CN111304766A - Functional modifier containing tea polyphenol, tea polyphenol modified polyamide fiber and preparation method thereof - Google Patents
Functional modifier containing tea polyphenol, tea polyphenol modified polyamide fiber and preparation method thereof Download PDFInfo
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- CN111304766A CN111304766A CN202010250952.4A CN202010250952A CN111304766A CN 111304766 A CN111304766 A CN 111304766A CN 202010250952 A CN202010250952 A CN 202010250952A CN 111304766 A CN111304766 A CN 111304766A
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- tea polyphenol
- chinlon
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- polyamide fiber
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
Abstract
The invention discloses a functional modifier containing tea polyphenol, which comprises the following raw materials: tea polyphenol, montmorillonite, zeolite powder, aerogel and porous nano TiO2/SiO2 microspheres. Simultaneously discloses a preparation method of the tea polyphenol modified polyamide fiber, which comprises the following steps: preparing functional master batch containing tea polyphenol, mixing and spinning chinlon 6 or chinlon 66 slices and the functional master batch containing the tea polyphenol to prepare the tea polyphenol modified chinlon fiber. The invention has simple process and convenient control.
Description
Technical Field
The invention relates to the technical field of chemical fibers, in particular to a tea polyphenol-containing functional modifier, tea polyphenol-modified polyamide fiber and a preparation method thereof.
Background
Chinlon, a known name of polyamide fiber, is a general name of polyamide fiber produced in China. Is internationally called nylon. High strength, high antiwear performance and high resilience, and may be used in spinning and blending to produce various kinds of clothing and knitwear. The main varieties are nylon 6 and nylon 66, and the physical properties of the nylon 6 and the nylon 66 are not much different. The moisture absorption and dyeing property of chinlon are better than those of terylene, and the chinlon is alkali-resistant but not acid-resistant, and the fiber strength of the chinlon can be reduced after long-term exposure to sunlight. The nylon has heat setting property, and can keep the bending deformation formed during heating. The long filament of nylon can be made into stretch yarn, and the short filament can be blended with cotton and acrylic fibre to raise its strength and elasticity.
The nylon has various varieties, including nylon 6, nylon 66, nylon 11 and nylon 610, wherein the most important nylon 66 and nylon 6 are adopted. It is widely used in industry such as cord, transmission belt, hose, rope, fishing net, etc. The nanometer nylon has the advantages of higher thermal performance, mechanical performance, fire resistance and barrier property than pure nylon, and the manufacturing cost is equivalent to that of common nylon.
In order to improve the physical and chemical properties of nylon and increase the clothes function, people modify nylon fibers, and the types of the conventional modified nylon fibers are not rich enough.
Currently, CN201810553400.3 discloses a preparation process of a tea polyphenol modified viscose fiber, which comprises the steps of using commercially available tea polyphenols and viscose fibers as raw materials, pretreating the viscose fibers by preparing a surfactant, preparing cellulase hydrolyzed viscose fibers, preparing adsorbed tea polyphenol viscose fibers, and preparing grafted tea polyphenol viscose fibers, so as to prepare the viscose fibers with the tea polyphenol grafting rate of 8-10%. However, this method is complicated in process.
Therefore, the development of a new tea polyphenol-containing functional modifier, tea polyphenol modified polyamide fiber and a preparation method thereof not only have urgent research values, but also have good economic benefits and industrial application potentials, which are the basis of the power of the invention.
Disclosure of Invention
The present inventors have conducted intensive studies to overcome the above-identified drawbacks of the prior art, and as a result, have completed the present invention after having made a great deal of creative efforts.
Specifically, the technical problems to be solved by the present invention are: provides a functional modifier containing tea polyphenol, tea polyphenol modified polyamide fiber and a preparation method thereof, and aims to solve the technical problems.
In order to solve the technical problems, the technical scheme of the invention is as follows:
in a first aspect, the present invention provides a tea polyphenol-containing functional modifier, which comprises the following raw materials: tea polyphenol, montmorillonite, zeolite powder, aerogel and porous nano TiO2/SiO2 microspheres.
