CN115044106A - Preparation method of anti-ultraviolet high-strength starch nano composite film - Google Patents
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Abstract
The invention discloses a preparation method of an uvioresistant high-strength starch nano composite film, belonging to the technical field of high-strength starch nano composite films, which comprises the following steps of (1) performing moist heat treatment on 10-33.3 parts of starch; 1 part of lignosulfonic acid nanoparticles and 4-13.3 parts of plasticizer; step two, preparing a moist heat treatment starch stock solution: and (2) mixing the moist heat treatment starch powder with distilled water according to the mass ratio of 1: 10-16.7, adding into distilled water, and mechanically stirring at 40-90 deg.C for 10-60min until completely dissolving to obtain wet heat treated starch stock solution; step three, preparing a damp and hot starch-lignosulfonic acid mixed solution; the breaking elongation and tensile strength of the starch-lignosulfonic acid nano composite film with the thickness of 30-50 mu m can respectively reach 140% and more than 54MPa (the breaking elongation and the tensile strength are respectively improved by 152% and 1642% compared with a pure starch film), and the nano composite film has excellent ultraviolet resistance and can fully meet the application of food packaging films.
Description
Technical Field
The invention relates to the technical field of high-strength starch nano composite films, in particular to a preparation method of an anti-ultraviolet high-strength starch nano composite film.
Background
The current overuse of petroleum-based packaging and the diminishing petroleum resources have led to an increased interest in natural high molecular weight polymers.
Starch is a natural high molecular compound with low price, easy acquisition, biodegradability and good biocompatibility. Among them, starch-based food packaging films are considered to be one of the most promising "green packaging materials". However, due to the limitation of the properties of the starch material, the prepared pure starch food packaging film often has the defects of low mechanical property, poor hydrophobic property, lack of activity (such as necessary oxidation resistance and antibacterial activity), and the like.
The wet-heat treatment of the starch refers to that the starch is treated for a certain time (15 min-6 h) under the conditions of low moisture content (10% -30%) and high temperature (90-130 ℃), namely the structure and the physical and chemical properties of the starch are changed through the combined action of water molecules and heat, so that the application properties of the starch are influenced, and the wet-heat treatment method has the advantages of simple process, energy conservation, environmental protection, rapidness, safety and the like, and is a green, environment-friendly and efficient physical modification technology.
The Lignosulfonic Acid (LA) is mainly derived from sodium lignosulfonate, which is a common byproduct in the sulfite pulping industry, and has the characteristics of low price, easy obtainment, no toxicity and environmental protection. LA molecules contain structures of benzene rings and phenylpropane with abundant hydrophobicity and hydroxyl groups and sulfonic groups with abundant hydrophilicity, and due to special amphipathy, after the lignosulfonic acid molecules are dispersed in an aqueous solution, the lignosulfonic acid molecules can be self-assembled to form nanoparticles with 3D complex molecular structures. A large number of hydrophilic groups can form strong hydrogen bonds with starch molecules, so that amorphous starch molecules are dynamically restricted by sacrificing the hydrogen bonds, chain extension and regularity are promoted, and excellent reinforcing and toughening effects can be achieved. In addition, the polyphenol unit and a large number of chromophore structures in the LA molecule bring excellent uvioresistant performance to the composite membrane,
in the prior art, a great deal of research is carried out on the aspects of modifying starch, forming a composite film and the like by technicians in the field, and a series of modification modes such as chemical modification (esterification, etherification, grafting and crosslinking), physical modification (heat treatment, extrusion, ultrasonic radiation), biological modification (enzyme) and the like are carried out on the aspects of improving the performance of a starch film, improving the preparation process of a starch film and the like. These modification methods have problems of high modification cost and complex process. The starch film is modified by combining simple damp-heat physical treatment and green biomass nanoparticle compounding, a composite film with excellent mechanical property, ultraviolet resistance and hydrophobic property is obtained, and the preparation process has the characteristics of low cost, high efficiency and green.
Based on the above, the invention designs a preparation method of an anti-ultraviolet high-strength starch nano composite film, so as to solve the above problems.
