CN117645466B - Magnesium carbonaceous castable and preparation method thereof - Google Patents
Magnesium carbonaceous castable and preparation method thereof Download PDFInfo
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- CN117645466B CN117645466B CN202410121489.1A CN202410121489A CN117645466B CN 117645466 B CN117645466 B CN 117645466B CN 202410121489 A CN202410121489 A CN 202410121489A CN 117645466 B CN117645466 B CN 117645466B
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- butoxycarboxylic
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 239000011777 magnesium Substances 0.000 title claims abstract description 9
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 84
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 60
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 48
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 42
- -1 butoxycarboxylic acid modified carbon Chemical class 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 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 16
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 16
- 239000011230 binding agent Substances 0.000 claims abstract description 5
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 5
- MCORDGVZLPBVJB-UHFFFAOYSA-N 2-(2-butoxyethoxy)acetic acid Chemical compound CCCCOCCOCC(O)=O MCORDGVZLPBVJB-UHFFFAOYSA-N 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 16
- LAUFPZPAKULAGB-UHFFFAOYSA-N 4-butoxybenzoic acid Chemical compound CCCCOC1=CC=C(C(O)=O)C=C1 LAUFPZPAKULAGB-UHFFFAOYSA-N 0.000 claims description 15
- 229910002804 graphite Inorganic materials 0.000 claims description 15
- 239000010439 graphite Substances 0.000 claims description 15
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 15
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 14
- DFFDSQBEGQFJJU-UHFFFAOYSA-N butyl hydrogen carbonate Chemical compound CCCCOC(O)=O DFFDSQBEGQFJJU-UHFFFAOYSA-N 0.000 claims description 13
- 239000006229 carbon black Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 238000005266 casting Methods 0.000 claims description 4
- 229910021487 silica fume Inorganic materials 0.000 claims description 4
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 4
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 4
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 claims 1
- 239000011819 refractory material Substances 0.000 abstract description 4
- RWDBMHZWXLUGIB-UHFFFAOYSA-N [C].[Mg] Chemical compound [C].[Mg] RWDBMHZWXLUGIB-UHFFFAOYSA-N 0.000 abstract 1
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N dimethyl sulfoxide Natural products CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 31
- 238000010438 heat treatment Methods 0.000 description 11
- 238000001035 drying Methods 0.000 description 10
- 238000001914 filtration Methods 0.000 description 10
- 238000005406 washing Methods 0.000 description 10
- 239000002245 particle Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 241000872198 Serjania polyphylla Species 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000012615 aggregate Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 125000004106 butoxy group Chemical group [*]OC([H])([H])C([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Ceramic Products (AREA)
Abstract
The invention relates to the technical field of refractory materials, and provides a magnesia carbon castable and a preparation method thereof. The magnesium carbonaceous castable comprises the following components in parts by mass: 70-90 parts of magnesia, 6-12 parts of butoxycarboxylic acid modified carbon, 3-8 parts of silicon carbide, 1-5 parts of alumina micropowder, 3-5 parts of binding agent and 0.1-1 part of water reducer. By the technical scheme, the problems of poor compactness and low strength of the finished product of the magnesium-carbon castable in the prior art are solved.
Description
Technical Field
The invention relates to the technical field of refractory materials, in particular to a magnesia carbon castable and a preparation method thereof.
Background
The refractory castable is a pug which is formed by mixing refractory aggregate, binding agent and additive, and then adding water to blend into the pug which can be constructed by a casting method. Compared with other unshaped refractory materials, the refractory castable has certain setting and hardening time after construction, so that the castable can be demolded after being subjected to maintenance for a certain time after casting molding, and then can be put into baking after natural maintenance. The refractory castable is an unshaped refractory material which is most widely produced and used at present, and is mainly used for constructing various integral structures such as heating furnace linings, and the like, wherein the magnesia carbon castable is mainly used for smelting furnaces eroded by alkaline slag.
At present, carbon is mainly introduced into the magnesium carbonaceous castable by adding carbon-containing substances such as graphite and carbon black, but the wettability of the carbon and water is poor, so that the water addition amount in the casting process is increased, and the final finished product has poor compactness and low strength.
Disclosure of Invention
The invention provides a magnesia carbon castable and a preparation method thereof, which solve the problems of poor compactness and low strength of finished magnesia carbon castable products in the related technology.
The technical scheme of the invention is as follows:
the magnesium carbonaceous castable comprises the following components in parts by mass: 70-90 parts of magnesia, 6-12 parts of butoxycarboxylic acid modified carbon, 3-8 parts of silicon carbide, 1-5 parts of alumina micropowder, 3-5 parts of binding agent and 0.1-1 part of water reducer.
