CN116041068B - Antioxidant silicon oxynitride combined silicon carbide brick for low-oxygen copper rod smelting furnace - Google Patents
Antioxidant silicon oxynitride combined silicon carbide brick for low-oxygen copper rod smelting furnace Download PDFInfo
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- CN116041068B CN116041068B CN202310209388.5A CN202310209388A CN116041068B CN 116041068 B CN116041068 B CN 116041068B CN 202310209388 A CN202310209388 A CN 202310209388A CN 116041068 B CN116041068 B CN 116041068B
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- silicon carbide
- silicon oxynitride
- brick
- heat preservation
- thermal expansion
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- 239000011449 brick Substances 0.000 title claims abstract description 76
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 73
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 55
- 239000010703 silicon Substances 0.000 title claims abstract description 55
- 239000001301 oxygen Substances 0.000 title claims abstract description 38
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 38
- 239000003963 antioxidant agent Substances 0.000 title claims abstract description 23
- 230000003078 antioxidant effect Effects 0.000 title claims abstract description 23
- 238000003723 Smelting Methods 0.000 title claims abstract description 16
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 12
- 239000010949 copper Substances 0.000 title claims abstract description 12
- 239000004005 microsphere Substances 0.000 claims abstract description 38
- 238000004321 preservation Methods 0.000 claims abstract description 35
- 238000002156 mixing Methods 0.000 claims abstract description 33
- 238000005245 sintering Methods 0.000 claims abstract description 33
- 239000000843 powder Substances 0.000 claims abstract description 24
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 23
- 239000007767 bonding agent Substances 0.000 claims abstract description 19
- 230000003647 oxidation Effects 0.000 claims abstract description 15
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 15
- 229910052582 BN Inorganic materials 0.000 claims abstract description 12
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 12
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 229910021487 silica fume Inorganic materials 0.000 claims abstract description 11
- 230000003064 anti-oxidating effect Effects 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 39
- 238000010438 heat treatment Methods 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- 239000000203 mixture Substances 0.000 claims description 29
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims description 17
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 14
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 13
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 12
- 239000005011 phenolic resin Substances 0.000 claims description 12
- 229920001568 phenolic resin Polymers 0.000 claims description 12
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical group [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 240000004808 Saccharomyces cerevisiae Species 0.000 claims description 8
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- 229910002804 graphite Inorganic materials 0.000 claims description 7
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- NHTMVDHEPJAVLT-UHFFFAOYSA-N Isooctane Chemical compound CC(C)CC(C)(C)C NHTMVDHEPJAVLT-UHFFFAOYSA-N 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 235000019425 dextrin Nutrition 0.000 claims description 6
- JVSWJIKNEAIKJW-UHFFFAOYSA-N dimethyl-hexane Natural products CCCCCC(C)C JVSWJIKNEAIKJW-UHFFFAOYSA-N 0.000 claims description 6
- 238000000265 homogenisation Methods 0.000 claims description 6
- 239000002893 slag Substances 0.000 claims description 6
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims description 6
- AJLNZWYOJAWBCR-OOPVGHQCSA-N (4s)-4-acetamido-5-[[(2s)-1-[[(2s)-1-[[(2s)-5-amino-1-[[(2s)-1-[[(2s)-1-amino-5-(diaminomethylideneamino)-1-oxopentan-2-yl]amino]-5-(diaminomethylideneamino)-1-oxopentan-2-yl]amino]-1,5-dioxopentan-2-yl]amino]-4-methylsulfanyl-1-oxobutan-2-yl]amino]-4-car Chemical compound OC(=O)CC[C@H](NC(C)=O)C(=C)N[C@@H](CCC(O)=O)C(=O)N[C@@H](CCSC)C(=O)N[C@@H](CCC(N)=O)C(=O)N[C@@H](CCCN=C(N)N)C(=O)N[C@@H](CCCN=C(N)N)C(N)=O AJLNZWYOJAWBCR-OOPVGHQCSA-N 0.000 claims description 5
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical group NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 5
- KOVPXZDUVJGGFU-UHFFFAOYSA-N 8-methoxy-8-oxooctanoic acid Chemical group COC(=O)CCCCCCC(O)=O KOVPXZDUVJGGFU-UHFFFAOYSA-N 0.000 claims description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 5
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- 229910001873 dinitrogen Inorganic materials 0.000 claims description 5
- 230000001804 emulsifying effect Effects 0.000 claims description 5
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical group [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 229920001184 polypeptide Polymers 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 102000004196 processed proteins & peptides Human genes 0.000 claims description 4
- 108090000765 processed proteins & peptides Proteins 0.000 claims description 4
- 239000001593 sorbitan monooleate Chemical group 0.000 claims description 4
- 229940035049 sorbitan monooleate Drugs 0.000 claims description 4
- 239000011203 carbon fibre reinforced carbon Substances 0.000 claims description 3
- 229920001577 copolymer Polymers 0.000 claims description 3
