CN105860470A - Composite food packaging material with polylactic acid and method for preparing composite food packaging material - Google Patents
Composite food packaging material with polylactic acid and method for preparing composite food packaging material Download PDFInfo
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- CN105860470A CN105860470A CN201610295250.1A CN201610295250A CN105860470A CN 105860470 A CN105860470 A CN 105860470A CN 201610295250 A CN201610295250 A CN 201610295250A CN 105860470 A CN105860470 A CN 105860470A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/04—Polyesters derived from hydroxycarboxylic acids, e.g. lactones
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention provides a composite food packaging material with polylactic acid and a method for preparing the composite food packaging material. The method includes mixing microcrystalline celluloses and water with one another to obtain a mixture, placing the mixture in ice-water bath, stirring the mixture by the aid of a magnetic stirrer, simultaneously adding concentrated sulfuric acid into the first mixtures drop by drop, taking the mixture out of the ice-water bath after the concentrated sulfuric acid is completely added drop by drop, continuing to stir the mixture, placing the mixture in a centrifugal machine, centrifuging the mixture, removing supernatant, repeatedly carrying out previous procedures by three times, then carrying out ultrasonic treatment on the mixture and regulating the PH (potential of hydrogen) of the mixture until the mixture is neutral; adding polyethylene glycol into the mixture, and stirring, then filtering and drying the polyethylene glycol and the mixture to obtain substances; mixing the substances, the polylactic acid, poly-acyl and ester copolymers, polyhydroxybutyrate, carrageenan, 3, 4-dihydroxy benzaldehyde, phosphatidylcholine, phosphatidylethanolamine, citric acid, erucamide, beeswax and 5-hydroxymethylfurfural with one another to obtain second mixtures, dispersing the second mixtures in a high-speed dispersion machine, then ultimately adding the second mixtures into a Banbury mixer and mixing the second mixtures to obtain the composite food packaging material. The composite food packaging material with the polylactic acid and the method have the advantages that the composite food packaging material is made of the polylactic acid, is good in biodegradation, free of environmental pollution and excellent in mechanical property and impact resistance and is green and environmentally friendly.
Description
Technical field
The present invention relates to packaging material field, be specifically related to a kind of PLA Composite food packaging and preparation method thereof.
Background technology
Economical fast development, the most severe and philosophy of life the transformation day by day short, environment of resource make people also there occurs great change for the consumption concept of food, people do not require nothing more than the healthy and safe property of food now, also require that the healthy and safe property of its packaging material simultaneously.Although at present food constantly develops towards green health, but step also do not caught up with by packaging material, and major part food is still using disposable plastic articles for use, with the presence of the material even using some potential hazards and toxicity.On the other hand, due to difficult degradation and the non-biodegradable of disposable plastic, had resulted in serious " white ", not only have impact on the attractive in appearance of city, it is often more important that badly influenced environment and quality of life.Further, since with the addition of some harmful substances in the plastic, especially human body is caused harm.Therefore, researching and developing environmental protection packaging material, for solving these problems, protect environment, the healthy and safe level improving people further has great importance.
Summary of the invention
Solve the technical problem that:It is an object of the invention to provide a kind of PLA Composite food packaging with PLA as raw material, have good biological degradability, degradation speed is fast, environmentally safe, and environmental protection has good mechanical property and shock resistance simultaneously.
Technical scheme:A kind of PLA Composite food packaging, be prepared from weight portion by following component: PLA 50-70 part, polyamides resin copolymer 5-10 part, poly butyric ester 5-10 part, carragheen 0.2-0.4 part, polyethylene glycol 7-15 part, 3,4-4-dihydroxy benzaldehyde 0.1-0.2 part, phosphatid ylcholine 1-2 part, phosphatidyl ethanolamine 0.5-1 part, citric acid 0.1-0.2 part, microcrystalline cellulose 5-10 part, erucyl amide 0.5-1 part, beeswax 0.2-0.5 part, 5 hydroxymethyl furfural 0.1-0.2 part, concentrated sulfuric acid 4-8 part, water 10-20 part.
