CN114057499A - Sliding plate brick and preparation method thereof - Google Patents
Sliding plate brick and preparation method thereof Download PDFInfo
- Publication number
- CN114057499A CN114057499A CN202111556880.7A CN202111556880A CN114057499A CN 114057499 A CN114057499 A CN 114057499A CN 202111556880 A CN202111556880 A CN 202111556880A CN 114057499 A CN114057499 A CN 114057499A
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- China
- Prior art keywords
- plate brick
- sliding plate
- graphite
- modified
- epoxy resin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000011449 brick Substances 0.000 title claims abstract description 145
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 97
- 239000003822 epoxy resin Substances 0.000 claims abstract description 45
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 45
- 230000003628 erosive effect Effects 0.000 claims abstract description 35
- 239000000463 material Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 26
- 238000003763 carbonization Methods 0.000 claims abstract description 21
- 239000010431 corundum Substances 0.000 claims abstract description 19
- 239000003921 oil Substances 0.000 claims abstract description 19
- -1 aluminum-zirconium-carbon Chemical compound 0.000 claims abstract description 17
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 17
- 238000007654 immersion Methods 0.000 claims abstract description 16
- 239000002243 precursor Substances 0.000 claims abstract description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011230 binding agent Substances 0.000 claims abstract description 8
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 8
- 239000012783 reinforcing fiber Substances 0.000 claims abstract description 7
- 238000003754 machining Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- VGEREEWJJVICBM-UHFFFAOYSA-N phloretin Chemical compound C1=CC(O)=CC=C1CCC(=O)C1=C(O)C=C(O)C=C1O VGEREEWJJVICBM-UHFFFAOYSA-N 0.000 claims description 60
- 239000010439 graphite Substances 0.000 claims description 34
- 229910002804 graphite Inorganic materials 0.000 claims description 34
- ZWTDXYUDJYDHJR-UHFFFAOYSA-N (E)-1-(2,4-dihydroxyphenyl)-3-(2,4-dihydroxyphenyl)-2-propen-1-one Natural products OC1=CC(O)=CC=C1C=CC(=O)C1=CC=C(O)C=C1O ZWTDXYUDJYDHJR-UHFFFAOYSA-N 0.000 claims description 30
- YQHMWTPYORBCMF-UHFFFAOYSA-N Naringenin chalcone Natural products C1=CC(O)=CC=C1C=CC(=O)C1=C(O)C=C(O)C=C1O YQHMWTPYORBCMF-UHFFFAOYSA-N 0.000 claims description 30
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- 229910000831 Steel Inorganic materials 0.000 claims description 16
- 239000010959 steel Substances 0.000 claims description 16
- 239000004593 Epoxy Substances 0.000 claims description 13
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 13
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 12
- 229910052710 silicon Inorganic materials 0.000 claims description 11
- 239000010703 silicon Substances 0.000 claims description 11
- 239000010426 asphalt Substances 0.000 claims description 10
- CPSIMDUNVYMPAH-UHFFFAOYSA-N 1,3-bis(4-methoxyphenyl)urea Chemical compound C1=CC(OC)=CC=C1NC(=O)NC1=CC=C(OC)C=C1 CPSIMDUNVYMPAH-UHFFFAOYSA-N 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 6
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- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 5
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 5
- 239000004327 boric acid Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- HQWKKEIVHQXCPI-UHFFFAOYSA-L disodium;phthalate Chemical compound [Na+].[Na+].[O-]C(=O)C1=CC=CC=C1C([O-])=O HQWKKEIVHQXCPI-UHFFFAOYSA-L 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 235000002906 tartaric acid Nutrition 0.000 claims description 5
- 239000011975 tartaric acid Substances 0.000 claims description 5
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- 238000005498 polishing Methods 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 230000004913 activation Effects 0.000 claims description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims 1
- 229910052845 zircon Inorganic materials 0.000 claims 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims 1
- 230000035939 shock Effects 0.000 abstract description 23
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- 238000009991 scouring Methods 0.000 abstract description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 abstract description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 abstract description 2
- 238000009740 moulding (composite fabrication) Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 description 11
- 230000008569 process Effects 0.000 description 11
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 9
- 238000005299 abrasion Methods 0.000 description 8
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 8
- 230000014759 maintenance of location Effects 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
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- 229910052726 zirconium Inorganic materials 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
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- 229910052749 magnesium Inorganic materials 0.000 description 2
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- QOHMWDJIBGVPIF-UHFFFAOYSA-N n',n'-diethylpropane-1,3-diamine Chemical compound CCN(CC)CCCN QOHMWDJIBGVPIF-UHFFFAOYSA-N 0.000 description 2
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- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 2
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- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 description 1
- OQZDJLFNMXRJHZ-UHFFFAOYSA-N 1-benzyl-2-ethylimidazole Chemical compound CCC1=NC=CN1CC1=CC=CC=C1 OQZDJLFNMXRJHZ-UHFFFAOYSA-N 0.000 description 1
- QKVROWZQJVDFSO-UHFFFAOYSA-N 2-(2-methylimidazol-1-yl)ethanamine Chemical compound CC1=NC=CN1CCN QKVROWZQJVDFSO-UHFFFAOYSA-N 0.000 description 1
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- FDLQZKYLHJJBHD-UHFFFAOYSA-N [3-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=CC(CN)=C1 FDLQZKYLHJJBHD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
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- 230000002776 aggregation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
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- 238000005336 cracking Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
