A CN 202110272815 A CN202110272815 A CN 202110272815A CN 112959740 A CN112959740 A CN 112959740A
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 124
- 238000002360 preparation method Methods 0.000 title claims abstract description 47
- 238000010227 cup method (microbiological evaluation) Methods 0.000 title description 2
- 239000003242 anti bacterial agent Substances 0.000 claims abstract description 42
- 238000005507 spraying Methods 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 13
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- 239000002562 thickening agent Substances 0.000 claims abstract description 11
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 8
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 8
- 229920001661 Chitosan Polymers 0.000 claims description 97
- 239000000243 solution Substances 0.000 claims description 45
- 239000002245 particle Substances 0.000 claims description 37
- 239000007788 liquid Substances 0.000 claims description 27
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- 239000000853 adhesive Substances 0.000 claims description 15
- 230000001070 adhesive effect Effects 0.000 claims description 15
- 239000000839 emulsion Substances 0.000 claims description 14
- 239000000499 gel Substances 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 230000006196 deacetylation Effects 0.000 claims description 10
- 238000003381 deacetylation reaction Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 9
- 238000004108 freeze drying Methods 0.000 claims description 9
- 238000009210 therapy by ultrasound Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 8
- 238000009833 condensation Methods 0.000 claims description 8
- 230000005494 condensation Effects 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 238000004026 adhesive bonding Methods 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 238000004132 cross linking Methods 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000011265 semifinished product Substances 0.000 claims description 3
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 2
- 108010010803 Gelatin Proteins 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 2
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 2
- 239000008273 gelatin Substances 0.000 claims description 2
- 229920000159 gelatin Polymers 0.000 claims description 2
- 235000019322 gelatine Nutrition 0.000 claims description 2
- 235000011852 gelatine desserts Nutrition 0.000 claims description 2
- 229920002401 polyacrylamide Polymers 0.000 claims description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims 1
- 239000000123 paper Substances 0.000 description 133
- LUEWUZLMQUOBSB-FSKGGBMCSA-N (2s,3s,4s,5s,6r)-2-[(2r,3s,4r,5r,6s)-6-[(2r,3s,4r,5s,6s)-4,5-dihydroxy-2-(hydroxymethyl)-6-[(2r,4r,5s,6r)-4,5,6-trihydroxy-2-(hydroxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-4,5-dihydroxy-2-(hydroxymethyl)oxan-3-yl]oxy-6-(hydroxymethyl)oxane-3,4,5-triol Chemical compound O[C@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@@H](O[C@@H]2[C@H](O[C@@H](OC3[C@H](O[C@@H](O)[C@@H](O)[C@H]3O)CO)[C@@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O LUEWUZLMQUOBSB-FSKGGBMCSA-N 0.000 description 19
- 241001312219 Amorphophallus konjac Species 0.000 description 19
- 235000001206 Amorphophallus rivieri Nutrition 0.000 description 19
- 229920002581 Glucomannan Polymers 0.000 description 19
- 229920002752 Konjac Polymers 0.000 description 19
- 229940046240 glucomannan Drugs 0.000 description 19
- 239000000252 konjac Substances 0.000 description 19
- 235000010485 konjac Nutrition 0.000 description 19
- 239000011148 porous material Substances 0.000 description 11
- 238000012360 testing method Methods 0.000 description 11
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- 239000007864 aqueous solution Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000000725 suspension Substances 0.000 description 6
- 230000001580 bacterial effect Effects 0.000 description 5
- 239000001963 growth medium Substances 0.000 description 5
- 125000003277 amino group Chemical group 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- 241000588724 Escherichia coli Species 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 241000191967 Staphylococcus aureus Species 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000007872 degassing Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 230000001954 sterilising effect Effects 0.000 description 3
- 238000004659 sterilization and disinfection Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 230000015271 coagulation Effects 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000006916 nutrient agar Substances 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000003172 aldehyde group Chemical group 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000035622 drinking Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000007783 nanoporous material Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000011087 paperboard Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000002504 physiological saline solution Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229910021426 porous silicon Inorganic materials 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
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- 239000012798 spherical particle Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- -1 sucrose ester Chemical class 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B31—MAKING ARTICLES OF PAPER, CARDBOARD OR MATERIAL WORKED IN A MANNER ANALOGOUS TO PAPER; WORKING PAPER, CARDBOARD OR MATERIAL WORKED IN A MANNER ANALOGOUS TO PAPER
- B31B—MAKING CONTAINERS OF PAPER, CARDBOARD OR MATERIAL WORKED IN A MANNER ANALOGOUS TO PAPER
- B31B50/00—Making rigid or semi-rigid containers, e.g. boxes or cartons
- B31B50/74—Auxiliary operations
- B31B50/742—Coating; Impregnating; Waterproofing; Decoating
- B31B50/753—Coating; Impregnating; Waterproofing; Decoating by spraying
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
- D21H21/36—Biocidal agents, e.g. fungicidal, bactericidal, insecticidal agents
Abstract
The application relates to the field of paper cups, in particular to an antibacterial paper cup and a preparation method thereof. The antibacterial paper cup is characterized in that an antibacterial layer is formed on the surface of the antibacterial paper cup, and the antibacterial layer is obtained by mixing and spraying the following raw materials in parts by weight: porous nanoparticles: 15-25 parts; food-grade antibacterial agent: 0.5-2 parts; polyvinyl alcohol: 13-18 parts; thickening agent: 1-3 parts; water: 25-36 parts. The antibacterial paper cup prepared by the method has excellent antibacterial performance, the antibacterial layer is not easy to fall off, and the durability is high.
