CN111057289A - LDPE/corn starch/TiO2Antibacterial composite membrane and preparation method thereof - Google Patents
LDPE/corn starch/TiO2Antibacterial composite membrane and preparation method thereof Download PDFInfo
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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
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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
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
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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
- C08J2403/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2403/02—Starch; Degradation products thereof, e.g. dextrin
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- 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
- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2471/02—Polyalkylene oxides
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- 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
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
Abstract
The invention relates to the technical field of composite membranes, in particular to LDPE (Low-Density polyethylene)/corn starch/TiO (TiO)2An antibacterial composite film and a preparation method thereof. The antibacterial composite membrane comprises the following raw materials: 90-120 parts of LDPE, 10-30 parts of corn starch and modified nano TiO in mass ratio22-10 parts of glycerol, 3-15 parts of glycerol and 5-20 parts of polyethylene glycol. Method for preparing composite filmCarrying out banburying on rice starch, glycerol and polyethylene glycol to prepare thermoplastic starch; LDPE is taken as matrix resin, thermoplastic starch and modified nano TiO are added2Banburying to prepare LDPE/corn starch/TiO2A composite material; the LDPE/corn starch/TiO is obtained by crushing and extrusion blow molding2An antibacterial composite film. The invention improves the dispersion effect of starch and various modifiers in an LDPE matrix by controlling the process, improves the mechanical property and the antibacterial property of the polymer film, and endows LDPE/corn starch/TiO with the LDPE/corn starch/TiO2The light-biodegradable function and the antibacterial function of the composite film.
Description
The technical field is as follows:
the invention relates to the technical field of composite membranes, in particular to LDPE (Low-Density polyethylene)/corn starch/TiO (TiO)2An antibacterial composite film and a preparation method thereof.
Background art:
the starch is a green renewable biodegradable substance, has good film forming property, transparency, edibility, safety, excellent biocompatibility and chemical stability, wide source and low price. The excellent biodegradability of starch is acknowledged, and the final decomposition product is CO2And H2O, is a good environment-friendly material without environmental pollution. Starch has been used in various fields, particularly in the preservation of food products. Starch biodegradable plastics are divided into two types: one is a filling type degradable plastic with the starch content of 7-30 percent, and the other is a complete type degradable plastic with the starch content of more than 90 percent. Among them, starch-completely degradable plastics are one of the most ideal biodegradable materials, but starch contains a large amount of hydroxyl groups, has high crystallinity and strong water absorption capacity, and limits the application of replacing petroleum-based materials. Therefore, the research on starch-filled degradable plastics is still a hot topic. At present, the preparation of starch composite films by adopting an extrusion blow molding process flow is rare, and the problem exists that the preparation of starch films by adopting the extrusion blow molding process has the limitation of process conditions, namely, precipitationThe melting temperature of the powder is higher than the decomposition temperature, and the starch is not easy to be modified for forming. Therefore, a plasticizer or a stabilizer with a certain proportion is required to be added to be mixed with a starch matrix to form a complex to replace the hydrogen bond action between starch molecules or in the starch molecules, so that the aggregation state structure of the starch is controlled, the crystallinity of the starch is reduced, and finally film blowing is realized.
Currently, for the preparation of antibacterial polymer films, the majority of matrix resins are single LDPE or LLDPE; there is a problem in that the selection of a matrix resin, the degradability of the film, the toxicity of the antibacterial agent, and the dispersibility of the antibacterial agent in the polymer matrix need to be considered, thereby preparing a multifunctional and excellent-performance polymer film.
The invention content is as follows:
the purpose of the invention is as follows:
the invention aims to provide LDPE (low-density polyethylene)/corn starch/TiO (TiO)2The antibacterial composite film and its preparation process solve the technological problems of plasticizing corn starch to reduce its crystallinity, avoiding its decomposition in forming process and adding modified nanometer TiO2And (4) modifying the antibacterial agent. The dispersion effect of starch and various modifiers in an LDPE matrix is improved by controlling the process, the mechanical property and the antibacterial property of the polymer film are improved, and LDPE/corn starch/TiO is endowed with2The light-biodegradable function and the antibacterial function of the composite film.
