CN114457607A - Preparation method of nano-cellulose and nano-lignin particle composite system - Google Patents
Preparation method of nano-cellulose and nano-lignin particle composite system Download PDFInfo
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- CN114457607A CN114457607A CN202210305298.1A CN202210305298A CN114457607A CN 114457607 A CN114457607 A CN 114457607A CN 202210305298 A CN202210305298 A CN 202210305298A CN 114457607 A CN114457607 A CN 114457607A
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21D—TREATMENT OF THE MATERIALS BEFORE PASSING TO THE PAPER-MAKING MACHINE
- D21D1/00—Methods of beating or refining; Beaters of the Hollander type
- D21D1/02—Methods of beating; Beaters of the Hollander type
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21B—FIBROUS RAW MATERIALS OR THEIR MECHANICAL TREATMENT
- D21B1/00—Fibrous raw materials or their mechanical treatment
- D21B1/02—Pretreatment of the raw materials by chemical or physical means
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21B—FIBROUS RAW MATERIALS OR THEIR MECHANICAL TREATMENT
- D21B1/00—Fibrous raw materials or their mechanical treatment
- D21B1/04—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres
- D21B1/06—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres by dry methods
- D21B1/061—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres by dry methods using cutting devices
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21D—TREATMENT OF THE MATERIALS BEFORE PASSING TO THE PAPER-MAKING MACHINE
- D21D1/00—Methods of beating or refining; Beaters of the Hollander type
- D21D1/20—Methods of refining
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21D—TREATMENT OF THE MATERIALS BEFORE PASSING TO THE PAPER-MAKING MACHINE
- D21D1/00—Methods of beating or refining; Beaters of the Hollander type
- D21D1/20—Methods of refining
- D21D1/30—Disc mills
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Abstract
The invention discloses a preparation method of a nano-cellulose and nano-lignin particle composite system, which comprises the steps of fibrillating a wood fiber raw material to obtain a suspension, and sequentially carrying out high-pressure homogenization treatment and high-shear treatment on the suspension to obtain a finished product; wherein the high shear treatment condition is that the rotating speed is 20000-30000rpm, the sample concentration of the suspension is 0.5-3 wt%, the suspension is put into the container to be cooled after 3-7 minutes of each shear treatment, the high shear treatment is carried out again after the temperature is cooled to room temperature, and the total time of the high shear treatment is 8-15 minutes. The method adopts a green mechanical method to prepare the composite system containing the nano-cellulose and the nano-lignin particles in a unified system, does not use chemicals, avoids environmental pollution, has simple process, low raw material cost and short treatment time, and is convenient for industrial popularization.
Description
Technical Field
The invention relates to the technical field of cellulose, in particular to a preparation method of a nano-cellulose and nano-lignin particle composite system.
Background
The stable Pickering emulsion of the wood fiber nano material as a novel emulsifier has become the focus of attention of scientific researchers at home and abroad. The most abundant lignocellulosic feedstocks are cellulose and lignin. Compared with the traditional emulsifier, the cellulose and lignin nano material has the characteristics of reproducibility, degradability, high biocompatibility, multiple functions and the like, and can further expand the application of the emulsion in the fields of daily cosmetics, biomedicine, ultralight materials, interface catalysis and the like.
There are two main types of nanocellulose, namely Cellulose Nanocrystals (CNCs) and Cellulose Nanofibrils (CNFs), both of which have good emulsifying capacity. The CNCs are whiskers which are needle-shaped or spindle-shaped and have small length-diameter ratio, and as the CNCs have hydrophobic crystal faces, the contact angle of an oil phase-CNCs-water phase is less than 90 degrees, the CNCs can be directionally arranged in the oil phase and irreversibly adsorbed on the surface of emulsion liquid drops to form a covering layer to prevent the liquid drops from being fused, so that a stable oil-in-water emulsion system is obtained. CNFs are mainly elongated and intertwined filamentous fibers obtained by subjecting fibers to processes such as shearing, grinding, cavitation and the like, and have a large aspect ratio. When the CNFs are used as the emulsifier stabilizer, the CNFs are generally distributed on an oil-water interface in a net structure in the form of single fibers or dispersed fibers or fiber flocculation, so that the emulsion droplet fusion is prevented, and a good emulsification effect is achieved. It was found that as the degree of fibrillation of CNFs increases, the size of the stable emulsion droplets becomes smaller, the stability of the emulsion also increases, and the stable emulsions of CNFs have higher stability to ion concentration, pH and temperature. The preparation of nanocellulose at the present stage needs to remove lignin in raw materials in advance, the process needs to consume a large amount of chemicals, and the removed lignin is difficult to recycle and realize the goal of jointly stabilizing emulsion of cellulose and lignin.