Description
Technical Field
The application relates to the field of paper cups, in particular to an antibacterial paper cup and a preparation method thereof.
Background
The paper cup is formed by processing and printing packaging base paper and gluing the packaging base paper by a paper cup machine, and has certain waterproofness. Paper cups are widely used due to their portability and low price, and are common drinking tools in many families and public places. However, when the paper cup is idle, bacteria are easy to breed, the paper cup on the market has single function, and the paper cup with the antibacterial effect is few.
The Chinese patent application with the application number of CN201810274696.5 discloses a konjac glucomannan antibacterial paper cup and a preparation method thereof, wherein chitosan, konjac glucomannan and other raw materials are subjected to degassing and plate pouring to prepare a konjac glucomannan film with antibacterial property, and the film is attached to the surface of the paper cup to prepare the antibacterial paper cup.
In the technical scheme, the antibacterial film with antibacterial effect is prepared by utilizing the film forming property of konjac glucomannan and the spectral antibacterial property of chitosan, but the antibacterial property of chitosan is general, so that the antibacterial property of the prepared antibacterial paper cup is improved to a limited extent.
Content of application
In order to improve the antibacterial performance of the paper cup and improve the safety of preparation, the application provides an antibacterial paper cup and a preparation method thereof.
In a first aspect, the application provides an antibacterial paper cup, which adopts the following technical scheme:
the antibacterial paper cup is characterized in that an antibacterial layer is formed on the surface of the antibacterial paper cup, and the antibacterial layer is prepared by mixing and spraying the following raw materials in parts by weight:
porous nanoparticles: 15-25 parts;
food-grade antibacterial agent: 0.5-2 parts;
polyvinyl alcohol: 13-18 parts;
thickening agent: 1-3 parts;
water: 25-36 parts.
The antibacterial layer made by matching the porous nanoparticles and the food-grade antibacterial agent is adopted, so that the antibacterial performance of the paper cup is obviously improved. Compared with the adoption of a spectrum antibacterial agent such as chitosan and the like, the antibacterial performance of the paper cup can be effectively improved by adopting the food-grade antibacterial agent; and because the surfaces of the porous nano particles are provided with more holes, the surface area of the porous nano particles is larger, the porous nano particles can be used as a carrier, more space is provided for the attachment of food-grade antibacterial agents, and the antibacterial performance of the paper cup is promoted to be improved.
In addition, the antibacterial agent attached to the inside of the pore channel of the porous nano-particles has higher water resistance compared with the antibacterial agent exposed on the surface, so that the antibacterial agent is not easy to fall off, and the long-acting property of the antibacterial effect of the paper cup is improved.
Preferably, the porous nano material is one or more of porous nano chitosan, porous alumina and porous silica.
The porous nano chitosan, the porous alumina and the porous silicon dioxide have high porosity and good adsorption performance, and are favorable for the attachment of the antibacterial agent; the porous nano chitosan also has a certain broad-spectrum antibacterial effect, and is beneficial to improving the antibacterial performance of the paper cup antibacterial layer.
