CN114790000B - High-temperature-resistant sealing material based on expanded graphite and preparation method thereof - Google Patents
High-temperature-resistant sealing material based on expanded graphite and preparation method thereof Download PDFInfo
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- CN114790000B CN114790000B CN202210411713.1A CN202210411713A CN114790000B CN 114790000 B CN114790000 B CN 114790000B CN 202210411713 A CN202210411713 A CN 202210411713A CN 114790000 B CN114790000 B CN 114790000B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 187
- 239000010439 graphite Substances 0.000 title claims abstract description 180
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 180
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000003566 sealing material Substances 0.000 title claims abstract description 14
- 239000010455 vermiculite Substances 0.000 claims abstract description 94
- 235000019354 vermiculite Nutrition 0.000 claims abstract description 94
- 229910052902 vermiculite Inorganic materials 0.000 claims abstract description 94
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 48
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 47
- INQDDHNZXOAFFD-UHFFFAOYSA-N 2-[2-(2-prop-2-enoyloxyethoxy)ethoxy]ethyl prop-2-enoate Chemical compound C=CC(=O)OCCOCCOCCOC(=O)C=C INQDDHNZXOAFFD-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000002002 slurry Substances 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 28
- IEPRKVQEAMIZSS-AATRIKPKSA-N diethyl fumarate Chemical compound CCOC(=O)\C=C\C(=O)OCC IEPRKVQEAMIZSS-AATRIKPKSA-N 0.000 claims abstract description 23
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000003825 pressing Methods 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 10
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 6
- 238000009830 intercalation Methods 0.000 claims abstract description 5
- 230000002687 intercalation Effects 0.000 claims abstract description 5
- 230000001590 oxidative effect Effects 0.000 claims abstract description 4
- 238000005470 impregnation Methods 0.000 claims abstract description 3
- 239000007800 oxidant agent Substances 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- 238000001035 drying Methods 0.000 claims description 38
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- 238000001914 filtration Methods 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 19
- 230000007935 neutral effect Effects 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 12
- 239000003963 antioxidant agent Substances 0.000 claims description 10
- 230000003078 antioxidant effect Effects 0.000 claims description 10
- 238000002386 leaching Methods 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000011159 matrix material Substances 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- 238000000643 oven drying Methods 0.000 claims description 2
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 238000000576 coating method Methods 0.000 abstract description 6
- 239000011248 coating agent Substances 0.000 abstract description 5
- 239000000945 filler Substances 0.000 abstract description 4
- 238000007789 sealing Methods 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 239000003513 alkali Substances 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 40
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 32
- 239000012153 distilled water Substances 0.000 description 25
- 238000012360 testing method Methods 0.000 description 20
- 239000000243 solution Substances 0.000 description 18
- 238000000498 ball milling Methods 0.000 description 16
- 229910052759 nickel Inorganic materials 0.000 description 16
- 238000005259 measurement Methods 0.000 description 14
- 239000011259 mixed solution Substances 0.000 description 13
- 235000021355 Stearic acid Nutrition 0.000 description 10
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical group CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 10
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 10
- 239000008117 stearic acid Substances 0.000 description 10
- CUVLMZNMSPJDON-UHFFFAOYSA-N 1-(1-butoxypropan-2-yloxy)propan-2-ol Chemical compound CCCCOCC(C)OCC(C)O CUVLMZNMSPJDON-UHFFFAOYSA-N 0.000 description 9
- 239000002202 Polyethylene glycol Substances 0.000 description 9
- 238000004140 cleaning Methods 0.000 description 9
- 238000007254 oxidation reaction Methods 0.000 description 9
- 229920001223 polyethylene glycol Polymers 0.000 description 9
- 239000004359 castor oil Substances 0.000 description 8
- 235000019438 castor oil Nutrition 0.000 description 8
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 8
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 7
- 239000007770 graphite material Substances 0.000 description 7
- 238000000227 grinding Methods 0.000 description 7
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 7
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 7
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 7
- -1 acrylic ester Chemical class 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 230000004580 weight loss Effects 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000011229 interlayer Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 150000005837 radical ions Chemical class 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/22—Intercalation
- C01B32/225—Expansion; Exfoliation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/10—Materials in mouldable or extrudable form for sealing or packing joints or covers
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides a high-temperature resistant sealing material based on expanded graphite and a preparation method thereof, belonging to the technical field of sealing filler, wherein the high-temperature resistant sealing material comprises the steps of mixing water, diethyl fumarate, absolute ethyl alcohol, triethylene glycol diacrylate and natural crystalline flake graphite, and purifying the graphite by an alkali acid method; potassium permanganate is used as an oxidant, perchloric acid and ammonium nitrate are used as intercalation agents, and high-purity graphite is intercalated; expanding and pressing graphite; and coating vermiculite slurry on the flexible graphite by adopting a coating method or an impregnation method to obtain the high-temperature-resistant flexible graphite. The high-temperature-resistant flexible graphite and the preparation method thereof have the advantages of low cost, simplicity in operation and excellent tensile strength and high-temperature resistance of products.
Description
Technical Field
The invention belongs to the technical field of sealing fillers, and particularly relates to a high-temperature-resistant sealing material based on expanded graphite and a preparation method thereof.