As a further technical scheme, the raw materials of the butoxycarboxylic acid modified carbon comprise carbon and butoxycarboxylic acid in a mass ratio of 1:0.3-0.5.
As a further technical scheme, the carbon comprises one or two of graphite and carbon black.
As a further technical scheme, the butoxycarboxylic acid comprises one or two of (2-n-butoxyethoxy) acetic acid and 4-butoxybenzoic acid.
As a further technical scheme, the butoxycarboxylic acid comprises 4-butoxybenzoic acid and (2-n-butoxyethoxy) acetic acid in a mass ratio of 1:4-3:2.
As a further technical scheme, the butoxycarboxylic acid comprises 4-butoxybenzoic acid and (2-n-butoxyethoxy) acetic acid in a mass ratio of 2:3.
As a further technical scheme, the preparation method of the butoxycarboxylic acid modified carbon comprises the following steps: mixing carbon, butoxycarboxylic acid and solvent, and reacting to obtain butoxycarboxylic acid modified carbon.
As a further technical scheme, the solvent is dimethyl sulfoxide.
As a further technical scheme, the reaction temperature is 100-120 ℃, and the reaction time is 1-3 h.
As a further technical scheme, the bonding agent comprises one or two of silica fume and silica sol.
As a further technical scheme, the water reducer comprises one or two of sodium tripolyphosphate and sodium hexametaphosphate.
The invention also provides a preparation method of the magnesia carbon castable, which comprises the following steps: and uniformly mixing the components in parts by mass to obtain the magnesia carbon castable.
The working principle and the beneficial effects of the invention are as follows:
1. the invention adopts butoxycarboxylic acid to modify carbon, and utilizes the reaction of the butoxy in the butoxycarboxylic acid and the hydroxyl on the carbon surface to endow the carbon surface with oxygen-containing functional groups: ether bond and carboxyl, oxygen-containing functional group is easy to form hydrogen bond with water molecule and hydrophilic, thus improving the wettability of carbon and water, and achieving the technical effect of improving the compactness and compressive strength of the finished product of the magnesium carbonaceous castable.
2. According to the invention, the butoxycarboxylic acid is limited to 4-butoxybenzoic acid and (2-n-butoxyethoxy) acetic acid modified carbon with a mass ratio of 1:4-3:2, so that the compactness and the compressive strength of a finished product of the magnesia carbon castable are further improved. The 4-butoxybenzoic acid contains a rigid benzene ring structure, but the benzene ring has larger steric hindrance and can influence the modification effect; while (2-n-butoxyethoxy) acetic acid has good modification effect, the molecular structure of the (2-n-butoxyethoxy) acetic acid is flexible relative to that of 4-butoxybenzoic acid, so that the compactness and the compressive strength of a magnesium carbonaceous castable finished product obtained by modifying carbon with the 4-butoxybenzoic acid and the (2-n-butoxyethoxy) acetic acid are better than those of the carbon modified with the 4-butoxybenzoic acid or the (2-n-butoxyethoxy) acetic acid alone.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the following examples and comparative examples:
the magnesia is sintered magnesia which consists of particles with the particle size of less than or equal to 5mm and 3mm and particles with the particle size of less than or equal to 3mm and 1mm and particles with the particle size of less than or equal to 1mm and 0 mm and less than or equal to 1mm in the mass ratio of 1:1:2;
the graphite is 200-mesh flake graphite and has a carbon content of 75wt%;
the granularity of the silicon carbide is 200 meshes, and the SiC content is more than or equal to 98wt%;
alumina powder of 2 μm alumina powder, al 2 O 3 The content is more than or equal to 99.8 weight percent, fe 2 O 3 The content is less than or equal to 0.03 weight percent, siO 2 The content is less than or equal to 0.10wt%;
the silica sol is alkaline silica sol with the solid content of 30 wt%;
the micro silicon powder is 200 meshes, and the silicon content is more than or equal to 95wt%;
the carbon black is metallurgical carbon black with the particle diameter of 20nm, and the purity is more than or equal to 99.9wt%;
the sodium tripolyphosphate is industrial grade sodium tripolyphosphate, the content is more than or equal to 95wt%, and the granularity is 200 meshes.
Example 1
S1, dissolving 1.5g of (2-n-butoxyethoxy) acetic acid in 300mL of DMSO, adding 15g of graphite, heating to 110 ℃ for reaction for 2 hours, filtering, washing with water, and drying to obtain butoxycarboxylic acid modified carbon;
and S2, uniformly mixing 80 parts of magnesia, 9 parts of butoxycarboxylic acid modified carbon, 5 parts of silicon carbide, 3 parts of alumina micropowder, 4.5 parts of silica sol and 0.5 part of sodium tripolyphosphate to obtain the magnesia carbon castable.
