CN110183830B - Inorganic filler modified nano-cellulose and polylactic acid composite membrane and preparation thereof - Google Patents
Inorganic filler modified nano-cellulose and polylactic acid composite membrane and preparation thereof Download PDFInfo
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- CN110183830B CN110183830B CN201910485549.7A CN201910485549A CN110183830B CN 110183830 B CN110183830 B CN 110183830B CN 201910485549 A CN201910485549 A CN 201910485549A CN 110183830 B CN110183830 B CN 110183830B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B5/00—Preparation of cellulose esters of inorganic acids, e.g. phosphates
- C08B5/14—Cellulose sulfate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/08—Cellulose derivatives
- C08J2401/16—Esters of inorganic acids
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- C—CHEMISTRY; METALLURGY
- 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
- C08K3/28—Nitrogen-containing compounds
Abstract
The invention relates to an inorganic filler modified nano cellulose and polylactic acid composite membrane and a preparation method thereof. And blending the modified nano-cellulose and polylactic acid to prepare the nano-cellulose and polylactic acid composite film. The method provided by the invention is simple to operate and low in production cost, and the prepared film has high mechanical property, high barrier property, good antibacterial effect and good comprehensive performance, and can meet the application requirements in the fields of agricultural films, packaging films, food packaging materials and the like.
Description
Technical Field
The invention belongs to the field of packaging materials and preparation thereof, and particularly relates to an inorganic filler modified nano cellulose and polylactic acid composite film and preparation thereof.
Background
The development of petroleum products in large quantities to produce packaging materials has caused a huge environmental problem worldwide since the 20 th century. At present, the packaging film generally used by people is mainly polyethylene or polyvinyl chloride plastic film. A large amount of non-degradable plastic packages cause great pressure to the environment, and the whole ecology is threatened. Development of a novel green packaging material is an important task, and natural polymer materials are selected as the first choice, wherein starch, chitosan, lignin and the like are included in the research scope. Research on novel biomass materials has become a hotspot, and development of degradable packaging materials to relieve environmental pressure is gradually being paid attention to. Polylactic acid (PLA) is a new environment-friendly material which can be completely degraded, and lactic acid generated by hydrolysis is acidic and has certain antibacterial activity. However, since pure PLA cannot be widely commercialized due to its high price and high brittleness, it needs to be modified and plasticized to some extent to improve its performance and reduce its production cost. Cellulose, which is the most abundant material in nature, is an important biological material because of its abundant and natural source and many excellent physical and chemical properties. The nano cellulose (NCC) with a certain size is in a short rod shape and can be added into a material to reinforce the material. PLA is used as a matrix, NCC is used as a filler, the aim of modifying PLA can be achieved, the defects of the material are made up, and the degradable packaging material with high mechanical property and high barrier property is prepared. The nano-silver modified nano-cellulose with obvious antibacterial effect can increase the antibacterial effect of the composite film and expand the application range of the film. CN103483786A discloses a fully biodegradable composite membrane filled with nano silver/cellulose nanocrystalline composite particles and a preparation method thereof, but the preparation of the acid is complex, and the dispersion effect of the composite particles in the polymer is not good.
Disclosure of Invention
The invention aims to solve the technical problem of providing an inorganic filler modified nano cellulose and polylactic acid composite film and a preparation method thereof, and overcomes the defect that the existing inorganic particles are not uniformly dispersed in a high polymer.
The inorganic filler modified nano-cellulose and polylactic acid composite film is characterized by comprising, by weight, 85-100 parts of polylactic acid, 2.5-4 parts of nano-cellulose and 2-4 parts of silver nitrate.
The invention relates to a preparation method of an inorganic filler modified nano cellulose and polylactic acid composite membrane, which comprises the following steps:
(1) adding sulfuric acid into microcrystalline cellulose, stirring under the condition of constant-temperature oil bath, adding distilled water for dilution, standing, pouring out upper-layer acid liquor, centrifugally washing residual solution, putting the obtained concentrated nano-cellulose suspension into a vacuum freeze dryer, and freeze-drying to obtain nano-cellulose; wherein the mass ratio of the microcrystalline cellulose to the sulfuric acid is 8-15: 0.1-0.3;
(2) adding water into the nano-cellulose, performing ultrasonic dispersion, adding a silver nitrate solution, adding water to obtain a mixed solution, performing magnetic stirring under the condition of constant-temperature oil bath, adjusting and maintaining the pH value, performing centrifugal separation, collecting precipitate, and freeze-drying the precipitate to obtain modified nano-cellulose;
(3) dissolving polylactic acid in a solvent, stirring at room temperature until the polylactic acid is completely dissolved, adding modified nano-cellulose, stirring by a high-pressure homogenizer, performing ultrasonic dispersion, uniformly mixing the solution by ultrasonic dispersion, pouring the mixture into a template, drying at room temperature, and removing the film to obtain the inorganic filler modified nano-cellulose and polylactic acid composite film.