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- UJTGYJODGVUOGO-UHFFFAOYSA-N diethoxy-methyl-propylsilane Chemical compound CCC[Si](C)(OCC)OCC UJTGYJODGVUOGO-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000002635 electroconvulsive therapy Methods 0.000 description 1
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- 125000003700 epoxy group Chemical group 0.000 description 1
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- 229940018564 m-phenylenediamine Drugs 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- DRRZZMBHJXLZRS-UHFFFAOYSA-N n-[3-[dimethoxy(methyl)silyl]propyl]cyclohexanamine Chemical compound CO[Si](C)(OC)CCCNC1CCCCC1 DRRZZMBHJXLZRS-UHFFFAOYSA-N 0.000 description 1
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- 238000009210 therapy by ultrasound Methods 0.000 description 1
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
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- 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
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- 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
- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
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- 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
- C04B2235/9676—Resistance against chemicals, e.g. against molten glass or molten salts against molten metals such as steel or aluminium
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- 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
- C04B2235/9684—Oxidation resistance
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Abstract
The invention provides a sliding plate brick and a preparation method thereof, belonging to the technical field of refractory materials and specifically comprising the following steps: the method comprises the steps of mixing a base material consisting of tabular corundum, zirconium oxide, silicon carbide, aluminum powder and modified graphite, reinforcing fibers and a modified epoxy resin binder, carrying out die forming, heat treatment and sintering on the mixed material to obtain a slide plate brick precursor, sequentially carrying out oil immersion carbonization and finish machining on the slide plate brick precursor to obtain the slide plate brick, and controlling the content and preparation process conditions of each component to obtain the slide plate brick with high compactness, excellent scouring resistance, erosion resistance, thermal shock stability and wear resistance, thereby overcoming the defects of the existing aluminum-zirconium-carbon slide plate brick.
Description
Technical Field
The invention belongs to the technical field of refractory materials, and particularly relates to a sliding plate brick and a preparation method thereof.
Background
The slide plate brick is an important refractory material in the steelmaking process, and is mainly applied to converter slag stopping, molten steel tank and tundish flow control and the like. With the rapid development of steel refining technology, the function of the slide plate brick is more and more important. In the using process of the sliding plate brick, the sliding plate brick needs to repeatedly bear the chemical erosion and physical scouring of high-temperature molten steel for a long time and bear high thermal shock and mechanical abrasion, so that the sliding plate brick needs to have higher wear resistance, high-temperature strength, erosion resistance, thermal shock resistance, oxidation resistance and the like.
The sliding plate brick mainly comprises aluminum carbon, aluminum zirconium carbon and magnesium sliding plates, wherein corundum and zirconium-containing raw materials are generally selected as main components, and phenolic resin or epoxy resin is taken as a bonding agent. The common aluminum-carbon sliding plate can not meet the process requirements; the magnesium sliding plate has good erosion resistance to high-corrosion steel, but has large thermal expansion coefficient, low strength and poor erosion resistance; the production process of the aluminum zirconium carbon sliding plate brick is complex, high-temperature sintering at about 1400 ℃ is required, the energy consumption is high, and the molten steel erosion resistance of the aluminum zirconium carbon is general.
Patent CN106630976A discloses a gate valve slide plate brick for converter slag blocking and a preparation method thereof, wherein tabular corundum, zirconium corundum and expanded graphite are introduced into a re-sintered aluminum-zirconium-carbon slide plate, so that the service life, the oxidation resistance, the thermal shock stability and the erosion resistance are improved. Patent CN107382347A discloses a sliding plate brick for converter slag blocking prepared by medium temperature heat treatment, compared with the traditional high temperature firing, the medium temperature heat treatment not only reduces the production cost, but also is beneficial to obtaining the medium temperature sliding plate brick for converter slag blocking with erosion resistance, scouring resistance, oxidation resistance and thermal shock resistance. However, the sliding plate brick produced by the method still has certain defects, such as high temperature resistance, wear resistance and the like, which are still to be improved.
Therefore, a sliding plate brick with excellent comprehensive performance is urgently needed to be developed to meet the production requirements of the modern steelmaking industry.
Disclosure of Invention
Technical purpose
The invention aims to make up the defects of the existing sliding plate brick and provides the sliding plate brick prepared from the modified graphite.
(II) technical scheme
The technical scheme adopted by the invention is as follows:
a preparation method of modified graphite comprises the following steps:
1) in an ethanol water solution, boric acid and tartaric acid are used for carrying out surface activation on the expanded graphite to obtain activated graphite;
2) modifying the activated graphite by using an epoxy silane coupling agent to obtain organic silicon modified graphite;
3) treating the organic silicon modified graphite with phloretin under alkaline conditions, and crushing to obtain the product.
