CN112920471A - Antibacterial water-resistant material and preparation method thereof - Google Patents
Antibacterial water-resistant material and preparation method thereof Download PDFInfo
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- CN112920471A CN112920471A CN202110222898.7A CN202110222898A CN112920471A CN 112920471 A CN112920471 A CN 112920471A CN 202110222898 A CN202110222898 A CN 202110222898A CN 112920471 A CN112920471 A CN 112920471A
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- fatty acid
- acid ester
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L3/00—Compositions of starch, amylose or amylopectin or of their derivatives or degradation products
- C08L3/12—Amylose; Amylopectin; Degradation products thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2303/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2303/12—Amylose; Amylopectin; Degradation products thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2489/00—Characterised by the use of proteins; Derivatives thereof
-
- 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
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- 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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention belongs to the field of preparation of antibacterial water-resistant materials, and particularly relates to an antibacterial water-resistant material and a preparation method thereof. The specific technical scheme is as follows: the tea polyphenol composition comprises, by weight, 15-40 parts of amylose, 15-30 parts of tea polyphenol, and 5-15 parts of composite fatty acid ester and hydrophobic fatty acid ester in total. Amylose and tea polyphenol are crosslinked to form a matrix material with a net structure, fatty acid ester is compounded on the matrix material, and hydrophobic fatty acid ester is filled in the matrix material to form a more compact grid structure material, so that the material has excellent degradation performance, has the functions of bacteriostasis and oxidation resistance, and improves the water resistance of the material.
Description
Technical Field
The invention belongs to the field of preparation of antibacterial water-resistant materials, and particularly relates to an antibacterial water-resistant material and a preparation method thereof.
Background
The traditional packaging material generally adopts petroleum-based materials such as polyethylene, and the materials are difficult to degrade and cannot be recycled after being discarded, and if the incineration disposal mode is adopted, a plurality of toxic byproducts are generated; if a direct landfill treatment is used, it takes a long time to completely degrade. Therefore, the search for a degradable, environment-friendly and durable packaging material is a hot point of research in the field of materials in recent years.
Starch is a nutrient stored in plants, has wide sources, is degradable macromolecular carbohydrate, has good film forming property, and can be used for preparing degradable materials. However, the material prepared by using starch as the main component has poor antibacterial performance, and is easily infected by various bacteria to influence the use of the material. Tea polyphenol is a fused ring aromatic hydrocarbon, and contains various components such as various alcohols, ketones, phenolic acids and the like, wherein catechin is mainly used, and the content of the tea polyphenol is about 70%. Tea polyphenol has strong antioxidation, and the antioxidation performance of the tea polyphenol is enhanced along with the rise of temperature, while the packaging material generally requires the tea polyphenol to have the antioxidation capability; besides the antioxidant effect, the tea polyphenol also has the bacteriostatic effect, such as the inhibitory effect on glucose bacteria, escherichia coli, bacillus subtilis and the like, and also has the effects of deodorizing, preventing food discoloration and inhibiting the formation of nitrite.
The packaging material is also required to have a water-resistant function, and the water-resistant agent is generally applied to the interior or the surface of the packaging material so as to make the packaging material have the water-resistant function, but the water-resistant agent usually releases a certain amount of pollutants during the production and use processes, so that the environment is polluted.
Disclosure of Invention
The invention aims to provide a bacteriostatic water-resistant material and a preparation method thereof, wherein the material has the characteristics of degradability, antibacterial property, water resistance and good heat resistance.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows: the bacteriostatic water-resistant material comprises, by weight, 15-40 parts of amylose, 15-30 parts of tea polyphenol, and 5-15 parts of composite fatty acid ester and hydrophobic fatty acid ester in total.
Preferably: the composite material also comprises 3-10 parts of degradable composite material, wherein the degradable composite material comprises one or more of PLA, PBAT, gelatin and chitosan.
Preferably: the mass ratio of the composite fatty acid ester to the hydrophobic fatty acid ester is (1-5): 1 to 8.
Preferably: the complex index ACI of the composite fatty acid ester is more than 50, and the composite fatty acid ester comprises one or more of glyceryl monostearate, stearoyl lactate, sodium stearoyl lactylate and calcium stearoyl lactylate.
Preferably: the water oil degree HLB of the hydrophobic fatty acid ester is lower than 5, and the hydrophobic fatty acid ester comprises one or more of medium-carbon chain polyglycerol fatty acid ester, sucrose glycerol fatty acid ester, soybean phospholipid, glycerol monostearate and propylene glycol ester.
