WO2020057093A1 - 利用氧化硅基固体废弃物制备碳化硅基多孔陶瓷的方法 - Google Patents

利用氧化硅基固体废弃物制备碳化硅基多孔陶瓷的方法 Download PDF

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WO2020057093A1
WO2020057093A1 PCT/CN2019/080543 CN2019080543W WO2020057093A1 WO 2020057093 A1 WO2020057093 A1 WO 2020057093A1 CN 2019080543 W CN2019080543 W CN 2019080543W WO 2020057093 A1 WO2020057093 A1 WO 2020057093A1
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silicon oxide
solid waste
silicon carbide
based solid
silicon
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马北越
任鑫明
苏畅
于景坤
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Northeastern University China
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  • the invention belongs to the technical field of efficient comprehensive utilization of secondary resources and preparation of porous ceramic materials, and relates to a method for preparing silicon carbide-based porous ceramics by using silicon oxide-based solid waste.
  • silicon carbide-based porous ceramics can be applied in various fields, such as: metallurgy, chemical industry, environment, energy and so on.
  • silicon oxide-based solid waste instead of clay as the ceramic raw material can not only reduce the cost of ceramic raw materials, prepare high-performance silicon carbide-based porous ceramics, but also scale and efficiently use a large amount of silicon oxide-based solid waste, which solves the problem of stacking. Problems of land occupation and environmental pollution.
  • the preparation methods of silicon carbide-based porous ceramics mainly include particle stacking sintering method, direct foam molding method and organic foam impregnation method, etc., but it requires higher raw materials and restricts the shape of the product, and the pore-forming agent method can be effective This defect is avoided, and silicon carbide-based porous ceramics with various pore structures and complex shapes are prepared.
  • the purpose of the present invention is to overcome the shortcomings of the prior art mentioned above and provide a method for preparing silicon carbide-based porous ceramics using silicon oxide-based solid waste.
  • the method realizes the efficient comprehensive utilization of silicon oxide-based solid waste, and has the advantages of simple operation, convenient industrial production, and the like.
  • the method for preparing silicon carbide-based porous ceramics from silicon oxide-based solid wastes is performed according to the following steps:
  • Step 1 Raw material processing
  • Silicon oxide-based solid waste is subjected to high-temperature calcination and sieving to obtain silicon-based clinker;
  • the silicon-based clinker: reducing agent: binder: pore-forming agent 100: (5-60): (5-40): (5-60).
  • Step 3 High temperature sintering
  • the dried material is placed in a high-temperature sintering device, sintered in a protective atmosphere, and held for a certain period of time to obtain a silicon carbide-based porous ceramic, and related performance tests are performed on the silicon carbide-based porous ceramic.
  • the silicon oxide-based solid waste is one or more of fly ash, gangue, iron ore tailings, or rice hull ash, and its main components are SiO 2 and Al 2 O 3 .
  • step 1 calcining and crushing and sieving are used to remove impurities in the silicon oxide-based solid waste.
  • the calcining furnace is one of a box-type resistance wire furnace, a silicon carbon rod furnace, a silicon molybdenum rod furnace, or a tunnel kiln used in an unprotected atmosphere.
  • the crushing and sieving process is as follows: a jaw crusher is used for crushing, and the powder is passed through a 200-mesh sieve to obtain a silicon-based clinker.
  • the reducing agent carbon powder is one or more of carbon black, high-quality coal, or activated carbon.
  • the amount of the reducing agent is higher than 5% -20% of the consumption of the reaction between SiO 2 and the reducing agent in the silicon oxide-based solid waste.
  • the binder is one or more of polyvinyl alcohol, phenol resin, water glass, or aluminum dihydrogen phosphate.
  • the pore-forming agent is one or more of starch, graphite powder, ammonium bicarbonate, or ammonium chloride.
  • the material mixing equipment is a high-energy ball mill
  • the rotation speed is 200-600 r ⁇ min -1
  • the running time is 1-10 hours.
  • the forming pressure is 50 to 300 MPa, and the dwell time is 3 to 5 minutes.
  • the drying temperature of the drying operation is 120 ° C
  • the drying time is 12-24 hours
  • the drying equipment is a drying box or a tunnel drying kiln.
  • the protective gas is a high-purity Ar gas.
  • the high-temperature sintering equipment is one of a box-type resistance furnace, a tube-type resistance furnace, a vacuum high-temperature furnace, or a tunnel kiln that can pass through the atmosphere.
  • the sintering temperature is 1400-1800 ° C, and the sintering holding time is 2-10 hours.
  • the main phase of the obtained silicon carbide-based porous ceramic is ⁇ -SiC or ⁇ -Al 2 O 3 , the apparent porosity is 30% to 70%, and the compressive strength at room temperature is 4 to 15 MPa.
  • the pore size distribution is uniform.
  • the present invention is a method for preparing silicon carbide-based porous ceramics using silicon oxide-based solid waste. Compared with the prior art, its beneficial effects are:
  • the method for preparing silicon carbide-based porous ceramics using silicon oxide-based solid wastes of the present invention realizes the efficient and comprehensive utilization of silicon oxide-based solid wastes, which is not only conducive to the production of high-performance silicon carbide-based porous ceramics, but also reduces its impact on Environmental pollution has good economic and environmental benefits.
  • the method for preparing silicon carbide-based porous ceramics using silicon oxide-based solid waste according to the present invention has simple operation and is convenient for industrialized production.
  • the method for preparing silicon carbide-based porous ceramics using silicon oxide-based solid waste according to the present invention seeks alternative raw materials for natural mineral resources, and is inexpensive and pollution-free, thereby achieving the purpose of turning waste into treasure.
  • FIG. 1 is a process flow chart of the present invention.
  • the related tests include phase composition, apparent porosity, and compressive strength at room temperature.
  • the phase composition of the silicon carbide-based porous ceramics is determined by X-ray diffraction (XRD) analysis, and the test conditions are Cu-Ka rays as the light source.
  • the compressive strength at room temperature is tested in accordance with GB / T 1964-1996 Porous Ceramic Compression Test.
  • the method for preparing silicon carbide-based porous ceramics from silicon oxide-based solid wastes is performed according to the following steps:
  • Step 1 Raw material pretreatment
  • Step 3 High temperature sintering
  • the main phases of the obtained silicon carbide-based porous ceramics were ⁇ -SiC and ⁇ -Al 2 O 3 , the apparent porosity was 37%, the compressive strength at room temperature was 8.2 MPa, and the pore size distribution was uniform.
  • the method for preparing silicon carbide-based porous ceramics from silicon oxide-based solid wastes is performed according to the following steps:
  • Step 1 Raw material pretreatment
  • the rice husk ash is placed in a box-type resistance wire furnace, calcined at 1000 ° C for 5 hours, and then crushed by a jaw crusher, and the powder is passed through a 200 mesh sieve to obtain a clinker with good stability;
  • Step 3 High temperature sintering
  • the main phase of the obtained silicon carbide-based porous ceramic was ⁇ -SiC, the apparent porosity was 42%, and the compressive strength at room temperature was 7.8 MPa.
  • the method for preparing silicon carbide-based porous ceramics from silicon oxide-based solid wastes is performed according to the following steps:
  • Step 1 Raw material pretreatment
  • Coal gangue is placed in a box-type resistance wire furnace, calcined at 1000 ° C for 5 hours, and then crushed by a jaw crusher, and the powder is passed through a 200 mesh sieve to obtain a clinker with good stability;
  • Step 3 High temperature sintering
  • the main phases of the obtained silicon carbide-based porous ceramics were ⁇ -SiC and ⁇ -Al 2 O 3 , the apparent porosity was 48%, and the compressive strength at room temperature was 6.7 MPa.
  • the method for preparing silicon carbide-based porous ceramics from silicon oxide-based solid wastes is performed according to the following steps:
  • Step 1 Raw material pretreatment
  • the iron ore tailings are placed in a box resistance wire furnace, calcined at 1000 ° C for 5 hours, and then crushed by a jaw crusher, and the powder is passed through a 200 mesh sieve to obtain a clinker with good stability;
  • Step 3 High temperature sintering
  • the main phases of the obtained silicon carbide-based porous ceramics were ⁇ -SiC and ⁇ -Al 2 O 3 , the apparent porosity was 55%, and the compressive strength at room temperature was 4.5 MPa.
  • the method for preparing silicon carbide-based porous ceramics from silicon oxide-based solid wastes is performed according to the following steps:
  • Step 1 Raw material pretreatment
  • Step 3 High temperature sintering
  • the main phases of the obtained silicon carbide-based porous ceramics were ⁇ -SiC and ⁇ -Al 2 O 3 , the apparent porosity was 65%, the compressive strength at room temperature was 5.6 MPa, and the pore size distribution was uniform.
  • the method for preparing silicon carbide-based porous ceramics from silicon oxide-based solid wastes is performed according to the following steps:
  • Step 1 Raw material pretreatment
  • Step 3 High temperature sintering
  • the main phases of the obtained silicon carbide-based porous ceramics were ⁇ -SiC and ⁇ -Al 2 O 3 , the apparent porosity was 53%, the compressive strength at room temperature was 7.2 MPa, and the pore size distribution was uniform.
  • the method for preparing silicon carbide-based porous ceramics from silicon oxide-based solid wastes is performed according to the following steps:
  • Step 1 Raw material pretreatment
  • Step 3 High temperature sintering
  • the main phases of the obtained silicon carbide-based porous ceramics were ⁇ -SiC and ⁇ -Al 2 O 3 , the apparent porosity was 32%, the compressive strength at room temperature was 8.9 MPa, and the pore size distribution was uniform.

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  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
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Abstract

一种利用氧化硅基固体废弃物制备碳化硅基多孔陶瓷的方法。首先，将氧化硅基固体废弃物进行预处理，除去杂质，其次，根据氧化硅基固体废弃物组分配比掺入还原剂；然后，以预处理后的氧化硅基固体废弃物为原料，加入粘结剂与造孔剂，将物料混匀；最后，经干压成型并干燥，在保护气氛下高温烧结制得碳化硅基多孔陶瓷。该方法实现了氧化硅基固体废弃物的高附加值利用，减少其对环境造成的污染，有利于降低生产成本，而且该方法操作简单易行，便于工业化生产。

Description

利用氧化硅基固体废弃物制备碳化硅基多孔陶瓷的方法 技术领域：
本发明属于二次资源高效综合利用及多孔陶瓷材料制备技术领域，涉及利用氧化硅基固体废弃物制备碳化硅基多孔陶瓷的方法。
背景技术：
随着科学技术的不断进步和社会经济的不断的发展，近年来工业得到了迅速的发展，然而，工业生产过程中产生的固体废弃物也日益增多，已经引起严重的储存和环境污染问题。因此，合理利用工业生产过程中产生的固废资源，变废为宝对全球经济的发展显得尤为重要。
与此同时，陶瓷生产行业的快速发展，对陶瓷原料的需求也是日益增多，陶瓷生产的主要原料粘土为此面临资源枯竭的困境。为此，寻找可替代粘土的陶瓷原料是陶瓷产业的重要研究方向。
其中，碳化硅基多孔陶瓷，可以应用于多种领域，如：冶金、化工、环境、能源等。以氧化硅基固体废弃物代替黏土作为陶瓷原料，既可以降低陶瓷原料的成本，制备出高性能碳化硅基多孔陶瓷，又可规模化高效利用大量的氧化硅基固体废弃物，解决了其堆放占用土地及污染环境的问题。
目前，碳化硅基多孔陶瓷的制备方法主要有颗粒堆积烧结法、直接发泡成型法和有机泡沫浸渍法等，但其对原料要求较高且限制制品的形状，而添加造孔剂法可有效避免这一缺陷，制备出气孔结构多样、形状复杂的碳化硅基多孔陶瓷。
发明内容：
本发明的目的是克服上述现有技术存在的不足，提供利用氧化硅基固体废弃物制备碳化硅基多孔陶瓷的方法。该方法实现了氧化硅基固体废弃物的高效综合利用；而且具有操作简单易行，便于工业化生产等优点。
利用氧化硅基固体废弃物制备碳化硅基多孔陶瓷的方法，按以下步骤进行：
步骤1：原料处理
将氧化硅基固体废弃物经高温煅烧与粉碎过筛处理，制得硅基熟料；
步骤2：干压成型
(1)按配比，硅基熟料：还原剂：粘结剂：造孔剂＝100:(5～60):(5～40):(5～60)，将物料混合均匀，球磨得混匀物料；
(2)将混匀物料干压成型，并干燥；
步骤3：高温烧结
将干燥后物料置于高温烧结设备中，于保护气氛下烧结并保温一定时间，制得碳化硅基多孔陶瓷，并对碳化硅基多孔陶瓷进行相关性能测试。
所述的步骤1中，所述的氧化硅基固体废弃物为粉煤灰、煤矸石、铁矿石尾矿或稻壳灰中的一种或几种，其主要成分是SiO 2和Al 2O 3。
所述的步骤1中，煅烧与粉碎过筛处理用于去除氧化硅基固体废弃物中的杂质。
所述的步骤1中，所述的煅烧炉为在无保护气氛下使用的箱式电阻丝炉、硅碳棒炉、硅钼棒炉或隧道窑中的一种。
所述的步骤1中，所述的粉碎过筛处理过程为：采用颚式破碎机粉碎处理，粉末经200目筛后，制得硅基熟料。
所述的步骤2(1)中，所述的还原剂碳粉为炭黑、优质煤或活性炭中的一种或多种。
所述的步骤2(1)中，所述的还原剂用量高于氧化硅基固体废弃物中SiO 2与还原剂反应消耗量的5％～20％。
所述的步骤2(1)中，所述的粘结剂为聚乙烯醇、酚醛树脂、水玻璃或磷酸二氢铝中的一种或多种。
所述的步骤2(1)中，所述的造孔剂为淀粉、石墨粉、碳酸氢铵或氯化铵中的一种或多种。
所述的步骤2(1)中，所述的物料混合设备为高能球磨机，其转速为200～600r·min -1，运行时间为1～10h。
所述的步骤2(2)中，所述的成型压力为50～300MPa，保压时间为3～5min。
所述的步骤2(2)中，所述的干燥操作的干燥温度为120℃，干燥时间为12～24h，干燥设备为干燥箱或隧道干燥窑。
所述的步骤3中，所述的保护气为高纯度的Ar气。
所述的步骤3中，高温烧结设备为可通气氛的箱式电阻炉、管式电阻炉、真空高温炉或隧道窑中的一种。
所述的步骤3中，烧结温度为1400～1800℃，烧结保温时间为2～10h。
所述的步骤3中，制得的碳化硅基多孔陶瓷的主要物相为β-SiC或α-Al 2O 3，显气孔率为30％～70％，常温抗压强度为4～15MPa，孔径分布均匀。
本发明为利用氧化硅基固体废弃物制备碳化硅基多孔陶瓷的方法，与现有技术相比，其有益效果在于：
1.本发明的利用氧化硅基固体废弃物制备碳化硅基多孔陶瓷的方法实现了氧化硅基固体废弃物的高效综合利用，不仅利于制得高性能的碳化硅基多孔陶瓷，还减少其对环境产生 的污染，具有较好的经济效益和环保效益。
2.本发明的利用氧化硅基固体废弃物制备碳化硅基多孔陶瓷的方法操作简单易行，便于工业化生产。
3.本发明的利用氧化硅基固体废弃物制备碳化硅基多孔陶瓷的方法，为天然矿物资源寻找可代替的原料，且其价格低廉、无污染，达到了变废为宝的目的。
附图说明：
图1是本发明的工艺流程图。
具体实施方式：
下面结合实施例对本发明作进一步的详细说明。
所述的相关检测包括物相组成、显气孔率和常温抗压强度；其中，碳化硅基多孔陶瓷的物相组成采用X射线衍射仪(XRD)分析鉴定，测试条件为Cu-Ka射线作为光源，管电压30kV，管电流30mA，扫描形式为步进扫描，步长为0.02°，扫描速度为9℃/min，扫描范围为5°～90°；显气孔率按照GB/T 1997-2000测定，常温抗压强度按照GB/T 1964-1996多孔陶瓷耐压试验法进行测试。
实施例1
利用氧化硅基固体废弃物制备碳化硅基多孔陶瓷的方法，按以下步骤进行：
步骤1：原料预处理
(1)将粉煤灰置于箱式电阻丝炉中，1000℃下煅烧5h，再经颚式破碎机粉碎，粉末过200目筛，得到稳定性良好的熟料；
(2)根据粉煤灰中SiO 2的组成配比，配制活性炭；
步骤2：干压成型
(1)选取酚醛树脂为粘结剂，碳酸氢铵为造孔剂，按粉煤灰:活性炭:酚醛树脂:碳酸氢氨＝100:30:5:10的质量配比称量原料，并将其高能球磨1h；
(2)将混匀物料置于压力机中干压成型，100MPa下保压5min，并置于干燥箱中120℃下保温24h；
步骤3：高温烧结
将干燥后物料置于1400℃的真空高温炉中，Ar气氛下烧结2h，待高温炉冷却至室温，得到碳化硅基多孔陶瓷，并对碳化硅基多孔陶瓷进行相关性能测试；
经检测，所得碳化硅基多孔陶瓷的主要物相为β-SiC和α-Al 2O 3,显气孔率为37％，常温抗压强度为8.2MPa，孔径分布均匀。
实施例2
利用氧化硅基固体废弃物制备碳化硅基多孔陶瓷的方法，按以下步骤进行：
步骤1：原料预处理
(1)将稻壳灰置于箱式电阻丝炉中，1000℃下煅烧5h，再经颚式破碎机粉碎，粉末过200目筛，得到稳定性良好的熟料；
(2)根据稻壳灰中SiO 2的组成配比，配制炭黑；
步骤2：干压成型
(1)选取酚醛树脂为粘结剂，碳酸氢铵为造孔剂，按稻壳灰:炭黑:酚醛树脂:碳酸氢氨＝100:60:30:10的质量配比称量原料，并将其高能球磨1h；
(2)将混匀物料置于压力机中干压成型，100MPa下保压5min，并置于干燥箱中120℃下保温24h；
步骤3：高温烧结
将干燥后物料置于1400℃的真空高温炉中，Ar气氛下烧结2h，待高温炉冷却至室温，得到碳化硅基多孔陶瓷，并对碳化硅基多孔陶瓷进行相关性能测试；
经检测，所得碳化硅基多孔陶瓷的主要物相为β-SiC，显气孔率为42％，常温抗压强度为7.8MPa。
实施例3
利用氧化硅基固体废弃物制备碳化硅基多孔陶瓷的方法，按以下步骤进行：
步骤1：原料预处理
(1)将煤矸石置于箱式电阻丝炉中，1000℃下煅烧5h，再经颚式破碎机粉碎，粉末过200目筛，得到稳定性良好的熟料；
(2)根据煤矸石中SiO 2的组成配比，配制炭黑；
步骤2：干压成型
(1)选取酚醛树脂为粘结剂，碳酸氢铵为造孔剂，按煤矸石:炭黑:酚醛树脂:碳酸氢氨＝100:45:40:10的质量配比称量原料，并将其高能球磨3h；
(2)将混匀物料置于压力机中干压成型，100MPa下保压5min，并置于干燥箱中120℃下保温24h；
步骤3：高温烧结
将干燥后物料置于1600℃的真空高温炉中，Ar气氛下烧结4h，待高温炉冷却至室温，得到碳化硅基多孔陶瓷，并对碳化硅基多孔陶瓷进行相关性能测试；
经检测，所得碳化硅基多孔陶瓷的主要物相为β-SiC和α-Al 2O 3，显气孔率为48％，常温抗压强度为6.7MPa。
实施例4
利用氧化硅基固体废弃物制备碳化硅基多孔陶瓷的方法，按以下步骤进行：
步骤1：原料预处理
(1)将铁矿石尾矿置于箱式电阻丝炉中，1000℃下煅烧5h，再经颚式破碎机粉碎，粉末过200目筛，得到稳定性良好的熟料；
(2)根据铁矿石尾矿中SiO 2的组成配比，配制炭黑；
步骤2：干压成型
(1)选取磷酸二氢铝为粘结剂，石墨粉为造孔剂，按铁矿石尾矿:炭黑:磷酸二氢铝:石墨粉＝100:5:20:20的质量配比称量原料，并将其高能球磨5h；
(2)将混匀物料置于压力机中干压成型，100MPa下保压5min，并置于干燥箱中120℃下保温24h；
步骤3：高温烧结
将干燥后物料置于1700℃的真空高温炉中，Ar气氛下烧结6h，待高温炉冷却至室温，得到碳化硅基多孔陶瓷，并对碳化硅基多孔陶瓷进行相关性能测试；
经检测，所得碳化硅基多孔陶瓷的主要物相为β-SiC和α-Al 2O 3，显气孔率为55％，常温抗压强度为4.5MPa。
实施例5
利用氧化硅基固体废弃物制备碳化硅基多孔陶瓷的方法，按以下步骤进行：
步骤1：原料预处理
(1)将粉煤灰置于箱式电阻丝炉中，1000℃下煅烧5h，再经颚式破碎机粉碎，粉末过200目筛，得到稳定性良好的熟料；
(2)根据粉煤灰中SiO 2的组成配比，配制活性炭；
步骤2：干压成型
(1)选取酚醛树脂为粘结剂，碳酸氢铵为造孔剂，按粉煤灰:活性炭:酚醛树脂:碳酸氢氨＝100:60:15:60的质量配比称量原料，并将其高能球磨1h；
(2)将混匀物料置于压力机中干压成型，100MPa下保压5min，并置于干燥箱中120℃下保温24h；
步骤3：高温烧结
将干燥后物料置于1400℃的真空高温炉中，Ar气氛下烧结2h，待高温炉冷却至室温，得到碳化硅基多孔陶瓷，并对碳化硅基多孔陶瓷进行相关性能测试；
经检测，所得碳化硅基多孔陶瓷的主要物相为β-SiC和α-Al 2O 3,显气孔率为65％，常温 抗压强度为5.6MPa，孔径分布均匀。
实施例6
利用氧化硅基固体废弃物制备碳化硅基多孔陶瓷的方法，按以下步骤进行：
步骤1：原料预处理
(1)将粉煤灰置于箱式电阻丝炉中，1000℃下煅烧5h，再经颚式破碎机粉碎，粉末过200目筛，得到稳定性良好的熟料；
(2)根据粉煤灰中SiO 2的组成配比，配制活性炭；
步骤2：干压成型
(1)选取酚醛树脂为粘结剂，碳酸氢铵为造孔剂，按粉煤灰:活性炭:酚醛树脂:碳酸氢氨＝100:30:25:60的质量配比称量原料，并将其高能球磨1h；
(2)将混匀物料置于压力机中干压成型，300MPa下保压5min，并置于干燥箱中120℃下保温24h；
步骤3：高温烧结
将干燥后物料置于1400℃的真空高温炉中，Ar气氛下烧结2h，待高温炉冷却至室温，得到碳化硅基多孔陶瓷，并对碳化硅基多孔陶瓷进行相关性能测试；
经检测，所得碳化硅基多孔陶瓷的主要物相为β-SiC和α-Al 2O 3,显气孔率为53％，常温抗压强度为7.2MPa，孔径分布均匀。
实施例7
利用氧化硅基固体废弃物制备碳化硅基多孔陶瓷的方法，按以下步骤进行：
步骤1：原料预处理
(1)将粉煤灰置于箱式电阻丝炉中，1000℃下煅烧5h，再经颚式破碎机粉碎，粉末过200目筛，得到稳定性良好的熟料；
(2)根据粉煤灰中SiO 2的组成配比，配制活性炭；
步骤2：干压成型
(1)选取酚醛树脂为粘结剂，碳酸氢铵为造孔剂，按粉煤灰:活性炭:酚醛树脂:碳酸氢氨＝100:30:5:10的质量配比称量原料，并将其高能球磨1h；
(2)将混匀物料置于压力机中干压成型，100MPa下保压5min，并置于干燥箱中120℃下保温24h；
步骤3：高温烧结
将干燥后物料置于1800℃的真空高温炉中，Ar气氛下烧结2h，待高温炉冷却至室温，得到碳化硅基多孔陶瓷，并对碳化硅基多孔陶瓷进行相关性能测试；
经检测，所得碳化硅基多孔陶瓷的主要物相为β-SiC和α-Al 2O 3,显气孔率为32％，常温抗压强度为8.9MPa，孔径分布均匀。

Claims (10)

  1. 利用氧化硅基固体废弃物制备碳化硅基多孔陶瓷的方法，按以下步骤进行：
    步骤1：原料处理
    将氧化硅基固体废弃物经高温煅烧与粉碎过筛处理，制得硅基熟料；
    步骤2：干压成型
    (1)按配比，硅基熟料：还原剂：粘结剂：造孔剂＝100:(5～60):(5～40):(5～60)，将物料混合均匀，球磨得混匀物料；
    (2)将混匀物料干压成型，并干燥；
    步骤3：高温烧结
    将干燥后物料置于高温烧结设备中，于保护气氛下烧结并保温一定时间，制得碳化硅基多孔陶瓷，并对碳化硅基多孔陶瓷进行相关性能测试。
  2. 根据权利要求1所述的方法，其特征在于，所述的步骤1中，所述的氧化硅基固体废弃物为粉煤灰、煤矸石、铁矿石尾矿或稻壳灰中的一种或几种，其主要成分是SiO 2和Al 2O 3。
  3. 根据权利要求1所述的方法，其特征在于，所述的步骤1中，所述的煅烧与粉碎过筛处理用于去除氧化硅基固体废弃物中的杂质；所述的煅烧炉为在无保护气氛下使用的箱式电阻丝炉、硅碳棒炉、硅钼棒炉或隧道窑中的一种；所述的粉碎过筛处理过程为采用颚式破碎机粉碎处理，粉末经200目筛。
  4. 根据权利要求1所述的方法，其特征在于，所述的步骤2(1)中，所述的还原剂碳粉为炭黑、优质煤或活性炭中的一种或多种；所述的还原剂用量高于氧化硅基固体废弃物中SiO 2与还原剂反应消耗量的5％～20％。
  5. 根据权利要求1所述的方法，其特征在于，所述的步骤2(1)中，所述的粘结剂为聚乙烯醇、酚醛树脂、水玻璃或磷酸二氢铝中的一种或多种。
  6. 根据权利要求1所述的方法，其特征在于，所述的步骤2(1)中，所述的造孔剂为淀粉、石墨粉、碳酸氢铵或氯化铵中的一种或多种。
  7. 根据权利要求1所述的方法，其特征在于，所述的步骤2(1)中，所述的物料混合设备为高能球磨机，其转速为200～600r·min -1，运行时间为1～10h。
  8. 根据权利要求1所述的方法，其特征在于，所述的步骤2(2)中，所述的成型压力为50～300MPa，保压时间为3～5min；所述的干燥操作的干燥温度为120℃，干燥时间为12～24h，干燥设备为干燥箱或隧道干燥窑。
  9. 根据权利要求1所述的方法，其特征在于，所述的步骤3中，所述的保护气为高纯度的Ar气。
  10. 根据权利要求1所述的方法，其特征在于，所述的步骤3中，所述的高温烧结设备 为可通气氛的箱式电阻炉、管式电阻炉、真空高温炉或隧道窑中的一种；烧结温度为1400～1800℃，烧结保温时间为2～10h。
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CN107399988A (zh) * 2017-08-22 2017-11-28 东北大学 一种利用铝硅系工业废渣制备氧化铝‑碳化硅复合多孔陶瓷的方法
CN107686369A (zh) * 2017-08-22 2018-02-13 东北大学 一种用晶体硅的碳化硅切割废料制备碳化硅多孔陶瓷的方法
CN109133934A (zh) * 2018-09-20 2019-01-04 东北大学 利用氧化硅基固体废弃物制备碳化硅基多孔陶瓷的方法

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CN118271115A (zh) * 2024-03-29 2024-07-02 中冶建筑研究总院有限公司 一种基于固废材料的吸音隔音陶瓷材料及其制备方法和应用

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