CN111961263A - Preparation method of antibacterial degradable food packaging film material - Google Patents
Preparation method of antibacterial degradable food packaging film material Download PDFInfo
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- CN111961263A CN111961263A CN202010886856.9A CN202010886856A CN111961263A CN 111961263 A CN111961263 A CN 111961263A CN 202010886856 A CN202010886856 A CN 202010886856A CN 111961263 A CN111961263 A CN 111961263A
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- food packaging
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- packaging film
- degradable food
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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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D65/00—Wrappers or flexible covers; Packaging materials of special type or form
- B65D65/38—Packaging materials of special type or form
- B65D65/46—Applications of disintegrable, dissolvable or edible materials
- B65D65/466—Bio- or photodegradable packaging materials
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives 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
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
- C08J2305/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives 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
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/08—Cellulose derivatives
- C08J2401/26—Cellulose ethers
- C08J2401/28—Alkyl ethers
-
- 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
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/04—Alginic acid; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
Abstract
The invention relates to the technical field of food packaging material preparation, and aims to solve the problem that the current food packaging film is easy to cause environmental pollution. The food packaging film has good tensile property and excellent antibacterial property, is beneficial to storage of food, and has certain practical application value.
Description
Technical Field
The invention belongs to the technical field of food packaging material preparation, and particularly relates to a preparation method of an antibacterial degradable food packaging film material.
Background
The current plastic packaging material is widely applied to food packaging and fresh keeping due to low price and stable property. However, these plastic packages are difficult to degrade and easily cause "white pollution" after being discarded, which poses a serious threat to the environment. The degradable packaging film is adopted to replace plastic packaging, so that the influence on the contents and the pollution to the environment are reduced, the more excellent comprehensive performance is exerted, and the degradable packaging film becomes a new trend for the development of the food industry and the packaging field.
The biomass material has wide application prospect in the field of food due to the nature, safety and degradability of the biomass material and the fact that people pursue green and healthy concepts. Meanwhile, the application of natural antibacterial materials in food packaging films is increasing. Tea polyphenols are phenolic compounds extracted from tea leaves, and have been widely used in foods because of their natural safety and good bacteriostatic and antioxidant activities. It can prolong shelf life, prevent food from fading, maintain food quality and effectively protect various nutritional components; in addition, the compound antibacterial material is easy to dissolve in water, so that the taste of food is not influenced, and the compound antibacterial material can play a better antibacterial effect after being compounded with other materials, so that the preparation of the compound antibacterial material by using the tea polyphenol becomes a research hotspot. Therefore, there is a great need for the development of antibacterial and degradable composite food packaging materials which are prepared by compounding natural biomass as a green raw material with a natural antibacterial material, namely tea polyphenol.
Disclosure of Invention
The invention provides a preparation method of an antibacterial degradable food packaging film material, aiming at solving the problem that the current food packaging film is easy to cause environmental pollution. The green biomass material is used as a raw material, and the packaging film is endowed with good tensile property and antibacterial property through the graft modification of the antibacterial substance, is beneficial to the storage of food, and has a certain practical application value.
The invention is realized by the following technical scheme:
a preparation method of an antibacterial degradable food packaging film material comprises the following steps:
(1) preparation of carboxylated chitosan (CMCS)
And (3) swelling chitosan in NaOH-isopropanol solution, and activating with alkali at 40-50 ℃ for 1-2 h. Then dropwise adding chloroacetic acid-isopropanol solution, and stirring and reacting for 4-6 h at 40-50 ℃. And then placing the precipitate into an ethanol solution for soaking for 0.5-1 h, adjusting the pH value to be neutral by hydrochloric acid, washing the product by absolute ethyl alcohol, and performing vacuum filtration and drying. The product carboxylated chitosan (CMCS) is obtained.
The specific preparation route is as follows:
the mass ratio of the chitosan to the NaOH to the chloroacetic acid is 1: 1.1-1.3: 1.4 to 1.6.
The mass fraction of the isopropanol solution is 85-90%.
The mass fraction of the ethanol solution is 75-85%.
Preferably, the temperature for vacuum drying is 50-70 ℃.
(2) Preparation of tea polyphenol grafted chitosan complex (TP/CS)
Dissolving the carboxylated chitosan CMCS prepared in the step (1) in an acetic acid solution, and stirring and dissolving at room temperature; and then weighing tea polyphenol TP, dissolving in water, quickly adding into the solution, mechanically stirring at 80-90 ℃ for reaction for 10-12 h, and cooling to room temperature to obtain the tea polyphenol grafted chitosan solution.
The specific preparation route is as follows:
the mass ratio of the carboxylated chitosan CMCS to the tea polyphenol TP is 1: 0.25 to 3.