- 239000012792 core layer Substances 0.000 claims description 3
- -1 glycidyl ester Chemical group 0.000 claims description 3
- 239000000178 monomer Substances 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 3
- 229920002554 vinyl polymer Polymers 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims 3
- ZORQXIQZAOLNGE-UHFFFAOYSA-N 1,1-difluorocyclohexane Chemical group FC1(F)CCCCC1 ZORQXIQZAOLNGE-UHFFFAOYSA-N 0.000 claims 1
- 235000011069 sorbitan monooleate Nutrition 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229920000103 Expandable microsphere Polymers 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
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- 238000005260 corrosion Methods 0.000 description 2
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- 239000012535 impurity Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
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- 229920000642 polymer Polymers 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 241000124033 Salix Species 0.000 description 1
- 229920001587 Wood-plastic composite Polymers 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
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- 229910001882 dioxygen Inorganic materials 0.000 description 1
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- 238000004945 emulsification Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
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- 239000004088 foaming agent Substances 0.000 description 1
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- 238000000227 grinding Methods 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
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- 239000011819 refractory material Substances 0.000 description 1
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- 239000011734 sodium Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
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- 239000011155 wood-plastic composite Substances 0.000 description 1
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- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- 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
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- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
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Abstract
The invention discloses an antioxidation silicon oxynitride combined silicon carbide brick for a low-oxygen copper rod smelting furnace, which comprises 15-20% of silicon oxynitride and 5-8% of alpha-Al by weight percent 2 O 3 Micro powder, 4-6% of boron nitride powder, 10-15% of silica fume, 4-7% of bonding agent, 1-3% of antioxidant, 0.5-1% of thermal expansion microsphere and the balance of nano silicon carbide; the preparation method of the antioxidant silicon oxynitride combined silicon carbide brick comprises the following steps: s1, mixing raw materials; s2, sintering and forming; according to the invention, the silicon nitride combined silicon carbide brick with excellent thermal stability, high temperature resistance and oxidation resistance is obtained by adding the thermal expansion microspheres and controlling the heat preservation time.
Description
Technical Field
The invention relates to the technical field of refractory materials, in particular to an antioxidant silicon oxynitride combined silicon carbide brick for a low-oxygen copper rod smelting furnace.
Background
The elements are easy to oxidize and the alloy is easy to inhale in the smelting process of the low-oxygen copper rod, and in order to obtain the alloy liquid with small burning loss, low air content, few inclusions and uniform and high quality chemical components, the smelting furnace has the following requirements: 1) The rapid melting and heating of the metal furnace burden are facilitated, the melting time is shortened, the element burning loss and the air suction are reduced, and the alloy liquid is pure; 2) Low energy consumption, high heat efficiency and production efficiency, long service life of a crucible and a furnace lining; 3) The operation is simple, the furnace temperature is convenient to adjust and control, and the working environment is good.
The refractory bricks are mainly used for building smelting furnaces, can resist high temperature of 1580-1770 ℃ and can be divided into baked bricks, unburned bricks, fused bricks (fused cast bricks) and refractory heat-insulating bricks according to a preparation process method; the brick can be divided into standard bricks, ordinary bricks, special bricks and the like according to the shape and the size. Can be used as high-temperature building materials and structural materials of building kilns and various thermal equipment, and can withstand various physical and chemical changes and mechanical actions at high temperature. Such as refractory clay bricks, high alumina bricks, silica bricks, magnesia bricks, and the like.
In the use process of the existing smelting furnace, the internal furnace brick has poor oxidation resistance and is easy to crack and separate, in order to prevent overheat damage of certain parts of the internal furnace brick, water cooling measures are often adopted, and the best material for the water cooling pipe slide rail system is silicon nitride combined with silicon carbide material brick.
Disclosure of Invention
In order to solve the technical problems, the invention provides an antioxidant silicon oxynitride combined silicon carbide brick for a low-oxygen copper rod smelting furnace.
