CN107556753A - A kind of micropore silicon rubber composite material of high temperature resistant environment-protective and preparation method thereof - Google Patents
A kind of micropore silicon rubber composite material of high temperature resistant environment-protective and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to silicone rubber art, and in particular to a kind of environmental protection and regulatable silicon rubber composite material of performance and preparation method thereof.The silicon rubber composite material, it is made up of the raw material of following percentage by weight：100 parts of vinyl polysiloxane, 0.1 2 parts of reaction suppressor, 0.1 2 parts of crosslinking catalyst, 2 10 parts of containing hydrogen silicone oil, ultra-fine 5 70 parts of carbonate, 0.5 7 parts of carbonate modifiers, 5 70 parts of hollow glass microballoon.It will be filled by modified ultra-fine carbonate and hollow glass microballoon according to premix ratio to silica gel colloid, it is dispersed in silica gel colloid, obtain compound silica gel pre-composition.Then premix silica gel is placed in suitable temperature, finally obtains high-temperature resistant micropore silicon rubber composite material product.
Description
Technical field
The present invention relates to a kind of silicone rubber products and preparation method thereof, and in particular to a kind of microporous silicon of high temperature resistant environment-protective
The preparation of rubber composite.
Background technology
Silastic material is macromolecular material that is a kind of while having organic nature and inorganic in nature, its molecular backbone
Alternately it is made up of (Si-O), its side-chain radical is that the organic groups such as methyl, vinyl, phenyl, trifluoro propyl are formed.Because its is only
Special structure and composition so that silicon rubber has excellent resistant of high or low temperature, nontoxic, remarkable chemical stability, excellent electricity
Insulating properties, light fastness aging and physiological inertia etc., so as in chemical industry, automobile, electric, mechanical, medical science, Aero-Space etc.
Field is widely used.
But with the continuous improvement of living standard and industrialized level, simple silastic material has been difficult to full
The sufficient higher and higher feature requirement of people, thus silicon rubber is modified it is imperative.By to silicon rubber
Physics or chemical modification, make its mechanical property, thermal stability, anti-flaming thermal-insulation performance, ageing-resistant, each side such as feature of environmental protection
The performance in face gets a promotion, so as to further widen the use range and application value of silastic material.
In some existing modification technologies, prepare composite modified silastic material used in modifying agent do not meet environmental protection
It is required that the accessory substance of toxicity and damage to the environment can be produced in modifying process, or its modifying agent inherently noxious material,
It is remained in final composite modified silica gel colloid, does not meet green requirement, is to limit one that silicon rubber uses
Key factor.
The content of the invention
The purpose of the present invention is the performance deficiency for single silastic material, is ensureing preparation process and final compound production
On the premise of product environmental protection, there is provided a kind of regulatable silicon rubber composite material of environmental-protecting performance and preparation method thereof.The silicon rubber is answered
Condensation material preparation method is simple, and controllable with excellent resistance to thermal insulation, product asepsis environment-protecting, performance.
To achieve these goals, the present invention uses following technical scheme：
A kind of micropore silicon rubber composite material, it is characterised in that the micropore silicon rubber composite material is by following component by weight
Percentage is measured to form：
Described reaction suppressor is acetylene basic ring alcohol；Described crosslinking catalyst is platinum catalyst；Described carbon
Sulfonate modified dose is erucyl amide, stearic acid or Metallic stearates, and the particle size range of the ultra-fine carbonate is micro- for 1~20
Rice, a diameter of 1~50 micron of the hollow glass microballoon.
Further, Metallic stearates of the present invention refer to the Metallic stearates such as zinc stearate.
Further, platinum catalyst of the present invention mainly has chloroplatinic acid and its complex such as platinum-vinyl siloxane
Composition catalyst etc. forms.
Further, reactive hydrogen mass fraction is 0.18% in containing hydrogen silicone oil of the present invention, viscosity 1000mpa.s.
Further, vinyl polysiloxane of the present invention is the vinyl containing two or more vinyl
Polysiloxanes.
Further, vinyl polysiloxane of the present invention is the poly- silica of vinyl by gas-phase silica reinforcement
Alkane.The technology being known to the skilled person using gas-phase silica reinforcement vinyl polysiloxane, the present invention is in 1 mass parts
Vinyl polysiloxane add 0.3 part of white carbon, through kneader high intensity be kneaded and obtain the vinyl polysiloxane of reinforcement.
