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    • 专利摘要:
    This invention discloses a germicidal dissolvable polymer and its production method and use, wherein the C-PPC film is produced by centrifugal sizing and electrospinning, with UV phototransplantation SBMA and MA are transplanted on its surfaces to achieve the introduction of the carboxyl, then one or two active factors including cathelicidine (C) and lysozyme (LYZ) are connected on the surface of C-PPC-gP (SBMA-co-MA) by electrostatic interaction to finally get the broad spectrum antibacterial dissolvable polymer. The germicidal dissolvable polymer disclosed in this invention is produced without the use of plasticizer and organic solvent, and has the properties of biodegradation and good antimicrobial ability. Therefore it is very suitable for food packaging, especially for food freshening film.
    公开号:BE1027415B1
    申请号:E20205450
    申请日:2020-06-20
    公开日:2021-02-01
    发明作者:Man Xi；Jing Jin；Yang Jiang
    申请人:Univ Jiaxing；
    IPC主号:
    专利说明:

    Production Method and Use of Germicidal Dissolvable Polymer Technical Field This invention belongs to the field of polymer materials, specifically it concerns a production method and its use of the germicidal dissolvable polymer.
    Technology Background Food-related corruption and pathogenic microorganisms are the most important factors affecting food safety and quality, as food packaging is the key link in suppressing food spoilage and pathogenic microorganisms in the area of food circulation. In the current field of food packaging, polymer packaging is popular with consumers because of its low price and convenient use, especially plastic packaging made of polyethylene (PE), polyvinylidene chloride (PVDC) and polyvinyl chloride (PVC), because of its high transparency and good elasticity often used in everyday food packaging. But with the widespread use of this polymer packaging, we are also very concerned about the white pollution, which has led to the great stability, which is naturally not degradable. Especially for PVC, for example, it needs a large amount of plasticizer in the production of traditional poly packaging, and when it comes into contact with food, plasticizer gradually spreads into food, so it can cause pollution and threaten the health of consumers. That is why the focus of the researchers is to invent a naturally degradable and plasticizer-free, environmentally friendly plastic.
    In addition, traditional packaging uses physical insulation to avoid spoilage and standard surges caused by external factors. For the inhibition of the inside factors of the food is only the germicidal property of food additive. During these years, researchers in the field have become very interested in a revolutionary recipe to guarantee food quality with the active and germicidal packaging, as people want to take more care of their own health and further improve food safety.
    The packaging with active and antibacterial agent first introduces the active factors into the polymer matrix, then it slowly and persistently gets out of the packaging of the finished product for a long-term antibacterial effect. There is currently research into using natural biological macromolecules such as chitosan, starch, cellulose, sodium alginate and so on, or natural plants such as grapefruit peel powder and tea polyphenol and so on for novel food packaging. But some weaknesses like poor water vapor barrier and bad brittleness and heavy film formation has entangled direct use in food packaging.
    That is why it has become an urgent problem for the researchers in this field to develop a polymeric packaging that is biologically soluble, germicidal, air-barrier-able and also has excellent mechanical properties.
    Content of the invention With regard to this, the purpose of the invention is to offer a new production method for the problems in the existing technology of a polymerizate which is biologically dissolvable, germicidal, air-barrier-able and also has very good mechanical properties.
    In order to achieve the above objects, the present invention will adopt the following technical solutions: The manufacturing method of the germicidal dissolvable polymer has the following concrete manufacturing steps: | The solution of chlorine polypropylene carbonate C-PPC to the C-PPC film is produced by the film formation process; II. C-PPC film produced in step | by plasma treatment, then to make the plasma treated C-PPC sheet with methacrylic acid MA and betaine methacrylic acid SBMA in UV photo-transplant to get C-PPC-g-P (SBMA-co-MA); II. Combine C-PPC-g-P (SBMA-co-MA) produced in step II with active factor in order to then get the germicidal dissolvable polymer at the end.
    It should be noted that the weight average molecular weight of the above chloro-polypropylene carbonate (C-PPC) is 2.62 × 10 5, Mw / Mn = 4.5.
