CN107383435B - Preparation method of cellulose/chitosan-based nano fresh-keeping drug-loaded sponge - Google Patents
Preparation method of cellulose/chitosan-based nano fresh-keeping drug-loaded sponge Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/08—Cellulose derivatives
- C08L1/26—Cellulose ethers
- C08L1/28—Alkyl ethers
- C08L1/286—Alkyl ethers substituted with acid radicals, e.g. carboxymethyl cellulose [CMC]
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/048—Elimination of a frozen liquid phase
- C08J2201/0482—Elimination of a frozen liquid phase the liquid phase being organic
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/048—Elimination of a frozen liquid phase
- C08J2201/0484—Elimination of a frozen liquid phase the liquid phase being aqueous
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- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
- C08J2301/26—Cellulose ethers
- C08J2301/28—Alkyl ethers
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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
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
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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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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- 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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2203/00—Applications
- C08L2203/14—Applications used for foams
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Abstract
The invention relates to a preparation method of a cellulose/chitosan-based nano fresh-keeping drug-loaded sponge, belonging to the technical field of food packaging materials. The invention takes sodium carboxymethyl cellulose and chitosan as main base materials. The preparation method comprises the following steps: firstly, respectively dissolving sodium carboxymethylcellulose and chitosan in a certain mass ratio, mixing the two solutions, adjusting the pH value to 1.0 by using hydrochloric acid, adding bacteriostatic factor nano titanium dioxide, ethylene adsorption factor bentonite and plasticizer glycerol, fully stirring, standing for defoaming, finally pouring into a mould, and performing vacuum freeze-drying to form a sponge product. The product is non-toxic, harmless and biodegradable, and is an environment-friendly product; the product is added with nano antibacterial factors and ethylene adsorption factors, and has excellent antibacterial and fresh-keeping effects while having the basic mechanical buffering performance of filling sponge.
Description
Technical Field
The invention belongs to the technical field of food packaging materials, relates to a preparation method of a spongy material, and particularly relates to a preparation method of a biodegradable packaging filling sponge with antibacterial and fresh-keeping effects.
Background
Along with the increasing serious problem of environmental pollution, a non-toxic, degradable and environment-friendly packaging material becomes a current research hotspot. For a long time, the traditional tropical fruit fresh-keeping technology mainly depends on the soaking of the fruit by chemicals and the use of petroleum-derived plastic products. The method for soaking the medicament is simple and efficient, but has the harm and risk of medicament residues to human health; the use of plastic packaging has the problems of food safety caused by the migration of small molecular organic matters to food on one hand, and energy consumption and environmental pollution on the other hand.
Sodium carboxymethylcellulose (CMC) is a cellulose derivative which takes natural fiber substances as raw materials, has good biocompatibility, wettability, dispersibility, adhesiveness, thickening property, emulsibility, water-retaining property and film-forming property, is non-toxic and harmless, and is biodegradable; the hydrogel system of CMC is a space network structure formed by covalent bond, hydrogen bond, van der Waals force, physical entanglement and other crosslinking actions among macromolecules, so that the macromolecule composite material prepared by taking CMC as a base material has excellent mechanical properties. Chitosan (CS), also known as Chitosan, polyThe chitosan has free amino group, physical and chemical properties are very active, and has the characteristics of no toxic or side effect, good biocompatibility, controllable biodegradation, no antigenicity and the like2Content, decrease of O2The content, the respiration and the water loss are inhibited, the aging of the tissues and mechanisms of the fruits and the vegetables is slowed down, but the antiseptic and bacteriostatic properties of the fruits and the vegetables cannot be fully exerted, so that the excellent properties of the potential food packaging material are greatly reduced.
Disclosure of Invention
The invention provides a cellulose/chitosan-based nano fresh-keeping medicine-carrying sponge and a preparation method thereof aiming at the existing problems of chitosan fruit fresh-keeping materials in the background art and aiming at giving full play to the good antiseptic and bacteriostatic properties of chitosan materials.