Example 2
S1, dissolving 1.5g of (2-n-butoxyethoxy) acetic acid in 300mL of DMSO, adding 15g of graphite, heating to 100 ℃ for reaction for 3 hours, filtering, washing with water, and drying to obtain butoxycarboxylic acid modified carbon;
s2, uniformly mixing 70 parts of magnesia, 6 parts of butoxycarboxylic acid modified carbon, 3 parts of silicon carbide, 1 part of alumina micropowder, 1 part of silica fume, 2 parts of silica sol and 0.1 part of sodium hexametaphosphate to obtain the magnesia carbon castable.
Example 3
S1, dissolving 1.5g of (2-n-butoxyethoxy) acetic acid in 300mL of DMSO, adding 15g of carbon black, heating to 120 ℃ for reaction for 1h, filtering, washing with water, and drying to obtain butoxycarboxylic acid modified carbon;
s2, uniformly mixing 90 parts of magnesia, 12 parts of butoxycarboxylic acid modified carbon, 8 parts of silicon carbide, 5 parts of alumina micropowder, 1.5 parts of silica fume, 3.5 parts of silica sol, 0.5 part of sodium tripolyphosphate and 0.5 part of sodium hexametaphosphate to obtain the magnesia carbon castable.
Example 4
S1, dissolving 4.5g of (2-n-butoxyethoxy) acetic acid in 300mL of DMSO, adding 15g of graphite, heating to 110 ℃ for reaction for 2 hours, filtering, washing with water, and drying to obtain butoxycarboxylic acid modified carbon;
and S2, uniformly mixing 80 parts of magnesia, 9 parts of butoxycarboxylic acid modified carbon, 5 parts of silicon carbide, 3 parts of alumina micropowder, 4.5 parts of silica sol and 0.5 part of sodium tripolyphosphate to obtain the magnesia carbon castable.
Example 5
S1, dissolving 7.5g of (2-n-butoxyethoxy) acetic acid in 300mL of DMSO, adding 15g of graphite, heating to 110 ℃ for reaction for 2 hours, filtering, washing with water, and drying to obtain butoxycarboxylic acid modified carbon;
and S2, uniformly mixing 80 parts of magnesia, 9 parts of butoxycarboxylic acid modified carbon, 5 parts of silicon carbide, 3 parts of alumina micropowder, 4.5 parts of silica sol and 0.5 part of sodium tripolyphosphate to obtain the magnesia carbon castable.
Example 6
S1, dissolving 10g of (2-n-butoxyethoxy) acetic acid in 300mL of DMSO, adding 15g of graphite, heating to 110 ℃ for reaction for 2h, filtering, washing with water, and drying to obtain butoxycarboxylic acid modified carbon;
and S2, uniformly mixing 80 parts of magnesia, 9 parts of butoxycarboxylic acid modified carbon, 5 parts of silicon carbide, 3 parts of alumina micropowder, 4.5 parts of silica sol and 0.5 part of sodium tripolyphosphate to obtain the magnesia carbon castable.
Example 7
S1, dissolving 7.5g of 4-butoxybenzoic acid in 300mL of DMSO, adding 15g of graphite, heating to 110 ℃ for reaction for 2 hours, filtering, washing with water, and drying to obtain butoxycarboxylic acid modified carbon;
and S2, uniformly mixing 80 parts of magnesia, 9 parts of butoxycarboxylic acid modified carbon, 5 parts of silicon carbide, 3 parts of alumina micropowder, 4.5 parts of silica sol and 0.5 part of sodium tripolyphosphate to obtain the magnesia carbon castable.
Example 8
S1, dissolving 1.5g of 4-butoxybenzoic acid, (2-n-butoxyethoxy) acetic acid and 6g of (2-n-butoxyethoxy) acetic acid in 300mL of DMSO, adding 15g of graphite, heating to 110 ℃ for reaction for 2 hours, filtering, washing with water, and drying to obtain butoxycarboxylic acid modified carbon;
and S2, uniformly mixing 80 parts of magnesia, 9 parts of butoxycarboxylic acid modified carbon, 5 parts of silicon carbide, 3 parts of alumina micropowder, 4.5 parts of silica sol and 0.5 part of sodium tripolyphosphate to obtain the magnesia carbon castable.
