CN113215860B - Lignin/cellulose composite film and preparation method thereof - Google Patents
Lignin/cellulose composite film and preparation method thereof Download PDFInfo
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B31—MAKING ARTICLES OF PAPER, CARDBOARD OR MATERIAL WORKED IN A MANNER ANALOGOUS TO PAPER; WORKING PAPER, CARDBOARD OR MATERIAL WORKED IN A MANNER ANALOGOUS TO PAPER
- B31F—MECHANICAL WORKING OR DEFORMATION OF PAPER, CARDBOARD OR MATERIAL WORKED IN A MANNER ANALOGOUS TO PAPER
- B31F1/00—Mechanical deformation without removing material, e.g. in combination with laminating
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H23/00—Processes or apparatus for adding material to the pulp or to the paper
- D21H23/02—Processes or apparatus for adding material to the pulp or to the paper characterised by the manner in which substances are added
- D21H23/22—Addition to the formed paper
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Abstract
The invention relates to the field of film preparation, and discloses a lignin/cellulose composite film and a preparation method thereof, wherein the formula of the film comprises 74.7-78.9% of cellulose, 19.5-22.8% of lignin and 1.6-2.5% of zinc chloride in percentage by weight. The method comprises (1) dissolving lignin powder in acetone solution to obtain lignin acetone solution; (2) preparing a cellulose solution, performing ultrasonic treatment to obtain the cellulose solution, and drying to obtain ultrasonic cellulose paper; (3) dissolving zinc chloride in distilled water to obtain a zinc chloride solution; (4) soaking the ultrasonic cellulose paper in the step (2) in the zinc chloride solution in the step (3), washing, and soaking in the lignin/acetone solution in the step (1); (5) and (4) carrying out hot pressing on the ultrasonic cellulose paper impregnated with the lignin/acetone solution in the step (4), and cooling to obtain the lignin/cellulose composite film. The invention has the advantages of high strength and toughness of the composite film of the lignin and the cellulose, simple operation and low cost.
Description
Technical Field
The invention belongs to the field of film preparation, and particularly relates to a lignin/cellulose composite film and a preparation method thereof.
Background
Cellulose is a natural polymer with the largest reserve on the earth, and has the advantages of good mechanical property, no toxicity, degradability and the like. However, the hydrophilicity and lack of versatility of cellulose have limited the use of cellulose in a wider range. The lignin as another natural polymer with huge reserves has the advantages of no toxicity, good water resistance, ultraviolet resistance, good thermal stability and the like, and can well make up the defects of cellulose. Due to poor compatibility of lignin and cellulose re-compounding, the current methods for improving the compatibility of lignin and cellulose are mainly limited to chemical modification and the like. But chemical modification is expensive on one hand, and on the other hand, toxic substances are generated, so that green utilization of biomass is not facilitated. More importantly, the current means of improved compatibility is difficult to achieve simultaneous improvement in toughness and strength, often at the expense of material toughness.
Disclosure of Invention
In order to solve the problem that the toughness and the strength are difficult to be simultaneously improved in the compatibility improvement process of the lignin/cellulose composite film in the prior art, the invention provides the lignin/cellulose composite film and the preparation method thereof.
The invention adopts the specific scheme that: a composite lignin/cellulose film is prepared from cellulose (74.7-78.9 wt.%), lignin (19.5-22.8 wt.%) and zinc chloride (1.6-2.5 wt.%).
In another aspect, the present invention provides a method for preparing a lignin/cellulose composite film, comprising the steps of:
(1) dissolving lignin powder in an acetone solution, and centrifuging to remove precipitates to obtain a lignin acetone solution;
(2) preparing a cellulose solution, performing ultrasonic treatment to obtain the cellulose solution, and drying to obtain ultrasonic cellulose paper;
(3) dissolving zinc chloride in distilled water to obtain a zinc chloride solution;
(4) soaking the ultrasonic cellulose paper in the step (2) in the zinc chloride solution in the step (3), washing, and soaking in the lignin/acetone solution in the step (1);
(5) and (4) carrying out hot pressing on the ultrasonic cellulose paper impregnated with the lignin/acetone solution in the step (4), and cooling to obtain the lignin/cellulose composite film.
