CN113666761A - High-temperature-resistant roller and preparation method thereof - Google Patents
High-temperature-resistant roller and preparation method thereof Download PDFInfo
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- CN113666761A CN113666761A CN202111150021.8A CN202111150021A CN113666761A CN 113666761 A CN113666761 A CN 113666761A CN 202111150021 A CN202111150021 A CN 202111150021A CN 113666761 A CN113666761 A CN 113666761A
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- 238000002360 preparation method Methods 0.000 title abstract description 6
- 239000002245 particle Substances 0.000 claims abstract description 80
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical class [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 239000003607 modifier Substances 0.000 claims abstract description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 7
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 41
- 239000012065 filter cake Substances 0.000 claims description 41
- 238000001914 filtration Methods 0.000 claims description 35
- 238000003756 stirring Methods 0.000 claims description 35
- 239000000243 solution Substances 0.000 claims description 30
- 239000000706 filtrate Substances 0.000 claims description 25
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 24
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 17
- 229910021641 deionized water Inorganic materials 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 16
- 235000019441 ethanol Nutrition 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 10
- 229910021389 graphene Inorganic materials 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 238000010992 reflux Methods 0.000 claims description 10
- 230000003014 reinforcing effect Effects 0.000 claims description 10
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 8
- ASOKPJOREAFHNY-UHFFFAOYSA-N 1-Hydroxybenzotriazole Chemical compound C1=CC=C2N(O)N=NC2=C1 ASOKPJOREAFHNY-UHFFFAOYSA-N 0.000 claims description 8
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 8
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 8
- 239000004917 carbon fiber Substances 0.000 claims description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 8
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims description 8
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 8
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 8
- 239000001119 stannous chloride Substances 0.000 claims description 8
- 235000011150 stannous chloride Nutrition 0.000 claims description 8
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 7
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 7
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 7
- 235000019838 diammonium phosphate Nutrition 0.000 claims description 7
- 238000010304 firing Methods 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 7
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 5
- 229910052681 coesite Inorganic materials 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 229910052906 cristobalite Inorganic materials 0.000 claims description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 5
- 238000005245 sintering Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 229910052682 stishovite Inorganic materials 0.000 claims description 5
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 229910052905 tridymite Inorganic materials 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 238000000748 compression moulding Methods 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- 238000003825 pressing Methods 0.000 abstract description 5
- 239000000654 additive Substances 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 abstract description 2
- 238000004299 exfoliation Methods 0.000 abstract 1
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 11
- 239000000919 ceramic Substances 0.000 description 5
- 238000005452 bending Methods 0.000 description 4
- 238000000465 moulding Methods 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 239000011819 refractory material Substances 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000009990 desizing Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Classifications
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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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/481—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing silicon, e.g. zircon
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
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Abstract
The invention discloses a high temperature resistant roller and a preparation method thereof, the roller is prepared by blending and pressing modified reinforced particles and modified zirconium silicate particles, the modified zirconium silicate particles are treated by a modifier to deform island-shaped structures, [ SiO ]4]Tetrahedra and [ ZrO ]8]Dodecahedral exfoliation of SiO2‑Al2O3The composite oxide has a more stable structure, and the [ SiO ] is controlled by the additive4]Tetrahedron, [ AlO6]Octahedron forms a tightly connected spherical structure under certain conditions, and the spherical structure is connected with [ ZrO ]8]The dodecahedron is recombined to form the ring [ ZrO ]8]The dodecahedron island-shaped structure and the island-shaped structure of zirconium silicate are unchanged, so that the high temperature resistance, the wear resistance and the toughness of the roller are improved, modified reinforced particles are prepared, and the toughness of the high temperature resistant roller is further improvedAnd the service life of the roller rod is prolonged.
Description
Technical Field
The invention relates to the technical field of roller rod preparation, in particular to a high-temperature-resistant roller rod and a preparation method thereof.
Background
The roller kiln has the characteristics of small firing temperature difference, short firing period, high yield, low energy consumption, easy control and the like, is widely applied to the industries of building sanitary ceramics (particularly wall and floor tiles and sanitary wares), household ceramics, special ceramics and ferrites, glass, metal annealing and the like, and the requirements on the manufacturing technology and the used refractory materials of the roller kiln are continuously improved along with the increasing expansion of the application range of the roller kiln;
in the roller kiln, the roller is the most critical refractory material and plays a role in bearing and conveying products in the kiln, namely the strength and high-temperature mechanical property of the roller determine the service temperature and the loading capacity of the roller kiln, and further determine the application range of the roller kiln, so that the key point for further popularization and application of the roller kiln is to research the performance of the roller by using materials for manufacturing the roller to improve the performance of the roller.