Preferably, the mass ratio of the graphite to the boric acid and the tartaric acid in the step 1) is 1: 0.1-0.2: 0.01-0.08.
As a preferable embodiment, the epoxy silane coupling agent in the step 2) is any one of 3-glycidoxypropyltrimethoxysilane, 3-glycidoxypropyltriethoxysilane, 3- (2, 3-glycidoxy) propylmethyldimethoxysilane and 3- (2, 3-glycidoxy) propylmethyldiethoxysilane.
As a preferable technical scheme, the mass ratio of the activated graphite to the epoxy silane coupling agent in the step 2) is 1: 1-3.
As a preferable technical scheme, the mass ratio of the organic silicon modified graphite to the phloretin in the step 3) is 1: 2-5.
As a preferable technical scheme, the alkali used in the alkaline condition in the step 3) is sodium hydroxide or potassium hydroxide.
As a preferable technical scheme, the modified graphite in the step 3) is crushed to 200-500 meshes.
According to the method, firstly, the surface of the expanded graphite is activated, then, the surface of the expanded graphite is modified by using the epoxy silane coupling agent, silanol groups and other groups in the epoxy silane coupling agent react with active groups such as carboxyl groups and other groups on the surface of the graphite, the epoxy silane coupling agent is successfully grafted to the surface of the graphite, the defect that the graphite is easy to agglomerate is overcome, the compatibility with a base material is increased, then, phloretin is used for further modifying the graphite, the dispersibility is further improved, the dispersion uniformity of the graphite in the base material is ensured, the interface bonding property among all components in the sliding plate brick is good, and the problem of stress concentration caused by aggregation can be reduced, so that the uniformity of the sliding plate brick material is favorably improved, and the sliding plate brick has a good reinforcing effect; the graphite layers of the modified expanded graphite have fewer nano-pore structures, so that nano-pores can be generated in the sintering process, and the thermal stress can be absorbed in the thermal shock cycle process on the premise of ensuring higher strength, so that the thermal shock resistance of the material is improved, and the oxidation resistance and the erosion resistance of the material are improved; in addition, the expanded graphite is modified by the phloretin, so that the wear resistance and molten steel erosion resistance of the material can be improved, and probably because the expanded graphite is modified by a certain amount of phloretin, on one hand, the uniformity of the material can be increased, the compactness of the slide plate brick can be improved, on the other hand, the introduction of impurities in the subsequent heat treatment and oil immersion carbonization processes can be reduced, and the molten steel erosion resistance of the material can be improved.
The modified graphite is applied to the preparation of the sliding plate brick.
The applications include improving the molten steel erosion resistance of the slide plate brick;
the applications also include improving the wear resistance of the slide plate tile.
The invention also discloses a slide plate brick, which comprises:
a base material consisting of tabular corundum, zirconia, silicon carbide, aluminum powder and modified graphite;
a reinforcing fiber; and
modified epoxy resin binder.
The sliding plate brick with the components is provided, the modified graphite is added into the sliding plate brick, the compatibility with other components is good, the thermal shock resistance of the sliding plate brick can be obviously improved, the oxidation resistance and the corrosion resistance of the material are improved, and the wear resistance is improved; using modified epoxy resin as bonding agentThe agent can increase the cohesiveness among all components in the sliding plate brick, reduce cracking and stripping and further increase the corrosion resistance of the sliding plate brick; the plate corundum and the zirconium corundum are used as main components of the sliding plate brick to play a role in supporting, and the sliding plate brick has a larger compactness by matching with other components, the apparent porosity is as low as 1.1 percent, and the volume density is 3.88g/cm3The aluminum-zirconium-carbon sliding plate brick has excellent scouring resistance, erosion resistance, thermal shock stability and wear resistance, long service life and capability of making up the defects of the traditional aluminum-zirconium-carbon sliding plate brick.
As a preferred technical scheme, the reinforcing fiber is glass fiber or carbon fiber;
as a preferred technical scheme, the slide plate brick comprises the following components in percentage by weight:
40-65 wt% of tabular corundum, 20-30 wt% of zirconium corundum, 3-5 wt% of zirconia, 5-10 wt% of silicon carbide, 2-5 wt% of aluminum powder, 3-8 wt% of modified graphite, 1-3 wt% of reinforcing fiber and 2-4 wt% of modified epoxy resin binder.
Preferably, the modified epoxy resin is 1, 3-bis (4-methoxyphenyl) urea modified epoxy resin.
As a preferred technical scheme, the modified epoxy resin is prepared by the following method:
adding epoxy resin and 1, 3-bis (4-methoxyphenyl) urea into acetone, carrying out pre-reaction for 10-30 min at 90-100 ℃, adding sodium phthalate, continuing to react for 20-50 min, then adding a curing agent and an accelerant, stirring, carrying out vacuum defoaming, and cooling to obtain the modified epoxy resin.
According to a further preferable technical scheme, the epoxy resin is bisphenol F type epoxy resin or bisphenol A type epoxy resin, and the molecular weight is 5000-10000.