As an improvement, the functional modifier containing tea polyphenol is prepared from the following raw materials in parts by weight: 3-7 parts of tea polyphenol, 1-2 parts of montmorillonite, 0.5-0.9 part of zeolite powder, 0.4-0.6 part of aerogel and 0.1-0.3 part of porous nano TiO2/SiO2 microspheres.
As an improvement, the functional modifier containing tea polyphenol is obtained by adopting the following preparation method: weighing one or more of montmorillonite, zeolite powder, aerogel and porous nano-microspheres, adding into tea polyphenol, stirring uniformly at the speed of 20-30rad/s, and sieving with a 10000-mesh sieve to obtain a functional modifier containing tea polyphenol; the porous nano-microsphere is one or more of TiO2/SiO 2.
In the functional modifier containing tea polyphenol, the tea polyphenol is a general name of polyphenol substances in tea leaves, is white amorphous powder, and comprises the following main components: flavanones, anthocyanidins, flavonols, anthocyanins, phenolic acids and depside 6 compounds. The invention adopts the process with specific steps to prepare the tea polyphenol so as to ensure the purity:
(1) weighing green tea as a raw material, and crushing the green tea by using a crusher into powder of 100-150 meshes;
(2) adding 10-25ml/g of deionized water into the powder obtained in the step (1), performing ultrasonic extraction for 15-35 minutes at the ultrasonic power of 200-300W and the temperature of 60-80 ℃, and filtering after extraction to obtain a leaching solution A;
(3) adding 5-15ml/g of deionized water into the filter residue obtained in the step (2), performing ultrasonic extraction for 5-15 minutes at the ultrasonic power of 200-300W and the temperature of 75-90 ℃, and filtering after the extraction is finished to obtain a leaching liquor B;
(4) mixing the leaching solution A and B, and evaporating at 50-75 deg.C to obtain tea polyphenol powder.
In a second aspect, the invention provides tea polyphenol modified nylon fiber, and the preparation raw materials of the tea polyphenol modified nylon fiber at least contain the functional modifier containing tea polyphenol.
In a third aspect, the invention provides a preparation method of tea polyphenol modified polyamide fiber, which comprises the following steps: preparing functional master batch containing tea polyphenol, mixing and spinning chinlon 6 or chinlon 66 slices and the functional master batch containing the tea polyphenol to prepare the tea polyphenol modified chinlon fiber.
As an improvement, the functional master batch containing tea polyphenol is prepared by the following preparation method:
(1) weighing chinlon 6 or chinlon 66 slices, an antioxidant, a dispersant and a functional modifier containing tea polyphenol;
(2) sequentially adding the chinlon 6 or chinlon 66 slices, the antioxidant, the dispersing agent and the functional master batch containing the tea polyphenol into a double-screw extruder, mixing at a high speed, extruding and granulating to obtain the functional master batch containing the tea polyphenol.
As an improvement, the weight ratio of the chinlon 6 or chinlon 66 slices, the antioxidant, the dispersant and the tea polyphenol-containing functional modifier is 10: 0.1: 0.3: 1.3.
as an improvement, the antioxidant adopts dioctadecyl thiodipropionate.
As a refinement, the dispersant employs HPMA.
As an improvement, the mixing speed is 200-230 r/min.
As an improvement, the functional master batch containing tea polyphenol accounts for 1-8wt% of the total weight.
After the technical scheme is adopted, the invention has the beneficial effects that:
the tea polyphenol-containing functional modifier is prepared by adopting a specific process, and is sheared and mixed with montmorillonite, zeolite powder, aerogel and porous nano TiO2/SiO2 microspheres, so that the uniformity of the components is greatly improved, the tea polyphenol can be uniformly distributed on the porous nano TiO2/SiO2 microspheres and forms a nano composite material with the montmorillonite, the zeolite powder and the aerogel, and a quasi-honeycomb structure formed in the nano composite material is favorable for the next production of nylon fibers.
