CN113026417B - Preparation method of biodegradable oilproof paper - Google Patents
Preparation method of biodegradable oilproof paper Download PDFInfo
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- CN113026417B CN113026417B CN202110273898.XA CN202110273898A CN113026417B CN 113026417 B CN113026417 B CN 113026417B CN 202110273898 A CN202110273898 A CN 202110273898A CN 113026417 B CN113026417 B CN 113026417B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000011248 coating agent Substances 0.000 claims abstract description 110
- 238000000576 coating method Methods 0.000 claims abstract description 110
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims abstract description 91
- 235000017491 Bambusa tulda Nutrition 0.000 claims abstract description 91
- 241001330002 Bambuseae Species 0.000 claims abstract description 91
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims abstract description 91
- 239000011425 bamboo Substances 0.000 claims abstract description 91
- 239000000843 powder Substances 0.000 claims abstract description 81
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 68
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 68
- 210000001724 microfibril Anatomy 0.000 claims abstract description 52
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000010297 mechanical methods and process Methods 0.000 claims abstract description 12
- 238000010170 biological method Methods 0.000 claims abstract description 10
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
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- 108010059892 Cellulase Proteins 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 20
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- 229920000742 Cotton Polymers 0.000 claims description 2
- 101710112457 Exoglucanase Proteins 0.000 claims description 2
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- 229920001131 Pulp (paper) Polymers 0.000 claims description 2
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- 239000000243 solution Substances 0.000 description 19
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- XPFJYKARVSSRHE-UHFFFAOYSA-K trisodium;2-hydroxypropane-1,2,3-tricarboxylate;2-hydroxypropane-1,2,3-tricarboxylic acid Chemical compound [Na+].[Na+].[Na+].OC(=O)CC(O)(C(O)=O)CC(O)=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O XPFJYKARVSSRHE-UHFFFAOYSA-K 0.000 description 9
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- 235000015895 biscuits Nutrition 0.000 description 1
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- 150000001875 compounds Chemical class 0.000 description 1
- 235000015220 hamburgers Nutrition 0.000 description 1
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- 229910052739 hydrogen Inorganic materials 0.000 description 1
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Images
Classifications
-
- 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
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
- D21H21/16—Sizing or water-repelling agents
-
- 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
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/21—Macromolecular organic compounds of natural origin; Derivatives thereof
- D21H17/24—Polysaccharides
- D21H17/25—Cellulose
-
- 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
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/36—Polyalkenyalcohols; Polyalkenylethers; Polyalkenylesters
-
- 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
- D21H19/00—Coated paper; Coating material
- D21H19/10—Coatings without pigments
-
- 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
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/50—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by form
- D21H21/52—Additives of definite length or shape
Abstract
The invention relates to a preparation method of biodegradable oilproof paper. The method comprises a nano microfibril preparation process and a micro-nano bamboo powder preparation process, wherein the coating is prepared by mixing polyvinyl alcohol, the nano microfibril and the micro-nano bamboo powder, and the target object can be obtained by coating the surface of the prepared coating on base paper. The preparation method comprises the steps of pretreating the micro-nano bamboo powder by a mechanical method or a biological method, and homogenizing under high pressure to obtain the micro-nano bamboo powder. According to the invention, the micro-nano bamboo powder is added into the coating, so that the coating and the nano microfibrils are in synergistic effect, the oil resistance of the coated paper is improved, and the application value of the paper is improved.
Description
Technical Field
The invention belongs to the field of special paper manufacturing, and particularly relates to a preparation method of biodegradable oilproof paper, in particular to a surface treatment process taking cellulose-based paper as an object and application thereof.
Background
The oil-proof paper is paper with the functions of resisting oil penetration and absorption, and is mainly characterized in that the oil-proof paper can meet the requirements of protecting products, facilitating carrying, promoting sale and the like, and reducing the penetration of oil-containing substances. The packaging method is widely used for packaging foods such as hamburgers, baked bread, biscuits and other oil-containing articles. Along with the promotion of the plastic-limiting order and the plastic-prohibiting order, the technological requirements on the oil-proof paper are higher and higher.
The main raw material of the oil-proof paper is plant fiber which has biodegradability. Most of the oil-proof papers on the current market realize the oil-proof effect of the paper by means of film coating and surface modification. In order to obtain the oil and oil resistant effect, people can use plastic packaging materials such as polyethylene, polypropylene and polyvinyl chloride to make films, and transfer the films to the surface of paper, but the film materials are difficult to degrade or degrade very slowly in nature, and the plastic packaging material wastes which are difficult to recycle can cause great pollution to human environment. The surface modification relates to fluorocarbon compounds, and the fluorocarbon compounds are listed in the list of carcinogens published by international cancer research institution of world health organization in 2017. Although the process of surface modification to make grease barrier paper is well established and effective, it poses not only environmental hazards, but also risks to human health. However, other methods for preparing biodegradable oil-proof paper involve practical problems such as high raw material cost, limited applicability, and limited oil-proof grade.
