CN110591307A - Preparation method of high-strength full-degradable multifunctional bio-based composite film - Google Patents
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/04—Polyesters derived from hydroxy carboxylic acids, e.g. lactones
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- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/08—Cellulose derivatives
- C08J2401/26—Cellulose ethers
- C08J2401/28—Alkyl ethers
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- C08J2403/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2403/04—Starch derivatives
- C08J2403/08—Ethers
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- 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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- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
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- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a preparation method of a high-strength full-degradable multifunctional bio-based composite film. According to the invention, polylactic acid is taken as a base material, and a high-strength fully-degradable polylactic acid-based composite material system is constructed by compounding various biological base materials such as cationic modified starch, carboxymethyl modified cellulose, guar gum, xylitol and chitosan, so that the multifunctional biological-based composite film which has good heat resistance, barrier property and antibacterial property and is combined with excellent mechanical properties such as high impact resistance, high toughness and high elastic modulus is prepared. The raw materials used by the bio-based composite film are taken from nature and can be degraded, so that the bio-based composite film is a green and environment-friendly composite material; the raw material source is wide, the production cost is reduced, the industrial production benefit is improved, and the method can be widely applied to the fields of agricultural mulching films, food packages, cosmetic packaging materials, medical functional materials and the like.
Description
Technical Field
The invention relates to the field of composite materials, in particular to a preparation method of a high-strength fully-degradable multifunctional bio-based composite film.
Background
The bio-based material is a novel material and chemicals and the like which are manufactured by using renewable biomass such as grains, leguminous plants, straws, bamboo wood powder and the like as raw materials, comprises basic bio-based chemicals such as biological alcohol, organic acid, alkane, olefin and the like obtained in the processes of biosynthesis, biological processing and biorefinery, and also comprises plastic materials and the like obtained by performing thermoplastic processing on bio-based plastics, bio-based fibers, sugar engineering products, bio-based rubber and biomass. The bio-based materials are gradually becoming the leading industry of scientific and technological innovation and economic development in the world due to the characteristics of green, environment-friendly, resource saving and the like. Among them, polylactic acid, as an environment-friendly material, is most prominently characterized by its degradability and biocompatibility, and in addition, polylactic acid has excellent post-processability, transparency, and gas barrier property, but polylactic acid materials also have some disadvantages, including slow crystallization rate, poor heat resistance, poor impact resistance, etc., which limit the wide application of polylactic acid.
At present, aiming at the problem of poor mechanical properties of polylactic acid, many researchers add biomass materials such as nanocrystalline cellulose, nanofibrillated cellulose and the like for reinforcement, and in order to improve the interface bonding force between the fiber material and the polylactic acid, silane coupling agents are often used for modification, or organic solvents such as trichloromethane and chloroform are used for dissolving the polylactic acid, and the used auxiliary agents, solvents and the like have certain toxicity and are not easy to degrade. In addition, only the nano-cellulose is used for reinforcing the polylactic acid, so that the effect is single and not obvious, the production cost is increased, and the formation of the industrial chain of the polylactic acid is not facilitated. Therefore, the invention constructs a high-strength fully-degradable polylactic acid-based composite material system by compounding a plurality of bio-based materials, prepares a multifunctional bio-based composite film which has good heat resistance, barrier property and antibacterial property and integrates excellent mechanical properties such as high impact resistance, high toughness, high elastic modulus and the like, and is widely applied to the fields of agricultural mulching films, food, cosmetic packaging materials, medical functional materials and the like.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a high-strength fully-degradable multifunctional bio-based composite film and a preparation method thereof.
The invention is realized by the following technical scheme:
a high-strength full-degradable multifunctional bio-based composite film comprises the following raw materials in parts by weight: 100 parts of polylactic acid; 10-15 parts of cation modified starch; 5 parts of nano calcium carbonate; 3-5 parts of xylitol; 3-5 parts of carboxymethyl modified nano-cellulose; 1-3 parts of chitosan; 1-3 parts of polyethylene glycol; 0.5-1.0 part of guar gum powder, and the method for preparing the high-strength fully-degradable multifunctional bio-based composite film comprises the following steps:
step (1): weighing the cationic modified starch in parts by weight, mixing with a proper amount of distilled water to prepare a cationic starch suspension, then adding the nano calcium carbonate in parts by weight, heating to 65 ℃, uniformly stirring and dispersing, then adding polyethylene glycol, continuously stirring until the polyethylene glycol is completely dissolved, and carrying out ultrasonic treatment on the mixed suspension for 10 min for later use.