The technical scheme of the invention is as follows: an antioxidation silicon oxynitride combined silicon carbide brick for a low-oxygen copper rod smelting furnace comprises the following components in percentage by weight: 15-20% of silicon oxynitride and 5-8% of alpha-Al 2 O 3 Micro powder, 4-6% of boron nitride powder, 10-15% of silica fume, 4-7% of bonding agent, 1-3% of antioxidant, 0.5-1% of thermal expansion microsphere and the balance of nano silicon carbide;
the preparation method of the silicon oxynitride combined silicon carbide brick comprises the following steps:
s1, mixing raw materials:
silicon oxynitride, alpha-Al 2 O 3 Pretreating micro powder, boron nitride powder, silica fume and an antioxidant, mixing for 30-40 min according to the proportion to obtain a first mixture, weighing nano silicon carbide, a bonding agent and thermal expansion microspheres according to the proportion, adding the nano silicon carbide, the bonding agent and the thermal expansion microspheres into the first mixture, mixing to obtain a second mixture, adding deionized water accounting for 65-70% of the second mixture, stirring for 20-30 min, and trapping the mixture for 35-40 h after stirring to obtain a blank;
s2, sintering and forming:
after the blank obtained in the step S1 is pressed into a green brick, the green brick is sintered and molded through the following steps:
preheating: placing the green bricks into a sintering furnace for preheating to 130-150 ℃, and introducing a L nitrogen during preheating;
wet oxygen temperature rise: raising the temperature of the sintering furnace to 800-900 ℃ at a heating rate of 40-60 ℃/min, and introducing O with certain humidity into the sintering furnace in the heating process 2 And (3) carrying out heat preservation after the temperature rise is finished, wherein the calculation formula of the heat preservation time is as follows:
t＝w(50+T)/0.6a，T∈[800，850] (1)
t＝w|50-T|/0.6a，T∈(850，900] (2)
the temperature of the wet oxygen temperature rise is T, and the unit is DEG C; the heat preservation time is t, and the unit is min; o (O) 2 The humidity of the water is w, the unit is RH, and the value range is 5-10%;
heating by nitrogen burning: raising the temperature of the sintering furnace to 1200-1450 ℃ at a heating rate with the value of 2-3%T, and introducing nitrogen into the sintering furnace in the heating process;
and (3) preserving heat by dry oxygen: preserving heat for 1.6 to 2.0t at 1400 to 1450 ℃ and introducing O without water in the heat preservation process 2 Cooling the green bricks to room temperature along with the furnace after heat preservation is finished;
wherein a is 0.3-0.4; o for wet oxygen heating 2 The inlet amount is 2.0-2.5 a; the nitrogen inlet quantity of nitrogen heating is 1.2-1.4 a; o during heat preservation 2 The inlet amount is 1.6-1.8 a.
Further, the bonding agent is formed by mixing water yeast Liu Fenmo, yellow dextrin, polyvinyl alcohol, liquid phenolic resin and the like in volume; the antioxidant is prepared from blast furnace slag, graphite and sodium stearate according to a volume ratio of 2-3: 1:1, and mixing.
Description: the water yeast Liu Fenmo has good toughness, the yellow dextrin has good effect on preventing collapse and corner and edge protection, the aqueous solution of the polyvinyl alcohol has extremely strong adhesive force on the water yeast willow containing cellulose, the water yeast wood-plastic composite material has the advantages of safety and innocuity, and the phenolic resin modified by the polyvinyl alcohol can be used as an adhesive; the graphite product has chemical stability and corrosion resistance, and the blast furnace slag, graphite and sodium stearate have good oxidation resistance.
Further, the purity of silicon carbide in the nano silicon carbide is more than 90 percent.
Description: the higher the purity of the silicon carbide in the silicon carbide, the less the impurities, the more stable the high temperature resistance of the silicon carbide, the smaller the granularity, the greater the density, the higher the compactness and the better the performance of the silicon carbide.
Further, in step S1, the pretreatment is as follows: ball milling for 45-55 min at 800-1200 r/min, calcining for 4-6 h at 950-1050 ℃, and cooling to room temperature.
Description: the grinding action can be weakened or lost when the rotation speed of the ball milling is too high or too low, the longer the ball milling time is, the more the crushing and extrusion actions on ball milling materials are deepened among ball milling media, the more energy is generated in the ball milling, but the efficiency and the fineness and quality of the materials can be influenced when the rotation speed of the ball milling is too high or too low; the ball is ground into powder and then calcined at high temperature, thereby playing the roles of dehydration and impurity volatilization.
Further, the nano silicon carbide is prepared from 4-6 parts by weight of phenolic resin, 2-4 parts by weight of chitin and 5-25 parts by weight of silicon monoxide.
Description: the phenolic resin pre-chitin is used as a carbon source, and the silicon monoxide is used as a silicon source to prepare the silicon carbide with nanometer granularity, so that the silicon carbide has high porosity, stable chemical property, high heat conductivity coefficient, small thermal expansion coefficient and good wear resistance.
Further, in step S2, the method of pressing the blank into the green brick is as follows: applying pressure at a constant speed of 0.7-0.9 KN/s by using a press, and standing for 6-7 min when the pressure value reaches 15-20 MPa.
Description: too much pressure can easily cause cracking of the material, too little pressure can not achieve the molding effect, and too much or too little pressure can cause damage and deficiency of plasticity of the material.
Further, the thermal expansion microsphere consists of a shell and an inner core, wherein the shell consists of a copolymer of a plurality of vinyl monomers containing one carbon-carbon double bond, and the core layer is a mixture of alkane and polypeptide.
Description: when the microsphere is heated, the internal vaporization or decomposition generates pressure, and the shell layer is softened to generate expansion, if the thermoplasticity of the polymer and the gas pressure generated by high temperature are balanced with each other, a good expansion effect can be obtained, and after cooling, the shell of the polymer does not shrink.
