CN108582601A - A kind of semi-permanent mould silicone release and preparation method thereof - Google Patents
A kind of semi-permanent mould silicone release and preparation method thereof Download PDFInfo
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- CN108582601A CN108582601A CN201810462028.5A CN201810462028A CN108582601A CN 108582601 A CN108582601 A CN 108582601A CN 201810462028 A CN201810462028 A CN 201810462028A CN 108582601 A CN108582601 A CN 108582601A
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- permanent mould
- silicone release
- releasing agent
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C33/00—Moulds or cores; Details thereof or accessories therefor
- B29C33/56—Coatings, e.g. enameled or galvanised; Releasing, lubricating or separating agents
- B29C33/60—Releasing, lubricating or separating agents
- B29C33/62—Releasing, lubricating or separating agents based on polymers or oligomers
- B29C33/64—Silicone
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C33/00—Moulds or cores; Details thereof or accessories therefor
- B29C33/56—Coatings, e.g. enameled or galvanised; Releasing, lubricating or separating agents
- B29C33/60—Releasing, lubricating or separating agents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/46—Block-or graft-polymers containing polysiloxane sequences containing polyether sequences
Abstract
The present invention relates to a kind of semi-permanent mould silicone releases and preparation method thereof, belong to manufacturing technology field.The present invention is used as function monomer by adding Organic fluoride in synthetic silicone resin,Fluorocarbon side chains are in surface enrichment,The highest fluorine atom of electronegativity surrounds carbochain,Form a helical structure,Play hydrophobic effect,Carbon key is also protected to be not easy to be destroyed by chemical mediator simultaneously,And chemical bonding occurs with silicon atom using hydroxyl group and acts on,Preparing has high surface,High thermal stability and high chemically inert releasing agent,With the volatilization of releasing agent petrochina ether,Polymeric particles are gradually assembled and ultimately form releasing agent,Since hydroxyl and silicon atom form covalent bond,And the Si O in organosilicon is combined to be combined with Si O Si,Surface is set to become finer and close,Fine and close releasing agent effectively prevents the invasion of material molecule,It is not easy incrustation,And the surface of macromolecule material product is not transferred to,Influence the following process of product,Improve demoulding efficiency.
Description
Technical field
The present invention relates to a kind of semi-permanent mould silicone releases and preparation method thereof, belong to manufacturing technology field.
Background technology
Releasing agent is a kind of functional processing aid for playing the role of assisting disengaging, be in mold and moulded products it
Between, the product of the elastomers such as rubber, resin, plastics and some other material can be prevented viscous on the mold surface.It is raw in industry
In production, in order to weaken the adhesion or absorption between product and mold, generally use coats releasing agent in die surface, product and mold
Dielectric film layer is formed between contact surface, which is only micron order, and thermal stability is good, and the film that is effectively isolated of formation can be with
It is connected chemically with die surface formation, mold and product is isolated, so that peeling force weakens, profiled part is allowed quickly to take off easily
It falls.
Releasing agent is essential a kind of auxiliary agent in modern industry, with plastics, rubber, polyurethane product and metal
The continuous development of the processing manufacturing industries such as zero component, for releasing agent dosage while increasing substantially, use scope is also increasingly
Extensively.It is various that there are many releasing agents, if classified by its service life, can be divided into conventional release agent and semi-permanent mould releasing agent.
Currently, having three categories using more wide releasing agent：Inorganic releasing agent（Soil, talcum powder, mica etc. are
Row）, organic release agent（Natural and artificial synthesized wax, fatty acid salt, aliphatic acid etc.）, polymeric release agent（Organosilicon has
The polymer etc. of machine fluorine）.