Preferably, the porous nano chitosan is prepared according to the following method:
s101, mixing a sodium hydroxide solution with the mass concentration of 3-7% and an ethanol solution with the mass concentration of 90-95% according to the volume ratio of (3-5) to 1 to obtain a condensate;
s102, fully dissolving chitosan in an acetic acid solution to obtain a chitosan solution, adding a glutaraldehyde solution into the chitosan solution, uniformly mixing, and placing in a hot water bath (50 ℃) for reaction and crosslinking to obtain a gel solution;
and S103, dropwise adding the gel liquid into the condensation liquid, fully mixing, filtering, washing with water, and drying to obtain the porous nano chitosan.
Compared with common chitosan, the chitosan prepared by the method has higher porosity and better antibacterial and bactericidal effects. After the chitosan is fully dissolved in the acid solution, ethanol is used as a pore-making agent, and chitosan molecules are gradually precipitated to form porous spherical particles in an alkaline environment; as glutaraldehyde is added as a cross-linking agent before precipitation, amino groups on chitosan molecules and aldehyde groups of the glutaraldehyde are cross-linked, so that the porous nano chitosan with higher strength and more stable structure is favorably formed.
The nano porous chitosan has a synergistic effect, and the antibacterial effect can be obviously improved by the cooperation of the nano porous chitosan and the nano porous chitosan. Under alkaline environment, a large number of amino groups can be formed on the molecular chain of the chitosan, so that the surface of the porous nano chitosan is promoted to be positively charged, and therefore, an electrostatic adsorption effect is generated between the porous nano chitosan and negatively charged bacteria, and the antibacterial agent attached to the nano porous chitosan plays a role in bacteriostasis and sterilization.
Preferably, in step S102, the degree of deacetylation of the chitosan is > 90%.
The chitosan with higher deacetylation degree is adopted, so that on one hand, the solubility of the chitosan is improved, and the formation of porous nano chitosan is promoted; on the other hand, the higher the deacetylation degree is, the higher the amino content on the surface of chitosan is, which is beneficial to improving the electrostatic adsorption effect on bacteria, thereby improving the bacteriostatic and antibacterial properties of the paper cup.
Preferably, the specific operation of step S103 is: and (3) dropwise adding the gel liquid into the condensation liquid, carrying out ultrasonic treatment on the mixed solution in the dropwise adding process, filtering, washing, and carrying out freeze drying treatment to obtain the porous nano chitosan.
According to the method, a large amount of micro bubbles are introduced into the solution in the precipitation forming process of the porous nano chitosan by utilizing the cavitation generated by ultrasonic treatment, so that the porosity of the porous nano chitosan is improved, the attachment amount of the antibacterial agent is increased, and the antibacterial effect of the paper cup is enhanced; meanwhile, the air bubbles in the nano porous chitosan are promoted to be broken to form pore channels by being matched with freeze drying treatment, and meanwhile, the moisture permeated into the moisture particles is freeze-dried, so that the antibacterial performance of the paper cup is further improved, and finally, the antibacterial performance of the paper cup is improved.
Preferably, the ultrasonic frequency is 20KHz to 30 KHz.
The ultrasonic frequency is too low, so that the cavitation is difficult to generate, and the porosity of the nano porous chitosan is not easy to improve; the ultrasonic frequency is too high, so that the structure of the nano porous chitosan is easily damaged, the porosity and the antibacterial agent loading rate are reduced, and the antibacterial performance of the paper cup is reduced.
Preferably, the thickening agent is one or more of carboxymethyl cellulose, gelatin and polyacrylamide.
The thickening agent is adopted, so that the fixation strength of the nano porous chitosan and the antibacterial agent on the surface of the paper cup can be improved, and the long-acting property of the antibacterial effect of the paper cup can be improved; meanwhile, the phenomenon that the adhesive and the antibacterial agent penetrate into the paper can be reduced, so that the strength and the antibacterial performance of the paper cup are reduced.
In a second aspect, the application provides a method for preparing an antibacterial paper cup, which adopts the following technical scheme:
a preparation method of the antibacterial paper cup comprises the following steps:
s201, uniformly mixing polyvinyl alcohol and 85-95% of water to obtain adhesive emulsion, taking 80-90% of adhesive emulsion, sequentially adding nano porous particles and a thickening agent, and fully mixing to obtain spraying liquid;
s202, uniformly mixing the antibacterial agent, the rest water and the rest adhesive emulsion to obtain an antibacterial liquid;
s203, spraying the spraying liquid prepared in the step S201 on the surface of the base paper of the paper cup, and drying to obtain a semi-finished base paper of the paper cup;
s203, spraying the antibacterial liquid prepared in the step S202 on the surface of the semi-finished product of the raw paper of the paper cup, and drying to obtain a finished product of the raw paper of the paper cup;
and S204, gluing the paper cup base paper into the antibacterial paper cup by adopting a paper cup machine.