Preferred modes of the above production methods:
the grain size of the microcrystalline cellulose in the step (1) is 250 μm (product number C104844, Shanghai Aladdin Biotechnology Co., Ltd.).
The temperature of the constant-temperature oil bath in the step (1) is 35-55 ℃; stirring for 0.5-1h by magnetic stirring; standing for 1-2 d; centrifugally washing until the pH value is 6-7.
The volume percentage concentration of the sulfuric acid in the step (1) is 64-65%.
The ultrasonic dispersion time in the step (2) is 20-30 min; oil bath at constant temperature of 70-80 ℃.
The concentration of the silver nitrate solution in the step (2) is 0.5-0.7 mol/L.
The step (2) of adjusting the pH value and keeping the pH value specifically comprises the following steps: and adjusting the pH value by using a sodium hydroxide solution and keeping the pH value for 15-30min, wherein the concentration of the sodium hydroxide solution is 1mol/L, the pH value is 10-12.
The weight average molecular weight of the polylactic acid in the step (3) is 8.9 multiplied by 105(Ingeo 6201D, NatureWorks); the solvent is dichloromethane; the template is a polytetrafluoroethylene template.
The stirring speed of the high-pressure homogenizer in the step (3) is 8000-; drying at room temperature for 12-24 h.
The inorganic filler modified nano-cellulose and polylactic acid composite film prepared by the method is provided.
The invention relates to an application of an inorganic filler modified nano-cellulose and polylactic acid composite membrane.
Advantageous effects
The method provided by the invention is simple to operate and low in production cost, and the prepared film has high mechanical property, high barrier property, good antibacterial effect and good comprehensive performance, and can meet the application requirements in the fields of agricultural films, packaging films, food packaging materials and the like.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The microcrystalline cellulose had a particle size of 250 μm (product No. C104844, Shanghai Aladdin Biotechnology Co., Ltd.)
The weight average molecular weight of the polylactic acid is 8.9X 105(Ingeo 6201D，NatureWorks)
Example 1
Step 1: preparation of nanocellulose
10 parts of microcrystalline cellulose are weighed and 0.15 part of 64% -65% sulfuric acid solution is slowly added. Magnetically stirring for 1h under the condition of constant-temperature oil bath at 35-55 ℃. Adding a large amount of distilled water to dilute the solution, standing for 1-2 days, and pouring off the upper layer acid solution. And (4) centrifugally washing the residual solution until the pH value is 6-7, putting the obtained concentrated nano cellulose suspension into a vacuum freeze dryer, and freeze-drying to obtain nano cellulose powder.
Step 2: modification of nanocellulose
3 parts of nano cellulose powder is weighed, 5mL of deionized water is added, and ultrasonic dispersion is carried out for 20-30 min. Adding 30mL0.5mol/L silver nitrate solution, adding 5mL deionized water to prepare 40mL mixed solution, and magnetically stirring under the condition of constant-temperature oil bath at 70-80 ℃. Slowly adding 1mol/L sodium hydroxide solution to adjust pH value to 10-12 and keeping for 15-30 min. And (4) carrying out centrifugal separation, collecting the precipitate, and carrying out freeze drying on the precipitate to obtain the modified nano cellulose.
And step 3: preparation of nano-cellulose and polylactic acid composite film
90 parts of polylactic acid is weighed, 30mL of dichloromethane is added, and the solution is magnetically stirred at room temperature until the polylactic acid is completely dissolved. Adding modified nano cellulose, stirring at 8000r/min with a high-pressure homogenizer for 10min, and ultrasonically dispersing for 10min to uniformly mix the solution. The solution was poured into a teflon template and dried at room temperature for 24 h. And (5) removing the film to obtain the composite film.
Example 2
Step 1: preparation of nanocellulose
12 parts of microcrystalline cellulose are weighed and 0.2 part of 64% -65% sulfuric acid solution is slowly added. Magnetically stirring for 1h under the condition of constant-temperature oil bath at 35-55 ℃. Adding a large amount of distilled water to dilute the solution, standing for 1-2 days, and pouring off the upper layer acid solution. And (4) centrifugally washing the residual solution until the pH value is 6-7, putting the obtained concentrated nano cellulose suspension into a vacuum freeze dryer, and freeze-drying to obtain nano cellulose powder.
