CN117585987A - 一种中间包涂抹料及其制备方法 - Google Patents
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- 239000011248 coating agent Substances 0.000 title claims abstract description 32
- 238000000576 coating method Methods 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000000463 material Substances 0.000 title description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000000835 fiber Substances 0.000 claims abstract description 54
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000440 bentonite Substances 0.000 claims abstract description 15
- 229910000278 bentonite Inorganic materials 0.000 claims abstract description 15
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 15
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 5
- 239000007767 bonding agent Substances 0.000 claims abstract description 4
- MXJFARPIWAGEAP-UHFFFAOYSA-N 4-[4-(hydroxymethyl)phenyl]benzenesulfonic acid Chemical compound C1=CC(CO)=CC=C1C1=CC=C(S(O)(=O)=O)C=C1 MXJFARPIWAGEAP-UHFFFAOYSA-N 0.000 claims description 16
- 238000002156 mixing Methods 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
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 239000003607 modifier Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 7
- 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
- HNUWDURNWORUHQ-UHFFFAOYSA-N 2-amino-5-hydroxy-4,4-bis(hydroxymethyl)pentane-2-sulfonic acid Chemical compound OCC(CC(S(=O)(=O)O)(N)C)(CO)CO HNUWDURNWORUHQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000005995 Aluminium silicate Substances 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- PZZYQPZGQPZBDN-UHFFFAOYSA-N aluminium silicate Chemical compound O=[Al]O[Si](=O)O[Al]=O PZZYQPZGQPZBDN-UHFFFAOYSA-N 0.000 claims 1
- 229910000323 aluminium silicate Inorganic materials 0.000 claims 1
- 235000012211 aluminium silicate Nutrition 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 239000011819 refractory material Substances 0.000 abstract description 5
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 35
- 229940092782 bentonite Drugs 0.000 description 13
- 229920000049 Carbon (fiber) Polymers 0.000 description 12
- 239000004917 carbon fiber Substances 0.000 description 12
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 12