    Firstly, with regard to the properties of biodegradability, flexibility and air barrier properties, this invention is designed with chlorine-polypropylene carbonate (C-PPC) as the matrix of the polymer, compared to the PPC of modern technology, C-PPC has all the good properties of PPC, and better germicidal ability than that of PPC. So it is better suited for food cling film. At the same time, the low cost of C-PPC effectively increases the competitiveness compared to other traditional biodegradable plastics.
    In addition, chlorine polypropylene carbonate (PPC) belongs to the polyester, the surface of which has strong hydrophobicity. If you want to use it in the field of medical materials or food packaging, you have to modify its surface in order to increase its hydrophilicity. But take into account the low temperature of the glazing of PPC, its thermal stability is poor compared to normal polymer, it will partially decompose during hot work treatment and can disturb its function, so it should be avoided to improve its property by melt blending processes;
    However, it also needs organic solvent for property improvement with the solution mixing method, nor does it conform to the recipe of using PPC as an environmentally friendly agent. The current change in properties of the surface of the polymer is mainly due to the chemical method, the main methods are: (1) plasma treatment; (2) surface graft; (3) irradiation crosslinking technology; (4) Atomic force microscope probe oscillation and so on. In order not to use organic solutions and other pollutants, this invention first uses chlorine-polypropylene carbonate (C-PPC) as a raw material, the introduction of chlorides improves the germicidal ability of PPC, it is used for the use of PPC in the field of medicine and food packaging and so on; Second, with plasma treatment for the surface of C-PPC, it may favor UV phototransplantation to transplant the -COOH-retaining MA and SBMA on the surface of C-PPC, then introduce lysozyme and cathelicidins through the electro-interaction.
    Finally, the invention uses the active germicidal packaging method for good germicidal ability of the polymer, by electroreaction the positively charged active factors are in the surface of negatively charged polymer C-PPC-gP (SBMA-co-MA), so one can then obtain broadband antibacterial composite polymer .
    Optimally, the production method for the C-PPC film includes step | according to the following concrete step: | -1. Using a film-forming process to produce a solution of C-PPC from a mass concentration of 8 - 13% to C-PPC film; | -2. The C-PPC film obtained from step I-1 to lie in the evacuated drying box to allow it to dry at room temperature to constant weight.
    More optimally, the film formation process includes spin coating and electrospinning.
    The method used to manufacture C-PPC film with the above-mentioned spin coating is exemplary: take the C-PPC water solution with a manufacturing concentration of 8-13%, 100-200 μl drops with a pipette and drop them onto a spin coater, the rotation speed from 8000 rpm - 10000 rpm and the treatment time set to 30 s in order to obtain C-PPC film.
    A production method of the mentioned electrospinning for C-PPC film is exemplary: the C-PPC solution composed with a mass concentration of 8 - 13%, with an inner diameter of the spinning needle 0.33 - 0.80 mm, spinning voltage of 4 - 15 kV, with push speed of 0.06 - 0.3 mm / min, rotation speed of the receiving roller of 20 - 60 rpm, receiving distance of 5 - 15 cm, the spinning needle temperature of 20 - 30 ° C, humidity of 30 - 60%, of spiders to be obtained from C-PPC film.
    Optimally, the production method of C-PPC-g-P (SBMA-co-MA) in step II as in the following specific step: II-1. That in step | clean the produced C-PPC film of constant weight in the plasma, with the setting of 100W power and 60 - 90 s treatment time; II-2. To compose the aqueous MA-SBMA-water solution, the weight ratio of MA: SBMA: water being 1: 1: 4; II-3. The aqueous solution compiled in step II-2 on the C-PPC film plasma-treated in step 1-1, and also by the UV phototransplantation with the UV wavelength of 365 nm, the power of 300 W, the treatment duration of 5-30 min to get C-PPC-gP (SBMA-co-MA).
    Optimally, the active factors mentioned in step III comprise at least one or two types of lysozyme (LYZ) and cathelicidine (C).
    Of which, lysozyme (Lysozyme, LYZ) is an excellent natural antibacterial protein that can be produced in an inexpensive commercial manner, it is a glycoside hydrolase that can specifically hydrolyze the main component peptidoglycan in the prokaryotic bacterial cell wall. It can interact directly with negatively charged viral proteins, and form salts with DNA, RNA, and apoproteins to inactivate viruses and directly hydrolyze gram-positive bacteria; with the participation of secreted immunoglobulin A and complement, it can also hydrolyze gram-negative bacteria such as E. coli.