According to the technical scheme, the two-step spraying process is adopted, the nano porous particles are sprayed on the surface of the base paper for the paper cup, after the nano porous particles are solidified to form the adsorption layer, the antibacterial solution is sprayed on the adsorption layer, the loading capacity of the antibacterial agent is effectively improved, and the antibacterial performance of the paper cup is improved.
In summary, the present application has the following beneficial effects:
1. according to the paper cup antibacterial agent, the antibacterial agent and the nano porous particles are matched together, so that the loading capacity of the antibacterial agent on the surface of the paper cup is remarkably improved, the antibacterial agent is not easy to fall off, and the antibacterial period of the paper cup is prolonged.
2. The paper cup is preferably made of porous nano chitosan, the content of the surface antibacterial agent is improved by utilizing the loading effect of the chitosan, and meanwhile, the antibacterial performance of the paper cup is further enhanced by utilizing the broad-spectrum antibacterial effect of the nano porous chitosan and the electrostatic adsorption effect on bacteria.
3. According to the method, the antibacterial agent loading capacity on the surface and in the pore channels of the nano porous chitosan is increased by adopting a two-step spraying method, and the antibacterial period of the antibacterial agent is effectively prolonged by utilizing the protective effect of the nano porous chitosan on the antibacterial agent.
Detailed Description
The present application will be described in further detail with reference to examples.
Preparation example
Preparation example 1, a porous nano chitosan was prepared according to the following steps:
s101, mixing 4L of 6% sodium hydroxide solution with mass concentration and 1L of 95% ethanol solution with mass concentration to obtain a condensate;
s102, fully dissolving chitosan with the deacetylation degree of 95% in an acetic acid solution with the mass concentration of 2%, and standing at room temperature (23 ℃) for 24 hours to obtain 1L of chitosan solution with the mass concentration of 5%; adding 2L of 0.5% glutaraldehyde solution serving as a cross-linking agent into the chitosan solution, uniformly mixing, and placing in a hot water bath at 50 ℃ for oscillation reaction for 1h to obtain a gel solution;
and S103, dropwise adding the gel solution prepared in the step S102 into the condensation solution prepared in the step S101 for 1.5 hours, carrying out ultrasonic treatment on the solution in the dropwise adding process, wherein the ultrasonic frequency is 25KHz, filtering to obtain particles, washing the particles to be neutral, placing the particles into a freeze dryer, carrying out freeze drying at-40 ℃ for 30min, removing water permeating into the particles, taking out, and airing to obtain the porous nano chitosan.
Preparation example 2, a porous nano chitosan, which is different from preparation example 1 in that a chitosan solution is prepared in step S102, and crosslinking is performed without adding glutaraldehyde; in step S103, a chitosan solution is added to the coagulation liquid in place of the gel droplet.
Preparation example 3, a porous nano-chitosan, was different from preparation example 1 in that chitosan having a degree of deacetylation of 85% was used instead of chitosan having a degree of deacetylation of 95% in step S101.
Preparation example 4, a porous nano chitosan, was different from preparation example 1 in that the specific operation of step S103 was: and (3) dropwise adding the gel solution prepared in the step (S102) into the condensation solution prepared in the step (S101) for 1.5 hours, filtering to obtain particles, washing the particles to be neutral, placing the particles into a freeze dryer, freeze-drying the particles at-40 ℃ for 30min, removing water permeating into the particles, taking out and drying in the air to obtain the porous nano chitosan. That is, the ultrasonic treatment was not performed, and only the freeze-drying treatment was performed.
Preparation example 5, a porous nano-chitosan, was different from preparation example 1 in that the specific operation of step S103 was: and (3) dropwise adding the gel solution prepared in the step (S102) into the condensation solution prepared in the step (S101) for 1.5h, carrying out ultrasonic treatment on the solution in the dropwise adding process, wherein the ultrasonic frequency is 20KHz, filtering to obtain particles, washing the particles to be neutral, taking out and airing to obtain the porous nano chitosan. That is, the freeze-drying treatment was not performed, and only the ultrasonic treatment was performed.
Preparation example 6, a porous nano chitosan, was different from preparation example 1 in that the specific operation of step S103 was: and (4) dropwise adding the gel solution prepared in the step (S102) into the condensation solution prepared in the step (S101) for 1.5h, filtering to obtain particles, washing the particles to be neutral, taking out and airing to obtain the porous nano chitosan. Namely, neither freeze drying nor ultrasonic treatment was carried out.