A more preferable embodiment is one in which the mass ratio of the epoxy resin to the 1, 3-bis (4-methoxyphenyl) urea is 1:0.2 to 0.4.
In a more preferable embodiment, the amount of sodium phthalate added is 0.1 to 0.3 times the mass of the epoxy resin.
In a more preferable embodiment, the curing agent is any one of hexamethylenediamine, diethylaminopropylamine, m-phenylenediamine and m-xylylenediamine, and the amount of the curing agent added is 0.05 to 0.3 times the mass of the epoxy resin.
In a more preferable embodiment, the accelerator is any one of 2-ethyl-4-methyl-imidazole, 1-benzyl-2-ethyl-imidazole, and 1-aminoethyl-2-methyl-imidazole, and the amount of the accelerator added is 0.1 to 0.2 times the mass of the epoxy resin.
Epoxy groups in the epoxy resin react with carbamido groups in 1, 3-bis (4-methoxyphenyl) urea to modify the epoxy resin, so that the high temperature resistance of the epoxy resin is improved, the modified epoxy resin is used as a bonding agent of the slide brick, and compared with unmodified epoxy resin, the modified epoxy resin has improved high temperature resistance, so that the modified epoxy resin has higher bonding strength at high temperature, the bonding fastness among components can be increased in the high-temperature sintering process, the shedding phenomenon is reduced, the compactness of the slide brick is increased, and the molten steel erosion resistance of the slide brick is increased.
The invention also discloses a preparation method of the sliding plate brick, which comprises the following steps:
s1: mixing the materials;
s2: molding, heat treating and sintering the mixed material by a mold to obtain a sliding plate brick precursor;
s3: and sequentially carrying out oil immersion carbonization and finish machining on the sliding plate brick precursor to obtain the sliding plate brick.
As a preferred technical scheme, the heat treatment temperature is 150-200 ℃, and the heat treatment time is 20-40 h.
As an optimal technical scheme, the sintering temperature is 960-1000 ℃, and the sintering time is 10-16 h.
As a preferred technical scheme, the oil immersion carbonization is the treatment of immersion in asphalt oil, and the specific steps are as follows: immersing a sliding plate brick precursor into asphalt, increasing the temperature from room temperature to 175-190 ℃ at the speed of 3-8 ℃/min, carrying out oil immersion and pressure maintaining for 2-5 h under the pressure of 1.2-1.5 MPa, then increasing the temperature to 220-240 ℃ at the speed of 2-4 ℃/min, carrying out oil immersion and pressure maintaining for 1-3 h under the pressure of 1-1.3 MPa, carrying out sealed carbonization on the oil immersed sliding plate brick in a carbonization kiln at the carbonization temperature of 400-500 ℃ for 8-12 h, and polishing to remove residual asphalt on the surface of the sliding plate brick to obtain a semi-finished sliding plate brick.
As a preferred technical scheme, the finishing treatment comprises the steps of hooping, casing, drying, grinding, shell turning, drying and the like.
According to the invention, by utilizing the steps, the materials of the sliding plate brick are mixed, the components are uniformly dispersed, then the sliding plate brick precursor is prepared by molding, drying and sintering through a mold, and then the sliding plate brick is obtained by oil immersion carbonization and finish machining treatment.
(III) the beneficial effects are as follows:
the invention provides a sliding plate brick, which takes plate-shaped corundum and zirconium corundum as main components, and the prepared sliding plate brick has good physical and chemical properties and the volume density of the sliding plate brick is up to 3.88g/cm by adjusting the formula and the preparation process of the sliding plate brick3The apparent porosity reaches 1.1 percent at least, and the material has good high temperature resistance, excellent scour resistance, erosion resistance, thermal shock stability and wear resistance and long service life; in the process of preparing the sliding plate brick, the modified epoxy resin is used as a bonding agent, so that the compactness of the sliding plate brick can be obviously improved, and the molten steel erosion resistance of the sliding plate brick is improved; the modified graphite is added into the sliding plate brick and is matched with other components, so that the sintering performance of the sliding plate brick is obviously improved, the sliding plate brick is convenient to form, the structure is more compact under the same pressure, the thermal shock resistance, the oxidation resistance and the corrosion resistance of the material are improved, and the wear resistance is improved.
Drawings
FIG. 1 is an infrared spectrum of modified graphite; in the figure, a represents expanded graphite, b represents organosilicon modified graphite, and c represents modified graphite;
FIG. 2 is a graph showing the results of bulk density and apparent porosity tests on a sliding brick; in the figure, B represents the bulk density, and C represents the apparent porosity;
FIG. 3 is a graph showing the results of the thermal shock resistance (retention of rupture strength) test of the slide brick;
FIG. 4 is a graphical representation of the results of an erosion resistance (depth of erosion) test for a slide plate brick;
fig. 5 is a graph showing the results of the wear resistance (wear amount) test of the slide brick.
Detailed Description
The following examples are presented to further illustrate the essence of the present invention, and it should be noted that these examples are only intended to specifically describe the present invention and should not be construed as limiting the present invention.
