CN115557675A - 一种用于玻璃生产的改性石墨复合陶瓷料槽及其制备方法 - Google Patents
一种用于玻璃生产的改性石墨复合陶瓷料槽及其制备方法 Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- 239000011521 glass Substances 0.000 title claims abstract description 21
- 239000000919 ceramic Substances 0.000 title claims abstract description 19
- 239000002131 composite material Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000011449 brick Substances 0.000 claims abstract description 58
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 36
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 32
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 32
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 32
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910000423 chromium oxide Inorganic materials 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 17
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 14
- 229910001868 water Inorganic materials 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 11
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract 2
- 238000001816 cooling Methods 0.000 claims description 34
- 238000002156 mixing Methods 0.000 claims description 34
- 238000010438 heat treatment Methods 0.000 claims description 27
- 238000005245 sintering Methods 0.000 claims description 27
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 19
- 238000000498 ball milling Methods 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 14
- 238000002844 melting Methods 0.000 claims description 14
- 230000008018 melting Effects 0.000 claims description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 12
- 239000007767 bonding agent Substances 0.000 claims description 11
- 239000000047 product Substances 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 9
- 238000004321 preservation Methods 0.000 claims description 9
- 238000003825 pressing Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical class [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- NHBRUUFBSBSTHM-UHFFFAOYSA-N n'-[2-(3-trimethoxysilylpropylamino)ethyl]ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCNCCN NHBRUUFBSBSTHM-UHFFFAOYSA-N 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 229960001149 dopamine hydrochloride Drugs 0.000 claims description 3