Conventional releasing agent must be coated to mold again based on disposable releasing agent before manufacturing each product
On surface.Regrettably, many problems be will produce using disposable releasing agent：（1）With the Reusability of releasing agent, releasing agent
It can gather and form incrustation on the mold surface, to keep the detailed features of mold fuzzy, this can lead to die surface feature structure
In the duplicating that can not be cleaned to the surface of high molecular products, so that destroy the integrality of product surface.（2）Due to incrustation
In the presence of needing the regular cleaning to mold, this leads to the increase of man power and material, and production capacity is made to reduce；In addition, in cleaning mold
During, the destruction for not allowing degree can be generated to mold, to reduce the service life of mold.（3）Due to disposably demoulding
Agent can be transferred to the surface of macromolecule material product, so the following process of product can be influenced.（4）Since disposable releasing agent needs
It to be administered to die surface again before manufacturing each product, this makes the demand of releasing agent greatly increase, while also can
Increase the discharge capacity of volatile organic matter, so that the production cost increases, and the pressure of environmental protection aspect can also increase, therefore urgently
It needs to improve.
Invention content
The technical problems to be solved by the invention：For the easy incrustation of releasing agent Reusability, need to the regular clear of mold
Clean and releasing agent can be transferred to the surface of macromolecule material product, the problem of influencing the following process of product, provide a kind of half
Permanent type silicone release and preparation method thereof.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A kind of semi-permanent mould silicone release, the releasing agent include following weight parts raw material：
6~10 parts of modified organic silicone resins, 4~6 parts of hydroxy silicon oils, 80~90 parts of petroleum ethers, 0.5~0.8 part of tin dilaurate two
Butyl tin, 0.75~1.25 part of tri-n-butylamine.
The modified organic silicone resin be tetramethyl disiloxane, methyltrimethoxysilane, phenyltrimethoxysila,e,
Ethyl orthosilicate, fluorinated modified liquid are fitted into reaction kettle and mix, and it is 10% salt to add deionized water, absolute ethyl alcohol, mass fraction
Acid is heated to 80~90 DEG C of insulation reactions, and decompression after reaction steams low-boiling-point substance and is made.
The fluorinated modified liquid is by perfluoropolyether carboxylic acid, trifluoroethyl methacrylate, Sodium perfluorooctanoate, perfluoro capryl sulphur
Sour sodium, acetone composition.
The parts by weight of the fluorinated modified liquid component material are 5~6 parts of perfluoropolyether carboxylic acids, 3~5 parts of methacrylic acids three
Fluorine ethyl ester, 1~2 part of Sodium perfluorooctanoate, 2~3 parts of perfluoro octyl sulfonic acid sodium, 50~80 parts of acetone.
The perfluoropolyether carboxylic acid be perfluoropolyether be fitted into mixed with deionized water in there-necked flask after be warming up to 60~80 DEG C,
Removing water is evaporated under reduced pressure after 4~5h of insulation reaction and hydrofluoric acid is made.
The mass ratio of the perfluoropolyether and deionized water is 1：4~1：6.
The parts by weight of raw materials be 5~25 parts of tetramethyl disiloxanes, 24~36 parts of methyltrimethoxysilane, 18~32
Part phenyltrimethoxysila,e, 5~15 parts of ethyl orthosilicates, 50~60 parts of fluorinated modified liquid, 18~25 parts of deionized waters, 20~
30 parts of absolute ethyl alcohols, 0.20~0.25 part of mass fraction are 10% hydrochloric acid.
It is 180~200 DEG C that the decompression, which steams temperature,.
A kind of preparation method of the semi-permanent mould silicone release, the specific steps are：
（1）Take perfluoropolyether be fitted into mixed with deionized water in there-necked flask after be warming up to 60~80 DEG C, subtract after 4~5h of insulation reaction
Pressure evaporation removes water and hydrofluoric acid, obtains perfluoropolyether carboxylic acid；
（2）Perfluoropolyether carboxylic acid, trifluoroethyl methacrylate, Sodium perfluorooctanoate, perfluoro octyl sulfonic acid sodium are taken, is added in acetone
It is uniformly mixed, obtains fluorinated modified liquid；
（3）Take tetramethyl disiloxane, methyltrimethoxysilane, phenyltrimethoxysila,e, ethyl orthosilicate, fluorinated modified
Liquid is uniformly mixed, and it is 10% hydrochloric acid to add deionized water, absolute ethyl alcohol, mass fraction, and 5~8h is reacted in heating, after reaction
Decompression steams low-boiling-point substance at 180~200 DEG C, obtains modified organic silicone resin；
（4）Take modified organic silicone resin, hydroxy silicon oil be added petroleum ether in be uniformly mixed, add dibutyl tin laurate,
Tri-n-butylamine stirs and evenly mixs to obtain semi-permanent mould silicone release.