Further, the preparation method of the thermal expansion microsphere comprises the following steps:
1) The mass ratio is 3-5: 1:1:5:2:40, mixing tertiary glycidyl ester, sodium persulfate, 3-sorbitol anhydride monooleate, methyl suberate, calcium carbonate and water, and then mixing and emulsifying for 30-45 min in an ice water bath at the temperature of 2-10 ℃ to obtain a solution to be titrated for later use;
2) The mass ratio of the pre-added materials in the reactor is 20:1 to 3:0.2 of water, isooctane and acetyl hexapeptide-3, stirring and heating to 40-55 ℃ to obtain an alkane mixed solution, and then dropwise adding the to-be-titrated liquid obtained in the step 1) into a reactor, wherein the volume ratio of the to-be-titrated liquid to the alkane mixed solution is 0.2-0.4: 1, starting a stirrer for homogenization after the dripping is finished, wherein the rotating speed of the stirrer is 1500-2500 r/min, the stirring time is 15-25 min, and the heat preservation is carried out for 20-30 min, and then the heat expansion microsphere is obtained through suction filtration and water removal.
Description: the materials are mixed and emulsified under the condition of ice-water bath, so that the volatilization of the materials can be reduced; the polypeptide is mixed with alkane, so that the reduction of alkane content can be inhibited, and the expansion performance of the thermal expansion microsphere is maintained; and through ice water bath emulsification and stirring homogenization, the volume expansion multiple cannot be influenced due to the change of the addition amount of solid particles, and the homogeneity of the microspheres is ensured.
Further, the silicon oxynitride contains 95 to 98% of silicon nitride.
Description: the silicon nitride material has excellent wear resistance, high temperature resistance, corrosion resistance and thermal shock resistance, and the silicon nitride has high content, fine powder and stronger silicon oxynitride.
The beneficial effects of the invention are as follows:
(1) According to the silicon oxynitride-combined silicon carbide brick, siC is added into silicon oxynitride for particle dispersion strengthening, so that not only can the mechanical property better than that of single silicon oxynitride be obtained, but also the high-temperature property of the silicon oxynitride can be further improved; siC particle or whisker pair Si 3 N 4 The matrix material has various strengthening and toughening effects, the fracture toughness is far higher than that of single-phase SiC, and the high temperature resistance, the creep resistance, the high temperature oxidation resistance and the like are far higher than those of single-phase Si 3 N 4 。
(2) The silicon oxynitride-combined silicon carbide brick of the invention is prepared by adding boron nitride and alpha-Al 2 O 3 The micro powder and the antioxidant are doped with a large amount of boron, aluminum or nitrogen in the silicon carbide, so that the doped silicon carbide has conductivity which is in an order of magnitude comparable to that of metal, and the antioxidant can improve the oxidation resistance of the brick; will be heated by the brickWhen heat is transferred to the thermal expansion microsphere, the foaming agent in the thermal expansion microsphere is vaporized or decomposed to generate pressure, and meanwhile, the shell layer is softened to generate a good expansion effect, so that the high-temperature resistance and heat resistance of the inside of the brick can be enhanced.
(3) According to the silicon oxynitride-combined silicon carbide brick, the brick blank is sintered in sections, and nitrogen is filled as a protective atmosphere during preheating so as to facilitate the reaction; the temperature-keeping time is adjusted by oxygen humidity when the wet oxygen is heated, so that the uniform diffusion of silicon monoxide in silicon carbide and the diffusion effect of the silicon carbide in silicon oxynitride can be enhanced, and the high-temperature performance of the brick is improved; and finally, the thermal stability of the green brick is enhanced through dry oxygen heat preservation, so that the silicon nitride combined silicon carbide brick with excellent thermal stability, high temperature resistance and oxidation resistance is obtained.
Detailed Description
The invention will be described in further detail with reference to the following embodiments to better embody the advantages of the invention.
Example 1
An antioxidation silicon oxynitride combined silicon carbide brick for a low-oxygen copper rod smelting furnace comprises the following components in percentage by weight: 18% silicon oxynitride, 6% alpha-Al 2 O 3 Micro powder, 5% of boron nitride powder, 13% of silica fume, 6% of bonding agent, 2% of antioxidant, 0.8% of thermal expansion microsphere and the balance of nano silicon carbide;
the nano silicon carbide is prepared from 5 parts of phenolic resin, 3 parts of chitin and 18 parts of silicon monoxide according to parts by weight, wherein the purity of the silicon carbide in the nano silicon carbide is 95%; the silicon oxynitride contains 96% of silicon nitride; the bonding agent is formed by mixing water yeast Liu Fenmo, yellow dextrin, polyvinyl alcohol, liquid phenolic resin and the like in volume; the antioxidant is prepared from blast furnace slag, graphite and sodium stearate according to a volume ratio of 2.5:1:1, mixing;