The purpose of the invention can be realized by the following technical scheme: a preparation method of a cellulose/chitosan-based nano fresh-keeping drug-loaded sponge is characterized by comprising the following steps:
(1) dissolving sodium carboxymethylcellulose in distilled water to form sodium carboxymethylcellulose solution, dissolving chitosan in acetic acid solution, and adjusting pH value of the two solutions with hydrochloric acid;
(2) blending the two solutions in the step (1), adding nano titanium dioxide, bentonite and glycerol, uniformly stirring, and standing for defoaming;
(3) pouring the mixed liquid obtained in the step (2) into a mould, and carrying out vacuum freeze drying to obtain the sponge product.
The substitution degree of the sodium carboxymethylcellulose in the step (1) is 0.7-1.2, and the deacetylation degree of the chitosan is 50-95%. The mass ratio is as follows: the ratio of chitosan is 2-5: 1;
the pH value range of the solution in the step (1) is 1.0-4.0;
the granularity of the nano titanium dioxide in the step (2) is 50-400nm, the adding amount is 1-10% of the total dry matter weight, and the density of the bentonite is 2-3 g/cm3The adding amount is 1-6% of the total dry matter, and the adding amount of the glycerol is 1-8% of the total dry matter;
the mould in the step (3) is a mould prepared from a polystyrene material.
Compared with the prior art, the invention has the following advantages:
(1) the adopted base materials of sodium carboxymethyl cellulose and chitosan are biomass high molecular substances, have good cross-linking film-forming performance, and the formed sponge has a uniform spatial network structure, has excellent buffering capacity, and also has good loading and controlled release capacity on the antibacterial factor nano titanium dioxide and the ethylene adsorption factor bentonite.
(2) One of the base materials of the invention, chitosan, has natural bacteriostatic activity, the added functional factor, namely nano titanium dioxide, also has excellent bacteriostatic ability, and bentonite is an excellent ethylene adsorbent. Therefore, the sponge product has the effects of resisting bacteria, keeping fresh and delaying decay while having the mechanical buffering function. The following experimental results show the preservation period of some common fruits packaged by common sponge net, chitosan sponge and nano titanium dioxide chitosan sponge at 15 ℃ (sample amount: 20, average value in the table):
(3) the invention applies the biomass polymer composite material and the drug sustained-release technology to the field of food packaging filling materials, accords with the development direction of green materials, and has important social and economic benefits.
Detailed Description
Example 1:
(1) weighing sodium carboxymethylcellulose and chitosan powder according to the mass ratio of 2: 1; wherein the substitution degree of the sodium carboxymethylcellulose is 0.7, the deacetylation degree of the chitosan is 50%, the sodium carboxymethylcellulose is dissolved in distilled water to form a 2% sodium carboxymethylcellulose solution, the chitosan is dissolved in an acetic acid solution to form a 1.5% chitosan solution, and hydrochloric acid is used for adjusting the pH values of the two solutions to 1.0;
(2) blending the two solutions in the step (1), adding nano titanium dioxide, bentonite and glycerol, uniformly stirring, and standing for defoaming; wherein the particle size of the nano titanium dioxide is 60 nm, the addition amount is 1% of the total dry matter, the density of the bentonite is 2-3 g/cm3, the addition amount is 6% of the total dry matter, and the addition amount of the glycerol is 4% of the total dry matter;
(3) pouring the mixed liquid obtained in the step (2) into a mould, and carrying out vacuum freeze drying to obtain the sponge product.
Example 2:
(1) weighing sodium carboxymethylcellulose and chitosan powder according to the mass ratio of 3: 1; wherein the substitution degree of the sodium carboxymethylcellulose is 0.8, the deacetylation degree of the chitosan is 60%, the sodium carboxymethylcellulose is dissolved in distilled water to form a 2% sodium carboxymethylcellulose solution, the chitosan is dissolved in an acetic acid solution to form a 1.5% chitosan solution, and hydrochloric acid is used for adjusting the pH values of the two solutions to 1.0;
(2) blending the two solutions in the step (1), adding nano titanium dioxide, bentonite and glycerol, uniformly stirring, and standing for defoaming; wherein the particle size of the nano titanium dioxide is 150 nm, the addition amount of the nano titanium dioxide is 4% of the total dry matter, the density of the bentonite is 2-3 g/cm3, the addition amount of the nano titanium dioxide is 4% of the total dry matter, and the addition amount of the glycerol is 4% of the total dry matter;
(3) pouring the mixed liquid obtained in the step (2) into a mould, and carrying out vacuum freeze drying to obtain the sponge product.