Correspondingly: a preparation method of a bacteriostatic water-resistant material comprises the following steps:
a1, preparing an amylose and tea polyphenol solution which are uniformly mixed, adding a cross-linking agent at the temperature of 20-60 ℃, and continuously stirring the mixed solution to prepare a cross-linked product of the amylose and the tea polyphenol, thereby obtaining a base material;
a2, adding the fatty acid ester for compounding into the cross-linked product prepared in the step A1 at the temperature of 20-50 ℃, stirring continuously in the whole process to form a compound of amylose and the fatty acid ester for compounding, standing the mixture solution for 2-5 hours, and separating the upper-layer free water in the mixed solution to obtain a composite base material;
a3, adding the hydrophobic fatty acid ester into the composite base material prepared in the step A2, and after the hydrophobic fatty acid ester is subjected to ultrasonic treatment and is dispersed uniformly, enabling the hydrophobic fatty acid ester to enter cross-linked grid pores of the composite base material, so as to obtain the antibacterial waterproof material.
Preferably: and A4, compounding the antibacterial waterproof material prepared in the step A3 with the degradable material, and then preparing the antibacterial waterproof material by a tape casting method or a screw extrusion method.
Preferably: the cross-linking agent in the step A1 comprises any one of glutaraldehyde, trimethylolpropane, pentaerythritol, epichlorohydrin, 1, 3-dichloro-dipropanol and acrylic acid.
Preferably: and in the step A1, mechanical stirring is adopted, the stirring speed is 50-150 r/min, and the continuous stirring time is 30-120 min.
Preferably: in the step A3, the ultrasonic treatment time is 10-30 min, and the treatment power is 300-600W.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, the hydroxyl groups of amylose and the phenolic hydroxyl groups of tea polyphenol are crosslinked to form a crosslinked product with a net structure, both amylose and tea polyphenol belong to degradable substances, and the prepared material has excellent degradation performance and cannot cause pollution to the environment; meanwhile, the tea polyphenol has the functions of bacteriostasis and antioxidation, and the service life and the safety of the material are prolonged.
2. According to the invention, the composite fatty acid ester is added into the substrate material of amylose and tea polyphenol, the fatty acid ester can react with the amylose, the amylose solution can generate a d-helical structure, the amylose is subjected to the action of intramolecular hydrogen bonds to form an alpha-helical structure, fatty acid chains in the composite fatty acid ester enter the d-helical structure of the amylose and are arranged in a spiral body in an oriented manner to form a stable composite, and a more compact matrix material with a grid structure is formed.
3. The method adopts an ultrasonic treatment mode to oscillate the fatty acid ester for hydrophobicity to the space between the pores in the matrix material with the grid structure and fill the pores to form a more compact material with the grid structure, and meanwhile, the fatty acid ester for hydrophobicity has a hydrophobic function, so that the water resistance function of the material is further improved; the hydrophobic fatty acid ester has good stability and heat resistance, is not easy to hydrolyze, has the functions of fresh keeping and corrosion prevention and has the inhibiting effect on various bacteria, wherein the medium-chain fatty acid polyglycerol ester has stronger antibacterial effect on bacteria, mould, clostridium botulinum, heat-resistant bacteria, yeast and spores, and the antibacterial performance of the material is further improved.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Unless otherwise indicated, the technical means used in the examples are conventional means well known to those skilled in the art.
The solvents and materials used in the present invention can be obtained commercially, unless otherwise specified. In the invention, PLA is polylactic acid, PBAT is poly adipic acid/butylene terephthalate, the composite fatty acid ester is a fatty acid ester which can perform composite reaction with amylose, and the hydrophobic fatty acid ester is a lipophilic fatty acid ester.
The invention discloses a bacteriostatic water-resistant material which comprises, by weight, 15-40 parts of amylose, 15-30 parts of tea polyphenol, and 5-15 parts of composite fatty acid ester and hydrophobic fatty acid ester.
Further, the antibacterial water-resistant material also comprises 3-10 parts of degradable composite material, including one or more of PLA, PBAT, gelatin and chitosan.
Further, the mass ratio of the composite fatty acid ester to the hydrophobic fatty acid ester is 1-5: 1-8.
Further, the complex index ACI of the composite fatty acid ester is more than 50, and the composite fatty acid ester comprises one or more of glycerol monostearate, stearoyl lactate, sodium stearoyl lactylate and calcium stearoyl lactylate, and preferably glycerol monostearate.
