CN115044106B - 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 ultraviolet-resistant high-strength starch nano composite film in the technical field of high-strength starch nano composite films, which comprises 10-33.3 parts of wet heat treated starch; 1 part of lignin sulfonic acid nano particles and 4-13.3 parts of plasticizer; secondly, preparing a wet heat treatment starch stock solution: the starch powder is subjected to damp heat treatment according to the mass ratio of the starch powder to distilled water of 1:10-16.7, adding into distilled water, mechanically stirring at 40-90deg.C for 10-60min until completely dissolving to obtain wet heat treated starch stock solution; thirdly, preparing wet and hot starch-lignin sulfonic acid mixed solution; the thickness of the starch-lignin sulfonic acid nano composite film is 30-50 mu m, the elongation at break and the tensile strength of the starch-lignin sulfonic acid nano composite film can respectively reach 140% and above 54MPa (152% and 1642% are respectively improved 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 ultraviolet-resistant high-strength starch nano composite film.
Background
Currently, the overuse of petroleum-based packaging and the ever decreasing petroleum resources have led to an increasing interest in natural high molecular weight polymers.
Starch is a natural high molecular compound which has low price, easy acquisition, biodegradability and good biocompatibility. Among them, starch-based food packaging films are considered as one of the most promising "green packaging materials". However, due to the limitation of the self-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 bacteriostasis) and the like.
The wet heat treatment of the starch is to treat the starch for a certain time (15 min-6 h) under the conditions of lower moisture content (10% -30%) and higher temperature (90-130 ℃), namely the structure and physical and chemical properties of the starch are changed through the combined action of water molecules and heat so as to influence the application properties of the starch.
The lignin sulfonic acid (LA) is mainly derived from sodium lignin sulfonate which is a common byproduct in the sulfite pulping industry, and has the characteristics of low cost, easy obtainment, no toxicity and environmental protection. LA molecules contain structures of benzene rings and phenylpropanes rich in hydrophobicity and hydroxyl and sulfonic groups rich in hydrophilicity, and the special amphipathy enables lignin sulfonic acid molecules to be self-assembled to form nano particles with 3D complex molecular structures after being dispersed in aqueous solution. And a large number of hydrophilic groups can form strong hydrogen bonds with starch molecules, so that amorphous starch molecules are dynamically restrained by sacrificing the hydrogen bonds, and excellent reinforcing and toughening effects can be achieved by promoting chain extension and regularity. In addition, the polyphenol units and a large number of chromophore structures in the LA molecules lead the LA molecules to bring excellent ultraviolet resistance to the composite membrane,
in the prior art, a great deal of research is carried out on the aspects of starch modification, composite film formation and the like by the person skilled in the art, and a series of modification modes such as chemical modification (esterification, etherification, grafting, 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 the starch film, improving the preparation process of the starch film and the like. These modification methods have problems of high modification cost and complicated process. The method combines simple wet and hot physical treatment with green biomass nano particle compounding, modifies the starch film, and obtains the composite film with excellent mechanical property, ultraviolet resistance and hydrophobic property.
Based on the above, the invention designs a preparation method of an anti-ultraviolet high-strength starch nano composite film to solve the above problems.
Disclosure of Invention
The invention aims to provide a preparation method of an ultraviolet-resistant high-strength starch nano composite film, which aims to solve the problems in the background technology.
In order to achieve the above purpose, the present invention provides the following technical solutions: the preparation method of the ultraviolet-resistant high-strength starch nano composite film comprises the following steps:
firstly, preparing raw materials: 10-33.3 parts of wet heat treated starch; 1 part of lignin sulfonic acid nano particles and 4-13.3 parts of plasticizer;
secondly, preparing a wet heat treatment starch stock solution: the starch powder is subjected to damp heat treatment according to the mass ratio of the starch powder to distilled water of 1:10-16.7, adding into distilled water, mechanically stirring at 40-90deg.C for 10-60min until completely dissolving to obtain wet heat treated starch stock solution;
thirdly, preparing wet and hot starch-lignin sulfonic acid mixed solution:
dropwise adding the lignin sulfonic acid nano dispersion liquid into the wet and hot starch stock solution under 500-800rmp stirring, and stirring for 1-2h to obtain uniform wet and hot starch-lignin sulfonic acid nano dispersion liquid;
fourth, adding plasticizer:
and adding a plasticizer into the wet and hot starch-lignin sulfonic acid nano dispersion liquid, and stirring for 1h to prepare the ultraviolet-resistant high-strength starch nano composite film casting solution.