The technical scheme is as follows:
LDPE/corn starch/TiO2Antibiotic complex film, antibiotic complex film raw materials include: according to the mass ratio, the LDPE90-120 parts, the corn starch 10-30 parts and the modified nano TiO22-10 parts of glycerol, 3-15 parts of glycerol and 5-20 parts of polyethylene glycol.
Further, modified nano TiO2Is made of nano TiO2And silane coupling agent.
Further, the mass of the silane coupling agent is TiO21-5% of the total amount of the active carbon, and adopting an ultrasonic modification method.
Further, a packaging film having LDPE designation 2426K.
LDPE/corn starch/TiO2AntibacterialThe preparation method of the composite membrane specifically comprises the following steps:
the method comprises the following steps: banburying rice starch, glycerol and polyethylene glycol to obtain thermoplastic starch;
step two: LDPE is taken as matrix resin, thermoplastic starch and modified nano TiO are added2Banburying to prepare LDPE/corn starch/TiO2A composite material;
step three: the LDPE/corn starch/TiO is obtained by crushing and extrusion blow molding2An antibacterial composite film.
Further, thermoplastic starch is prepared as follows: premixing the dried corn starch, glycerol and polyethylene glycol for 5-10min, and blending in an internal mixer to obtain the thermoplastic starch.
Further, the mixing time of the second banburying step is 5-30 min, and the forming temperature is 140-160 ℃.
Further, the corn starch is placed in an electric heating air blast drying oven, dried for 12 hours at the temperature of 80 ℃ and taken out for standby application, and the dried corn starch is obtained.
Furthermore, the process temperature is 150-170 ℃ and the die head temperature is 160 ℃ during blow molding.
The advantages and effects are as follows:
the invention provides LDPE/corn starch/TiO2The antibacterial composite membrane and the preparation method thereof have the following advantages:
1. because the corn starch is a natural polymer, the crystallinity of the corn starch is reduced by adopting glycerol and polyethylene glycol as plasticizers, and the decomposition of the corn starch before melting is avoided by controlling the process, so that the LDPE and the corn starch can be processed by melt molding.
2. Nano TiO22The modified LDPE/corn starch composite film is well dispersed in a LDPE/corn starch matrix, so that the antibacterial property and the photodegradation property of the LDPE/corn starch composite film are improved. Modified nano TiO2Can catalyze the degradation rate of a polymer film under the irradiation of ultraviolet light, and can modify nano TiO under the illumination condition2The electrons in the middle valence band are excited and jump to the conduction band to form' electrons-Hole' structure, with H2O and O2Oxidation-reduction reaction is carried out to generate OH and O2-Thereby playing a role of killing bacteria and having no harm to human body due to the antibacterial capacity.
3. The matrix resin of the invention adopts blending of LDPE and corn starch, has the advantages of tensile resistance, penetration resistance, impact resistance and excellent environmental stress cracking resistance which are slightly lower than those of a single LDPE film, and can not influence the application effect.
Description of the drawings:
FIG. 1 is LDPE/corn starch/TiO2DSC melting curve diagram of the antibacterial composite film.
FIG. 2 is LDPE/corn starch/TiO2DSC crystallization curve chart of the antibacterial composite membrane.
FIG. 3 is an infrared spectrum before and after photodegradation of an LDPE/corn starch/TiO 2 antibacterial composite membrane.
FIG. 4 is LDPE/corn starch/TiO2The light degradation diagram of the antibacterial composite film.
The specific implementation mode is as follows:
the invention is further described below with reference to the accompanying drawings:
the Low Density Polyethylene (LDPE) used in the embodiment of the invention is a product number of 2426K of China oil and gas Limited.
Example 1
In this example LDPE/corn starch/TiO2The antibacterial composite film is prepared by using LDPE as matrix, corn starch and TiO2Polyethylene glycol and glycerol are used as modifiers, and the modifier is obtained by firstly mixing through an internal mixer, then crushing, and then carrying out extrusion blow molding.