As mentioned above, there are still some problems with the preparation of grease barrier paper. With the progress of society, mankind has not only made higher demands on production environment and product safety in the field of food packaging, but also in the field of industrial production. Therefore, the conventional processes of film coating and surface modification will be replaced by new manufacturing processes in the near future.
Disclosure of Invention
The invention aims to provide a preparation method of biodegradable oil-proof paper (degradable biopolymer is coated on the surface of paper to obtain high oil-proof performance). The oil-proof paper has excellent oil-proof performance and good paper strength, and is safe to use, environment-friendly and degradable.
The technical scheme adopted by the invention for solving the technical problem is as follows:
a preparation method of biodegradable oilproof paper comprises the following steps:
(1) preparing nano microfibrils: weighing 10-20g of pulp board, using a fluffer to fluff 10000 times for 50000 turns, centrifugally dewatering, controlling the concentration of the pulp to be 10% -30%, adding citric acid-sodium citrate buffer solution, adjusting the pH value to be 5-7, then adding 20-100U/g of cellulase, vibrating at the constant temperature of 20-60 ℃ for 2-10h, after the reaction is finished, heating to 90-95 ℃, preserving the temperature for 15-30min, and stopping the enzyme reaction. Then, the slurry is washed to be neutral, and prepared into aqueous suspension with the concentration of 1-3%, and the aqueous suspension is homogenized for 1-2 times under the pressure of 300-700bar and for 2-10 times under the pressure of 1000-1200bar, so as to obtain the nano microfibril (CNF).
(2) Micro-nano bamboo powder preparation: the bamboo powder of 80-125 meshes is used as a raw material and is pretreated by a mechanical method or a biological method. The mechanical method adopts colloid grinding mode, and the circular grinding is carried out for 10-20 min; the biological method uses cellulase, and the cellulase reacts for 2 to 12 hours at the pH value of 5 to 7 and the temperature of 40 to 60 ℃, and is washed to be neutral by distilled water. And (3) carrying out high-pressure homogenization on the pretreated bamboo powder, carrying out high-pressure homogenization for 1-2 times under the pressure of 300-700bar and carrying out homogenization for 2-5 times under the pressure of 1000-1200bar to obtain micro-nano bamboo powder (NBF), which is respectively named as NBF (mechanical method) and FCD-NBF (biological method).
(3) Preparing polyvinyl alcohol/nano microfibril/micro-nano bamboo powder coating: adding water into polyvinyl alcohol (PVA) with the molecular mass of 15000-85000 to prepare a solution with the mass percent of 1-10%, swelling for 15-30min at 50-60 ℃, slowly adding nano microfibril with the mass percent of 1-10% relative to the mass percent of the polyvinyl alcohol, uniformly stirring, heating to 90-95 ℃, and preserving heat for 1-1.5 h. Then adding micro-nano bamboo powder with the mass percent of 1-10 percent relative to the polyvinyl alcohol, stirring for 1-5min at the rotating speed of 1000-5000r/min by using a stirrer, and then placing the mixture under the ultrasonic wave of 90-100Hz for dispersing for 15-30min to remove bubbles, thus obtaining the coating with good dispersibility.
(4) Preparing coated paper: coating the surface of base paper with the prepared coating, and drying at 50-105 deg.C for 10-30min to obtain coating weight of 1.0-6.0g/m2The coated paper of (1).
The pulp board is one or two of a bamboo pulp board, a wood pulp board or a cotton pulp board.
The cellulase is one or two of endoglucanase, exoglucanase and laccase.
The invention has the beneficial effects that:
(1) the oil-proof paper obtained by the invention can reach the highest grade 12 of TAPPI T559 oil-proof test standard, has excellent oil-proof performance, and the polyvinyl alcohol coated paper and the polyvinyl alcohol/nano microfibril composite coated paper with the same coating amount can only reach 7-9 grades.
(2) According to the invention, the micro-nano bamboo powder is introduced into the coating system, compared with a polyvinyl alcohol/nano microfibril coating, the nano microfibrils in the coating system and the micro-nano bamboo powder generate a synergistic effect, and the prepared coated paper has better oil resistance under the same coating weight.
(3) The raw materials used in the invention can be completely degraded into carbon dioxide and water, and micro-plastics are not generated.
(4) The method is simple to operate, environment-friendly and easy for industrial mass production.
Drawings
FIG. 1 is a graph of the oil repellency properties of paper for different coating formulations.