    Cathelicidine (Cecropin) is a class of low molecular weight peptides that are widely used, have a small molecular weight, good thermal stability, a broad spectrum antibacterial, and an effective broad spectrum antibacterial spectrum against Gram negative and positive bacteria, and other properties. It has been reported at home and abroad that at least 113 different bacteria can be killed by antibacterial peptides, and some antibacterial peptides have a strong killing effect on some bacteria, fungi, protozoa and viruses. It is generally believed that some cathelicidins act on cell membranes and form transmembrane ion channels on the membranes, thereby disrupting the integrity of the membranes and allowing the cell contents to leak, then killing the cells.
    The production process of the germicidal dissolvable polymer in step II includes more optimally: II-1. Compiled individual active factors with a concentration of 0.1 - 2 mg / ml PBS solution; IIl-2. C-PPC-gP (SBMA-co-MA) produced by step II to be put in the active factors / PBS solution compiled from step III-1, and with the condition of 37 + 0.5 ° C and the constant temperature for 30 - 150 min, then showering three times with PBS buffer solution to get germicidal dissolvable polymer of single active factor;
    II-3. Repeat steps III-1 - III-2 to get germicidal dissolvable polymer of multi-active factor.
    The pH of the PBS buffer is preferably 7.4.
    Compared with modern technology, C-PPC is fully bio-dissolvable 5 polymer materials in this invention as the matrix, the presented manufacturing method has avoided the use of plasticizers and organic solutions, and through the introduction of active factors such as lysozyme and cathelicidine, the antibiotic activity is dissolvable Polymerizate has increased, this manufacturing method is easy to use, and it is also environmentally friendly and has good prospects for use in the future.
    The other object thereof is to provide a method for preparing the above germicidal dissolvable polymer and to obtain a germicidal dissolvable polymer.
    The germicidal dissolvable polymer preferably comprises C-PPC-gP (SBMA-co-MA) - co-LYZ conjugated polymer, C-PPC-gP (SBMA-co-MA) -co-C conjugated polymer or C- PPC-gP ( SBMA-co-MA) -co-LYZ / C conjugated polymer.
    Another aim is to offer a method for preparing the germicidal dissolvable polymer with the use of film and corresponding film production. In some application situations, the film and the corresponding film production includes the food freshness film.
    According to the technical production proposal, this invention, compared to modern technology, offers a germicidal dissolvable polymer and its production method and its use to prepare C-PPC film by spin coating and electrospinning, and P (SBMA-co-MA) with UV phototransplantation on the To transplant surface to achieve the introduction of hydroxyl, finally to combine one or two active factors including cathelicidine (C) and lysozyme (LYZ) through the electro-interaction on the surface of C-PPC-gP (SBMA-co-MA) Dissolvable polymer C-PPC-gP (SBMA-co-MA) -co-LYZ, C-PPC-gP (SBMA-co-MA) -co-C and C-PPC-gP (SBMA-co-MA) -co -LYZ / C with antimicrobial properties, in addition, the use of plasticizers in the preparation of the germicidal dissolvable polymer is avoided, so it is very suitable for food packaging, specifically for food wrap.
    Description of Figures In order to explain the embodiments of the present invention or the technical solutions in the current state of the art more clearly, the drawings required in the embodiments or the description of the state of the art are briefly presented below. Obviously the drawings in the following description are only one embodiment, those of ordinary skill in the art can design other drawings in accordance with the drawings provided without using any creative work. Figure No. 1 is the diagram of the manufacturing process of the germicidal dissolvable polymer C-PPC-g-P (SBMA-co-MA) -co-C conjugated polymer.
    Figure No. 2 is an XPS grid energy spectrum offered by the C-PPC film, C-PPC-g-P (SBMA-co-MA) film and C-PPC-gP (SBMA-co-MA) -co-LYZ film in example 1. of the invention.
    Figure 3 is the bacterial inhibition rate diagram of the PPC film, C-PPC film, C-PPC-gP (SBMA-co-MA) film and C-PPC-gP (SBMA-co-MA) -co- LYZ film offered in Example 2 of the invention. DETAILED METHOD OF EMBODIMENT Now, the technical proposals having the embodiments of the present invention will be clearly and fully described in conjunction with the drawings of the present invention. Obviously, the exemplary embodiments described are only a part of the present examples of the invention, not all of them. Based on the exemplary embodiments of the present invention, all other examples that are designed by a person skilled in the art without creative efforts also fall within the scope of the present invention.