The preparation method of the tea polyphenol modified polyamide fiber adopted by the invention has the advantages of simple process flow and strong controllability, firstly, the functional master batch containing tea polyphenol is prepared, the uniformity and consistency of the functional modifier containing tea polyphenol in the master batch are ensured, then, the polyamide 6 or polyamide 66 slices, the antioxidant and the dispersing agent are added, the addition sequence is also very critical in practice, and the antioxidant can generate mutual influence and influence the dispersibility when the content of the functional modifier containing tea polyphenol is higher, so that after long-term test, an inventor firstly prepares the functional modifier containing tea polyphenol into the functional master batch, and then further mixes the functional modifier containing tea polyphenol with the mixture of the polyamide 6 or polyamide 66 slices, the antioxidant and the dispersing agent, and the uniformity of the tea polyphenol in the tea polyphenol modified polyamide fiber is ensured.
In conclusion, the method has the advantages of simple process flow, easy control and convenience for large-scale production.
Detailed Description
The invention is further illustrated by the following specific examples. The use and purpose of these exemplary embodiments are to illustrate the present invention, not to limit the actual scope of the present invention in any way, and not to limit the scope of the present invention in any way.
Example 1
The functional modifier containing tea polyphenol comprises the following raw materials: tea polyphenol, montmorillonite, zeolite powder, aerogel and porous nano TiO2/SiO2 microspheres, wherein the weight parts of the components are as follows: tea polyphenol 3, montmorillonite 1, zeolite powder 0.5, aerogel 0.4 and porous nano TiO2/SiO2 microspheres 0.1. The functional modifier containing tea polyphenol of the embodiment is prepared by the following preparation method: weighing montmorillonite, zeolite powder, aerogel and porous nanometer TiO2/SiO2 microspheres, then adding the montmorillonite, the zeolite powder, the aerogel and the porous nanometer TiO2/SiO2 microspheres into tea polyphenol, uniformly stirring the mixture at the speed of 20rad/s, and then sieving the mixture by a 10000-mesh sieve to obtain the functional modifier containing the tea polyphenol. In the functional modifier containing tea polyphenol, the tea polyphenol is a general name of polyphenol substances in tea leaves, is white amorphous powder, and comprises the following main components: flavanones, anthocyanidins, flavonols, anthocyanins, phenolic acids and depside 6 compounds. The invention adopts the process with specific steps to prepare the tea polyphenol so as to ensure the purity: (1) weighing green tea as raw material, and pulverizing with a pulverizer to obtain 100 mesh powder; (2) adding 10ml/g of deionized water into the powder obtained in the step (1), performing ultrasonic extraction for 15 minutes at the ultrasonic power of 200W and the temperature of 60 ℃, and filtering after the extraction is finished to obtain a leaching solution A; (3) adding 5ml/g of deionized water into the filter residue obtained in the step (2), performing ultrasonic extraction for 5 minutes at the ultrasonic power of 200W and the temperature of 75 ℃, and filtering after the extraction is finished to obtain a leaching solution B; (4) mixing the leaching solution A and the leaching solution B, and evaporating at low temperature of 50 deg.C to obtain tea polyphenol powder.
Example 2
The functional modifier containing tea polyphenol comprises the following raw materials: tea polyphenol, montmorillonite, zeolite powder, aerogel and porous nano TiO2/SiO2 microspheres, wherein the weight parts of the components are as follows: tea polyphenol 7, montmorillonite 2, zeolite powder 0.9, aerogel 0.6 and porous nano TiO2/SiO2 microspheres 0.3. The functional modifier containing tea polyphenol of the embodiment is prepared by the following preparation method: weighing montmorillonite, zeolite powder, aerogel and porous nanometer TiO2/SiO2 microspheres, then adding the montmorillonite, the zeolite powder, the aerogel and the porous nanometer TiO2/SiO2 microspheres into tea polyphenol, uniformly stirring the mixture at the speed of 30rad/s, and then sieving the mixture by a 10000-mesh sieve to obtain the functional modifier containing the tea polyphenol. In the functional modifier containing tea polyphenol, the tea polyphenol is a general name of polyphenol substances in tea leaves, is white amorphous powder, and comprises the following main components: flavanones, anthocyanidins, flavonols, anthocyanins, phenolic acids and depside 6 compounds. The invention adopts the process with specific steps to prepare the tea polyphenol so as to ensure the purity: (1) weighing green tea as raw material, and pulverizing with a pulverizer to obtain 150 mesh powder; (2) adding 25ml/g of deionized water into the powder obtained in the step (1), performing ultrasonic extraction for 35 minutes at the ultrasonic power of 300W and the temperature of 80 ℃, and filtering after the extraction is finished to obtain a leaching solution A; (3) adding 15ml/g of deionized water into the filter residue obtained in the step (2), performing ultrasonic extraction for 15 minutes at the ultrasonic power of 300W and the temperature of 90 ℃, and filtering after the extraction is finished to obtain a leaching solution B; (4) mixing the leaching solution A and the leaching solution B, and evaporating at 75 deg.C to dryness to obtain tea polyphenol powder.
Example 3
The functional modifier containing tea polyphenol comprises the following raw materials: tea polyphenol, montmorillonite, zeolite powder, aerogel and porous nano TiO2/SiO2 microspheres, wherein the weight parts of the components are as follows: tea polyphenol 5, montmorillonite 1.5, zeolite powder 0.7, aerogel 0.5, porous nano TiO2/SiO2 microspheres 0.2. The functional modifier containing tea polyphenol of the embodiment is prepared by the following preparation method: weighing montmorillonite, zeolite powder, aerogel and porous nanometer TiO2/SiO2 microspheres, then adding the montmorillonite, zeolite powder, aerogel and porous nanometer TiO2/SiO2 microspheres into tea polyphenol, uniformly stirring at the speed of 25rad/s, and then sieving by a 10000-mesh sieve to obtain the functional modifier containing the tea polyphenol. In the functional modifier containing tea polyphenol, the tea polyphenol is a general name of polyphenol substances in tea leaves, is white amorphous powder, and comprises the following main components: flavanones, anthocyanidins, flavonols, anthocyanins, phenolic acids and depside 6 compounds. The invention adopts the process with specific steps to prepare the tea polyphenol so as to ensure the purity: (1) weighing green tea as raw material, and pulverizing with a pulverizer to obtain 130 mesh powder; (2) adding 20ml/g of deionized water into the powder obtained in the step (1), performing ultrasonic extraction for 20 minutes at the ultrasonic power of 250W and the temperature of 75 ℃, and filtering after the extraction is finished to obtain a leaching solution A; (3) adding 10ml/g of deionized water into the filter residue obtained in the step (2), performing ultrasonic extraction for 10 minutes at the ultrasonic power of 260W and the temperature of 80 ℃, and filtering after the extraction is finished to obtain a leaching solution B; (4) mixing the leaching solution A and the leaching solution B, and evaporating at low temperature of 62 deg.C to obtain tea polyphenol powder.
Example 4
The tea polyphenol modified nylon fiber is characterized in that the preparation raw materials of the tea polyphenol modified nylon fiber at least contain the functional modifier containing tea polyphenol prepared in the embodiment 1. In this embodiment, the preparation method of the tea polyphenol modified polyamide fiber includes the following steps: preparing a functional master batch containing tea polyphenol: weighing chinlon 6 or chinlon 66 slices, an antioxidant, a dispersing agent and a functional modifier containing tea polyphenol, wherein the weight ratio of the chinlon 6 or chinlon 66 slices, the antioxidant, the dispersing agent and the functional modifier containing tea polyphenol is 10: 0.1: 0.3: 1.3; sequentially adding chinlon 6 or chinlon 66 slices, an antioxidant, a dispersing agent and the functional master batch containing tea polyphenol into a double-screw extruder, mixing at a high speed, mixing at a speed of 200 revolutions per minute during high-speed mixing, and performing extrusion granulation to obtain the functional master batch containing tea polyphenol; the antioxidant adopts dioctadecyl thiodipropionate; the dispersing agent adopts HPMA; the functional master batch containing tea polyphenol accounts for 1wt% of the total weight.
Example 5
The raw materials for preparing the tea polyphenol modified nylon fiber at least contain the functional modifier containing tea polyphenol prepared in the embodiment 2. In this embodiment, the preparation method of the tea polyphenol modified polyamide fiber includes the following steps: preparing a functional master batch containing tea polyphenol: weighing chinlon 6 or chinlon 66 slices, an antioxidant, a dispersing agent and a functional modifier containing tea polyphenol, wherein the weight ratio of the chinlon 6 or chinlon 66 slices, the antioxidant, the dispersing agent and the functional modifier containing tea polyphenol is 10: 0.1: 0.3: 1.3; sequentially adding chinlon 6 or chinlon 66 slices, an antioxidant, a dispersing agent and the functional master batch containing tea polyphenol into a double-screw extruder, mixing at a high speed, mixing at a speed of 230 r/min during high-speed mixing, and performing extrusion granulation to obtain the functional master batch containing tea polyphenol; the antioxidant adopts dioctadecyl thiodipropionate; the dispersing agent adopts HPMA; the functional master batch containing tea polyphenol accounts for 8wt% of the total weight.
Example 6
The tea polyphenol modified nylon fiber is characterized in that the preparation raw materials of the tea polyphenol modified nylon fiber at least contain the functional modifier containing tea polyphenol prepared in the embodiment 3. In this embodiment, the preparation method of the tea polyphenol modified polyamide fiber includes the following steps: preparing a functional master batch containing tea polyphenol: weighing chinlon 6 or chinlon 66 slices, an antioxidant, a dispersing agent and a functional modifier containing tea polyphenol, wherein the weight ratio of the chinlon 6 or chinlon 66 slices, the antioxidant, the dispersing agent and the functional modifier containing tea polyphenol is 10: 0.1: 0.3: 1.3; sequentially adding chinlon 6 or chinlon 66 slices, an antioxidant, a dispersing agent and the functional master batch containing tea polyphenol into a double-screw extruder, mixing at a high speed, mixing at a speed of 220 r/min during high-speed mixing, and performing extrusion granulation to obtain the functional master batch containing tea polyphenol; the antioxidant adopts dioctadecyl thiodipropionate; the dispersing agent adopts HPMA; the functional master batch containing tea polyphenol accounts for 5wt% of the total weight.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The tea polyphenol modified polyamide fiber is characterized in that: the tea polyphenol mass content in the tea polyphenol modified polyamide fiber is 0.1-5%; and the raw materials for preparing the tea polyphenol modified polyamide fiber at least contain the functional modifier containing tea polyphenol.
2. The functional modifier containing tea polyphenol is characterized in that: the functional modifier containing tea polyphenol comprises the following raw materials: tea polyphenol, montmorillonite, zeolite powder, aerogel and porous nano TiO2/SiO2 microspheres.
3. The functional modifier comprising tea polyphenol according to claim 1, characterized in that: the feed is prepared from the following raw materials in parts by weight: 3-7 parts of tea polyphenol, 1-2 parts of montmorillonite, 0.5-0.9 part of zeolite powder, 0.4-0.6 part of aerogel and 0.1-0.3 part of porous nano TiO2/SiO2 microspheres.
4. The tea polyphenol-containing functional modifier according to claim 1 or 2, wherein: the preparation method comprises the following steps: weighing one or more of montmorillonite, zeolite powder, aerogel and porous nano TiO2/SiO2 microspheres, adding the mixture into tea polyphenol, uniformly stirring at the speed of 20-30rad/s, and then sieving by a 10000-mesh sieve to obtain the functional modifier containing the tea polyphenol.