Preparation example 7, a porous nano-chitosan, was different from preparation example 1 in that the ultrasonic frequency was 20KHz in step S103.
Preparation example 8, a porous nano-chitosan, was different from preparation example 1 in that the ultrasonic frequency was 35KHz in step S103.
Examples
Example 1, an antibacterial paper cup, the selection of each raw material component and the corresponding amount thereof are shown in table 1, and is prepared according to the following steps:
s201, mixing 90% of water and polyvinyl alcohol according to the raw material ratio in the table 1, and uniformly stirring at the rotating speed of 2000rpm to obtain adhesive emulsion; taking 85% of adhesive emulsion, sequentially adding the nano porous particles and the thickening agent prepared in the preparation example 1, and stirring and mixing at the rotating speed of 800rpm to prepare a spraying liquid;
s202, uniformly mixing the antibacterial agent, the remaining 10% of water and the remaining 15% of adhesive emulsion to obtain an antibacterial liquid;
s203, spraying the spraying liquid prepared in the step S201 on the surface of the base paper of the paper cup, and drying at the constant temperature of 40 ℃ for 8 hours to obtain a semi-finished base paper of the paper cup;
s203, spraying the antibacterial liquid prepared in the step S202 on the surface of the semi-finished product of the paper cup base paper, drying at the constant temperature of 40 ℃ for 3 hours, and drying to obtain the finished product of the paper cup base paper;
and S204, gluing the paper cup base paper into the antibacterial paper cup by a paper cup machine.
The raw paper for paper cups in step S203 is raw paper for paper cups of 210 g/square meter, which is purchased from Shandong gold sun paper industry, Inc.
Examples 2 to 5, an antibacterial paper cup, different from example 1, were as shown in table 1 for the selection of each raw material component and the corresponding amount thereof.
Table 1 shows the raw material composition and the corresponding content (kg) of the antibacterial layer in examples 1 to 5
TABLE 2 manufacturer information of raw material components
Example 6, an antibacterial paper cup, is different from example 1 in that, in step S201, the nano-porous particles prepared in preparation example 2 are used instead of the nano-porous particles prepared in preparation example 1.
Example 7, an antibacterial paper cup, was different from example 1 in that the nanoporous particles prepared in preparation example 3 were used instead of the nanoporous particles prepared in preparation example 1 in step S201.
Example 8, an antibacterial paper cup, is different from example 1 in that, in step S201, the nano-porous particles prepared in preparation example 4 are used instead of the nano-porous particles prepared in preparation example 1.
Example 9, an antibacterial paper cup, was different from example 1 in that, in step S201, the nanoporous particles prepared in preparation example 5 were used instead of the nanoporous particles prepared in preparation example 1.
Example 10, an antibacterial paper cup, differs from example 1 in that, in step S201, the nanoporous particles prepared in preparation example 6 are used instead of the nanoporous particles prepared in preparation example 1.
Example 11, an antibacterial paper cup, was different from example 1 in that, in step S201, the nanoporous particles prepared in preparation example 7 were used instead of the nanoporous particles prepared in preparation example 1.
Example 12, an antibacterial paper cup, was different from example 1 in that, in step S201, the nanoporous particles prepared in preparation example 8 were used instead of the nanoporous particles prepared in preparation example 1.
Example 13, an antibacterial paper cup was prepared as follows:
step 1: according to the raw material proportion of the embodiment 1, 90% of water is mixed with polyvinyl alcohol, and the mixture is uniformly stirred at the rotating speed of 2000rpm to obtain adhesive emulsion;
step 2: dissolving the antibacterial agent in the remaining 10% of water to obtain an antibacterial solution; sequentially adding the nano-porous particles prepared in the preparation example 1, an antibacterial liquid and a thickening agent into the adhesive emulsion, and stirring and mixing at the rotating speed of 800rpm to prepare a spraying liquid;
and step 3: spraying the spraying liquid on the surface of the base paper of the paper cup, and drying at the constant temperature of 40 ℃ for 8 hours to obtain a finished product of the base paper of the paper cup;
and 4, step 4: and gluing the paper cup base paper into the antibacterial paper cup by a paper cup machine.
Comparative example
Comparative example 1, an antibacterial paper cup, is different from example 1 in that a nano-porous material is not added to the raw material of the antibacterial layer, and thus, nano-porous chitosan is not added in step S201.