Background
As a graphite finishing material, flexible graphite was invented by united carbide corporation in the sixty of the last century. The preparation principle is as follows: the natural crystalline flake graphite is used as raw material, and the intercalation of oxyacid radical ions into the interlayer of graphite to form Graphite Interlayer Compound (GIC) with new interlayer property and without damaging the graphite layered structure under proper reaction conditions. Through high-temperature heat treatment, oxygen acid radicals in the interlayer compound of the graphite are rapidly vaporized, decomposed and volatilized, and huge tension is generated between graphite layers, so that the expandable graphite is rapidly expanded into a worm shape. This expanded vermicular graphite is known as expanded graphite. The vermicular expanded graphite is mutually extruded and locked by rolling, mould pressing and other modes, and the flexible graphite sheet with smooth surface is prepared.
The flexible graphite material is widely applied in the field of sealing materials because of its excellent performance. However, in industrial production, there are many industrial environments where high temperature and oxygen are required to use sealing materials, and the requirements on the high temperature and oxidation resistance of the sealing materials are becoming more and more severe. And the flexible graphite sealing material has a tolerance temperature of not more than 450 ℃ under the aerobic condition. After the temperature exceeds 750 ℃, the oxidation reaction of the flexible graphite is aggravated, and the weight is quickly lost. After being oxidized, the smooth and flat surface of the flexible graphite sealing material becomes uneven, so that leakage is easy to occur, the sealing element is invalid, and serious production safety accidents are caused. Therefore, improving the oxidation resistance of flexible graphite sealing materials is an important point of current research.
The prior art, such as the Chinese patent with publication number of CN 111662678A, discloses a preparation method of high-temperature antioxidant flexible graphite filler, which comprises the following steps: soaking natural crystalline flake graphite in intercalation agent solution, washing with water, and expanding at 850-950 deg.c for 10-15 s to obtain expanded graphite worms; uniformly covering the surface of the reinforced material with the adhesive with the step-expanded graphite worms, and mechanically pressing to obtain a flexible graphite sheet; and (3) immersing the flexible graphite sheet in an antioxidant solution, drying, and heating in a gradient way to obtain the high-temperature antioxidant flexible graphite filler. The invention solves the problem of poor high-temperature oxidation resistance of flexible graphite in the prior art. The antioxidant is soaked on the surface of the flexible graphite sheet or inside the flexible graphite sheet, and the temperature is raised in a gradient way, so that the antioxidant permeates into the graphite material to be converted into a high-temperature antioxidant substance, and the high-temperature antioxidant substance is filled into the graphite material and covers the surface of the graphite. The antioxidant does not need to crush and impregnate the flexible graphite sheet material, and the operation is simpler and more convenient.
Disclosure of Invention
The invention aims to provide high-temperature-resistant flexible graphite and a preparation method thereof, and the method has the advantages of low cost and simplicity in operation, and can improve the purity of graphite, reduce the chipping rate of expanded graphite and improve the tensile strength and high-temperature resistance of flexible graphite.
The technical scheme adopted by the invention for achieving the purpose is as follows:
provided is a method for preparing expanded graphite, comprising:
s1, preparing high-purity graphite: mixing natural crystalline flake graphite with solid NaOH, adding water, diethyl fumarate, absolute ethyl alcohol and triethylene glycol diacrylate, performing ultrasonic dispersion, drying, roasting, washing to be neutral, and filtering; adding hydrochloric acid solution for leaching, washing with water to neutrality, filtering, and oven drying;
s2, preparing expandable graphite: the method comprises the steps of (1) intercalation is carried out on high-purity graphite by taking potassium permanganate as an oxidant and perchloric acid and ammonium nitrate as intercalators, so that sulfur-free expandable graphite is obtained;
and S3, heating and expanding the sulfur-free expandable graphite to obtain the expanded graphite. When the method is used for preparing the high-purity graphite, the cost can be simplified, and the purity of the prepared graphite is higher, so that the chipping rate can be reduced when the method is used for preparing the expanded graphite.
In certain embodiments, the mass ratio of potassium permanganate to high purity graphite is 0.35 to 0.6:1.
In certain embodiments, the mass ratio of perchloric acid to high purity graphite is 8-10:1 and the mass ratio of ammonium nitrate to high purity graphite is 0.04-0.12:1.
In certain embodiments, the mass ratio of the natural crystalline flake graphite to the solid NaOH is 1:0.35-0.5.
In certain embodiments, the mass to volume ratio of the natural crystalline flake graphite to the hydrochloric acid solution is 1:1-1.5.
Preferably, the concentration of the above hydrochloric acid solution is 36 to 38wt%.
In certain embodiments, the volume ratio of diethyl fumarate to absolute ethanol is 1:2.5-4.
In certain embodiments, the mass ratio of diethyl fumarate to triethylene glycol diacrylate is from 1:0.3 to 0.7. The existence of impurities such as oil stain on the surface of the graphite ensures that the surface of the graphite is hydrophobic, and the existence of triethylene glycol diacrylate and diethyl fumarate is beneficial to removing the oil stain on the surface of the graphite, so that the reaction of sodium hydroxide and the graphite impurities is facilitated, the purity of the graphite is further improved, the debris rate of the expanded graphite is reduced, and the tensile strength of the flexible graphite is improved.
The expanded graphite is prepared by the preparation method of the expanded graphite.