Disclosure of Invention
The invention aims to provide a high-temperature-resistant roller and a preparation method thereof, and solves the problem that the mechanical property of the ceramic roller used at the present stage is reduced under the high-temperature-resistant condition through modified zirconium silicate particles and modified reinforcing particles.
The purpose of the invention can be realized by the following technical scheme:
a high-temperature resistant roller rod comprises the following raw materials in parts by weight: 95-98 parts of modified zirconium silicate particles and 2-5 parts of modified reinforcing particles;
the high-temperature resistant roller rod is prepared by the following steps:
uniformly blending the modified zirconium silicate particles and the modified reinforcing particles by using absolute ethyl alcohol, performing compression molding under the pressure of 25-35MPa, and then performing sintering and heat preservation for 2-3h under the temperature of 1570-1580 ℃ to obtain the high-temperature-resistant roller rod.
The modified zirconium silicate particles are prepared by the following steps:
step A1: uniformly mixing zirconium silicate, a modifier and a sodium chloride aqueous solution, and performing ball milling for 3-5 hours to prepare a mixture;
step A2: and (3) firing the mixture at the temperature of 1570-.
Furthermore, the dosage ratio of the modified zirconium silicate particles to the modified reinforcing particles is 10: 1.
Furthermore, the size of the modified zirconium silicate particles is D50:1.6-2.0 μm, D97:2.0-3.0 μm, the number of particles smaller than 2 μm is more than or equal to 85 percent, and the specific surface area of the modified zirconium silicate particles is 5.0-10.0m2/c.c.。
Further, the modifier comprises the following raw materials: ZrO2 is more than or equal to 64 percent, SiO2 is less than or equal to 35.0 percent, Al2O3 is less than or equal to 3.0 percent, CaO + MgO is less than or equal to 0.1 percent, K2O is less than or equal to 0.1 percent, Na2O is less than or equal to 0.1 percent, and Fe2O3+ TiO2 is less than or equal to 0.5 percent.
Further, the modified reinforced particles are prepared by the following steps:
step B1: adding graphene into ethanol, carrying out ultrasonic treatment for 1-1.5h under the condition of the frequency of 50-60kHz, adding gamma-aminopropyltriethoxysilane and deionized water, reacting for 10-15h under the conditions of the rotation speed of 200-70 ℃ and the temperature of 60-70 ℃, cooling to room temperature, centrifuging to remove ethanol and deionized water, drying a substrate, dispersing the substrate in N, N-dimethylformamide, stirring and adding silver nitrate under the conditions of the rotation speed of 800-1000r/min and the temperature of 85-95 ℃, stirring for 3-5h in a dark place, filtering, soaking a filter cake in diammonium hydrogen phosphate for 20-25h, taking out, carrying out heat preservation for 1-1.3h under the conditions of the pressure of 0.01-0.02MPa and the temperature of 650-700 ℃, preparing modified graphene;
step B2: adding carbon fiber particles into acetone, refluxing for 10-15h at 60-70 ℃, filtering to remove filtrate, drying a filter cake, adding the filter cake into concentrated nitric acid, refluxing for 1-3h at the rotation speed of 200-300r/min and the temperature of 70-80 ℃, filtering to remove filtrate, washing the filter cake to the pH value of 7 by deionized water, drying and dispersing in tetrahydrofuran, stirring and adding modified graphene and 1-hydroxybenzotriazole at the rotation speed of 150-200r/min and the temperature of 60-70 ℃, reacting for 8-10h, and filtering to obtain pre-modified particles;
step B3: adding the pre-modified particles into a stannous chloride solution, stirring for 10-15min at the rotation speed of 200-300r/min and the temperature of 25-30 ℃, filtering to remove the filtrate, adding the filter cake into a palladium chloride solution, continuously stirring for 10-15min at the rotation speed of 200-300r/min and the temperature of 30-40 ℃, filtering to remove the filtrate, adding the filter cake into a nickel chloride hexahydrate solution, stirring at the rotation speed of 300-500r/min and the temperature of 60-70 ℃, adding sodium hypophosphite, keeping the pH value of the reaction solution at 9-11, stirring for 2-4h, filtering to remove the filtrate, and drying the filter cake to obtain the modified reinforced particles.
