CN107903608A - A kind of halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material and preparation method thereof - Google Patents

A kind of halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material and preparation method thereof Download PDF

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Publication number
CN107903608A
CN107903608A CN201711443814.2A CN201711443814A CN107903608A CN 107903608 A CN107903608 A CN 107903608A CN 201711443814 A CN201711443814 A CN 201711443814A CN 107903608 A CN107903608 A CN 107903608A
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Prior art keywords
resistant
halogen
temperature
polyphenyl ether
free flame
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CN201711443814.2A
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袁伟
佘庆彦
李涛
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Zhejiang Wanma Tyco New Material Co Ltd
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Zhejiang Wanma Tyco New Material Co Ltd
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Priority to CN201711443814.2A priority Critical patent/CN107903608A/en
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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
    • C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
    • C08L71/08—Polyethers derived from hydroxy compounds or from their metallic derivatives
    • C08L71/10—Polyethers derived from hydroxy compounds or from their metallic derivatives from phenols
    • C08L71/12—Polyphenylene oxides
    • C08L71/123—Polyphenylene oxides not modified by chemical after-treatment
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/02—Flame or fire retardant/resistant
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/22—Halogen free composition
    • 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

Abstract

The invention discloses a kind of halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material and preparation method thereof, in parts by mass including following component：40 60 parts of polyphenylene oxide, 10 20 parts of polystyrene, 10 20 parts of toughener, 5 10 parts of compound flame retardant, 6 15 parts of thermoplastic polyimide, 25 parts of compatilizer, 0.3 part of antioxidant.Halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material of the present invention improves processing performance and shock resistance, reaches halogen-free flame retardant feature, improve the heat-resisting quantity of composite material on the basis of the high-mechanical property of polyphenylene oxide is ensured.Halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material has extensive use in fields such as electrotechnical, electronic, communication photovoltaics.