Further preferred, described a kind of PLA Composite food packaging, it is prepared from weight portion by following component: PLA 55-65 part, polyamides resin copolymer 6-9 part, poly butyric ester 6-9 part, carragheen 0.25-0.35 part, polyethylene glycol 9-13 part, 3, 4-4-dihydroxy benzaldehyde 0.11-0.16 part, phosphatid ylcholine 1.2-1.8 part, phosphatidyl ethanolamine 0.6-0.8 part, citric acid 0.11-0.17 part, microcrystalline cellulose 6-9 part, erucyl amide 0.6-0.9 part, beeswax 0.3-0.4 part, 5 hydroxymethyl furfural 0.12-0.16 part, concentrated sulfuric acid 5-7 part, water 12-18 part.
The preparation method of above-mentioned PLA Composite food packaging comprises the following steps:
Step 1: microcrystalline cellulose and water are mixed and is placed in ice-water bath, stir under rotating speed 50-80r/min with magnetic stirrer, be simultaneously added dropwise the concentrated sulfuric acid, take out from ice-water bath after dripping off, continue stirring 15-20 minute；
Step 2: put in centrifuge, is centrifuged 8-12 minute under rotating speed 11000-13000rpm, removes supernatant, be repeated 3 times；
Step 3: put in Ultrasound Instrument ultrasonic 30-40 minute, regulation PH is to neutral；
Step 4: add polyethylene glycol, stir 2-3 hour under rotating speed 60-80r/min with magnetic stirrer；
Step 5: filter, puts in vacuum drying chamber and is dried 10-12 hour；
Step 6: mixed by all components, to disperse 1-3 minute under rotating speed 6000-8000rpm in high speed dispersor；
Step 7: add in banbury, at temperature 160-180 DEG C, rotating speed 25-35rpm mixing 5 minutes and get final product.
It is further preferred that step 1 medium speed is 60-70r/min, mixing time is 16-19 minute.
It is further preferred that step 2 medium speed is 12000rpm, the time is 9-11 minute.
It is further preferred that ultrasonic time is 32-36 minute in step 3.
It is further preferred that step 4 medium speed is 65-75r/min, the time is 2.2-2.8 hour.
It is further preferred that in step 5 drying time be 10.5-11.5 hour.
It is further preferred that step 6 medium speed is 6500-7500rpm, jitter time is 2 minutes.
It is further preferred that temperature is 165-175 DEG C in step 7, rotating speed is 30rpm.
Beneficial effect:The PLA Composite food packaging of the present invention is with PLA as raw material, there is good biological degradability, degradation speed is fast, environmentally safe, environmental protection, there is good mechanical property simultaneously, its hot strength is maximum up to 36.4MPa, break-draw strain rate is 159%, and elasticity and toughness are good, and impact strength is up to 5.140KJ/m simultaneously2, there is excellent impact resistance.
Detailed description of the invention
Embodiment 1
A kind of PLA Composite food packaging, be prepared from weight portion by following component: PLA 70 parts, polyamides resin copolymer 10 parts, poly butyric ester 10 parts, carragheen 0.4 part, polyethylene glycol 15 parts, 3,4-4-dihydroxy benzaldehyde 0.2 part, phosphatid ylcholine 2 parts, phosphatidyl ethanolamine 1 part, citric acid 0.2 part, microcrystalline cellulose 10 parts, erucyl amide 1 part, 0.5 part of beeswax, 5 hydroxymethyl furfural 0.2 part, the concentrated sulfuric acid 8 parts, 20 parts of water.