Nano lignin particles (LNPs), as spherical nanoparticles, exhibit unique advantages in shape and size, and can achieve a desired surface charge through a simple modification process, and are good emulsifiers. For example, sulfonated LNPs can undergo self-assembly adsorption on the surface of emulsion droplets, and due to the high desorption energy of sulfonated LNPs, the adsorption on the surface of emulsion droplets is irreversible, and a rigid adsorption layer is formed to stabilize the emulsion. In addition, the nano lignin particles have the characteristics of high oxidation resistance, ultraviolet resistance, high compatibility with polymers and the like, and can improve the performance of the emulsion in the aspects of daily cosmetics, polymer materials prepared by taking the emulsion as a template and the like when being used as an emulsifier. The preparation of nano lignin particles at the present stage mainly adopts methods of self-assembly, polymerization assembly, freeze-drying carbonization, mechanical treatment and the like, raw materials of the methods are lignin solution or lignin suspension, nano lignin particles can be prepared only singly, and the joint preparation of cellulose and lignin in the same system cannot be realized.
The nano-cellulose and nano-lignin particles are both from plant fiber raw materials, but are prepared by different systems and methods. Therefore, how to prepare a composite system containing nano-cellulose and nano-lignin particles under the same system is the key for efficiently utilizing the two major components of the wood fiber.
Disclosure of Invention
The invention aims to provide a preparation method of a nano-cellulose and nano-lignin particle composite system. The method adopts a green mechanical method to prepare the composite system containing the nano-cellulose and the nano-lignin particles in a unified system, does not use chemicals, avoids environmental pollution, has simple process, low raw material cost and short treatment time, and is convenient for industrial popularization.
The technical scheme of the invention is as follows: a preparation method of a nano-cellulose and nano-lignin particle composite system comprises the steps of fibrillating a wood fiber raw material to obtain a suspension, and sequentially carrying out high-pressure homogenization treatment and high-shear treatment on the suspension to obtain a finished product; wherein the high shear treatment condition is that the rotation speed is 20000-30000rpm, the sample concentration of the suspension is 0.5-3 wt%, the suspension is placed for cooling after 3-7 minutes of each shear treatment, the high shear treatment is carried out again after the temperature is reduced to room temperature, and the total time of the high shear treatment is 8-15 minutes.
The fibrillation treatment is to soak the wood fiber raw material in water to obtain pulp with the concentration of 0.8-1.2 wt%, to disintegrate the paper pulp by a beater for 0.5-2h, to obtain the pulp subjected to the superfine grinding treatment, to obtain the pulp subjected to the primary grinding treatment, and to circularly grind the pulp subjected to the primary grinding treatment for 35-45 times under the condition that the disc grinding gap is-80 mu m to-120 mu m, to obtain the suspension.
In the fibrillation treatment, the wood fiber raw material is soaked in water to obtain the pulp with the concentration of 1.0 wt%, a pulping machine is adopted to disintegrate the paper pulp, the pulping time is 1h, the disintegrated pulp is subjected to superfine particle grinding treatment to obtain the pulp subjected to primary grinding treatment, and the pulp subjected to primary grinding treatment is subjected to cyclic grinding treatment for 40 times under the condition that the disc grinding gap is-100 mu m to obtain the suspension.