Further, ultra-fine carbonate of the present invention is sodium acid carbonate, ammonium carbonate, the one or more of ammonium hydrogen carbonate
Combination.
Further, the mass parts ratio of ultra-fine carbonate and carbonate modifiers of the present invention is preferably 10：1.
Preferably, micropore silicon rubber composite material of the present invention is recommended to be made up of by weight percentage following component：
The present invention provides the preparation method of described micropore silicon rubber composite material：
(1) each component is weighed by proportioning, crosslinking catalyst is added in vinyl polysiloxane and is kneaded uniformly with kneader；
Reaction suppressor is added in containing hydrogen silicone oil, is stirred with mixer；Carbonate modifiers are added in carbonate, use ball milling
Machine is uniformly dispersed, and obtains the carbonate powder being modified；
(2) the above-mentioned each component by pretreatment is subjected to blending processing using mechanical means, each component is uniformly dispersed,
Pre-composition is obtained, pre-composition is subjected to vacuum degassing bubble processing, is poured into afterwards in mould, is placed in 45~70 DEG C of temperature and is consolidated
Change, then by 80~160 DEG C of 1~2h of isothermal holding, obtain described micropore silicon rubber composite material.
The profitable fruit of the present invention：1) ultra-fine carbonate and hollow glass microballoon are made according to suitable proportioning in the present invention
With passing through suitable Temperature Treatment so that ultra-fine carbonate is thermally decomposed in silica gel colloid, produces fine and closely woven uniform hole,
So that silicon rubber has soft and high resiliency, meanwhile, the addition of hollow glass microballoon so that the thermal insulation separation of silicon rubber composite material
The combination properties such as hot property, shrink of product performance, hardness, insulation, sound insulation, wear-resisting, machining property, rheology, density obtain
It is effectively improved and is lifted., can be with centering meanwhile hole caused by carbonate makes compound silica gel product when being impacted and being compressed
Empty glass microsphere plays buffer protection function, so as to reduce the breakage of hollow glass microballoon, plays synergy, micro- so as to improve
Hole silicon rubber composite material overall performance.2) silicon rubber composite material that this method is prepared, it is environment-protecting and non-poisonous, and preparation technology
Simply.
Embodiment
With reference to specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in
This.
In following comparative example and embodiment, feed ethylene based polysiloxane is all containing two or more vinyl
And the vinyl polysiloxane Jing Guo gas-phase silica reinforcement, commercially available, producer is Dongguan Lianzhan Silicone Technology Co., Ltd.；
Reaction suppressor is acetylene basic ring alcohol；The viscosity of containing hydrogen silicone oil is 1000mpas, and reactive hydrogen mass fraction is 0.18%, is purchased from
Dongguan Lianzhan Silicone Technology Co., Ltd.；The ultra-fine sodium acid carbonate powder particle diameter distribution is 1-20 μm, commercially available；Ultra-fine carbon
Sour ammonium diameter of particle is distributed as 1-20 μm, commercially available；The hollow glass microballoon trade mark is S60HS, and Minnesota Mining and Manufacturing Company produces；Stearic acid article No.
For S108288, Aladdin reagent；Erucyl amide article No. is E107867, Aladdin reagent；The platinum catalyst is commercially available, and this is urged
Agent is to add the complex of platinum catalyst, its platinum load capacity 5000ppm.Comparative example 1
The vinyl polysiloxane of 100 mass parts is taken, is previously added 0.2 part of platinum catalyst；The mass parts of containing hydrogen silicone oil 10,
It is previously added 0.2 part of reaction suppressor.Then two components are sequentially added in reaction vessel, using mechanical mixture 20min, obtained
Mixture；Then processing is ground to mixed material using three-roll grinder, obtains well mixed material, while excluded mixed
Bubble in rubber alloy body, in order to ensure the complete exclusion of bubble, vacuum tank is reused to its further pump-down process.Will blending
Good sizing material is poured into the mould of design, is then put into the mould equipped with sizing material in the vacuum drying chamber that temperature is 50 DEG C, Gu
Change 1 hour, obtain the silicone rubber compounds of non-compound carbonate and hollow glass microballoon sample as a comparison.