The preparation method of above-mentioned PLA Composite food packaging is: first microcrystalline cellulose and water is mixed and is placed in ice-water bath, stirs with magnetic stirrer, be simultaneously added dropwise the concentrated sulfuric acid, take out after dripping off from ice-water bath, continue stirring 20 minutes under rotating speed 80r/min；Put in centrifuge, it is centrifuged 12 minutes under rotating speed 13000rpm, remove supernatant, it is repeated 3 times, placing in Ultrasound Instrument ultrasonic 40 minutes, regulation PH, to neutral, is subsequently adding polyethylene glycol, stir 3 hours under rotating speed 80r/min with magnetic stirrer, put into after filtration in vacuum drying chamber and be dried 12 hours；All components is mixed, to disperse 3 minutes under rotating speed 8000rpm in high speed dispersor, is eventually adding in banbury, temperature 180 DEG C, under rotating speed 35rpm mixing 5 minutes and get final product.
Embodiment 2
A kind of PLA Composite food packaging, be prepared from weight portion by following component: PLA 65 parts, polyamides resin copolymer 9 parts, poly butyric ester 9 parts, carragheen 0.35 part, polyethylene glycol 13 parts, 3,4-4-dihydroxy benzaldehyde 0.16 part, phosphatid ylcholine 1.8 parts, phosphatidyl ethanolamine 0.8 part, citric acid 0.17 part, microcrystalline cellulose 9 parts, erucyl amide 0.9 part, 0.4 part of beeswax, 5 hydroxymethyl furfural 0.16 part, the concentrated sulfuric acid 7 parts, 18 parts of water.
The preparation method of above-mentioned PLA Composite food packaging is: first microcrystalline cellulose and water is mixed and is placed in ice-water bath, stirs with magnetic stirrer, be simultaneously added dropwise the concentrated sulfuric acid, take out after dripping off from ice-water bath, continue stirring 19 minutes under rotating speed 70r/min；Put in centrifuge, it is centrifuged 11 minutes under rotating speed 12000rpm, remove supernatant, it is repeated 3 times, placing in Ultrasound Instrument ultrasonic 36 minutes, regulation PH, to neutral, is subsequently adding polyethylene glycol, stir 2.8 hours under rotating speed 75r/min with magnetic stirrer, put into after filtration in vacuum drying chamber and be dried 11.5 hours；All components is mixed, to disperse 2 minutes under rotating speed 7500rpm in high speed dispersor, is eventually adding in banbury, temperature 175 DEG C, under rotating speed 30rpm mixing 5 minutes and get final product.
Embodiment 3
A kind of PLA Composite food packaging, be prepared from weight portion by following component: PLA 60 parts, polyamides resin copolymer 7.5 parts, poly butyric ester 7.5 parts, carragheen 0.3 part, polyethylene glycol 12 parts, 3,4-4-dihydroxy benzaldehyde 0.15 part, phosphatid ylcholine 1.5 parts, phosphatidyl ethanolamine 0.75 part, citric acid 0.15 part, microcrystalline cellulose 7.5 parts, erucyl amide 0.75 part, 0.35 part of beeswax, 5 hydroxymethyl furfural 0.15 part, the concentrated sulfuric acid 6 parts, 15 parts of water.
The preparation method of above-mentioned PLA Composite food packaging is: first microcrystalline cellulose and water is mixed and is placed in ice-water bath, stirs with magnetic stirrer, be simultaneously added dropwise the concentrated sulfuric acid, take out after dripping off from ice-water bath, continue stirring 17 minutes under rotating speed 65r/min；Put in centrifuge, it is centrifuged 10 minutes under rotating speed 12000rpm, remove supernatant, it is repeated 3 times, placing in Ultrasound Instrument ultrasonic 35 minutes, regulation PH, to neutral, is subsequently adding polyethylene glycol, stir 2.5 hours under rotating speed 70r/min with magnetic stirrer, put into after filtration in vacuum drying chamber and be dried 11 hours；All components is mixed, to disperse 2 minutes under rotating speed 7000rpm in high speed dispersor, is eventually adding in banbury, temperature 170 DEG C, under rotating speed 30rpm mixing 5 minutes and get final product.