- 238000001035 drying Methods 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 10
- 238000005406 washing Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 239000002245 particle Substances 0.000 description 6
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 5
- 238000006703 hydration reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000036571 hydration Effects 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000009749 continuous casting Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- DBEDTBJGEXDPBT-UHFFFAOYSA-N 1-amino-4-hydroxy-3,3-bis(hydroxymethyl)butane-1-sulfonic acid Chemical compound OS(=O)(=O)C(N)CC(CO)(CO)CO DBEDTBJGEXDPBT-UHFFFAOYSA-N 0.000 description 1
- GLOZHJZEJIXYLM-UHFFFAOYSA-N 4-hydroxy-3,3-bis(hydroxymethyl)-1-(methylamino)butane-1-sulfonic acid Chemical compound OCC(CC(S(=O)(=O)O)NC)(CO)CO GLOZHJZEJIXYLM-UHFFFAOYSA-N 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- ONCZQWJXONKSMM-UHFFFAOYSA-N dialuminum;disodium;oxygen(2-);silicon(4+);hydrate Chemical group O.[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Na+].[Na+].[Al+3].[Al+3].[Si+4].[Si+4].[Si+4].[Si+4] ONCZQWJXONKSMM-UHFFFAOYSA-N 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- -1 oxygen ions Chemical class 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009467 reduction Effects 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
- 229940080314 sodium bentonite Drugs 0.000 description 1
- 229910000280 sodium bentonite Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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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
- C04B35/03—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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
- C04B35/04—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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
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Abstract
本发明涉及耐火材料技术领域，提出了一种中间包涂抹料及其制备方法。一种中间包涂抹料，包括以下质量份的组分：镁砂60~80份、磺酸化纤维2~5份、结合剂2~5份、碳化硅3~8份、膨润土1~3份、减水剂0.1~1份。通过上述技术方案，解决了现有技术中的镁质中间包涂抹料的镁砂易水化的问题。
Description
技术领域
本发明涉及耐火材料技术领域，具体的，涉及一种中间包涂抹料及其制备方法。
背景技术
中间包简称中包，是连铸工艺流程中位于钢包与结晶器之间的过渡容器，用于接收钢包浇铸的钢水，起着减压、稳流、去渣、储钢、分流等作用。在现代连铸的应用和发展过程中，中间包的作用显得越来越重要。