The mass fraction of the cellulose solution prepared in the step (2) is 0.5-1%.
The ultrasonic condition in the step (2) is 700-800W of power ultrasonic for 6-8 hours.
The drying condition in the step (2) is that the drying is carried out for 30-60 minutes under the pressure of 3-8MPa and the hot pressing temperature of 110-120 ℃ after the water is squeezed on a flattening machine.
And (4) dissolving zinc chloride in distilled water, and adding a hydrochloric acid solution to prepare a zinc chloride solution.
The washing condition in the step (4) is that the volume ratio of the washing solution to the washing solution is 1: 1-1: 2, washing in an ethanol/water mixed solution, and soaking in alcohol for 30-45 minutes.
The hot pressing condition of the ultrasonic cellulose paper impregnated with the lignin/acetone solution in the step (5) is that the hot pressing is carried out for 2 to 2.5 hours at the temperature of 110 ℃ and 120 ℃ under the pressure of 8 to 10 MPa.
The time for soaking in the step (4) is 20-24 h.
The soaking time in the step (4) is 20-24 h.
Compared with the prior art, the invention has the following beneficial effects:
the invention utilizes zinc chloride to construct a sacrificial network formed by combining hydrogen bonds and coordination bonds on a lignin/cellulose interface so as to improve the compatibility between lignin and cellulose and improve the strength and toughness at the same time. Compared with the traditional method for improving the performance of the cellulose, the method has the advantages of simple operation, low cost and no generation of toxic and harmful chemical substances, and is a green, simple and convenient means for improving the performance of the cellulose.
Detailed Description
The onset is further described below in conjunction with the detailed description.
A composite lignin/cellulose film is prepared from cellulose (74.7-78.9 wt.%), lignin (19.5-22.8 wt.%) and zinc chloride (1.6-2.5 wt.%).
In another aspect, the present invention provides a method for preparing a lignin/cellulose composite film, comprising the steps of:
(1) dissolving lignin powder in an acetone solution, and centrifuging to remove precipitates to obtain a lignin acetone solution;
(2) preparing a cellulose solution, performing ultrasonic treatment to obtain the cellulose solution, and drying to obtain ultrasonic cellulose paper;
(3) dissolving zinc chloride in distilled water to obtain a zinc chloride solution;
(4) soaking the ultrasonic cellulose paper in the step (2) in the zinc chloride solution in the step (3), washing, and soaking in the lignin/acetone solution in the step (1);
(5) and (4) carrying out hot pressing on the ultrasonic cellulose paper impregnated with the lignin/acetone solution in the step (4), and cooling to obtain the lignin/cellulose composite film.
The mass fraction of the cellulose solution prepared in the step (2) is 0.5-1%.
The ultrasonic condition in the step (2) is 700-800W of power ultrasonic for 6-8 hours.
The drying condition in the step (2) is that the drying is carried out for 30-60 minutes under the pressure of 3-8MPa and the hot pressing temperature of 110-120 ℃ after the water is squeezed on a flattening machine.
And (4) dissolving zinc chloride in distilled water, and adding a hydrochloric acid solution to prepare a zinc chloride solution. Adding 20-30 g of hydrochloric acid solution with the mass fraction of 1% to prevent the zinc chloride from hydrolyzing and precipitating
The washing condition in the step (4) is that the volume ratio of the washing solution to the washing solution is 1: 1-1: 2, washing in an ethanol/water mixed solution, and soaking in alcohol for 30-45 minutes.
The hot pressing condition of the ultrasonic cellulose paper impregnated with the lignin/acetone solution in the step (5) is that the hot pressing is carried out for 2 to 2.5 hours at the temperature of 110 ℃ and 120 ℃ under the pressure of 8 to 10 MPa.
The time for soaking in the step (4) is 20-24 h.
The soaking time in the step (4) is 20-24 h.