Detailed Description
The principle of the method of the invention is as follows: polyvinyl alcohol is a biodegradable polymer and has good film-forming properties and superior barrier properties. When the coating is coated on base paper, the oil resistance of paper can be improved, but the improvement degree is limited in practice. The surface of the nano microfibril has a large amount of hydroxyl groups, and a compact film can be formed by coating the nano microfibril on the surface of paper, so that the nano microfibril has a good barrier effect, but because the main component of the nano microfibril is cellulose and has certain lipophilicity, the nano microfibril and polyvinyl alcohol compound coating still cannot achieve an ideal oil-resistant effect. The surface of the micro-nano bamboo powder is wrapped by a large amount of lignin, and the specific surface is huge, so that a good barrier effect is provided. According to the invention, the lignin content in the micro-nano bamboo powder is controlled by changing the pretreatment mode, and the micro-nano bamboo powder is added on the basis of the polyvinyl alcohol/nano microfibril composite coating, so that the oleophylic properties of the polyvinyl alcohol and the nano microfibril are reduced, and the coated paper obtains a good oil-proof effect.
The pretreatment of the micro-nano bamboo powder can be divided into a mechanical method, a biological method and a chemical method. The pretreatment can ensure the smooth proceeding of the subsequent high-pressure homogenization, wherein the mechanical method can reduce the size of the bamboo powder, and the biological method and the chemical method can soften the bamboo powder. After high-pressure homogenization, the bamboo powder is changed into a sheet structure from a rod-shaped structure, so that hydrogen bonding between the micro-nano bamboo powder and the nano microfibrils is promoted, and the barrier property of the coating is enhanced. Wherein, the mechanical method and the biological method do not influence the lignin content of the bamboo powder, and the chemical method can remove part of the lignin in the bamboo powder. The lignin has low polarity, low surface energy and good oil resistance, so that the micro-nano bamboo powder is pretreated mainly by a mechanical method and a biological method.
The following examples are provided to further illustrate and compare conventional processes with the present invention, including but not limited to the examples (note: the base papers used in the following examples all have a rating of 0).
One, the following examples 1 to 3 illustrate the effect of a single polyvinyl alcohol coating on the oil repellency properties of paper.
Example 1
(1) Preparing a polyvinyl alcohol coating: adding water into polyvinyl alcohol with the molecular weight of 15000 to prepare a solution with the mass percentage of 10%, swelling for 15min at 50 ℃, heating to 90 ℃, preserving heat for 1.5h, then placing the solution under 90Hz ultrasonic waves for dispersing for 15min, and removing bubbles to obtain the polyvinyl alcohol coating.
(2) Preparing coated paper: coating the surface of base paper with the prepared coating, and drying at 80 deg.C for 10min to obtain coating weight of 2.0g/m2The coated paper of (1).
(3) And (3) testing: the paper obtained in this example had an oil resistance rating of 2 (TAPPI T559 test standard).
Example 2
(1) Preparing a polyvinyl alcohol coating: adding water into polyvinyl alcohol with the molecular mass of 40000 to prepare a solution with the mass percentage of 10%, swelling at 50 ℃ for 30min, heating to 95 ℃, preserving heat for 1h, then placing the solution under 90Hz ultrasonic waves for dispersing for 30min, and removing bubbles to obtain the polyvinyl alcohol coating.
(2) Preparing coated paper: coating the surface of base paper with the prepared coating, and drying at 80 ℃ for 10 minutes to obtain the coating weight of 2.0g/m2The coated paper of (1).
(3) And (3) testing: the paper obtained in this example had an oil resistance rating of 6 (TAPPI T559 test standard).
Example 3
(1) Preparing a polyvinyl alcohol coating: adding water into 75000 molecular weight polyvinyl alcohol to prepare 10% solution, swelling at 60 deg.C for 15min, heating to 90 deg.C, maintaining for 1h, dispersing under 100Hz ultrasonic wave for 15min, and removing bubbles to obtain polyvinyl alcohol coating.
(2) Preparing coated paper: coating the surface of base paper with the prepared coating, and drying at 80 deg.C for 10min to obtain coating weight of 2.0g/m2The coated paper of (1).
(3) And (3) testing: the paper obtained in this example had an oil resistance rating of 7 (TAPPI T559 test standard).
And conclusion one:
based on examples 1 to 3, it is possible to achieve a maximum oil resistance rating of only 7 for the paper coated with polyvinyl alcohol.
Two, the following examples 4 to 6 illustrate the effect of polyvinyl alcohol/nanofibril coating application on the oil repellency properties of paper.
Example 4
(1) Preparing nano microfibrils: accurately weighing 10g of bamboo pulp board, using a fluffer to fluff by 10000 turns, centrifugally dewatering, controlling the pulp concentration to be 25%, adding citric acid-sodium citrate buffer solution, adjusting the pH value to be 5, then adding 60U/g of cellulase, vibrating at the constant temperature of 50 ℃ for 6h, after the reaction is finished, heating to 90 ℃, preserving the temperature for 15min, and stopping the enzyme reaction. Then, the slurry was washed to be neutral, prepared into an aqueous suspension having a concentration of 1%, and homogenized at a high pressure of 300bar for 1 time, at a high pressure of 500bar for 1 time, and at 1000bar for 10 times, to obtain nanofibrils.