Further, the dosage ratio of the graphene, the ethanol, the gamma-aminopropyltriethoxysilane and the deionized water in the step B1 is 1g:100mL:5mL:20mL, and the dosage ratio of the substrate, the N, N-dimethylformamide, the silver nitrate and the diammonium hydrogen phosphate is 15g:100mL:6g:4 g.
Further, the mass ratio of the filter cake, the modified graphene and the 1-hydroxybenzotriazole in the step B2 is 1:3: 0.8.
Further, the dosage ratio of the pre-modified particles and the stannous chloride solution in the step B3 is 1g:6mL, the mass fraction of the stannous chloride solution is 20%, the dosage ratio of the filter cake and the palladium chloride solution is 1g:8mL, the mass fraction of the palladium chloride solution is 15%, the dosage ratio of the filter cake, the nickel chloride hexahydrate solution and the sodium hypophosphite is 1g:30mL:3g, and the mass fraction of the nickel chloride hexahydrate solution is 10%.
The invention has the beneficial effects that:
the high-temperature-resistant roller rod is prepared by blending and pressing modified reinforced particles and modified zirconium silicate particles, wherein the modified zirconium silicate particles are treated by a modifier to deform island-shaped structures, [ SiO ]4]Tetrahedra and [ ZrO ]8]The dodecahedron is detached. SiO22-Al2O3The composite oxide has a more stable structure, and the [ SiO ] is controlled by the additive4]Tetrahedron, [ AlO6]Octahedron forms a tightly connected spherical structure under certain conditions, and the spherical structure is connected with [ ZrO ]8]The dodecahedron is recombined to form the ring [ ZrO ]8]The dodecahedron island-shaped structure and the island-shaped structure of zirconium silicate are unchanged, so that the high temperature resistance, the wear resistance and the toughness of the roller rod are improved, modified reinforced particles are prepared, graphene is used as a raw material, surface treatment is firstly carried out on the modified reinforced particles, amino groups are grafted on the surface of the graphene, andthe modified graphene is prepared by treating with silver nitrate, embedding silver into gaps on the surface of the graphene, desizing the carbon fiber and oxidizing the carbon fiber with concentrated nitric acid, so that active hydroxyl on the surface of the carbon fiber is converted into amino, and then the amino is subjected to dehydration condensation with the modified graphene under the action of 1-hydroxybenzotriazole to prepare modified particles, and then the modified particles are subjected to nickel plating to prepare modified reinforced particles.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A high-temperature resistant roller rod comprises the following raw materials in parts by weight: 95 parts of modified zirconium silicate particles and 2 parts of modified reinforcing particles;
the high-temperature resistant roller rod is prepared by the following steps:
uniformly blending the modified zirconium silicate particles and the modified reinforced particles by using absolute ethyl alcohol, pressing and molding under the condition that the pressure is 25MPa, and sintering and keeping the temperature for 2 hours under the condition that the temperature is 1570 ℃ to prepare the high-temperature resistant roller rod.
The modified zirconium silicate particles are prepared by the following steps:
step A1: uniformly mixing zirconium silicate, a modifier and a sodium chloride aqueous solution, and performing ball milling for 3 hours to prepare a mixture;
step A2: and firing the mixture at 1570 ℃ for 1h to obtain the modified zirconium silicate particles.