(1) Mixing nanometer titanium dioxide with anhydrous ethanol solvent, adjusting pH to about 9 with hydrochloric acid and sodium hydroxide, stirring in magnetic stirrer (KH-50A) for 20min, and ultrasonically dispersing for 30min to obtain nanometer titanium dioxide dispersion. Mixing a silane coupling agent with deionized water, adding an absolute ethyl alcohol solvent, and heating and mixing in a water bath at the temperature of 75-85 ℃ for 5min to obtain a silane coupling agent aqueous solution. Mixing the raw materials, pouring the mixture into a reaction device, stirring and boiling the mixture for 3 hours at the temperature of 75-85 ℃, then carrying out vacuum filtration, and drying the product in a vacuum drying oven at the temperature of 85 DEG CGrinding after drying for 24h to obtain the modified nano TiO2。
(2) Firstly, placing corn starch in an electric heating forced air drying oven, drying for 12h at 80 ℃, and taking out for later use. Then premixing the corn starch, glycerol and polyethylene glycol, and finally blending in an internal mixer (SU-70C) for 10min to obtain the thermoplastic starch.
(3) Modified nano TiO obtained in the step (1)22-10 parts of LDPE and 100 parts of thermoplastic starch. Adding the mixture into a high-speed mixer, mixing for 30 minutes, standing for 24 hours, and preparing the nano modified composite master batch by using an internal mixer, wherein the molding temperature of the internal mixer is 140-160 ℃.
(4) Blow molding the LDPE obtained in the step (2) as the matrix nano modified composite master batch by adopting an extrusion film blowing system to obtain LDPE/corn starch/TiO2An antibacterial composite film. When blow molding, the process temperature is 150-170 ℃, and the die head temperature is 160 ℃.
FIG. 1 is a melting curve of Differential Scanning Calorimetry (DSC), FIG. 2 is a DSC crystallization curve, and it can be seen from FIGS. 1 and 2 that after starch is plasticized by glycerol and polyethylene glycol, the melting temperature (Tm) of the mixed system is 107.35-108.28 ℃, the crystallization temperature (Tc) of the composite film is 91.15-91.79 ℃, the temperature change is not great, and only one melting peak and crystallization peak are provided, which indicates that the modified nano-TiO compound film has a modified nano-TiO2And TPS compatibility number with matrix LDPE, and is dispersed uniformly in the LDPE matrix.
3394cm in FIG. 3-1Is starch and nano-TiO2Forming characteristic peak related to hydrogen bond of 1250cm-1Is C-O-H bending vibration peak 1104cm in starch-1Is the C-O bond stretching vibration in C-O-H, 946cm-1Is the skeleton vibration of starch with asymmetric environment formula (α -1,4 glycosidic bond (C-O-C)), No. 4 film is irradiated by sunlight for 8 days, and is 3394cm-1And 1104cm-1The absorption peak is reduced at 1740cm-1A characteristic peak of C ═ O appears nearby. Indicating that the LDPE undergoes oxidative degradation and a small proportion of the starch is decomposed. Microcracks are generated in the film, the contact between LDPE molecular chains and air is increased, and the degradation of LDPE is accelerated.
As can be seen from fig. 4, the left side is a pure LDPE film, which is relatively smooth; on the right side is LDPE/corn starch/TiO2The antibacterial composite film can be obviously observed to have a plurality of micropores with different sizes on the surface after being subjected to light degradation for 60 days. Thus, it can be stated that LDPE/corn starch/TiO is prepared2The antibacterial composite film has photodegradable capability.
Example 2
The raw materials of the embodiment are as follows by mass ratio: 90 parts of LDPE (Low-Density polyethylene), 20 parts of corn starch and modified nano TiO210 parts, 6 parts of glycerol and 20 parts of polyethylene glycol.
(1) Mixing nanometer titanium dioxide with anhydrous ethanol solvent, adjusting pH to about 9 with hydrochloric acid and sodium hydroxide, stirring in magnetic stirrer (KH-50A) for 30min, and ultrasonically dispersing for 20min to obtain nanometer titanium dioxide dispersion. Mixing a silane coupling agent with the mass of 1% of titanium dioxide with deionized water, adding an absolute ethyl alcohol solvent, and heating and mixing in a water bath at the temperature of 75-85 ℃ for 5-10min to obtain a silane coupling agent aqueous solution. Mixing the raw materials, pouring the mixture into a reaction device, stirring and boiling the mixture at 75-85 ℃ for 3h, then carrying out vacuum filtration, drying the product in a vacuum drying oven at 85 ℃ for 24h, and then grinding to obtain the modified nano TiO2。
(2) Firstly, placing corn starch in an electric heating forced air drying oven, drying for 12h at 80 ℃, and taking out for later use. Then 20 parts of the corn starch to be prepared, 6 parts of glycerin and 20 parts of polyethylene glycol are premixed, and finally are mixed in an internal mixer (SU-70C) for 30min to obtain the thermoplastic starch.