Embodiment 4
A kind of PLA Composite food packaging, be prepared from weight portion by following component: PLA 55 parts, polyamides resin copolymer 6 parts, poly butyric ester 6 parts, carragheen 0.25 part, polyethylene glycol 9 parts, 3,4-4-dihydroxy benzaldehyde 0.11 part, phosphatid ylcholine 1.2 parts, phosphatidyl ethanolamine 0.6 part, citric acid 0.11 part, microcrystalline cellulose 6 parts, erucyl amide 0.6 part, 0.3 part of beeswax, 5 hydroxymethyl furfural 0.12 part, the concentrated sulfuric acid 5 parts, 12 parts of water.
The preparation method of above-mentioned PLA Composite food packaging is: first microcrystalline cellulose and water is mixed and is placed in ice-water bath, stirs with magnetic stirrer, be simultaneously added dropwise the concentrated sulfuric acid, take out after dripping off from ice-water bath, continue stirring 16 minutes under rotating speed 60r/min；Put in centrifuge, it is centrifuged 9 minutes under rotating speed 12000rpm, remove supernatant, it is repeated 3 times, placing in Ultrasound Instrument ultrasonic 32 minutes, regulation PH, to neutral, is subsequently adding polyethylene glycol, stir 2.2 hours under rotating speed 65r/min with magnetic stirrer, put into after filtration in vacuum drying chamber and be dried 10.5 hours；All components is mixed, to disperse 2 minutes under rotating speed 6500rpm in high speed dispersor, is eventually adding in banbury, temperature 165 DEG C, under rotating speed 30rpm mixing 5 minutes and get final product.
Embodiment 5
A kind of PLA Composite food packaging, be prepared from weight portion by following component: PLA 50 parts, polyamides resin copolymer 5 parts, poly butyric ester 5 parts, carragheen 0.2 part, polyethylene glycol 7 parts, 3,4-4-dihydroxy benzaldehyde 0.1 part, phosphatid ylcholine 1 part, phosphatidyl ethanolamine 0.5 part, citric acid 0.1 part, microcrystalline cellulose 5 parts, erucyl amide 0.5 part, 0.2 part of beeswax, 5 hydroxymethyl furfural 0.1 part, the concentrated sulfuric acid 4 parts, 10 parts of water.
The preparation method of above-mentioned PLA Composite food packaging is: first microcrystalline cellulose and water is mixed and is placed in ice-water bath, stirs with magnetic stirrer, be simultaneously added dropwise the concentrated sulfuric acid, take out after dripping off from ice-water bath, continue stirring 15 minutes under rotating speed 50r/min；Put in centrifuge, it is centrifuged 8 minutes under rotating speed 11000rpm, remove supernatant, it is repeated 3 times, placing in Ultrasound Instrument ultrasonic 30 minutes, regulation PH, to neutral, is subsequently adding polyethylene glycol, stir 2 hours under rotating speed 60r/min with magnetic stirrer, put into after filtration in vacuum drying chamber and be dried 10 hours；All components is mixed, to disperse 1 minute under rotating speed 6000rpm in high speed dispersor, is eventually adding in banbury, temperature 160 DEG C, under rotating speed 25rpm mixing 5 minutes and get final product.
Comparative example 1
The present embodiment is not contain phosphatid ylcholine and phosphatidyl ethanolamine with the difference of embodiment 5.Specifically:
A kind of PLA Composite food packaging, be prepared from weight portion by following component: PLA 50 parts, polyamides resin copolymer 5 parts, poly butyric ester 5 parts, carragheen 0.2 part, polyethylene glycol 7 parts, 3,4-4-dihydroxy benzaldehyde 0.1 part, citric acid 0.1 part, microcrystalline cellulose 5 parts, erucyl amide 0.5 part, 0.2 part of beeswax, 5 hydroxymethyl furfural 0.1 part, the concentrated sulfuric acid 4 parts, 10 parts of water.