According to the invention, an energy sacrifice network is constructed on a lignin/cellulose interface by using zinc chloride to improve the compatibility between lignin and cellulose, and ultrasonic treatment on the cellulose is combined, so that the strength and toughness are improved at the same time, and the technical resistance that the strength and toughness are difficult to improve while the compatibility between the lignin and the cellulose is improved in the prior art is overcome.
The sacrificial bond refers to a bond which is broken before stronger bond deformation failure, and is a key mechanism of tough mechanical properties of natural biomaterials (such as mussel shells and the like). Inspired by the toughness mechanism of biological materials in the nature, the invention utilizes zinc chloride to construct a sacrificial network formed by combining hydrogen bonds and coordination bonds on a lignin/cellulose interface so as to improve the compatibility between lignin and cellulose and realize the improvement of strength and toughness at the same time. The reason mechanism that the sacrificial network endows the material with the strength and toughness is that at the initial stage of loading of the composite film, hydrogen bonds of lignin and cellulose are firstly broken in the form of sacrificial bonds, and along with continuous loading of the composite film, coordinate bonds constructed by a zinc chloride and lignin/cellulose composite system are gradually broken, so that a large amount of energy is finally dissipated, and the strength and toughness are improved at the same time. Compared with the traditional method for improving the performance of the cellulose, the method has the advantages of simple operation, low cost and no generation of toxic and harmful chemical substances, and is a green, simple and convenient means for improving the performance of the cellulose.
Example 1
1. Dissolving 4.0 g lignin powder in 150 ml acetone solution, continuously stirring for 10min, then performing ultrasonic treatment at 600 watts for 1h, finally centrifuging the solution at 5000rpm for 8 min, and removing precipitate to obtain 30 mg/ml lignin acetone solution;
2. preparing a cellulose solution with the mass fraction of 0.5%, and then carrying out ultrasonic treatment for 6 hours at the power of 800W to obtain an ultrasonic cellulose solution;
3. weighing 100 g of cellulose solution after ultrasonic treatment, carrying out vacuum filtration, then squeezing water on a flattening machine, and finally carrying out hot-pressing drying at 110 ℃ for 30 minutes under the pressure of 8MPa to obtain ultrasonic cellulose paper;
4. dissolving 15-30 g of zinc chloride in 100 g of distilled water, and then adding 20 g of hydrochloric acid solution with the mass fraction of 1% to prevent the zinc chloride from hydrolysis and precipitation to prepare zinc chloride solution;
5. the resulting ultrasonic cellulose paper was immersed in a zinc chloride solution for 20h, followed by heating at a volume ratio of 1: 1, cleaning the mixed solution of ethanol and water to remove redundant zinc chloride and hydrochloric acid, soaking the mixed solution in pure alcohol for 30 minutes to perform solvent exchange to remove water, and finally soaking the mixed solution in 30 mg/ml lignin/acetone solution for 20 hours;
6. the ultrasonic cellulose paper impregnated with the lignin/acetone solution is hot-pressed for 2 to 2.5 hours at the temperature of 110-120 ℃ under the pressure of 8 to 10MPa, and finally the lignin/cellulose composite film with high strength and high toughness is obtained.
In example 1, the lignin/cellulose composite film consisted of 78.9% by weight of cellulose, 19.5% by weight of lignin, and 1.6% by weight of zinc chloride.
