CN116082046A - Impregnant with high-temperature ablation resistance of graphite sealing ring, preparation method and use method - Google Patents
Impregnant with high-temperature ablation resistance of graphite sealing ring, preparation method and use method Download PDFInfo
- Publication number
- CN116082046A CN116082046A CN202310130891.1A CN202310130891A CN116082046A CN 116082046 A CN116082046 A CN 116082046A CN 202310130891 A CN202310130891 A CN 202310130891A CN 116082046 A CN116082046 A CN 116082046A
- Authority
- CN
- China
- Prior art keywords
- sealing ring
- impregnant
- graphite
- graphite sealing
- temperature
- 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.)
- Granted
Links
- 238000007789 sealing Methods 0.000 title claims abstract description 96
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 239000010439 graphite Substances 0.000 title claims abstract description 90
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 90
- 238000002679 ablation Methods 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 33
- RGPUVZXXZFNFBF-UHFFFAOYSA-K diphosphonooxyalumanyl dihydrogen phosphate Chemical compound [Al+3].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O RGPUVZXXZFNFBF-UHFFFAOYSA-K 0.000 claims abstract description 30
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 27
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 27
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 25
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 25
- 238000002791 soaking Methods 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 4
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- 238000005303 weighing Methods 0.000 description 19
- 238000005245 sintering Methods 0.000 description 12
- 238000001723 curing Methods 0.000 description 11
- 229910052751 metal Inorganic materials 0.000 description 11
- 239000002184 metal Substances 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 10
- 238000002474 experimental method Methods 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 238000011056 performance test Methods 0.000 description 4
- 230000002378 acidificating effect Effects 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 238000005549 size reduction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
- C04B41/515—Other specific metals
- C04B41/5155—Aluminium
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16J—PISTONS; CYLINDERS; SEALINGS
- F16J15/00—Sealings
- F16J15/16—Sealings between relatively-moving surfaces
- F16J15/26—Sealings between relatively-moving surfaces with stuffing-boxes for rigid sealing rings
- F16J15/30—Sealings between relatively-moving surfaces with stuffing-boxes for rigid sealing rings with sealing rings made of carbon
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/40—Metallic constituents or additives not added as binding phase
- C04B2235/402—Aluminium
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/447—Phosphates or phosphites, e.g. orthophosphate, hypophosphite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9669—Resistance against chemicals, e.g. against molten glass or molten salts
Abstract
The invention discloses an impregnant with high-temperature ablation resistance of a graphite sealing ring, a preparation method and a use method, wherein the impregnant comprises an aluminum dihydrogen phosphate solution with the concentration of 30%, magnesium oxide, sodium silicate and aluminum powder; wherein, the ratio of the aluminum dihydrogen phosphate solution to the magnesium oxide to the sodium silicate to the aluminum powder is 100mL: 1-3 g: 5-8 g: 10-30 g. The impregnant is environment-friendly, pollution-free, safe to use and reusable; the graphite sealing ring is subjected to simple soaking and drying curing treatment, so that the anti-ablation performance of the sealing ring can be remarkably improved, the service life of the sealing ring is prolonged by more than twice, and the effect is remarkable.
Description
Technical Field
The invention belongs to the technical field of sealing elements, and particularly relates to an impregnant with high-temperature ablation resistance of a graphite sealing ring, a preparation method and a use method.
Background
Valves are devices used to control the direction, pressure and flow of fluids in pipes and equipment, and when in use, sealing elements made of graphite are usually needed to seal, especially in the fields of electric power, petroleum, coal, chemical industry, water conservancy and hydropower, etc., and graphite sealing rings are more commonly used.
As the first material of the steam valve sealing member of the power station, the graphite sealing ring faces the severe test of high temperature, high pressure, steam, scouring and other environments. Because the graphite sealing ring has the fatal weaknesses of easy oxidation under the high-temperature environment like other carbon materials, and the characteristics of a multi-layer structure, a larger specific surface, porosity and the like, the graphite sealing ring is more easily oxidized and ablated under the high-temperature condition of the power station of more than 600 ℃, the volume shrinkage, the strength reduction and even pulverization of the sealing ring are caused after a large amount of carbon is lost, the sealing effect of the valve is greatly threatened, the valve is required to be disassembled periodically for overhauling and replacing the graphite sealing ring, and the normal and safe operation of the unit is seriously influenced. Therefore, the problem of poor high-temperature ablation resistance of the graphite sealing ring is solved, and the graphite sealing ring has great application value and engineering significance in prolonging the service life of the graphite sealing ring.