Fifth, casting film:
ultrasonic treatment is carried out on the composite membrane solution for 20-40min to remove bubbles;
then pouring the mixture into a mould for casting to form a film, placing the film and the mould in a blast drying box together, and drying the film for 12 hours at the temperature of 40 ℃ to obtain the dry wet and hot starch-lignin sulfonic acid nano composite film.
The wet and hot starch comprises the following treatment processes: the water content of the starch granules is respectively adjusted to 20 percent, 25 percent and 30 percent; equilibrated at 4deg.C for 12h, sealed, and placed in an oven for heat treatment at 100deg.C, 105deg.C and 110deg.C, respectively, for 6h.
The preparation process of the lignin sulfonic acid nano particles comprises the following steps: preparing 5wt% sodium lignin sulfonate solution, and soaking the solution in 732 type cation exchange resin for 72 hours; then passing through 717 type anion exchange resin, the elution rate is kept 1d/4-5s in the whole process.
The preparation process of the lignin sulfonic acid nano dispersion liquid comprises the following steps: dispersing lignin sulfonic acid nano particles in distilled water according to the proportion of 1:50-100, and intermittently stirring and ultrasonic treating for 0.5h to prepare uniformly dispersed lignin sulfonic acid nano dispersion liquid.
As a further aspect of the invention, the starch is corn starch, potato starch or tapioca starch.
As a further aspect 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 nanoparticle size is 10-100nm.
As a further aspect of the present invention, the plasticizer is glycerin.
As a further aspect of the present invention, the material of the mold is 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 prepared sodium alginate-nano silicon dioxide composite film; the thickness is 40-50 μm.
Compared with the prior art, the invention has the beneficial effects that:
the thickness of the starch-lignin sulfonic acid nano composite film is 30-50 mu m, the elongation at break and the tensile strength of the starch-lignin sulfonic acid nano composite film can reach 140% and 54MPa respectively (152% and 1642% are respectively improved compared with a pure starch film), and in addition, the nano composite film has excellent ultraviolet resistance, 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 the UV resistance of the composite film;
FIG. 3 shows degradation of the composite membrane in four common environments.
Detailed Description
Referring to fig. 1-3, the present invention provides a technical solution: the preparation method of the ultraviolet-resistant high-strength starch nano composite film comprises the following steps:
firstly, preparing raw materials: 10-33.3 parts of wet heat treated starch; 1 part of lignin sulfonic acid nano particles and 4-13.3 parts of plasticizer;
secondly, preparing a wet heat treatment starch stock solution: the starch powder is subjected to damp heat treatment according to the mass ratio of the starch powder to distilled water of 1:10-16.7, adding into distilled water, mechanically stirring at 40-90deg.C for 10-60min until completely dissolving to obtain wet heat treated starch stock solution;
thirdly, preparing wet and hot starch-lignin sulfonic acid mixed solution:
dropwise adding the lignin sulfonic acid nano dispersion liquid into the wet and hot starch stock solution under 500-800rmp stirring, and stirring for 1-2h to obtain uniform wet and hot starch-lignin sulfonic acid nano dispersion liquid;
fourth, adding plasticizer:
and adding a plasticizer into the wet and hot starch-lignin sulfonic acid nano dispersion liquid, and stirring for 1h to prepare the ultraviolet-resistant high-strength starch nano composite film casting solution.