    In the embodiments of the present invention, a germicidal dissolvable polymer and its production method and use are fully published, the polymerisate materials produced by this method are biologically dissolvable and good germicidal, while it does not consume any organic solution and pollutant, where the deficiency is remedied with current technology, so it is suitable for use in food packaging.
    The manufacturing process for the germicidal dissolvable polymer is characterized by the following specific manufacturing steps: |. The solution of chlorine polypropylene carbonate C-PPC to the C-PPC film is produced by the film formation process; II. C-PPC film produced in step | by plasma treatment, then to make the plasma treated C-PPC sheet with methacrylic acid (MA) and betaine methacrylic acid (SBMA) in UV photo transplant to get C-PPC-g-P (SBMA-co-MA); Il. C-PPC-g-P (SBMA-co-MA) produced in step II to be combined with active factor in order to finally get the germicidal dissolvable polymer.
    C-PPC film is optimal in the aforementioned step | the following concrete steps: | -1. Using a film-forming process to produce a solution of C-PPC from a mass concentration of 8 - 13% to C-PPC film;
    | -2. The C-PPC film obtained from step I-1 to lie in the evacuated drying box to allow it to dry at room temperature to constant weight.
    Optimally, the film formation process presented in step 1-1 includes spin coating and electrospinning.
    The following are optimally included in the production method of C-PPC-g-P (SBMA-co-MA) in step II: II-1. That in step | Clean the produced C-PPC film of constant weight in the plasma, with the setting of 100W power and 60 - 90s treatment duration II-2. To compose the aqueous MA-SBMA-water solution, the weight ratio of MA: SBMA: water being 1: 1: 4; I -3. The aqueous solution compiled in step II-2 on the C-PPC film plasma-treated in step 1-1, and also through the UV photo transplantation with the UV wavelength of 365 nm, the power of 300 W, the treatment duration of 5 - 30 min, to get C-PPC-gP (SBMA-co-MA).
    Optimally, the active factors mentioned in step III include at least one or two types of lysozyme LYZ and cathelicidine C.
    Optimally, the manufacturing process of the germicidal dissolvable polymer in step III comprises more precisely: II-1. Compiled individual active factors with a concentration of 0.1 - 2 mg / ml PBS solution; IIl-2. C-PPC-gP (SBMA-co-MA) produced by step II to be put in the active factors / PBS solution compiled from step III-1, and with the condition of 37 + 0.5 ° C and the constant temperature for 30 - 150mim, then shower three times with PBS buffer solution to get germicidal, dissolvable polymer of single active factor; II-3. Repeat steps III-1 - III-2 to get germicidal dissolvable polymer of multi-active factor.
    The invention claims patent protection for the manufacturing process of the germicidal dissolvable polymer, the germicidal dissolvable polymer preferably comprises C-PPC-gP (SBMA-co-MA) -co-LYZ conjugated polymer, C-PPC-gP (SBMA-co-MA) - co-C conjugated polymer or C-PPC-gP (SBMA-co-MA) -co-LYZ / C conjugated polymer.
    At the same time, the property right also requires the use of the above-mentioned germicidal dissolvable polymer in the manufacture of the film and its corresponding film production.
    The mentioned film and the corresponding film production are ideally suited for food freshness film.
    For a better understanding of this invention, there are specific embodiments for further interpretation, but they are not a limitation on this invention if those skilled in the art are familiar
    ; BE2020 / 5450 make some insignificant changes and improvements from this technical area, should it also belong to the scope of protection. If a range of values is given in the examples, it should be understood, without any other explanation of the invention, that any value between the two end values can be considered an alternative end value. In addition, all technical terms of all technologies and academic terms have the same meanings as those of ordinary skill in the art to understand this invention. Without any specific explanation, all raw materials used for the invention are the general products on the market.