Disclosure of Invention
The invention aims to provide a preparation method of an anti-ultraviolet high-strength starch nano composite film, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of an anti-ultraviolet high-strength starch nano composite film comprises the following steps:
firstly, preparing raw materials: 10-33.3 parts of moist heat treatment starch; 1 part of lignosulfonic acid nanoparticles and 4-13.3 parts of plasticizer;
step two, preparing a moist heat treatment starch stock solution: and (3) mixing the moist heat treatment starch powder with distilled water according to the mass ratio of 1: 10-16.7, adding into distilled water, and mechanically stirring at 40-90 deg.C for 10-60min until completely dissolving to obtain wet heat treated starch stock solution;
step three, preparing a moist heat starch-lignosulfonic acid mixed solution:
dropwise adding the lignosulfonic acid nano dispersion into the wet and hot starch stock solution under stirring of 500-800rmp, and stirring for 1-2h to obtain uniform wet and hot starch-lignosulfonic acid nano dispersion;
step four, adding a plasticizer:
and adding a plasticizer into the moist heat starch-lignosulfonic acid nano dispersion liquid, and stirring for 1h to prepare the ultraviolet-resistant high-strength starch nano composite membrane casting solution.
Step five, casting to form a film:
performing ultrasonic treatment on the composite membrane solution for 20-40min to remove bubbles;
then pouring the mixture into a mould to carry out casting film forming, putting the mixture into an air-blast drying oven along with the mould, and drying the mixture for 12 hours at the temperature of 40 ℃ to prepare the dry wet and hot starch-lignosulfonic acid nano composite film.
The wet and hot starch is prepared by the following processing technology: respectively adjusting the moisture content of the starch granules to 20 percent, 25 percent and 30 percent; equilibrating at 4 deg.C for 12h, sealing, and heat treating at 100 deg.C, 105 deg.C and 110 deg.C for 6h in an oven.
The preparation process of the lignosulfonic acid nanoparticles comprises the following steps: preparing a 5 wt% sodium lignosulfonate solution, and soaking the sodium lignosulfonate solution in 732 type cation exchange resin for 72 hours; then passes through 717 type anion exchange resin, the elution rate is kept to be 1d/4-5s in the whole process.
The preparation process of the lignosulfonic acid nano dispersion liquid comprises the following steps: dispersing the lignosulfonic acid nanoparticles in distilled water according to the proportion of 1:50-100, intermittently stirring and ultrasonically treating for 0.5h to prepare uniformly dispersed lignosulfonic acid nano dispersion liquid.
As a further aspect of the present invention, the starch is corn starch, potato starch, or tapioca starch.
As a further embodiment of the invention, the starch has a molecular weight of 130kDa and a purity of > 99%.
As a further aspect of the invention, the lignosulfonic acid nanoparticles have a size of 10-100 nm.
As a further aspect of the invention, the plasticizer is glycerin.
In a further aspect of the present invention, the mold is made of a transparent material.
In a further aspect of the present invention, the transparent material is glass or polymethyl methacrylate.
As a further scheme of the invention, the sodium alginate-nano silicon dioxide composite membrane is prepared; the thickness is 40-50 μm.
Compared with the prior art, the invention has the beneficial effects that:
the starch-lignosulfonic acid nano composite film with the thickness of 30-50 μm has the elongation at break and tensile strength respectively up to 140% and more than 54MPa (the elongation and tensile strength are respectively increased by 152% and 1642% compared with pure starch films), and in addition, the nano composite film has excellent uvioresistant performance and can fully meet the application of food packaging films.
Drawings
FIG. 1 is a water soluble picture of a composite film;
FIG. 2 is a graph of the UV resistance of a composite film;
fig. 3 illustrates the degradation of a composite membrane in four common environments.
Detailed Description
Referring to fig. 1-3, the present invention provides a technical solution: a preparation method of an uvioresistant high-strength starch nano composite film comprises the following steps:
firstly, preparing raw materials: 10-33.3 parts of moist heat treatment starch; 1 part of lignosulfonic acid nanoparticles and 4-13.3 parts of plasticizer;
step two, preparing a moist heat treatment starch stock solution: and (3) mixing the moist heat treatment starch powder with distilled water according to the mass ratio of 1: 10-16.7, adding into distilled water, and mechanically stirring at 40-90 deg.C for 10-60min until completely dissolving to obtain wet heat treated starch stock solution;
step three, preparing a moist heat starch-lignosulfonic acid mixed solution:
dropwise adding the lignosulfonic acid nano dispersion into the wet and hot starch stock solution under stirring of 500-800rmp, and stirring for 1-2h to obtain uniform wet and hot starch-lignosulfonic acid nano dispersion;
step four, adding a plasticizer:
and adding a plasticizer into the moist heat starch-lignosulfonic acid nano dispersion liquid, and stirring for 1h to prepare the ultraviolet-resistant high-strength starch nano composite membrane casting solution.