(2) Preparation of polyvinyl alcohol/nano microfibril coating: adding water into 75000 molecular weight polyvinyl alcohol to obtain 10% solution, swelling at 60 deg.C for 30min, slowly adding 1% nanometer microfibril, stirring, heating to 90 deg.C, and keeping the temperature for 1.5 h. And then the mixture is placed under 90Hz ultrasonic waves for dispersion for 15min, bubbles are removed, and the coating with good dispersibility is obtained.
(3) Preparing coated paper: coating the surface of base paper with the prepared coating, and drying at 80 deg.C for 10min to obtain coating weight of 2.0g/m2The coated paper of (1).
(4) And (3) testing: the paper obtained in this example had an oil resistance rating of 8 (TAPPI T559 test standard).
Example 5
(1) Preparing nano microfibrils: accurately weighing 10g of bamboo pulp board, fluffing by a fluffer for 30000 turns, centrifugally dewatering, controlling the pulp concentration to be 25%, adding citric acid-sodium citrate buffer solution, adjusting the pH value to be 6, then adding 80U/g of cellulase, vibrating at the constant temperature of 50 ℃ for 6h, after the reaction is finished, heating to 90 ℃, preserving the temperature for 20min, and stopping the enzyme reaction. Then, the slurry was washed to neutrality to prepare a 2% aqueous suspension, and the suspension was homogenized under high pressure at 500bar for 2 times and 1000bar for 10 times to obtain nanofibrils.
(2) Preparation of polyvinyl alcohol/nano microfibril coating: adding water into 75000 molecular weight polyvinyl alcohol to obtain 10% solution, swelling in 60 deg.C water bath for 30min, slowly adding 3% nanometer microfibril, stirring, heating to 95 deg.C, and keeping the temperature for 1 h. And then the mixture is placed under 90Hz ultrasonic waves for dispersion for 30min, bubbles are removed, and the coating with good dispersibility is obtained.
(3) Preparing coated paper: coating the surface of base paper with the prepared coating, and drying at 80 deg.C for 10min to obtain coating weight of 2.0g/m2The coated paper of (1).
(4) And (3) testing: the paper obtained in this example had an oil resistance rating of 9 (TAPPI T559 test standard) of 0.
Example 6
(1) Preparing nano microfibrils: accurately weighing 10g of bamboo pulp board, fluffing by a fluffer for 50000 turns, centrifugally dewatering, controlling the pulp concentration to be 30%, adding citric acid-sodium citrate buffer solution, adjusting the pH value to be 7, then adding 100U/g of cellulase, vibrating at the constant temperature of 50 ℃ for 6h, after the reaction is finished, heating to 90 ℃, preserving the temperature for 30min, and stopping the enzyme reaction. Then, the slurry was washed to neutrality to prepare a 3% aqueous suspension, which was then homogenized at high pressure 1 time at a pressure of 700bar and 10 times at 1000bar to obtain nanofibrils.
(2) Preparation of polyvinyl alcohol/nano microfibril coating: adding water into 75000 molecular weight polyvinyl alcohol to obtain 10% solution, swelling in 60 deg.C water bath for 15min, slowly adding 8% nanometer microfibril, stirring, heating to 90 deg.C, and keeping the temperature for 1 h. And then the mixture is placed under 100Hz ultrasonic waves for dispersion for 15min, bubbles are removed, and the coating with good dispersibility is obtained.
(3) Preparing coated paper: coating the surface of base paper with the prepared coating, and drying at 80 deg.C for 10min to obtain coating weight of 2.0g/m2The coated paper of (1).
(4) And (3) testing: the paper obtained in this example had an oil resistance rating of 9 (TAPPI T559 test standard).
And a second conclusion:
based on examples 4 to 6, the maximum oil resistance of the paper coated with the polyvinyl alcohol/nano microfibril coating reaches 9 grades, which is improved to a certain extent compared with the oil resistance of the paper coated with the polyvinyl alcohol alone, and the nano microfibrils are proved to play a certain blocking role.
Third, the following examples 7 to 9 illustrate the effect of the coating of polyvinyl alcohol/micro-nano bamboo powder on the oil-proof performance of paper by replacing the micro-nano fibrils with micro-nano bamboo powder.
Example 7
(1) Micro-nano bamboo powder preparation: the method comprises the steps of circularly grinding 125-mesh bamboo powder serving as a raw material for 20min in a colloid grinding mode, then homogenizing at high pressure for 1 time under the pressure of 300bar, 1 time under the pressure of 500bar and 5 times under the pressure of 1000bar to obtain the micro-nano bamboo powder (NBF).
