CN108698931A - 耐火的成型体和物料以及粘合剂和它们的制造方法 - Google Patents
耐火的成型体和物料以及粘合剂和它们的制造方法 Download PDFInfo
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- CN108698931A CN108698931A CN201680077676.8A CN201680077676A CN108698931A CN 108698931 A CN108698931 A CN 108698931A CN 201680077676 A CN201680077676 A CN 201680077676A CN 108698931 A CN108698931 A CN 108698931A
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Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—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
- C04B35/013—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 containing carbon
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—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
本发明涉及用于制造耐高温或耐火的成型体的物料,其由下列材料的混合物构成:耐火或耐高温的无机粉末、颗粒和/或粒料,与由碳制成或无碳的可流动物料或粉末,粘合剂,其中所述粘合剂由单宁、乳糖、细粒二氧化硅和铝粉的组合构成,以及涉及所述粘合剂本身和由所述具有粘合剂的物料制造的成型体以及它的制造方法。
Description
本发明涉及用于制造耐火成型体的物料,其由耐火或耐高温的无机粉末、颗粒和/或粒料以及粘合剂的混合物构成,其中优选添加由碳制成的可流动物料或粉末。
此外,本发明涉及用于制造耐火的物料或成型体的用于此类物料的粘合剂以及由此类具有粘合剂的物料制成的成型体。最后,本发明涉及用于由耐高温或耐火的无机粉末、颗粒和/或粒料和粘合剂制造耐火或耐高温的成型体或物料的方法。
碳结合的含石墨的产品广泛地用作冶金容器中的内衬,例如用作转炉中的碳结合的氧化镁石或用作连续铸造领域中的关键部件,例如浸入式水口或滑动板或塞棒或流槽(Grießrinnen)。碳结合的耐火产品此外用于高炉区域中、用于运输容器,例如钢水包中或用于化学工业中或用于垃圾焚烧工业中作为耐高温管或用于混凝土工业中作为内衬材料。
作为粘合剂,在此优选使用纯酚树脂,例如可熔酚醛树脂或线型酚醛清漆,人造沥青(Kunstpech),例如Carbores或煤沥青(Steinkohlepech)。为了优化含酚的碳结合的产品的耐氧化性,主要使用金属添加剂,例如Si或Al或Mg。在DE 199 54 893 A1中提出了具有改进的氧化性能的碳结合的产品。通过将来自过渡元素的易于还原的化合物,特别是铜、铬、镍或铁的茂金属或金属苯甲酸盐(Metallobenzoate)或金属环烷酸盐(Metallonaphtenate)的催化活性物质添加到人造树脂组分中,在低于1000℃时产生结晶高度石墨化(hochgraphisiert)碳,其有助于改进的化学性能。
已知粘合剂体系在其环保性和工作安全性方面通过在树脂情况中的游离酚成分或通过其在源于沥青的粘合剂的情况中的苯并[a]芘成分而具有巨大问题。
由现有技术出发,本发明的基本目的是提供环保、耐火的,优选碳结合的含石墨的成型体和物料,其由具有或不具有其它碳添加剂的细粒和粗粒无机原料制成并基于环保粘合剂,其对于500℃至2000℃的温度范围内的应用温度而言具有非常好的机械、热机械和化学性能。
细粒无机原料表示粒度为</= 100 µm的天然或合成原料,粗粒无机原料表示粒度为>100 µm的天然或合成原料。