Disclosure of Invention
The invention aims to overcome the defect of high-temperature ablation resistance of an active graphite sealing ring, and provides an impregnant with high-temperature ablation resistance of the graphite sealing ring, a preparation method and a use method thereof, which specifically solve the problem of oxidation ablation of the graphite sealing ring at high temperature; the impregnant disclosed by the invention is simple in formula, easy to operate and remarkable in effect of improving the oxidation and ablation resistance of the graphite sealing ring at the high temperature of more than 600 ℃, and the service life of the sealing ring is greatly prolonged.
In order to achieve the above purpose, the invention adopts the following technical scheme:
an impregnant for graphite sealing ring with high-temperature ablation resistance comprises aluminum dihydrogen phosphate solution, magnesium oxide, sodium silicate and aluminum powder;
the ratio of the aluminum dihydrogen phosphate solution, the magnesium oxide, the sodium silicate and the aluminum powder is 100mL: 1-3 g: 5-8 g: 10-30 g; wherein the mass concentration of the aluminum dihydrogen phosphate solution is 30%.
Further, the magnesium oxide is AR grade analytically pure with the mass fraction of 99.9%; sodium silicate is AR analytically pure; the mass fraction of the aluminum powder is 99.9 percent, and the granularity is 3000 meshes.
The preparation method of the impregnant with high-temperature ablation resistance of the graphite sealing ring comprises the steps of heating an aluminum dihydrogen phosphate solution, adding magnesium oxide and sodium silicate, dissolving under heating, adding aluminum powder, and uniformly stirring to obtain the impregnant with high-temperature ablation resistance of the graphite sealing ring.
Further, the heating temperature was 90 ℃.
Further, in every 100mL of the aluminum dihydrogen phosphate solution, the addition amount of magnesium oxide is 1-3 g, the addition amount of sodium silicate is 5-8 g, and the addition amount of aluminum powder is 10-30 g.
The application method of the impregnant with the high-temperature ablation resistance of the graphite sealing ring comprises the following steps:
and immersing the graphite sealing ring to be treated in the heated immersion liquid, and then solidifying.
Further, the heating temperature of the impregnating solution is 70-80 ℃.
Further, the soaking time is 24-48 hours.
Further, the curing temperature is 150-200 ℃ and the curing time is more than 48 hours.
Compared with the prior art, the invention has the following beneficial effects:
the impregnant with high-temperature ablation resistance of the graphite sealing ring for the 650 ℃ ultra-supercritical thermal power generating unit is environment-friendly, pollution-free, safe to use, capable of being repeatedly utilized, free of waste liquid or waste discharge and environment-friendly.
The impregnant with high-temperature ablation resistance for the graphite sealing ring for the 650 ℃ ultra-supercritical thermal power generating unit has the advantages of common raw materials, low cost, quick and convenient preparation process, simple use method, easiness in handling, wide application range and obvious application advantages for graphite sealing materials such as various special-shaped pieces, complex pieces and the like.
The main component of the impregnant for resisting high temperature ablation is aluminumThe powder is characterized in that a layer of compact metal aluminum film is formed on the surface of a graphite sealing ring by soaking and solidifying the graphite sealing ring in an impregnant, and the surface layer of the aluminum film is oxidized at the high temperature of 600 ℃ to form Al with compact structure and continuous structure 2 O 3 The protective oxide film effectively prevents the graphite sealing ring from being ablated and consumed at high temperature, and improves the ablation resistance of the sealing ring. The soaking liquid can obviously improve the ablation resistance of the graphite sealing ring at the high temperature of more than 600 ℃, greatly prolong the service life, reduce the equipment shutdown, maintenance and replacement frequency caused by the failure of the sealing ring, and has great significance in energy conservation and consumption reduction.