(3) Modified nano TiO obtained in the step (1)210 parts of LDPE and 90 parts of the thermoplastic starch obtained in the step (2) are added into a high-speed mixer to be mixed for 30 minutes and then are kept stand for 24 hours, and then the mixture is prepared into the nano modified composite master batch through a mixer, wherein the forming temperature of the mixer is 140 ℃.
(4) Blow molding the LDPE obtained in the step (2) as the matrix nano modified composite master batch by adopting an extrusion film blowing system to obtain LDPE/corn starch/TiO2An antibacterial composite film. When blow molding is carried out, the process temperature is 150 ℃ and the die head temperature is 160 ℃.
Example 3
The raw materials of the embodiment are as follows by mass ratio: 120 parts of LDPE, 30 parts of corn starch and modified nano TiO28 parts, 15 parts of glycerol and 5 parts of polyethylene glycol.
(1) Mixing nanometer titanium dioxide with anhydrous ethanol solvent, adjusting pH to about 9 with hydrochloric acid and sodium hydroxide, stirring in magnetic stirrer (KH-50A) for 30min, and ultrasonically dispersing for 20min to obtain nanometer titanium dioxide dispersion. Mixing a silane coupling agent with the mass of 5% of titanium dioxide with deionized water, adding an absolute ethyl alcohol solvent, and heating and mixing in a water bath at the temperature of 75-85 ℃ for 5-10min to obtain a silane coupling agent aqueous solution. Mixing the raw materials, pouring the mixture into a reaction device, stirring and boiling the mixture at 75-85 ℃ for 3h, then carrying out vacuum filtration, drying the product in a vacuum drying oven at 85 ℃ for 24h, and then grinding to obtain the modified nano TiO2。
(2) Firstly, placing corn starch in an electric heating forced air drying oven, drying for 12h at 80 ℃, and taking out for later use. Then premixing 30 parts of corn starch for later use with 15 parts of glycerin and 5 parts of polyethylene glycol, and finally blending in an internal mixer (SU-70C) for 5min to obtain the thermoplastic starch.
(3) Modified nano TiO obtained in the step (1)2And (3) adding 8 parts of LDPE (low-density polyethylene) and 120 parts of the thermoplastic starch obtained in the step (2) into a high-speed mixer, mixing for 30 minutes, standing for 24 hours, and preparing the nano modified composite master batch by using an internal mixer, wherein the molding temperature of the internal mixer is 160 ℃.
(4) Blow molding the LDPE obtained in the step (2) as the matrix nano modified composite master batch by adopting an extrusion film blowing system to obtain LDPE/corn starch/TiO2An antibacterial composite film. In the blow molding process, the process temperature is 170 ℃ and the die head temperature is 160 ℃.
Example 4
The raw materials of the embodiment are as follows by mass ratio: 100 parts of LDPE, 20 parts of corn starch and modified nano TiO210 parts, 12 parts of glycerol and 12 parts of polyethylene glycol.
(1) Mixing nanometer titanium dioxide with anhydrous ethanol solvent, adjusting pH to about 9 with hydrochloric acid and sodium hydroxide, stirring in magnetic stirrer (KH-50A) for 30min, and ultrasonically dispersing for 20miAnd n, preparing the nano titanium dioxide dispersion liquid. Mixing a silane coupling agent with the mass of 2.5% of titanium dioxide with deionized water, adding an absolute ethyl alcohol solvent, and heating and mixing in a water bath at the temperature of 75-85 ℃ for 5-10min to obtain a silane coupling agent aqueous solution. Mixing the raw materials, pouring the mixture into a reaction device, stirring and boiling the mixture at 75-85 ℃ for 3h, then carrying out vacuum filtration, drying the product in a vacuum drying oven at 85 ℃ for 24h, and then grinding to obtain the modified nano TiO2。
(2) Firstly, placing corn starch in an electric heating forced air drying oven, drying for 12h at 80 ℃, and taking out for later use. Then 20 parts of the corn starch to be prepared, 12 parts of glycerin and 12 parts of polyethylene glycol are premixed, and finally are mixed in an internal mixer (SU-70C) for 10min to obtain the thermoplastic starch.