Embodiment 1
The vinyl polysiloxane of 100 mass parts is taken, is previously added 0.2 part of platinum catalyst, the mass parts of containing hydrogen silicone oil 10,
0.2 part of reaction suppressor is previously added, the ultra-fine mass parts of sodium acid carbonate 5, has been previously added at stearic acid modified dose of 0.5 mass parts
Reason, the mass parts of hollow glass microballoon 5.Then each component is sequentially added in reaction vessel, then using mechanical mixture 20min,
Obtain mixture；Then processing is ground to mixed material using the three-roll grinder that roll spacing is 0.1mm, is well mixed
Material, while exclude the bubble in colloid mixture, in order to ensure the complete exclusion of bubble, reuse vacuum tank and one is entered to it
Walk pump-down process.The sizing material being blended is poured into the mould of design, be placed in 50 DEG C and solidified, then blend glue stuff will be housed
Mould be put into 150 DEG C of vacuum drying chamber, insulation 1 hour after, be cooled to room temperature, obtain silicon rubber Composite rubber material.
Embodiment 2
The vinyl polysiloxane of 100 mass parts is taken, is previously added 0.1 part of platinum catalyst；The mass parts of containing hydrogen silicone oil 10, in advance
2 parts of reaction suppressors are first added, the ultra-fine mass parts of sodium acid carbonate 40, have been previously added the stearic acid modified dose of processing of 4 mass parts, in
The empty mass parts of glass microsphere 40.Then each component is sequentially added in reaction vessel, then using mechanical mixture 20min, obtained
Mixture；Then processing is ground to mixed material using the three-roll grinder that roll spacing is 0.1mm, obtains well mixed thing
Material, while the bubble in colloid mixture is excluded, in order to ensure the complete exclusion of bubble, vacuum tank is reused to its further row
Gas disposal.The sizing material being blended is poured into the mould of design, carry out curing process at a temperature of being first placed in 70 DEG C, then will be equipped with
The mould of solidification blend glue stuff is put into 160 DEG C of vacuum drying chamber, after being incubated 1 hour, is cooled to room temperature, is obtained silicon rubber and answer
Rubber alloy material.
Embodiment 3
The vinyl polysiloxane of 100 mass parts is taken, is previously added 0.2 part of platinum catalyst；The mass parts of containing hydrogen silicone oil 10, in advance
First add 0.5 part of reaction suppressor.The ultra-fine mass parts of sodium acid carbonate 70, the stearic acid modified dose of processing of 7 mass parts is previously added,
The mass parts of hollow glass microballoon 70.Then each component is sequentially added in reaction vessel, then using mechanical mixture 20min, obtained
To mixture；Then processing is ground to mixed material using the three-roll grinder that roll spacing is 0.1mm, obtained well mixed
Material, while the bubble in colloid mixture is excluded, in order to ensure the complete exclusion of bubble, it is further to its to reuse vacuum tank
Pump-down process.The sizing material being blended is poured into the mould of design, curing process is carried out at a temperature of being first placed in 50 DEG C, then will dress
The mould for having solidification blend glue stuff is put into 150 DEG C of vacuum drying chamber, is incubated 1 hour, is cooled to room temperature, obtains silicon rubber and answer
Rubber alloy material.
Embodiment 4
The vinyl polysiloxane of 100 mass parts is taken, is previously added 0.2 part of platinum catalyst；The mass parts of containing hydrogen silicone oil 10, in advance
First add 0.2 part of reaction suppressor.The ultra-fine mass parts of ammonium hydrogen carbonate 5, it has been previously added at 0.5 mass erucyl amide modifying agent
Reason, the mass parts of hollow glass microballoon 5.Then each component is sequentially added in reaction vessel, then using mechanical mixture 20min,
Obtain mixture；Then processing is ground to mixed material using the three-roll grinder that roll spacing is 0.1mm, is well mixed
Material, while exclude the bubble in colloid mixture, in order to ensure the complete exclusion of bubble, reuse vacuum tank and one is entered to it
Walk pump-down process.The sizing material being blended is poured into the mould of design, curing process is carried out at a temperature of being first placed in 70 DEG C, then
Mould equipped with solidification blend glue stuff is put into 90 DEG C of vacuum drying chamber, 2 hours is incubated, is cooled to room temperature, obtains silicon rubber
Glue Composite rubber material.