Fifth, casting film:
ultrasonic treatment is carried out on the composite membrane solution for 20-40min to remove bubbles;
then pouring the mixture into a mould for casting to form a film, placing the film and the mould in a blast drying box together, and drying the film for 12 hours at the temperature of 40 ℃ to obtain the dry wet and hot starch-lignin sulfonic acid nano composite film.
The wet and hot starch comprises the following treatment processes: the water content of the starch granules is respectively adjusted to 20 percent, 25 percent and 30 percent; equilibrated at 4deg.C for 12h, sealed, and placed in an oven for heat treatment at 100deg.C, 105deg.C and 110deg.C, respectively, for 6h.
The preparation process of the lignin sulfonic acid nano particles comprises the following steps: preparing 5wt% sodium lignin sulfonate solution, and soaking the solution in 732 type cation exchange resin for 72 hours; then passing through 717 type anion exchange resin, the elution rate is kept 1d/4-5s in the whole process.
The preparation process of the lignin sulfonic acid nano dispersion liquid comprises the following steps: dispersing lignin sulfonic acid nano particles in distilled water according to the proportion of 1:50-100, and intermittently stirring and ultrasonic treating for 0.5h to prepare uniformly dispersed lignin sulfonic acid nano dispersion liquid.
Wherein the starch is corn starch, potato starch or tapioca starch.
Wherein the molecular weight of the starch is 130kDa, and the purity is more than 99%.
Wherein the size of the lignosulfonic acid nano particles is 10-100nm.
Wherein the plasticizer is glycerol.
Wherein, the material of mould is transparent material.
Wherein the transparent material is glass or polymethyl methacrylate.
Wherein the prepared sodium alginate-nano silicon dioxide composite membrane; the thickness is 40-50 μm.
Example 1:
the preparation method comprises the following steps:
firstly, respectively taking 1 part of lignin sulfonic acid, 33.3 parts of wet-heat modified starch (110 ℃ and 30% water content) and 13.3 parts of glycerin for later use;
secondly, 33.3 parts of wet-heat modified starch (110 ℃ and 30% of water content) is added into 555mL of water to prepare a 6wt% starch solution;
thirdly, dispersing 1 part of lignin sulfonic acid particles into 10mL of distilled water, intermittently and ultrasonically stirring for 30min, and slowly dripping into 6wt% of starch solution by using a constant pressure dropping funnel;
fourthly, adding 13.3 parts of glycerol, and stirring for 1h to obtain casting solution
Fifth, casting the film-forming solution into a mold to form a film; and then, putting the mould into a baking oven, and drying for 10 hours at 40 ℃ to obtain the dried starch-lignin sulfonic acid nano composite film.
Product detection and inspection results:
the elongation at break of the prepared composite film is 75.3 percent, and the tensile strength is 50.6MPa;
soaking in water for 24 hr, no change, and high water resistance.
Has a blocking rate of 88% and 93% for UVA and UVB, respectively.
Example 2:
the preparation method comprises the following steps:
firstly, respectively taking 1 part of lignin sulfonic acid, 14.3 parts of wet-heat modified starch (110 ℃ and 25% of water content) and 5.7 parts of glycerol for later use;
secondly, 14.3 parts of damp-heat modified starch (110 ℃ and 25% of water content) is added into 238mL of water to prepare a 6wt% starch solution;
thirdly, dispersing 1 part of lignin sulfonic acid particles into 10mL of distilled water, intermittently and ultrasonically stirring for 30min, and slowly dripping into 6wt% of starch solution by using a constant pressure dropping funnel;
fourth, adding 5.7 parts of glycerol, and stirring for 1h to obtain a casting solution
The rest is the same as in 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 60MPa;
soaking in water for 24 hr, no change, and high water resistance.
Has a blocking rate of 99% and 100% for UVA and UVB, respectively.