Step 2: modification of nanocellulose
3.3 parts of nano cellulose powder is weighed, 7mL of deionized water is added, and ultrasonic dispersion is carried out for 20-30 min. Adding 35mL0.5mol/L silver nitrate solution, adding 7mL deionized water to prepare 49 mixed solution, and magnetically stirring under the condition of constant-temperature oil bath at 70-80 ℃. Slowly adding 1mol/L sodium hydroxide solution to adjust pH value to 10-12 and keeping for 15-30 min. And (4) carrying out centrifugal separation, collecting the precipitate, and carrying out freeze drying on the precipitate to obtain the modified nano cellulose.
And step 3: preparation of nano-cellulose and polylactic acid composite film
95% polylactic acid was weighed, 40mL of methylene chloride was added, and the solution was magnetically stirred at room temperature until the polylactic acid had completely dissolved. Adding modified nano cellulose, stirring at 8500 r/min with a high-pressure homogenizer for 10min, and ultrasonically dispersing for 10min to uniformly mix the solution. The solution was poured into a teflon template and dried at room temperature for 24 h. And (5) removing the film to obtain the composite film.
Example 3
Step 1: preparation of nanocellulose
13.5 parts of microcrystalline cellulose is weighed and 0.25 part of 64-65% sulfuric acid solution is slowly added. Magnetically stirring for 1h under the condition of constant-temperature oil bath at 35-55 ℃. Adding a large amount of distilled water to dilute the solution, standing for 1-2 days, and pouring off the upper layer acid solution. And (4) centrifugally washing the residual solution until the pH value is 6-7, putting the obtained concentrated nano cellulose suspension into a vacuum freeze dryer, and freeze-drying to obtain nano cellulose powder.
Step 2: modification of nanocellulose
3.6 parts of nano cellulose powder is weighed, 10mL of deionized water is added, and ultrasonic dispersion is carried out for 20-30 min. Adding 35mL0.5mol/L silver nitrate solution, adding 10mL deionized water to prepare 55mL mixed solution, and magnetically stirring at the constant temperature of 70-80 ℃ under the condition of oil bath. Slowly adding 1mol/L sodium hydroxide solution to adjust pH value to 10-12 and keeping for 15-30 min. And (4) carrying out centrifugal separation, collecting the precipitate, and carrying out freeze drying on the precipitate to obtain the modified nano cellulose.
And step 3: preparation of nano-cellulose and polylactic acid composite film
96 portions of polylactic acid were weighed, 50mL of methylene chloride was added, and the solution was magnetically stirred at room temperature until all polylactic acid had dissolved. Adding modified nano cellulose, stirring at 9000r/min with a high-pressure homogenizer for 10min, and ultrasonically dispersing for 10min to uniformly mix the solution. The solution was poured into a teflon template and dried at room temperature for 24 h. And (5) removing the film to obtain the composite film.
Example 4
Step 1: preparation of nanocellulose
14.5 parts of microcrystalline cellulose are weighed and 0.3 part of 64% -65% sulfuric acid solution is slowly added. Magnetically stirring for 1h under the condition of constant-temperature oil bath at 35-55 ℃. Adding a large amount of distilled water to dilute the solution, standing for 1-2 days, and pouring off the upper layer acid solution. And (4) centrifugally washing the residual solution until the pH value is 6-7, putting the obtained concentrated nano cellulose suspension into a vacuum freeze dryer, and freeze-drying to obtain nano cellulose powder.
Step 2: modification of nanocellulose
3.8 parts of nano cellulose powder is weighed, 12mL of deionized water is added, and ultrasonic dispersion is carried out for 20-30 min. Adding 35mL0.5mol/L silver nitrate solution, adding 12mL deionized water to prepare 59mL mixed solution, and magnetically stirring at the constant temperature of 70-80 ℃ under the condition of oil bath. Slowly adding 1mol/L sodium hydroxide solution to adjust pH value to 10-12 and keeping for 15-30 min. And (4) carrying out centrifugal separation, collecting the precipitate, and carrying out freeze drying on the precipitate to obtain the modified nano cellulose.
And step 3: preparation of nano-cellulose and polylactic acid composite film
100 portions of polylactic acid are weighed, 60mL of methylene chloride is added, and the solution is magnetically stirred at room temperature until all the polylactic acid is dissolved. Adding modified nano cellulose, stirring at 10000r/min with a high-pressure homogenizer for 10min, and ultrasonically dispersing for 10min to uniformly mix the solution. The solution was poured into a teflon template and dried at room temperature for 24 h. And (5) removing the film to obtain the composite film.
In order to fully prove that the polylactic acid/nano cellulose/silver composite material obtained by the preparation method has excellent performance, the materials prepared in the examples 1, 2, 3 and 4 are selected and subjected to tensile property test and moisture permeability barrier property test.
Testing one:
tensile properties were measured using a general-purpose mechanical tester (H5K-S, Hounsfield) with a gauge length of 30mm and a test speed set at 10 mm/min.
The specific test results are shown in the following table:
| item | Blank space | Example 1 | Example 2 | Example 3 | Example 4 |
| Tensile strength/MPa | 35 | 42 | 50 | 57 | 53 |
According to the data in the table, the tensile strength of the polylactic acid/nano cellulose/hydroxyapatite composite material is improved. The tensile properties test above was carried out in accordance with the determination of the tensile properties of the plastics of GB/T1040-.
And (2) testing:
according to GB1037-88, pure polylactic acid and polylactic acid/nano cellulose/silver composite materials obtained in example 1, example 2, example 3 and example 4 are respectively subjected to moisture permeability barrier property test by a moisture permeability tester.
The specific test results are shown in the following table:
| item | Blank space | Example 1 | Example 2 | Example 3 | Example 4 |
| Moisture permeability/g/(m 2, 24h) | 121.5 | 93.6 | 60.5 | 24.3 | 52.7 |
According to the data in the table, the moisture permeability of the polylactic acid/nano cellulose/silver composite material is obviously reduced compared with that of pure polylactic acid, which indicates that the moisture permeability barrier property of the polylactic acid/nano cellulose/silver composite material is far better than that of pure polylactic acid.
Claims (9)
1. An inorganic filler modified nano cellulose and polylactic acid composite film with moisture permeable and barrier properties is characterized in that raw material components comprise, by weight, 85-100 parts of polylactic acid, 2.5-4 parts of nano cellulose and 2-4 parts of silver nitrate;
wherein the composite membrane is prepared by the following method:
(1) adding sulfuric acid into microcrystalline cellulose, stirring under the condition of constant-temperature oil bath, diluting, standing, centrifugally washing, and freeze-drying to obtain nano cellulose;
(2) adding water into the nano-cellulose, performing ultrasonic dispersion, adding a silver nitrate solution, adding water to obtain a mixed solution, performing magnetic stirring under the condition of constant-temperature oil bath, adjusting and maintaining the pH value, performing centrifugal separation, and performing freeze drying to obtain modified nano-cellulose;
(3) dissolving polylactic acid in a solvent, stirring and dissolving, adding modified nano-cellulose, stirring by a high-speed homogenizing stirrer, performing ultrasonic dispersion, then pouring into a template, and drying at room temperature to obtain the inorganic filler modified nano-cellulose and polylactic acid composite membrane.
2. A preparation method of the inorganic filler modified nano cellulose and polylactic acid composite film with moisture permeable barrier property of claim 1, which comprises the following steps:
(1) adding sulfuric acid into microcrystalline cellulose, stirring under the condition of constant-temperature oil bath, diluting, standing, centrifugally washing, and freeze-drying to obtain nano cellulose;
(2) adding water into the nano-cellulose, performing ultrasonic dispersion, adding a silver nitrate solution, adding water to obtain a mixed solution, performing magnetic stirring under the condition of constant-temperature oil bath, adjusting and maintaining the pH value, performing centrifugal separation, and performing freeze drying to obtain modified nano-cellulose;
(3) dissolving polylactic acid in a solvent, stirring and dissolving, adding modified nano-cellulose, stirring by a high-speed homogenizing stirrer, performing ultrasonic dispersion, then pouring into a template, and drying at room temperature to obtain the inorganic filler modified nano-cellulose and polylactic acid composite membrane.
3. The preparation method according to claim 2, wherein the temperature of the constant-temperature oil bath in the step (1) is 35-55 ℃; stirring for 0.5-1h by magnetic stirring; standing for 1-2 d; centrifugally washing until the pH value is 6-7.
4. The preparation method according to claim 2, wherein the ultrasonic dispersion time in the step (2) is 20-30 min; oil bath at constant temperature of 70-80 ℃.
5. The method according to claim 2, wherein the concentration of the silver nitrate solution in the step (2) is 0.5 to 0.7 mol/L.
6. The method according to claim 2, wherein the step (2) of adjusting the pH and maintaining is specifically: and adjusting the pH value by using a sodium hydroxide solution and keeping the pH value for 15-30min, wherein the concentration of the sodium hydroxide solution is 1mol/L, the pH value is 10-12.
7. The method according to claim 2, wherein the weight average molecular weight of the polylactic acid in the step (3) is 8.9X 105(ii) a The solvent is dichloromethane; the template is a polytetrafluoroethylene template.
8. The preparation method according to claim 2, wherein the stirring speed of the high-pressure homogenizer in the step (3) is 8000-10000r/min, and the stirring and ultrasonic dispersion time of the high-pressure homogenizer is 5-15 min; drying at room temperature for 12-24 h.
9. The application of the inorganic filler modified nanocellulose and polylactic acid composite film with moisture-permeable barrier property of claim 1 in the fields of agricultural films, packaging films and food packaging materials.
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