Embodiment 5
The vinyl polysiloxane of 100 mass parts is taken, is previously added 2 parts of platinum catalysts；The mass parts of containing hydrogen silicone oil 10, in advance
Add 2 parts of reaction suppressors.The ultra-fine mass parts of ammonium hydrogen carbonate 40,4 mass parts erucyl amide modifier treatments are previously added, in
The empty mass parts of glass microsphere 40.Then each component is sequentially added in reaction vessel, then using mechanical mixture 20min, obtained
Mixture；Then processing is ground to mixed material using the three-roll grinder that roll spacing is 0.1mm, obtains well mixed thing
Material, while the bubble in colloid mixture is excluded, in order to ensure the complete exclusion of bubble, vacuum tank is reused to its further row
Gas disposal.The sizing material being blended is poured into the mould of design, curing process is carried out at a temperature of being first placed in 45 DEG C, then will dress
The mould for having solidification blend glue stuff is put into 80 DEG C of vacuum drying chamber, is incubated 2 hours, is cooled to room temperature, obtains silicon rubber and answer
Rubber alloy material.
Embodiment 6
The vinyl polysiloxane of 100 mass parts is taken, is previously added 0.2 part of platinum catalyst；The mass parts of containing hydrogen silicone oil 10, in advance
First add 0.2 part of reaction suppressor.The ultra-fine mass parts of ammonium hydrogen carbonate 70, it has been previously added at 7 mass parts erucyl amide modifying agent
Reason, the mass parts of hollow glass microballoon 70.Then each component is sequentially added in reaction vessel, then using mechanical mixture 20min,
Obtain mixture；Then processing is ground to mixed material using the three-roll grinder that roll spacing is 0.1mm, is well mixed
Material, while exclude the bubble in colloid mixture, in order to ensure the complete exclusion of bubble, reuse vacuum tank and one is entered to it
Walk pump-down process.The sizing material being blended is poured into the mould of design, curing process is carried out at a temperature of being first placed in 50 DEG C, then will
Mould equipped with solidification blend glue stuff is put into 90 DEG C of vacuum drying chamber, is incubated 2 hours, is cooled to room temperature, obtains silicon rubber
Composite rubber material.
Embodiment 7
The vinyl polysiloxane of 100 mass parts is taken, is previously added 2 parts of platinum catalysts；The mass parts of containing hydrogen silicone oil 10, in advance
Add 0.1 part of reaction suppressor.The ultra-fine mass parts of ammonium carbonate 5,0.5 mass parts zinc stearate modifier treatment is previously added,
The mass parts of hollow glass microballoon 5.Then each component is sequentially added in reaction vessel, then using mechanical mixture 20min, obtained
Mixture；Then processing is ground to mixed material using the three-roll grinder that roll spacing is 0.1mm, obtains well mixed thing
Material, while the bubble in colloid mixture is excluded, in order to ensure the complete exclusion of bubble, vacuum tank is reused to its further row
Gas disposal.The sizing material being blended is poured into the mould of design, curing process is carried out at a temperature of being first placed in 45 DEG C, then will dress
The mould for having solidification blend glue stuff is put into 80 DEG C of vacuum drying chamber, is incubated 1 hour, is cooled to room temperature, obtains silicon rubber and answer
Rubber alloy material.
Embodiment 8
The vinyl polysiloxane of 100 mass parts is taken, is previously added 0.5 part of platinum catalyst；The mass parts of containing hydrogen silicone oil 10, in advance
First add 0.5 part of reaction suppressor.The ultra-fine mass parts of ammonium carbonate 40,4 mass parts zinc stearate modifier treatments are previously added,
The mass parts of hollow glass microballoon 40.Then each component is sequentially added in reaction vessel, then using mechanical mixture 20min, obtained
To mixture；Then processing is ground to mixed material using the three-roll grinder that roll spacing is 0.1mm, obtained well mixed
Material, while the bubble in colloid mixture is excluded, in order to ensure the complete exclusion of bubble, it is further to its to reuse vacuum tank
Pump-down process.The sizing material being blended is poured into the mould of design, curing process is carried out at a temperature of being first placed in 50 DEG C, then will dress
The mould for having solidification blend glue stuff is put into 90 DEG C of vacuum drying chamber, is incubated 1 hour, is cooled to room temperature, obtains silicon rubber and answer
Rubber alloy material.