Further, the water oil degree HLB of the hydrophobic fatty acid ester is lower than 5, the hydrophobic fatty acid ester comprises one or more of medium-carbon chain polyglycerol fatty acid ester, sucrose glycerol fatty acid ester, soybean phospholipid, glycerol monostearate and propylene glycol ester, and the medium-carbon chain polyglycerol fatty acid ester is preferred.
The invention also discloses a preparation method of the antibacterial water-resistant material, which comprises the following steps:
a1, dissolving amylose in a solvent at 20-60 ℃ to prepare an amylose solution, dissolving tea polyphenol in the solvent at 20-50 ℃ to prepare a tea polyphenol solution, and continuously stirring the solutions in a mechanical stirring mode at a stirring speed of 20-60 r/min until the solutions are completely dissolved. Uniformly mixing the two solutions at 20-60 ℃, continuously stirring the mixed solution, adding a cross-linking agent into the mixed solution at 20-60 ℃, continuously stirring the mixed solution by adopting a mechanical stirring mode, wherein the stirring speed is 50-150 r/min, and the continuous stirring time is 30-120 min, so that cross-linking occurs between hydroxyl groups of amylose and phenolic hydroxyl groups of tea polyphenol, a cross-linked product with a network structure is formed, and a base material is obtained. The temperature of the prepared solution and the temperature of the generated crosslinking reaction need to be lower than the gelatinization temperature of the starch by 65 ℃, the solvent is distilled water, and the crosslinking agent is any one of glutaraldehyde, trimethylolpropane, pentaerythritol, epichlorohydrin, 1, 3-dichloro-dipropanol and acrylic acid.
A2, adding the composite fatty acid ester into the cross-linked product prepared in the step A1 at 20-50 ℃, adding the composite fatty acid ester into the cross-linked product several times, wherein the adding process is accompanied by continuous stirring, the stirring speed is 30-100 r/min, the continuous stirring time is 20-80 min, the composite fatty acid ester can react with amylose, the amylose is subjected to the action of intramolecular hydrogen bonds to form a d-spiral structure, fatty acid chains in the composite fatty acid ester enter an alpha-spiral structure of the amylose and are directionally arranged in a spiral body to form a stable compound, the compound of the amylose and the composite fatty acid ester is formed, a more compact grid structure base material is formed, the mixture solution is kept stand for 2-5 hours, and then free water on the upper layer in the mixture solution is separated, so that the composite base material is obtained.
A3, adding the hydrophobic fatty acid ester into the composite base material prepared in the step A2, carrying out ultrasonic oscillation treatment to disperse the mixture uniformly, carrying out ultrasonic treatment for 10-30 min at a treatment power of 300-600W, and enabling the hydrophobic fatty acid ester to enter cross-linked grid pores of the composite base material in an ultrasonic oscillation mode to fill the pores to form a more compact grid structure material, so that the water resistance is further improved, and a part of the hydrophobic fatty acid ester can be compounded with amylose to form a stable grid structure.
A4, compounding the antibacterial waterproof material prepared in the step A3 with the degradable material, and preparing the antibacterial waterproof material by a tape casting method or a screw extrusion method, wherein the screw extrusion temperature is 70-120 ℃. The antibacterial water-resistant material disclosed by the invention has an antibacterial effect, the amylose and the tea polyphenol are crosslinked to form a net-shaped structure material, the composite fatty acid ester is compounded with a crosslinking product to form a more compact net-shaped structure material, and then the hydrophobic fatty acid ester is filled into pores of a grid structure, so that the net-shaped structure material is more compact and can be well resistant to water; meanwhile, the hydrophobic fatty acid ester fills the pores of the composite matrix material to form a compact grid structure material, and the hydrophobic fatty acid ester also has a hydrophobic function, so that the water resistance of the material is greatly improved.
The invention will be further illustrated with reference to the following examples.
Examples
1. The antibacterial waterproof material is prepared according to the formula and the method, the specific proportion is shown in the following table 1, and all groups in the table 1 are carried out according to the following operation parameters: after the cross-linking agent is added, the cross-linking reaction temperature is 50 ℃, the stirring speed is 120r/min, and the stirring time is 40 min; after the fatty acid ester for compounding is added, the compounding reaction temperature is 50 ℃, the stirring speed is 80r/min, and the stirring time is 50 min; after the hydrophobic fatty acid ester is added, the ultrasonic oscillation time is 20min, and the treatment power is 500W; after the composite of PBAT and gelatin was added, the film material was extruded at 100 ℃ with a screw extruder.
TABLE 1 respective group ratio (parts by weight)
2. The antibacterial waterproof materials prepared from the above groups are made into films and then are subjected to antibacterial tests, staphylococcus aureus is selected for antibacterial tests, and the results are shown in the following table 2.