    Embodiment 1. The manufacturing process of a germicidal dissolvable polymer comprises the following steps: |. Prepare C-PPC solution with a concentration of 9%, drop 100 μl drops with a pipette on a spin coater, with the setting of rotation speed 8500 rpm, treatment time 30 s, to produce C-PPC film, place the film in an evacuated drying box to let it dry to constant weight at room temperature, then let it treat in plasma with the power of 100 W, take it out after 60 s. Il. The methacrylic acid (MA) and betaine methacrylic acid (SBMA) each put together 0.25 g plus 1 g water to the solution, then 100 μl drops with pipette to drop on the C-PPC film treated by the plasma, then in UV microwave If you take UV-Ultrasonic-Triune- Synthesizer, with the UV-wavelength of 365nm and the power 300W and the UV-treatment time 10 min, then you can get C-PPC-gP (SBMA-co-MA). III. Put together a lysozyme (LYZ) / PBS solution with a concentration of 1 mg / ml, put C-PPC-gP (SBMA-co-MA) into the LYZ / PBS solution, then place it in the shaking table at a constant temperature of 37 + 0.5 ° C for 60 min; Then rinse three times with PBS buffer solution, then you can obtain C-PPC-g-P (SBMA-co-MA) -co-LYZ germicidal dissolvable polymer. Embodiment 2. The manufacturing process of a germicidal dissolvable polymer comprises the following steps: |. Compile C-PPC spinning solution with a concentration of 10%, diameter of the spinning needle is 0.41 mm, spinning voltage 6 kV, push speed of 0.08 mm / min, the rotational speed of the receiving roller 20 rpm, receiving distance 10 cm, spinning temperature 25 ° C, humidity 40%, then it is made by spinning C-PPC film. place the C-PPC film in an evacuated drying box to allow it to dry to constant weight at room temperature.
    Il. Have the C-PPC film treated in the plasma with the power of 100W, take it out after 70 s, then take it in the UV-microwave-UV-ultrasound-Triune-Synthesizer. The methacrylic acid (MA) and betaine methacrylic acid (SBMA) each add 0.55 g plus 2.2 g water to the solution, then drop 200 μl drops with a pipette onto the C-PPC film treated by the plasma, and then with the UV treatment duration for 20 minutes, one can get C-PPC-gP (SBMA-co-MA).
    III. Put together a lysozyme (LYZ) / PBS solution with a concentration of 0.5 mg / ml, insert C-PPC-gP (SBMA-co-MA) into the LYZ / PBS solution, then place it in the shaking table at a constant temperature of 37 + 0 , 5 ° C for 100 min; Then rinse three times with PBS buffer solution, then you can obtain C-PPC-g-P (SBMA-co-MA) -co-LYZ germicidal dissolvable polymer.
    Embodiment 3.
    |. Prepare C-PPC solution with a concentration of 11%, drop 130 μl drops with a pipette onto the spin coater, with the setting of rotation speed 10000 rpm, treatment duration 30 s, to produce C-PPC film.
    Il. Have the C-PPC film treated in the plasma with a power of 100W, take it out after 80s, then put it in a UV-microwave-UV-ultrasound-Triune-Synthesizer. The methacrylic acid (MA) and betaine methacrylic acid (SBMA) each add 0.1 g plus 0.4 g water to the solution, then drop 200uL drops with a pipette on the C-PPC film treated by the plasma, and then with the UV -Treatment time for 30min, one can get C-PPC-gP (SBMA-co-MA).
    III. Assemble Cathelicidine (C) / PBS solution with a concentration of 2 mg / ml, insert C-PPC-gP (SBMA-co-MA) into the C / PBS solution, then place it in the shaking table at a constant temperature of 37 ° C for 60 minutes lie still; Then rinse three times with PBS buffer solution, then one can obtain C-PPC-g-P (SBMA-co-MA) -co-C germicidal dissolvable polymer.
    Embodiment 4.
    The manufacturing process of a germicidal dissolvable polymer comprises the following steps: |. C-PPC spinning solution with a concentration of 13%, diameter of the spinning needle is 0.51 mm, spinning voltage 8kV, push speed of 0.09 mmmin, the rotational speed of the receiving roller 60 rpm, receiving distance 8 cm, spinning temperature 25 ° C, humidity 35% then it is made from spinning C-PPC film. To lay the C-PPC film in the evacuated drying box to let it dry at room temperature to a constant weight.