Comparative example 2, an antibacterial paper cup, which is different from example 1 in that food-grade antibacterial agents are not added to the raw materials of the antibacterial layer; therefore, the preparation steps are as follows:
the method comprises the following steps: mixing water and polyvinyl alcohol, and uniformly stirring at the rotating speed of 2000rpm to obtain adhesive emulsion; sequentially adding the nano porous particles and the thickening agent prepared in the preparation example 1 into the adhesive emulsion, and stirring and mixing at the rotating speed of 800rpm to prepare a spraying liquid;
step two: spraying the spraying liquid prepared in the step one on the surface of the base paper of the paper cup, and drying at the constant temperature of 40 ℃ for 8 hours to obtain a finished product of the base paper of the paper cup;
step three: and gluing the paper cup base paper into the antibacterial paper cup by a paper cup machine.
Comparative example 3: an antibacterial paper cup, wherein the raw paper of the paper cup is not treated, and is directly glued into the antibacterial paper cup by a paper cup machine.
Comparative example 4, an antibacterial paper cup, was different from example 1 in that chitosan having a degree of deacetylation of 95% was used instead of the nanoporous chitosan prepared in preparation example 1 in step S201.
Comparative example 5, a konjac glucomannan antibacterial paper cup was prepared as follows:
(1) preparing konjac glucomannan composite solution: dissolving konjac glucomannan in deionized water to prepare a konjac glucomannan aqueous solution with the weight volume ratio of 0.9g/mL, placing the konjac glucomannan aqueous solution in a water bath at 50 ℃, placing the konjac glucomannan aqueous solution in a magnetic stirrer, and stirring the konjac glucomannan aqueous solution for 2.3 hours at 3000 r/min; according to the weight volume ratio of chitosan to acetic acid solution of 0.9% (g/mL), dissolving chitosan in acetic acid solution with weight concentration of 1%, placing in a water bath at 48 ℃, placing in a magnetic stirrer, and stirring at the rotating speed of 3000r/min for 2.3 h; respectively filtering, mixing the filtered konjac glucomannan aqueous solution with a chitosan acetic acid solution, stirring at 3000r/min for 13min, adding deionized water with the same volume as the konjac glucomannan aqueous solution, adding glycerol accounting for 0.7% of the total volume, uniformly mixing, and adjusting the pH value to 3 by using 1mol/L HCl solution to obtain a mixed solution; putting the mixed solution into a magnetic stirrer, stirring, simultaneously respectively adding stearic acid accounting for 0.27 percent of the weight of the mixed solution, sucrose ester accounting for 0.25 percent of the weight of the mixed solution, paraffin accounting for 0.5 percent of the weight of the mixed solution and polyethylene glycol accounting for 0.15 percent of the weight of the mixed solution, stirring at 3000r/min for 2.5 hours to prepare a konjac glucomannan composite solution; (2) degassing: placing the konjac glucomannan composite solution obtained in the step (1) in a centrifuge, centrifuging and degassing at 3000r/min for 28min at room temperature to obtain a konjac glucomannan mixed gel solution for later use; (3) and (3) plate reversing and film making: flatly paving the konjac glucomannan mixed gel obtained in the step (2) in a mould, drying for 6 hours in an oven at 50 ℃, cooling to room temperature, and then uncovering the film; (4) preparing the konjac glucomannan antibacterial paper cup: and (4) cutting the film obtained in the step (3) according to the specification of the paper cup, and then attaching the film to the inner layer and the outer layer of a raw paper cup made of chemical wood pulp to prepare the konjac glucomannan antibacterial paper cup.
Performance test
Test 1: the antibacterial performance test standard of the paper cup is as follows: detection is carried out according to the detection standard in SN/T15979-2002 "food contact material detection method paper, regenerated fiber cable material paper and paperboard antibacterial substance determination inhibition circle qualitative analysis test method".
Sample preparation: the plain paper cup-forming base papers obtained in examples 1 to 13 and comparative examples 1 to 5 were used as samples in the form of 6mm diameter sheets with a punch.
Preparing a bacterial suspension: respectively separating and purifying staphylococcus aureus and escherichia coli, inoculating a common nutrient agar culture medium slant, and culturing at 37 ℃ for 24 hours; taking a fresh slant culture, washing the slant culture with physiological saline and diluting the slant culture into a bacterial suspension; during the test, the bacterial suspension and the organic interferent are subjected to double dilution to prepare the bacterial suspension with the test concentration for later use.