Description

A kind of halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material and preparation method thereof
Technical field
The present invention relates to a kind of halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material and preparation method thereof, belong to high polymer alloy Materials processing technology field.
Background technology
Polyphenylene oxide resin (Polyphenylene ether, abbreviation PPE or PPO) is one of five big general-purpose plastics, has electricity The non-crystalline type thermoplastic resin of the excellent performances such as insulating properties, heat resistance, mechanicalness, fire resistance and chemical stability.It is produced Product are widely used in the fields such as electric appliance and electronic, office equipment, auto parts and components, chemical industry.
But polyphenylene oxide is poor there are melt flow, processing and forming is difficult, easy to crack, high temperature resistant more sensitive to notch PPE and PS/HIPS, are usually blended or modification by copolymerization, improve fluidity of molten, improve processability by the shortcomings of insufficient Can, while cost is also reduced, market major product is mostly modified product (MPPE), accounts for more than the 90% of PPE yield.Traditional resistance Combustion agent is mostly the compound flame retardant of bromine system and antimony oxide, but is produced in the heavy metal and combustion process in material a large amount of Brominated toxic gas and black smoke bring huge harm to human health and environment, therefore halogen-free flameproof changes as flame retardant plastics The trend of property.The addition of polystyrene and halogen-free flame retardants greatly reduces the heat resistance of polyphenyl ether material at the same time, limits it Application in high temperature resistant field, therefore it need to be further modified and improve heat resistance.
Thermoplastic polyimide (TPI) is mostly that soft segment is introduced in polyimide structures, such as ehter bond, thioether bond, ketone Base, alicyclic structure etc., increase the compliance of polyimides, reduce its glass transition temperature, improve its processing performance, can use The conventional machining molding modes such as molding, extrusion, injection.It has prominent heat endurance, mechanical performance, electrical property, anti-flammability Can etc., the numerous areas such as automobile, aerospace are widely used in, pass through thermoplastic polyimide modified polyphenylene oxide comprehensive performance It is superior, greatly widen its application range.The particular advantages that thermoplastic polyimide is had applied to engineering plastics, CN101570634 discloses imperial 66 blends of thermoplastic polyimide modified nylon and preparation method thereof, by adding thermoplastic poly Acid imide improves the mechanical property, heat resistance and wear property of nylon 66 material.CN102234419 discloses a kind of nothing Halogen flame-retardant polyphenyl ether resin composition and preparation method thereof, using fiberglass reinforced polyphenylene oxide, using glass improve mechanical property and Heat resistance, but glass must add fine mouth to add in extruder, glass addition fraction is more, and technique is complex, at the same glass and The poor compatibility of polyphenylene oxide needs to add substantial amounts of compatilizer, causes high processing costs, and the density of thermoplastic polyimide is less than Glass, is conducive to the lighting development trend of polyphenyl ether material.
The content of the invention
The present invention is intended to provide a kind of halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material and preparation method thereof, to improve polyphenyl The mechanical strength of ether material, heat-resisting quantity and anti-flammability, so as to improve the application value of polyphenylene oxide alloy.
The present invention improves the processing performance of polyphenylene oxide with polystyrene, and the shock resistance of polyphenylene oxide is improved with toughener, The anti-flammability of polyphenylene oxide is improved by compounding halogen-free flame retardants, compatilizer improves the interfacial tension of each component material, polyphenyl The addition of ethene and fire retardant reduces the glass transition temperature of polyphenylene oxide, so that cause the heat-resisting quantity deficiency of material, this Invention improves the heat-resisting quantity of composite material by the thermoplastic polyimide added.
Halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material of the present invention, in parts by mass including following component：
The polyphenylene oxide is powdered, and the inherent viscosity in 25 DEG C of chloroforms is 0.3-0.5dL/g, and weight average molecular weight is 22000-57000。
The polystyrene is General Purpose Polystyrenre (GPPS), of low cost for improving the processing performance of polyphenylene oxide, Optimum condition, melt index is 10-20g/10min under 200 DEG C/5kg load.