Compared with other methods, advantageous effects are the present invention：
（1）The present invention is used as function monomer by adding Organic fluoride in synthetic silicone resin, fluorocarbon side chains in surface enrichment,
The highest fluorine atom of electronegativity surrounds carbochain, forms a helical structure, plays hydrophobic effect, while also protecting carbon key
It is not easy to be destroyed by chemical mediator, and chemical bonding occurs with silicon atom using hydroxyl group and acts on, preparing, there is high surface to live
Property, high thermal stability and high chemically inert releasing agent, with the volatilization of releasing agent petrochina ether, polymeric particles gradually gather
Collect and ultimately form releasing agent, since hydroxyl and silicon atom form covalent bond, and the Si-O and Si-O-Si in organosilicon is combined to tie
It closes, so that surface is become finer and close, fine and close releasing agent effectively prevents the invasion of material molecule, is not easy incrustation, and will not shift
To the surface of macromolecule material product, the following process of product is influenced, demoulding efficiency is improved；
（2）Releasing agent of the present invention easily forms a film, and improves mold temperature in use by the way of fluosilicic combination, increases release agent coating table
Face contact angle reduces its surface tension, and increases the adhesive force with mold, improves release times, can using dispersing aid
So that releasing agent is uniformly dispersed in a solvent, improves the storage stability of demoulding agent emulsion.
Specific implementation mode
It takes 50~60g perfluoropolyether to be fitted into there-necked flask, adds in 240~300mL deionized waters, with 300~400r/
Min stirrings are warming up to 60~80 DEG C, are packed on Rotary Evaporators after 4~5h of insulation reaction, are evaporated under reduced pressure and remove water and hydrofluoric acid,
Perfluoropolyether carboxylic acid, take 5~6g perfluoropolyether carboxylic acids, 3~5g trifluoroethyl methacrylates, 1~2g Sodium perfluorooctanoates, 2
~3g perfluoro octyl sulfonic acid sodium is added in 50~80g acetone, stirs 20~30min with 300~400r/min, obtains fluorinated modified
Liquid, takes 15~25g tetramethyl disiloxanes, 24~36g methyltrimethoxysilane, 18~32g phenyltrimethoxysila,es, and 5
~15g ethyl orthosilicates, the fluorinated modified liquid of 50~60g are fitted into reaction kettle, and 20~30min is stirred with 200~300r/min, then
18~25mL deionized waters are added, 20~30g absolute ethyl alcohols, 0.20~0.25g mass fractions are 10% hydrochloric acid, at 80~90 DEG C
5~8h of lower reaction is packed on Rotary Evaporators after reaction, is depressurized at 180~200 DEG C and is steamed low-boiling-point substance, must be modified
Machine silicones, takes 6~10g modified organic silicone resins, 4~6g hydroxy silicon oils, is added in 80~90g petroleum ethers, with 300~
400r/min stirs 20~30min, adds 0.5~0.8g dibutyl tin laurates, 0.75~1.25g tri-n-butylamines, after
20~30min of continuous stirring, obtains semi-permanent mould silicone release.