the thermal expansion microsphere consists of a shell and an inner core, wherein the shell consists of a plurality of copolymers of vinyl monomers containing one carbon-carbon double bond, and the core layer is a mixture of isooctane and polypeptide; the preparation method of the thermal expansion microsphere comprises the following steps:
1) The mass ratio is 4:1:1:5:2:40, mixing tertiary glycidyl ester, sodium persulfate, 3-sorbitan monooleate, methyl suberate, calcium carbonate and water, and then mixing and emulsifying for 38min in an ice water bath at 6 ℃ to obtain a solution to be titrated for later use;
2) The mass ratio of the pre-added materials in the reactor is 20:2:0.2 of water, isooctane and acetyl hexapeptide-3, stirring and heating to 48 ℃ to obtain an alkane mixed solution, and then dropwise adding the to-be-titrated liquid obtained in the step 1) into a reactor, wherein the volume ratio of the to-be-titrated liquid to the alkane mixed solution is 0.3:1, starting a stirrer for homogenization after the dripping is completed, wherein the rotation speed of the stirrer is 2000r/min, the stirring time is 20min, and filtering out water after heat preservation is carried out for 25min, so as to obtain the thermal expansion microsphere;
the preparation method of the silicon oxynitride combined silicon carbide brick comprises the following steps:
s1, mixing raw materials:
silicon oxynitride, alpha-Al 2 O 3 Pretreating micro powder, boron nitride powder, silica fume and an antioxidant, mixing for 35min according to the proportion to obtain a first mixture, weighing nano silicon carbide, a bonding agent and thermal expansion microspheres according to the proportion, adding the nano silicon carbide, the bonding agent and the thermal expansion microspheres into the first mixture, mixing to obtain a second mixture, adding deionized water accounting for 68% of the total mass of the second mixture, stirring for 25min, and trapping the mixture for 38h after stirring to obtain a blank;
the pretreatment mode is as follows: ball milling for 50min at 1000r/min, calcining for 5h at 1000 ℃, and cooling to room temperature;
s2, sintering and forming:
applying pressure to the blank obtained in the step S1 at a constant speed of 0.8KN/S by using a press machine, standing for 6.5min when the pressure value reaches 18MPa, and sintering and forming the green brick by the following steps:
preheating: placing the green bricks into a sintering furnace for preheating to 140 ℃, and introducing a, namely 0.35L of nitrogen gas during preheating;
wet oxygen temperature rise: raising the temperature of the sintering furnace to 850 ℃ at a heating rate of 50 ℃/min, and guiding the sintering furnace to the temperature during the heating2.3a of O with humidity of 8% RH, namely 0.805L, is introduced into a sintering furnace 2 And (3) carrying out heat preservation after the temperature rise is finished, wherein the calculation formula of the heat preservation time is as follows:
t＝w(50+T)/0.6a (1)
the temperature of the wet oxygen temperature rise is T, and the unit is DEG C; the heat preservation time is t, and the unit is min; o (O) 2 Humidity of w, unit is RH;
substituting t=850 ℃, w=8%, a=0.35 into the formula, and calculating t=343; the heat preservation time is 343min;
heating by nitrogen burning: raising the temperature of the sintering furnace to 1300 ℃ at a heating rate of 21.25 ℃/min with the value of 2.5%T, and introducing 1.3a of 0.455L of nitrogen into the sintering furnace in the heating process;
and (3) preserving heat by dry oxygen: preserving heat at 1425 deg.C for 1.8t or 617min, and introducing 1.7a or 0.595L of anhydrous O 2 And after the heat preservation is finished, cooling the green bricks to room temperature along with the furnace.
Example 2
This example differs from example 1 in that it comprises, by weight, 15% silicon oxynitride, 8% α -Al 2 O 3 Micro powder, 6% of boron nitride powder, 15% of silica fume, 7% of bonding agent, 3% of antioxidant, 1% of thermal expansion microsphere and the balance of nano silicon carbide;
the bonding agent is formed by mixing water yeast Liu Fenmo, yellow dextrin, polyvinyl alcohol, liquid phenolic resin and the like in volume; the antioxidant is prepared from blast furnace slag, graphite and sodium stearate according to a volume ratio of 2:1:1, and mixing.
Example 3
This example differs from example 1 in that it comprises, by weight, 20% silicon oxynitride, 5% α -Al 2 O 3 Micro powder, 4% of boron nitride powder, 10% of silica fume, 4% of bonding agent, 1% of antioxidant, 0.5% of thermal expansion microsphere and the balance of nano silicon carbide;
the bonding agent is formed by mixing water yeast Liu Fenmo, yellow dextrin, polyvinyl alcohol, liquid phenolic resin and the like in volume; the antioxidant is prepared from blast furnace slag, graphite and sodium stearate according to a volume ratio of 3:1:1, and mixing.
Example 4
The embodiment is different from embodiment 1 in that the nano silicon carbide is made of 4 parts of phenolic resin, 2 parts of chitin and 25 parts of silicon monoxide in parts by weight; the silicon oxynitride contained 98% of silicon nitride.
Example 5
The embodiment is different from embodiment 1 in that the nano silicon carbide is made of 6 parts of phenolic resin, 4 parts of chitin and 5 parts of silicon monoxide in parts by weight; the silicon oxynitride contains 95% of silicon nitride.
Example 6
The difference between this embodiment and embodiment 1 is that, in step S1, the pretreatment is as follows: ball milling is carried out for 45min under the condition of 800r/min by a dry method, calcining is carried out for 4h under the condition of 950 ℃ and then cooling is carried out to room temperature.