The modifier comprises the following raw materials: ZrO (ZrO)2 67.3%、SiO2 30%、Al2O3 2.5%、CaO+MgO 0.05%、K2O 0.05%、Na2O 0.05%、Fe2O3+TiO2 0.05%。
The modified reinforced particles are prepared by the following steps:
step B1: adding graphene into ethanol, carrying out ultrasonic treatment for 1h under the condition of 50kHz, adding gamma-aminopropyltriethoxysilane and deionized water, reacting for 10h under the conditions of 200r/min of rotation speed and 60 ℃, cooling to room temperature, centrifuging to remove ethanol and deionized water, drying a substrate, dispersing the substrate in N, N-dimethylformamide, stirring and adding silver nitrate under the conditions of 800r/min of rotation speed and 85 ℃, stirring for 3h in a dark place, filtering, soaking a filter cake in diammonium hydrogen phosphate for 20h, taking out, and carrying out heat preservation for 1h under the conditions of 0.01MPa of pressure and 650 ℃ to obtain modified graphene;
step B2: adding carbon fiber particles into acetone, refluxing for 10 hours at the temperature of 60 ℃, filtering to remove filtrate, drying a filter cake, adding the filter cake into concentrated nitric acid, refluxing for 1 hour at the rotation speed of 200r/min and the temperature of 70 ℃, filtering to remove the filtrate, washing the filter cake to a pH value of 7 by using deionized water, drying and dispersing in tetrahydrofuran, stirring at the rotation speed of 150r/min and the temperature of 60 ℃, adding modified graphene and 1-hydroxybenzotriazole, reacting for 8 hours, and filtering to obtain pre-modified particles;
step B3: adding the pre-modified particles into a stannous chloride solution, stirring for 10min at the rotation speed of 200r/min and the temperature of 25 ℃, filtering to remove filtrate, adding a filter cake into a palladium chloride solution, continuously stirring for 10min at the rotation speed of 200r/min and the temperature of 30 ℃, filtering to remove the filtrate, adding the filter cake into a nickel chloride hexahydrate solution, stirring and adding sodium hypophosphite at the rotation speed of 300r/min and the temperature of 60 ℃, keeping the pH value of the reaction solution at 9, stirring for 2h, filtering to remove the filtrate, and drying the filter cake to obtain the modified reinforced particles.
Example 2
A high-temperature resistant roller rod comprises the following raw materials in parts by weight: 96 parts of modified zirconium silicate particles and 3 parts of modified reinforcing particles;
the high-temperature resistant roller rod is prepared by the following steps:
uniformly blending the modified zirconium silicate particles and the modified reinforced particles by using absolute ethyl alcohol, pressing and molding under the condition that the pressure is 30MPa, and then sintering and preserving heat for 2.5 hours under the condition that the temperature is 1575 ℃ to obtain the high-temperature resistant roller rod.
The modified zirconium silicate particles are prepared by the following steps:
step A1: uniformly mixing zirconium silicate, a modifier and a sodium chloride aqueous solution, and performing ball milling for 4 hours to prepare a mixture;
step A2: and firing the mixture at 1575 ℃ for 2h to obtain the modified zirconium silicate particles.
The modifier comprises the following raw materials: ZrO (ZrO)2 66.2%、SiO2 30.0%、Al2O3 3.0%、CaO+MgO 0.1%、K2O 0.1%、Na2O 0.1%、Fe2O3+TiO2 0.5%。
The modified reinforced particles are prepared by the following steps:
step B1: adding graphene into ethanol, carrying out ultrasonic treatment for 1.3h under the condition of 55kHz, adding gamma-aminopropyltriethoxysilane and deionized water, carrying out reaction for 13h under the conditions of 200r/min of rotation speed and 65 ℃, cooling to room temperature, centrifuging to remove ethanol and deionized water, drying a substrate, dispersing the substrate in N, N-dimethylformamide, stirring and adding silver nitrate under the conditions of 900r/min of rotation speed and 90 ℃, stirring for 4h in a dark place, filtering, soaking a filter cake in diammonium hydrogen phosphate for 23h, taking out, and carrying out heat preservation for 1.2h under the conditions of 0.015MPa of pressure and 680 ℃ to obtain modified graphene;
step B2: adding carbon fiber particles into acetone, refluxing for 13 hours at the temperature of 65 ℃, filtering to remove filtrate, drying a filter cake, adding the filter cake into concentrated nitric acid, refluxing for 2 hours at the rotation speed of 300r/min and the temperature of 75 ℃, filtering to remove the filtrate, washing the filter cake to a pH value of 7 by using deionized water, drying and dispersing in tetrahydrofuran, stirring at the rotation speed of 180r/min and the temperature of 65 ℃, adding modified graphene and 1-hydroxybenzotriazole, reacting for 9 hours, and filtering to obtain pre-modified particles;
step B3: adding the pre-modified particles into a stannous chloride solution, stirring for 13min at the rotation speed of 300r/min and the temperature of 28 ℃, filtering to remove filtrate, adding a filter cake into a palladium chloride solution, continuously stirring for 13min at the rotation speed of 300r/min and the temperature of 35 ℃, filtering to remove filtrate, adding the filter cake into a nickel chloride hexahydrate solution, stirring and adding sodium hypophosphite at the rotation speed of 500r/min and the temperature of 65 ℃, keeping the pH value of a reaction solution at 10, stirring for 3h, filtering to remove filtrate, and drying the filter cake to obtain the modified reinforced particles.