Example 1
It takes 50g perfluoropolyether to be fitted into there-necked flask, adds in 240mL deionized waters, 60 DEG C are warming up to 300r/min stirrings,
It is packed on Rotary Evaporators after insulation reaction 4h, is evaporated under reduced pressure and removes water and hydrofluoric acid, obtain perfluoropolyether carboxylic acid, take 5g perfluors poly-
Ether carboxylic acid, 3g trifluoroethyl methacrylates, 1g Sodium perfluorooctanoates, 2g perfluoro octyl sulfonic acid sodium are added in 50g acetone, with
300r/min stirs 20min, obtains fluorinated modified liquid, takes 15g tetramethyl disiloxanes, 24g methyltrimethoxysilane, 18g benzene
Base trimethoxy silane, 5g ethyl orthosilicates, the fluorinated modified liquid of 50g are fitted into reaction kettle, and 20min is stirred with 200r/min, then
18mL deionized waters, 20g absolute ethyl alcohols is added, 0.20g mass fractions are 10% hydrochloric acid, 5h are reacted at 80 DEG C, after reaction
It is packed on Rotary Evaporators, is depressurized at 180 DEG C and steam low-boiling-point substance, obtained modified organic silicone resin, take 6g modified organic silicon trees
Fat, 4g hydroxy silicon oils are added in 80g petroleum ethers, stir 20min with 300r/min, add 0.5g dibutyl tin laurates,
0.75g tri-n-butylamines continue 20~30min of stirring, obtain semi-permanent mould silicone release.
Example 2
It takes 55g perfluoropolyether to be fitted into there-necked flask, adds in 280mL deionized waters, 70 DEG C are warming up to 360r/min stirrings,
It is packed on Rotary Evaporators after insulation reaction 4h, is evaporated under reduced pressure and removes water and hydrofluoric acid, obtain perfluoropolyether carboxylic acid, take 5g perfluors poly-
Ether carboxylic acid, 4g trifluoroethyl methacrylates, 1g Sodium perfluorooctanoates, 2g perfluoro octyl sulfonic acid sodium are added in 60g acetone, with
360r/min stirs 25min, obtains fluorinated modified liquid, takes 20g tetramethyl disiloxanes, 30g methyltrimethoxysilane, 25g benzene
Base trimethoxy silane, 10g ethyl orthosilicates, the fluorinated modified liquid of 55g are fitted into reaction kettle, and 25min is stirred with 240r/min, then
20mL deionized waters, 25g absolute ethyl alcohols is added, 0.24g mass fractions are 10% hydrochloric acid, 6h are reacted at 85 DEG C, after reaction
It is packed on Rotary Evaporators, is depressurized at 180 DEG C and steam low-boiling-point substance, obtained modified organic silicone resin, take 8g modified organic silicon trees
Fat, 5g hydroxy silicon oils are added in 85g petroleum ethers, stir 25min with 360r/min, add 0.6g dibutyl tin laurates,
1g tri-n-butylamines continue to stir 25min, obtain semi-permanent mould silicone release.
Example 3
It takes 60g perfluoropolyether to be fitted into there-necked flask, adds in 300mL deionized waters, 80 DEG C are warming up to 400r/min stirrings,
It is packed on Rotary Evaporators after insulation reaction 5h, is evaporated under reduced pressure and removes water and hydrofluoric acid, obtain perfluoropolyether carboxylic acid, take 6g perfluors poly-
Ether carboxylic acid, 5g trifluoroethyl methacrylates, 2g Sodium perfluorooctanoates, 3g perfluoro octyl sulfonic acid sodium are added in 80g acetone, with
400r/min stirs 30min, obtains fluorinated modified liquid, takes 25g tetramethyl disiloxanes, 36g methyltrimethoxysilane, 32g benzene
Base trimethoxy silane, 15g ethyl orthosilicates, the fluorinated modified liquid of 60g are fitted into reaction kettle, and 30min is stirred with 300r/min, then
25mL deionized waters, 30g absolute ethyl alcohols is added, 0.25g mass fractions are 10% hydrochloric acid, 8h are reacted at 90 DEG C, after reaction
It is packed on Rotary Evaporators, is depressurized at 200 DEG C and steam low-boiling-point substance, obtained modified organic silicone resin, take 10g modified organic silicon trees
Fat, 6g hydroxy silicon oils are added in 90g petroleum ethers, stir 30min with 400r/min, add 0.8g dibutyl tin laurates,
1.25g tri-n-butylamines continue to stir 30min, obtain semi-permanent mould silicone release.