Example 3:
the preparation method comprises the following steps:
firstly, respectively taking 1 part of lignin sulfonic acid, 10 parts of wet-heat modified starch (105 ℃ and 30% water content) and 4 parts of glycerin for later use;
secondly, 10 parts of wet and hot modified starch (105 ℃ and 30% of water content) is added into 166mL of water to prepare a starch solution with the concentration of 6 wt%;
thirdly, dispersing 1 part of lignin sulfonic acid particles into 10mL of distilled water, intermittently and ultrasonically stirring for 30min, and slowly dripping into 6wt% of starch solution by using a constant pressure dropping funnel;
fourth, adding 4 parts of glycerin, and stirring for 1h to obtain a casting solution
The rest is the same as in 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 45.6MPa;
soaking in water for 24 hr, no change, and high water resistance.
Has a blocking rate of 99.5% and 100% for UVA and UVB, respectively.
Example 4:
the preparation method comprises the following steps:
firstly, respectively taking 1 part of lignin sulfonic acid, 33.3 parts of wet-heat modified starch (100 ℃ and 25% of water content) and 13.3 parts of glycerin for later use;
secondly, 33.3 parts of damp-heat modified starch (100 ℃ and 25% of water content) is added into 333mL of water to prepare 10wt% starch solution;
thirdly, dispersing 1 part of lignin sulfonic acid particles into 10mL of distilled water, intermittently and ultrasonically stirring for 30min, and slowly dripping into 10wt% of starch solution by using a constant pressure dropping funnel;
the rest is the same as in the first embodiment.
Product detection and inspection results:
the elongation at break of the prepared composite film is 75.3 percent, and the tensile strength is 53.6MPa;
soaking in water for 24 hr, no change, and high water resistance.
Has a blocking rate of 88% and 93% for UVA and UVB, respectively.
Example 5:
the preparation method comprises the following steps:
firstly, respectively taking 1 part of lignin sulfonic acid, 14.3 parts of wet-heat modified starch (110 ℃ and 25% of water content) and 5.7 parts of glycerol for later use;
secondly, 14.3 parts of damp-heat modified starch (110 ℃ and 25% of water content) is added into 143mL of water to prepare 10wt% starch solution;
thirdly, dispersing 1 part of lignin sulfonic acid particles into 10mL of distilled water, intermittently and ultrasonically stirring for 30min, and slowly dripping into 10wt% of starch solution by using a constant pressure dropping funnel;
fourth, adding 5.7 parts of glycerol, and stirring for 1h to obtain a casting solution
The rest is the same as in 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 56.6MPa;
soaking in water for 24 hr, no change, and high water resistance.
Has a blocking rate of 99% and 100% for UVA and UVB, respectively.
Example 6:
the preparation method comprises the following steps:
firstly, respectively taking 1 part of lignin sulfonic acid, 10 parts of wet-heat modified starch (105 ℃ and 25% water content) and 4 parts of glycerin for later use;
secondly, 10 parts of wet and hot modified starch (105 ℃ and 25% of water content) is added into 100mL of water to prepare 10wt% starch solution;
thirdly, dispersing 1 part of lignin sulfonic acid particles into 10mL of distilled water, intermittently and ultrasonically stirring for 30min, and slowly dripping into 10wt% of starch solution by using a constant pressure dropping funnel;
fourth, adding 4 parts of glycerin, and stirring for 1h to obtain a casting solution
The rest is the same as in 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 48.6MPa;
soaking in water for 24 hr, no change, and high water resistance.
Has a blocking rate of 99.5% and 100% for UVA and UVB, respectively.
Analysis and detection of water solubility, ultraviolet resistance indexes and degradability of the product:
the water solubility was exemplified by example 3 in comparison to a pure starch film (fig. 1).
The water-soluble pictures show that the composite film still keeps a good shape after being soaked in water for 24 hours.