The preparation method of above-mentioned PLA Composite food packaging is: first microcrystalline cellulose and water is mixed and is placed in ice-water bath, stirs with magnetic stirrer, be simultaneously added dropwise the concentrated sulfuric acid, take out after dripping off from ice-water bath, continue stirring 15 minutes under rotating speed 50r/min；Put in centrifuge, it is centrifuged 8 minutes under rotating speed 11000rpm, remove supernatant, it is repeated 3 times, placing in Ultrasound Instrument ultrasonic 30 minutes, regulation PH, to neutral, is subsequently adding polyethylene glycol, stir 2 hours under rotating speed 60r/min with magnetic stirrer, put into after filtration in vacuum drying chamber and be dried 10 hours；All components is mixed, to disperse 1 minute under rotating speed 6000rpm in high speed dispersor, is eventually adding in banbury, temperature 160 DEG C, under rotating speed 25rpm mixing 5 minutes and get final product.
Comparative example 2
The present embodiment is not contain erucyl amide and beeswax with the difference of embodiment 5.Specifically:
A kind of PLA Composite food packaging, be prepared from weight portion by following component: PLA 50 parts, polyamides resin copolymer 5 parts, poly butyric ester 5 parts, carragheen 0.2 part, polyethylene glycol 7 parts, 3,4-4-dihydroxy benzaldehyde 0.1 part, phosphatid ylcholine 1 part, phosphatidyl ethanolamine 0.5 part, citric acid 0.1 part, microcrystalline cellulose 5 parts, 5 hydroxymethyl furfural 0.1 part, the concentrated sulfuric acid 4 parts, 10 parts of water.
The preparation method of above-mentioned PLA Composite food packaging is: first microcrystalline cellulose and water is mixed and is placed in ice-water bath, stirs with magnetic stirrer, be simultaneously added dropwise the concentrated sulfuric acid, take out after dripping off from ice-water bath, continue stirring 15 minutes under rotating speed 50r/min；Put in centrifuge, it is centrifuged 8 minutes under rotating speed 11000rpm, remove supernatant, it is repeated 3 times, placing in Ultrasound Instrument ultrasonic 30 minutes, regulation PH, to neutral, is subsequently adding polyethylene glycol, stir 2 hours under rotating speed 60r/min with magnetic stirrer, put into after filtration in vacuum drying chamber and be dried 10 hours；All components is mixed, to disperse 1 minute under rotating speed 6000rpm in high speed dispersor, is eventually adding in banbury, temperature 160 DEG C, under rotating speed 25rpm mixing 5 minutes and get final product.
The performance indications of material of the present invention are as follows, it may be seen that the present invention has good mechanical property, from most preferred embodiment 2 it can be seen that, its hot strength is maximum up to 36.4MPa, break-draw strain rate is 159%, and elasticity and toughness are good, and impact strength is up to 5.140KJ/m simultaneously2, there is excellent impact resistance.
The performance indications of table 1 PLA Composite food packaging
| Name of product | Hot strength (MPa) | Break-draw strain rate (%) | Impact strength (KJ/m2) |
| Embodiment 1 | 36.2 | 158 | 5.138 |
| Embodiment 2 | 36.4 | 159 | 5.140 |
| Embodiment 3 | 36.2 | 158 | 5.137 |
| Embodiment 4 | 36.1 | 157 | 5.136 |
| Embodiment 5 | 36.1 | 156 | 5.134 |
| Comparative example 1 | 35.8 | 153 | 4.249 |
| Comparative example 2 | 32.2 | 135 | 5.102 |
Claims (10)
1. a PLA Composite food packaging, it is characterized in that: be prepared from weight portion by following component: PLA 50-70 part, polyamides resin copolymer 5-10 part, poly butyric ester 5-10 part, carragheen 0.2-0.4 part, polyethylene glycol 7-15 part, 3,4-4-dihydroxy benzaldehyde 0.1-0.2 part, phosphatid ylcholine 1-2 part, phosphatidyl ethanolamine 0.5-1 part, citric acid 0.1-0.2 part, microcrystalline cellulose 5-10 part, erucyl amide 0.5-1 part, beeswax 0.2-0.5 part, 5 hydroxymethyl furfural 0.1-0.2 part, concentrated sulfuric acid 4-8 part, water 10-20 part.