The invention provides a sliding plate brick, which comprises the following components: 40-65 wt% of tabular corundum, 20-30 wt% of zirconium corundum, 3-5 wt% of zirconia, 5-10 wt% of silicon carbide, 2-5 wt% of aluminum powder, 3-8 wt% of modified graphite, 1-3 wt% of reinforcing fiber and 2-4 wt% of modified epoxy resin binder.
Al in the plate-shaped corundum2O3Not less than 99 percent and the average grain diameter is 0.05-2 mm.
Al in the zirconia corundum2O3+ZrO2≥98％，ZrO2Not less than 23 percent, and the average grain diameter is 0.1-2 mm.
Al in the zirconium oxide2O3The content is more than or equal to 90 percent.
The SiC content in the silicon carbide is more than or equal to 97 percent.
The content of active aluminum in the aluminum powder is more than or equal to 98%, and the average particle size is 40-100 mu m;
the modified graphite is prepared by the following method:
1) adding 1 part by weight of expanded graphite into 10-20 parts by weight of 10-30 vol% ethanol water solution, uniformly stirring, adding 0.1-0.2 part by weight of boric acid and 0.01-0.08 part by weight of tartaric acid, stirring for 2-6 h for activation, then washing with deionized water, and drying to obtain activated graphite;
2) adding activated graphite and an epoxy silane coupling agent into sufficient acetone according to the mass ratio of 1: 1-3, stirring and reacting for 5-10 h, filtering, washing with acetone and deionized water for multiple times in sequence, and drying to obtain organic silicon modified graphite;
3) adding organic silicon modified graphite and phloretin into sufficient acetone according to the mass ratio of 1: 2-5, uniformly stirring, adding potassium hydroxide or sodium hydroxide, carrying out ultrasonic auxiliary reaction for 2-6 hours at the temperature of 80-100 ℃, filtering, sequentially washing with acetone and deionized water for multiple times, and drying to obtain modified graphite;
4) and crushing the modified graphite to 200-500 meshes to obtain the modified graphite.
The modified epoxy resin binder is prepared by the following method:
adding 1 part by weight of bisphenol A type epoxy resin (with the molecular weight of 5000-10000) and 0.2-0.4 part by weight of 1, 3-bis (4-methoxyphenyl) urea into acetone, carrying out pre-reaction for 10-30 min at 90-100 ℃, adding 0.1-0.3 part by weight of sodium phthalate, continuing to react for 20-50 min, then adding 0.05-0.3 part by weight of curing agent and 0.1-0.2 part by weight of accelerator, stirring, carrying out vacuum defoaming, and cooling to obtain the modified epoxy resin.
The preparation method of the sliding plate brick comprises the following steps:
s1: mixing the materials;
s2: molding, heat treating and sintering the mixed material by a mold to obtain a sliding plate brick precursor; the heat treatment temperature is 150-200 ℃, and the heat treatment time is 20-40 h; the sintering temperature is 960-1000 ℃, and the sintering time is 10-16 h;
s3: immersing a sliding plate brick precursor into asphalt, increasing the temperature from room temperature to 175-190 ℃ at the speed of 3-8 ℃/min, carrying out oil immersion and pressure maintaining for 2-5 h under the pressure of 1.2-1.5 MPa, then increasing the temperature to 220-240 ℃ at the speed of 2-4 ℃/min, carrying out oil immersion and pressure maintaining for 1-3 h under the pressure of 1-1.3 MPa, carrying out sealed carbonization on the oil-immersed sliding plate brick in a carbonization kiln, carrying out carbonization at the temperature of 400-500 ℃ for 8-12 h, and polishing to remove residual asphalt on the surface of the sliding plate brick to obtain a semi-finished sliding plate brick; and then the sliding plate brick is obtained after finish machining treatment.
Example 1:
a preparation method of a sliding plate brick comprises the following steps:
s1: mixing the materials in the sliding brick, wherein the materials comprise the following components in percentage by weight: 50 wt% of tabular corundum with the average particle size of 0.4mm, 25 wt% of zirconium corundum with the average particle size of 0.5mm, 4 wt% of zirconium oxide, 8 wt% of silicon carbide, 3 wt% of aluminum powder with the average particle size of 55 mu m, 5 wt% of modified graphite, 2 wt% of reinforcing fiber and 3 wt% of modified epoxy resin binder;
s2: molding the mixed material by using a mold, carrying out heat treatment at 180 ℃ for 36h, and then sintering at 980 ℃ for 12h to obtain a sliding plate brick precursor;
s3: oil immersion carbonization is carried out on the sliding plate brick precursor, specifically, the sliding plate brick precursor is immersed in asphalt, the temperature is increased to 180 ℃ from room temperature at the speed of 5 ℃/min, the oil immersion and pressure maintaining are carried out for 3.5h under the pressure of 1.4MPa, then the temperature is increased to 230 ℃ at the speed of 3 ℃/min, the oil immersion and pressure maintaining are carried out for 2h under the pressure of 1.2MPa, the oil immersed sliding plate brick is subjected to sealing carbonization in a carbonization kiln, the carbonization temperature is 440 ℃, the carbonization time is 10h, and the residual asphalt on the surface of the sliding plate brick is removed through polishing, so that a semi-finished sliding plate brick is obtained; and then hooping, casing, drying, grinding, turning and drying to obtain the slide plate brick.