The toughener is styrene-butadiene-styrene (SBS), hydrogenated styrene-butadiene-styrene Copolymer (SEBS), styrene-butadiene-isoprene block copolymer (SIS), butadiene-styrene rubber (SBR), hydrogenated styrene-butadiene rubber At least one of (HSBR), it is preferably hydrogenated styrene-butadiene-styrene copolymer (SEBS), addition SEBS can be significantly Improve the shock resistance of polyphenyl ether material.(above product is commercially available, does not have special parameter request)
The compound flame retardant is halogen-free flame retardants, is made of phosphorus flame retardant and nitrogenated flame retardant, phosphorus flame retardant Mass ratio with nitrogenated flame retardant is 2：1.
It is double (diphenyl phosphoester) that the phosphorus flame retardant is selected from bisphenol-A double (diphenyl phosphoester) (BDP), a phenol (RDP), double two (the 2,6- dimethyl of hydroquinone double (diphenyl phosphoester) (PX200), triphenyl phosphate (TPP), resorcinol At least one of phenyl) phosphate (RXP).
The nitrogenated flame retardant is selected from melamine (PPA), melamine polyphosphate (MPP), melamine cyanurate At least one of salt (MCA).
The thermoplastic polyimide preferred thermoplastic polyetherimide (TPI), number-average molecular weight 10000-50000g/ mol。
The compatilizer is one kind in PPE-g-MAH, SEBS-g-MAH, and preferably grafting rate is 0.3%-0.6%.It is compatible Agent improves the compatibility of polyphenylene oxide and thermoplastic polyimide, optimizes the processing performance of alloy.
The antioxidant is hindered phenol antioxygen and phosphite ester kind antioxidant compound system, selected from antioxidant 1010, 1076th, at least one of 168 3 kinds.
The preparation method of halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material of the present invention, comprises the following steps：
Each component dispensing is put into high-speed mixer and is uniformly mixed, then mixture is put into double screw extruder and is melted Melt extruding pelletization, that is, obtain halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material.
The rotating speed of double screw extruder is 200-400r/min, feeding rotating speed 30-40r/min, screw rod melting temperature section For 200-280 DEG C.
Polyphenyl ether alloy material of the present invention can also add suitable processing in addition to above-mentioned component and help in preparation process Agent, such as color masterbatch, light stabilizer, anti ultraviolet agent, accelerating agent, plasticizer, filler etc. so that Noryl multifunction, is applicable in Various different fields.
Polyphenyl ether alloy material of the present invention is the enhanced polyphenylene oxide of non-glass fibre, improves halogen-free flameproof with thermoplastic polyimide The heat-resisting quantity and mechanical property of agent polyphenylene oxide, preparation method moulding process is simple, suitable for serialization industrial production.
Beneficial effects of the present invention are embodied in：
1st, the present invention improves polyphenylene oxide processing performance using high fluidity polystyrene；Thermoplastic elastomer (TPE) improves polyphenylene oxide Toughness and shock resistance；The good flame retardation effect of nitrogen phosphorus Compositional type halogen-free flame retardants, meet European Union RoHS, IEC it is non-halogen and Reach laws and regulations requirements；Thermoplastic polyimide can improve the mechanical strength of polyphenyl ether material, and heat-resisting quantity, anti-flammability, is improved The application value of polyphenylene oxide alloy.
2nd, Polyphenyl ether alloy material of the present invention has high intensity, high impact-resistant, high temperature resistant, the excellent combination of high fire-retardance Energy.
3rd, this hair invention Polyphenyl ether alloy material preparation method is simple, and technique is simple, suitable for large-scale continuous production.
Embodiment
Technical scheme is further elaborated below in conjunction with specific embodiment.It is described herein Specific embodiment only to explain the present invention, is not intended to limit the present invention.
Halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material of the present invention, in parts by mass including following component：
In all embodiments provided by the invention, there is provided raw material can from market purchase obtain.Wherein,
The polyphenylene oxide powder selects PPE：S201A and S202A, Japanese Asahi Chemical Industry.
The polystyrene selects universal GPPS：PG-22, PG-33, Zhenjiang Qi Mei Chemical Co., Ltd.s.
The toughener selects SEBS：YH503, Yueyang petrochemical industry；S1605, Japanese Asahi Chemical Industry.
The fire retardant is RDP, BDP, PX-220, MCA, Zhejiang Wansheng Co., Ltd..
The thermoplastic polyimide selects TPI：AURUM PL450, Dupont；ULTEM 1000, SABIC.
The compatilizer is PPE-g-MAH, CX-1, Japanese Asahi Chemical Industry；SEBS-g-MAH, 9901, the long Rong Huagong of Lee.
The material that other materials in embodiment and comparative example can be commercially available both from the market.
Embodiment 1：