中间包涂抹料是涂抹在中间包永久层的表面上作为工作衬的涂料，是由细耐火骨料、粉料、结合剂混合而成，然后在施工过程中加入水搅拌成可涂抹的不定形耐火材料，多呈膏状或泥浆状，再用手工或机械方法涂抹或喷涂在工作表面。其中，应用最多的就是镁质中间包涂抹料，但是镁砂在遇到水时会发生水化反应，由于镁砂水化生成的氢氧化镁脱水而失去胶结作用，耐火骨料和粉料的结合很松弛，固相反应又很弱，致使中间包涂抹料的强度急剧下降，易发生疏松，剥落的现象。
发明内容
本发明提出一种中间包涂抹料及其制备方法，解决了相关技术中的镁质中间包涂抹料的镁砂易水化的问题。
本发明的技术方案如下：
一种中间包涂抹料，包括以下质量份的组分：镁砂60~80份、磺酸化纤维2~5份、结合剂2~5份、碳化硅3~8份、膨润土1~3份、减水剂0.1~1份。
作为进一步的技术方案，所述磺酸化纤维为经改性剂改性的纤维；
所述改性剂包括4’-(羟基甲基)-4-联苯基磺酸、三羟甲基甲胺基丙磺酸中的一种或两种。
作为进一步的技术方案，所述纤维包括硅酸铝纤维、碳纤维中的一种或两种。
作为进一步的技术方案，所述磺酸化纤维的原料包括质量比为1:0.3~0.8的纤维和改性剂。
本发明将磺酸化纤维的原料限定为质量比1:0.3~0.8的纤维和改性剂，进一步提高了中间包涂抹料的致密性和强度。
作为进一步的技术方案，所述磺酸化纤维的原料包括质量比为1:0.5的纤维和改性剂。
作为进一步的技术方案，所述磺酸化纤维的制备方法包括以下步骤：将纤维、改性剂和溶剂混合，进行反应，得到磺酸化纤维。
作为进一步的技术方案，所述反应的温度为145~160℃，时间为20~40min。
作为进一步的技术方案，所述镁砂与磺酸化纤维的质量比为70:3~4。
本发明将镁砂与磺酸化纤维的质量比优化为70:3~4，进一步提高了中间包涂抹料的致密性和强度。这是因为随着磺酸化纤维的用量增加，镁砂的水化效果逐渐被改善，但磺酸化纤维过量时，易分散不均、团聚成球，从而导致中间包涂抹料致密性和强度下降。
作为进一步的技术方案，所述结合剂包括微硅粉、硅溶胶中的一种或两种。
作为进一步的技术方案，所述减水剂包括三聚磷酸钠、六偏磷酸钠中的一种或两种。
本发明还提出了一种中间包涂抹料的制备方法，包括以下步骤：将所述质量份的组分混合均匀，得到中间包涂抹料。
本发明的工作原理及有益效果为：
本发明中磺酸化纤维的表面含有磺酸基，在施工过程中提供了大量的未键合的氧离子，被镁砂中MgO表面的镁离子吸附，减少了OH-基团，很大程度上削弱了镁砂的水化，解决了相关技术中的镁质中间包涂抹料的镁砂易水化的问题，达到了提高中间包涂抹料致密性和强度的效果。
具体实施方式
下面将结合本发明实施例，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都涉及本发明保护的范围。
以下实施例及对比例中：
镁砂为烧结镁砂由质量比1:1:2的3mm＜粒径≤5mm颗粒、1mm＜粒径≤3mm颗粒、0＜粒径≤1mm颗粒组成；
碳化硅为200目碳化硅粉，铝含量90wt%，Fe2O3≤2wt%；
硅溶胶为固含量30wt%的碱性硅溶胶；
微硅粉为200目，硅含量≥95wt%；
三聚磷酸钠为工业级三聚磷酸钠，含量≥95%，粒度200目；
膨润土为200目的钠基膨润土；
硅酸铝纤维的直径为2~5μm、长度为8mm；
碳纤维的直径为12μm，长度为5mm；
DMSO为二甲基亚砜。
实施例1
S1、将4’-(羟基甲基)-4-联苯基磺酸0.5g溶于DMSO 150mL，加入碳纤维5g升温至150℃反应30min，水洗，干燥，得到磺酸化纤维；
S2、将镁砂70份、磺酸化纤维2份、硅溶胶3.5份、碳化硅5份、膨润土2份、三聚磷酸钠0.5份混合均匀，得到中间包涂抹料。
实施例2
S1、将三羟甲基甲胺基丙磺酸0.5g溶于DMSO 150mL，加入硅酸铝纤维5g升温至145℃反应40min，水洗，干燥，得到磺酸化纤维；
S2、将镁砂60份、磺酸化纤维2份、微硅粉1份、硅溶胶1份、碳化硅3份、膨润土1份、六偏磷酸钠0.1份混合均匀，得到中间包涂抹料。
实施例3
S1、将4’-(羟基甲基)-4-联苯基磺酸0.2g、三羟甲基甲胺基丙磺酸0.3g溶于DMSO150mL，加入硅酸铝纤维2g、碳纤维3g升温至160℃反应20min，水洗，干燥，得到磺酸化纤维；
S2、将镁砂80份、磺酸化纤维2份、微硅粉1份、硅溶胶4份、碳化硅8份、膨润土3份、六偏磷酸钠0.1份、三聚磷酸钠0.9份混合均匀，得到中间包涂抹料。
实施例4
S1、将4’-(羟基甲基)-4-联苯基磺酸1.5g溶于DMSO 150mL，加入碳纤维5g升温至150℃反应30min，水洗，干燥，得到磺酸化纤维；
S2、将镁砂70份、磺酸化纤维2份、硅溶胶3.5份、碳化硅5份、膨润土2份、三聚磷酸钠0.5份混合均匀，得到中间包涂抹料。
实施例5
S1、将4’-(羟基甲基)-4-联苯基磺酸2.5g溶于DMSO 150mL，加入碳纤维5g升温至150℃反应30min，水洗，干燥，得到磺酸化纤维；
S2、将镁砂70份、磺酸化纤维2份、硅溶胶3.5份、碳化硅5份、膨润土2份、三聚磷酸钠0.5份混合均匀，得到中间包涂抹料。
实施例6
S1、将4’-(羟基甲基)-4-联苯基磺酸4g溶于DMSO 150mL，加入碳纤维5g升温至150℃反应30min，水洗，干燥，得到磺酸化纤维；
S2、将镁砂70份、磺酸化纤维2份、硅溶胶3.5份、碳化硅5份、膨润土2份、三聚磷酸钠0.5份混合均匀，得到中间包涂抹料。
实施例7