本发明的另一基本目的是提供用于具有或不具有碳添加剂的耐火产品的环保粘合剂体系,其与低孔隙率组合着符合对于足够耐氧化性和耐腐蚀性的强度要求。
为了实现所述目的,本发明根据权利要求1建议所述粘合剂由单宁、乳糖、细粒二氧化硅和铝粉的组合构成。根据本发明,也在根据权利要求2的物料中使用相同粘合剂。
此外,本发明根据权利要求3提供用于制造相应物料或成型体的粘合剂,其中该粘合剂由单宁、乳糖、细粒二氧化硅和铝粉的组合构成。
优选地,乳糖与单宁的比率在此为0.1至0.3。
此外,在所述粘合剂中优选地设置,细粒二氧化硅的粒度为<50 µm,优选<1 µm且铝粉的粒度为<200 µm。
本发明还建议,向所述粘合剂添加最多30重量%的粉末形式的酚树脂,基于乳糖和单宁的混合物计。
本发明还建议,向所述粘合剂添加其它细粒添加剂,即镁或碳化物,特别是SiC、B4C、TiC或氮化物,特别是Si3N4、AlN、TiN或硼化物,特别是BN、TiB2。
还可能优选的是,向所述粘合剂加入掺杂硅。
特别优选是,向所述粘合剂添加乙二醇,优选以0.1至5重量%的量,基于粘合剂总量计。
还优选的是,单宁含量大于乳糖含量,单宁优选为70至90重量%,基于粘合剂总量计。
在用于制造相应产品且由具有粘合剂的混合物构成的物料的情况下优选地设置,所添加的碳是石墨和/或炭黑和/或碳纤维材料和/或碳纳米管(CNT)和/或石墨烯和/或预焦化沥青、地沥青或酚树脂。
相应的物料优选与根据上述定义的粘合剂混合。
优选地设置,向所述物料添加最多50重量%,优选0.5至20重量%,特别优选2至8重量%的含量的粘合剂,基于整个物料计。
根据本发明,还有成型体,其由具有粘合剂的相应物料构成。
本发明的主题还是由耐高温或耐火的无机粉末、颗粒和/或粒料和粘合剂制造耐火或耐高温的成型体或物料的方法,其中根据本发明设置,向< 100 µm的无机细粒添加至少一种> 100 µm 的无机粗粒和碳和基于单宁、乳糖、细粒二氧化硅和铝粉的组合粘合剂,并且——优选在混合机中——混合,所述混合物通过原始成型法,例如浇铸、压制、挤出而转变成产品,该产品在使用之前或过程中在> 100℃的温度下热处理,优选在两个工艺阶段中,即在最多250℃的第一阶段和高于600℃的温度下的第二阶段中,优选在排除氧气的情况下。
根据本发明,在所述方法中使用如权利要求书中所示的物料和/或粘合剂。
本发明涉及用于制造碳结合的含石墨的耐火成型体和物料的组合粘合剂体系,其基于单宁、乳糖、细粒SiO2和铝并与至少一种耐火粗粒组合。
根据本发明,所述粘合剂体系提供环保的变体,其根据本发明还可以与其它较不环保的粘合剂组合着有助于降低有害健康的排放。
根据本发明,所述组合粘合剂体系可以由单宁、乳糖、细粒SiO2、铝和含酚的粉末树脂构成。
根据本发明,为了压制成型,在准备所述物料时将乙二醇作为溶剂添加到混合机中。
所用的无机颗粒可以由氧化、非氧化的天然或合成原料、碳和/或金属颗粒构成。所用原料的粒度为30 mm至30 mm。
作为氧化颗粒,可以例如使用氧化钙、氧化镁、白云石、氧化铬、氧化铝、富铝红柱石、锆莫来石(Zirkonmullit)、二氧化锆、铝酸镁尖晶石、铝土矿、氧化钇、二氧化钛。
作为非氧化颗粒,可以例如使用碳化硅、氮化硅、氮化硼、碳化硼和碳。
根据本发明,石墨和/或炭黑和/或碳纤维和/或碳纳米管(CNT)和/或石墨烯和/或预焦化沥青、地沥青或酚树脂用作碳载体。
根据本发明,所述粘合剂体系与至少一种无机粗粒的组合特别适合用于传统注浆成型、加压注浆成型、振动物料(Vibrationsmassen)和自流动物料的浇注,作为挤出时、压制成型时的可塑物料中的粘合剂,特别地用于单轴压制和冷等静压压制。
根据本发明,来自食品工业的糖,例如乳糖与来自次级植物成分的具有对位酚类羟基的多羟基酚,例如单宁的组合用作新型绝对环保的粘合剂体系,其用于制造耐火产品的具有或不具有石墨、石墨烯或炭黑形式的碳且由氧化物、非氧化物构成的含碳或无碳的耐火混合物中。
乳糖还称为乳糖或乳糖。其是由D-葡萄糖和D-半乳糖形成的二糖,其以β-1,4-糖苷键的方式连接(4-O-(β-D-吡喃半乳糖基-D-吡喃葡萄糖)。
乳糖由其立体异构体,即α-和β-形式组成。其因此以各种形式存在:
- α-乳糖-一水合物
- 稳定的无水α-乳糖
- 不稳定的无水α-乳糖