The test method comprises the following steps: and pouring the sterilized nutrient agar culture medium into a vacuum-dried culture dish, standing for a period of time, after the culture medium is solidified, dropwise adding 1ml of bacterial suspension onto the surface of the culture medium, and uniformly coating by using a coating rod. Then, the paper sheet of the coated paper was placed on a culture medium plate, and placed in a 30 ℃ constant temperature incubator, the size of the zone of inhibition around the sample was measured after 24 hours, each suspension was tested 3 times, and the mean value was taken as the measurement result to measure the zone of inhibition (D) of the sample after Staphylococcus aureus treatment, respectively1) Inhibition zone size (D) of E.coli-treated sample2) The test results are shown in Table 3.
Test 2: the paper cup antibacterial agent adhesion force test method comprises the following steps: filling 100 ℃ boiled water into the paper cup, cooling and standing the paper cup for 12h at room temperature (25 ℃), sampling the side wall of the paper cup according to the operation steps in the test 1, testing, and respectively measuring the size (D) of the inhibition zone of the sample after the staphylococcus aureus treatment3) Inhibition zone size (D) of E.coli-treated sample4) The test results are shown in table 4.
TABLE 3 paper cup antibacterial property test results
Table 4 paper cup antibacterial agent adhesion test results
The observation of no zone of inhibition in tables 2 and 3 indicates that colonies were grown on the sample.
And (3) analyzing test results:
(1) it can be seen by combining examples 1-13 and comparative examples 1-5 and combining tables 3 and 4 that the antibacterial layer prepared by compounding the porous nanoparticles and the food-grade antibacterial agent can significantly improve the antibacterial performance of the paper cup, and the antibacterial layer is not easy to fall off and has a long effective period. The reason for this may be that the pores inside the porous nanoparticles and the larger surface area thereof enable the surface of the paper cup to be attached with more food-grade antibacterial agents, thereby promoting the antibacterial performance of the paper cup to be effectively improved.
(2) By combining the examples 1 and 2-5 and combining the tables 3 and 4, the antibacterial property of the paper cup is better, the antibacterial layer is not easy to fall off, and the effective period is long compared with the porous alumina and the porous silica, and the porous nano chitosan is adopted. The reason for this may be that the nanoporous chitosan has a spectrum antibacterial effect, and can be used in combination with an antibacterial agent to achieve a better antibacterial effect.
In addition, after the nano porous chitosan prepared by the method is treated by sodium hydroxide, more amino groups are formed on the molecular chain of the nano porous chitosan, so that the nano porous chitosan is positively charged, can generate electrostatic adsorption with bacteria (cell membranes have negative charges), improves the contact efficiency of the nano porous particles and the bacteria, and promotes the effects of sterilization and antibiosis.
(3) By combining the examples 1 and 2-5 and combining the tables 3 and 4, the antibacterial property of the paper cup is better, the antibacterial layer is not easy to fall off, and the effective period is long compared with the porous alumina and the porous silica, and the porous nano chitosan is adopted.
The reason for this may be that,
(4) by combining the embodiment 1 and the embodiment 6 and combining the table 3 and the table 4, the porous nano chitosan prepared by crosslinking glutaraldehyde has better antibacterial performance on paper cups and longer effective period of antibacterial action. The reason for this may be that after glutaraldehyde crosslinking, more hydrogen bonds are formed between the molecules of the nanoporous chitosan, and the van der waals force is larger, so that the strength of the molded nanoporous chitosan is higher, the nanoporous chitosan is not easy to collapse during pore formation, and more pore structures can be formed, thereby facilitating the improvement of the antibacterial agent loading capacity, and finally, the antibacterial performance of the preparation is enhanced, and the effective period of the antibacterial action is increased.
(5) By combining the embodiment 1 and the embodiment 7 and combining the tables 3 and 4, the chitosan with the deacetylation degree of more than 90 is used as the raw material to prepare the porous nano chitosan, which is beneficial to improving the antibacterial performance of the paper cup. The reason for this may be that the chitosan with high deacetylation degree has a high content of amine groups on its molecular chain, and can promote the electrostatic adsorption of the porous nano chitosan on bacteria, thereby improving the sterilization and antibacterial effects.