The mass fraction of the acetic acid solution is 1-3%.
(3) Preparation of antibacterial degradable food packaging film
Adding sodium alginate, carboxymethyl cellulose and glycerol into the tea polyphenol grafted chitosan solution obtained in the step (2), stirring and blending for 1-2 h, degassing and standing to obtain a molding slurry; and then carrying out tape casting, drying and film uncovering on the slurry to obtain the antibacterial degradable food packaging film.
The mass ratio of the sodium alginate to the carboxymethyl cellulose to the glycerol to the carboxylated chitosan CMCS is (0.5-1): 0.2-1.0: 1-2: 5 to 20.
The vacuum degree in the degassing process is not lower than-0.090 MPa.
The casting process comprises the following steps: and pouring the formed slurry onto a dry and clean glass dish of 25cm multiplied by 25cm for casting to form a film, and controlling the thickness of the slurry to be 0.2-0.4 cm.
The drying temperature is 50-60 ℃, and the drying time is 5-8 hours.
The invention provides a preparation method of an antibacterial biodegradable food packaging film material. Aiming at the problem that the food packaging plastic film is easy to cause environmental pollution, the natural biomass chitosan is used as a substrate, and the tea polyphenol is introduced into the film material through graft modification, so that the film material has the advantages of simplicity and convenience in operation, excellent antibacterial performance, biodegradability and environmental friendliness, and has a good development prospect in the aspect of food packaging.
Compared with the prior art, the invention has the beneficial effects that:
1. the packaging film obtained by the invention has excellent tensile property;
2. the raw materials of the invention are green biomass, which can be biologically degraded and does not pollute the environment;
3. the invention has good antibacterial property, and is beneficial to the storage of food;
4. the preparation method is simple, does not need any harmful reagent, and is easy for large-scale production and application.
Detailed Description
The technical solution of the present invention is further described in detail with reference to the following embodiments:
example 1:
a preparation method of an antibacterial degradable food packaging film material comprises the following steps:
(1) preparation of carboxylated chitosan (CMCS)
5g of low molecular weight chitosan was swollen in 50ml of NaOH-isopropanol solution (6g of NaOH dissolved in 90% isopropanol) and alkali-activated at 40 ℃ for 1 h. A solution of 6.5g chloroacetic acid in isopropanol (10 mL) was added dropwise to the separatory funnel. Stirred at 40 ℃ for 4 h. And (3) soaking the precipitate in 200mL of ethanol (80%) for 0.5h, adjusting the pH value to 7.0 by using hydrochloric acid, washing the product by using absolute ethanol, carrying out vacuum filtration, and carrying out vacuum drying at 60 ℃ to obtain a product of carboxylated chitosan (CMCS).
(2) Preparation of tea polyphenol grafted chitosan complex (TP/CS)
Dissolving 1g of carboxylated chitosan CMCS prepared in the step (1) in 1% 100mL of acetic acid solution, and stirring and dissolving at room temperature; weighing 0.25g of tea polyphenol TP, dissolving in water, quickly adding into the solution, mechanically stirring at 80 ℃ for reaction for 10h, and cooling to room temperature to obtain the tea polyphenol grafted chitosan solution.
(3) Preparation of antibacterial degradable food packaging film
Adding 0.5g of sodium alginate, 1g of carboxymethyl cellulose and 0.5g of glycerol into the tea polyphenol grafted chitosan solution obtained in the step (2), stirring and blending for 2 hours, degassing at-0.090 MPa, and standing for 4 hours to obtain a molding slurry; and pouring the formed slurry onto a dry and clean glass dish of 25cm multiplied by 25cm for casting to form a film, and controlling the thickness of the slurry to be 0.2 cm. Drying at 50 deg.C for 5h, and removing the film to obtain antibacterial degradable food packaging film.
Example 2:
a preparation method of an antibacterial degradable food packaging film material comprises the following steps:
(1) preparation of carboxylated chitosan (CMCS)
10g of low molecular weight chitosan was swollen in 100ml of NaOH-isopropanol solution (13g of NaOH in 90% isopropanol) and alkali-activated at 45 ℃ for 1.5 h. An isopropyl alcohol (20mL) solution of 15g chloroacetic acid was added dropwise to the separatory funnel. Stirred at 40 ℃ for 4 h. And (3) soaking the precipitate in 200mL of ethanol (80%) for 0.5h, adjusting the pH value to 7.0 by using hydrochloric acid, washing the product by using absolute ethanol, carrying out vacuum filtration, and carrying out vacuum drying at 60 ℃ to obtain a product of carboxylated chitosan (CMCS).