Example 7
The difference between this embodiment and embodiment 1 is that, in step S1, the pretreatment is as follows: ball milling is carried out for 55min under the condition of 1200r/min, calcining is carried out for 6h under the condition of 1050 ℃ and then cooling is carried out to room temperature.
Example 8
The present embodiment is different from embodiment 1 in that in step S1, the pretreated silicon oxynitride and α -Al are mixed in the above ratio 2 O 3 Mixing the micro powder, the boron nitride powder, the silica fume and the antioxidant for 30min to obtain a first mixture, weighing the nano silicon carbide, the bonding agent and the thermal expansion microsphere according to the proportion, adding the nano silicon carbide, the bonding agent and the thermal expansion microsphere into the first mixture, mixing to obtain a second mixture, adding deionized water accounting for 65% of the total mass of the second mixture, stirring for 20min, and trapping the mixture for 35h after stirring is finished to obtain a blank.
Example 9
The present embodiment is different from embodiment 1 in that in step S1, the pretreated silicon oxynitride and α -Al are mixed in the above ratio 2 O 3 Mixing micropowder, boron nitride powder, silica fume and antioxidant for 40min to obtain a first mixture, and weighing sodium according to the above ratioAdding the rice silicon carbide, the binding agent and the thermal expansion microspheres into the mixture I, mixing to obtain a mixture II, adding deionized water accounting for 70% of the total mass of the mixture II, stirring for 30min, and trapping the mixture for 40h after stirring is finished to obtain a blank.
Example 10
This example differs from example 1 in that in step 1) of the method for producing thermally expandable microspheres, the mass ratio is 3:1:1:5:2:40, sodium persulfate, 3-sorbitan monooleate, methyl suberate, calcium carbonate and water, and mixing and emulsifying for 30min in ice water bath at 10deg.C.
Example 11
This example differs from example 1 in that in step 1) of the method for producing thermally expandable microspheres, the mass ratio is 5:1:1:5:2:40, sodium persulfate, 3-sorbitan monooleate, methyl suberate, calcium carbonate and water, and mixing and emulsifying for 45min in ice water bath at 2deg.C.
Example 12
This example is different from example 1 in that in the preparation method of thermally expanded microspheres in step 2), a mass ratio of 20:1:0.2 of water, isooctane and acetyl hexapeptide-3, stirring and heating to 4 ℃ to obtain an alkane mixed solution, and then dropwise adding the to-be-titrated liquid obtained in the step 1) into a reactor, wherein the volume ratio of the to-be-titrated liquid to the alkane mixed solution is 0.2:1, starting a stirrer for homogenization after the dripping is completed, wherein the rotating speed of the stirrer is 1500r/min, the stirring time is 15min, and filtering out water after heat preservation is carried out for 20min, so that the thermal expansion microsphere is obtained.
Example 13
This example is different from example 1 in that in the preparation method of thermally expanded microspheres in step 2), a mass ratio of 20:3:0.2 of water, isooctane and acetyl hexapeptide-3, stirring and heating to 55 ℃ to obtain an alkane mixed solution, and then dropwise adding the to-be-titrated liquid obtained in the step 1) into a reactor, wherein the volume ratio of the to-be-titrated liquid to the alkane mixed solution is 0.4:1, starting a stirrer for homogenization after the dripping is finished, wherein the rotation speed of the stirrer is 2500r/min, the stirring time is 25min, and filtering out water after heat preservation is carried out for 30min, so that the thermal expansion microsphere is obtained.
Example 14
The present embodiment is different from embodiment 1 in that, in step S2, the blank is pressed into a green brick in the following manner: pressure was applied at a constant speed of 0.7KN/s using a press, and allowed to stand for 6min when the pressure value reached 15 MPa.
Example 15
The present embodiment is different from embodiment 1 in that, in step S2, the blank is pressed into a green brick in the following manner: pressure was applied at a constant speed of 0.9KN/s using a press, and allowed to stand for 7min when the pressure value reached 20 MPa.
Example 16
This embodiment is different from embodiment 1 in that in step S2, preheating: placing the green bricks into a sintering furnace for preheating to 140 ℃, and introducing a, namely 0.3L of nitrogen gas during preheating;
wet oxygen temperature rise: raising the temperature of the sintering furnace to 800 ℃ at a heating rate of 40 ℃/min, and introducing 2.0a, namely 0.6L O with humidity of 5% RH into the sintering furnace in the heating process 2 And (3) carrying out heat preservation after the temperature rise is finished, wherein the calculation formula of the heat preservation time is as follows:
t＝w(50+T)/0.6a (1)
the temperature of the wet oxygen temperature rise is T, and the unit is DEG C; the heat preservation time is t, and the unit is min; o (O) 2 Humidity of w, unit is RH;
substituting t=800 ℃, w=5%, a=0.3 into formula (1), and calculating t=236; the heat preservation time is 236min;
heating by nitrogen burning: raising the temperature of the sintering furnace to 1200 ℃ at a heating rate of 16 ℃/min with the value of 2.0%T, and introducing 1.2a of 0.36L of nitrogen into the sintering furnace in the heating process;
and (3) preserving heat by dry oxygen: maintaining at 1400 deg.C for 1.6t or 378min, and introducing 1.6a or 0.48L of anhydrous O 2 And after the heat preservation is finished, cooling the green bricks to room temperature along with the furnace.