(6) It can be seen from the combination of examples 1 and 8-10 and tables 3 and 4 that the antibacterial performance of the paper cup is greatly improved by adopting ultrasonic treatment and the preparation of the porous nano chitosan, and the effect cannot be achieved without any operation. The reason for this may be that, when the chitosan sol is added dropwise, ultrasonic cavitation can be used to introduce a large amount of micro bubbles into the coagulation liquid, thereby promoting the formation of a large amount of pores in the nanoporous chitosan structure, which is helpful for improving the porosity of the nanoporous chitosan structure, however, the pores are usually closed, no through-channels are formed, and the antibacterial agent is difficult to load; therefore, the method of freeze drying is adopted, so that the moisture permeated into the nano porous chitosan structure is quickly freeze-dried to form pores, and meanwhile, the communication of the pores is promoted, so that more pore channels capable of loading the antibacterial agent are formed, and finally, the antibacterial effect is enhanced.
(7) By combining the examples 1 and 11-12 and combining the tables 3 and 4, it can be seen that the antibacterial layer prepared by the two-step spraying method has a great improvement in the antibacterial performance of the paper cup. The reason for this is probably that if the antibacterial agent is directly mixed with the porous nano chitosan, the adhesive emulsion and other substances for spraying, the antibacterial agent is easily wrapped by the latex and is difficult to exert the antibacterial effect; and the two-step spraying is adopted, the porous Nanmen chitosan is sprayed and fixed to form a bottom coating, and then the antibacterial agent is sprayed, so that the antibacterial agent is fixed on the surface of the bottom coating and is loaded on the porous nano chitosan as much as possible, and the antibacterial effect is fully exerted.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (8)
1. The antibacterial paper cup is characterized in that an antibacterial layer is formed on the surface of the antibacterial paper cup, and the antibacterial layer is prepared by mixing and spraying the following raw materials in parts by weight:
porous nanoparticles: 15-25 parts;
food-grade antibacterial agent: 0.5-2 parts;
polyvinyl alcohol: 13-18 parts;
thickening agent: 1-3 parts;
water: 25-36 parts.
2. The antibacterial paper cup according to claim 1, wherein the porous nanoparticles are one or more of porous nano chitosan, porous alumina and porous silica.
3. The antibacterial paper cup according to claim 2, wherein the porous nano chitosan is prepared according to the following method:
s101, mixing a sodium hydroxide solution with the mass concentration of 3-7% and an ethanol solution with the mass concentration of 90-95% according to the volume ratio of (3-5) to 1 to obtain a condensate;
s102, fully dissolving chitosan in an acetic acid solution to obtain a chitosan solution, adding a glutaraldehyde solution into the chitosan solution, uniformly mixing, and placing in a hot water bath (50 ℃) for reaction and crosslinking to obtain a gel solution;
and S103, dropwise adding the gel liquid into the condensation liquid, fully mixing, filtering, washing with water, and drying to obtain the porous nano chitosan.
4. The antibacterial paper cup according to claim 3, wherein in step S102, the deacetylation degree of chitosan is greater than 90%.
5. The antibacterial paper cup according to claim 3, wherein the specific operations of step S103 are as follows: and (3) dropwise adding the gel liquid into the condensation liquid, carrying out ultrasonic treatment on the mixed solution in the dropwise adding process, filtering, washing, and carrying out freeze drying treatment to obtain the porous nano chitosan.
6. The antibacterial paper cup according to claim 5, wherein the ultrasonic frequency is 20 KHz-30 KHz.
7. The antibacterial paper cup according to claim 1, wherein the thickening agent is one or more of carboxymethyl cellulose, gelatin and polyacrylamide.
8. The preparation method of the antibacterial paper cup according to any one of claims 1 to 7, characterized by comprising the following steps:
s201, uniformly mixing polyvinyl alcohol and 85-95% of water to obtain adhesive emulsion, taking 80-90% of adhesive emulsion, sequentially adding nano porous particles, light calcium carbonate and a thickening agent, and fully mixing to prepare spraying liquid;
s202, uniformly mixing the antibacterial agent, the rest water and the rest adhesive emulsion to obtain an antibacterial liquid;
s203, spraying the spraying liquid prepared in the step S201 on the surface of the base paper of the paper cup, and drying to obtain a semi-finished base paper of the paper cup;
s203, spraying the antibacterial liquid prepared in the step S202 on the surface of the semi-finished product of the raw paper of the paper cup, and drying to obtain a finished product of the raw paper of the paper cup;
and S204, gluing the paper cup base paper into the antibacterial paper cup by adopting a paper cup machine.
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