The modified graphite is prepared by the following steps:
adding 1 part by weight of expanded graphite into 10 parts by weight of 20 vol% ethanol aqueous solution, uniformly stirring, adding 0.15 part by weight of boric acid and 0.05 part by weight of tartaric acid, stirring and activating for 4 hours, washing with deionized water, and drying to obtain activated graphite; adding 1 part by weight of activated graphite and 2.5 parts by weight of 3-glycidyl ether oxypropyltriethoxysilane into 20 parts by weight of acetone, stirring for reaction for 6 hours, filtering, washing with acetone and deionized water for multiple times in sequence, and drying to obtain organic silicon modified graphite; adding 1 weight part of organic silicon modified graphite and 4.2 weight parts of phloretin into 20 weight parts of acetone, stirring uniformly, adding 0.2 weight part of potassium hydroxide, and performing ultrasonic treatment at 90 ℃ and ultrasonic frequency of 40KHz and ultrasonic power density of 0.5W/cm2Ultrasonic-assisted treatment is carried out for 5 hours under the condition, filtration is carried out, acetone and deionized water are sequentially used for washing for multiple times, and drying are carried out to obtain modified graphite; and crushing the modified graphite to 400 meshes to obtain the modified graphite.
The modified epoxy resin binder is prepared by the following steps:
adding 1 weight part of bisphenol A type epoxy resin (molecular weight is 8000) and 0.35 weight part of 1, 3-bis (4-methoxyphenyl) urea into acetone, pre-reacting for 20min at 95 ℃, adding 0.2 weight part of sodium phthalate, continuing to react for 40min, then adding 0.1 weight part of diethylaminopropylamine and 0.1 weight part of 2-ethyl-4-methyl-imidazole, stirring, defoaming in vacuum, and cooling to obtain the modified epoxy resin.
Example 2:
the other preparation method of the sliding brick is basically the same as the step of the embodiment 1, except that the addition amount of the phloretin is 1 part by weight in the preparation process of the modified graphite, namely the mass ratio of the organosilicon modified graphite to the phloretin is 1: 1.
Example 3:
the other preparation method of the sliding brick is basically the same as the step of the embodiment 1, except that the addition amount of the phloretin is 2 parts by weight in the preparation process of the modified graphite, namely the mass ratio of the organosilicon modified graphite to the phloretin is 1: 2.
Example 4:
the other preparation method of the sliding brick is basically the same as the step of the embodiment 1, except that the addition amount of the phloretin is 3.5 parts by weight in the preparation process of the modified graphite, namely the mass ratio of the organosilicon modified graphite to the phloretin is 1: 3.5.
Example 5:
the other preparation method of the sliding brick is basically the same as the step of the embodiment 1, except that the addition amount of the phloretin is 5 parts by weight in the preparation process of the modified graphite, namely the mass ratio of the organosilicon modified graphite to the phloretin is 1: 5.
Example 6:
the other preparation method of the sliding brick is basically the same as the step of the embodiment 1, except that the addition amount of the phloretin is 6 parts by weight in the preparation process of the modified graphite, namely the mass ratio of the organosilicon modified graphite to the phloretin is 1: 6.
Example 7:
another method of making a slide plate tile substantially the same as in example 1, except that the graphite was modified with only the epoxy silane coupling agent and not with phloretin.
Example 8:
another method for producing a slide brick was carried out in substantially the same manner as in example 1 except that the modified graphite was replaced with an unmodified expanded graphite having a particle size of 400 mesh.
Example 9:
another process for producing a slide brick substantially comprises the same steps as in example 1, except that a bisphenol A type epoxy resin (molecular weight: 8000) is used in place of the modified epoxy resin.
Test example 1:
structural characterization of the modified graphite:
the organosilicon modified graphite, the modified graphite and the unmodified expanded graphite obtained in example 1 were used as raw materials, and subjected to infrared characterization by using a U.S. bruke tesser-27 infrared spectrometer, and the results are shown in fig. 1.
FIG. 1 is an infrared spectrum of a modified graphite, wherein a represents an unmodified expanded graphite, b represents an organosilicon modified graphite, and c represents a modified graphite, as shown, compared with curve a, curve b at 1580cm-1An absorption peak of a silicon ester group appears nearby, so that the fact that the silanol group of the 3-glycidyl ether oxypropyl triethoxysilane reacts with the carboxyl group on the surface of the graphite can be proved to successfully graft the 3-glycidyl ether oxypropyl triethoxysilane to the surface of the graphite; comparing the curve b with the curve c at 1600-1500 cm-1、700～900cm-1The characteristic peak of 1260cm appears nearby-1Characteristic peaks attributed to C-O bonds appear nearby, and the results show that phloretin successfully modifies the expanded graphite.