Step (2): respectively weighing the guar gum powder and the xylitol powder in parts by weight, uniformly stirring and mixing, adding a certain amount of absolute ethyl alcohol, stirring and dispersing, slowly adding a proper amount of distilled water during continuous stirring, performing high-speed shearing and dispersing at a speed of 1500 r/min to obtain a colorless and transparent viscous liquid, mixing the obtained viscous liquid with the suspension prepared in the step (1), sequentially adding the carboxymethyl modified nano-cellulose and the chitosan, performing high-speed shearing and dispersing uniformly at a speed of 2500 r/min, and finally performing ultrasonic treatment on the mixed dispersion liquid for 30 min for later use.
And (3): weighing the polylactic acid particles in parts by weight in N, N-dimethylformamide, stirring by magnetic force at 65 ℃ until the polylactic acid particles are completely dissolved, slowly adding the mixed dispersion liquid obtained in the step (2) into the polylactic acid solution, uniformly dispersing by magnetic stirring, finally pouring a certain amount of mixed liquid into a glass culture dish, and setting the temperature of an oven to 85 ℃ for drying to obtain the high-strength multifunctional fully-degradable bio-based composite film.
Furthermore, the cation modified starch is modified by using quaternary ammonium salt as an etherifying agent, the carboxymethyl modified nano-cellulose is obtained by etherifying mechanically treated paper pulp fibers with chloroacetic acid, the diameter of the carboxymethyl modified nano-cellulose is 20 ~ 150 nm, the length of the carboxymethyl modified nano-cellulose is 1.0 ~ 6.0.0 mu m, and the molecular weight of polyethylene glycol is 6000.
Furthermore, the mass fraction of the cationic starch suspension in the step (1) is 5% ~ 6%, the mass fraction of the colorless and transparent viscous liquid obtained in the step (2) is 1.0% ~ 1.5.5%, the mixing volume ratio of absolute ethyl alcohol and distilled water in the liquid is 1:2, and the mass fraction of the polylactic acid solution in the step (3) is 4% ~ 6%.
Furthermore, the thickness of the high-strength full-degradable multifunctional bio-based composite film prepared by the invention is 0.08 mm.
The invention has the beneficial effects that: the raw materials used by the bio-based composite film are taken from nature and can be degraded, so that the bio-based composite film is a green and environment-friendly composite material; the raw material source is wide, which is beneficial to reducing the production cost and improving the industrial production benefit.
The invention constructs a compound system of cationic starch and nano calcium carbonate, realizes the coating of cationic modified starch on the nano calcium carbonate, reduces the surface energy of the nano calcium carbonate, and increases the wettability and the dispersibility of the nano calcium carbonate in water.
According to the invention, a certain amount of xylitol and guar gum are added, and under the action of ethanol, a space network structure is formed between the xylitol and the guar gum, so that the guar gum has better stability and dispersibility, and the characteristics of low solid content and high viscosity of the guar gum are fully exerted; certain carboxymethyl modified nano-cellulose is added, and good toughening and reinforcement effects are achieved on the polylactic acid material by utilizing the size effect, high elastic modulus and good impact resistance of the nano-cellulose.
The nano-cellulose modified by carboxymethylation can effectively improve the interface combination between polylactic acid molecules and fiber materials; in addition, the existence of chitosan and xylitol in the composite film can prevent bacteria from breeding on the surface of the composite material to a certain extent.
Detailed Description
The present invention is further illustrated by the following examples.
Example 1
Step (1): mixing 10 parts of cationic modified starch with 190 parts of distilled water to prepare cationic starch suspension, then heating 5 parts of nano calcium carbonate to 65 ℃, uniformly stirring and dispersing, then adding 2 parts of polyethylene glycol, continuously stirring until the polyethylene glycol is completely dissolved, and carrying out ultrasonic treatment on the mixed suspension for 10 min for later use.
Step (2): 1 part of guar gum powder and 5 parts of xylitol powder are stirred and mixed uniformly, 198 parts of absolute ethyl alcohol is added to be stirred and dispersed, 396 parts of distilled water is slowly added during continuous stirring, colorless and transparent viscous liquid is obtained through high-speed shearing and dispersion at the speed of 1500 r/min, the obtained viscous liquid is mixed with the suspension prepared in the step (1), the 5 parts of carboxymethyl modified nano-cellulose and 3 parts of chitosan are sequentially added, the uniform dispersion is obtained through high-speed shearing and dispersion at the speed of 2500 r/min, and finally the mixed dispersion liquid is subjected to ultrasound for 30 min for later use.
And (3): and (3) putting 100 parts of polylactic acid particles into N, N-dimethylformamide, and performing magnetic stirring at 65 ℃ until the polylactic acid particles are completely dissolved to obtain a polylactic acid solution with the mass fraction of 4%, then slowly adding the mixed dispersion liquid obtained in the step (2) into the polylactic acid solution, uniformly dispersing by magnetic stirring, finally pouring a certain amount of mixed liquid into a glass culture dish, and setting the temperature of an oven to 85 ℃ for drying to obtain the high-strength multifunctional fully-degradable bio-based composite film.
Example 2
Step (1): mixing 10 parts of cationic modified starch with 190 parts of distilled water to prepare cationic starch suspension, then heating 5 parts of nano calcium carbonate to 65 ℃, uniformly stirring and dispersing, then adding 2 parts of polyethylene glycol, continuously stirring until the polyethylene glycol is completely dissolved, and carrying out ultrasonic treatment on the mixed suspension for 10 min for later use; .
Step (2): 1 part of guar gum powder and 3 parts of xylitol powder are stirred and mixed uniformly, 120 parts of absolute ethyl alcohol is added to be stirred and dispersed, then 240 parts of distilled water is slowly added during continuous stirring, colorless and transparent viscous liquid is obtained through high-speed shearing and dispersion at the speed of 1500 r/min, the obtained viscous liquid is mixed with the suspension prepared in the step (1), 5 parts of carboxymethyl modified nano-cellulose and 3 parts of chitosan are sequentially added, the uniform dispersion is obtained through high-speed shearing and dispersion at the speed of 2500 r/min, and finally the mixed dispersion liquid is subjected to ultrasound for 30 min for later use.
And (3): and (3) putting 100 parts of polylactic acid particles into N, N-dimethylformamide, and performing magnetic stirring at 65 ℃ until the polylactic acid particles are completely dissolved to obtain a polylactic acid solution with the mass fraction of 6%, then slowly adding the mixed dispersion liquid obtained in the step (2) into the polylactic acid solution, uniformly dispersing by magnetic stirring, finally pouring a certain amount of mixed liquid into a glass culture dish, and setting the temperature of an oven to 85 ℃ for drying to obtain the high-strength multifunctional fully-degradable bio-based composite film.
Example 3
Step (1): mixing 15 parts of cation modified starch with 235 parts of distilled water to prepare cation starch suspension, then heating 5 parts of nano calcium carbonate to 65 ℃, stirring and dispersing uniformly, then adding 3 parts of polyethylene glycol, continuously stirring until the polyethylene glycol is completely dissolved, and carrying out ultrasonic treatment on the mixed suspension for 10 min for later use.
Step (2): 1 part of guar gum powder and 5 parts of xylitol powder are stirred and mixed uniformly, 198 parts of absolute ethyl alcohol is added to be stirred and dispersed, 396 parts of distilled water is slowly added during continuous stirring, colorless and transparent viscous liquid is obtained through high-speed shearing and dispersion at the speed of 1500 r/min, the obtained viscous liquid is mixed with the suspension prepared in the step (1), the 5 parts of carboxymethyl modified nano-cellulose and 3 parts of chitosan are sequentially added, the uniform dispersion is obtained through high-speed shearing and dispersion at the speed of 2500 r/min, and finally the mixed dispersion liquid is subjected to ultrasound for 30 min for later use.
And (3): and (3) putting 100 parts of polylactic acid particles into N, N-dimethylformamide, and performing magnetic stirring at 65 ℃ until the polylactic acid particles are completely dissolved to obtain a polylactic acid solution with the mass fraction of 5%, then slowly adding the mixed dispersion liquid obtained in the step (2) into the polylactic acid solution, uniformly dispersing by magnetic stirring, finally pouring a certain amount of mixed liquid into a glass culture dish, and setting the temperature of an oven to 85 ℃ for drying to obtain the high-strength multifunctional fully-degradable bio-based composite film.
In conclusion, the high-strength fully-degradable multifunctional bio-based composite film obtained by the invention not only has good heat resistance, barrier property and antibacterial property, but also combines excellent mechanical properties such as high impact resistance, high toughness, high elastic modulus and the like, and can be widely applied to the fields of agricultural mulching films, foods, cosmetic packaging materials, medical functional materials and the like.
Claims (8)
1. A preparation method of a high-strength full-degradable multifunctional bio-based composite film comprises the following raw materials in parts by weight: 100 parts of polylactic acid; 10-15 parts of cation modified starch; 5 parts of nano calcium carbonate; 3-5 parts of xylitol; 3-5 parts of carboxymethyl modified nano-cellulose; 1-3 parts of chitosan; 1-3 parts of polyethylene glycol; 0.5-1.0 part of guar gum powder; the method is characterized by comprising the following steps:
step (1): weighing the cationic modified starch in parts by weight, mixing with a proper amount of distilled water to prepare a cationic starch suspension, then adding the nano calcium carbonate in parts by weight, heating, stirring and dispersing uniformly, then adding polyethylene glycol, continuously stirring until the polyethylene glycol is completely dissolved, and carrying out ultrasonic treatment on the mixed suspension for later use;
step (2): respectively weighing the guar gum powder and the xylitol powder in parts by weight, uniformly stirring and mixing, adding a certain amount of absolute ethyl alcohol, stirring and dispersing, slowly adding a proper amount of distilled water during continuous stirring, performing high-speed shearing and dispersing to obtain a colorless and transparent viscous liquid, mixing the obtained viscous liquid with the suspension prepared in the step (1), sequentially adding the carboxymethyl modified nano-cellulose and the chitosan in parts by weight, uniformly shearing and dispersing at a high speed, and finally performing ultrasonic treatment on the mixed dispersion liquid for later use;
and (3): weighing the polylactic acid particles in parts by weight in N, N-dimethylformamide, stirring by magnetic force at a set temperature until the polylactic acid particles are completely dissolved, slowly adding the mixed dispersion liquid obtained in the step (2) into the polylactic acid solution, uniformly dispersing by magnetic stirring, finally pouring a certain amount of mixed liquid into a glass culture dish, and drying in an oven to obtain the high-strength multifunctional fully-degradable bio-based composite film.
2. The method for preparing the high-strength fully-degradable multifunctional bio-based composite film according to claim 1, wherein the cation modified starch is modified by using quaternary ammonium salt as an etherifying agent.
3. The method for preparing the high-strength fully-degradable multifunctional bio-based composite film according to claim 1, wherein the carboxymethyl modified nanocellulose is obtained by chloroacetic acid etherification of mechanically treated pulp fibers, and has a diameter of 20 ~ 150 nm and a length of 1.0 ~ 6.0.0 μm.
4. The high-strength fully-degradable multifunctional bio-based composite film and the preparation method thereof according to claim 1, wherein the molecular weight of the polyethylene glycol is 6000.
5. The preparation method of the high-strength fully-degradable multifunctional bio-based composite film according to claim 1, wherein the mass fraction of the cationic starch suspension in the step (1) is 5% ~ 6%, the temperature is raised to 65 ℃ after the nano calcium carbonate is added, and the obtained mixed suspension is subjected to ultrasonic treatment for 10 min for standby.
6. The preparation method of the high-strength fully-degradable multifunctional bio-based composite film according to claim 1, wherein the mass fraction of the colorless and transparent viscous liquid obtained in the step (2) is 1.0% ~ 1.5%, the mixing volume ratio of absolute ethyl alcohol and distilled water in the liquid is 1:2, wherein the colorless and transparent viscous liquid is obtained by high-speed shearing and dispersing at 1500 r/min, after the carboxymethyl modified nano-cellulose and chitosan are sequentially added, the high-speed shearing and dispersing are carried out at 2500 r/min, and finally the mixed dispersion liquid is subjected to ultrasound for 30 min for later use.
7. The method for preparing a high-strength fully-degradable multifunctional bio-based composite film according to claim 1, wherein the polylactic acid particles in the step (3) are dissolved completely in N, N-dimethylformamide by magnetic stirring at 65 ℃, the mixed dispersion obtained in the step (2) is slowly added into the polylactic acid solution, the mass fraction of the polylactic acid solution is 4% ~ 6%, and the oven temperature is set to 85 ℃.
8. The method for preparing a high-strength fully-degradable multifunctional bio-based composite film according to claim 1, wherein the thickness of the high-strength fully-degradable multifunctional bio-based composite film prepared in the step (3) is 0.08 mm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115260718A (en) * | 2022-07-22 | 2022-11-01 | 广东汇齐新材料有限公司 | High-strength high-antibacterial-property composite adhesive film and preparation method thereof |
| CN115304898A (en) * | 2022-09-09 | 2022-11-08 | 浙江瑞昶实业有限公司 | Preparation method of high-strength antibacterial high polymer material and application of high-strength antibacterial high polymer material in water emulsion bottle |
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