Step five, casting to form a film:
performing ultrasonic treatment on the composite membrane solution for 20-40min to remove bubbles;
then pouring the mixture into a mould to carry out casting film forming, putting the mixture into an air-blast drying oven along with the mould, and drying the mixture for 12 hours at the temperature of 40 ℃ to prepare the dry wet and hot starch-lignosulfonic acid nano composite film.
The wet and hot starch is prepared by the following processing technology: respectively adjusting the moisture content of the starch granules to 20 percent, 25 percent and 30 percent; equilibrating at 4 deg.C for 12h, sealing, and heat treating at 100 deg.C, 105 deg.C and 110 deg.C for 6h in an oven.
The preparation process of the lignosulfonic acid nanoparticles comprises the following steps: preparing a 5 wt% sodium lignosulfonate solution, and soaking the sodium lignosulfonate solution in 732 type cation exchange resin for 72 hours; then passes through 717 type anion exchange resin, the elution rate is kept to be 1d/4-5s in the whole process.
The preparation process of the lignosulfonic acid nano dispersion liquid comprises the following steps: dispersing the lignosulfonic acid nanoparticles in distilled water according to the proportion of 1:50-100, intermittently stirring and ultrasonically treating for 0.5h to prepare uniformly dispersed lignosulfonic acid nano dispersion liquid.
Wherein the starch is corn starch, potato starch or tapioca starch.
Wherein the starch has a molecular weight of 130kDa and a purity of > 99%.
Wherein the size of the lignosulfonic acid nanoparticles is 10-100 nm.
Wherein the plasticizer is glycerol.
Wherein, the material of mould is transparent material.
Wherein, the transparent material is glass or polymethyl methacrylate.
Wherein the sodium alginate-nano silicon dioxide composite membrane is prepared; the thickness is 40-50 μm.
Example 1:
the preparation method comprises the following steps:
firstly, respectively taking 1 part of lignosulfonic acid, 33.3 parts of moist heat modified starch (110 ℃, 30% of water content) and 13.3 parts of glycerol for later use;
secondly, adding 33.3 parts of moist heat modified starch (110 ℃, 30% water content) into 555mL of water to prepare 6 wt% starch solution;
dispersing 1 part of lignosulfonic acid particles into 10mL of distilled water, intermittently ultrasonically stirring for 30min, and slowly dripping into 6 wt% starch solution by using a constant-pressure dropping funnel;
fourthly, adding 13.3 parts of glycerol, and stirring for 1 hour to obtain casting solution
Fifthly, casting the film forming solution into a mold to form a film; and then, putting the mould into an oven, and drying for 10 hours at 40 ℃ to obtain the dried starch-lignosulfonic acid nano-composite membrane.
Product detection and inspection results:
the elongation at break of the prepared composite film is 75.3%, and the tensile strength is 50.6 MPa;
the composite membrane is soaked in water for 24 hours without change, which shows that the composite membrane has good water resistance.
Blocking rates of 88% and 93% for UVA and UVB, respectively.
Example 2:
the preparation method comprises the following steps:
firstly, respectively taking 1 part of lignosulfonic acid, 14.3 parts of moist heat modified starch (110 ℃, 25% of water content) and 5.7 parts of glycerol for later use;
secondly, 14.3 parts of moist heat modified starch (110 ℃, 25% of water content) is added into 238mL of water to prepare 6 wt% of starch solution;
dispersing 1 part of lignosulfonic acid particles into 10mL of distilled water, intermittently ultrasonically stirring for 30min, and slowly dripping into 6 wt% starch solution by using a constant-pressure dropping funnel;
fourthly, adding 5.7 parts of glycerol, and stirring for 1 hour to obtain casting solution
The rest is the same as the first embodiment.
Product detection and inspection results:
the elongation at break of the prepared composite film is 140 percent, and the tensile strength is 60 MPa;
the composite membrane is soaked in water for 24 hours without change, which shows that the composite membrane has good water resistance.
Has 99% and 100% blocking rate for UVA and UVB respectively.