Example 3:
(1) weighing sodium carboxymethylcellulose and chitosan powder according to the mass ratio of 4: 1; wherein the substitution degree of the sodium carboxymethylcellulose is 0.7, the deacetylation degree of the chitosan is 50%, the sodium carboxymethylcellulose is dissolved in distilled water to form a 2% sodium carboxymethylcellulose solution, the chitosan is dissolved in an acetic acid solution to form a 1.5% chitosan solution, and hydrochloric acid is used for adjusting the pH values of the two solutions to 1.0;
(2) blending the two solutions in the step (1), adding nano titanium dioxide, bentonite and glycerol, uniformly stirring, and standing for defoaming; wherein the particle size of the nano titanium dioxide is 60 nm, the addition amount of the nano titanium dioxide is 7% of the total dry matter, the density of the bentonite is 2-3 g/cm3, the addition amount of the nano titanium dioxide is 2% of the total dry matter, and the addition amount of the glycerol is 4% of the total dry matter;
(3) pouring the mixed liquid obtained in the step (2) into a mould, and carrying out vacuum freeze drying to obtain the sponge product.
Example 4:
(1) weighing sodium carboxymethylcellulose and chitosan powder according to the mass ratio of 5: 1; wherein the substitution degree of the sodium carboxymethylcellulose is 0.7, the deacetylation degree of the chitosan is 50%, the sodium carboxymethylcellulose is dissolved in distilled water to form a 2% sodium carboxymethylcellulose solution, the chitosan is dissolved in an acetic acid solution to form a 1.5% chitosan solution, and hydrochloric acid is used for adjusting the pH values of the two solutions to 1.0;
(2) blending the two solutions in the step (1), adding nano titanium dioxide, bentonite and glycerol, uniformly stirring, and standing for defoaming; wherein the particle size of the nano titanium dioxide is 200 nm, the addition amount is 10% of the total dry matter, the density of the bentonite is 2-3 g/cm3, the addition amount is 1% of the total dry matter, and the addition amount of the glycerol is 4% of the total dry matter;
(3) pouring the mixed liquid obtained in the step (2) into a mould, and carrying out vacuum freeze drying to obtain the sponge product.
Example 5:
(1) weighing sodium carboxymethylcellulose and chitosan powder according to the mass ratio of 2: 1; wherein the substitution degree of the sodium carboxymethylcellulose is 0.7, the deacetylation degree of the chitosan is 50%, the sodium carboxymethylcellulose is dissolved in distilled water to form a 2% sodium carboxymethylcellulose solution, the chitosan is dissolved in an acetic acid solution to form a 1.5% chitosan solution, and hydrochloric acid is used for adjusting the pH values of the two solutions to 2.0;
(2) blending the two solutions in the step (1), adding nano titanium dioxide, bentonite and glycerol, uniformly stirring, and standing for defoaming; wherein the particle size of the nano titanium dioxide is 170 nm, the addition amount is 1% of the total dry matter, the density of the bentonite is 2-3 g/cm3, the addition amount is 6% of the total dry matter, and the addition amount of the glycerol is 8% of the total dry matter;
(3) pouring the mixed liquid obtained in the step (2) into a mould, and carrying out vacuum freeze drying to obtain the sponge product.
Example 6:
(1) weighing sodium carboxymethylcellulose and chitosan powder according to the mass ratio of 3: 1; wherein the substitution degree of the sodium carboxymethylcellulose is 0.8, the deacetylation degree of the chitosan is 60%, the sodium carboxymethylcellulose is dissolved in distilled water to form a 2% sodium carboxymethylcellulose solution, the chitosan is dissolved in an acetic acid solution to form a 1.5% chitosan solution, and hydrochloric acid is used for adjusting the pH values of the two solutions to 4.0;
(2) blending the two solutions in the step (1), adding nano titanium dioxide, bentonite and glycerol, uniformly stirring, and standing for defoaming; wherein the particle size of the nano titanium dioxide is 80 nm, the addition amount of the nano titanium dioxide is 4% of the total dry matter, the density of the bentonite is 2-3 g/cm3, the addition amount of the nano titanium dioxide is 4% of the total dry matter, and the addition amount of the glycerol is 8% of the total dry matter;
(3) pouring the mixed liquid obtained in the step (2) into a mould, and carrying out vacuum freeze drying to obtain the sponge product.