S1、将4’-(羟基甲基)-4-联苯基磺酸5g溶于DMSO 150mL，加入碳纤维5g升温至150℃反应30min，水洗，干燥，得到磺酸化纤维；
S2、将镁砂70份、磺酸化纤维2份、硅溶胶3.5份、碳化硅5份、膨润土2份、三聚磷酸钠0.5份混合均匀，得到中间包涂抹料。
实施例8
S1、将4’-(羟基甲基)-4-联苯基磺酸2.5g溶于DMSO 150mL，加入碳纤维5g升温至150℃反应30min，水洗，干燥，得到磺酸化纤维；
S2、将镁砂70份、磺酸化纤维3份、硅溶胶3.5份、碳化硅5份、膨润土2份、三聚磷酸钠0.5份混合均匀，得到中间包涂抹料。
实施例9
S1、将4’-(羟基甲基)-4-联苯基磺酸2.5g溶于DMSO 150mL，加入碳纤维5g升温至150℃反应30min，水洗，干燥，得到磺酸化纤维；
S2、将镁砂70份、磺酸化纤维4份、硅溶胶3.5份、碳化硅5份、膨润土2份、三聚磷酸钠0.5份混合均匀，得到中间包涂抹料。
实施例10
S1、将4’-(羟基甲基)-4-联苯基磺酸2.5g溶于DMSO 150mL，加入碳纤维5g升温至150℃反应30min，水洗，干燥，得到磺酸化纤维；
S2、将镁砂70份、磺酸化纤维5份、硅溶胶3.5份、碳化硅5份、膨润土2份、三聚磷酸钠0.5份混合均匀，得到中间包涂抹料。
对比例1
将镁砂70份、碳纤维2份、硅溶胶3.5份、碳化硅5份、膨润土2份、三聚磷酸钠0.5份混合均匀，得到中间包涂抹料。
分别将实施例1~10及对比例1得到的中间包涂抹料加入总质量15%的水搅拌均匀后，涂抹形成70mm的中间包耐火材料层，晾干1h，盖上热包下来的300℃的红包盖养护1h，养护完成后，先在300℃小火烘烤60min，再在600℃中火烘烤30min，最后在800℃大火烘烤60min。
实施例1~10得到的耐火材料层浇铸9炉，均未出现坍塌现象，同时没有出现崩裂、剥落的现象，而对比例1得到的耐火材料层浇铸6炉时，便出现崩裂和剥落的现象。
将实施例1~10及对比例1得到的中间包涂抹料加入总质量15%的水搅拌均匀后，成型，养护，焙烧后参考YB/T 5200-93《致密耐火浇注料显气孔率和体积密度试验方法》的液体静力称量法，进行体积密度的测试；参考GB/T 5072-2008《耐火材料 常温耐压强度试验方法》的方法，进行110℃×24h耐压强度的测试；参考GB/T 34218-2017《耐火材料 高温耐压强度试验方法》的方法，进行1500℃×3h耐压强度的测试；测试结果记录在表1。
表1体积密度和耐压强度
由表1可以看出，本发明得到的中间包涂抹料110℃×24h体积密度在2.36g/cm3以上，110℃×24h耐压强度在12.0MPa以上，1500℃×3h耐压强度在16.8MPa以上，具有高的致密性和强度。
实施例1~10与对比例1相比，实施例1~10中使用磺酸化纤维，对比例1中未对纤维进行磺酸化，实施例1~10得到的中间包涂抹料的体积密度和耐压强度高于对比例1，说明使用磺酸化纤维，可以提高中间包涂抹料的致密性和强度。
实施例1与实施例4~7相比，实施例1中纤维和4’-(羟基甲基)-4-联苯基磺酸的质量比为1:0.1，实施例4中纤维和4’-(羟基甲基)-4-联苯基磺酸的质量比为1:0.3，实施例5中纤维和4’-(羟基甲基)-4-联苯基磺酸的质量比为1:0.5，实施例6中纤维和4’-(羟基甲基)-4-联苯基磺酸的质量比为1:0.8，实施例7中纤维和4’-(羟基甲基)-4-联苯基磺酸的质量比为1:1，实施例4~6得到的中间包涂抹料的体积密度和耐压强度高于实施例1和实施例7，说明纤维和改性剂的质量比为1:0.3~0.8可以进一步提高中间包涂抹料的致密性和强度。
以上仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (10)
1.一种中间包涂抹料，其特征在于，包括以下质量份的组分：镁砂60~80份、磺酸化纤维2~5份、结合剂2~5份、碳化硅3~8份、膨润土1~3份、减水剂0.1~1份。
2.根据权利要求1所述的一种中间包涂抹料，其特征在于，所述磺酸化纤维为经改性剂改性的纤维；
所述改性剂包括4’-(羟基甲基)-4-联苯基磺酸、三羟甲基甲胺基丙磺酸中的一种或两种。
3.根据权利要求2所述的一种中间包涂抹料，其特征在于，所述纤维包括硅酸铝纤维、碳纤维中的一种或两种。
4.根据权利要求2所述的一种中间包涂抹料，其特征在于，所述磺酸化纤维的原料包括质量比为1:0.3~0.8的纤维和改性剂。
5.根据权利要求4所述的一种中间包涂抹料，其特征在于，所述磺酸化纤维的制备方法包括以下步骤：将纤维、改性剂和溶剂混合，进行反应，得到磺酸化纤维。
6.根据权利要求5所述的一种中间包涂抹料，其特征在于，所述反应的温度为145~160℃，时间为20~40min。
7.根据权利要求1所述的一种中间包涂抹料，其特征在于，所述镁砂与磺酸化纤维的质量比为70:3~4。
8.根据权利要求1所述的一种中间包涂抹料，其特征在于，所述结合剂包括微硅粉、硅溶胶中的一种或两种。
9.根据权利要求1所述的一种中间包涂抹料，其特征在于，所述减水剂包括三聚磷酸钠、六偏磷酸钠中的一种或两种。
10.根据权利要求1~9任意一项所述的一种中间包涂抹料的制备方法，其特征在于，包括以下步骤：将所述质量份的组分混合均匀，得到中间包涂抹料。
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