In the preparation method of the nano-cellulose and nano-lignin particle composite system, the wood fiber raw material is cut into the pulp crushing plate with the size of 5cm multiplied by 5cm, and the pulp crushing plate is soaked in water for 24 hours, and then the pulp with the concentration of 1 wt% is obtained.
In the preparation method of the composite system of nano-cellulose and nano-lignin particles, the ultra-fine particle grinding treatment is to adjust the disc grinding gap to zero at a rotation speed of 1200-1800rpm for 3-6 times, then adjust the disc grinding gap to a range of-30 to-60 μm for 8-12 times, finally adjust the rotation speed to 1900-2200rpm, and circularly grind the disc grinding gap to a range of-70 to-100 μm for 8-12 times, thereby obtaining the slurry subjected to the primary grinding treatment.
In the preparation method of the nano-cellulose and nano-lignin particle composite system, the ultra-fine particle grinding treatment is to adjust the disc grinding gap to zero at a rotation speed of 1500rpm, circularly grind for 5 times, adjust the disc grinding gap to be-50 μm, circularly grind for 10 times, finally adjust the rotation speed to 2000rpm, and circularly grind for 10 times at the disc grinding gap of-80 μm to obtain the primary grinding treated slurry.
According to the preparation method of the nano-cellulose and nano-lignin particle composite system, the high shear treatment condition is that the rotating speed is 25000rpm, the sample concentration of the suspension is 1 wt%, the suspension is cooled after 5 minutes of each shear treatment, and high shear treatment is carried out after the temperature is reduced to room temperature, wherein the total time of the high shear treatment is 10 minutes.
Compared with the prior art, the method comprises the steps of fibrillating a wood fiber raw material to obtain a suspension, sequentially carrying out high-pressure homogenization treatment and high-shear treatment on the suspension, and obtaining a finished product after the high-shear treatment; the method adopts a green mechanical method to prepare the composite system containing the nano-cellulose and the nano-lignin particles in a unified system, does not use chemicals, avoids environmental pollution, has simple process, low raw material cost and short treatment time, and is convenient for industrial popularization. In addition, the invention further optimizes the treatment process of the fibrillation treatment, and the size of the fibers in the pulp can be prevented from blocking the instrument. The ultrafine particle grinding of the invention can fibrillate the fiber, and a plurality of slender cellulose nanofibrils are connected with the fiber main body, wherein nano lignin particles formed by lignin after being subjected to multiple ultrafine particle grinding treatments are bonded on the surface of the cellulose. After the high-shear treatment, lignin particles adhered to the surface of the fiber can be obviously reduced, and the lignin particles can be stripped from the fiber main body; the surface of the fiber is smoother, and most of the cellulose nano-fibrils are separated from the fiber main body, and a plurality of fine fibers are intertwined and twisted under the action of high-shearing force.
Drawings
FIG. 1 is a graph of fiber and lignin morphology after ultra-fine particle milling treatment;
FIG. 2 is a graph showing a fiber size distribution after the ultra-fine particle grinding treatment;
FIG. 3 is a composite system configuration diagram of the finished product of example 5;
FIG. 4 is a composite system fiber size distribution plot for the finished product of example 5;
FIG. 5 is a morphology of the bottom fiber of the composite system after centrifugation at 5000 rpm;
FIG. 6 is a graph of the dimensional distribution of the bottom fiber of the composite system after centrifugation at 5000 rpm;
FIG. 7 is a diagram showing the morphology of the supernatant after centrifugation at 5000rpm of the complex system;
FIG. 8 is a graph of the fiber size distribution of the supernatant after centrifugation at 5000rpm of the composite system;
FIG. 9 is a bottom sediment pattern of the complex system after the second centrifugation;
FIG. 10 is a graph of fiber size distribution of the bottom pellet of the composite system after the second centrifugation treatment;
FIG. 11 is a diagram of the complex system in a second centrifugation supernatant;
FIG. 12 is a graph of the fiber size distribution of the composite system on the second centrifugation supernatant.
Detailed Description
The invention is further illustrated by the following figures and examples, which are not to be construed as limiting the invention.