Example 2
1. Dissolving 6.0 g lignin powder in 200 ml acetone solution, continuously stirring for 15 minutes, then carrying out ultrasonic treatment for 1 hour at 600 watts, finally centrifuging the solution for 10 minutes at the speed of 5000 r/min, and removing precipitates to obtain 30 mg/ml lignin acetone solution;
2. preparing a cellulose solution with the mass fraction of 1%, and then carrying out ultrasonic treatment for 6 hours at the power of 800W to obtain an ultrasonic cellulose solution;
3. weighing 100 g of cellulose solution after ultrasonic treatment, carrying out vacuum filtration, then squeezing water on a flattening machine, and finally carrying out hot-pressing drying at 120 ℃ for 60 minutes under the pressure of 3MPa to obtain ultrasonic cellulose paper;
4. dissolving 30 g of zinc chloride in 200 g of distilled water, and then adding 30 g of hydrochloric acid solution with the mass fraction of 1% to prevent the zinc chloride from hydrolysis and precipitation to prepare a zinc chloride solution;
5. the resulting ultrasonic cellulose paper was immersed in a zinc chloride solution for 24h, followed by heating at a volume ratio of 1: 2, cleaning the mixed solution of ethanol and water to remove redundant zinc chloride and hydrochloric acid, soaking the mixed solution in pure alcohol for 45 minutes to perform solvent exchange to remove water, and finally soaking the mixed solution in 30 mg/ml lignin/acetone solution for 24 hours;
6. and hot-pressing the ultrasonic cellulose paper impregnated with the lignin/acetone solution at 120 ℃ under 10MPa for 2.5 hours to finally obtain the high-strength and high-toughness lignin/cellulose composite film.
In example 2, the lignin/cellulose composite film was composed of 75.1% by weight of cellulose, 23.2% by weight of lignin, and 1.7% by weight of zinc chloride.
Example 3
1. Dissolving 5.0 g lignin powder in 180 ml acetone solution, continuously stirring for 12 minutes, then carrying out ultrasonic treatment for 1 hour at 600 watts, finally centrifuging the solution for 9 minutes at the speed of 5000 r/min, and removing precipitates to obtain 30 mg/ml lignin acetone solution;
2. preparing a cellulose solution with the mass fraction of 0.8%, and then carrying out ultrasonic treatment for 6 hours at the power of 800W to obtain an ultrasonic cellulose solution;
3. weighing 100 g of cellulose solution after ultrasonic treatment, carrying out vacuum filtration, then squeezing water on a flattening machine, and finally carrying out hot-pressing drying at 115 ℃ for 45 minutes under the pressure of 5MPa to obtain ultrasonic cellulose paper;
4. dissolving 25 g of zinc chloride in 180 g of distilled water, and then adding 25 g of hydrochloric acid solution with the mass fraction of 1% to prevent the zinc chloride from hydrolysis and precipitation to prepare a zinc chloride solution;
5. the resulting ultrasonic cellulose paper was dipped in a zinc chloride solution for 22h, followed by mixing in a volume ratio of 1: 1.5, cleaning the mixed solution of ethanol and water to remove redundant zinc chloride and hydrochloric acid, soaking the mixed solution in pure alcohol for 40 minutes to perform solvent exchange to remove water, and finally soaking the mixed solution in 30 mg/ml lignin/acetone solution for 22 hours;
6. and (3) hot-pressing the ultrasonic cellulose paper impregnated with the lignin/acetone solution at 115 ℃ under 9MPa for 2.3 hours to finally obtain the high-strength and high-toughness lignin/cellulose composite film.
In example 3, the lignin/cellulose composite film consisted of 74.7% by weight of cellulose, 22.8% by weight of lignin, and 2.5% by weight of zinc chloride.
Example 4
1. Dissolving 6.0 g lignin powder in 200 ml acetone solution, continuously stirring for 15 minutes, then carrying out ultrasonic treatment for 1 hour at 600 watts, finally centrifuging the solution for 10 minutes at the speed of 5000 r/min, and removing precipitates to obtain 30 mg/ml lignin acetone solution;
2. preparing a cellulose solution with the mass fraction of 1%, and then carrying out ultrasonic treatment for 6 hours at the power of 800W to obtain an ultrasonic cellulose solution;
3. weighing 100 g of cellulose solution after ultrasonic treatment, carrying out vacuum filtration, then squeezing water on a flattening machine, and finally carrying out hot-pressing drying at 120 ℃ for 60 minutes under the pressure of 3MPa to obtain ultrasonic cellulose paper;
4. dissolving 30 g of zinc chloride in 200 g of distilled water, and then adding 30 g of hydrochloric acid solution with the mass fraction of 1% to prevent the zinc chloride from hydrolysis and precipitation to prepare a zinc chloride solution;
5. the resulting ultrasonic cellulose paper was dipped in a zinc chloride solution for 21h, followed by mixing in a volume ratio of 1: 1.5, cleaning the mixed solution of ethanol and water to remove redundant zinc chloride and hydrochloric acid, soaking the mixed solution in pure alcohol for 45 minutes to carry out solvent exchange to remove water, and finally soaking the mixed solution in 30 mg/ml lignin/acetone solution for 21 hours;
6. and hot-pressing the ultrasonic cellulose paper impregnated with the lignin/acetone solution at 120 ℃ under 10MPa for 2.5 hours to finally obtain the high-strength and high-toughness lignin/cellulose composite film.