Example 17
This embodiment is different from embodiment 1 in that in step S2, preheating: placing the green bricks into a sintering furnace for preheating to 150 ℃, and introducing a, namely 0.4L of nitrogen gas during preheating;
wet oxygen temperature rise: raising the temperature of the sintering furnace to 900 ℃ at a heating rate of 60 ℃/min, and introducing 2.5a, namely 1L of O with humidity of 10% RH into the sintering furnace in the heating process 2 And (3) carrying out heat preservation after the temperature rise is finished, wherein the calculation formula of the heat preservation time is as follows:
t＝w|50-T|/0.6a (2)
the temperature of the wet oxygen temperature rise is T, and the unit is DEG C; the heat preservation time is t, and the unit is min; o (O) 2 Humidity of w, unit is RH;
substituting t=900 ℃, w=10%, a=0.4 into formula (2), and calculating t=354; the heat preservation time is 354min;
heating by nitrogen burning: raising the temperature of the sintering furnace to 1450 ℃ at a heating rate of 27 ℃/min with a value of 3%T, and introducing 1.4a, namely 0.56L of nitrogen into the sintering furnace in the heating process;
and (3) preserving heat by dry oxygen: preserving heat at 1450 deg.C for 1.8t or 637min, and introducing 1.8a or 0.72L of anhydrous O 2 And after the heat preservation is finished, cooling the green bricks to room temperature along with the furnace.
Experimental example
For the silicon oxynitride-bonded silicon carbide bricks prepared in each example, 5 samples of each example were taken to test the properties of the silicon oxynitride-bonded silicon carbide bricks, and the property measurements of the 5 samples of each example were averaged to give the property measurement of the example, which was specifically studied as follows:
1. the influence of the component proportion of the brick and the preparation parameters of the brick on the oxidation resistance and the high-temperature compressive strength of the silicon oxynitride-combined silicon carbide brick is explored, and the oxidation resistance is expressed by the total area ratio of the oxidation area.
The results of the experiment were shown in Table 1, using examples 1 to 17 and comparative examples 1 to 3 as experimental comparisons:
table 1 effects of examples and comparative examples on oxidation resistance (%) and high temperature (1200 ℃) compressive strength (MPa) of silicon oxynitride-bonded silicon carbide bricks
Comparative example 1 differs from example 1 in that the thermally expansive microspheres are not included in the composition of the silicon oxynitride-bonded silicon carbide brick;
comparative example 2 is different from example 1 in that the humidity of oxygen does not change throughout the sintering molding;
comparative example 3 differs from example 1 in that the holding time for sample temperature rise was adjusted only with the temperature rise;
as can be seen from the results in table 1, the thermal expansion microspheres lack in comparative example 1, the oxygen humidity lack in comparative example 2, and the humidity lack in comparative example 3, and the temperature rise of wet oxygen lack in comparative example 3, the oxidation resistance and the high-temperature compressive strength of the prepared silicon oxynitride-bonded silicon carbide brick are both remarkably reduced, which indicates that the different introduction of the thermal expansion microspheres, wet oxygen and dry oxygen and the temperature rise of wet oxygen have an influence on the silicon oxynitride-bonded silicon carbide brick;
and comparing examples 1-18, it is known that the silicon oxynitride-bonded silicon carbide brick has too much or too little silicon carbide, the silicon component in nano silicon carbide and the silicon nitride in silicon oxynitride have too much or too little silicon nitride component, the higher or lower the pretreatment speed and temperature, the longer or too slow ball milling time and calcination time can reduce the oxidation resistance and high temperature compressive strength of the silicon oxynitride-bonded silicon carbide brick; the mixing time, the synthesis rotating speed and other factors in the thermal expansion microsphere have smaller influence than other factors; the pressure intensity of the pressed blank is too large or too small, the sintering temperature is too high or too low, the nitrogen gas and oxygen gas are introduced too much or too little, and the heat preservation time is too long or too short, so that the oxidation resistance and the high-temperature compressive strength of the silicon oxynitride combined silicon carbide brick can be reduced;
therefore, the parameters of example 1 are relatively better from a cost and economic standpoint.