Example 1: a preparation method of a nano-cellulose and nano-lignin particle composite system comprises the steps of fibrillating a wood fiber raw material to obtain a suspension, and sequentially carrying out high-pressure homogenization treatment and high-shear treatment on the suspension to obtain a finished product; wherein the high shear treatment condition is that the rotating speed is 28000rpm, the sample concentration of the suspension is 2 wt%, the suspension is put into the reactor to be cooled after 4 minutes of each shear treatment, and the high shear treatment is carried out again after the temperature is reduced to the room temperature, and the total time of the high shear treatment is 12 minutes.
Example 2: a preparation method of a nano-cellulose and nano-lignin particle composite system comprises the steps of fibrillating a wood fiber raw material to obtain a suspension, and sequentially carrying out high-pressure homogenization treatment and high-shear treatment on the suspension to obtain a finished product; the fibrillation treatment comprises the steps of soaking a wood fiber raw material in water to obtain a slurry with the concentration of 0.8 wt%, disintegrating paper pulp by a beater for 1.5h, carrying out superfine particle grinding treatment on the disintegrated slurry to obtain a primary grinded slurry, and circularly grinding the primary grinded slurry for 35 times under the condition that a disc grinding gap is-90 mu m to obtain a suspension; the high shear treatment condition is that the rotating speed is 28000rpm, the sample concentration of the suspension is 2 wt%, the suspension is put into the reactor to be cooled after 4 minutes of each shear treatment, the high shear treatment is carried out again after the temperature is reduced to the room temperature, and the total time of the high shear treatment is 12 minutes.
Example 3: a preparation method of a nano-cellulose and nano-lignin particle composite system comprises the steps of fibrillating a wood fiber raw material to obtain a suspension, and sequentially carrying out high-pressure homogenization treatment and high-shear treatment on the suspension to obtain a finished product; the fibrillation treatment comprises the steps of soaking a wood fiber raw material in water to obtain slurry with the concentration of 1.0 wt%, disintegrating paper pulp by a beater for 1h, carrying out superfine particle grinding treatment on the disintegrated slurry to obtain primary grinded slurry, and circularly grinding the primary grinded slurry for 40 times under the condition that a disc grinding gap is-100 mu m to obtain suspension; the high shear treatment condition is that the rotating speed is 25000rpm, the sample concentration of the suspension is 1 wt%, the suspension is put into the reactor to be cooled after 5 minutes of each shear treatment, and high shear treatment is carried out after the temperature is reduced to the room temperature, wherein the total time of the high shear treatment is 10 minutes.
Example 4: a preparation method of a nano-cellulose and nano-lignin particle composite system comprises the steps of fibrillating a wood fiber raw material to obtain a suspension, and sequentially carrying out high-pressure homogenization treatment and high-shear treatment on the suspension to obtain a finished product; the fibrillation treatment comprises the steps of soaking a wood fiber raw material in water to obtain slurry with the concentration of 1.0 wt%, disintegrating paper pulp by a beater for 1h, carrying out superfine particle grinding treatment on the disintegrated slurry to obtain primary grinded slurry, and circularly grinding the primary grinded slurry for 40 times under the condition that a disc grinding gap is-100 mu m to obtain suspension; the ultra-fine particle grinding treatment is to adjust the disc grinding gap to zero at the rotating speed of 1400rpm, grind the disc grinding gap circularly for 6 times, adjust the disc grinding gap to 40 microns, grind the disc grinding gap circularly for 8 times, finally adjust the rotating speed to 2100rpm, grind the disc grinding gap circularly for 10 times to obtain the slurry subjected to primary grinding treatment; the high shear treatment condition is that the rotating speed is 25000rpm, the sample concentration of the suspension is 1 wt%, the suspension is put into the reactor to be cooled after 5 minutes of each shear treatment, and high shear treatment is carried out after the temperature is reduced to the room temperature, wherein the total time of the high shear treatment is 10 minutes.