In example 4, the lignin/cellulose composite film comprised 75.0% by weight of cellulose, 22.2% by weight of lignin, and 1.6% by weight of zinc chloride.
Comparative example 1: a pure cellulose film.
Comparative example 2: a lignin/cellulose composite film without zinc chloride treatment.
And (3) testing mechanical properties:
all test specimens were equilibrated for one day at 25 ℃ and 50% relative humidity in accordance with GBT 10739-.
For tensile property testing, test specimens were cut into 10mm by 50mm rectangular bars. Tensile properties were measured on a universal mechanical testing machine (CMT5504, MTS Systems Co. Ltd, China) with a 1-kN sensor at a tensile rate of 5 mm/min.
For the folding endurance test, test specimens were cut into rectangular strips of 100mm 15mm and tested on an MIT paper folding endurance Tester (IMT-205A, International Material Tester, China) at a test tension of 4.9N.
Water absorption test:
and cutting the film into square test pieces with the thickness of 10mm by 10mm, soaking the square test pieces in pure water for 10min, and calculating the water absorption of the film according to the change of the mass of the film.
Optical testing:
optical testing is carried out on a ultraviolet-visible light spectrum analyzer (persee, China) to test the transmittance of the film at different wavelengths, the tested wavelength range is 200 and 800nm, and the data of the method is based on the transmittance of the film when the wavelength of light is 400 nm.
The test results are shown in the following table:
| test object | Tensile strength | Modulus of elasticity in tension | Elongation at tensile break | Number of folding endurance |
| Example 1 | 125.96MPa | 4.18GPa | 13.01％ | 2415 |
| Example 2 | 138.14MPa | 4.74GPa | 14.78％ | 2687 |
| Example 3 | 150.32MPa | 5.3GPa | 16.55％ | 2959 |
| Example 4 | 138.32MPa | 4.71GPa | 14.50％ | 2513 |
| Comparative example 1 | 40.48MPa | 2.85GPa | 11.16％ | —— |
| Comparative example 2 | 75.79MPa | 4.32GPa | 6.43％ | 1149 |
As can be seen from the above table, in the best example 3, compared with comparative examples 1 and 2, the tensile strength, the tensile elastic modulus and the tensile elongation at break are all significantly improved, the folding resistance is improved by about 133.8%, and the strength and the toughness of the film prepared by the method are both significantly improved.
And (3) testing the oxidation resistance:
the oxidation resistance comparison was measured by testing the free radical scavenging rate, which was tested as follows:
1. preparing DPPH (1, 1-diphenyl-2-trinitrophenylhydrazine) and DMF (N, N-dimethylformamide) into a DPPH/DMF solution with the concentration of 25 mg/L; 2. stirring 50mg of the film sample in 10ml of DMF at room temperature for 24 hours, and then centrifuging the film sample in a centrifuge at the rotating speed of 5000rpm for 10min to obtain a supernatant to obtain a film extract; 3. mixing 2ml of the film extract with 2ml of prepared DPPH/DMF solution with the concentration of 25mg/L, and reacting for 1 hour at room temperature in a dark place; 4. after the reaction was kept away from light, 2ml of the reacted solution was subjected to an ultraviolet-visible spectrophotometer (Persee, China) to measure the absorbance (A) of the solution at 517nmSample (I)) And calculating the clearance rate of free radicals by using the formula 1 as a basis for measuring the oxidation resistance. A. theSample (I)The absorbance of the thin film extract at 517nm, AControlAs a control group solvent(DMF) absorbance at 517 nm.