    Il. Have the C-PPC film treated in the plasma with a power of 100 W, take it out after 90 s, then put it in a UV-microwave-UV-ultrasound-Triune-Synthesizer. The methacrylic acid (MA) and betaine methacrylic acid (SBMA) each add 0.25 g plus 1 g of water to the
    To assemble the solution, then to drop 150 µl drops with a pipette on the plasma treated C-PPC sheet, and then with the UV treatment time for 10min, one can get C-PPC-g-P (SBMA-co-MA). III. Assemble Cathelicidine (C) / PBS solution with a concentration of 1 mg / ml, insert C-PPC-gP (SBMA-co-MA) into the C / PBS solution, then place it in the shaking table at a constant temperature of 37 ° C for 60 minutes lie; Then rinse three times with PBS buffer solution, then one can obtain C-PPC-g-P (SBMA-co-MA) -co-C germicidal dissolvable polymer. Embodiment 5. The method for producing a germicidal dissolvable polymer comprises the following steps: |. C-PPC spinning solution with the concentration of 12%, diameter of the spinning needle is 0.75 mm, spinning voltage 12 kV, push speed of 0.15 mm / min, the rotational speed of the receiving roller 40 rpm, receiving distance 15 cm, spinning temperature 30 ° C , Humidity 55%, then it is made from spinning C-PPC film. the C-PPC film in the evacuated drying box to let it dry at room temperature to constant weight. Il. Have the C-PPC film treated in the plasma with a power of 100 W, take it out after 85 s, then put it in a UV-microwave-UV-ultrasound-Triune-Synthesizer. The methacrylic acid (MA) and betaine methacrylic acid (SBMA) each add 1 g plus 4 g water to the solution, then drop 200 μl drops with pipette onto the plasma-treated C-PPC film, and then with the UV treatment duration for 25min, you can get C-PPC-gP (SBMA-co-MA). III. Put the LYZ / PBS and C / PBS solution together, insert the C-PPC-gP (SBMA-co-MA) into the LYZ / PBS solution of 2 mg / ml, then lie in the shaking table at a constant temperature for 145 min, then with Rinse the PBS buffer solution three times, then place it in the C / PBS solution of 2 mg / ml at constant temperature for 145 min; Then rinse three times with PBS buffer solution to obtain C-PPC-g-P (SBMA-co-MA) -co-LYZ / C germicidal dissolvable polymer.
    Embodiment 6. The manufacturing process of a germicidal dissolvable polymer comprises the following steps: |. Put together C-PPC spinning solution with a concentration of 12%, drop 150 μl drops with a pipette onto the spin coater, setting a rotation speed of 9500 rpm, treatment time 30 s, in order to produce C-PPC film. Il. Have the C-PPC film treated in the plasma with a power of 100 W, take it out after 85 s, then put it in a UV-microwave-UV-ultrasound-Triune-Synthesizer. The
    Add methacrylic acid (MA) and betaine methacrylic acid (SBMA) each 0.5 g plus 2 g water to the solution, then drop 200 µl drops with pipette on the plasma-treated C-PPC film, and then with the UV treatment duration for 7 min, one can get C-PPC-gP (SBMA-co-MA). III. Put the LYZ / PBS and C / PBS solution together, put C-PPC-gP (SBMA-co-MA) into the LYZ / PBS solution of 1.5 mg / ml, then lie in the shaking table at constant temperature for 100 min , rinse with PBS buffer solution three times, then put it in the C / PBS solution of 1.5 mg / mL again in the shaking table at constant temperature for 100 min; Then rinse with PBS buffer solution three times, you can then obtain C-PPC-g-P (SBMA-co-MA) -co-LYZ / C germicidal dissolvable polymer. The contents of the invention are not limited to the above-mentioned exemplary embodiments, of which the combinations of one or some examples can also achieve the objects of this invention. In order to further verify the advantageous effects of the present invention, the inventors also carried out the following experiments: Experiment 1: The invention is proven by XPS energy spectrum, C-PPC-gP (SBMA-co-MA) film successfully by UV - Obtain phototransplantation of SBMA and MA on the C-PPC film, as well as successfully introduce LYZ through the electro-interaction and then one can obtain C-PPC-gP (SBMA-co-MA) -co-LYZ germicidal dissolvable polymer. (See Figure # 2) It's worth noting that the purpose of UV phototransplantation is to introduce SBMA and MA with COOH- on the C-PPC sheet so that positively charged lysozyme (LYZ) and cathelicidine (C) pass through Electrostatic interaction Interaction can be introduced.