- 239000011344 liquid material Substances 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract description 13
- 230000035939 shock Effects 0.000 abstract description 7
- 239000005329 float glass Substances 0.000 abstract description 6
- VYFYYTLLBUKUHU-UHFFFAOYSA-N Dopamine Natural products NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 abstract description 2
- 229960003638 dopamine Drugs 0.000 abstract description 2
- -1 dopamine modified graphite Chemical class 0.000 abstract description 2
- 239000007770 graphite material Substances 0.000 abstract description 2
- 239000011819 refractory material Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 8
- 230000032683 aging Effects 0.000 description 7
- 239000011230 binding agent Substances 0.000 description 7
- 229910000077 silane Inorganic materials 0.000 description 4
- DDSWIYVVHBOISO-UHFFFAOYSA-N ctk0i1982 Chemical compound N[SiH](N)N DDSWIYVVHBOISO-UHFFFAOYSA-N 0.000 description 3
- ZYAASQNKCWTPKI-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propan-1-amine Chemical compound CO[Si](C)(OC)CCCN ZYAASQNKCWTPKI-UHFFFAOYSA-N 0.000 description 2
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 238000007496 glass forming Methods 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910052656 albite Inorganic materials 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000006060 molten glass Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000010434 nepheline Substances 0.000 description 1
- 229910052664 nepheline Inorganic materials 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 125000000467 secondary amino group Chemical group [H]N([*:1])[*:2] 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 125000001302 tertiary amino group Chemical group 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
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Abstract