Test example 2:
the apparent porosity and the volume density of the sliding plate brick prepared in the examples 1 to 9 are tested by referring to GB/T2997-2005 'test method for volume density, apparent porosity and true porosity of compact shaped refractory product', and the measured results are shown in FIG. 2.
FIG. 2 shows the results of the apparent porosity and bulk density tests of the sliding brick, wherein B represents the bulk density and C represents the apparent porosity, and as shown in the figure, the sliding brick prepared by the scheme provided by the invention has lower apparent porosity and higher bulk density; data in comparative examples 1 to 8It can be seen that the apparent porosity of preferred examples 1 and 3 to 5 is in the range of 1.1 to 1.5%, and the bulk density is in the range of 3.72 to 3.88g/cm3In the range, as can be seen from comparison of examples 1 to 6, in the preparation process of the modified graphite, along with the increase of the addition amount of phloretin, the apparent porosity of the sliding plate brick is reduced, and the volume density of the sliding plate brick is increased, which indicates that the modification treatment of phloretin on the graphite can directly influence the compactness of the sliding plate brick; the apparent porosity of the sliding plate brick in the embodiments 7 and 8 is higher than that of the sliding plate brick in the embodiment 1, and the volume density of the sliding plate brick is lower than that of the sliding plate brick in the embodiment 1, which shows that compared with graphite or organic silicon modified graphite, the graphite modified by adding phloretin is more beneficial to improving the compactness of the sliding plate brick; the apparent porosity of example 9 is higher than that of example 1, and the bulk density is lower than that of example 1, which illustrates that the modification treatment of the epoxy resin contributes to increase of the adhesion between the components and increase of the degree of densification of the slide brick.
Test example 3:
the sliding plate brick prepared in the embodiments 1 to 8 is used as a sample, the normal-temperature breaking strength of the sliding plate brick after 6 times of thermal shock cycles from 1100 ℃ to cold water is tested by referring to a method in GB/T30873-2014 thermal shock resistance test method, the breaking strength retention rate is calculated according to the breaking strength before thermal shock and after thermal shock, the thermal shock resistance is evaluated by using the breaking strength retention rate, and the test result is shown in FIG. 3.
FIG. 3 shows the result of the retention rate of the flexural strength of the sliding plate brick after thermal shock cycling from 1100 ℃ to cold water for 6 times, as shown in the figure, the highest retention rate of the flexural strength of the sliding plate brick obtained by the method of the present invention is 84.8%, the retention rate of the flexural strength is high, which indicates that the thermal shock resistance is excellent, and as can be seen from the retention rate of the flexural strength in comparative examples 1 to 8, the addition of graphite modified by epoxy silane coupling agent and phloretin in the sliding plate brick is helpful for improving the thermal shock resistance of the material, so that the material still has a high retention rate of the flexural strength after 6 times of thermal shock treatment, and can also be obtained, the addition of phloretin directly affects the thermal shock resistance of the sliding plate brick in the preparation process of the modified graphite, and when the mass ratio of the organosilicon modified graphite to the phloretin is within the range of 1:2 to 5, the prepared modified graphite has a proper degree of compactness, on the premise of keeping higher strength, a certain nano-pore structure is kept, nano-pores are generated in the sintering process, and the nano-pores absorb thermal stress in the thermal shock cycle process, so that the thermal shock resistance is improved.
Test example 4:
the sliding plate bricks prepared in the examples 1 to 9 are used as samples, the sliding plate bricks are soaked in molten steel at 1600 ℃ for erosion for 40min after being kept at 1600 ℃, then the sliding plate bricks are taken out to rotate at a high speed to throw away surface adherends, the sliding plate bricks are longitudinally cut along the center line of the samples, erosion depths are measured and used for evaluating the molten steel erosion resistance of the sliding plate bricks, and the measured results are shown in fig. 4.
FIG. 4 shows the molten steel erosion resistance of the sliding plate brick, and it can be seen that the components of the sliding plate brick have a large influence on the erosion resistance, the methods described in examples 1 to 6 are different in the addition of phloretin in the preparation process of the modified graphite, that is, the modification treatment degrees of graphite are different, the erosion depth of the sliding plate brick prepared in examples 1 and 3 to 5 is significantly lower than that of examples 2 and 6, the smaller the erosion depth is, the better the erosion resistance is, which shows that the treatment degree of the modified graphite has a significant influence on the erosion resistance of the final product sliding plate brick, and when the mass ratio of the organosilicon modified graphite to phloretin is in the range of 1:2 to 5, the better gain effect on the erosion resistance of the sliding plate brick is achieved; example 7 is graphite modified only with epoxy silane coupling agent, example 8 is unmodified graphite, the erosion depth of the sliding plate brick prepared by examples 7 and 8 has a larger difference with that of example 1, while the erosion depth of examples 7 and 8 is almost equivalent, which shows that the graphite modified only with epoxy silane coupling agent has no obvious influence on the erosion resistance of the final sliding plate brick; the erosion depth of example 9 is higher than that of example 1, which shows that compared with epoxy resin, the modified epoxy resin is used as a bonding agent, so that the interfacial bonding capability among particles in the sliding plate brick under high temperature can be increased, the infiltration erosion of molten steel is reduced, and the molten steel erosion resistance is improved.