    The element content of the material surface can be obtained by X-ray photoelectron spectroscopy (XPS). PPC is a polyester polymer, the components of chlorinated PPC (C-PPC) are C, O and Cl, the Cl element content is 3.1%; The main elements in C-PPC-gP (SBMA-co-MA) are C, O, CI and a small amount of N and S, since in the SBMA and MA there is quaternary ammonium salt (-N * (ChH2n + 1) *), There are sulfonic acid group (- SOs) and carboxyl group (-COOH), therefore there are small amounts of N and S elements, and yet the part of O increases; Introduce lysozyme (LYZ) into C-PPC-g-P (SBMA-co-MA) -co-LYZ to produce C-PPC-g-P (SBMA-co-MA); LYZ is a kind of single molecule single globule protein linked by 129 amino acids by four disulfide bonds, therefore the introduction of LYZ makes the increase of N and S. By XPS data, the success of the sample preparation can be proven, the concrete data is the See table 1.
    Table 1 Content of all elements in the sample by XPS test sample C O C N [oo | C-PPC 7 2 3 / /
    EDEN C-PPC-g-P (SBMA-co-MA) 6 3 2 0 0 [ae an en C-PPC-g-P (SBMA-co-MA) -co-LYZ 6 2 2 2 0
    ES Experiment 2: Testing the germicidal ability of the polymer An important indicator for food preservation is the guarantee of freshness of food without bacteria. When the fresh-keeping film comes into contact with food, if the fresh-keeping film has antibacterial properties, the bacteria generated during the transportation, storage, etc. of the food can be suppressed or even killed. The antibacterial and antibacterial performance is therefore an important indicator of the freshness film of the food.
    The invention uses a turbidimetric spectrophotometer method to determine the bacteriostatic effect of the target material. First, Colibacillus (gram negative bacteria) was placed in a nutrient agar medium in a carbon dioxide incubator and incubated at 37 ° C for 24 hours. Pick up the bacteria with a pipette, then incubate them in an Erlenmeyer flask in the liquid LB solution medium and on the shaking table at 37 ° C and 170 r / min. During the period of logarithmic growth, the germicidal and dissolvable polymer should be added, of which 0.2 g should be taken in each 50 ml LB solution medium and at the same time incubated with a control group (no germicidal and dissolvable polymer), then further incubated on the shaking table.
    Effect test of the antibacterial dissolvable polymer: For the group with antibacterial dissolvable polymer 12 hours test ODs4 in comparison with the control group. Different antibacterial rates, where different dissolvable polymer cling films were used, the antibacterial rate should then be calculated: Antibacterial rate = (control group OD value-test group OD value) / (test group OD value) x 100%.
    In the antibacterial test it was discovered that the PPC film, C-PPC film, C-PPC-gP (SBMA-co-MA) film and C-PPC-gP (SBMA-co-MA) -co-LYZ- Foil have very good antibacterial properties against Colibacillus (Gram-negative bacteria), antibacterial rate for 12 hours can be seen in Figure 3.
    In all performance examples of this explanation, it is described progressively, each embodiment concentrates on the differences from other embodiments, the same and similar parts therebetween can be related to each other. For the method disclosed in the exemplary embodiment, the description is relatively simple since it corresponds to the method disclosed in the experiment, and the relevant part can also be referred to the description in the method section.
    The above descriptions of the experiments described could be realized by any person skilled in the art and utilize the invention. Many changes in the experiments can be made by those skilled in the art simply on the basis of the general principles and claims, without departing from the scope and idea of this invention. Therefore, this invention is not limited to the examples given, but should be the widest scope that corresponds to the creative nature and published principles.
    权利要求:
    Claims (9)
    [1]
    1. Manufacturing process of a germicidal dissolvable polymer, characterized by the following specific manufacturing steps: |. The solution of chlorine-polypropylene carbonate (C-PPC) to the C-PPC film is produced through the film formation process; Il. C-PPC film produced at step | by plasma treatment, then to make the plasma treated C-PPC sheet with methacrylic acid (MA) and betaine methacrylic acid (SBMA) in UV photo transplant to get C-PPC-g-P (SBMA-co-MA); II. C-PPC-g-P (SBMA-co-MA) produced in step I to be combined with active factor in order to finally get the germicidal dissolvable polymer.