The preparation method of the high-temperature-resistant flexible graphite comprises the following steps:
A. pressing the expanded graphite to obtain flexible graphite;
B. the high-temperature-resistant flexible graphite is prepared by taking vermiculite slurry as an antioxidant and flexible graphite as a matrix.
In certain embodiments, the method of making a vermiculite slurry described above comprises: dissolving castor oil in absolute ethyl alcohol, mixing with peeled expanded vermiculite powder, ball milling, wherein the rotating speed of a mill is 180-220r/min, and the ball milling time is 20-40min; continuously adding polyvinyl butyral, dipropylene glycol butyl ether, polyethylene glycol acrylic ester and distilled water for secondary ball milling, wherein the rotating speed of a mill is 180-220r/min, and the ball milling time is 60-120min. The dipropylene glycol butyl ether and polyethylene glycol acrylic ester are added in the process of preparing the vermiculite slurry, so that on one hand, the adhesion of the vermiculite to the flexible graphite material can be promoted, on the other hand, the flow property of the vermiculite slurry can be optimized, the uniform coverage of the vermiculite to the flexible graphite is facilitated, and the purposes of reducing the aperture ratio of the flexible graphite and improving the high temperature resistance of the flexible graphite are achieved.
Preferably, the vermiculite slurry contains 0.5 to 1.0wt% castor oil.
Preferably, the vermiculite slurry contains 2.5 to 3.5wt% polyvinyl butyral.
Preferably, the vermiculite slurry contains 30-42wt% exfoliated expanded vermiculite powder.
Preferably, the vermiculite slurry contains 40-50wt% absolute ethyl alcohol.
Preferably, the vermiculite slurry contains 0.1 to 0.5wt% dipropylene glycol butyl ether.
Preferably, the vermiculite slurry contains 0.4-0.8wt% of polyethylene glycol acrylate.
In certain embodiments, step B above comprises: spraying the vermiculite slurry on the surface of flexible graphite, and drying at 102-108 ℃.
In certain embodiments, step B above comprises: the flexible graphite is put into vermiculite slurry, impregnated for 1-2 hours under the conditions of vacuum degree of 0.02-0.06MPa, impregnation temperature of 25-30 ℃ and stirring speed of 150-180r/min, and then the flexible graphite is taken out and dried at 102-108 ℃.
In some embodiments, the preparation method of the peeled expanded vermiculite powder comprises the following steps: placing the expanded vermiculite in a planetary ball mill, adding sodium hexametaphosphate accounting for 0.2-0.3wt% of the expanded vermiculite, absolute ethyl alcohol, grinding at a rotating speed of 180-220r/min and for 3.5-5h, filtering and drying to obtain peeled expanded vermiculite powder.
In certain embodiments, the exfoliated vermiculite is stearic acid modified exfoliated vermiculite.
Preferably, the method for peeling the stearic acid modified exfoliated expanded vermiculite comprises the following steps: dissolving stearic acid in absolute ethyl alcohol, dripping the absolute ethyl alcohol into peeled expanded vermiculite powder in a high-speed mixer for modification, taking out the modified powder after 20 to 30 minutes, and drying the modified powder to obtain peeled expanded vermiculite powder. More preferably, the stearic acid is 2-2.5wt% of the exfoliated expanded vermiculite powder.
The high-temperature-resistant flexible graphite is prepared by adopting the preparation method of the high-temperature-resistant flexible graphite.
The application of the preparation method of the high-temperature-resistant flexible graphite in preparing sealing materials is provided.
In the preparation of the high-purity graphite, the diethyl fumarate, the triethylene glycol diacrylate and the ethanol are adopted to remove oil stains on the surface of the graphite, so that the preparation method has the following beneficial effects: the presence of triethylene glycol diacrylate and diethyl fumarate is beneficial to removing oil stains on the surface of graphite, so that the reaction of sodium hydroxide and graphite impurities is facilitated, the purity of graphite is further improved, the debris rate of expanded graphite is reduced, and the tensile strength of flexible graphite is improved.
The invention has the following beneficial effects that dipropylene glycol butyl ether and polyethylene glycol acrylic ester are added in the preparation process of vermiculite slurry when preparing high-temperature-resistant flexible graphite, and the invention has the following advantages: the method can optimize the flow property of vermiculite slurry, is favorable for uniformly covering the flexible graphite by the vermiculite, and can promote the adhesion of the vermiculite to the flexible graphite material, thereby achieving the purposes of reducing the aperture ratio of the flexible graphite and improving the high temperature resistance of the flexible graphite.
Therefore, the invention is the high-temperature-resistant flexible graphite with lower cost, simple operation and excellent tensile strength and high-temperature resistance of the product and the preparation method thereof.
Drawings
FIG. 1 is a measurement result of the contact angle in test example 1 of the present invention;
FIG. 2 is a graph showing the results of measuring the fixed carbon content in test example 1 of the present invention;
FIG. 3 is a graph showing the result of measurement of the chipping rate in test example 1 of the present invention;
FIG. 4 shows the measurement results of tensile strength in test example 1 of the present invention;
FIG. 5 is a scanning electron microscope image of test example 2 according to the present invention;
FIG. 6 is a graph showing the results of measurement of the viscosity in test example 2 according to the present invention;
FIG. 7 shows the results of measuring the rate of decrease in the aperture ratio in test example 2 of the present invention;
FIG. 8 shows the results of measurement of the oxidation weight loss ratio in test example 2 according to the present invention.