Drawings
FIG. 1 is a graph of macroscopic morphology photographs and ablative performance weightlessness data of a graphite seal ring treated under the parameters of example 1 of the present invention after sintering at 650 ℃ for 50 hours; wherein, (a) is a weight loss data curve of the sealing ring in the embodiment 1 and the non-soaking treatment, (b) is a macro-morphology photo of the sealing ring in the non-soaking treatment, and (c) is a macro-morphology photo of the sealing ring in the embodiment 1.
FIG. 2 is a graph of macroscopic morphology and ablation performance weightlessness data obtained after sintering the graphite seal ring treated under the parameters of example 2 of the present invention and the original graphite seal ring at 650℃for 90 hours. Wherein, (a) is a weight loss data curve of the embodiment 2 and the non-soaking treatment, (b) is a macro-morphology photograph of the non-soaking treatment sealing ring, and (c) is a macro-morphology photograph of the sealing ring of the embodiment 2.
Detailed Description
The invention is described in further detail below with reference to the accompanying drawings.
The invention relates to an impregnant with high-temperature ablation resistance for a graphite sealing ring for a 650 ℃ ultra-supercritical thermal power generating unit, which comprises an aluminum dihydrogen phosphate solution, magnesium oxide, sodium silicate and aluminum powder; wherein, the concentration of the aluminum dihydrogen phosphate solution is 30 percent, and the ratio of the aluminum dihydrogen phosphate solution to the magnesium oxide to the sodium silicate to the aluminum powder is 100mL: 1-3 g: 5-8 g: 10-30 g.
Further, the magnesium oxide is AR grade analytically pure with the mass fraction of 99.9%, the sodium silicate is AR grade analytically pure, the aluminum powder is 99.9% with the mass fraction and the granularity of 3000 meshes.
Firstly, weighing a proper amount of aluminum dihydrogen phosphate solution, pouring the solution into a beaker, and placing the beaker into a water bath at 90 ℃ for full heating; then weighing a proper amount of magnesium oxide and sodium silicate respectively according to the proportion, adding the magnesium oxide and the sodium silicate into an aluminum dihydrogen phosphate solution, fully dissolving, and filtering residues; and finally, weighing a proper amount of metal aluminum powder, adding the metal aluminum powder into the filtered solution, uniformly stirring, and cooling to room temperature to obtain the impregnant.
Further, the addition amount of magnesium oxide is 1-3 g, the addition amount of sodium silicate is 5-8 g, and the addition amount of aluminum powder is 10-30 g per 100mL of aluminum dihydrogen phosphate solution.
Further, the solid powder is slowly added in sequence of magnesium oxide, sodium silicate and aluminum powder and is continuously stirred until the solid powder is fully dissolved. Because the liquid-phase aluminum dihydrogen phosphate solution is acidic, magnesium oxide is used as a curing agent, and the magnesium oxide needs to be subjected to chemical reaction with the acidic aluminum dihydrogen phosphate solution at first, so that the curing capability of the magnesium oxide is fully exerted; secondly, aluminum powder is used as a main component for resisting high-temperature ablation, sodium silicate is added to neutralize the acidity of phosphoric acid before adding in order to prevent the aluminum powder from being deteriorated due to reaction with the rest of acidic aluminum dihydrogen phosphate solution, so as to ensure that the aluminum powder is not reacted. Therefore, it must be slowly added in this order.
The application method of the impregnant comprises the following steps:
(1) Cleaning impurities such as oil stains, dust and the like on the surface of the graphite sealing ring to be treated by acetone or alcohol, and keeping the graphite sealing ring for standby;
(2) Pouring the prepared impregnant into a beaker, and placing the beaker in a water bath with the temperature of 70-80 ℃ for full preheating;
(3) Suspending and soaking the cleaned graphite sealing ring in an impregnant to ensure that the impregnant completely submerges the graphite sealing ring;
(4) And (3) placing the soaked graphite sealing ring in an oven at 150-200 ℃ for drying and curing.
Further, the soaking time of the graphite sealing ring is 24-48 hours, and the drying and curing time is more than 48 hours.
The following are specific examples.