Example 3:
the preparation method comprises the following steps:
firstly, respectively taking 1 part of lignosulfonic acid, 10 parts of moist heat modified starch (with the water content of 30 percent at 105 ℃) and 4 parts of glycerol for later use;
secondly, adding 10 parts of moist heat modified starch (105 ℃, 30% of water content) into 166mL of water to prepare 6 wt% of starch solution;
dispersing 1 part of lignosulfonic acid particles into 10mL of distilled water, intermittently ultrasonically stirring for 30min, and slowly dripping into 6 wt% starch solution by using a constant-pressure dropping funnel;
fourthly, adding 4 parts of glycerol, and stirring for 1 hour to obtain casting solution
The rest is the same as the first embodiment.
Product detection and inspection results:
the elongation at break of the prepared composite film is 110.3 percent, and the tensile strength is 45.6 MPa;
the composite membrane is soaked in water for 24 hours without change, which shows that the composite membrane has good water resistance.
The film has 99.5% and 100% blocking rate for UVA and UVB respectively.
Example 4:
the preparation method comprises the following steps:
firstly, respectively taking 1 part of lignosulfonic acid, 33.3 parts of moist heat modified starch (at 100 ℃, the water content of 25%) and 13.3 parts of glycerol for later use;
secondly, adding 33.3 parts of moist heat modified starch (100 ℃, 25% of water content) into 333mL of water to prepare 10 wt% of starch solution;
dispersing 1 part of lignosulfonic acid particles into 10mL of distilled water, intermittently ultrasonically stirring for 30min, and slowly dripping into 10 wt% of starch solution by using a constant-pressure dropping funnel;
the rest is the same as the first embodiment.
Product detection and inspection results:
the elongation at break of the prepared composite film is 75.3%, and the tensile strength is 53.6 MPa;
the composite membrane is soaked in water for 24 hours without change, which shows that the composite membrane has good water resistance.
Blocking rates of 88% and 93% for UVA and UVB, respectively.
Example 5:
the preparation method comprises the following steps:
firstly, respectively taking 1 part of lignosulfonic acid, 14.3 parts of moist heat modified starch (110 ℃, 25% of water content) and 5.7 parts of glycerol for later use;
secondly, 14.3 parts of moist heat modified starch (110 ℃, 25 percent of water content) is added into 143mL of water to prepare 10 weight percent of starch solution;
dispersing 1 part of lignosulfonic acid particles into 10mL of distilled water, intermittently ultrasonically stirring for 30min, and slowly dripping into 10 wt% of starch solution by using a constant-pressure dropping funnel;
fourthly, adding 5.7 parts of glycerol, and stirring for 1 hour to obtain casting solution
The rest is the same as the first embodiment.
Product detection and inspection results:
the elongation at break of the prepared composite film is 145.3 percent, and the tensile strength is 56.6 MPa;
the composite membrane is soaked in water for 24 hours without change, which shows that the composite membrane has good water resistance.
Has 99% and 100% blocking rate for UVA and UVB respectively.
Example 6:
the preparation method comprises the following steps:
firstly, respectively taking 1 part of lignosulfonic acid, 10 parts of moist heat modified starch (at 105 ℃, 25% of water content) and 4 parts of glycerol for later use;
step two, adding 10 parts of moist heat modified starch (105 ℃, 25% of water content) into 100mL of water to prepare 10 wt% of starch solution;
dispersing 1 part of lignosulfonic acid particles into 10mL of distilled water, intermittently ultrasonically stirring for 30min, and slowly dripping into 10 wt% of starch solution by using a constant-pressure dropping funnel;
fourthly, adding 4 parts of glycerol, and stirring for 1 hour to obtain casting solution
The rest is the same as the first embodiment.
Product detection and inspection results:
the elongation at break of the prepared composite film is 120.3 percent, and the tensile strength is 48.6 MPa;
the composite membrane is soaked in water for 24 hours without change, which shows that the composite membrane has good water resistance.
The film has 99.5% and 100% blocking rate for UVA and UVB respectively.
Analyzing and detecting water solubility, ultraviolet resistance indexes and degradability of the product:
water solubility is illustrated in example 3 in comparison to a pure starch film (figure 1).
The water-soluble picture shows that the composite membrane still keeps a better shape after being soaked in water for 24 hours.
The ultraviolet resistance is exemplified by example 1, example 2, example 3, example 6 (fig. 2):
graph of the degradation performance of starch composite film (fig. 3), using example 2 as an example:
fig. 3 shows that the composite membrane can be completely degraded in soil within 40 days, and can be degraded to different degrees in seawater, acidic and alkaline environments.