Detailed Description
The invention is described in further detail below with reference to examples:
example 1:
1. a method of preparing expanded graphite comprising:
1.1, mixing 5g of natural crystalline flake graphite and 2g of solid NaOH, adding 5mL of water, 2mL of diethyl fumarate, 6mL of absolute ethyl alcohol and 1mL of triethylene glycol diacrylate into a nickel crucible, dispersing by adopting ultrasonic waves, and drying at 70 ℃ for 3 hours; placing the nickel crucible into a muffle furnace, and roasting for 2 hours at 650 ℃; after roasting, washing the mixture to be neutral by distilled water, and filtering; 7mL 36wt% hydrochloric acid solution is added, leaching is carried out for 1h at 70 ℃, then distilled water is used for cleaning to neutrality, and drying is carried out for 3h at 70 ℃ to obtain high purity graphite.
1.2 adding 2.5g of potassium permanganate into a beaker filled with 45g of perchloric acid, uniformly stirring, adding 5g of high-purity graphite with the particle size of +0.500mm, uniformly stirring, then adding 0.4g of ammonium nitrate, uniformly stirring, stirring at 30 ℃ for reaction for 30min, controlling the stirring speed to be 200r/min, washing with distilled water to be neutral after the reaction is finished, carrying out suction filtration, removing filtrate, and then drying at 70 ℃ for 3h to obtain the expandable graphite.
1.3 the expandable graphite was subjected to expansion at 400℃for 20s to obtain expanded graphite.
2. A preparation method of a high-temperature-resistant flexible sealing material comprises the following steps:
2.1 pressing the expanded graphite obtained in 1 under the following conditions: the initial pressure intensity is 1MPa, and the pressing is performed four times, and the time is 1min each time; the re-pressing pressure is 2MPa, the pressing time is 1min each time, the final pressing pressure is 3MPa, the pressing time is 1min each time; after the completion of the pressing, a square sheet (thickness 0.89 mm) of 50mm×50mm was cut to obtain a flexible graphite sample.
2.2 preparation of vermiculite slurry:
2.2.1 placing 16g of expanded vermiculite in a planetary ball mill, adding 0.032g of sodium hexametaphosphate, 64g of absolute ethyl alcohol, rotating at 200r/min, grinding for 4h, filtering, and drying at 105 ℃ for 1h to obtain peeled expanded vermiculite powder.
2.2.2 stirring 16g of exfoliated expanded vermiculite powder in a high-speed mixer, dissolving 0.32g of stearic acid in 16g of absolute ethyl alcohol, then dripping into the high-speed mixer filled with exfoliated expanded vermiculite powder for stirring and modifying, taking out after modifying for 20min, and drying for 30min at 105 ℃ to obtain exfoliated expanded vermiculite modified powder.
2.2.3, 0.36g of castor oil is dissolved in 18g of absolute ethyl alcohol, mixed with 16g of exfoliated expanded vermiculite modified powder, ball-milled at the rotating speed of 200r/min for 30min; continuously adding 1.3g of polyvinyl butyral, 0.1g of dipropylene glycol butyl ether, 0.24g of polyethylene glycol acrylic ester and 4g of distilled water for secondary ball milling, wherein the rotating speed of a mill is 200r/min, and the ball milling time is 80min, so as to obtain vermiculite slurry.
2.3 uniformly spraying 5mL of vermiculite slurry on the surface of the 50mm multiplied by 50mm flexible graphite sample, and then drying at 105 ℃ for 1h to obtain the high-temperature-resistant flexible graphite sample.
Example 2:
1. a method of preparing expanded graphite comprising:
1.1, adding 5g of natural crystalline flake graphite and 2g of solid NaOH into a nickel crucible, adding 5mL of water, 2mL of diethyl fumarate, 6mL of absolute ethyl alcohol and 0.8mL of triethylene glycol diacrylate, dispersing by adopting ultrasonic waves, and drying at 70 ℃ for 3 hours; placing the nickel crucible into a muffle furnace, and roasting for 2 hours at 650 ℃; after roasting, washing the mixture to be neutral by distilled water, and filtering; 7mL 36wt% hydrochloric acid solution is added, leaching is carried out for 1h at 70 ℃, then distilled water is used for cleaning to neutrality, and drying is carried out for 3h at 70 ℃ to obtain high purity graphite. The remainder is the same as in example 1.
Example 3:
1. a method of preparing expanded graphite comprising:
1.1, adding 5g of natural crystalline flake graphite and 2g of solid NaOH into a nickel crucible, adding 5mL of water, 2mL of diethyl fumarate, 6mL of absolute ethyl alcohol and 1.2mL of triethylene glycol diacrylate, dispersing by adopting ultrasonic waves, and drying at 70 ℃ for 3 hours; placing the nickel crucible into a muffle furnace, and roasting for 2 hours at 650 ℃; after roasting, washing the mixture to be neutral by distilled water, and filtering; 7mL 36wt% hydrochloric acid solution is added, leaching is carried out for 1h at 70 ℃, then distilled water is used for cleaning to neutrality, and drying is carried out for 3h at 70 ℃ to obtain high purity graphite. The remainder is the same as in example 1.