The invention is illustrated by taking an original state high temperature valve graphite sealing ring as an example.
Example 1
Step one: preparation of impregnant
Firstly, 100mL of aluminum dihydrogen phosphate solution with the concentration of 30% is measured and poured into a beaker, and the beaker is placed in a water bath with the temperature of 90 ℃ for full heating; then respectively weighing 1g of magnesium oxide and 5g of sodium silicate, sequentially and slowly adding into the aluminum dihydrogen phosphate solution, continuously stirring, fully dissolving, and filtering residues; finally, weighing 10g of metal aluminum powder, adding the metal aluminum powder into the filtered solution, uniformly stirring, and cooling to room temperature to obtain the impregnant.
Step two: method for using impregnant
Firstly, pouring the prepared impregnant into a beaker, and placing the beaker in a water bath at 70 ℃ for full preheating; then suspending and soaking the graphite sealing ring which is cleaned by acetone or alcohol in the impregnant for 24 hours to ensure that the impregnant completely submerges the graphite sealing ring; and finally, placing the soaked graphite sealing ring in a baking oven at 150 ℃ for drying and curing for 48 hours, and taking out to finish the soaking of the graphite sealing ring.
Step three: 650 ℃ high temperature ablation performance test
Accurately weighing the soaked, dried and solidified graphite sealing ring, and recording data; then placing the graphite in a high-temperature furnace at 650 ℃ for sintering, simultaneously placing an original graphite sealing ring as a comparison sample, taking out, observing and weighing at intervals, and continuing the experiment for 50 hours; and after the experiment is finished, calculating mass difference values under different sintering times, drawing a time-weightlessness curve, analyzing experimental data, and evaluating ablation performance.
According to analysis, the graphite sealing ring of the embodiment 1 has the ablation rate of 0.0270g/h, which is 49.00% of the original sealing ring, and the service life is 2.04 times of the original sealing ring.
Example 2
Step one: preparation of impregnant
Firstly, 100mL of aluminum dihydrogen phosphate solution with the concentration of 30% is measured and poured into a beaker, and the beaker is placed in a water bath with the temperature of 90 ℃ for full heating; then respectively weighing 2g of magnesium oxide and 8g of sodium silicate, sequentially and slowly adding into the aluminum dihydrogen phosphate solution, continuously stirring, fully dissolving, and filtering residues; finally, weighing 10g of metal aluminum powder, adding the metal aluminum powder into the filtered solution, uniformly stirring, and cooling to room temperature to obtain the impregnant.
Step two: method for using impregnant
Firstly, pouring the prepared impregnant into a beaker, and placing the beaker in a water bath at 75 ℃ for full preheating; then suspending and soaking the graphite sealing ring which is cleaned by acetone or alcohol in the impregnant for 36 hours to ensure that the impregnant completely submerges the graphite sealing ring; and finally, placing the soaked graphite sealing ring in a baking oven at 150 ℃ for drying and curing for 48 hours, and taking out to finish the soaking of the graphite sealing ring.
Step three: 650 ℃ high temperature ablation performance test
Accurately weighing the soaked, dried and solidified graphite sealing ring, and recording data; then placing the graphite in a high-temperature furnace at 650 ℃ for sintering, simultaneously placing an original graphite sealing ring as a comparison sample, taking out, observing and weighing at intervals, and continuing the experiment for 90 hours; and after the experiment is finished, calculating mass difference values under different sintering times, drawing a time-weightlessness curve, analyzing experimental data, and evaluating ablation performance.
According to analysis, the graphite sealing ring of the embodiment 2 has an ablation rate of 0.0264g/h, which is 47.91% of the original sealing ring, and the service life is 2.09 times of that of the original sealing ring.
Example 3
Step one: preparation of impregnant
Firstly, 100mL of aluminum dihydrogen phosphate solution with the concentration of 30% is measured and poured into a beaker, and the beaker is placed in a water bath with the temperature of 90 ℃ for full heating; then respectively weighing 2g of magnesium oxide and 6g of sodium silicate, sequentially and slowly adding into the aluminum dihydrogen phosphate solution, continuously stirring, fully dissolving, and filtering residues; and finally, weighing 20g of metal aluminum powder, adding the metal aluminum powder into the filtered solution, uniformly stirring, and cooling to room temperature to obtain the impregnant.