Reference examples：The releasing agent of Dalian company production.
The releasing agent of example and reference examples is detected, specific detection is as follows：
Demolding performace is tested：Disbonded test is taken to carry out, the BLD- produced using Jinan blue light mechanical ＆ electrical technology Co., Ltd
200N type electron detachment testing machines carry out disbonded test, releasing agent are sprayed or wiped the epoxy resin board clean in surface treatment
On, it places 30 minutes, is then fixed on electron detachment testing machine at room temperature, after setting stripping program, use standard pressure sensitive
Adhesive tape does 180 ° of disbonded tests with the speed of 25mm/min, analyzes releasing agent release times.
Curability is tested：The releasing agent prepared is coated on polyethylene layer platen or on glass slide, is then placed within
Temperature is set as heating 30min in 100 DEG C of heated air circulation type baking oven, forms cured film, and curability is made and measures examination
Sample.
Surface contact angle is tested：Releasing agent is coated on smooth clean glass slide, places wait for that it is completely solid at room temperature
After being melted into film, by water droplet on glass slide, contact angle of the water in mold film surface is measured using contact angle instrument.Test-strips
Part：Need sample to choose three different measurement points, test water its surface static contact angle, and using the flat of these three points
Mean value.
Viscosity Analysis：Viscosity test is carried out to releasing agent, using Shanghai Ji Di Co., Ltds NDJ-79 type rotational viscometers.
Test condition：Releasing agent is poured into test container, ascending selection rotor number, rotor is gradually immersed into and is measured in liquid,
Until rotor liquid surface mark is equal with liquid level.So that rotor is rotated 25s or so in a liquid, after pointer stabilization, reads reading.
Specific testing result such as table 1.
1 performance characterization contrast table of table
As shown in Table 1, the releasing agent that prepared by the present invention has good stripping result and stability.
Claims (9)
1. a kind of semi-permanent mould silicone release, which is characterized in that the releasing agent includes following weight parts raw material：
6~10 parts of modified organic silicone resins, 4~6 parts of hydroxy silicon oils, 80~90 parts of petroleum ethers, 0.5~0.8 part of tin dilaurate two
Butyl tin, 0.75~1.25 part of tri-n-butylamine.
2. a kind of semi-permanent mould silicone release as described in claim 1, which is characterized in that the modified organic silicone resin
It is packed into for tetramethyl disiloxane, methyltrimethoxysilane, phenyltrimethoxysila,e, ethyl orthosilicate, fluorinated modified liquid
It is mixed in reaction kettle, it is that 10% hydrochloric acid is heated to 80~90 DEG C of insulation reactions to add deionized water, absolute ethyl alcohol, mass fraction,
Decompression steams low-boiling-point substance and is made after reaction.
3. a kind of semi-permanent mould silicone release as claimed in claim 2, which is characterized in that the fluorinated modified liquid is by complete
Perfluoroalkyl polyether carboxylic acid, trifluoroethyl methacrylate, Sodium perfluorooctanoate, perfluoro octyl sulfonic acid sodium, acetone composition.
4. a kind of semi-permanent mould silicone release as claimed in claim 2 or claim 3, which is characterized in that the fluorinated modified liquid
The parts by weight of component material are 5~6 parts of perfluoropolyether carboxylic acids, 3~5 parts of trifluoroethyl methacrylates, 1~2 part of perfluoro caprylic acid
Sodium, 2~3 parts of perfluoro octyl sulfonic acid sodium, 50~80 parts of acetone.
5. a kind of semi-permanent mould silicone release as described in claim 3 or 4, which is characterized in that the perfluoropolyether carboxylic
Acid be perfluoropolyether is fitted into mix with deionized water in there-necked flask after be warming up to 60~80 DEG C, decompression steaming after 4~5h of insulation reaction
Hair removes water and hydrofluoric acid is made.