Example 4:
1. a method of preparing expanded graphite comprising:
1.1, adding 5g of natural crystalline flake graphite and 2g of solid NaOH into a nickel crucible, adding 5mL of water, 2mL of diethyl fumarate, 6mL of absolute ethyl alcohol and 0.2mL of triethylene glycol diacrylate, dispersing by adopting ultrasonic waves, and drying at 70 ℃ for 3 hours; placing the nickel crucible into a muffle furnace, and roasting for 2 hours at 650 ℃; after roasting, washing the mixture to be neutral by distilled water, and filtering; 10mL of 36wt% hydrochloric acid solution is added, leaching is carried out for 1h at 70 ℃, then distilled water is used for cleaning to be neutral, and drying is carried out for 3h at 70 ℃ to obtain high-purity graphite. The remainder is the same as in example 1.
Example 5:
1. a method of preparing expanded graphite comprising:
1.1, adding 5g of natural crystalline flake graphite and 2g of solid NaOH into a nickel crucible, adding 5mL of water, 2mL of diethyl fumarate, 6mL of absolute ethyl alcohol and 1.8mL of triethylene glycol diacrylate, dispersing by adopting ultrasonic waves, and drying at 70 ℃ for 3 hours; placing the nickel crucible into a muffle furnace, and roasting for 2 hours at 650 ℃; after roasting, washing the mixture to be neutral by distilled water, and filtering; 10mL of 36wt% hydrochloric acid solution is added, leaching is carried out for 1h at 70 ℃, then distilled water is used for cleaning to be neutral, and drying is carried out for 3h at 70 ℃ to obtain high-purity graphite. The remainder is the same as in example 1.
Example 6:
1. a method of preparing expanded graphite comprising:
1.1, adding 5g of natural crystalline flake graphite and 2g of solid NaOH into a nickel crucible, adding 5mL of water, 2mL of diethyl fumarate and 6mL of absolute ethyl alcohol, dispersing by adopting ultrasonic waves, and drying at 70 ℃ for 3 hours; placing the nickel crucible into a muffle furnace, and roasting for 2 hours at 650 ℃; after roasting, washing the mixture to be neutral by distilled water, and filtering; 10mL of 36wt% hydrochloric acid solution is added, leaching is carried out for 1h at 70 ℃, then distilled water is used for cleaning to be neutral, and drying is carried out for 3h at 70 ℃ to obtain high-purity graphite. The remainder is the same as in example 1.
Example 7:
1. a method of preparing expanded graphite comprising:
1.1, adding 5g of natural crystalline flake graphite and 2g of solid NaOH into a nickel crucible, adding 5mL of water, 6mL of absolute ethyl alcohol and 1mL of triethylene glycol diacrylate, dispersing by adopting ultrasonic waves, and drying at 70 ℃ for 3 hours; placing the nickel crucible into a muffle furnace, and roasting for 2 hours at 650 ℃; after roasting, washing the mixture to be neutral by distilled water, and filtering; 10mL of 36wt% hydrochloric acid solution is added, leaching is carried out for 1h at 70 ℃, then distilled water is used for cleaning to be neutral, and drying is carried out for 3h at 70 ℃ to obtain high-purity graphite. The remainder is the same as in example 1.
Example 8:
1. a method of preparing expanded graphite comprising:
1.1, mixing 5g of natural crystalline flake graphite and 2g of solid NaOH, adding 5mL of water and 6mL of absolute ethyl alcohol into a nickel crucible, dispersing by adopting ultrasonic waves, and drying at 70 ℃ for 3 hours; placing the nickel crucible into a muffle furnace, and roasting for 2 hours at 650 ℃; after roasting, washing the mixture to be neutral by distilled water, and filtering; 10mL of 36wt% hydrochloric acid solution is added, leaching is carried out for 1h at 70 ℃, then distilled water is used for cleaning to be neutral, and drying is carried out for 3h at 70 ℃ to obtain high-purity graphite. The remainder is the same as in example 1.
Example 9:
2.2 preparation of vermiculite slurry:
2.2.1 placing 16g of expanded vermiculite in a planetary ball mill, adding 0.032g of sodium hexametaphosphate, 64g of absolute ethyl alcohol, rotating at 200r/min, grinding for 4h, filtering, and drying at 105 ℃ for 1h to obtain peeled expanded vermiculite powder.
2.2.2 stirring 16g of exfoliated expanded vermiculite powder in a high-speed mixer, dissolving 0.32g of stearic acid in 16g of absolute ethyl alcohol, then dripping into the high-speed mixer filled with exfoliated expanded vermiculite powder for stirring and modifying, taking out after modifying for 20min, and drying for 30min at 105 ℃ to obtain exfoliated expanded vermiculite modified powder.
2.2.3, 0.36g of castor oil is dissolved in 18g of absolute ethyl alcohol, mixed with 16g of exfoliated expanded vermiculite modified powder, ball-milled at the rotating speed of 200r/min for 30min; continuously adding 1.3g of polyvinyl butyral, 0.12g of dipropylene glycol butyl ether, 0.22g of polyethylene glycol acrylic ester and 4g of distilled water for secondary ball milling, wherein the rotating speed of a mill is 200r/min, and the ball milling time is 80min, so as to obtain vermiculite slurry. The remainder is the same as in example 1.