Example 5: a preparation method of a nano-cellulose and nano-lignin particle composite system comprises the steps of fibrillating a wood fiber raw material to obtain a suspension, and sequentially carrying out high-pressure homogenization treatment and high-shear treatment on the suspension to obtain a finished product; the fibrillation treatment comprises the steps of cutting a wood fiber raw material into a pulp crushing plate with the size of 5cm multiplied by 5cm, soaking the pulp crushing plate in water for 24 hours, then crushing paper pulp with the concentration of 1 wt% by using a tile power beater, wherein the beating time is 1 hour, the crushed pulp is subjected to superfine particle grinding treatment to obtain pulp subjected to primary grinding treatment, and then the pulp subjected to the primary grinding treatment is subjected to circulating grinding treatment for 40 times under the condition that the disc grinding gap is-100 mu m to obtain suspension; the ultra-fine particle grinding treatment is to adjust the disc grinding clearance to zero at the rotating speed of 1500rpm, circularly grind for 5 times, adjust the disc grinding clearance to be 50 microns, circularly grind for 10 times, finally adjust the rotating speed to 2000rpm, and circularly grind for 10 times at the disc grinding clearance of 80 microns to obtain the slurry subjected to primary grinding treatment; the high shear treatment condition is that the rotating speed is 25000rpm, the sample concentration of the suspension is 1 wt%, the suspension is put into the reactor to be cooled after 5 minutes of each shear treatment, and high shear treatment is carried out after the temperature is reduced to the room temperature, wherein the total time of the high shear treatment is 10 minutes.
The applicant has observed the morphology and size distribution of the fibers and lignins obtained from example 5, as shown in fig. 1 and 2, and it can be seen from fig. 1 and 2 that after the ultra-fine grinding treatment, part of the fibers are fibrillated and a plurality of elongated cellulose nanofibrils are connected to the fiber bulk, wherein nano-lignin particles formed by the lignin after a plurality of ultra-fine grinding treatments are bonded to the surface of the cellulose. Further, applicants observed the morphology of the composite system and the fiber size distribution of the finished product of example 5, as shown in fig. 3 and 4, and from fig. 3 and 4, it can be seen that the high shear treatment resulted in a significant reduction in the lignin particles adhering to the surface of the fibers, indicating that the high shear treatment was able to strip the lignin particles from the bulk of the fibers; the surface of the fiber is smoother, and most of the cellulose nano-fibrils are separated from the fiber main body, and a plurality of fine fibers are intertwined and twisted under the action of high-shearing force.
Because the size difference of cellulose and lignin in the composite system is large, in order to more visually observe the appearances of the cellulose and the lignin, the composite system is subjected to centrifugal separation treatment and is centrifuged for 10min at 5000 rpm. Fig. 5 and 6 are a morphology and size distribution plot of the bottom fibers after centrifugation at 5000rpm, and it can be seen that the bottom pellet has both microfibrillar bodies of larger size and elongated nanofibrils, which are dispersed as individual entities into the system due to the high shear treatment cutting the connection between the fibrillated cellulose nanofibrils and the non-fibrillated microfibrillar bodies. FIGS. 7 and 8 are morphology and size distribution plots of the supernatant after centrifugation at 5000rpm, with the majority of the nano-lignin particles in the supernatant. The supernatant of the complex system contains lignin particles with larger sizes, and the lignin particles with larger sizes are stripped from the fiber main body under the action of high shearing force, so that the lignin particles are dispersed in the system. And centrifuging the supernatant obtained by centrifuging the composite system at 5000rpm again, wherein the rotation speed of the second centrifugation is 10000rpm, the centrifugation time is 10min, and respectively representing the bottom layer precipitate and the supernatant. Fig. 9 and 10 are a morphology and size distribution graph of the bottom sediment after the second centrifugation, and it can be seen that the centrifugation at 10000rpm contained smaller sized LCNFs in the bottom sediment and the presence of significant nano-lignin particles on the surface, these small sized LCNFs also being formed by the cutting action during the high shear treatment. FIGS. 11 and 12 are a morphology and size distribution diagram of the supernatant of the second centrifugation, and the size of nano-lignin particles in the supernatant obtained by centrifugation at 10000rpm was uniform. The method is proved to successfully prepare the composite system containing nano-cellulose and nano-lignin particles by centrifuging and characterizing the composite system combining ultra-fine particle grinding with high shear treatment.