Step two: method for using impregnant
Firstly, pouring the prepared impregnant into a beaker, and placing the beaker in a water bath at 75 ℃ for full preheating; then suspending and soaking the graphite sealing ring which is cleaned by acetone or alcohol in the impregnant for 36 hours to ensure that the impregnant completely submerges the graphite sealing ring; and finally, placing the soaked graphite sealing ring in a baking oven at 175 ℃ for drying and curing for 48 hours, and taking out to finish the soaking of the graphite sealing ring.
Step three: 650 ℃ high temperature ablation performance test
Accurately weighing the soaked, dried and solidified graphite sealing ring, and recording data; then placing the graphite in a high-temperature furnace at 650 ℃ for sintering, simultaneously placing an original graphite sealing ring as a comparison sample, taking out, observing and weighing at intervals, and continuing the experiment for 90 hours; and after the experiment is finished, calculating mass difference values under different sintering times, drawing a time-weightlessness curve, analyzing experimental data, and evaluating ablation performance.
According to analysis, the graphite sealing ring of the embodiment 3 has the ablation rate of 0.0262g/h, which is 47.55% of the original sealing ring, and the service life is 2.10 times of the original sealing ring.
Example 4
Step one: preparation of impregnant
Firstly, 100mL of aluminum dihydrogen phosphate solution with the concentration of 30% is measured and poured into a beaker, and the beaker is placed in a water bath with the temperature of 90 ℃ for full heating; then respectively weighing 3g of magnesium oxide and 8g of sodium silicate, sequentially and slowly adding into the aluminum dihydrogen phosphate solution, continuously stirring, fully dissolving, and filtering residues; and finally weighing 30g of metal aluminum powder, adding the metal aluminum powder into the filtered solution, uniformly stirring, and cooling to room temperature to obtain the impregnant.
Step two: method for using impregnant
Firstly, pouring the prepared impregnant into a beaker, and placing the beaker in a water bath at 80 ℃ for full preheating; then suspending and soaking the graphite sealing ring which is cleaned by acetone or alcohol in the impregnant for 48 hours to ensure that the impregnant completely submerges the graphite sealing ring; and finally, placing the soaked graphite sealing ring in a baking oven at 200 ℃ for drying and curing for 48 hours, and taking out to finish the soaking of the graphite sealing ring.
Step three: 650 ℃ high temperature ablation performance test
Accurately weighing the soaked, dried and solidified graphite sealing ring, and recording data; then placing the graphite in a high-temperature furnace at 650 ℃ for sintering, simultaneously placing an original graphite sealing ring as a comparison sample, taking out, observing and weighing at intervals, and continuing the experiment for 90 hours; and after the experiment is finished, calculating mass difference values under different sintering times, drawing a time-weightlessness curve, analyzing experimental data, and evaluating ablation performance.
According to analysis, the graphite sealing ring of the embodiment 4 has an ablation rate of 0.0265g/h, which is 48.09% of the original sealing ring, and the service life is 2.08 times of the original sealing ring.
Referring to fig. 1 (a), (b) and (c), it can be seen that the impregnant treated graphite seal ring sample of example 1 had significantly less loss of ablation after 50h sintering at 650 c (fig. 1 (a)), less sample size reduction (fig. 1 (b) and (c)), and the sample surface still retained a large area of white Al as compared to the original graphite seal ring sample 2 O 3 The protective film (fig. 1 (c)) shows that the graphite seal ring sample treated by the impregnant has better high-temperature ablation resistance.
Referring to fig. 2 (a), (b) and (c), it can be seen that the impregnant treated graphite seal ring sample at the parameters of example 2 had a similarly smaller ablative weight after sintering at 650 ℃ for 90 hours than the original graphite seal ring sample. In FIG. 2 (a)), although the sample surface is subject to ablation cracking, the original graphite seal ring sample has more than half of its ablation loss (FIGS. 2 (b) and (c)), and the sample surface is white Al 2 O 3 The protective film was still fully depleted (fig. 2 (c)), indicating that the impregnant treated graphite seal ring samples also had better resistance to high temperature ablation.
