CN110127706A - A kind of preparation method of compound aerosil - Google Patents
A kind of preparation method of compound aerosil Download PDFInfo
- Publication number
- CN110127706A CN110127706A CN201910492062.1A CN201910492062A CN110127706A CN 110127706 A CN110127706 A CN 110127706A CN 201910492062 A CN201910492062 A CN 201910492062A CN 110127706 A CN110127706 A CN 110127706A
- Authority
- CN
- China
- Prior art keywords
- preparation
- compound aerosil
- compound
- wet gel
- aging
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910002012 Aerosil® Inorganic materials 0.000 title claims abstract description 31
- 150000001875 compounds Chemical class 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000011240 wet gel Substances 0.000 claims abstract description 17
- 239000000243 solution Substances 0.000 claims abstract description 12
- 230000032683 aging Effects 0.000 claims abstract description 11
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003365 glass fiber Substances 0.000 claims abstract description 7
- 125000002091 cationic group Chemical group 0.000 claims abstract description 6
- 239000003599 detergent Substances 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 238000002604 ultrasonography Methods 0.000 claims abstract description 5
- 230000007062 hydrolysis Effects 0.000 claims abstract description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 4
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims abstract description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Natural products CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical group [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 125000005909 ethyl alcohol group Chemical group 0.000 claims 1
- 238000009826 distribution Methods 0.000 abstract description 5
- 239000011148 porous material Substances 0.000 abstract description 5
- 239000004964 aerogel Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 239000000499 gel Substances 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 150000004703 alkoxides Chemical class 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- -1 oxygroup silicon alkane Chemical class 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000004965 Silica aerogel Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000003483 aging Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 1
- 230000004087 circulation Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
- C01B33/158—Purification; Drying; Dehydrating
- C01B33/1585—Dehydration into aerogels
Landscapes
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The present invention relates to aeroge technical field more particularly to a kind of preparation methods of compound aerosil.The present invention provides a kind of preparation methods of compound aerosil, comprising the following steps: step 1: methyltrimethoxysilane, aqueous hydrochloric acid solution, cationic detergent and glass fibre being mixed, hydrolysis obtains mixed solution；Step 2: the mixed solution ultrasound is obtained into wet gel；Step 3: the wet gel being impregnated in a solvent, dries simultaneously aging；Step 4: the wet gel after aging is modified, dry and modify to obtain compound aerosil.The present invention provides a kind of preparation method of compound aerosil, solve aeroge distribution of pores made from existing preparation method and the undesirable technical problem of granular size.
Description
Technical field
The present invention relates to aeroge technical field more particularly to a kind of preparation methods of compound aerosil.
Background technique
It is that current inorganic aerogels prepare a kind of most common technique that sol-gel method, which prepares wet gel, and this method is usual
Wet gel is first obtained using soda acid two-step catalysis legal system as presoma using alkoxide or salt, then again by subsequent suitable
Drying Treatment Technology wet gel is dry, to achieve the purpose that prepare the complete aeroge of skeleton.
The preparation of aeroge has in the fields such as aviation, photocatalytic degradation and solar battery largely studies and answers
With because the performances such as its calorifics, optics and photocatalysis, absorption and storage directly affect the quality of aerogel material and use valence
Value, so improving these performances as far as possible is the important indicator pursued in the industry.In the prior art, in order to improve aeroge this
A little physical properties are studied and are attempted on reaction condition and reagent selection, these want experimental technique and operating condition
It asks all very high, needs to control reaction time, rate and temperature of each step etc., need to use some strong oxidizers and some
Organic reagent, some oxidants or organic reagent, high volatility, and be not easy to obtain, the at high cost of industrial regeneration, pollution are big.No
It is suitable for industrialized production application.
Currently, using organosilicon alkoxide as precursor preparation SiO2Aeroge enters in the visual field of people, has many excellent
Point is for example soluble in ordinary organic solvents, it is hereby achieved that the solution of high-purity and high dispersive, high uniformity；It can be according to change
Composition is learned to be matched；Reaction temperature is low, can reduce generation of by-product etc..Although utilizing waterglass, multi-polysiloxane etc.
Cheap chemical reagent can also obtain corresponding target silica aerogel, still, aeroge made from these raw materials as precursor
Distribution of pores and granular size it is not satisfactory
Therefore, aeroge distribution of pores made from existing preparation method and granular size is undesirable becomes this field skill
Art personnel technical problem urgently to be resolved.
Summary of the invention
The present invention provides a kind of preparation methods of compound aerosil, solve existing preparation method system
The aeroge distribution of pores and the undesirable technical problem of granular size obtained.
The present invention provides a kind of preparation methods of compound aerosil, comprising the following steps:
Step 1: methyltrimethoxysilane, aqueous hydrochloric acid solution, cationic detergent and glass fibre being mixed, water
Solution obtains mixed solution；
Step 2: the mixed solution ultrasound is obtained into wet gel；
Step 3: the wet gel being impregnated in a solvent, dries simultaneously aging；
Step 4: the wet gel after aging is modified, dry and modify to obtain compound aerosil.