本发明涉及耐火材料技术领域,尤其涉及一种用于玻璃生产的改性石墨复合陶瓷料槽及其制备方法。所述复合陶瓷料槽由耐火砖制成,所述耐火砖由以下重量百分比的原料制备而成:氧化铬绿50~55wt%、氧化铝4~6wt%、氧化锆`2~4wt%、碳化硅1~2%、水3~4wt%、改性石墨3~5wt%、余量为硅烷偶联剂改性的烧制高岭土。本发明中通过在防火砖材料中加入多巴胺改性的石墨材料,可以有效提高砖体的抗热震性能,使其能满足浮法玻璃生产过程中对锡槽底砖材料的抗热震性的特殊要求。
Description
技术领域
本发明涉及耐火材料技术领域,尤其涉及一种用于玻璃生产的改性石墨复合陶瓷料槽及其制备方法。
背景技术
浮法玻璃成形锡槽是浮法玻璃生产线的核心,在锡槽内,锡槽槽底砖起着承托熔融锡液和玻璃液的重要作用,是影响锡槽正常运行的关键结构材料。锡槽底砖在浮法玻璃生产中容易出现的问题:由于砖体积密度低、气孔率高,尤其是连通气孔多,砖抗碱渗透能力差,砖体上部会吸收Na2O生成钠长石或霞石类矿物,伴随20%左右的体积膨胀,发生块状剥片上浮,严重影响玻璃板的质量和锡槽的正常运行。此外,在浮法玻璃成型过程,需要将1100℃左右的玻璃液倒入锡槽中,随后则需要将玻璃液冷却至600~620℃,被过渡辊台抬起离开锡槽。在上述过程中,对锡槽的抗热震性提出了要求,尤其是对锡槽的底砖材料的抗热震性有更高的要求。
基于上述情况,本发明提出了一种用于玻璃生产的改性石墨复合陶瓷料槽及其制备方法。
发明内容
本发明的目的在于提供一种用于玻璃生产的改性石墨复合陶瓷料槽及其制备方法。
为实现上述目的,本发明提供一种用于玻璃生产的改性石墨复合陶瓷料槽,所述复合陶瓷料槽由耐火砖制成,所述耐火砖由以下重量百分比的原料制备而成:氧化铬绿50~55wt%、氧化铝4~6wt%、氧化锆`2~4wt%、碳化硅1~2%、水3~4wt%、改性石墨3~5wt%、余量为硅烷偶联剂改性的烧制高岭土。
优选地,所述改性石墨由以下方法制备而成:
(1)将硅烷偶联剂按料液比(g:ml)1:7.5~8.0与去离子水混合,并用盐酸调节pH至8.0~85;
(2)加入重量份为硅烷偶联剂2.3~2.5倍的超细石墨粉,并超声分散30~35min,加入重量份为硅烷偶联剂4.0~4.2倍的盐酸多巴胺,在25~30℃下持续搅拌20~24h;
(3)将混合体系离心分离,并依次用无水乙醇、去离子水将离心产物洗涤3~4次,放入真空干燥箱45~50℃干燥至恒定质量,即得。
优选地,所述硅烷偶联剂为单氨基硅烷、双氨基硅烷、三氨基硅烷、仲氨基硅烷、叔氨基硅烷的其中一种。
优选地,所述硅烷偶联剂为三氨基硅烷,所述三氨基硅烷为3-二乙烯三胺基丙基三甲氧基硅烷,CAS号为35141-30-1。
优选地,所述超细石墨粉的粒径为200~300目,固定碳含量为99.996%。
优选地,所述氧化铬绿为电熔级氧化铬绿,所述电熔级氧化铬绿的体积密度为5.0~5.5g/cm3,氧化铬含量≥99.9%。
优选地,所述电熔级氧化铬绿的组成为:粒径为200目含量为10wt%、粒径≤1mm含量为15wt%、1mm<粒径≤3mm含量为20wt%、余量均为3mm<粒径≤5mm。
优选地,所述氧化铝纯度为99.9%,比表面积为100~130m2/g,体积密度为0.9~1.1g/cm3,平均粒径为200~250nm。
优选地,所述氧化锆纯度为99.9%,比表面积为77~80m2/g,体积密度为2.4~2.5g/cm3,平均粒径为100~150nm。
优选地,所述碳化硅纯度为99.9%,比表面积为20~30m2/g,体积密度为0.1~0.2g/cm3,平均粒径为700~800nm。
优选地,所述硅烷偶联剂改性的烧制高岭土由以下方法制备而成:
(1)先将3~5%(g/ml)强碱溶液按液料比(ml:g)1:0.2~0.3与烧制高岭土混匀,在85~90℃下搅拌5~6h,随后冷却至室温,离心,取下层沉淀;
(2)将步骤(1)获得的沉淀物使用蒸馏水洗涤3~4次,在75~80℃下真空干燥48h,得到碱化的烧制高岭土;
(3)取步骤(2)获得的碱化的烧制高岭土按料液比(g:ml)1:7.5~8.0与无水乙醇混匀,使用弱酸溶液将溶液调至pH6~7,超声30~35min,随后加入重量份为碱化的烧制高岭土1.5~2倍的硅烷偶联剂,在85~90℃下搅拌反应5~6h,冷却至室温,离心,取下层物,并用无水乙醇洗涤2~3次,在75~80℃下真空干燥产物24h,得到硅烷偶联剂改性的烧制高岭土。
优选地,所述烧制高岭土的粒径为300~325目,二氧化硅含量为45~52%。
优选地,所述强碱溶液为氢氧化钠溶液、氢氧化钾溶液、氢氧化钙溶液的其中一种。
优选地,所述弱酸溶液为草酸溶液、乙酸溶液、甲酸溶液的其中一种。
优选地,所述硅烷偶联剂为KH550、KH560、KH570的其中一种。