In the invention, the amount of magnesium oxide, sodium silicate and aluminum powder is proportionally increased or decreased by taking each 100mL of aluminum dihydrogen phosphate solution as a unit; the impregnant provided by the invention can obviously improve the anti-ablation performance of the sealing ring by simply soaking and drying and curing the graphite sealing ring, prolongs the service life of the sealing ring by more than two times, and has obvious effect.
The above description and examples are only representative examples of the invention and any modifications, equivalents, improvements, etc. made within the scope of the claims of the present invention for any kind and shape of graphite sealing ring/gasket high temperature ablation problem are included in the scope of the present invention.
Claims (9)
1. The impregnant for graphite sealing ring with high temperature ablation resistance is characterized by comprising aluminum dihydrogen phosphate solution, magnesium oxide, sodium silicate and aluminum powder;
the ratio of the aluminum dihydrogen phosphate solution, the magnesium oxide, the sodium silicate and the aluminum powder is 100mL: 1-3 g: 5-8 g: 10-30 g; wherein the mass concentration of the aluminum dihydrogen phosphate solution is 30%.
2. The impregnant with high-temperature ablation resistance for a graphite seal ring according to claim 1, wherein the magnesium oxide is of an AR grade analytical purity of 99.9% by mass; sodium silicate is AR analytically pure; the mass fraction of the aluminum powder is 99.9 percent, and the granularity is 3000 meshes.
3. A preparation method of an impregnant with high-temperature ablation resistance of a graphite sealing ring is characterized in that magnesium oxide and sodium silicate are added after aluminum dihydrogen phosphate solution is heated, aluminum powder is added after dissolution under heating, and the impregnant with high-temperature ablation resistance of the graphite sealing ring is obtained after uniform stirring.
4. A method for preparing an impregnant with high-temperature ablation resistance for a graphite seal ring according to claim 3, wherein the heating temperature is 90 ℃.
5. The method for preparing the impregnant with high-temperature ablation resistance of the graphite sealing ring according to claim 3, wherein the addition amount of magnesium oxide is 1-3 g, the addition amount of sodium silicate is 5-8 g and the addition amount of aluminum powder is 10-30 g in every 100mL of aluminum dihydrogen phosphate solution.
6. A method of using the impregnant of the graphite seal ring with high temperature ablation resistance according to claim 1, comprising the steps of:
and immersing the graphite sealing ring to be treated in the heated immersion liquid, and then solidifying.
7. A method according to claim 6, wherein the impregnating solution is heated to a temperature of from 70℃to 80 ℃.
8. A method according to claim 6, wherein the soaking time is 24 to 48 hours.
9. A method according to claim 6, wherein the curing temperature is 150-200 ℃ and the curing time is 48 hours or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310130891.1A CN116082046B (en) | 2023-02-17 | 2023-02-17 | Impregnant with high-temperature ablation resistance of graphite sealing ring, preparation method and use method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310130891.1A CN116082046B (en) | 2023-02-17 | 2023-02-17 | Impregnant with high-temperature ablation resistance of graphite sealing ring, preparation method and use method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116082046A true CN116082046A (en) | 2023-05-09 |
| CN116082046B CN116082046B (en) | 2024-03-26 |
Family
ID=86210175
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310130891.1A Active CN116082046B (en) | 2023-02-17 | 2023-02-17 | Impregnant with high-temperature ablation resistance of graphite sealing ring, preparation method and use method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116082046B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3510347A (en) * | 1964-09-02 | 1970-05-05 | Carborundum Co | Oxidation resistant carbon |
| JP2004101009A (en) * | 2002-09-06 | 2004-04-02 | Godo Steel Ltd | Conductive oxidation prevention material of graphite electrode for arc type electric steel manufacture furnace and its painting method |
| CN104163657A (en) * | 2014-07-21 | 2014-11-26 | 中国矿业大学(北京) | Graphite mould antioxidant impregnation liquid, preparation method and application method thereof |