Preferably, cationic detergent described in step 1 is cetyl trimethylammonium bromide.
It preferably, further include adjusting pH between 3-4 in step 1 after mixing, before hydrolysis.
Preferably, the temperature of mixing described in step 1 is 30 DEG C.
It preferably, further include the ammonia spirit stirring 5 that 0.5mol/L is added after the step 1, before the step 2
Minute.
Preferably, solvent described in step 3 is the mixed solution of ethyl alcohol and n-hexane.
Preferably, the volume ratio of the ethyl alcohol and the n-hexane is 1:1.
Preferably, the time of aging described in step 3 is 12h.
Preferably, the temperature of aging described in step 3 is 60 DEG C.
Preferably, modification described in step 4 specifically includes the mixing of wet gel trim,ethylchlorosilane and n-hexane is molten
Liquid is modified.
Compared with prior art, the preparation method of compound aerosil provided by the invention, since surface is living
Property agent effectively control the condition and state of water-oil separating, so that silicon source is realized adequately dispersion and emulsification under high shear,
Under such circumstances, silica solution selectivity with higher in order to subsequent surface modification and adds the mixed of glass fibre
It closes, while the present invention is added glass fibre, mixes them thoroughly, obtain uniform aeroge under conditions of ultrasound.
Gas plural gel technology of preparing scheme made from preparation method provided by the invention is applied widely, especially suitable each
The preparation of kind aeroge such as inorganic aerogels, organic aerogel and organo-mineral complexing gel etc..It is provided by the invention compound
The preparation method of aerosil needs not move through interminable solvent displacement, and the technological process of production is short, at low cost, operation letter
It is single, it is desirable that few, hydrophobicity is strong, and the preferable enhancement aerosil product of performance parameter can be prepared, be conducive to
Industrialized production.The aeroge that preparation method provided by the invention is prepared both achievees the purpose that the various physical properties of improvement,
Very big environmental pollution is not will cause again.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention without any creative labor, may be used also for those of ordinary skill in the art
To obtain other attached drawings according to these attached drawings.
Fig. 1 is compound aerosil, pure silicon dioxide aeroge and glass made from the embodiment of the present invention 1
The infrared spectrum comparison diagram of fiber；
Fig. 2 is that the MTMS base aeroge uniaxial compression of compound aerosil made from the embodiment of the present invention 1 is bent
Line
Fig. 3 is that the uniaxial compression Rotation permutations of compound aerosil made from the embodiment of the present invention 1 are bent
Line chart
Wherein, appended drawing reference:
1, it recycles for the first time；2, it recycles for second；3, third time recycles
Specific embodiment
The embodiment of the invention provides a kind of preparation methods of compound aerosil, solve existing preparation
Aeroge distribution of pores made from method and the undesirable technical problem of granular size.
In order to make the invention's purpose, features and advantages of the invention more obvious and easy to understand, below in conjunction with the present invention
Attached drawing in embodiment, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that disclosed below
Embodiment be only a part of the embodiment of the present invention, and not all embodiment.Based on the embodiments of the present invention, this field
Those of ordinary skill's all other embodiment obtained without making creative work, belongs to protection of the present invention
Range.
Embodiment 1
After glass fibre is washed, 150 DEG C of oven drying 12h are put into, the substance of fiber residue is removed, carry out fluffy place
Reason.The MTMS (methyl trimethoxy oxygroup silicon alkane), H for being 0.08g by gross mass2O, aqueous hydrochloric acid solution and cationic detergent CTAB add
Enter in beaker, while a certain amount of glass fibre is added and is mixed evenly.PH is adjusted between 3-4, hydrolysis is stirred at 30 DEG C
1h, the ammonia spirit that 0.5mol/L is added stir after five minutes, and the gel in ultrasound guarantees that fibrous layer is evenly distributed, until formed
Wet gel.Wet gel is impregnated in the mixed solution of ethyl alcohol and n-hexane that volume ratio is 1:1, is put into 60 DEG C of oven ageings simultaneously
Replace 12h.It is modified with the mixed solution of TMCS and hexane solution, 12h is modified in 55-60 DEG C of baking oven.After the completion of modification
Wet gel, which is put into n-hexane, to be impregnated, rinses, 10 hours dry at 80 DEG C respectively, 2 hours dry at 120 DEG C, at 150 DEG C
Lower drying 1 hour.
To sum up, Fig. 1 is compound aerosil, general silica aeroge made from the embodiment of the present invention 1
And the infrared spectrum comparison diagram of fiber, as shown in Figure 1, composite aerogel made from the embodiment of the present invention has apparent hydrophobic group
Group.
As shown in Figure 2, the energy loss in 3 circulations of compound aerosil made from the embodiment of the present invention subtracts
Few partial white powder more and faster, fallen around each compression material simultaneously cracks with part, and pressure discharges
Afterwards sample can partial recovery, elasticity modulus reduction amount is greatly decreased.