(2) Preparation of tea polyphenol grafted chitosan complex (TP/CS)
Dissolving 5g of carboxylated chitosan CMCS prepared in the step (1) in 2% 100mL of acetic acid solution, and stirring and dissolving at room temperature; weighing 1.5g of tea polyphenol TP, dissolving in water, quickly adding into the solution, mechanically stirring at 80 ℃ for reaction for 10h, and cooling to room temperature to obtain the tea polyphenol grafted chitosan solution.
(3) Preparation of antibacterial degradable food packaging film
Adding 1g of sodium alginate, 1g of carboxymethyl cellulose and 1g of glycerol into the tea polyphenol grafted chitosan solution obtained in the step (2), stirring and blending for 2 hours, degassing at-0.090 MPa, and standing for 4 hours to obtain a molding slurry; and pouring the formed slurry onto a dry and clean glass dish of 25cm multiplied by 25cm for casting to form a film, wherein the thickness of the slurry is controlled to be 0.2 cm. Drying at 50 deg.C for 5h, and removing film to obtain antibacterial degradable food packaging film.
Example 3:
a preparation method of an antibacterial degradable food packaging film material comprises the following steps:
(1) preparation of carboxylated chitosan (CMCS)
1g of low molecular weight chitosan was swollen in 10ml of NaOH-isopropanol solution (1.4g NaOH dissolved in 90% isopropanol) and alkali-activated at 40 ℃ for 1 h. A solution of 1.5g chloroacetic acid in isopropanol (5mL) was added dropwise to the separatory funnel. Stirred at 40 ℃ for 4 h. And (3) soaking the precipitate in 50mL of ethanol (80%) for 0.5h, adjusting the pH value to 7.0 by hydrochloric acid, washing the product by absolute ethanol, carrying out vacuum filtration, and carrying out vacuum drying at 60 ℃ to obtain a product of carboxylated chitosan (CMCS).
(2) Preparation of tea polyphenol grafted chitosan complex (TP/CS)
Dissolving 1g of carboxylated chitosan CMCS prepared in the step (1) in 1% 100mL of acetic acid solution, and stirring and dissolving at room temperature; weighing 0.30g of tea polyphenol TP, dissolving in water, quickly adding into the solution, mechanically stirring at 80 ℃ for reaction for 10h, and cooling to room temperature to obtain the tea polyphenol grafted chitosan solution.
(3) Preparation of antibacterial degradable food packaging film
Adding 0.1g of sodium alginate, 0.1g of carboxymethyl cellulose and 0.15g of glycerol into the tea polyphenol grafted chitosan solution obtained in the step (2), stirring and blending for 2 hours, degassing at-0.090 MPa, and standing for 4 hours to obtain a molding slurry; and pouring the formed slurry onto a dry and clean glass dish of 25cm multiplied by 25cm for casting to form a film, and controlling the thickness of the slurry to be 0.2 cm. Drying at 50 deg.C for 5h, and removing the film to obtain antibacterial degradable food packaging film.
Test example 1:
and (3) testing the tensile property of the antibacterial degradable food packaging film.
Test samples: example-3 the antibacterial degradable food packaging film prepared in step (3).
The elongation at break of the antibacterial degradable food packaging films prepared in the step (3) of example 1, example 2 and example 3 were respectively tested, and the specific test results are shown in table 1.
Table 1 elongation at break test data table
Comparing the elongation at break of the antibacterial degradable food packaging films prepared in examples 1, 2 and 3, the result shows that the elongation at break of the antibacterial film is higher, and the packaging film is proved to have better tensile property and can be used for food packaging.
Test example 2:
and (3) testing the antibacterial performance of the antibacterial degradable food packaging film.
Test samples: the antibacterial degradable food packaging film prepared in step (3) of examples 1 to 3.
The food packaging films of examples 1-3 were each tested for their antimicrobial properties, as tested by reference to GB/T21510-2008, e.coli ATYCC25922, staphylococcus aureus ATCC 6538. The specific test results are shown in table 2.
TABLE 2 antibacterial Property test data sheet
As seen from the data in table 2, the antibacterial performance of the degradable food packaging film prepared in example 1 is optimal; the overall result shows that the antibacterial performance of the degradable food packaging film obtained by the preparation method is excellent and can reach 97.5 percent at most.