6. a kind of semi-permanent mould silicone release as claimed in claim 5, which is characterized in that the perfluoropolyether and go from
The mass ratio of sub- water is 1：4~1：6.
7. a kind of semi-permanent mould silicone release as claimed in claim 2, which is characterized in that the parts by weight of raw materials is 5
~25 parts of tetramethyl disiloxanes, 24~36 parts of methyltrimethoxysilane, 18~32 parts of phenyltrimethoxysila,es, 5~15
Part ethyl orthosilicate, 50~60 parts of fluorinated modified liquid, 18~25 parts of deionized waters, 20~30 parts of absolute ethyl alcohols, 0.20~0.25
Part mass fraction is 10% hydrochloric acid.
8. a kind of semi-permanent mould silicone release as claimed in claim 2, which is characterized in that the decompression steams temperature and is
180~200 DEG C.
9. a kind of preparation method of semi-permanent mould silicone release as described in claim 1~8 any one, feature exist
In, the specific steps are：
（1）Take perfluoropolyether be fitted into mixed with deionized water in there-necked flask after be warming up to 60~80 DEG C, subtract after 4~5h of insulation reaction
Pressure evaporation removes water and hydrofluoric acid, obtains perfluoropolyether carboxylic acid；
（2）Perfluoropolyether carboxylic acid, trifluoroethyl methacrylate, Sodium perfluorooctanoate, perfluoro octyl sulfonic acid sodium are taken, is added in acetone
It is uniformly mixed, obtains fluorinated modified liquid；
（3）Take tetramethyl disiloxane, methyltrimethoxysilane, phenyltrimethoxysila,e, ethyl orthosilicate, fluorinated modified
Liquid is uniformly mixed, and it is 10% hydrochloric acid to add deionized water, absolute ethyl alcohol, mass fraction, and 5~8h is reacted in heating, after reaction
Decompression steams low-boiling-point substance at 180~200 DEG C, obtains modified organic silicone resin；
（4）Take modified organic silicone resin, hydroxy silicon oil be added petroleum ether in be uniformly mixed, add dibutyl tin laurate,
Tri-n-butylamine stirs and evenly mixs to obtain semi-permanent mould silicone release.
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| CN201810462028.5A CN108582601B (en) | 2018-05-15 | 2018-05-15 | Semi-permanent type organic silicon release agent and preparation method thereof |
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| CN201810462028.5A CN108582601B (en) | 2018-05-15 | 2018-05-15 | Semi-permanent type organic silicon release agent and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109822793A (en) * | 2019-02-25 | 2019-05-31 | 湖南七纬科技有限公司 | A kind of aqueous semi-permanent mould Organic fluoride release agent |
| CN114654635A (en) * | 2021-12-24 | 2022-06-24 | 平高集团有限公司 | Method for improving surface smoothness of epoxy casting product |
| CN115851121A (en) * | 2022-12-15 | 2023-03-28 | 上海东恒化工有限公司 | Water-based magnetic particle-based demoulding coating and preparation method thereof |
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| US6204350B1 (en) * | 1997-03-14 | 2001-03-20 | 3M Innovative Properties Company | Cure-on-demand, moisture-curable compositions having reactive silane functionality |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109822793A (en) * | 2019-02-25 | 2019-05-31 | 湖南七纬科技有限公司 | A kind of aqueous semi-permanent mould Organic fluoride release agent |
| CN114654635A (en) * | 2021-12-24 | 2022-06-24 | 平高集团有限公司 | Method for improving surface smoothness of epoxy casting product |
| CN115851121A (en) * | 2022-12-15 | 2023-03-28 | 上海东恒化工有限公司 | Water-based magnetic particle-based demoulding coating and preparation method thereof |
| CN115851121B (en) * | 2022-12-15 | 2023-10-20 | 上海东恒化工有限公司 | Aqueous magnetic particle-based release coating and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN108582601B (en) | 2020-08-21 |
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