TABLE 2 results of antibacterial tests (% inhibition)
| Group of | 1h | 5h | 10h | 15h |
| 1 | 78.0 | 86.5 | 88.9 | 91.3 |
| 2 | 73.2 | 81.9 | 84.6 | 87.0 |
| 3 | 77.3 | 85.4 | 87.9 | 89.5 |
3. The antibacterial waterproof materials prepared from the above groups are made into films, and then subjected to a water resistance test, and the three groups of materials are immersed in water at 30 ℃, and the results are shown in table 3 below.
TABLE 3 Water resistance test results (% Water absorption)
| Group of | 1h | 5h | 10h | 15h |
| 1 | 0.1 | 3.5 | 4.7 | 6.1 |
| 2 | 0.1 | 3.1 | 4.0 | 5.3 |
| 3 | 0.3 | 5.1 | 6.9 | 8.6 |
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various changes, modifications, alterations, and substitutions which may be made by those skilled in the art without departing from the spirit of the present invention shall fall within the protection scope defined by the claims of the present invention.
Claims (10)
1. A bacteriostatic water-resistant material is characterized in that: the tea polyphenol composition comprises, by weight, 15-40 parts of amylose, 15-30 parts of tea polyphenol, and 5-15 parts of composite fatty acid ester and hydrophobic fatty acid ester in total.
2. The bacteriostatic water-resistant material according to claim 1, which is characterized in that: the composite material further comprises 3-10 parts of degradable composite material, wherein the composite material comprises one or more of PLA, PBAT, gelatin and chitosan.
3. The bacteriostatic water-resistant material according to claim 1, which is characterized in that: the mass ratio of the composite fatty acid ester to the hydrophobic fatty acid ester is 1-5: 1-8.
4. The bacteriostatic water-resistant material according to claim 1, which is characterized in that: the complex index ACI of the composite fatty acid ester is more than 50, and the composite fatty acid ester comprises one or more of glyceryl monostearate, stearoyl lactate, sodium stearoyl lactylate and calcium stearoyl lactylate.
5. The bacteriostatic water-resistant material according to claim 1, which is characterized in that: the water oil degree HLB of the hydrophobic fatty acid ester is lower than 5, and the hydrophobic fatty acid ester comprises one or more of medium-carbon chain polyglycerol fatty acid ester, sucrose glycerol fatty acid ester, soybean phospholipid, glycerol monostearate and propylene glycol ester.
6. A preparation method of a bacteriostatic water-resistant material is characterized by comprising the following steps: the method comprises the following steps:
a1, preparing an amylose and tea polyphenol solution which are uniformly mixed, adding a cross-linking agent at the temperature of 20-60 ℃, and continuously stirring the mixed solution to prepare a cross-linked product of the amylose and the tea polyphenol, thereby obtaining a base material;
a2, adding the fatty acid ester for compounding into the cross-linked product prepared in the step A1 at the temperature of 20-50 ℃, stirring continuously in the whole process to form a compound of amylose and the fatty acid ester for compounding, standing the mixture solution for 2-5 hours, and separating the upper-layer free water in the mixed solution to obtain a composite base material;
a3, adding the hydrophobic fatty acid ester into the composite base material prepared in the step A2, and after the hydrophobic fatty acid ester is subjected to ultrasonic treatment and is dispersed uniformly, enabling the hydrophobic fatty acid ester to enter cross-linked grid pores of the composite base material, so as to obtain the antibacterial waterproof material.
7. The preparation method of the bacteriostatic water-resistant material according to claim 6, characterized in that: and A4, compounding the antibacterial waterproof material prepared in the step A3 with the degradable material, and then preparing the antibacterial waterproof material by a tape casting method or a screw extrusion method.
8. The preparation method of the bacteriostatic water-resistant material according to claim 6, characterized in that: the cross-linking agent in the step A1 comprises any one of glutaraldehyde, trimethylolpropane, pentaerythritol, epichlorohydrin, 1, 3-dichloro-dipropanol and acrylic acid.
9. The preparation method of the bacteriostatic water-resistant material according to claim 6, characterized in that: and in the step A1, mechanical stirring is adopted, the stirring speed is 50-150 r/min, and the continuous stirring time is 30-120 min.
10. The preparation method of the bacteriostatic water-resistant material according to claim 6, characterized in that: in the step A3, the ultrasonic treatment time is 10-30 min, and the treatment power is 300-600W.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113842370A (en) * | 2021-11-01 | 2021-12-28 | 石家庄四药有限公司 | Arbidol hydrochloride tablet and preparation method thereof |
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