Example 10:
2.2 preparation of vermiculite slurry:
2.2.1 placing 16g of expanded vermiculite in a planetary ball mill, adding 0.032g of sodium hexametaphosphate, 64g of absolute ethyl alcohol, rotating at 200r/min, grinding for 4h, filtering, and drying at 105 ℃ for 1h to obtain peeled expanded vermiculite powder.
2.2.2 stirring 16g of exfoliated expanded vermiculite powder in a high-speed mixer, dissolving 0.32g of stearic acid in 16g of absolute ethyl alcohol, then dripping into the high-speed mixer filled with exfoliated expanded vermiculite powder for stirring and modifying, taking out after modifying for 20min, and drying for 30min at 105 ℃ to obtain exfoliated expanded vermiculite modified powder.
2.2.3, 0.36g of castor oil is dissolved in 18g of absolute ethyl alcohol, mixed with 16g of exfoliated expanded vermiculite modified powder, ball-milled at the rotating speed of 200r/min for 30min; continuously adding 1.3g of polyvinyl butyral, 0.16g of dipropylene glycol butyl ether, 0.18g of polyethylene glycol acrylic ester and 4g of distilled water for secondary ball milling, wherein the rotating speed of a mill is 200r/min, and the ball milling time is 80min, so as to obtain vermiculite slurry. The remainder is the same as in example 1.
Example 11:
2.2 preparation of vermiculite slurry:
2.2.1 placing 16g of expanded vermiculite in a planetary ball mill, adding 0.032g of sodium hexametaphosphate, 64g of absolute ethyl alcohol, rotating at 200r/min, grinding for 4h, filtering, and drying at 105 ℃ for 1h to obtain peeled expanded vermiculite powder.
2.2.2 stirring 16g of exfoliated expanded vermiculite powder in a high-speed mixer, dissolving 0.32g of stearic acid in 16g of absolute ethyl alcohol, then dripping into the high-speed mixer filled with exfoliated expanded vermiculite powder for stirring and modifying, taking out after modifying for 20min, and drying for 30min at 105 ℃ to obtain exfoliated expanded vermiculite modified powder.
2.2.3, 0.36g of castor oil is dissolved in 18g of absolute ethyl alcohol, mixed with 16g of exfoliated expanded vermiculite modified powder, ball-milled at the rotating speed of 200r/min for 30min; continuously adding 1.3g of polyvinyl butyral, 0.1g of dipropylene glycol butyl ether and 4.24g of distilled water for secondary ball milling, wherein the rotating speed of a mill is 200r/min, and the ball milling time is 80min, so as to obtain vermiculite slurry. The remainder is the same as in example 1.
Example 12:
2.2 preparation of vermiculite slurry:
2.2.1 placing 16g of expanded vermiculite in a planetary ball mill, adding 0.032g of sodium hexametaphosphate, 64g of absolute ethyl alcohol, rotating at 200r/min, grinding for 4h, filtering, and drying at 105 ℃ for 1h to obtain peeled expanded vermiculite powder.
2.2.2 stirring 16g of exfoliated expanded vermiculite powder in a high-speed mixer, dissolving 0.32g of stearic acid in 16g of absolute ethyl alcohol, then dripping into the high-speed mixer filled with exfoliated expanded vermiculite powder for stirring and modifying, taking out after modifying for 20min, and drying for 30min at 105 ℃ to obtain exfoliated expanded vermiculite modified powder.
2.2.3, 0.36g of castor oil is dissolved in 18g of absolute ethyl alcohol, mixed with 16g of exfoliated expanded vermiculite modified powder, ball-milled at the rotating speed of 200r/min for 30min; continuously adding 1.3g of polyvinyl butyral, 0.24g of polyethylene glycol acrylate and 4.1g of distilled water for secondary ball milling, wherein the rotating speed of a mill is 200r/min, and the ball milling time is 80min, so as to obtain vermiculite slurry. The remainder is the same as in example 1.
Example 13:
2.2 preparation of vermiculite slurry:
2.2.1 placing 16g of expanded vermiculite in a planetary ball mill, adding 0.032g of sodium hexametaphosphate, 64g of absolute ethyl alcohol, rotating at 200r/min, grinding for 4h, filtering, and drying at 105 ℃ for 1h to obtain peeled expanded vermiculite powder.
2.2.2 stirring 16g of exfoliated expanded vermiculite powder in a high-speed mixer, dissolving 0.32g of stearic acid in 16g of absolute ethyl alcohol, then dripping into the high-speed mixer filled with exfoliated expanded vermiculite powder for stirring and modifying, taking out after modifying for 20min, and drying for 30min at 105 ℃ to obtain exfoliated expanded vermiculite modified powder.
2.2.3, 0.36g of castor oil is dissolved in 18g of absolute ethyl alcohol, mixed with 16g of exfoliated expanded vermiculite modified powder, ball-milled at the rotating speed of 200r/min for 30min; and continuously adding 1.3g of polyvinyl butyral and 4.34g of distilled water for secondary ball milling, wherein the rotating speed of a mill is 200r/min, and the ball milling time is 80min, so as to obtain vermiculite slurry. The remainder is the same as in example 1.