Uv resistance as examples 1, 2, 3, 6 (fig. 2):
starch composite film degradation performance picture (fig. 3), taking example 2 as an example:
FIG. 3 shows that the composite membrane can be completely degraded in soil for 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 130kDa;
sodium lignin sulfonate is analytically pure, na type 732# cation exchange resin, and the mass total exchange capacity is more than or equal to 4.5mmol/g;717# anion exchange resin;
the mold used was made of a transparent material (glass or polymethyl methacrylate).
The tensile strength and elongation at break were measured as follows:
sample size at room temperature: 15mm X100 mm, a jig pitch of 50mm, and a stretching speed of 1mm/s were measured to determine the tensile strength and elongation at break of the film.
Claims (7)
1. A preparation method of an anti-ultraviolet 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 wet heat treated starch; 1 part of lignin sulfonic acid nano particles and 4-13.3 parts of plasticizer; the plasticizer is glycerol;
secondly, preparing a wet heat treatment starch stock solution: the starch powder is subjected to damp heat treatment according to the mass ratio of the starch powder to distilled water of 1:10-16.7, adding into distilled water, mechanically stirring at 40-90deg.C for 10-60min until completely dissolving to obtain wet heat treated starch stock solution;
thirdly, preparing wet and hot starch-lignin sulfonic acid mixed solution:
dropwise adding the lignin sulfonic acid nano dispersion liquid into the wet heat starch stock solution under 500-800rmp stirring, and stirring for 1-2h to obtain uniform wet heat starch-lignin sulfonic acid nano dispersion liquid;
fourth, adding plasticizer:
adding a plasticizer into the wet and hot starch-lignin sulfonic acid nano dispersion liquid, and stirring for 1h to prepare an ultraviolet-resistant high-strength starch nano composite film casting solution;
fifth, casting film:
ultrasonic treatment is carried out on the composite membrane solution for 20-40min to remove bubbles;
then pouring the mixture into a mould for casting to form a film, placing the film and the mould in a blast drying box together, and drying the film for 12 hours at the temperature of 40 ℃ to prepare a dry wet and hot starch-lignin sulfonic acid nano composite film;
the wet and hot starch comprises the following treatment processes: the water content of the starch granules is respectively adjusted to 20 percent, 25 percent and 30 percent; balancing at 4deg.C for 12 hr, sealing, and heat treating in oven at 100deg.C, 105deg.C and 110deg.C for 6 hr;
the preparation process of the lignin sulfonic acid nano particles comprises the following steps: preparing 5wt% sodium lignin sulfonate solution, and soaking the solution in 732 type cation exchange resin for 72 hours; then passing through 717 type anion exchange resin, and keeping the elution rate of 1d/4-5s in the whole process;
the preparation process of the lignin sulfonic acid nano dispersion liquid comprises the following steps: dispersing lignin sulfonic acid nano particles in distilled water according to the proportion of 1:50-100, and intermittently stirring and ultrasonic treating for 0.5h to prepare uniformly dispersed lignin sulfonic acid nano dispersion liquid.
2. The method for preparing the ultraviolet resistant high-strength starch nanocomposite film according to claim 1, wherein the method comprises the steps of: the starch is corn starch, potato starch or tapioca starch.
3. The method for preparing the ultraviolet resistant high-strength starch nanocomposite film according to claim 1, wherein the method comprises the steps of: the molecular weight of the starch is 130kDa, and the purity is more than 99%.
4. The method for preparing the ultraviolet resistant high-strength starch nanocomposite film according to claim 1, wherein the method comprises the steps of: the size of the lignosulfonic acid nano particles is 10-100nm.
5. The method for preparing the ultraviolet resistant high-strength starch nanocomposite film according to claim 1, wherein the method comprises the steps of: the material of the mould is transparent.
6. The method for preparing the ultraviolet resistant high-strength starch nano composite film according to claim 5, which is characterized in that: the transparent material is glass or polymethyl methacrylate.
7. The method for preparing the ultraviolet resistant high-strength starch nanocomposite film according to claim 1, wherein the method comprises the steps of: the thickness of the wet and hot starch-lignin sulfonic acid nano composite film is 40-50 mu m.
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