本发明还提供一种用于玻璃生产的改性石墨复合陶瓷料槽耐火砖的制备方法,所述方法包括如下步骤:
(1)将不同粒径的电熔级氧化铬绿以150~200rpm混合10~15min;
(2)将氧化铝与氧化锆、水混合球磨10~15min,得结合剂;
(3)将步骤(1)获得的电熔级氧化铬绿、步骤(2)获得的结合剂、碳化硅与硅烷偶联剂改性的烧制高岭土进行球磨混合15~20mi;
(4)取步骤(3)球磨好的混合料,经密闭罐内困料1~2h后压制成型,成型机规格:吨位≥630t,随后干燥24~36h;
(5)将步骤(4)砖坯置入加热炉中,控制加热炉温度为500℃,加热时间为1h,并保温处理5h;然后将加热处理后的砖坯置入充满氮气氛围的电烧结炉中进行烧结处理,控制烧结炉的温度为1150℃,保温处理6h,最后将烧结完成后的砖坯置入冷却炉中,以80℃/h的降温速度冷却到室温,即得料槽用的耐火砖材料。
与现有技术相比,本发明具有如下有益效果:
1.本发明中通过在防火砖材料中加入多巴胺改性的石墨材料,可以有效提高砖体的抗热震性能,使其能满足浮法玻璃生产过程中对锡槽底砖材料的抗热震性的特殊要求。
2.本发明的制备方法、操作方便,易于大规模生产,且质量稳定。
3.本发明原材料在国内充足,价格适宜,使其规模化生产没有太高的成本限制。
具体实施方式
实施例1
硅烷偶联剂改性的烧制高岭土的制备:
(1)先将5%(g/ml)氢氧化钠溶液按液料比(ml:g)1:0.3与烧制高岭土混匀,在85℃下搅拌6h,随后冷却至室温,离心,取下层沉淀;
(2)将步骤(1)获得的沉淀物使用蒸馏水洗涤4次,在75℃下真空干燥48h,得到碱化的烧制高岭土;
(3)取步骤(2)获得的碱化的烧制高岭土按料液比(g:ml)1:7.5与无水乙醇混匀,使用乙酸溶液将溶液调至pH6~7,超声35min,随后加入重量份为碱化的烧制高岭土2倍的硅烷偶联剂KH560,在90℃下搅拌反应5h,冷却至室温,离心,取下层物,并用无水乙醇洗涤3次,在75℃下真空干燥产物24h,得到硅烷偶联剂改性的烧制高岭土。
实施例2
改性石墨的制备:
(1)将3-二乙烯三胺基丙基三甲氧基硅烷按料液比(g:ml)1:7.5与去离子水混合,并用盐酸调节pH至8.0~85;
(2)加入重量份为3-二乙烯三胺基丙基三甲氧基硅烷2.5倍的超细石墨粉,并超声分散35min,加入重量份为3-二乙烯三胺基丙基三甲氧基硅烷4.2倍的盐酸多巴胺,在30℃下持续搅拌20h;
(3)将混合体系离心分离,并依次用无水乙醇、去离子水将离心产物洗涤3次,放入真空干燥箱50℃干燥至恒定质量,即得。
实施例3
各原料的用量见表1。
(1)将不同粒径的电熔级氧化铬绿以150rpm混合15min;
(2)将氧化铝与氧化锆、水混合球磨10min,得结合剂;
(3)将步骤(1)获得的电熔级氧化铬绿、步骤(2)获得的结合剂、碳化硅与实施例1制备的硅烷偶联剂改性的烧制高岭土、实施例2制备的改性石墨进行球磨混合15mi;
(4)取步骤(3)球磨好的混合料,经密闭罐内困料1h后压制成型,成型机规格:吨位≥630t,随后干燥24h;
(5)将步骤(4)砖坯置入加热炉中,控制加热炉温度为500℃,加热时间为1h,并保温处理5h;然后将加热处理后的砖坯置入充满氮气氛围的电烧结炉中进行烧结处理,控制烧结炉的温度为1150℃,保温处理6h,最后将烧结完成后的砖坯置入冷却炉中,以80℃/h的降温速度冷却到室温,即得料槽用的耐火砖材料。
实施例4
各原料的用量见表1。
(1)将不同粒径的电熔级氧化铬绿以200rpm混合10min;
(2)将氧化铝与氧化锆、水混合球磨15min,得结合剂;
(3)将步骤(1)获得的电熔级氧化铬绿、步骤(2)获得的结合剂、碳化硅与实施例1制备的硅烷偶联剂改性的烧制高岭土、实施例2制备的改性石墨进行球磨混合15mi;
(4)取步骤(3)球磨好的混合料,经密闭罐内困料2h后压制成型,成型机规格:吨位≥630t,随后干燥24h;
(5)将步骤(4)砖坯置入加热炉中,控制加热炉温度为500℃,加热时间为1h,并保温处理5h;然后将加热处理后的砖坯置入充满氮气氛围的电烧结炉中进行烧结处理,控制烧结炉的温度为1150℃,保温处理6h,最后将烧结完成后的砖坯置入冷却炉中,以80℃/h的降温速度冷却到室温,即得料槽用的耐火砖材料。
实施例5
各原料的用量见表1。
(1)将不同粒径的电熔级氧化铬绿以200rpm混合15min;
(2)将氧化铝与氧化锆、水混合球磨15min,得结合剂;
(3)将步骤(1)获得的电熔级氧化铬绿、步骤(2)获得的结合剂、碳化硅与实施例1制备的硅烷偶联剂改性的烧制高岭土、实施例2制备的改性石墨进行球磨混合20mi;
(4)取步骤(3)球磨好的混合料,经密闭罐内困料2h后压制成型,成型机规格:吨位≥630t,随后干燥36h;