Radical scavenging rate (%) ═ aControl-ASample (I))*100/AControl(formula 1)
The results are shown in the following table, calculated according to equation 1:
| test object | Water absorption rate | Ultraviolet light transmittance (400nm) | Free radical scavenging rate |
| Example 1 | 29.7％ | 0％ | 37.2％ |
| Example 2 | 28.2％ | 0％ | 36.4％ |
| Example 3 | 28.7％ | 0％ | 41.3％ |
| Example 4 | 28.0％ | 0％ | 36.1％ |
| Comparative example 1 | 68.4％ | 57.87％ | 3.23％ |
Examples 1 to 3 exhibited more excellent water resistance, ultraviolet resistance and oxidation resistance compared to comparative example 1.
According to the invention, an energy sacrifice network is constructed at the interface of the lignin/cellulose by using zinc chloride to improve the compatibility between the lignin and the cellulose, and the prepared film has high strength and high toughness. On the other hand, the preparation method adopted by the invention is non-toxic and harmless, environment-friendly, simple and easy to operate.
Claims (9)
1. A lignin/cellulose composite film is characterized in that the formula of the film comprises 74.7-78.9% of cellulose, 19.5-22.8% of lignin and 1.6-2.5% of zinc chloride by weight percent, and the preparation method of the film comprises the following steps:
(1) dissolving lignin powder in an acetone solution, and centrifuging to remove precipitates to obtain a lignin acetone solution;
(2) preparing a cellulose solution, performing ultrasonic treatment to obtain the cellulose solution, and drying to obtain ultrasonic cellulose paper;
(3) dissolving zinc chloride in distilled water to obtain a zinc chloride solution;
(4) soaking the ultrasonic cellulose paper in the step (2) in the zinc chloride solution in the step (3), washing, and soaking in the lignin/acetone solution in the step (1);
(5) and (4) carrying out hot pressing on the ultrasonic cellulose paper impregnated with the lignin/acetone solution in the step (4), and cooling to obtain the lignin/cellulose composite film.
2. The lignin/cellulose composite film according to claim 1, wherein the mass fraction of the cellulose solution prepared in step (2) in the film preparation method is 0.5-1%.
3. The lignin/cellulose composite film according to claim 1, wherein the ultrasonic conditions in step (2) of the film preparation method are 700-800W power ultrasonic for 6-8 hours.
4. The lignin/cellulose composite film according to claim 1, wherein the drying conditions in step (2) in the preparation method of the film are 110-120 ℃ hot press drying for 30-60 minutes under a pressure of 3-8MPa after pressing water on a press machine.
5. The lignin/cellulose composite film according to claim 1, wherein zinc chloride is dissolved in distilled water in step (3), and then a hydrochloric acid solution is added to prepare a zinc chloride solution.
6. The lignin/cellulose composite film according to claim 1, wherein the washing conditions in step (4) in the method for preparing the film are a washing condition in which the ratio of the volume of the lignin/cellulose composite film to the volume of the cellulose composite film is 1: 1-1: 2, washing in an ethanol/water mixed solution, and soaking in alcohol for 30-45 minutes.
7. The lignin/cellulose composite film according to claim 1, wherein the preparation method of the film comprises the step of hot pressing the ultrasonic cellulose paper impregnated with the lignin/acetone solution in step (5) at a temperature of 110-120 ℃ under a pressure of 8-10MPa for 2-2.5 hours.
8. The lignin/cellulose composite film according to any one of claims 1 to 7, wherein the dipping time in step (4) in the film preparation method is 20 to 24 hours.
9. The lignin/cellulose composite film according to any one of claims 1 to 7, wherein the soaking time in step (4) in the film preparation method is 20 to 24 hours.
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