From the figure 3, it may be seen that compound aerosil made from the embodiment of the present invention is just opened in compressive strength 20%
Begin fracture, is because by hydrophobic modification and fiber-loaded, the more ground surfaces of gel go out rigidity, are easily broken off.
The above, the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although referring to before
Stating embodiment, invention is explained in detail, those skilled in the art should understand that: it still can be to preceding
Technical solution documented by each embodiment is stated to modify or equivalent replacement of some of the technical features；And these
It modifies or replaces, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (10)
1. a kind of preparation method of compound aerosil, which comprises the following steps:
Step 1: methyltrimethoxysilane, aqueous hydrochloric acid solution, cationic detergent and glass fibre being mixed, hydrolyzed
To mixed solution；
Step 2: the mixed solution ultrasound is obtained into wet gel；
Step 3: the wet gel being impregnated in a solvent, dries simultaneously aging；
Step 4: the wet gel after aging is modified, dry and modify to obtain compound aerosil.
2. the preparation method of compound aerosil according to claim 1, which is characterized in that described in step 1
Cationic detergent is cetyl trimethylammonium bromide.
3. the preparation method of compound aerosil according to claim 1, which is characterized in that in step 1
It further include adjusting pH between 3-4 after mixing, before hydrolysis.
4. the preparation method of compound aerosil according to claim 1, which is characterized in that institute in step 1
The temperature for stating mixing is 30 DEG C.
5. the preparation method of compound aerosil according to claim 1, which is characterized in that in the step
It further include ammonia spirit stirring 5 minutes that 0.5mol/L is added after 1, before the step 2.
6. the preparation method of compound aerosil according to claim 1, which is characterized in that institute in step 3
State the mixed solution that solvent is ethyl alcohol and n-hexane.
7. the preparation method of compound aerosil according to claim 6, which is characterized in that the ethyl alcohol and
The volume ratio of the n-hexane is 1:1.
8. the preparation method of compound aerosil according to claim 1, which is characterized in that institute in step 3
The time for stating aging is 12h.
9. the preparation method of compound aerosil according to claim 1, which is characterized in that institute in step 3
The temperature for stating aging is 60 DEG C.
10. the preparation method of compound aerosil according to claim 1, which is characterized in that institute in step 4
Modified specifically include is stated to be modified the mixed solution of wet gel trim,ethylchlorosilane and n-hexane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910492062.1A CN110127706A (en) | 2019-06-06 | 2019-06-06 | A kind of preparation method of compound aerosil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910492062.1A CN110127706A (en) | 2019-06-06 | 2019-06-06 | A kind of preparation method of compound aerosil |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110127706A true CN110127706A (en) | 2019-08-16 |
Family
ID=67580709
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910492062.1A Pending CN110127706A (en) | 2019-06-06 | 2019-06-06 | A kind of preparation method of compound aerosil |
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| Country | Link |
|---|---|
| CN (1) | CN110127706A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115536914A (en) * | 2022-10-17 | 2022-12-30 | 山西浙大新材料与化工研究院 | Composite anti-aging agent, preparation method thereof and heat-resistant rubber material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101973752A (en) * | 2010-10-21 | 2011-02-16 | 厦门大学 | Glass fiber reinforced silicon dioxide aerogel composite material and preparation method thereof |
| CN103396086A (en) * | 2013-08-08 | 2013-11-20 | 厦门大学 | Preparation method for glass fiber-reinforced water glass-based silica composite aerogel |
| JP2017114744A (en) * | 2015-12-25 | 2017-06-29 | パナソニックＩｐマネジメント株式会社 | Hydrophilic silica aerogel and manufacturing method therefor and heat insulator |
| CN109516763A (en) * | 2019-01-07 | 2019-03-26 | 东华大学 | A kind of cellulose fibre/SiO2Aerogel composite and its preparation and application |
-
2019
- 2019-06-06 CN CN201910492062.1A patent/CN110127706A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101973752A (en) * | 2010-10-21 | 2011-02-16 | 厦门大学 | Glass fiber reinforced silicon dioxide aerogel composite material and preparation method thereof |
| CN103396086A (en) * | 2013-08-08 | 2013-11-20 | 厦门大学 | Preparation method for glass fiber-reinforced water glass-based silica composite aerogel |
| JP2017114744A (en) * | 2015-12-25 | 2017-06-29 | パナソニックＩｐマネジメント株式会社 | Hydrophilic silica aerogel and manufacturing method therefor and heat insulator |
| CN109516763A (en) * | 2019-01-07 | 2019-03-26 | 东华大学 | A kind of cellulose fibre/SiO2Aerogel composite and its preparation and application |
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| Title |
|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115536914A (en) * | 2022-10-17 | 2022-12-30 | 山西浙大新材料与化工研究院 | Composite anti-aging agent, preparation method thereof and heat-resistant rubber material |
| CN115536914B (en) * | 2022-10-17 | 2023-06-09 | 山西浙大新材料与化工研究院 | Composite anti-aging agent, preparation method thereof and heat-resistant rubber material |
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