(5)将步骤(4)砖坯置入加热炉中,控制加热炉温度为500℃,加热时间为1h,并保温处理5h;然后将加热处理后的砖坯置入充满氮气氛围的电烧结炉中进行烧结处理,控制烧结炉的温度为1150℃,保温处理6h,最后将烧结完成后的砖坯置入冷却炉中,以80℃/h的降温速度冷却到室温,即得料槽用的耐火砖材料。
对比例1
各原料的用量见表1。
(1)将不同粒径的电熔级氧化铬绿以200rpm混合15min;
(2)将氧化铝与氧化锆、水混合球磨15min,得结合剂;
(3)将步骤(1)获得的电熔级氧化铬绿、步骤(2)获得的结合剂、碳化硅与实施例1制备的硅烷偶联剂改性的烧制高岭土、超细石墨粉进行球磨混合20mi;
(4)取步骤(3)球磨好的混合料,经密闭罐内困料2h后压制成型,成型机规格:吨位≥630t,随后干燥36h;
(5)将步骤(4)砖坯置入加热炉中,控制加热炉温度为500℃,加热时间为1h,并保温处理5h;然后将加热处理后的砖坯置入充满氮气氛围的电烧结炉中进行烧结处理,控制烧结炉的温度为1150℃,保温处理6h,最后将烧结完成后的砖坯置入冷却炉中,以80℃/h的降温速度冷却到室温,即得料槽用的耐火砖材料。
对比例2
与实施例2制备的改性石墨不同,本对比例制备的改性石墨使用的硅烷偶联剂为N-2-氨乙基-3-氨丙基三甲氧基硅烷,CAS号为1760-24-3,属于双氨基硅烷。
各原料的用量见表1。
(1)将不同粒径的电熔级氧化铬绿以200rpm混合15min;
(2)将氧化铝与氧化锆、水混合球磨15min,得结合剂;
(3)将步骤(1)获得的电熔级氧化铬绿、步骤(2)获得的结合剂、碳化硅与实施例1制备的硅烷偶联剂改性的烧制高岭土、改性石墨进行球磨混合20mi;
(4)取步骤(3)球磨好的混合料,经密闭罐内困料2h后压制成型,成型机规格:吨位≥630t,随后干燥36h;
(5)将步骤(4)砖坯置入加热炉中,控制加热炉温度为500℃,加热时间为1h,并保温处理5h;然后将加热处理后的砖坯置入充满氮气氛围的电烧结炉中进行烧结处理,控制烧结炉的温度为1150℃,保温处理6h,最后将烧结完成后的砖坯置入冷却炉中,以80℃/h的降温速度冷却到室温,即得料槽用的耐火砖材料。
对比例3
与实施例2制备的改性石墨不同,本对比例制备的改性石墨使用的硅烷偶联剂为3-氨丙基甲基二甲氧基硅烷,CAS号为3663-44-3,属于单氨基硅烷。
各原料的用量见表1。
(1)将不同粒径的电熔级氧化铬绿以200rpm混合15min;
(2)将氧化铝与氧化锆、水混合球磨15min,得结合剂;
(3)将步骤(1)获得的电熔级氧化铬绿、步骤(2)获得的结合剂、碳化硅与实施例1制备的硅烷偶联剂改性的烧制高岭土、改性石墨进行球磨混合20mi;
(4)取步骤(3)球磨好的混合料,经密闭罐内困料2h后压制成型,成型机规格:吨位≥630t,随后干燥36h;
(5)将步骤(4)砖坯置入加热炉中,控制加热炉温度为500℃,加热时间为1h,并保温处理5h;然后将加热处理后的砖坯置入充满氮气氛围的电烧结炉中进行烧结处理,控制烧结炉的温度为1150℃,保温处理6h,最后将烧结完成后的砖坯置入冷却炉中,以80℃/h的降温速度冷却到室温,即得料槽用的耐火砖材料。
对比例4
与实施例2制备的改性石墨不同,本对比例制备的改性石墨使用的硅烷偶联剂为3-氨丙基三甲氧基硅烷,CAS号为13822-56-5,属于单氨基硅烷。
各原料的用量见表1。
(1)将不同粒径的电熔级氧化铬绿以200rpm混合15min;
(2)将氧化铝与氧化锆、水混合球磨15min,得结合剂;
(3)将步骤(1)获得的电熔级氧化铬绿、步骤(2)获得的结合剂、碳化硅与实施例1制备的硅烷偶联剂改性的烧制高岭土、改性石墨进行球磨混合20mi;
(4)取步骤(3)球磨好的混合料,经密闭罐内困料2h后压制成型,成型机规格:吨位≥630t,随后干燥36h;
(5)将步骤(4)砖坯置入加热炉中,控制加热炉温度为500℃,加热时间为1h,并保温处理5h;然后将加热处理后的砖坯置入充满氮气氛围的电烧结炉中进行烧结处理,控制烧结炉的温度为1150℃,保温处理6h,最后将烧结完成后的砖坯置入冷却炉中,以80℃/h的降温速度冷却到室温,即得料槽用的耐火砖材料。
表1
耐火砖性能评价测试
将实施例3~5以及对比例1~4制备得到的耐火砖分别进行显气孔率(%)测试、体积密度(g/cm3)测试,热震稳定性(1100℃,水冷)测试。其中显气孔率、体积密度按照GB/T2997-2015规定的方法进行。结果见表2。
表2
前述对本发明的具体示例性实施方案的描述是为了说明和例证的目的。这些描述并非想将本发明限定为所公开的精确形式,并且很显然,根据上述教导,可以进行很多改变和变化。对示例性实施例进行选择和描述的目的在于解释本发明的特定原理及其实际应用,从而使得本领域的技术人员能够实现并利用本发明的各种不同的示例性实施方案以及各种不同的选择和改变。本发明的范围意在由权利要求书及其等同形式所限定。