Wherein: the raw materials used were as follows:
the molecular weight of the starch is 130 kDa;
the sodium lignosulfonate is analytically pure, Na type 732# cation exchange resin, and the mass total exchange capacity is more than or equal to 4.5 mmol/g; 717# anion exchange resin;
the material of the used mold is transparent material (glass or polymethyl methacrylate).
The tensile strength and elongation at break were measured as follows:
at room temperature, sample size: the tensile strength and elongation at break of the film were measured at a distance of 15mm X100 mm, a clamp pitch of 50mm, and a drawing speed of 1 mm/s.
Claims (8)
1. A preparation method of an uvioresistant high-strength starch nano composite film is characterized by comprising the following steps: the method comprises the following steps:
firstly, preparing raw materials: 10-33.3 parts of moist heat treatment starch; 1 part of lignosulfonic acid nanoparticles and 4-13.3 parts of plasticizer;
step two, preparing a moist heat treatment starch stock solution: and (3) mixing the moist heat treatment starch powder with distilled water according to the mass ratio of 1: 10-16.7, adding into distilled water, and mechanically stirring at 40-90 deg.C for 10-60min until completely dissolving to obtain wet heat treated starch stock solution;
step three, preparing a moist heat starch-lignosulfonic acid mixed solution:
dropwise adding the lignosulfonic acid nano dispersion into the wet and hot starch stock solution under the stirring of 500-800rmp, and stirring for 1-2h to obtain uniform wet and hot starch-lignosulfonic acid nano dispersion;
step four, adding a plasticizer:
and adding a plasticizer into the moist heat starch-lignosulfonic acid nano dispersion liquid, and stirring for 1h to prepare the ultraviolet-resistant high-strength starch nano composite membrane casting solution.
Step five, casting to form a film:
performing ultrasonic treatment on the composite membrane solution for 20-40min to remove bubbles;
then pouring the mixture into a mould to carry out casting film forming, putting the mixture into an air-blast drying oven along with the mould, and drying the mixture for 12 hours at the temperature of 40 ℃ to prepare the dry wet and hot starch-lignosulfonic acid nano composite film.
The wet and hot starch is prepared by the following processing technology: respectively adjusting the moisture content of the starch granules to 20 percent, 25 percent and 30 percent; equilibrating at 4 deg.C for 12h, sealing, and heat treating in oven at 100 deg.C, 105 deg.C and 110 deg.C for 6 h.
The preparation process of the lignosulfonic acid nanoparticles comprises the following steps: preparing a 5 wt% sodium lignosulfonate solution, and soaking the sodium lignosulfonate solution in 732 type cation exchange resin for 72 hours; then passes through 717 type anion exchange resin, the elution rate is kept to be 1d/4-5s in the whole process.
The preparation process of the lignosulfonic acid nano dispersion liquid comprises the following steps: dispersing the lignosulfonic acid nanoparticles in distilled water according to the proportion of 1:50-100, intermittently stirring and ultrasonically treating for 0.5h to prepare uniformly dispersed lignosulfonic acid nano dispersion liquid.
2. The preparation method of the ultraviolet-resistant high-strength starch nanocomposite film according to claim 1, wherein the preparation method comprises the following steps: the starch is corn starch, potato starch or cassava starch.
3. The preparation method of the uvioresistant high-strength starch nano composite film according to claim 1, characterized in that: the starch has a molecular weight of 130kDa and a purity of > 99%.
4. The preparation method of the uvioresistant high-strength starch nano composite film according to claim 1, characterized in that: the size of the lignosulfonic acid nanoparticles is 10-100 nm.
5. The preparation method of the uvioresistant high-strength starch nano composite film according to claim 1, characterized in that: the plasticizer is glycerol.
6. The preparation method of the ultraviolet-resistant high-strength starch nanocomposite film according to claim 1, wherein the preparation method comprises the following steps: the mould is made of transparent materials.
7. The preparation method of the ultraviolet-resistant high-strength starch nanocomposite film according to claim 6, wherein the preparation method comprises the following steps: the transparent material is glass or polymethyl methacrylate.
8. The preparation method of the uvioresistant high-strength starch nano composite film according to claim 1, characterized in that: preparing the sodium alginate-nano silicon dioxide composite membrane; the thickness is 40-50 μm.
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| CN117183041B (en) * | 2023-07-11 | 2024-06-07 | 南京林业大学 | Gelatin-lignin sulfonic acid wood composite acoustic diaphragm and preparation method and application thereof |
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