    [2]
    2. Production method of a germicidal dissolvable polymer according to claim 1, characterized in that the in step | called C-PPC film has the following concrete steps: | -1. Using a film-forming process to produce a solution of C-PPC from a mass concentration of 8 - 13% to C-PPC film; | -2. To lay the C-PPC film obtained in step I-1 in the evacuated drying box to allow it to dry at room temperature to a constant weight.
    [3]
    3. The production method of a germicidal dissolvable polymer according to claim 2, characterized in that the film formation process mentioned in step 1-1 comprises spin coating and electrospinning.
    [4]
    4. The production method of a germicidal dissolvable polymer according to claim 1, characterized in that the production method of C-PPC-g-P (SBMA-co-MA) in step II comprises the following steps: II-1. That in step | clean the produced C-PPC film of constant weight in the plasma, with the setting of 100W power and 60 - 90 s treatment time; 1-2. To compose the aqueous MA-SBMA-water solution by weight ratio of MA: SBMA: water 1: 1: 4; II-3. The aqueous solution compiled in step II-2 on the C-PPC film plasma-treated in step 1-1, and also by the UV phototransplantation with the UV wavelength of 365 nm, the power of 300 W, the treatment duration of 5-30 min to get C-PPC-gP (SBMA-co-MA).
    [5]
    5. The production method of a germicidal dissolvable polymer according to claim 1, characterized in that the active factors mentioned in step III comprise at least one or two types of lysozyme LYZ and cathelicidine C.
    [6]
    6. The production method of a germicidal dissolvable polymer according to claim 1, characterized in that the production method of the germicidal dissolvable polymer in step II comprises more precisely: III-1. Compiled individual active factors with a concentration of 0.1 - 2 mg / ml / PBS solution; IIl-2. C-PPC-gP (SBMA-co-MA) produced from step II to be put in the active factors / PBS solution compiled from step III-1, and with the condition of 37 + 0.5 ° C and the constant temperature for 30 - 150 min, then showering three times with PBS buffer solution in order to get a germicidal, dissolvable polymer of individual active factors; II-3. Repeat steps II-1 - 1-2 to get the germicidal dissolvable polymer of multi-active factor.
    [7]
    7. Production method of a germicidal dissolvable polymer according to any one of claims 1-5, characterized in that the germicidal dissolvable polymer is C-PPC-gP (SBMA-co-MA) -co-LYZ conjugated polymer, C-PPC-gP (SBMA-co -MA) -co-C conjugated polymer or C-PPC-gP (SBMA-co-MA) -co-LYZ / C conjugated polymer.
    [8]
    8. Use of the germicidal dissolvable polymer according to claim 7 in film production and for film products.
    [9]
    9. Use of the germicidal dissolvable polymer according to claim 8, wherein the film products comprise food freshness film.
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    同族专利:
    公开号 | 公开日
    CN110628071A|2019-12-31|
    引用文献:
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    CN104479081B|2015-01-14|2017-03-29|河北工业大学|A kind of method by the modified polypropylene carbonate of reactive extrursion|
    CN106700108B|2016-12-05|2020-02-07|深圳职业技术学院|Degradable antibacterial preservative film and preparation method thereof|
    CN109232834A|2018-08-02|2019-01-18|浙江工业大学|It is a kind of with anti-pollution-sterilization-release triple functions antibacterial polymer brush and preparation method thereof|
    CN110105612A|2019-05-31|2019-08-09|苏州农业职业技术学院|A kind of preparation method of degradable composite multifunction packaging film|CN110511160A|2019-08-06|2019-11-29|浙江中科恒泰新材料科技有限公司|A kind of method thatacrylamide dehydration preparesacrylonitrile|
    法律状态:
    2021-04-19| FG| Patent granted|Effective date: 20210201 |
    优先权:
    申请号 | 申请日 | 专利标题
    CN201910912282.5A|CN110628071A|2019-09-25|2019-09-25|Antibacterial degradable polymer and preparation method and application thereof|
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