Test example 1:
1.1 measurement of contact angle:
mixed solution a:5mL of water, 2mL of diethyl fumarate, 6mL of absolute ethyl alcohol and 1mL of triethylene glycol diacrylate;
mixed solution b:5mL of water, 2mL of diethyl fumarate, 6mL of absolute ethyl alcohol and 0.8mL of triethylene glycol diacrylate;
mixing solution c:5mL of water, 2mL of diethyl fumarate, 6mL of absolute ethyl alcohol and 1.2mL of triethylene glycol diacrylate;
mixing solution d:5mL of water, 2mL of diethyl fumarate, 6mL of absolute ethyl alcohol and 0.2mL of triethylene glycol diacrylate;
mixed solution e:5mL of water, 2mL of diethyl fumarate, 6mL of absolute ethyl alcohol and 1.8mL of triethylene glycol diacrylate;
mixing solution f:5mL of water, 2mL of diethyl fumarate and 6mL of absolute ethyl alcohol;
mixed solution g:5mL of water, 6mL of absolute ethyl alcohol and 1mL of triethylene glycol diacrylate;
mixing solution h:5mL of water and 6mL of absolute ethanol;
respectively putting 5g of natural crystalline flake graphite into the mixed solution, dispersing by adopting ultrasonic waves, soaking for 3min, drying at 70 ℃ for 3h, putting a certain amount of natural crystalline flake graphite into a tabletting mold, tabletting by using a table tabletting machine, keeping the pressure at 10MPa for 2min, and obtaining a flaky sample; opening a contact angle measuring instrument and data processing software, filling deionized water into a needle cylinder, placing a pressed powder sample on a sample table, performing a contact angle test by a sitting-drop method, and reading the contact angle of liquid drops on the surface of a solid sample by a tangent method. The measurement results of the contact angle are shown in FIG. 1.
1.2 fixed carbon content determination: the method for testing the fixed carbon content of the graphite comprises the steps of firstly placing a high-purity graphite sample prepared in the embodiment in a baking oven at 120 ℃ to be dried to constant weight, then testing volatile matters and ash matters of the dried sample, finally removing the ash matters and volatile matters from the total amount, and calculating to obtain the fixed carbon content in the sample. Fixed carbon content of graphite in w 1 Expressed in% and can be calculated according to the following formula:
w 1 ＝100-w 2 -w 3
wherein w is 2 Volatile mass fraction,%; w (w) 3 Ash mass percent. The measurement result of the fixed carbon content is shown in FIG. 2.
1.3 determination of the chip Rate: the fraction of the expanded graphite having a particle size of less than 0.5mm is defined as the crumb, and the crumb rate can be determined by the following method: 1g of expanded graphite is weighed, and the mass is M 0 Sieving with 0.5mm sieve, weighing the undersize material with the mass of M 1 . Chip rate=m 1 /M 0 X 100%. The result of the measurement of the chipping rate is shown in fig. 3.
1.4 determination of tensile Strength: according to JB/T9141.2-2013 part 2 of flexible graphite sheet: tensile strength test method, the tensile strength of flexible graphite was calculated as σ=p/(bd). Wherein sigma is tensile strength, MPa; p is breaking load, N; b is the width of the sample, mm; d is the sample thickness, mm. The measurement results of the tensile strength are shown in FIG. 4.
As can be seen from fig. 1, the contact angle of the natural crystalline flake graphite treated by the mixed solution a, the mixed solution b and the mixed solution c is obviously smaller than that of the mixed solution d, the mixed solution e, the mixed solution f, the mixed solution g and the mixed solution h, and as can be seen from fig. 2, the fixed carbon content of the high-purity graphite prepared in the embodiment 1, the embodiment 2 and the embodiment 3 is obviously higher than that of the high-purity graphite prepared in the embodiment 4, the embodiment 5, the embodiment 6, the embodiment 7 and the embodiment 8, and as can be seen from fig. 3 and 4, the clastic ratio of the expanded graphite prepared in the embodiment 1, the embodiment 2 and the embodiment 3 is obviously lower and the tensile strength is obviously higher than that of the expanded graphite prepared in the embodiment 4, the embodiment 5, the embodiment 6, the embodiment 7 and the embodiment 8, which indicates that when the triethylene glycol diacrylate and the diethyl fumarate exist simultaneously, the grease on the surface of the graphite is favorably removed, the hydrophilicity of the graphite is improved, the reaction of sodium hydroxide and the graphite impurities is promoted, the purity of the graphite is further improved, and the clastic ratio of the expanded graphite is improved.
Test example 2:
2.1SEM test: scanning electron microscopy analysis was performed on the high temperature resistant flexible graphite prepared in example 1 and example 12. The scanning electron microscope is shown in fig. 5.
2.2 determination of viscosity: the viscosity of the above vermiculite slurry was tested using an NDJ-5S digital rotary viscometer. The results of the viscosity measurements are shown in FIG. 6.
2.3 adhesion test of high temperature resistant flexible graphite material coating: and judging the stability of the bonding of the coating and the matrix, and carrying out an adhesive force test. The paint adhesion was graded according to GB9286-1988, cross-hatch, the grading criteria being as follows:
table 1 coating adhesion test grading criteria
The adhesion test results are shown in Table 2.
Table 2 adhesion test results
2.3 determination of the open cell content: the flexible graphite before and after coating the vermiculite slurry in the above example was measured on a mercury porosimeter, and the reduction rate of the open porosity was calculated. The measurement results of the rate of decrease in the aperture ratio are shown in FIG. 7.