Example 3
A high-temperature resistant roller rod comprises the following raw materials in parts by weight: 98 parts of modified zirconium silicate particles and 5 parts of modified reinforcing particles;
the high-temperature resistant roller rod is prepared by the following steps:
uniformly blending the modified zirconium silicate particles and the modified reinforced particles by using absolute ethyl alcohol, pressing and molding under the condition that the pressure is 35MPa, and then sintering and preserving heat for 3 hours under the condition that the temperature is 1580 ℃ to prepare the high-temperature resistant roller rod.
The modified zirconium silicate particles are prepared by the following steps:
step A1: uniformly mixing zirconium silicate, a modifier and a sodium chloride aqueous solution, and performing ball milling for 5 hours to prepare a mixture;
step A2: and (3) firing the mixture at 1580 ℃ for 3h to obtain the modified zirconium silicate particles.
The modifier comprises the following raw materials: ZrO (ZrO)2 64%、SiO2 32.2%、Al2O3 3.0%、CaO+MgO 0.1%、K2O 0.1%、Na2O 0.1%、Fe2O3+TiO2 0.5%。
The modified reinforced particles are prepared by the following steps:
step B1: adding graphene into ethanol, carrying out ultrasonic treatment for 1.5h under the condition of 60kHz, adding gamma-aminopropyltriethoxysilane and deionized water, carrying out reaction for 15h under the conditions of 300r/min of rotation speed and 70 ℃, cooling to room temperature, centrifuging to remove ethanol and deionized water, drying a substrate, dispersing the substrate in N, N-dimethylformamide, stirring and adding silver nitrate under the conditions of 1000r/min of rotation speed and 95 ℃, stirring for 5h in a dark place, filtering, soaking a filter cake in diammonium hydrogen phosphate for 25h, taking out, and carrying out heat preservation for 1.3h under the conditions of 0.02MPa of pressure and 700 ℃ to obtain modified graphene;
step B2: adding carbon fiber particles into acetone, refluxing for 15 hours at the temperature of 70 ℃, filtering to remove filtrate, drying a filter cake, adding the filter cake into concentrated nitric acid, refluxing for 3 hours at the rotation speed of 300r/min and the temperature of 80 ℃, filtering to remove the filtrate, washing the filter cake to a pH value of 7 by using deionized water, drying and dispersing in tetrahydrofuran, stirring at the rotation speed of 200r/min and the temperature of 70 ℃, adding modified graphene and 1-hydroxybenzotriazole, reacting for 10 hours, and filtering to obtain pre-modified particles;
step B3: adding the pre-modified particles into a stannous chloride solution, stirring for 15min at the rotation speed of 300r/min and the temperature of 30 ℃, filtering to remove filtrate, adding a filter cake into a palladium chloride solution, continuously stirring for 15min at the rotation speed of 300r/min and the temperature of 40 ℃, filtering to remove the filtrate, adding the filter cake into a nickel chloride hexahydrate solution, stirring and adding sodium hypophosphite at the rotation speed of 500r/min and the temperature of 70 ℃, keeping the pH value of the reaction solution at 11, stirring for 4h, filtering to remove the filtrate, and drying the filter cake to obtain the modified reinforced particles.
Comparative example 1
This comparative example compared with example 1, in which zirconium silicate particles were used instead of the modified zirconium silicate particles, the remaining steps were the same.
Comparative example 2
This comparative example compares to example 1 without the addition of modified reinforcing particles and the rest of the procedure is the same.
Comparative example 3
This comparative example is a ceramic roller disclosed in chinese patent CN 105481349A.