Test example 5:
the sliding plate bricks prepared in the embodiments 1 to 8 are used as samples, the abrasion resistance of the materials is tested by referring to GB/T18301-2012 test method for abrasion resistance at normal temperature of refractory materials, and the test result is shown in FIG. 5.
FIG. 5The abrasion loss of the sliding plate brick is shown in the figure, the modification treatment of graphite and the modification treatment of epoxy resin have great influence on the abrasion resistance of the sliding plate brick, and the abrasion loss of the sliding plate brick prepared in the examples 1,3 and 5 is less than or equal to 2cm3While the abrasion loss of the sliding brick obtained in examples 2 and 6 was more than 2.5cm3The influence of the addition amount of phloretin on the wear resistance of the sliding plate brick in the modification process of the graphite is relatively large; the abrasion loss of the sliding brick obtained in examples 7 and 8 was higher than 3cm3Indicating that the fully modified graphite has a higher wear resistance gain effect than unmodified or incompletely modified graphite.
Conventional operations in the operation steps of the present invention are well known to those skilled in the art and will not be described herein.
The above embodiments are merely illustrative, and not restrictive, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention. Therefore, all equivalent technical solutions also belong to the scope of the present invention, and the protection scope of the present invention should be defined by the claims.
Claims (10)
1. The preparation method of the modified graphite is characterized by comprising the following steps:
1) in an ethanol water solution, boric acid and tartaric acid are used for carrying out surface activation on the expanded graphite to obtain activated graphite;
2) modifying the activated graphite by using an epoxy silane coupling agent to obtain organic silicon modified graphite;
3) treating the organic silicon modified graphite with phloretin under alkaline conditions, and crushing to obtain the product.
2. The method as claimed in claim 1, wherein the mass ratio of the activated graphite to the epoxy silane coupling agent in the step 2) is 1: 1-3.
3. The method according to claim 1, wherein the mass ratio of the organosilicon modified graphite to the phloretin in the step 3) is 1: 2-5.
4. The application of the modified graphite prepared by the method of any one of claims 1 to 3 in the preparation of slide bricks, which is characterized by comprising the following steps:
the molten steel erosion resistance of the sliding plate brick is improved; and/or
The wear resistance of the sliding plate brick is improved.
5. A slide tile, comprising:
a substrate composed of tabular corundum, zircon corundum, zirconia, silicon carbide, aluminum powder and modified graphite prepared by the method of any one of claims 1 to 3;
a reinforcing fiber; and
modified epoxy resin binder.
6. The sliding plate brick as claimed in claim 5, wherein the modified epoxy resin is 1, 3-bis (4-methoxyphenyl) urea modified epoxy resin, and is prepared by the following method:
adding epoxy resin and 1, 3-bis (4-methoxyphenyl) urea into acetone, carrying out pre-reaction for 10-30 min at 90-100 ℃, adding sodium phthalate, continuing to react for 20-50 min, then adding a curing agent and an accelerant, stirring, carrying out vacuum defoaming, and cooling to obtain the modified epoxy resin.
7. The sliding plate brick according to claim 6, wherein the mass ratio of the epoxy resin to the 1, 3-bis (4-methoxyphenyl) urea is 1:0.2 to 0.4.
8. A method of manufacturing a slide plate brick according to any one of claims 5 to 7, comprising the steps of:
s1: mixing the materials;
s2: molding, heat treating and sintering the mixed material by a mold to obtain a sliding plate brick precursor;
s3: and sequentially carrying out oil immersion carbonization and finish machining on the sliding plate brick precursor to obtain the sliding plate brick.
9. The method for preparing a slide plate brick according to claim 8, wherein the sintering temperature is 960 to 1000 ℃ and the sintering time is 10 to 16 hours.
10. The preparation method of the sliding brick according to claim 8, wherein the oil-immersed carbonization is an oil-immersed treatment with asphalt, and the specific steps are as follows:
immersing a sliding plate brick precursor into asphalt, increasing the temperature from room temperature to 175-190 ℃ at the speed of 3-8 ℃/min, carrying out oil immersion and pressure maintaining for 2-5 h under the pressure of 1.2-1.5 MPa, then increasing the temperature to 220-240 ℃ at the speed of 2-4 ℃/min, carrying out oil immersion and pressure maintaining for 1-3 h under the pressure of 1-1.3 MPa, carrying out sealed carbonization on the oil immersed sliding plate brick in a carbonization kiln at the carbonization temperature of 400-500 ℃ for 8-12 h, and polishing to remove residual asphalt on the surface of the sliding plate brick to obtain a semi-finished sliding plate brick.
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| CN117303924A (en) * | 2023-11-29 | 2023-12-29 | 河北国亮新材料股份有限公司 | Long-service-life sliding plate brick and preparation method thereof |
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