A kind of PLA Composite food packaging the most according to claim 1, it is characterized in that: be prepared from weight portion by following component: PLA 55-65 part, polyamides resin copolymer 6-9 part, poly butyric ester 6-9 part, carragheen 0.25-0.35 part, polyethylene glycol 9-13 part, 3, 4-4-dihydroxy benzaldehyde 0.11-0.16 part, phosphatid ylcholine 1.2-1.8 part, phosphatidyl ethanolamine 0.6-0.8 part, citric acid 0.11-0.17 part, microcrystalline cellulose 6-9 part, erucyl amide 0.6-0.9 part, beeswax 0.3-0.4 part, 5 hydroxymethyl furfural 0.12-0.16 part, concentrated sulfuric acid 5-7 part, water 12-18 part.
3. the preparation method of a kind of PLA Composite food packaging described in any one of claim 1 to 2, it is characterised in that: comprise the following steps:
Step 1: microcrystalline cellulose and water are mixed and is placed in ice-water bath, stir under rotating speed 50-80r/min with magnetic stirrer, be simultaneously added dropwise the concentrated sulfuric acid, take out from ice-water bath after dripping off, continue stirring 15-20 minute；
Step 2: put in centrifuge, is centrifuged 8-12 minute under rotating speed 11000-13000rpm, removes supernatant, be repeated 3 times；
Step 3: put in Ultrasound Instrument ultrasonic 30-40 minute, regulation PH is to neutral；
Step 4: add polyethylene glycol, stir 2-3 hour under rotating speed 60-80r/min with magnetic stirrer；
Step 5: filter, puts in vacuum drying chamber and is dried 10-12 hour；
Step 6: mixed by all components, to disperse 1-3 minute under rotating speed 6000-8000rpm in high speed dispersor；
Step 7: add in banbury, at temperature 160-180 DEG C, rotating speed 25-35rpm mixing 5 minutes and get final product.
The preparation method of a kind of PLA Composite food packaging the most according to claim 3, it is characterised in that: described step 1 medium speed is 60-70r/min, and mixing time is 16-19 minute.
The preparation method of a kind of PLA Composite food packaging the most according to claim 3, it is characterised in that: described step 2 medium speed is 12000rpm, and the time is 9-11 minute.
The preparation method of a kind of PLA Composite food packaging the most according to claim 3, it is characterised in that: in described step 3, ultrasonic time is 32-36 minute.
The preparation method of a kind of PLA Composite food packaging the most according to claim 3, it is characterised in that: described step 4 medium speed is 65-75r/min, and the time is 2.2-2.8 hour.
The preparation method of a kind of PLA Composite food packaging the most according to claim 3, it is characterised in that: in described step 5, drying time is 10.5-11.5 hour.
The preparation method of a kind of PLA Composite food packaging the most according to claim 3, it is characterised in that: described step 6 medium speed is 6500-7500rpm, and jitter time is 2 minutes.
The preparation method of a kind of PLA Composite food packaging the most according to claim 3, it is characterised in that: in described step 7, temperature is 165-175 DEG C, and rotating speed is 30rpm.
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| CN201610295250.1A CN105860470A (en) | 2016-05-06 | 2016-05-06 | Composite food packaging material with polylactic acid and method for preparing composite food packaging material |
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| CN201610295250.1A CN105860470A (en) | 2016-05-06 | 2016-05-06 | Composite food packaging material with polylactic acid and method for preparing composite food packaging material |
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Cited By (1)
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| CN106496984A (en) * | 2016-11-18 | 2017-03-15 | 郑州丽福爱生物技术有限公司 | A kind of food packaging degradation material and preparation method thereof |
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