(2) Preparing a polyvinyl alcohol/micro-nano bamboo powder (NBF) coating: adding water into 75000 molecular weight polyvinyl alcohol to obtain 10% solution, swelling at 60 deg.C for 30min, heating to 90 deg.C, and maintaining for 1.5 hr. Adding micro-nano bamboo powder (NBF) with the mass percent of 3 percent relative to the polyvinyl alcohol into the fully dissolved coating, stirring for 3min at the rotating speed of 1000r/min by using a stirrer, then placing the coating under 90Hz ultrasonic waves for dispersing for 15min, and removing bubbles to obtain the coating with good dispersibility.
(3) Preparing coated paper: coating the surface of base paper with the prepared coating, and drying at 80 deg.C for 10min to obtain coating weight of 2.0g/m2Coating ofPaper.
(4) And (3) testing: the paper obtained in this example had an oil resistance rating of 8 (TAPPI T559 test standard).
Example 8
(1) Micro-nano bamboo powder preparation: the method comprises the steps of adopting 80-mesh bamboo powder as a raw material, using cellulase to react for 6 hours at the temperature of 50 ℃ and the pH value of 5, washing the raw material to be neutral by using distilled water, and then carrying out high-pressure homogenization for 2 times under the pressure of 500bar and 5 times under the pressure of 1000bar to obtain the micro-nano bamboo powder (FCD-NBF).
(2) Preparing a polyvinyl alcohol/micro-nano bamboo powder (FCD-NBF) coating: adding water into 75000 molecular weight polyvinyl alcohol to obtain 10% solution, swelling at 50 deg.C for 30min, heating to 95 deg.C, and keeping the temperature for 1 h. Adding micro-nano bamboo powder (FCD-NBF) with the mass percent of 3 percent relative to the polyvinyl alcohol into the fully dissolved coating, stirring for 2min at the rotating speed of 2000r/min by using a stirrer, then placing the coating under the ultrasonic wave of 90Hz for dispersing for 30min, removing bubbles and obtaining the coating with good dispersibility.
(3) Preparing coated paper: coating the surface of base paper with the prepared coating, and drying at 80 deg.C for 10min to obtain coating weight of 2.0g/m2The coated paper of (1).
(4) And (3) testing: the paper obtained in this example exhibited an oil resistance rating of 9 (TAPPI T559 test standard).
Example 9
(1) Micro-nano bamboo powder preparation: the method comprises the steps of adopting 80-mesh bamboo powder as a raw material, using 1% sodium hydroxide solution, processing for 1h at 90 ℃, washing with distilled water to be neutral, then, carrying out high-pressure homogenization for 2 times at 700bar pressure, and carrying out homogenization for 5 times at 1000bar pressure to obtain the micro-nano bamboo powder (Na-NBF).
(2) Preparing a polyvinyl alcohol/micro-nano bamboo powder (Na-NBF) coating: adding water into 75000 molecular weight polyvinyl alcohol to obtain 10% solution, swelling at 60 deg.C for 15min, heating to 90 deg.C, and keeping the temperature for 1 h. Adding micro-nano bamboo powder (Na-NBF) with the mass percent of 3 percent relative to the polyvinyl alcohol into the fully dissolved coating, stirring for 1min at the rotating speed of 3000r/min by using a stirrer, then placing the coating under 100Hz ultrasonic waves for dispersing for 15min, removing bubbles and obtaining the coating with good dispersibility.
(3) Preparing coated paper: coating the surface of base paper with the prepared coating, and drying at 80 deg.C for 10min to obtain coating weight of 2.0g/m2The coated paper of (1).
(4) And (3) testing: the paper obtained in this example exhibited an oil resistance rating of 9 (TAPPI T559 test standard).
And conclusion three:
based on examples 7 to 9, the highest oil resistance level of the paper coated with the polyvinyl alcohol/micro-nano bamboo powder coating reaches 9 levels, and the addition of the micro-nano bamboo powder is proved to improve the oil resistance of the paper.
Fourthly, the following examples 10 to 12 are to illustrate the effect of polyvinyl alcohol/nano microfibril/micro nano bamboo powder coating on the oil resistance of paper.
Example 10
(1) Preparing nano microfibrils: accurately weighing 10g of bamboo pulp board, using a fluffer to fluff by 10000 turns, centrifugally dewatering, controlling the pulp concentration to be 25%, adding citric acid-sodium citrate buffer solution, adjusting the pH value to be 5, then adding 60U/g of cellulase, vibrating at the constant temperature of 50 ℃ for 6h, after the reaction is finished, heating to 90 ℃, preserving the temperature for 15min, and stopping the enzyme reaction. Then, the slurry was washed to be neutral, prepared into an aqueous suspension having a concentration of 1%, and homogenized at a high pressure of 300bar for 1 time, at a high pressure of 500bar for 1 time, and at 1000bar for 10 times, to obtain nanofibrils.