2.4 measurement of high temperature resistant flexible graphite oxidation weight loss ratio:
the experiment is carried out in a muffle furnace, the oxidizing atmosphere is static air, and the test temperature point selected in the experimental process is 700 ℃. The experimental procedure was as follows:
(1) Firstly, cleaning a square boat with distilled water, putting the square boat into an oven to be dried at 100 ℃, then putting the square boat into a muffle furnace to be burned at 700 ℃ for 4 hours, and measuring the dry weight of the square boat on an electronic precision balance after the square boat is cooled;
(2) Respectively placing the high-temperature-resistant flexible graphite into a square boat, and measuring the total weight of the graphite and the square boat;
(3) Raising the temperature of the muffle furnace, after the muffle furnace is stabilized at a certain temperature point, putting the ark and the anti-flexible graphite into the muffle furnace, half-opening the furnace door, taking out the muffle furnace after burning for a certain time, cooling to room temperature, and weighing.
The weight loss ratio w of the flexible graphite is calculated by an oxidation weight loss method, and the calculation formula is as follows:
wherein: m is the dry weight of the ark, unit g;
m 1 the unit g is the dry weight of flexible graphite and a square boat before firing;
m 2 the unit g is the dry weight of the soft graphite and the ark after firing. The measurement results of the oxidation weight loss rate are shown in FIG. 8.
As can be seen from fig. 5, compared with example 13, the vermiculite on the surface of the high temperature resistant flexible graphite prepared in example 1 is uniformly distributed and dense, and has less pores, as can be seen from fig. 6, the viscosity of the vermiculite slurry in example 1, example 9 and example 10 is obviously smaller than that in example 11, example 12 and example 13, as can be seen from table 2, the adhesion force of the vermiculite slurry in example 1, example 9 and example 10 is 1 grade and is larger than that in example 12 and example 13, as can be seen from fig. 7, the reduction rate of the open porosity of the vermiculite slurry in example 1, example 9 and example 10 is obviously larger than that of the open porosity of the vermiculite in example 11, example 12 and example 13, and as can be seen from fig. 8, the oxidation weight loss rate of the vermiculite slurry in example 1, example 9 and example 10 is obviously smaller than that of the embodiment 11, example 12 and example 13, which indicates that the dipropylene glycol butyl ether and polyethylene glycol acrylate are added in the process of the vermiculite slurry preparation, adhesion of the vermiculite to the flexible graphite material can be promoted, and the viscosity of the vermiculite slurry is lower, thereby being favorable for uniformly covering the flexible graphite and improving the high temperature resistance.
The conventional technology in the above embodiments is known to those skilled in the art, and thus is not described in detail herein.
The above embodiments are merely for illustrating the present invention and not for limiting the same, and various changes and modifications may be made by one of ordinary skill in the art without departing from the spirit and scope of the invention. Therefore, all equivalent technical solutions are also within the scope of the present invention, which is defined by the claims.
Claims (9)
1. A method for preparing expanded graphite, comprising:
s1, preparing high-purity graphite: mixing natural crystalline flake graphite with solid NaOH, adding water, diethyl fumarate, absolute ethyl alcohol and triethylene glycol diacrylate, performing ultrasonic dispersion, drying, roasting, washing to be neutral, and filtering; adding hydrochloric acid solution for leaching, washing with water to neutrality, filtering, and oven drying; the volume ratio of the diethyl fumarate to the absolute ethyl alcohol is 1:2.5-4, and the mass ratio of the diethyl fumarate to the triethylene glycol diacrylate is 1:0.3-0.7;
s2, preparing expandable graphite: the method comprises the steps of (1) intercalation is carried out on high-purity graphite by taking potassium permanganate as an oxidant and perchloric acid and ammonium nitrate as intercalators, so that sulfur-free expandable graphite is obtained;
and S3, heating and expanding the sulfur-free expandable graphite to obtain the expanded graphite.
2. The method of manufacturing according to claim 1, characterized in that: the mass ratio of the potassium permanganate to the high-purity graphite is 0.35-0.6:1.
3. The method of manufacturing according to claim 1, characterized in that: the mass ratio of perchloric acid to high-purity graphite is 8-10:1, and the mass ratio of ammonium nitrate to high-purity graphite is 0.04-0.12:1.
4. An expanded graphite, characterized in that: a preparation process according to any one of claims 1 to 3.
5. The preparation method of the high-temperature-resistant flexible graphite is characterized by comprising the following steps of:
A. pressing the expanded graphite of claim 4 to obtain flexible graphite;
B. the high-temperature-resistant flexible graphite is prepared by taking vermiculite slurry as an antioxidant and flexible graphite as a matrix.
6. The method of manufacturing according to claim 5, wherein: the step B comprises the following steps: and (3) spraying the vermiculite slurry on the surface of the flexible graphite, and drying at 102-108 ℃.
7. The method of manufacturing according to claim 5, wherein: the step B comprises the following steps: the flexible graphite is put into vermiculite slurry, impregnated for 1-2 hours under the conditions of vacuum degree of 0.02-0.06MPa, impregnation temperature of 25-30 ℃ and stirring speed of 150-180r/min, and then the flexible graphite is taken out and dried at 102-108 ℃.
8. A high temperature resistant flexible graphite, characterized in that: the method for preparing the high-temperature-resistant flexible graphite according to claim 5.
9. The use of a method for producing high temperature resistant flexible graphite as claimed in claim 5 for producing sealing materials.
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