- 无定形乳糖
- β-乳糖
- β/α混合的晶体。
乳糖天然存在于乳和乳产品中。乳中的乳糖含量为大约5 %。用于制备乳糖的初产物是在乳酪制造时出现的乳清,其含有4-5 %的乳糖。通过超滤和结晶,在过滤、提纯和干燥后最终以不同纯度获得终产物,即乳糖。
对于单宁分类,存在不同的可能方式。在本发明中将它们如下分类,即分为可水解单宁(或棓单宁)和缩合单宁(或儿茶属鞣质)。缩合单宁(也称为原花色素)是黄烷-3-醇的二聚体或更高级的低聚物。如其名已暗示,可水解单宁可以水解成葡萄糖、多元醇、棓酸或鞣花酸。
为了制备单宁,由热带或亚热带树种的树皮或木材起始。坚木单宁是柳叶红坚木(Schinopsis balansae)。通过从碱性水溶液提取而获得。最后一步是喷雾干燥,并且成品单宁以粉末形式进入市场。
根据本发明,坚木单宁 –成本有利的变体- 在多种单宁中是优选的。另一个原因是作为缩合单宁的5/11坚木单宁对于反应配对物的活性,这由化学结构不言而喻。
在现有技术中,单宁和乳糖或单宁与SiO2或单宁、乳糖和胺的组合被建议作为粘合剂。根据本发明,乳糖和单宁和细粒SiO2的组合才产生可用于粗粒、碳结合且特别是含石墨的耐火产品的粘合剂,但是其通过添加Al才产生足够的强度,以实现用于耐火应用中。当此外孔隙率要求也重要时,根据本发明必要的是在乳糖和单宁的混合物中少许添加最多30%范围的含酚粉末树脂(例如70%乳糖和单宁和30%酚树脂)。
在耐火应用中用于碳结合的含石墨的产品且基于单宁和乳糖和SiO2和Al的本发明组合粘合剂体系与无机粗粒的组合是现有技术中未知的。
DE 697 30 221 TS涉及基于缩合单宁的固化型胶粘剂组合物。其用作木材工业中生产木基材料,例如刨花板、纤维板(MDF)、胶合板、模板、层压板的胶粘剂。
DE 44 06 825 A1中阐明了在不同单宁种类下以各种浓度级(Konzentrationsschritt)添加SiO2作为固化剂。该粘合或胶粘剂对于木材加工工业而言也是重要的。
在DE 103 04 748 A1中描述了由粘合剂、填料和添加剂制成的物料,其在环境温度下可注射并且在高于150℃的温度下可固化。其包括漆料沉渣或粉末漆,其此外添加有单宁以实现6/11更好的操作性。其在机动车建造和机器制造时充当涂覆物料或隔音物料。
DE 696 06 052 T2涉及用于制造电路板的交联的生物基材料。其可以具有不同来源,例如木质素(包括改性的)、植物油、树胶、单宁、多糖树脂、纤维素(包括改性的)。
公开文献DE 1470914描述了制造用于铸型厂中金属熔体铸造的细粒且无石墨的铸模的可热固化(大约150℃) 物料的方法。其由碳水化合物、硫酸化单宁、胺和交联剂,例如六亚甲基四胺(HEXA)构成,它们进行反应。其在铸型厂中用于铸造。在一起使用粘土或陶瓷粘合剂制造塑料物体、烧结或多孔性金属产品、发泡隔热材料、型芯和铸模时,也可以使用该物料。
在DE 2050501 B中涉及用于型砂的交联剂和树脂形成剂。其含有还原性糖、磷酸、多元酚和水。
在WO 2010/037699 A2中涉及不含无机细粒或粗粒的纯碳水化合物的热解,其借助添加的SiO2而不发泡并因此产生含石墨的残余物,该残余物可进一步使用。
DE 2249103 A描述了借助还原性糖、磷酸、流化剂(Flüssigmacher)、多元酚、有机多异氰酸酯、多价金属的粉末和额外的固化剂制造耐火且阻燃的树脂类泡沫材料的方法。
在DE 2759132 A1中使用还原性糖、液体的树脂形成剂、磷酸、塑化剂(Verflüssiger)、多元酚和释放气体的膨胀剂或发泡剂,以制造涂层材料。该涂层在提高的热生成的情况下形成隔热的泡沫阻隔物,在较长的热生成时达到多孔性、不可燃的焦炭或残余物残余物,其不可着火。
EP 2 740 768 A1说明了在热和压力下压制含单宁的混合物的方法。借此应制造无石油产品的与塑料类似的模具和含木材的经胶粘的刨花板。为此将植物材料、多羧酸和糖混合并在最多250℃的温度下熔化。