(2) Micro-nano bamboo powder preparation: the method comprises the steps of taking 125-mesh bamboo powder as a raw material, circularly grinding for 10min in a colloid grinding mode, then carrying out high-pressure homogenization, carrying out high-pressure homogenization for 1 time under the pressure of 300bar, carrying out high-pressure homogenization for 1 time under the pressure of 700bar, and carrying out homogenization for 5 times under the pressure of 1000bar to obtain the micro-nano bamboo powder (NBF).
(3) Preparing a polyvinyl alcohol/nano microfibril/micro nano bamboo powder (NBF) coating: adding water into 75000 molecular weight polyvinyl alcohol to obtain 10% solution, swelling at 50 deg.C for 15min, slowly adding 2.4% nanometer microfibril, stirring, heating to 90 deg.C, and keeping the temperature for 1.5 h. Then, adding micro-nano bamboo powder (NBF) with the mass percent of 0.6 percent relative to the polyvinyl alcohol, stirring for 3min by using a stirrer at the rotating speed of 1000r/min, then placing the mixture under 90Hz ultrasonic waves for dispersing for 15min, and removing bubbles to obtain the coating with good dispersibility.
(4) Preparation of coated paper: coating the surface of base paper with the prepared coating, and drying at 80 deg.C for 10min to obtain coating weight of 2.0g/m2The coated paper of (1).
(5) And (3) testing: the paper obtained in this example exhibited an oil resistance rating of 9 (TAPPI T559 test standard).
Example 11
(1) Preparing nano microfibrils: accurately weighing 10g of bamboo pulp board, fluffing by a fluffer for 30000 turns, centrifugally dewatering, controlling the pulp concentration to be 25%, adding citric acid-sodium citrate buffer solution, adjusting the pH value to be 6, then adding 80U/g of cellulase, vibrating at the constant temperature of 50 ℃ for 6h, after the reaction is finished, heating to 90 ℃, preserving the temperature for 20min, and stopping the enzyme reaction. Then, the slurry was washed to neutrality to prepare a 2% aqueous suspension, and the suspension was homogenized under high pressure at 500bar for 2 times and 1000bar for 10 times to obtain nanofibrils.
(2) Micro-nano bamboo powder preparation: the method comprises the steps of taking 125-mesh bamboo powder as a raw material, circularly grinding for 20min in a colloid grinding mode, then carrying out high-pressure homogenization, carrying out high-pressure homogenization for 1 time under the pressure of 300bar, carrying out high-pressure homogenization for 1 time under the pressure of 500bar, and carrying out homogenization for 5 times under the pressure of 1000bar to obtain the micro-nano bamboo powder (NBF).
(3) Preparing a polyvinyl alcohol/nano microfibril/micro nano bamboo powder (NBF) coating: adding water into 75000 molecular weight polyvinyl alcohol to obtain 10% solution, swelling at 50 deg.C for 30min, slowly adding 1.8% nanometer microfibril, stirring, heating to 95 deg.C, and keeping the temperature for 1 h. Then, adding micro-nano bamboo powder (NBF) with the mass percent of 1.2 percent relative to the polyvinyl alcohol, stirring for 2min at the rotating speed of 2000r/min by using a stirrer, then placing the mixture under 100Hz ultrasonic waves for dispersing for 15min, and removing bubbles to obtain the coating with good dispersibility.
(4) Preparing coated paper: the prepared coating is used for coating the surface of base paper,then, the resultant was dried at 80 ℃ for 10min to give a coating weight of 2.0g/m2The coated paper of (1).
(5) And (3) testing: the paper obtained in this example exhibited an oil resistance rating of 10 (TAPPI T559 test standard).
Example 12
(1) Preparing nano microfibrils: accurately weighing 10g of bamboo pulp board, fluffing by a fluffer for 50000 turns, centrifugally dewatering, controlling the pulp concentration to be 30%, adding citric acid-sodium citrate buffer solution, adjusting the pH value to be 7, then adding 100U/g of cellulase, vibrating at the constant temperature of 50 ℃ for 6h, after the reaction is finished, heating to 90 ℃, preserving the temperature for 30min, and stopping the enzyme reaction. Then, the slurry was washed to neutrality to prepare a 3% aqueous suspension, which was then homogenized at high pressure 1 time at a pressure of 700bar and 10 times at 1000bar to obtain nanofibrils.
(2) Micro-nano bamboo powder preparation: the method comprises the steps of circularly grinding 80-mesh bamboo powder serving as a raw material for 30min in a colloid grinding mode, and finally carrying out high-pressure homogenization, wherein the high-pressure homogenization is carried out for 2 times at 500bar and 5 times at 1000bar, so as to obtain the micro-nano bamboo powder (NBF).