Claims (10)
1.一种用于玻璃生产的改性石墨复合陶瓷料槽,其特征在于,所述复合陶瓷料槽由耐火砖制成,所述耐火砖由以下重量百分比的原料制备而成:氧化铬绿50~55wt%、氧化铝4~6wt%、氧化锆`2~4wt%、碳化硅1~2%、水3~4wt%、改性石墨3~5wt%、余量为硅烷偶联剂改性的烧制高岭土。
2.根据权利要求1所述的用于玻璃生产的改性石墨复合陶瓷料槽,其特征在于,所述改性石墨由以下方法制备而成:
(1)将硅烷偶联剂按料液比(g:ml)1:7.5~8.0与去离子水混合,并用盐酸调节pH至8.0~85;
(2)加入重量份为硅烷偶联剂2.3~2.5倍的超细石墨粉,并超声分散30~35min,加入重量份为硅烷偶联剂4.0~4.2倍的盐酸多巴胺,在25~30℃下持续搅拌20~24h;
(3)将混合体系离心分离,并依次用无水乙醇、去离子水将离心产物洗涤3~4次,放入真空干燥箱45~50℃干燥至恒定质量,即得。
3.根据权利要求2所述的用于玻璃生产的改性石墨复合陶瓷料槽,其特征在于,所述硅烷偶联剂为单氨基硅烷、双氨基硅烷、三氨基硅烷、仲氨基硅烷、叔氨基硅烷的其中一种。
4.根据权利要求3所述的用于玻璃生产的改性石墨复合陶瓷料槽,其特征在于,所述硅烷偶联剂为三氨基硅烷,所述三氨基硅烷为3-二乙烯三胺基丙基三甲氧基硅烷,CAS号为35141-30-1。
5.根据权利要求2所述的用于玻璃生产的改性石墨复合陶瓷料槽,其特征在于,所述超细石墨粉的粒径为200~300目,固定碳含量为99.996%。
6.根据权利要求1所述的用于玻璃生产的改性石墨复合陶瓷料槽,其特征在于,所述硅烷偶联剂改性的烧制高岭土由以下方法制备而成:
(1)先将3~5%(g/ml)强碱溶液按液料比(ml:g)1:0.2~0.3与烧制高岭土混匀,在85~90℃下搅拌5~6h,随后冷却至室温,离心,取下层沉淀;
(2)将步骤(1)获得的沉淀物使用蒸馏水洗涤3~4次,在75~80℃下真空干燥48h,得到碱化的烧制高岭土;
(3)取步骤(2)获得的碱化的烧制高岭土按料液比(g:ml)1:7.5~8.0与无水乙醇混匀,使用弱酸溶液将溶液调至pH6~7,超声30~35min,随后加入重量份为碱化的烧制高岭土1.5~2倍的硅烷偶联剂,在85~90℃下搅拌反应5~6h,冷却至室温,离心,取下层物,并用无水乙醇洗涤2~3次,在75~80℃下真空干燥产物24h,得到硅烷偶联剂改性的烧制高岭土。
7.根据权利要求6所述的用于玻璃生产的改性石墨复合陶瓷料槽,其特征在于,所述烧制高岭土的粒径为300~325目,二氧化硅含量为45~52%;所述强碱溶液为氢氧化钠溶液、氢氧化钾溶液、氢氧化钙溶液的其中一种;所述弱酸溶液为草酸溶液、乙酸溶液、甲酸溶液的其中一种;所述硅烷偶联剂为KH550、KH560、KH570的其中一种。
8.根据权利要求1所述的用于玻璃生产的改性石墨复合陶瓷料槽,其特征在于,所述氧化铬绿为电熔级氧化铬绿,所述电熔级氧化铬绿的体积密度为5.0~5.5g/cm3,氧化铬含量≥99.9%;所述氧化铝纯度为99.9%,比表面积为100~130m2/g,体积密度为0.9~1.1g/cm3,平均粒径为200~250nm;所述氧化锆纯度为99.9%,比表面积为77~80m2/g,体积密度为2.4~2.5g/cm3,平均粒径为100~150nm;所述碳化硅纯度为99.9%,比表面积为20~30m2/g,体积密度为0.1~0.2g/cm3,平均粒径为700~800nm。
9.根据权利要求8所述的用于玻璃生产的改性石墨复合陶瓷料槽,其特征在于,所述电熔级氧化铬绿的组成为:粒径为200目含量为10wt%、粒径≤1mm含量为15wt%、1mm<粒径≤3mm含量为20wt%、余量均为3mm<粒径≤5mm。
10.一种制备权利要求1所述用于玻璃生产的改性石墨复合陶瓷料槽耐火砖的方法,其特征在于,所述方法包括如下步骤:
(1)将不同粒径的电熔级氧化铬绿以150~200rpm混合10~15min;
(2)将氧化铝与氧化锆、水混合球磨10~15min,得结合剂;
(3)将步骤(1)获得的电熔级氧化铬绿、步骤(2)获得的结合剂、碳化硅与硅烷偶联剂改性的烧制高岭土、改性石墨进行球磨混合15~20mi;
(4)取步骤(3)球磨好的混合料,经密闭罐内困料1~2h后压制成型,成型机规格:吨位≥630t,随后干燥24~36h;
(5)将步骤(4)砖坯置入加热炉中,控制加热炉温度为500℃,加热时间为1h,并保温处理5h;然后将加热处理后的砖坯置入充满氮气氛围的电烧结炉中进行烧结处理,控制烧结炉的温度为1150℃,保温处理6h,最后将烧结完成后的砖坯置入冷却炉中,以80℃/h的降温速度冷却到室温,即得料槽用的耐火砖材料。
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