The bending strength of the roller rods obtained in examples 1-3 and comparative examples 1-3 was measured in accordance with GB/T4741-1999 in environments of 1200, 1300, and 1400 ℃ and the results are shown in the following table;
| example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Flexural Strength (MPa) at 1200 DEG C | 52 | 55 | 53 | 36 | 38 | 43 |
| Bending Strength (MPa) at 1300 ℃ | 53 | 54 | 53 | 35 | 36 | 41 |
| Flexural Strength (MPa) at 1400 ℃ | 52 | 54 | 52 | 31 | 35 | 38 |
As can be seen from the above table, the bending strength of the roller rods prepared in examples 1-3 at 1200 deg.C, 1300 deg.C and 1400 deg.C respectively is not changed obviously, while the bending strength of the roller rods prepared in comparative examples 1-3 is reduced obviously, which shows that the roller rods prepared by the invention have good high temperature resistance and mechanical property.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (8)
1. A high temperature resistant roller rod is characterized in that: the feed comprises the following raw materials in parts by weight: 95-98 parts of modified zirconium silicate particles and 2-5 parts of modified reinforcing particles;
the modified zirconium silicate particles are prepared by the following steps:
step A1: uniformly mixing zirconium silicate, a modifier and a sodium chloride aqueous solution, and performing ball milling for 3-5 hours to prepare a mixture;
step A2: and (3) firing the mixture at the temperature of 1570-.
2. A refractory roll bar in accordance with claim 1, wherein: the size of the modified zirconium silicate particles is D50:1.6-2.0 μm, D97:2.0-3.0 μm, the number of particles smaller than 2 μm is more than or equal to 85 percent, and the specific surface area of the modified zirconium silicate particles is 5.0-10.0m2/c.c.。
3. A refractory roll bar in accordance with claim 1, wherein: the modifier comprises the following raw materials: ZrO2 is more than or equal to 64 percent, SiO2 is less than or equal to 35.0 percent, Al2O3 is less than or equal to 3.0 percent, CaO + MgO is less than or equal to 0.1 percent, K2O is less than or equal to 0.1 percent, Na2O is less than or equal to 0.1 percent, and Fe2O3+ TiO2 is less than or equal to 0.5 percent.
4. A refractory roll bar in accordance with claim 1, wherein: the modified reinforced particles are prepared by the following steps:
step B1: adding graphene into ethanol, carrying out ultrasonic treatment, adding gamma-aminopropyltriethoxysilane and deionized water, reacting, cooling to room temperature, centrifuging to remove ethanol and deionized water, drying a substrate, dispersing the substrate in N, N-dimethylformamide, stirring, adding silver nitrate, stirring in a dark place, filtering, soaking a filter cake in diammonium hydrogen phosphate, taking out, and carrying out heat preservation to obtain modified graphene;
step B2: adding carbon fiber particles into acetone, refluxing, filtering to remove filtrate, drying a filter cake, adding the filter cake into concentrated nitric acid, refluxing, filtering to remove filtrate, washing the filter cake with deionized water, drying, dispersing in tetrahydrofuran, stirring, adding modified graphene and 1-hydroxybenzotriazole, reacting, and filtering to obtain pre-modified particles;
step B3: adding the pre-modified particles into a stannous chloride solution, stirring, filtering to remove filtrate, adding a filter cake into a palladium chloride solution, continuously stirring, filtering to remove filtrate, adding the filter cake into a nickel chloride hexahydrate solution, stirring, adding sodium hypophosphite, keeping the pH value of a reaction solution, stirring, filtering to remove filtrate, and drying the filter cake to obtain the modified reinforced particles.
5. A refractory roll bar in accordance with claim 4, wherein: the using amount ratio of the graphene, the ethanol, the gamma-aminopropyltriethoxysilane and the deionized water in the step B1 is 1g to 100mL to 5mL to 20mL, and the using amount ratio of the substrate, the N, N-dimethylformamide, the silver nitrate and the diammonium hydrogen phosphate is 15g to 100mL to 6g to 4 g.
6. A refractory roll bar in accordance with claim 4, wherein: the mass ratio of the filter cake, the modified graphene and the 1-hydroxybenzotriazole in the step B2 is 1:3: 0.8.
7. A refractory roll bar in accordance with claim 4, wherein: the dosage ratio of the pre-modified particles and the stannous chloride solution in the step B3 is 1g to 6mL, the dosage ratio of the filter cake and the palladium chloride solution is 1g to 8mL, and the dosage ratio of the filter cake, the nickel chloride hexahydrate solution and the sodium hypophosphite is 1g to 30mL to 3 g.
8. The method for preparing the high-temperature resistant roller rod according to claim 1, wherein the method comprises the following steps: the method specifically comprises the following steps:
uniformly blending the modified zirconium silicate particles and the modified reinforcing particles by using absolute ethyl alcohol, performing compression molding under the pressure of 25-35MPa, and then performing sintering and heat preservation for 2-3h under the temperature of 1570-1580 ℃ to obtain the high-temperature-resistant roller rod.
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