43 parts of polyphenylene oxide (S201A), 15 parts of polystyrene (PG-22), toughener SEBS (YH503) 13 are weighed by mass parts Part, 9 parts of compound flame retardant (3 parts of 6 parts of PX200, MCA), 15 parts of thermoplastic polyimide (TPI450), compatilizer (PPE-g- MAH) 3 parts, (168) 0.3 parts of antioxidant, each component raw material is added in high mixed pot and is uniformly mixed, the material that then will be mixed Put into melting extrusion in twin-screw to be granulated, that is, obtain halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material；Wherein twin-screw rotating speed is 300r/min, screw rod melting temperature are 280 DEG C.
Embodiment 2：
49 parts of polyphenylene oxide (S201A), 15 parts of polystyrene (PG-22), toughener SEBS (YH503) 13 are weighed by mass parts Part, 9 parts of compound flame retardant (3 parts of 6 parts of PX200, MCA), 10 parts of thermoplastic polyimide (TPI450), compatilizer (PPE-g- MAH) 3 parts, (168) 0.3 parts of antioxidant, each component raw material is added in high mixed pot and is uniformly mixed, the material that then will be mixed Put into melting extrusion in twin-screw to be granulated, that is, obtain halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material；Wherein twin-screw rotating speed is 400r/min, screw rod melting temperature are 270 DEG C.
Embodiment 3：
52 parts of polyphenylene oxide (S201A), 15 parts of polystyrene (PG-22), toughener SEBS (YH503) 13 are weighed by mass parts Part, 6 parts of compound flame retardant (2 parts of 4 parts of PX200, MCA), 10 parts of thermoplastic polyimide (TPI450), compatilizer (PPE-g- MAH) 3 parts, (168) 0.3 parts of antioxidant, each component raw material is added in high mixed pot and is uniformly mixed, the material that then will be mixed Put into melting extrusion in twin-screw to be granulated, that is, obtain halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material；Wherein twin-screw rotating speed is 400r/min, screw rod melting temperature are 270 DEG C.
Embodiment 4：
56 parts of polyphenylene oxide (S201A), 15 parts of polystyrene (PG-22), toughener SEBS (YH503) 13 are weighed by mass parts Part, 6 parts of compound flame retardant (2 parts of 4 parts of PX200, MCA), 6 parts of thermoplastic polyimide (TPI450), compatilizer (PPE-g- MAH) 3 parts, (168) 0.3 parts of antioxidant, each component raw material is added in high mixed pot and is uniformly mixed, the material that then will be mixed Put into melting extrusion in twin-screw to be granulated, that is, obtain halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material；The wherein rotating speed of twin-screw For 400r/min, screw rod melting temperature is 270 DEG C.
Comparative example 1：
59 parts of polyphenylene oxide (S201A), 15 parts of polystyrene (PG-22), toughener SEBS (YH503) 13 are weighed by mass parts Part, 9 parts of halogen-free flame retardants of compounding (3 parts of 6 parts of PX200, MCA), 3 parts of compatilizer (PPE-g-MAH), antioxidant (168) 0.3 Part, each component raw material is added in high mixed pot and is uniformly mixed, the material mixed then is put into melting extrusion in twin-screw makes Grain, that is, obtain halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material；The wherein rotating speed of twin-screw is 300r/min, screw rod melting temperature For 270 DEG C.
Comparative example 2：
58 parts of polyphenylene oxide (S201A), 15 parts of polystyrene (PG-22), toughener SEBS (YH503) 13 are weighed by mass parts Part, 10 parts of thermoplastic polyimide (TPI450), 3 parts of compatilizer (PPE-g-MAH), (168) 0.3 parts of antioxidant, by each component Raw material is added in high mixed pot and is uniformly mixed, and the material mixed then is put into melting extrusion in twin-screw is granulated, that is, obtains nothing Halogen flame-resistant high-temperature-resistant Polyphenyl ether alloy material；Wherein the rotating speed of twin-screw is 400r/min, and screw rod melting temperature is 280 DEG C.
The resin composition formula of comparative example 1,2 and implementation 1-4 are shown in Table 1, its performance test data is shown in Table 2.
Table 1
Table 2
By table 2 as it can be seen that halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material of the present invention conventional physical property after tested：Yield strength 70-80MPa, elongation at break 10-20%, bending strength 90-110MPa, bending modulus 2300-2600MPa, cantilever beam notch Impact strength 15-25KJ/m2, anti-flammability V-0 (UL94/1.5mm), HDT temperature is 130-145 DEG C.The formula of fire retardant with Polyphenylene oxide number increases and reduces, and by nitrogen phosphorus interworking halogen-free flame retardants good flame retardation effect, the addition of thermoplastic polyimide is shown The heat distortion temperature of modified polyphenylene oxide alloy is write, the comprehensive performance of modified polyphenylene oxide composite material is superior, applicable electrotechnical, electronic, Communicate the fields such as photovoltaic apparatus.
The foregoing is merely the embodiment of the present invention, is not intended to limit the scope of the invention, every to utilize this hair The equivalent structure or equivalent flow shift that bright description is made, is directly or indirectly used in other relevant technology necks Domain, is included within the scope of the present invention.