Example 7:
(1) weighing sodium carboxymethylcellulose and chitosan powder according to the mass ratio of 4: 1; wherein the substitution degree of the sodium carboxymethylcellulose is 0.7, the deacetylation degree of the chitosan is 50%, the sodium carboxymethylcellulose is dissolved in distilled water to form a 2% sodium carboxymethylcellulose solution, the chitosan is dissolved in an acetic acid solution to form a 1.5% chitosan solution, and hydrochloric acid is used for adjusting the pH values of the two solutions to 3.0;
(2) blending the two solutions in the step (1), adding nano titanium dioxide, bentonite and glycerol, uniformly stirring, and standing for defoaming; wherein the particle size of the nano titanium dioxide is 120 nm, the addition amount of the nano titanium dioxide is 7% of the total dry matter, the density of the bentonite is 2-3 g/cm3, the addition amount of the nano titanium dioxide is 2% of the total dry matter, and the addition amount of the glycerol is 8% of the total dry matter;
(3) pouring the mixed liquid obtained in the step (2) into a mould, and carrying out vacuum freeze drying to obtain the sponge product.
Example 8:
(1) weighing sodium carboxymethylcellulose and chitosan powder according to the mass ratio of 5: 1; wherein the substitution degree of the sodium carboxymethylcellulose is 0.7, the deacetylation degree of the chitosan is 50%, the sodium carboxymethylcellulose is dissolved in distilled water to form a 2% sodium carboxymethylcellulose solution, the chitosan is dissolved in an acetic acid solution to form a 1.5% chitosan solution, and hydrochloric acid is used for adjusting the pH values of the two solutions to 2.0;
(2) blending the two solutions in the step (1), adding nano titanium dioxide, bentonite and glycerol, uniformly stirring, and standing for defoaming; wherein the particle size of the nano titanium dioxide is 70 nm, the addition amount is 10% of the total dry matter, the density of the bentonite is 2-3 g/cm3, the addition amount is 1% of the total dry matter, and the addition amount of the glycerol is 8% of the total dry matter;
(3) pouring the mixed liquid obtained in the step (2) into a mould, and carrying out vacuum freeze drying to obtain the sponge product.
Claims (2)
1. A preparation method of a cellulose/chitosan-based nano fresh-keeping drug-loaded sponge is characterized by comprising the following steps:
(1) dissolving sodium carboxymethylcellulose in distilled water to form sodium carboxymethylcellulose solution, dissolving chitosan in acetic acid solution, and adjusting pH value of the two solutions with hydrochloric acid;
(2) blending the two solutions in the step (1), adding nano titanium dioxide, bentonite and glycerol, uniformly stirring, and standing for defoaming;
(3) pouring the mixed liquid obtained in the step (2) into a mould, and finally carrying out vacuum freeze drying to obtain a finished product;
wherein the substitution degree of the sodium carboxymethylcellulose in the step (1) is 0.7-1.2, the deacetylation degree of the chitosan is 50-95%, and the mass ratio is that the sodium carboxymethylcellulose: the ratio of chitosan is 2-5: 1; the pH value range of the solution in the step (1) is 1.0-4.0; the particle size range of the nano titanium dioxide in the step (3) is 50-400nm, the adding amount is 1-10% of the total dry matter weight, and the density of the bentonite is 2-3 g/cm3The adding amount is 1-6% of the total dry matter, and the adding amount of the glycerol is 1-8% of the total dry matter.
2. The method according to claim 1, wherein the mold in the step (3) is a mold made of polystyrene material.
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Application publication date: 20171124 Assignee: Taizhou Zhike Feichuang Technology Co.,Ltd. Assignor: RESEARCH INSTITUTE OF ZHEJIANG University TAIZHOU Contract record no.: X2022980021767 Denomination of invention: A preparation method of cellulose/chitosan based nano fresh-keeping drug loaded sponge Granted publication date: 20200724 License type: Common License Record date: 20221115 |
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