Embodiment 9
The vinyl polysiloxane of 100 mass parts is taken, is previously added 0.2 part of platinum catalyst；The mass parts of containing hydrogen silicone oil 10, in advance
First add 0.2 part of reaction suppressor.The ultra-fine mass parts of ammonium carbonate 70,7 mass parts zinc stearate modifier treatments are previously added,
The mass parts of hollow glass microballoon 70.Then each component is sequentially added in reaction vessel, then using mechanical mixture 20min, obtained
To mixture；Then processing is ground to mixed material using the three-roll grinder that roll spacing is 0.1mm, obtained well mixed
Material, while the bubble in colloid mixture is excluded, in order to ensure the complete exclusion of bubble, it is further to its to reuse vacuum tank
Pump-down process.The sizing material being blended is poured into the mould of design, curing process is carried out at a temperature of being first placed in 50 DEG C, then will dress
The mould for having solidification blend glue stuff is put into 90 DEG C of vacuum drying chamber, is incubated 1 hour, is cooled to room temperature, obtains silicon rubber and answer
Rubber alloy material.
Embodiment 10
The vinyl polysiloxane of 100 mass parts is taken, is previously added 0.2 part of platinum catalyst, the mass parts of containing hydrogen silicone oil 2,
0.2 part of reaction suppressor is previously added, the ultra-fine mass parts of sodium acid carbonate 5, has been previously added at stearic acid modified dose of 0.5 mass parts
Reason, the mass parts of hollow glass microballoon 5.Then each component is sequentially added in reaction vessel, then using mechanical mixture 20min,
Obtain mixture；Then processing is ground to mixed material using the three-roll grinder that roll spacing is 0.1mm, is well mixed
Material, while exclude the bubble in colloid mixture, in order to ensure the complete exclusion of bubble, reuse vacuum tank and one is entered to it
Walk pump-down process.The sizing material being blended is poured into the mould of design, curing process is carried out at a temperature of being first placed in 50 DEG C, then will
Mould equipped with solidification blend glue stuff is put into 150 DEG C of vacuum drying chamber, after being incubated 1 hour, is cooled to room temperature, is obtained silicon rubber
Glue Composite rubber material.
Embodiment 11
The vinyl polysiloxane of 100 mass parts is taken, is previously added 0.2 part of platinum catalyst, the mass parts of containing hydrogen silicone oil 7,
0.2 part of reaction suppressor is previously added, the ultra-fine mass parts of sodium acid carbonate 5, has been previously added at stearic acid modified dose of 0.5 mass parts
Reason, the mass parts of hollow glass microballoon 5.Then each component is sequentially added in reaction vessel, then using mechanical mixture 20min,
Obtain mixture；Then processing is ground to mixed material using the three-roll grinder that roll spacing is 0.1mm, is well mixed
Material, while exclude the bubble in colloid mixture, in order to ensure the complete exclusion of bubble, reuse vacuum tank and one is entered to it
Walk pump-down process.The sizing material being blended is poured into the mould of design, be first placed in 50 DEG C of temperature and carry out curing process, then will dress
The mould for having the blend glue stuff after solidification is put into 150 DEG C of vacuum drying chamber, after being incubated 1 hour, is cooled to room temperature, is obtained silicon
Rubber composite sizing material.
Comparative example and the test result of each embodiment silicon rubber composite material are as shown in the table：
By testing and testing, the micropore silicon rubber composite material of gained high temperature resistant environment-protective is prepared compared to not compound silicon
Rubber, its heat insulation performance are obviously improved, meanwhile, carbonate and hollow glass microballoon asepsis environment-protecting itself, and
Carbonate decomposition product and carbonate modifiers also environment-protecting and non-poisonous evil, so, this method and its silicon rubber being prepared are compound
Meet environmental requirement.And by changing the ratio of inorganic carbonate and hollow glass microballoon, density and shore hardness can be regulated and controled
Etc. physical property.