对于在特别是高于 1500℃的高使用温度下的耐火成型体的使用者而言,力求改进的机械、热和化学性能(抗蠕变性、抗热冲击性和耐腐蚀性),以提高受高应力的耐火产品的使用寿命。通过在耐火产品中的无机粗粒和细粒与石墨、单宁和乳糖的组合,根据本发明一方面在原始成型,即压制、浇铸、挤出时实现高的坯体强度,其赋予所述绝对环保的耐火产品非常好的机械性能。根据本发明,向这两种粘合剂单宁和乳糖添加小于10 μm的细粒SiO2,以在热处理过程中减缓体积膨胀,并添加小于200 μm的铝粉,以实现在排除氧气的情况下高于600°的温度处理后(碳结合的耐火产品的焦化条件)大于35 MPa的冷抗压强度。
根据本发明,向由乳糖、单宁、SiO2和铝构成的粘合剂体系加入金属硅和/或半导体硅– 其例如具有磷掺杂,以提高残余碳含量。
为了优化新研发的粘合剂体系的耐氧化性,可以根据本发明添加其它细粒添加剂,例如Mg或碳化物,例如SiC、B4C、TiC或氮化物,例如Si3N4、AlN、TiN或硼化物,例如BN、TiB2。
应以下面的实施例更详细阐述本发明。
实施例1和2是用于碳结合的含石墨的MgO石的混合物,实施例3和4是用于碳结合的含石墨的Al2O3功能部件,例如塞棒、浸入式水口的混合物。
在Eirich强力混合机中混合氧化物与粘合剂体系后,进行用于石材规格的单轴压制(本发明实施例混合物1和2)和用于塞棒几何的冷等静压压制(本发明实施例混合物3和4)、在小于250℃的温度下的回火和随后在大于800℃的温度下的焦化。
在焦化状态下,由石材产品制成的圆柱样品达到大于40 MPa的冷抗压强度和小于14%的孔隙率,由塞棒几何制成的弯曲棒达到大于3 MPa的抗弯强度和小于18%的孔隙率。
所有的百分率数据是指重量百分率,并且基于分别为100 %的氧化物总质量计。
实施例
实施例1
原料 | % |
氧化物 | |
烧结氧化镁< 0.09 mm | 23 |
烧结氧化镁0-1 mm | 20 |
烧结氧化镁1-3 mm | 37 |
烧结氧化镁3-6 | 20 |
石墨 | 3.6 |
粘合剂体系 | |
单宁 | 3.4 |
乳糖 | 0.75 |
SiO2 | 0.23 |
铝 | 2.0 |
Hexa | 0.5 |
乙二醇 | 1.5 |
实施例2
原料 | % |
氧化物 | |
烧结氧化镁< 0.09 mm | 23 |
烧结氧化镁0-1 mm | 20 |
烧结氧化镁1-3 mm | 37 |
烧结氧化镁3-6 | 20 |
石墨 | 3.6 |
粘合剂体系 | |
单宁 | 3.4 |
乳糖 | 0.75 |
SiO2 | 0.23 |
铝 | 2.0 |
Hexa | 0.5 |
乙二醇 | 1.5 |
酚树脂(粉末) | 1.0 |
实施例3
原料 | % |
氧化物 | |
氧化铝 0-0.6 | 60 |
氧化铝 0-80 | 40 |
石墨 | 20 |
粘合剂体系 | |
单宁 | 5 |
乳糖 | 1 |
SiO2 | 0.25 |
硅 | 6.0 |
Hexa | 1.0 |
乙二醇 | 2.0 |
实施例4
原料 | % |
氧化物 | |
氧化铝 0-0.6 mm | 60 |
氧化铝 0-80 μm | 40 |
石墨 | 20 |
粘合剂体系 | |
单宁 | 5 |
乳糖 | 1 |
SiO2 | 0.25 |
硅 | 6.0 |
Hexa | 1.0 |
乙二醇 | 2.0 |
酚树脂粉末 | 1.5 |
Claims (16)
1.用于制造耐高温或耐火的成型体的物料,其由下列材料的混合物构成:
- 耐火或耐高温的无机粉末、颗粒和/或粒料,
- 粘合剂,
其特征在于,所述粘合剂由单宁、乳糖、细粒二氧化硅和铝粉的组合构成。
2.用于制造耐高温或耐火的成型体的物料,其由下列材料的混合物构成:
- 耐火或耐高温的无机粉末、颗粒和/或粒料,
- 与由碳制成的可流动物料或粉末,
- 粘合剂,
其特征在于,所述粘合剂由单宁、乳糖、细粒二氧化硅和铝粉的组合构成。
3.用于制造耐火的物料或成型体,特别是用于制造根据权利要求1或2任一项的物料的粘合剂,其特征在于,所述粘合剂由单宁、乳糖、细粒二氧化硅和铝粉的组合构成。
4.根据权利要求3的粘合剂,其特征在于,乳糖与单宁的比率为 0.1至0.3。
5.根据权利要求3的粘合剂,其特征在于,细粒二氧化硅的粒度为小于50 µm,优选小于1 µm,且铝粉的粒度为小于200 µm。