Claims (10)
1. The preparation method of the antibacterial degradable food packaging film material is characterized by comprising the following steps:
(1) preparation of carboxylated chitosan (CMCS)
Swelling chitosan in NaOH-isopropanol solution, activating with alkali at 40-50 ℃ for 1-2 h, then dropwise adding chloroacetic acid-isopropanol solution, stirring at 40-50 ℃ for reaction for 4-6 h, then soaking the precipitate in ethanol solution for 0.5-1 h, adjusting the pH value to be neutral with hydrochloric acid, washing the product with absolute ethanol, carrying out vacuum filtration, and drying to obtain a product of carboxylated chitosan (CMCS);
(2) preparation of tea polyphenol grafted chitosan complex (TP/CS)
Dissolving the carboxylated chitosan CMCS prepared in the step (1) in an acetic acid solution, and stirring and dissolving at room temperature; then weighing tea polyphenol TP, dissolving in water, quickly adding into the acetic acid solution of CMCS, mechanically stirring at 80-90 ℃ for reaction for 10-12 h, and cooling to room temperature to obtain a tea polyphenol grafted chitosan solution;
(3) preparation of antibacterial degradable food packaging film
Adding sodium alginate, carboxymethyl cellulose and glycerol into the tea polyphenol grafted chitosan solution obtained in the step (2), stirring and blending for 1-2 h, degassing and standing to obtain a molding slurry; and then carrying out tape casting, drying and film uncovering treatment on the molding slurry to obtain the antibacterial degradable food packaging film.
2. The preparation method of the antibacterial degradable food packaging film material according to claim 1, wherein the mass ratio of chitosan, NaOH and chloroacetic acid in the step (1) is 1: 1.1-1.3: 1.4 to 1.6.
3. The preparation method of the antibacterial degradable food packaging film material as claimed in claim 1, wherein the mass fraction of the isopropanol solution in the step (1) is 85-90%.
4. The preparation method of the antibacterial degradable food packaging film material as claimed in claim 1, wherein the mass fraction of the ethanol solution in step (1) is 75-85%.
5. The preparation method of the antibacterial degradable food packaging film material as claimed in claim 1, wherein the mass ratio of the carboxylated chitosan CMCS to the tea polyphenol TP in the step (2) is 1: 0.25 to 3.
6. The preparation method of the antibacterial degradable food packaging film material as claimed in claim 1, wherein the mass fraction of the acetic acid solution in the step (2) is 1-3%.
7. The preparation method of the antibacterial degradable food packaging film material as claimed in claim 1, wherein the mass ratio of sodium alginate, carboxymethyl cellulose, glycerol and carboxylated chitosan CMCS in step (3) is 0.5-1: 0.2-1.0: 1-2: 5 to 20.
8. The method for preparing antibacterial degradable food packaging film material as claimed in claim 1, wherein the vacuum degree in the degassing process in step (3) is not lower than-0.090 MPa.
9. The preparation method of the antibacterial degradable food packaging film material as claimed in claim 1, wherein the casting process in step (3) is: and pouring the formed slurry onto a dry and clean glass dish of 25cm multiplied by 25cm for casting to form a film, wherein the thickness of the slurry is controlled to be 0.2-0.4 cm.
10. The preparation method of the antibacterial degradable food packaging film material as claimed in claim 1, wherein the drying temperature in step (3) is 50-60 ℃ and the drying time is 5-8 h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010886856.9A CN111961263A (en) | 2020-08-28 | 2020-08-28 | Preparation method of antibacterial degradable food packaging film material |
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| CN202010886856.9A CN111961263A (en) | 2020-08-28 | 2020-08-28 | Preparation method of antibacterial degradable food packaging film material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112933289A (en) * | 2021-01-29 | 2021-06-11 | 赵春富 | Preparation method of sodium alginate grafted tea polyphenol antibacterial dressing |
| CN113831755A (en) * | 2021-10-09 | 2021-12-24 | 厦门市鹭益印刷包装有限公司 | High-temperature-resistant sealing packaging film and preparation method thereof |
| CN115124630A (en) * | 2021-02-08 | 2022-09-30 | 珠海市自然之旅生物技术有限公司 | Chitosan derivative and preparation method and application thereof |
-
2020
- 2020-08-28 CN CN202010886856.9A patent/CN111961263A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112933289A (en) * | 2021-01-29 | 2021-06-11 | 赵春富 | Preparation method of sodium alginate grafted tea polyphenol antibacterial dressing |
| CN115124630A (en) * | 2021-02-08 | 2022-09-30 | 珠海市自然之旅生物技术有限公司 | Chitosan derivative and preparation method and application thereof |
| CN115124630B (en) * | 2021-02-08 | 2024-02-23 | 珠海市自然之旅生物技术有限公司 | Chitosan derivative and preparation method and application thereof |
| CN113831755A (en) * | 2021-10-09 | 2021-12-24 | 厦门市鹭益印刷包装有限公司 | High-temperature-resistant sealing packaging film and preparation method thereof |
| CN113831755B (en) * | 2021-10-09 | 2022-08-30 | 厦门市鹭益印刷包装有限公司 | High-temperature-resistant sealing packaging film and preparation method thereof |
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