(3) Preparing a polyvinyl alcohol/nano microfibril/micro nano bamboo powder (NBF) coating: adding water into 75000 molecular weight polyvinyl alcohol to obtain 10% solution, swelling at 60 deg.C for 15min, slowly adding 1.2% nanometer microfibril, stirring, heating to 90 deg.C, and keeping the temperature for 1 h. Then, adding micro-nano bamboo powder (NBF) with the mass percent of 1.8 percent relative to the polyvinyl alcohol, stirring for 1min by using a stirrer at the rotating speed of 3000r/min, then placing the mixture under 90Hz ultrasonic waves for dispersing for 30min, and removing bubbles to obtain the coating with good dispersibility.
(4) Preparing coated paper: coating the surface of base paper with the prepared coating, and drying at 80 deg.C for 10min to obtain coating weight of 2.0g/m2The coated paper of (1).
(5) And (3) testing: the paper obtained in this example exhibited an oil resistance rating of 12 (TAPPI T559 test standard).
And conclusion four:
based on examples 10 to 12, the highest oil resistance level of the paper coated with the polyvinyl alcohol/nano microfibril/micro nano bamboo powder coating reaches 12 levels, the obtained paper has excellent oil resistance, and the polyvinyl alcohol, the nano microfibril and the micro nano bamboo powder are proved to have good synergistic effect and generate excellent barrier property.
Fifthly, the following examples 13 to 14 illustrate the influence of the pretreatment mode of the micro-nano bamboo powder in the polyvinyl alcohol/nano micro-fibril/micro-nano bamboo powder coating on the oil resistance of paper.
Example 13
(1) Preparing nano microfibrils: accurately weighing 10g of bamboo pulp board, using a fluffer to fluff by 10000 turns, centrifugally dewatering, controlling the pulp concentration to be 25%, adding citric acid-sodium citrate buffer solution, adjusting the pH value to be 5, then adding 60U/g of cellulase, vibrating at the constant temperature of 50 ℃ for 6h, after the reaction is finished, heating to 90 ℃, preserving the temperature for 15min, and stopping the enzyme reaction. Then, the slurry was washed to be neutral, prepared into an aqueous suspension having a concentration of 1%, and homogenized at a high pressure of 300bar for 1 time, at a high pressure of 500bar for 1 time, and at 1000bar for 10 times, to obtain nanofibrils.
(2) Micro-nano bamboo powder preparation: the method comprises the steps of adopting 80-mesh bamboo powder as a raw material, using 1% sodium hydroxide solution, processing for 1h at 90 ℃, washing with distilled water to be neutral, then, carrying out high-pressure homogenization for 2 times at 700bar pressure, and carrying out homogenization for 5 times at 1000bar pressure to obtain the micro-nano bamboo powder (Na-NBF).
(3) Preparing a polyvinyl alcohol/nano microfibril/micro nano bamboo powder (Na-NBF) coating: adding water into 75000 molecular weight polyvinyl alcohol to obtain 10% solution, swelling at 50 deg.C for 15min, slowly adding 1.2% nanometer microfibril, stirring, heating to 90 deg.C, and keeping the temperature for 1.5 h. Then, adding micro-nano bamboo powder (Na-NBF) with the mass percent of 1.8 percent relative to the polyvinyl alcohol, stirring for 3min at the rotating speed of 1000r/min by using a stirrer, then placing the mixture under 90Hz ultrasonic waves for dispersing for 15min, and removing bubbles to obtain the coating with good dispersibility.
(4) Preparation of coated paper: coating the surface of base paper with the prepared coating, and drying at 80 deg.C10min, a coating weight of 2.0g/m is obtained2The coated paper of (1).
(5) And (3) testing: the paper obtained in this example exhibited an oil resistance rating of 9 (TAPPI T559 test standard).
Example 14
(1) Preparing nano microfibrils: accurately weighing 10g of bamboo pulp board, using a fluffer to fluff by 10000 turns, centrifugally dewatering, controlling the pulp concentration to be 25%, adding citric acid-sodium citrate buffer solution, adjusting the pH value to be 5, then adding 60U/g of cellulase, vibrating at the constant temperature of 50 ℃ for 6h, after the reaction is finished, heating to 90 ℃, preserving the temperature for 15min, and stopping the enzyme reaction. Then, the slurry was washed to be neutral, prepared into an aqueous suspension having a concentration of 1%, and homogenized at a high pressure of 300bar for 1 time, at a high pressure of 500bar for 1 time, and at 1000bar for 10 times, to obtain nanofibrils.