6.根据权利要求3的粘合剂,其特征在于,向所述粘合剂添加最多30重量%的粉末形式的酚树脂,基于乳糖和单宁的混合物计。
7.根据权利要求3的装置,其特征在于,向所述粘合剂添加其它细粒添加剂,即镁或碳化物,特别是SiC、B4C、TiC或氮化物,特别是Si3N4、AlN、TiN或硼化物,特别是BN、Tib2。
8.根据权利要求3的粘合剂,其特征在于,向所述粘合剂加入掺杂硅。
9.根据权利要求3的粘合剂,其特征在于,向所述粘合剂添加乙二醇,优选以0.1至5重量%的量。
10.根据权利要求3的粘合剂,其特征在于,单宁的含量大于乳糖的含量,单宁优选为70至90重量%。
11.根据权利要求2的物料,其特别是具有根据权利要求3至10任一项的粘合剂 ,其特征在于,所添加的碳是石墨和/或炭黑和/或碳纤维材料和/或碳纳米管(CNT)和/或石墨烯和/或预焦化沥青、地沥青或酚树脂。
12.根据权利要求1或2任一项的物料,其具有根据权利要求3至10任一项的粘合剂。
13.根据权利要求1或2任一项的物料,其特征在于,向所述物料添加最多50重量%,优选0.5至20重量%,特别优选2至8重量%的含量的粘合剂。
14.由具有根据权利要求3至10任一项的粘合剂的根据权利要求1、2、11、12和13任一项的物料构成的成型体。
15.由耐高温或耐火的无机粉末、颗粒和/或粒料和粘合剂制造耐火或耐高温的成型体或物料的方法,其特征在于,向< 100 µm的无机细粒添加至少一种> 100 µm 的无机粗粒和碳和基于单宁、乳糖、细粒二氧化硅和铝粉的组合粘合剂,并且——优选在混合机中——混合,所述混合物通过原始成型法,例如浇铸、压制、挤出而转变成产品,所述产品在使用之前或过程中在大于100℃的温度下热处理,优选在两个工艺阶段中,即在最多250℃的第一阶段和高于600℃的温度下的第二阶段中,优选在排除氧气的情况下。
16.根据权利要求15的方法,其通过使用根据权利要求2至13任一项的物料和/或粘合剂。
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DE102016100083.3 | 2016-01-04 | ||
PCT/DE2016/100348 WO2017118449A1 (de) | 2016-01-04 | 2016-07-29 | Feuerfeste formkörper und massen sowie bindemittel und verfahren zu deren herstellung |
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EP3944762A1 (de) * | 2020-07-27 | 2022-02-02 | JFL-Materials GmbH | Biozid mit leitenden eigenschaften und dessen verwendung |
EP4144707A1 (de) | 2021-09-07 | 2023-03-08 | Biolac GmbH & Co. KG | Mischung zur herstellung eines formkörpers mit verbessertem bindemittel |
CN115537626B (zh) * | 2022-09-14 | 2023-05-12 | 首钢集团有限公司 | 一种镁碳耐火材料及其制备方法 |
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PL3400203T3 (pl) | 2020-10-19 |
EP3400203B1 (de) | 2020-04-01 |
DE102016100083B4 (de) | 2019-02-14 |
WO2017118449A1 (de) | 2017-07-13 |
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US20180362408A1 (en) | 2018-12-20 |
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