Claims (10)

1. a kind of halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material, it is characterised in that in parts by mass including following component：
2. halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material according to claim 1, it is characterised in that：
The polyphenylene oxide is powdered, and the inherent viscosity in 25 DEG C of chloroforms is 0.3-0.5dL/g, weight average molecular weight 22000- 57000。
3. halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material according to claim 1, it is characterised in that：
The polystyrene is General Purpose Polystyrenre, and melt index is 10-20g/10min under 200 DEG C/5kg load.
4. halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material according to claim 1, it is characterised in that：
The toughener is styrene-butadiene-styrene, hydrogenated styrene-butadiene-styrene copolymer, benzene At least one of ethylene-butylene-isoprene block copolymer, butadiene-styrene rubber, hydrogenated styrene-butadiene rubber.
5. halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material according to claim 4, it is characterised in that：
The toughener is hydrogenated styrene-butadiene-styrene copolymer.
6. halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material according to claim 1, it is characterised in that：
The compound flame retardant is halogen-free flame retardants, is made of phosphorus flame retardant and nitrogenated flame retardant, phosphorus flame retardant and nitrogen The mass ratio of flame retardant is 2：1.
7. halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material according to claim 6, it is characterised in that：
It is double that the phosphorus flame retardant is selected from bisphenol-A double (diphenyl phosphoesters), a phenol double (diphenyl phosphoesters), hydroquinone At least one of (diphenyl phosphoester), triphenyl phosphate, double two (2,6- 3,5-dimethylphenyls) phosphates of resorcinol；
The nitrogenated flame retardant is selected from least one of melamine, melamine polyphosphate, melamine cyanurate.
8. halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material according to claim 1, it is characterised in that：
The thermoplastic polyimide is thermoplastic polyetherimide, number-average molecular weight 10000-50000g/mol.
9. halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material according to claim 1, it is characterised in that：
The compatilizer is one kind in PPE-g-MAH, SEBS-g-MAH；
The antioxidant is hindered phenol antioxygen and phosphite ester kind antioxidant compound system.
A kind of 10. preparation method of the halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material described in claim 1, it is characterised in that bag Include following steps：
Each component dispensing is put into high-speed mixer and is uniformly mixed, then puts into melt mixture in double screw extruder and squeezes Go out to be granulated, that is, obtain halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material；
The rotating speed of double screw extruder is 200-400r/min, and feeding rotating speed 30-40r/min, screw rod melting temperature section is 200-280℃。
CN201711443814.2A 2017-12-27 2017-12-27 A kind of halogen-free flame-resistant high-temperature-resistant Polyphenyl ether alloy material and preparation method thereof Pending CN107903608A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110982245A (en) * 2019-12-17 2020-04-10 宁波华腾首研新材料有限公司 Modified polyphenyl ether resin material and preparation method and application thereof
CN111560164A (en) * 2020-06-11 2020-08-21 深圳市兴盛迪新材料有限公司 High-toughness weather-resistant high-temperature-resistant halogen-free flame-retardant polyphenyl ether composite material and preparation method thereof
CN113604026A (en) * 2021-08-27 2021-11-05 湖南恒屹新材料有限公司 Polyphenyl ether resin composite material capable of replacing PCB and preparation method thereof

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CN102850796A (en) * 2012-08-16 2013-01-02 深圳市科聚新材料有限公司 Polyetherimide composite material and its preparation method and use
CN103351617A (en) * 2013-06-28 2013-10-16 广东威林工程塑料有限公司 Environment-friendly, flame-retardant and high-impact-resistance PA6/PC/PPO (polyamide 6/polycarbonate/poly-p-phenylene oxide) alloy compound and preparation method for same
CN105273388A (en) * 2015-11-21 2016-01-27 东莞市百励兴新材料有限公司 High-heat-resistance halogen-free flame-retardant polyphenyl ether composite material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006041023A1 (en) * 2004-10-14 2006-04-20 Asahi Kasei Chemicals Corporation Resin composition
CN102850796A (en) * 2012-08-16 2013-01-02 深圳市科聚新材料有限公司 Polyetherimide composite material and its preparation method and use
CN103351617A (en) * 2013-06-28 2013-10-16 广东威林工程塑料有限公司 Environment-friendly, flame-retardant and high-impact-resistance PA6/PC/PPO (polyamide 6/polycarbonate/poly-p-phenylene oxide) alloy compound and preparation method for same
CN105273388A (en) * 2015-11-21 2016-01-27 东莞市百励兴新材料有限公司 High-heat-resistance halogen-free flame-retardant polyphenyl ether composite material and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110982245A (en) * 2019-12-17 2020-04-10 宁波华腾首研新材料有限公司 Modified polyphenyl ether resin material and preparation method and application thereof
CN111560164A (en) * 2020-06-11 2020-08-21 深圳市兴盛迪新材料有限公司 High-toughness weather-resistant high-temperature-resistant halogen-free flame-retardant polyphenyl ether composite material and preparation method thereof
CN113604026A (en) * 2021-08-27 2021-11-05 湖南恒屹新材料有限公司 Polyphenyl ether resin composite material capable of replacing PCB and preparation method thereof

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Application publication date: 20180413