(2) Micro-nano bamboo powder preparation: the method comprises the steps of adopting 80-mesh bamboo powder as a raw material, using cellulase to react for 6 hours at the temperature of 50 ℃ and the pH value of 5, washing the raw material to be neutral by using distilled water, and then carrying out high-pressure homogenization for 2 times under the pressure of 500bar and 5 times under the pressure of 1000bar to obtain the micro-nano bamboo powder (FCD-NBF).
(3) Preparing a polyvinyl alcohol/nano microfibril/micro nano bamboo powder (FCD-NBF) coating: adding water into 75000 molecular weight polyvinyl alcohol to obtain 10% solution, swelling at 50 deg.C for 15min, slowly adding 1.2% nanometer microfibril, stirring, heating to 90 deg.C, and keeping the temperature for 1.5 h. Then, adding micro-nano bamboo powder (FCD-NBF) with the mass percent of 1.8 percent relative to the polyvinyl alcohol, stirring for 3min at the rotating speed of 1000r/min by using a stirrer, then placing the mixture under 90Hz ultrasonic waves for dispersing for 15min, and removing bubbles to obtain the coating with good dispersibility.
(4) Preparation of coated paper: coating the surface of base paper with the prepared coating, and drying at 80 deg.C for 10min to obtain coating weight of 2.0g/m2The coated paper of (1).
(5) And (3) testing: the paper obtained in this example exhibited an oil resistance rating of 12 (TAPPI T559 test standard).
And a fifth conclusion:
as can be seen from examples 12, 13 and 14, the oil resistance grades of the paper obtained by the mechanical method and the enzymatic pretreatment method of the bamboo powder are 12 grades, and the paper obtained by the chemical pretreatment method is 9 grades. The reason is that the bamboo powder treated by the mechanical method and the enzymatic pretreatment method reserves most of lignin, especially lignin on the surface of fiber, so that the coated paper has excellent oil-proof performance, and the pretreatment by the sodium hydroxide chemical method dissolves out part of the lignin, so that the oil-proof performance of the coated paper is reduced.
The results of the oil repellency rating tests for the papers of examples 3, 5, 7, and 12 are shown in FIG. 1, and the PVA/CNF/NBF coated paper has excellent oil repellency.
Claims (5)
1. A preparation method of biodegradable oilproof paper is characterized in that:
firstly, preparing nano microfibrils:
weighing 10-20g of pulp board, using a fluffer to fluff 10000-;
adding cellulase 20-100U/g, shaking at 20-60 deg.C for 2-10 hr, heating to 90-95 deg.C after reaction, maintaining the temperature for 15-30min, and stopping enzyme reaction;
washing the slurry to be neutral, preparing aqueous suspension with the concentration of 1-3%, and homogenizing for 1-2 times under the pressure of 300-700bar and 2-10 times under the pressure of 1000-1200bar to obtain the nano microfibril;
secondly, micro-nano bamboo powder preparation:
using 80-125 mesh bamboo powder as raw material, and pretreating by mechanical method or biological method to adapt to subsequent high-pressure homogenization;
homogenizing the pretreated bamboo powder at high pressure for 1-2 times under the pressure of 300-700bar and 2-5 times under the pressure of 1000-1200bar to obtain micro-nano bamboo powder;
thirdly, preparing the polyvinyl alcohol/nano microfibril/micro nano bamboo powder coating:
adding water into polyvinyl alcohol with the molecular mass of 15000-85000 to prepare a solution with the mass percentage of 1-10%, and swelling for 15-30min at 50-60 ℃;
slowly adding 1-10% of nano microfibril by mass percent relative to the polyvinyl alcohol, uniformly stirring, heating to 90-95 ℃, and preserving heat for 1-1.5 h;
adding micro-nano bamboo powder with the mass percent of 1-10 percent relative to the polyvinyl alcohol, and stirring for 1-5min by using a stirrer at the rotating speed of 1000-;
dispersing the mixture under 90-100Hz ultrasonic wave for 15-30min to remove bubbles and obtain the coating with good dispersibility;
fourthly, preparing coated paper: coating the surface of the prepared coating on base paper, and drying at 50-105 deg.C for 10-30min to obtain coating weight of 1.0-6.0g/m2The coated paper of (1).
2. The method for preparing biodegradable oilproof paper according to claim 1, wherein: the mechanical method adopts colloid grinding mode and circulating grinding is carried out for 10-20 min.
3. The method for preparing biodegradable oilproof paper according to claim 1, wherein: the biological method uses cellulase to react for 2 to 12 hours at the pH value of 5 to 7 and the temperature of 40 to 60 ℃, and the cellulase is washed to be neutral by distilled water.
4. The method for preparing biodegradable oilproof paper according to claim 1, wherein the pulp sheet is one or two of bamboo pulp sheet, wood pulp sheet or cotton pulp sheet.
5. The method for preparing the biodegradable oil-proof paper as claimed in claim 3, wherein the cellulase is one or two of endoglucanase, exoglucanase and laccase.
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