Claims (7)
1. An antioxidation silicon oxynitride combined silicon carbide brick for a low-oxygen copper rod smelting furnace is characterized by comprising the following components in percentage by weightThe weight percentage comprises: 15-20% of silicon oxynitride and 5-8% of alpha-Al 2 O 3 Micro powder, 4-6% of boron nitride powder, 10-15% of silica fume, 4-7% of bonding agent, 1-3% of antioxidant, 0.5-1% of thermal expansion microsphere and the balance of nano silicon carbide;
the thermal expansion microsphere consists of a shell and an inner core, wherein the shell consists of a copolymer of a plurality of vinyl monomers containing one carbon-carbon double bond, and the core layer is a mixture of alkane and polypeptide;
the preparation method of the thermal expansion microsphere comprises the following steps:
1) The mass ratio is 3-5: 1:1:5:2:40, mixing tertiary glycidyl ester, sodium persulfate, sorbitan monooleate, methyl suberate, calcium carbonate and water, and then mixing and emulsifying for 30-45 min in an ice water bath at 2-10 ℃ to obtain a solution to be titrated for later use;
2) The mass ratio of the pre-added materials in the reactor is 20: 1-3: 0.2 of water, isooctane and acetyl hexapeptide-3, stirring and heating to 40-55 ℃ to obtain an alkane mixed solution, and then dropwise adding the to-be-titrated liquid obtained in the step 1) into a reactor, wherein the volume ratio of the to-be-titrated liquid to the alkane mixed solution is 0.2-0.4: 1, starting a stirrer for homogenization after the dripping is completed, wherein the rotation speed of the stirrer is 1500-2500 r/min, the stirring time is 15-25 min, and the heat preservation is carried out for 20-30 min, and then water is removed by suction filtration, so that the thermal expansion microsphere is obtained;
the preparation method of the silicon oxynitride combined silicon carbide brick comprises the following steps:
s1, mixing raw materials:
silicon oxynitride, alpha-Al 2 O 3 Pretreating micro powder, boron nitride powder, silica fume and an antioxidant, mixing for 30-40 min according to the proportion to obtain a first mixture, weighing nano silicon carbide, a bonding agent and thermal expansion microspheres according to the proportion, adding the nano silicon carbide, the bonding agent and the thermal expansion microspheres into the first mixture, mixing to obtain a second mixture, adding deionized water accounting for 65-70% of the total mass of the second mixture, stirring for 20-30 min, and trapping the mixture for 35-40 h after stirring to obtain a blank;
s2, sintering and forming:
after the blank obtained in the step S1 is pressed into a green brick, the green brick is sintered and molded through the following steps:
preheating: placing the green bricks into a sintering furnace for preheating to 130-150 ℃, and introducing a L nitrogen during preheating;
wet oxygen temperature rise: raising the temperature of the sintering furnace to 800-900 ℃ at a heating rate of 40-60 ℃/min, and introducing O with certain humidity into the sintering furnace in the heating process 2 And (3) carrying out heat preservation after the temperature rise is finished, wherein the calculation formula of the heat preservation time is as follows:
（1）
（2）
the temperature of the wet oxygen temperature rise is T, and the unit is DEG C; the heat preservation time is t, and the unit is min; o (O) 2 The humidity of the water is w, the unit is RH, and the value range is 5-10%;
heating by nitrogen burning: raising the temperature of the sintering furnace to 1200-1450 ℃ at a heating rate with the value of 2-3%T, and introducing nitrogen into the sintering furnace in the heating process;
and (3) preserving heat by dry oxygen: preserving heat for 1.6-2.0 t at 1400-1450 ℃, and introducing O without water in the heat preservation process 2 Cooling the green bricks to room temperature along with the furnace after heat preservation is finished;
wherein a is 0.3-0.4; o for wet oxygen heating 2 The inlet amount is 2.0-2.5 a; the nitrogen gas inlet amount for nitrogen burning and heating is 1.2-1.4a; o during heat preservation 2 The inlet amount is 1.6-1.8 a.
2. The antioxidation silicon oxynitride combined silicon carbide brick for a low-oxygen copper rod smelting furnace according to claim 1, wherein the bonding agent is formed by mixing water yeast Liu Fenmo, yellow dextrin, polyvinyl alcohol, liquid phenolic resin and the like in volume; the antioxidant is prepared from blast furnace slag, graphite and sodium stearate according to a volume ratio of 2-3: 1:1, and mixing.
3. An oxidation resistant silicon oxynitride bonded silicon carbide brick for use in a low oxygen copper rod melting furnace according to claim 1, wherein the purity of silicon carbide in said nano silicon carbide is > 90%.
4. An antioxidation silicon oxynitride combined silicon carbide brick for a low oxygen copper rod smelting furnace according to claim 1, wherein in step S1, the pretreatment is as follows: ball milling is carried out for 45-55 min under the condition of 800-1200 r/min, calcining is carried out for 4-6 h under the condition of 950-1050 ℃, and then cooling is carried out to room temperature.
5. The antioxidation silicon oxynitride combined silicon carbide brick for a low-oxygen copper rod smelting furnace according to claim 1, wherein the nano silicon carbide is prepared from 4-6 parts by weight of phenolic resin, 2-4 parts by weight of chitin and 5-25 parts by weight of silicon monoxide.
6. An oxidation resistant silicon oxynitride bonded silicon carbide brick for use in a low oxygen copper rod melting furnace according to claim 1, wherein in step S2, said blank is pressed into green bricks by: and applying pressure at a constant speed of 0.7-0.9 KN/s by using a press, and standing for 6-7 min when the pressure value reaches 15-20 MPa.
7. The antioxidation silicon oxynitride-bonded silicon carbide brick for a low-oxygen copper rod smelting furnace according to claim 1, wherein the silicon oxynitride contains 95-98% of silicon nitride.
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