It is pointed out that technical concepts and features of the embodiments of the invention only for the explanation present invention, its purpose exist
With allowing person skilled in the art it will be appreciated that the innovative point and content of the present invention, and implement according to this.According to patent of the present invention
The equivalent change or modification that application described construction, feature and principle are done, is included in the range of present patent application.
Claims (10)
1. a kind of high-temperature resistant micropore silicon rubber composite material, it is characterised in that the micropore silicon rubber composite material is by following component
Form by weight percentage：
Described reaction suppressor is acetylene basic ring alcohol；Described crosslinking catalyst is platinum catalyst；Described carbonate
Modifying agent is erucyl amide, stearic acid or Metallic stearates, and the particle size range of the ultra-fine carbonate is 1~20 micron, institute
State hollow glass microballoon a diameter of 1~50 micron.
2. micropore silicon rubber composite material as claimed in claim 1, it is characterised in that：The Metallic stearates are stearic acid
Zinc.
3. micropore silicon rubber composite material as claimed in claim 1, it is characterised in that：Described vinyl polysiloxane be containing
There is the vinyl polysiloxane of two or more vinyl.
4. micropore silicon rubber composite material as claimed in claim 1, it is characterised in that：Described vinyl polysiloxane is warp
Cross the vinyl polysiloxane of gas-phase silica reinforcement.
5. micropore silicon rubber composite material as claimed in claim 4, it is characterised in that：The ethene of the gas-phase silica reinforcement
Based polysiloxane is vinyl polysiloxane 0.3 part of white carbon of addition in 1 mass parts, is kneaded and obtains through kneader high intensity
The vinyl polysiloxane of reinforcement.
6. micropore silicon rubber composite material as claimed in claim 1, it is characterised in that：Reactive hydrogen matter in described containing hydrogen silicone oil
It is 0.18% to measure fraction, viscosity 1000mpa.s.
7. micropore silicon rubber composite material as claimed in claim 1, it is characterised in that：The ultra-fine carbonate is bicarbonate
One or more kinds of combinations of sodium, ammonium carbonate, ammonium hydrogen carbonate.
8. micropore silicon rubber composite material as claimed in claim 1, it is characterised in that：The ultra-fine carbonate and carbonate change
Property agent mass parts ratio be 10：1.
9. the micropore silicon rubber composite material as described in one of claim 1~8, it is characterised in that the microporous silicon is rubber combined
Material is made up of by weight percentage following component：
10. the preparation method of micropore silicon rubber composite material as claimed in claim 1, it is characterised in that methods described is：
(1) each component is weighed by proportioning, crosslinking catalyst is added in vinyl polysiloxane and is kneaded uniformly with kneader；Containing
Reaction suppressor is added in hydrogen silicone oil, is stirred with mixer；Carbonate modifiers are added in carbonate, with ball mill point
Dissipate uniformly, obtain the carbonate powder being modified；
(2) the above-mentioned each component by pretreatment is subjected to blending processing using mechanical means, each component is uniformly dispersed, obtain
Pre-composition, pre-composition is subjected to vacuum degassing bubble processing, is poured into afterwards in mould, is placed in 45~70 DEG C of temperature and is solidified, then
By 80~160 DEG C of 1~2h of isothermal holding, described micropore silicon rubber composite material is obtained.
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| CN109233770A (en) * | 2018-09-17 | 2019-01-18 | 天津大学 | A kind of high temperature resistant salt resistance elasticity profile control and water plugging particle and preparation method |
| CN109233770B (en) * | 2018-09-17 | 2020-10-30 | 天津大学 | High-temperature-resistant salt-resistant elastic profile control water plugging particles and preparation method thereof |
| CN110041711A (en) * | 2019-05-13 | 2019-07-23 | 河北宝瑞橡胶制品有限公司 | A kind of silicon rubber floating hollow sphere and preparation method thereof |
| CN114274578A (en) * | 2021-12-20 | 2022-04-05 | 深圳市众诚达应用材料科技有限公司 | Die sleeve and preparation and use methods thereof |
| CN114957770A (en) * | 2022-06-14 | 2022-08-30 | 华中科技大学 | Anisotropic porous material with adjustable pore diameter gradient and preparation method and application thereof |
| CN114957770B (en) * | 2022-06-14 | 2023-03-24 | 华中科技大学 | Anisotropic porous material with adjustable pore diameter gradient and preparation method and application thereof |
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