In summary, the method comprises the steps of fibrillating a wood fiber raw material to obtain a suspension, and then sequentially carrying out high-pressure homogenization treatment and high-shear treatment on the suspension to obtain a finished product; the method adopts a green mechanical method to prepare the composite system containing the nano-cellulose and the nano-lignin particles in a unified system, does not use chemicals, avoids environmental pollution, has simple process, low raw material cost and short treatment time, and is convenient for industrial popularization.
Claims (7)
1. A preparation method of a nano-cellulose and nano-lignin particle composite system is characterized by comprising the following steps: fibrillating a wood fiber raw material to obtain a suspension, and then carrying out high shear treatment on the suspension to obtain a finished product; wherein the high shear treatment condition is that the rotating speed is 20000-30000rpm, the sample concentration of the suspension is 0.5-3 wt%, the suspension is put into the container to be cooled after 3-7 minutes of each shear treatment, the high shear treatment is carried out again after the temperature is cooled to room temperature, and the total time of the high shear treatment is 8-15 minutes.
2. The method of claim 1, wherein the nanocellulose and nanocellulose particle composite system is produced by: the fibrillation treatment is to soak the wood fiber raw material in water to obtain pulp with the concentration of 0.8-1.2 wt%, to disintegrate pulp by a beater for 0.5-2h, to obtain the pulp after the disintegration treatment by ultra-fine grinding treatment, to circularly grind the pulp after the preliminary grinding treatment for 35-45 times under the condition that the disc grinding gap is-80 mu m to-120 mu m, to obtain the suspension.
3. The method of claim 1, wherein the nanocellulose and nanocellulose particle composite system is produced by: the fibrillation treatment is to soak the wood fiber raw material in water to obtain pulp with the concentration of 1.0 wt%, to disintegrate the paper pulp by a beater for 1h, to obtain the pulp subjected to the superfine grinding treatment, to circularly grind the pulp subjected to the preliminary grinding treatment for 40 times under the condition that the disc grinding gap is-100 mu m, to obtain the suspension.
4. The method for preparing a composite system of nanocellulose and nanocellulose particles according to claim 2 or 3, characterized in that: cutting the wood fiber raw material into a pulp crushing plate with the size of 5cm multiplied by 5cm, soaking the pulp crushing plate in water for 24h, and then obtaining the pulp with the concentration of 1 wt%.
5. The method for preparing a composite system of nanocellulose and nanocellulose particles according to claim 2 or 3, characterized in that: the ultra-fine particle grinding treatment is to adjust the disc grinding clearance to zero, rotate at 1800rpm of 1200-.
6. The method of claim 5, wherein the nanocellulose and nanocellulose particle composite system is produced by: the ultra-fine particle grinding treatment is to adjust the disc grinding clearance to zero at the rotating speed of 1500rpm, circularly grind for 5 times, adjust the disc grinding clearance to be 50 microns, circularly grind for 10 times, finally adjust the rotating speed to 2000rpm, and circularly grind for 10 times at the disc grinding clearance of 80 microns to obtain the slurry for primary grinding treatment.
7. The method of claim 1, wherein the nanocellulose and nanocellulose particle composite system is produced by: the high shear treatment condition is that the rotating speed is 25000rpm, the sample concentration of the suspension is 1 wt%, the suspension is placed for cooling after every 5 minutes of shear treatment, high shear treatment is carried out after the temperature is reduced to the room temperature, and the total time of the high shear treatment is 10 minutes.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116356607A (en) * | 2023-03-01 | 2023-06-30 | 仲恺农业工程学院 | High-barrier cellulose-based paper packaging material and preparation method and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116356607A (en) * | 2023-03-01 | 2023-06-30 | 仲恺农业工程学院 | High-barrier cellulose-based paper packaging material and preparation method and application thereof |
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