(3) Modified nano TiO obtained in the step (1)210 parts of LDPE and 100 parts of the thermoplastic starch obtained in the step (2) are added into a high-speed mixer to be mixed for 30 minutes and then are kept stand for 24 hours, and then the mixture is prepared into the nano modified composite master batch through a mixer, wherein the forming temperature of the mixer is 150 ℃.
(4) Blow molding the LDPE obtained in the step (2) as the matrix nano modified composite master batch by adopting an extrusion film blowing system to obtain LDPE/corn starch/TiO2An antibacterial composite film. In the blow molding process, the process temperature is 160 ℃ and the die head temperature is 160 ℃.
Claims (9)
- LDPE/corn starch/TiO 12Antibiotic complex film, its characterized in that: the antibacterial composite membrane comprises the following raw materials:90-120 parts of LDPE, 10-30 parts of corn starch and modified nano TiO in mass ratio22-10 parts of glycerol, 3-15 parts of glycerol and 5-20 parts of polyethylene glycol.
- 2. LDPE/corn starch/TiO according to claim 12Antibiotic complex film, its characterized in that: modified nano TiO2Is made of nano TiO2And silane coupling agent.
- 3. LDPE/corn starch/TiO according to claim 22Antibiotic complex film, its characterized in that: the mass of the silane coupling agent is TiO21-5% of the total amount of the active carbon, and adopting an ultrasonic modification method.
- 4. LDPE/corn starch/TiO according to claim 12Antibiotic complex film, its characterized in that: LDPE No. 2426K.
- 5. LDPE/corn starch/TiO according to any of claims 1 to 42The preparation method of the antibacterial composite membrane is characterized by comprising the following steps: the preparation method specifically comprises the following steps:the method comprises the following steps: banburying rice starch, glycerol and polyethylene glycol to obtain thermoplastic starch;step two: LDPE is taken as matrix resin, thermoplastic starch and modified nano TiO are added2Banburying to prepare LDPE/corn starch/TiO2A composite material;step three: the LDPE/corn starch/TiO is obtained by crushing and extrusion blow molding2An antibacterial composite film.
- 6. LDPE/corn starch/TiO according to claim 52The preparation method of the antibacterial composite membrane is characterized by comprising the following steps: the thermoplastic starch was prepared as follows: premixing the dried corn starch, glycerol and polyethylene glycol for 5-10min, and blending in an internal mixer to obtain the thermoplastic starch.
- 7. LDPE/corn starch/TiO according to claim 62The preparation method of the antibacterial composite membrane is characterized by comprising the following steps: and the mixing time of the second banburying step is 5-30 min, and the forming temperature is 140-160 ℃.
- 8. LDPE/corn starch/TiO according to claim 52The preparation method of the antibacterial composite membrane is characterized by comprising the following steps: placing the corn starch in an electric heating forced air drying oven, drying for 12h at 80 ℃, and taking out for later use to obtain dried corn starch.
- 9. LDPE/corn starch/TiO according to claim 52The preparation method of the antibacterial composite membrane is characterized by comprising the following steps: when blow molding, the process temperature is 150-170 ℃, and the die head temperature is 160 ℃.
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| CN112898665A (en) * | 2021-01-25 | 2021-06-04 | 孙牡花 | Environment-friendly composite plastic film and preparation method thereof |
| CN113121969A (en) * | 2021-04-15 | 2021-07-16 | 天津科技大学 | Degradable antibacterial plastic sheet and preparation |
| CN117141077A (en) * | 2023-11-01 | 2023-12-01 | 南通金丝楠膜材料有限公司 | Barrier type polyethylene single-material composite antibacterial film and preparation method thereof |
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Application publication date: 20200424 |
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