Example 9
S1, dissolving 3g of 4-butoxybenzoic acid, (2-n-butoxyethoxy) acetic acid and 4.5g of (2-n-butoxyethoxy) acetic acid in 300mL of DMSO, adding 15g of graphite, heating to 110 ℃ for reaction for 2h, filtering, washing with water, and drying to obtain butoxycarboxylic acid modified carbon;
and S2, uniformly mixing 80 parts of magnesia, 9 parts of butoxycarboxylic acid modified carbon, 5 parts of silicon carbide, 3 parts of alumina micropowder, 4.5 parts of silica sol and 0.5 part of sodium tripolyphosphate to obtain the magnesia carbon castable.
Example 10
S1, dissolving 4.5g of 4-butoxybenzoic acid and 3g of (2-n-butoxyethoxy) acetic acid in 300mL of DMSO, adding 15g of graphite, heating to 110 ℃ for reaction for 2 hours, filtering, washing with water, and drying to obtain butoxycarboxylic acid modified carbon;
and S2, uniformly mixing 80 parts of magnesia, 9 parts of butoxycarboxylic acid modified carbon, 5 parts of silicon carbide, 3 parts of alumina micropowder, 4.5 parts of silica sol and 0.5 part of sodium tripolyphosphate to obtain the magnesia carbon castable.
Comparative example 1
And uniformly mixing 80 parts of magnesia, 9 parts of graphite, 5 parts of silicon carbide, 3 parts of alumina micropowder, 4.5 parts of silica sol and 0.5 part of sodium tripolyphosphate to obtain the magnesia carbon castable.
The magnesia carbon castable obtained in examples 1 to 10 and comparative example 1 was added with water accounting for 4% of the total mass of the castable, stirred uniformly, poured into a mold, subjected to vibration molding, cured and baked at 110 ℃ for 24 hours, tested for bulk density by referring to the hydrostatic weighing method of YB/T5200-93, the method of GB/T5072-2008, the method of refractory normal temperature compressive strength test, and the test results recorded in Table 1.
TABLE 1 bulk Density and compressive Strength
As can be seen from Table 1, the volume density of the finished product obtained by the magnesia carbon castable provided by the invention is 3.04g/cm 3 The compressive strength is above 59.0MPa, and the high compactness and compressive strength are achieved.
Examples 1 to 10 compared with comparative example 1, the butoxycarboxylic acid was used to modify the carbon in examples 1 to 10, and the carbon was not modified in comparative example 1, and the bulk density and compressive strength of the finished magnesia-carbon castable obtained in examples 1 to 10 were higher than those of comparative example 1, indicating that the wettability of the carbon with water can be improved by modifying the carbon with butoxycarboxylic acid, thereby improving the compactness and compressive strength of the finished magnesia-carbon castable.
Compared with examples 1-7, examples 8-10 use 4-butoxybenzoic acid and (2-n-butoxyethoxy) acetic acid modified carbon in a mass ratio of 1:4-3:2 in examples 8-10, use (2-n-butoxyethoxy) acetic acid modified carbon in examples 1-6, use 4-butoxybenzoic acid modified carbon in example 7, and the bulk density and compressive strength of the finished product of the magnesia carbon castable obtained in examples 8-10 are higher than those of examples 1-7, which means that the compactness and compressive strength of the finished product of the magnesia carbon castable can be further improved by using 4-butoxybenzoic acid and (2-n-butoxyethoxy) acetic acid modified carbon in a mass ratio of 1:4-3:2.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (4)
1. The magnesium carbonaceous castable is characterized by comprising the following components in parts by mass: 70-90 parts of magnesia, 6-12 parts of butoxycarboxylic acid modified carbon, 3-8 parts of silicon carbide, 1-5 parts of alumina micropowder, 3-5 parts of binding agent and 0.1-1 part of water reducer;
the raw materials of the butoxycarboxylic acid modified carbon comprise carbon and butoxycarboxylic acid in a mass ratio of 1:0.3-0.5;
the carbon comprises one or two of graphite and carbon black;
the butoxycarboxylic acid comprises 4-butoxybenzoic acid and (2-n-butoxyethoxy) acetic acid in a mass ratio of 1:4-3:2;
the preparation method of the butoxycarboxylic acid modified carbon comprises the following steps: mixing carbon, butoxycarboxylic acid and a solvent, and reacting to obtain butoxycarboxylic acid modified carbon;
the reaction temperature is 100-120 ℃, and the reaction time is 1-3 h.
2. The magnesia carbon castable according to claim 1, wherein the binder comprises one or both of silica fume and silica sol.
3. The magnesium carbonaceous casting material according to claim 1, wherein the water reducing agent comprises one or both of sodium tripolyphosphate and sodium hexametaphosphate.
4. A method for preparing a magnesia carbon castable according to any one of claims 1 to 3, comprising the steps of: and uniformly mixing the components in parts by mass to obtain the magnesia carbon castable.
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