5. The functional modifier comprising tea polyphenol according to claim 3, characterized in that: the tea polyphenol is prepared by adopting the following process steps:
(1) weighing green tea as a raw material, and crushing the green tea by using a crusher into powder of 100-150 meshes;
(2) adding 10-25ml/g of deionized water into the powder obtained in the step (1), performing ultrasonic extraction for 15-35 minutes at the ultrasonic power of 200-300W and the temperature of 60-80 ℃, and filtering after extraction to obtain a leaching solution A;
(3) adding 5-15ml/g of deionized water into the filter residue obtained in the step (2), performing ultrasonic extraction for 5-15 minutes at the ultrasonic power of 200-300W and the temperature of 75-90 ℃, and filtering after the extraction is finished to obtain a leaching liquor B;
(4) mixing the leaching solution A and B, and evaporating at 50-75 deg.C to obtain tea polyphenol powder.
6. The preparation method of the tea polyphenol modified polyamide fiber is characterized by comprising the following steps: the method comprises the following steps: preparing functional master batch containing tea polyphenol, mixing and spinning chinlon 6 or chinlon 66 slices and the functional master batch containing the tea polyphenol to prepare the tea polyphenol modified chinlon fiber.
7. The method for preparing the tea polyphenol modified polyamide fiber as claimed in claim 6, wherein the method comprises the following steps: the functional master batch containing tea polyphenol is prepared by the following steps:
(1) weighing chinlon 6 or chinlon 66 slices, an antioxidant, a dispersant and a functional modifier containing tea polyphenol;
(2) sequentially adding the chinlon 6 or chinlon 66 slices, the antioxidant, the dispersing agent and the functional master batch containing the tea polyphenol into a double-screw extruder, mixing at a high speed, extruding and granulating to obtain the functional master batch containing the tea polyphenol.
8. The method for preparing the tea polyphenol modified polyamide fiber as claimed in claim 7, wherein the method comprises the following steps: the weight ratio of the chinlon 6 or chinlon 66 slices, the antioxidant, the dispersant and the functional modifier containing tea polyphenol is 10: 0.1: 0.3: 1.3.
9. the method for preparing the tea polyphenol modified polyamide fiber as claimed in claim 8, wherein the method comprises the following steps: the antioxidant adopts dioctadecyl thiodipropionate; the dispersant is HPMA.
10. The method for preparing the tea polyphenol modified polyamide fiber as claimed in claim 9, wherein the method comprises the following steps: the functional master batch containing tea polyphenol accounts for 1-8wt% of the total weight.
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| CN202010250952.4A CN111304766A (en) | 2020-04-01 | 2020-04-01 | Functional modifier containing tea polyphenol, tea polyphenol modified polyamide fiber and preparation method thereof |
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| CN202010250952.4A CN111304766A (en) | 2020-04-01 | 2020-04-01 | Functional modifier containing tea polyphenol, tea polyphenol modified polyamide fiber and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112144133A (en) * | 2020-09-04 | 2020-12-29 | 百事基材料（青岛）股份有限公司 | Plant functional slow-release aerogel molecular nest and preparation method thereof |
| WO2021088307A1 (en) * | 2019-11-06 | 2021-05-14 | 百事基材料（青岛）股份有限公司 | Plant functional polyester filament and preparation method therefor |
-
2020
- 2020-04-01 CN CN202010250952.4A patent/CN111304766A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021088307A1 (en) * | 2019-11-06 | 2021-05-14 | 百事基材料（青岛）股份有限公司 | Plant functional polyester filament and preparation method therefor |
| CN112144133A (en) * | 2020-09-04 | 2020-12-29 | 百事基材料（青岛）股份有限公司 | Plant functional slow-release aerogel molecular nest and preparation method thereof |
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