| CN113802088A (en) * | 2021-10-09 | 2021-12-17 | 西安热工研究院有限公司 | Preparation method of high-toughness high-temperature steam oxidation-resistant coating |
| CN115636689A (en) * | 2022-09-09 | 2023-01-24 | 华能国际电力股份有限公司 | Oxidation resistance dipping treatment method and oxidation resistance production line of graphite sealing member for thermal power generating unit |
-
2023
- 2023-02-17 CN CN202310130891.1A patent/CN116082046B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3510347A (en) * | 1964-09-02 | 1970-05-05 | Carborundum Co | Oxidation resistant carbon |
| JP2004101009A (en) * | 2002-09-06 | 2004-04-02 | Godo Steel Ltd | Conductive oxidation prevention material of graphite electrode for arc type electric steel manufacture furnace and its painting method |
| CN104163657A (en) * | 2014-07-21 | 2014-11-26 | 中国矿业大学(北京) | Graphite mould antioxidant impregnation liquid, preparation method and application method thereof |
| CN113802088A (en) * | 2021-10-09 | 2021-12-17 | 西安热工研究院有限公司 | Preparation method of high-toughness high-temperature steam oxidation-resistant coating |
| CN115636689A (en) * | 2022-09-09 | 2023-01-24 | 华能国际电力股份有限公司 | Oxidation resistance dipping treatment method and oxidation resistance production line of graphite sealing member for thermal power generating unit |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116082046B (en) | 2024-03-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104163657A (en) | Graphite mould antioxidant impregnation liquid, preparation method and application method thereof | |
| CN103173836B (en) | Magnesium alloy differential arc oxidation low energy consumption black ceramic membrane and preparation method | |
| CN102304741A (en) | Anodic oxidation method for preparing aluminum-based super-hydrophobic film | |
| CN116082046B (en) | Impregnant with high-temperature ablation resistance of graphite sealing ring, preparation method and use method | |
| CN114806231B (en) | Prebaked anode anti-oxidation coating capable of reducing energy consumption of aluminum electrolysis cell and preparation and application methods thereof | |
| CN103147112B (en) | A kind of electrolytic solution and for the preparation of the purposes of nuclear fuel rod zirconium alloy cladding micro-arc oxidation films and method | |
| CN102517542A (en) | Boriding agent for boriding on metallic titanium surface and boriding technique | |
| CN113307264A (en) | Preparation method of high-temperature-resistant graphite material | |
| CN102560531B (en) | Anti-oxidation treatment method for graphite anode for chlor-alkali industry | |
| CN109972078A (en) | A kind of 45 steel boriding process | |
| CN105837259A (en) | Method for corroding silicon carbide ceramics | |
| CN204841649U (en) | A retort for preparing fluoride fused salt | |
| JPS6058161B2 (en) | Flexible layered graphite material and its manufacturing method | |
| CN207581898U (en) | A kind of water high-temperature steam steel-iron components turn blue device | |
| CA2926597C (en) | Method for the in situ passivation of the steel surfaces of a nuclear reactor | |
| CN111468705B (en) | Composite treatment process for manufacturing corrosion-resistant protective layer on surface of cast aluminum alloy | |
| CN110252627B (en) | Preparation method of aluminum liquid corrosion resistant steel surface oxide coating | |
| CN103451595B (en) | Mg alloy surface fused salt oxygen carbon sulphur oozes Preparing Anti-corrosion Ceramic Coating and Synthesis and applications altogether | |
| CN113025445A (en) | Cleaning agent for cleaning high-temperature sintered metal filter | |
| CN113005396A (en) | Powder embedding aluminizing process for Q345 steel surface in air environment | |
| CN112281166A (en) | High-temperature environment-friendly alkali sand aluminum profile surface treatment process | |
| CN106636719B (en) | A kind of preparation method of Aluminum Matrix Composites Strengthened by SiC | |
| CN111039662A (en) | Electrolytic aluminum prebaked carbon anode ceramic-based high-temperature antioxidant coating and preparation method thereof | |
| CN110577299B (en) | Method for treating hot galvanizing pickling wastewater and preparing carbon-loaded iron-zinc binary metal composite material | |
| CN103435373A (en) | Carbon/carbon composite material connection layer and preparation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |