CN116102343B - 危废焚烧系统回转窑用耐酸耐盐改性刚玉砖及制备方法 - Google Patents
危废焚烧系统回转窑用耐酸耐盐改性刚玉砖及制备方法 Download PDFInfo
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- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims description 12
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- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
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Abstract
本发明公开了危废焚烧系统回转窑用耐酸耐盐改性刚玉砖及制备方法,改性刚玉砖按重量份数计包括:45~50份的致密电熔刚玉、20~30份的棕刚玉、10~15份的磷酸氧锆‑改性氧化锆复合体、10~15份的红柱石,5~10份的硅灰,本发明采用致密电熔刚玉与棕刚玉作为烧制刚玉砖的主材料,可以使烧成的刚玉砖具有良好的耐磨性、耐酸耐盐性以及抗侵蚀性等,由于致密电熔刚玉与棕刚玉价格低廉,可以节省刚玉砖的烧制成本,加入磷酸氧锆‑改性氧化锆复合体可显著增加刚玉砖的强度,添加红柱石可增加刚玉砖的抗热震性以及耐酸耐盐性,添加硅灰可以提高刚玉砖的抗渗、防腐能力,并且硅灰遇水会生成凝胶体,产生的凝胶体可对混合物中的缝隙起到填补的作用。
Description
技术领域
本发明涉及刚玉砖制备技术领域,具体是涉及危废焚烧系统回转窑用耐酸耐盐改性刚玉砖及制备方法。
背景技术
回转窑式焚烧炉是处理危废的主要设备之一,由于近年来危废物料中高热值组分逐年增加,导致回转窑实际运行温度大幅超过设计温度,同时很多危废处理厂为了确保烟气排放达到环保要求而提高烟气温度,也导致回转窑实际运行温度大幅提高,回转窑内温度的提高造成物料灰渣大量熔融,耐火材料损耗由每月5~7mm增加至每月10~15mm甚至更高。
刚玉砖,是以刚玉为主晶相的耐火材料制品,主要用于炼铁高炉、高炉热风炉、炼钢炉外精炼炉、玻璃熔窑以及石油化工工业炉等,现有技术中危废焚烧系统回转窑用刚玉砖的耐酸耐盐性较差,在使用的过程中经常会出现刚玉砖受腐蚀而导致需要经常更换的问题,这就会导致回转窑焚烧处理的效率下降,因此现需要危废焚烧系统回转窑用耐酸耐盐改性刚玉砖及制备方法。
发明内容
为解决上述技术问题,本发明提供了危废焚烧系统回转窑用耐酸耐盐改性刚玉砖及制备方法。
本发明的技术方案是:危废焚烧系统回转窑用耐酸耐盐改性刚玉砖,所述改性刚玉砖按重量份数计包括:45~50份的致密电熔刚玉、20~30份的棕刚玉、10~15份的磷酸氧锆-改性氧化锆复合体、10~15份的红柱石,5~10份的硅灰;
其中,磷酸氧锆-改性氧化锆复合体的制备方法为:
S1、磷酸氧锆制备
将二氯氧化锆与质量浓度为85%的磷酸溶液按质量比1:1.5加入至烧杯中,在60~90℃的条件下搅拌4.5h,接着用200目筛网对烧杯内的混合物进行过滤,将过滤出的沉淀物放置于干燥机内在150℃的条件下干燥5h,将干燥后的沉淀物在1500℃的条件下烧制1h得到磷酸氧锆粉末;
S2、改性氧化锆制备
S2-1:溶胶制备
将质量浓度为75%的氯氧化锆溶液与氨水按体积比1:1进行混合,在室温条件下搅拌2h形成含水的二氧化锆沉淀物,接着在65~70℃条件下搅拌3.5h,在搅拌的过程中以0.5ml/s的速率向含水的二氧化锆沉淀物中加入催化剂制得溶胶;
S2-2:凝胶制备
将步骤S2-1中制备的溶胶与水按质量比1:5进行混合,在10℃的条件下静置12h,接着将溶胶与水的混合物与稀土按体积比3:1加入至离心机中以5r/s的速率进行离心15~20h形成凝胶;
S2-3:制作改性氧化锆晶体
将步骤S2-2中制备的凝胶放入烘干机中,在230℃条件下烘干1.5h制成干凝胶,将干凝胶在1300℃的温度下煅烧5h后以5℃/min的速率冷却至室温得到改性氧化锆晶体;
S3、磷酸氧锆-改性氧化锆复合体制备
将步骤S1中制得的磷酸氧锆粉末与步骤S2中制得的改性氧化锆晶体按质量比1:1进行混合均匀,在1300~1500℃的条件下煅烧20h形成磷酸氧锆-改性氧化锆复合体。
说明:本发明采用致密电熔刚玉与棕刚玉作为烧制刚玉砖的主材料,不仅可以使烧成的刚玉砖具有良好的耐磨性、耐酸耐盐性以及抗侵蚀性等,并且由于致密电熔刚玉与棕刚玉价格低廉,还可以节省刚玉砖的烧制成本,在材料中加入磷酸氧锆-改性氧化锆复合体可显著增加刚玉砖的强度,提高了刚玉砖的使用寿命,在材料中添加红柱石可增加刚玉砖的抗热震性以及耐酸耐盐性,在材料中添加硅灰可以提高刚玉砖的抗渗、防腐能力,并且硅灰遇水会生成凝胶体,产生的凝胶体可对混合物中的缝隙起到填补的作用,可降低刚玉砖的气孔率,避免了焦炭及其炼焦产物对刚玉砖内部的渗透侵蚀,增加了刚玉砖的使用寿命;
并且通过上述方法制作磷酸氧锆-改性氧化锆复合体,相比于磷酸氧锆与氧化锆来说,具有高温下稳定、耐热性较高、高强度以及低热膨胀性的特点,在氧化锆中加入稀土改性,可有效提高材料的硬度、抗热震性以及抗老化性等性能,进一步提高了刚玉砖的使用寿命,并且磷酸氧锆与氧化锆在高温下不会发生反应,可有效地进行结合。
进一步地,所述步骤S2-1中使用的催化剂为质量浓度为99%的浓度冰醋酸,加入冰醋酸的量为含水的二氧化锆沉淀物质量的5%。
说明:选用质量浓度为99%的浓度冰醋酸作为催化剂,可使含水二氧化锆沉淀物的PH提高,从而有效降低溶胶所需要的时间。
进一步地,所述步骤S2-2中加入的稀土为CeO2、Y2O3、Sc2O3其中的任意一种或多种。
说明:利用稀土对氧化锆进行改性,可有效提刚玉砖的硬度、抗热震稳定性等性能,添加CeO2可使刚玉砖的断裂韧度得到提高,并且可使刚玉砖的抗老化性能得到提高,添加Y2O3可使刚玉砖的熔点以及抗热震稳定性得到提高,并且可使刚玉砖的热导率降低并且提高了刚玉砖的耐酸耐盐性,添加Sc2O3可使刚玉砖得耐热性以及抗热震稳定性得到显著的提高。
进一步地,在步骤S3煅烧的过程中,加入TiO2作为烧结助熔剂,加入TiO2的量为磷酸氧锆粉末与改性氧化锆晶体混合物质量的3~8%。
说明:在煅烧的过程中加入TiO2作为烧结助熔剂,可以在高温下促进磷酸氧锆-改性氧化锆复合体的致密性,并且可以提高磷酸氧锆-改性氧化锆复合体的强度。
进一步地,所述的危废焚烧系统回转窑用耐酸耐盐改性刚玉砖的制备方法,包括以下步骤:
S1、将致密电熔刚玉、棕刚玉、磷酸氧锆-改性氧化锆复合体、红柱石以及硅灰分别放入碎料机中进行碎料,利用筛网分别对粉碎完成后的原料进行筛选;
S2、将步骤S1中筛选出的原料投放至碾轮式混料机中预混料15min使各原材料进行充分混合,接着向混料机中加入与原材料质量比1:1.5的水继续混料3h后形成具有流动性的砂浆;
S3、将步骤S2中制备的砂浆倒入模具中,将模具放置于室温条件下自然干燥48h然后脱模;
S4、将步骤S3中制备的混凝土块放入至高温电炉中进行烧结制成刚玉砖。
说明:通过上述方法,首先将原材料放入破碎机中进行破碎,之后再经过筛网筛选,可以使后续制作的刚玉砖更加细密,避免了因原材料大小不一而导致烧结过后刚玉砖出现大量裂缝的问题,将原材料充分的进行混合形成砂浆,避免了后续烧制过程中因砂浆混合不均匀而出现气孔率过高的问题。
进一步地,步骤S1中选用的筛网为800目筛网。
说明:通过利用800目的筛网对粉碎过后的原材料进行筛选,首先可以保证后续混料过程中各原材料的尺径统一,也避免了使用过细筛网而导致原材料出现浪费的问题。
进一步地,在步骤S2中原料加水进行混料的同时向混料机中加入与原料质量比0.1:1的结合剂,所述结合剂按重量百分比计包括:55~60%的SiO2,10~15%的Al2O3,余量为水。
说明:在混料时添加结合剂可以有效提高混合物的致密性,SiO2采用纳米氧化硅胶体,吸附性较强,可使各原料之间更好得进行结合,降低了气孔率,Al2O3可有效提高混合物的耐火性。
进一步地,在步骤S3中的烧结方法为:从室温以5℃/s的速率升温至900℃后保持1h,接着以2℃/s的速率升温至1300~1600℃后保持2h。
说明:通过上述方法进行烧结,可使混凝土块快速成型,并且在成型温度下保持1h后再继续升温,避免了短时间内升温速率过快而导致混凝土块内水分蒸发过快出现裂纹而导致烧结失败的问题出现。
本发明的有益效果是:
(1)本发明采用致密电熔刚玉与棕刚玉作为烧制刚玉砖的主材料,不仅可以使烧成的刚玉砖具有良好的耐磨性、耐酸耐盐性以及抗侵蚀性等,并且由于致密电熔刚玉与棕刚玉价格低廉,还可以节省刚玉砖的烧制成本,在材料中加入磷酸氧锆-改性氧化锆复合体可显著增加刚玉砖的强度,提高了刚玉砖的使用寿命。
(2)本发明在材料中添加红柱石可增加刚玉砖的抗热震性以及耐酸耐盐性,在材料中添加硅灰可以提高刚玉砖的抗渗、防腐能力,并且硅灰遇水会生成凝胶体,产生的凝胶体可对混合物中的缝隙起到填补的作用,可降低刚玉砖的气孔率,避免了焦炭及其炼焦产物对刚玉砖内部的渗透侵蚀,增加了刚玉砖的使用寿命。
(3)本发明并通过制作磷酸氧锆-改性氧化锆复合体,相比于磷酸氧锆与氧化锆来说,具有高温下稳定、耐热性较高、高强度以及低热膨胀性的特点,在氧化锆中加入稀土改性,可有效提高材料的硬度、抗热震性以及抗老化性等性能,进一步提高了刚玉砖的使用寿命,并且磷酸氧锆与氧化锆在高温下不会发生反应,可有效地进行结合。
具体实施方式
下面结合具体实施方式来对本发明进行更进一步详细的说明,以更好地体现本发明的优势。
实施例1
危废焚烧系统回转窑用耐酸耐盐改性刚玉砖,所述改性刚玉砖按重量份数计包括:50份的致密电熔刚玉、30份的棕刚玉、15份的磷酸氧锆-改性氧化锆复合体、15份的红柱石,10份的硅灰;
其中,磷酸氧锆-改性氧化锆复合体的制备方法为:
S1、磷酸氧锆制备
将二氯氧化锆与质量浓度为85%的磷酸溶液按质量比1:1.5加入至烧杯中,在90℃的条件下搅拌4.5h,接着用200目筛网对烧杯内的混合物进行过滤,将过滤出的沉淀物放置于干燥机内在150℃的条件下干燥5h,将干燥后的沉淀物在1500℃的条件下烧制1h得到磷酸氧锆粉末;
S2、改性氧化锆制备
S2-1:溶胶制备
将质量浓度为75%的氯氧化锆溶液与氨水按体积比1:1进行混合,在室温条件下搅拌2h形成含水的二氧化锆沉淀物,接着在70℃条件下搅拌3.5h,在搅拌的过程中以0.5ml/s的速率向含水的二氧化锆沉淀物中加入质量浓度为99%的浓度冰醋酸,加入冰醋酸的量为含水的二氧化锆沉淀物质量的5%制得溶胶;
S2-2:凝胶制备
将步骤S2-1中制备的溶胶与水按质量比1:5进行混合,在10℃的条件下静置12h,接着将溶胶与水的混合物与CeO2按体积比3:1加入至离心机中以5r/s的速率进行离心20h形成凝胶;
S2-3:制作改性氧化锆晶体
将步骤S2-2中制备的凝胶放入烘干机中,在230℃条件下烘干1.5h制成干凝胶,将干凝胶在1300℃的温度下煅烧5h后以5℃/min的速率冷却至室温得到改性氧化锆晶体;
S3、磷酸氧锆-改性氧化锆复合体制备
将步骤S1中制得的磷酸氧锆粉末与步骤S2中制得的改性氧化锆晶体按质量比1:1进行混合均匀,在1500℃的条件下煅烧20h形成磷酸氧锆-改性氧化锆复合体,在煅烧的过程中加入TiO2作为烧结助熔剂,加入TiO2的量为磷酸氧锆粉末与改性氧化锆晶体混合物质量的8%。
实施例2
与实施例1不同之处在于:
改性刚玉砖按重量份数计包括:47份的致密电熔刚玉、25份的棕刚玉、13份的磷酸氧锆-改性氧化锆复合体、13份的红柱石,7份的硅灰。
实施例3
与实施例1不同之处在于:
改性刚玉砖按重量份数计包括:45份的致密电熔刚玉、20份的棕刚玉、10份的磷酸氧锆-改性氧化锆复合体、10份的红柱石,5份的硅灰。
实施例4
与实施例1不同之处在于:
步骤S1中,将二氯氧化锆与质量浓度为85%的磷酸溶液按质量比1:1.5加入至烧杯中,在75℃的条件下搅拌4.5h。
实施例5
与实施例1不同之处在于:
步骤S1中,将二氯氧化锆与质量浓度为85%的磷酸溶液按质量比1:1.5加入至烧杯中,在60℃的条件下搅拌4.5h。
实施例6
与实施例1不同之处在于:
步骤S1中,将质量浓度为75%的氯氧化锆溶液与氨水按体积比1:1进行混合,在室温条件下搅拌2h形成含水的二氧化锆沉淀物,接着在67℃条件下搅拌3.5h。
实施例7
与实施例1不同之处在于:
步骤S1中,将质量浓度为75%的氯氧化锆溶液与氨水按体积比1:1进行混合,在室温条件下搅拌2h形成含水的二氧化锆沉淀物,接着在65℃条件下搅拌3.5h。
实施例8
与实施例1不同之处在于:
步骤S2-2中,将溶胶与水的混合物与CeO2按体积比3:1加入至离心机中以5r/s的速率进行离心17h形成凝胶。
实施例9
与实施例1不同之处在于:
步骤S2-2中,将溶胶与水的混合物与CeO2按体积比3:1加入至离心机中以5r/s的速率进行离心15h形成凝胶。
实施例10
与实施例1不同之处在于:
步骤S2-2中,将溶胶与水的混合物与CeO2与Y2O3按体积比3:1加入至离心机中以5r/s的速率进行离心20h形成凝胶,CeO2与Y2O3的重量比为1:2。
实施例11
与实施例1不同之处在于:
步骤S2-2中,将溶胶与水的混合物与CeO2、Y2O3与Sc2O3按体积比3:1加入至离心机中以5r/s的速率进行离心20h形成凝胶,CeO2、Y2O3与Sc2O3的重量比为1:1:2。
实施例12
本实施例记载的实施例1的危废焚烧系统回转窑用耐酸耐盐改性刚玉砖的制备方法,其特征在于,包括以下步骤:
S1、将致密电熔刚玉、棕刚玉、磷酸氧锆-改性氧化锆复合体、红柱石以及硅灰分别放入碎料机中进行碎料,利用800目筛网分别对粉碎完成后的原料进行筛选;
S2、将步骤S1中筛选出的原料投放至碾轮式混料机中预混料15min使各原材料进行充分混合,接着向混料机中加入与原材料质量比1:1.5的水,并向混料机中加入与原料质量比0.1:1的结合剂,所述结合剂按重量百分比计包括:60%的SiO2,15%的Al2O3,余量为水,继续混料3h后形成具有流动性的砂浆;
S3、将步骤S2中制备的砂浆倒入模具中,将模具放置于室温条件下自然干燥48h然后脱模;
S4、将步骤S3中制备的混凝土块放入至高温电炉中从室温以5℃/s的速率升温至900℃后保持1h,接着以2℃/s的速率升温至1600℃后保持2h制成刚玉砖。
实施例13
与实施例12不同之处在于:
所述结合剂按重量百分比计包括:57%的SiO2,13%的Al2O3,余量为水。
实施例14
与实施例12不同之处在于:
所述结合剂按重量百分比计包括:55%的SiO2,10%的Al2O3,余量为水。
实施例15
与实施例12不同之处在于:
步骤S3中,以2℃/s的速率升温至1450℃后保持2h制成刚玉砖。
实施例16
与实施例12不同之处在于:
步骤S3中,以2℃/s的速率升温至1300℃后保持2h制成刚玉砖。
实验例
1、探究烧制刚玉砖时各材料用量不同对刚玉砖性能的影响
表1实施例1-3中各材料用量不同对刚玉砖性能的影响
结论:不同的致密电熔刚玉、棕刚玉、磷酸氧锆-改性氧化锆复合体、红柱石、硅灰的用量,对刚玉砖的性能有着一定的影响,由表一可得,实施例1中各材料的用量为烧制刚玉砖时的最佳用量。
2、探究搅拌温度不同对沉淀物析出率的影响
表2实施例1、实施例4、实施例5中搅拌温度不同对沉淀物析出率的影响
组别 | 温度 | 沉淀物析出率 |
实施例1 | 90℃ | 99.6% |
实施例3 | 75℃ | 95.3% |
实施例4 | 60℃ | 87.6% |
结论:在不同温度下对二氯氧化锆与85%磷酸溶液的混合溶液进行搅拌,所得的沉淀物的量也不同,温度越高,沉淀物的析出率越高,由表2数据可得实施例1中的搅拌温度为最优搅拌温度。
3、探究不同温度下搅拌对溶胶率的影响
表3实施例1、实施例6、实施例7中不同温度下搅拌对溶胶率的影响
组别 | 温度 | 溶胶率 |
实施例1 | 70℃ | 90% |
实施例6 | 67℃ | 86.2% |
实施例7 | 65℃ | 81.7% |
结论:在不同温度下搅拌对溶胶率有着一定的影响,温度越高溶胶率越高,由表3数据可得,实施例1中的搅拌温度为最优搅拌温度。
4、探究离心的时间对凝胶成胶率的影响
表4实施例1、实施例8、实施例9中离心的时间对凝胶成胶率的影响
组别 | 离心时间 | 成胶率 |
实施例1 | 20h | 94.1% |
实施例8 | 17h | 99.8% |
实施例9 | 15h | 96.3% |
结论:离心的时间对凝胶成胶率有着一定的影响,在离心机中离心的时间过短会导致凝胶成胶率过低,在离心机中离心的时间过长反而也会使凝胶成胶率降低,因此由表4数据可得,实施例8中的离心时间为最优离心时间。
5、探究加入稀土种类的不同对刚玉砖性能的影响
表5实施例1、实施例10、实施例11中加入稀土种类的不同对刚玉砖性能的影响
结论:加入稀土种类的不同对刚玉砖性能有着一定的影响,由表5数据可得,实施例11的添加种类为最优选择,但是由于Sc2O3的材料结构复杂,制备起来较困难,因此实施例10的添加种类为最优选择。
6、探究结合剂中成分的不同对刚玉砖气孔率以及耐热性的影响
表6实施例12、实施例13、实施例14结合剂中成分的不同对刚玉砖气孔率以及耐热性的影响
组别 | SiO2含量 | Al2O3含量 | 水含量 | 气孔率 | 耐热性 |
实施例12 | 60% | 15% | 25% | 10.3% | 2550℃ |
实施例13 | 57% | 13% | 30% | 12.8% | 2320℃ |
实施例14 | 55% | 10% | 35% | 14.1% | 2170℃ |
结论:结合剂中成分的不同对刚玉砖气孔率以及耐热性有着一定的影响,结合剂中二氧化硅与三氧化二铝的含量越高,刚玉砖的气孔率越低、耐热性越高、由表6数据可得,实施例12为最优选择。
Claims (2)
1.危废焚烧系统回转窑用耐酸耐盐改性刚玉砖,其特征在于,所述改性刚玉砖按重量份数计包括:45~50份的致密电熔刚玉、20~30份的棕刚玉、10~15份的磷酸氧锆-改性氧化锆复合体、10~15份的红柱石,5~10份的硅灰;
其中,磷酸氧锆-改性氧化锆复合体的制备方法为:
S1、磷酸氧锆制备
将二氯氧化锆与质量浓度为85%的磷酸溶液按质量比1:1.5加入至烧杯中,在60~90℃的条件下搅拌4.5h,接着用200目筛网对烧杯内的混合物进行过滤,将过滤出的沉淀物放置于干燥机内在150℃的条件下干燥5h,将干燥后的沉淀物在1500℃的条件下烧制1h得到磷酸氧锆粉末;
S2、改性氧化锆制备
S2-1:溶胶制备
将质量浓度为75%的氯氧化锆溶液与氨水按体积比1:1进行混合,在室温条件下搅拌2h形成含水的二氧化锆沉淀物,接着在65~70℃条件下搅拌3.5h,在搅拌的过程中以0.5mL/s的速率向含水的二氧化锆沉淀物中加入催化剂制得溶胶;
S2-2:凝胶制备
将步骤S2-1中制备的溶胶与水按质量比1:5进行混合,在10℃的条件下静置12h,接着将溶胶与水的混合物与稀土按体积比3:1加入至离心机中以5r/ s的速率进行离心15~20h形成凝胶;
S2-3:制作改性氧化锆晶体
将步骤S2-2中制备的凝胶放入烘干机中,在230℃条件下烘干1.5h制成干凝胶,将干凝胶在1300℃的温度下煅烧5h后以5℃/min的速率冷却至室温得到改性氧化锆晶体;
S3、磷酸氧锆-改性氧化锆复合体制备
将步骤S1中制得的磷酸氧锆粉末与步骤S2中制得的改性氧化锆晶体按质量比1:1进行混合均匀,在1300~1500℃的条件下煅烧20h形成磷酸氧锆-改性氧化锆复合体;
所述步骤S2-1中使用的催化剂为质量浓度为99%的冰醋酸,加入冰醋酸的量为含水的二氧化锆沉淀物质量的5%;
所述步骤S2-2中加入的稀土为CeO2、Y2O3、Sc2O3其中的任意一种或多种;
在步骤S3煅烧的过程中,加入TiO2作为烧结助熔剂,加入TiO2的量为磷酸氧锆粉末与改性氧化锆晶体混合物质量的3~8%;
所述的危废焚烧系统回转窑用耐酸耐盐改性刚玉砖的制备方法,包括以下步骤:
(1)将致密电熔刚玉、棕刚玉、磷酸氧锆-改性氧化锆复合体、红柱石以及硅灰分别放入碎料机中进行碎料,利用筛网分别对粉碎完成后的原料进行筛选;
(2)将步骤(1)中筛选出的原料投放至碾轮式混料机中预混料15min使各原料进行充分混合,接着向混料机中加入与原料质量比1:1.5的水继续混料3h后形成具有流动性的砂浆;
(3)将步骤(2)中制备的砂浆倒入模具中,将模具放置于室温条件下自然干燥48h然后脱模;
(4)将步骤(3)中制备的混凝土块放入高温电炉中进行烧结制成刚玉砖;
在步骤(2)中原料加水进行混料的同时向混料机中加入与原料质量比0.1:1的结合剂,所述结合剂按重量百分比计包括:55~60%的SiO2,10~15%的Al2O3,余量为水;
在步骤(3)中的烧结方法为:从室温以5℃/s的速率升温至900℃后保持1h,接着以2℃/s的速率升温至1300~1600℃后保持2h。
2.根据权利要求1中所述的危废焚烧系统回转窑用耐酸耐盐改性刚玉砖,其特征在于,步骤(1)中选用的筛网为800目筛网。
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