CN116444254A - 一种丙烷脱氢废催化剂制备铬刚玉轻质骨料的方法 - Google Patents
一种丙烷脱氢废催化剂制备铬刚玉轻质骨料的方法 Download PDFInfo
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Abstract
本发明属于耐火材料技术领域，涉及一种丙烷脱氢废催化剂制备铬刚玉轻质骨料的方法。涉及的一种丙烷脱氢废催化剂制备铬刚玉轻质骨料的方法，废催化剂分装到匣钵内，匣钵的上沿设有过气通道，匣钵堆叠在窑车上，进入高温窑内进行无害化处理及烧结；废催化剂表面结焦的烧失处理，烧失催化剂表面的结焦；废催化剂烧焦完成后，继续升温，温度在1000~1200℃时，氧化气氛调整为还原气氛，还原气氛下将废催化剂中有害的高价铬还原成无害稳定的低价铬，同时低价氧化铬与催化剂的载体材料氧化铝进行固化反应形成铝铬固溶体；无害化处理后的催化剂进一步升温；氧化铬和氧化铝的固溶进一步强化，形成了多孔的铬刚玉烧结料。
Description
技术领域
本发明属于耐火材料技术领域，具体来讲涉及一种丙烷脱氢废催化剂制备铬刚玉轻质骨料的方法。
背景技术
丙烯是一种重要的有机化工原料，用于生产聚丙烯、丙烯腈、丁醇等产品；世上约66%的丙烯来自烃类蒸汽裂解制乙烯装置，32%来之炼油厂催化裂化装置，其余由丙烷脱氢（PDH）和甲醇制烯烃（MTO/MTP）获得；随着对丙烯需求量的日益增加，拓宽丙烯原料来源的生产工艺成为研究和产业化热点，其中丙烷脱氢制丙烯工艺最受关注；催化脱氢制备丙烯的方法有多种其中Catofin、FBD、Linde的丙烷催化脱氢工艺使用的催化剂为Cr2O3/Al2O3系列催化剂；随着催化反应时间的增加、反应温度的升高和还原-脱氢-再生循环次数的增加，催化剂的可再生会失活，定期更换下来的失活催化剂为丙烷脱氢废催化剂。
Catofin丙烷脱氢废含铬催化剂，按照《国家危险废物名录（2021年版）》划分属于HW50废物，废物代码261-156-50，危险特性为T（Toxicity毒性）；危废处理厂家往往通过填埋或复杂的熔炼工艺来无害化处理，既容易造成二次污染，又花费较大，浪费了能源和资源。《中华人民共和国固体废物污染环境保护法》中: 第九十三条：国家鼓励和支持科研单位、固体废物产生单位、固体废物利用单位、固体废物处置单位等联合攻关，研究开发固体废物综合利用、集中处置等新的技术，推动固体废物污染环境防治技术进步。
发明内容
为了能够实现铬资源循环利用，本发明公开一种丙烷脱氢废催化剂制备铬刚玉轻质骨料的方法，全部以废催化剂为原料，利用高温窑炉对催化剂进行火法氧化/还原反应，使得废催化剂中的有毒有害成分价态发生变化，转化为无毒害且具有化学稳定性的物质，同时利用催化剂多孔结构的特点，控制烧结温度，制成铬刚玉轻质骨料。
一种丙烷脱氢废催化剂制备铬刚玉轻质骨料的方法，具体步骤如下：
废催化剂分装到匣钵内，匣钵的上沿设有过气通道，匣钵堆叠在窑车上，进入高温窑内进行无害化处理及烧结；
废催化剂表面结焦的烧失处理，控制窑温在600~700℃，保持氧化气氛，该温度段维持时间60~75分钟，烧失催化剂表面的结焦；
废催化剂烧焦完成后，继续升温，温度在1000~1200℃时，氧化气氛调整为还原气氛，还原气氛CO浓度控制在3~4万PPM； 还原气氛下将废催化剂中有害的高价铬还原成无害稳定的低价铬，同时低价氧化铬与催化剂的载体材料氧化铝进行固化反应形成铝铬固溶体；
无害化处理后的催化剂进一步升温，温度升到1350~1450℃，气氛保持弱还原气氛，还原气氛CO浓度控制在1~2万PPM；氧化铬和氧化铝的固溶进一步强化，形成了多孔的铬刚玉烧结料。
废催化剂为Catofin丙烷脱氢废含铬催化剂中，Cr2O3的重量百分比为18~20%，少量的Na2O，重量百分比0.5%，其余为催化剂的载体Al2O3。为了有更好的催化效果，催化剂及载体属于多孔的结构，催化剂的颗粒密度为900-1100Kg/m3。这种含铬催化剂与以往其他的含铬催化剂有着明显的不同之处，催化剂中Cr2O3和Al2O3的合量比例非常高，且Cr2O3和Al2O3可以形成任意比例互溶的铬铝固溶体，有非常高的利用价值。
由于采用上述技术方案，本发明具有如下的有益效果：
利用匣钵分装，废催化剂在窑炉火法氧化/还原时，接触到窑内气氛均匀，同时温度传导也均匀，更有利于废催化剂的烧焦、无害化处理和烧结；
窑炉内控制窑温在600~700℃时，保持60~75分钟的氧化气氛，处理后废催化剂中残碳量数值可以降到0%，表面结焦烧失很干净；
窑炉内温度在1000~1200℃时，窑内保持还原气氛CO浓度控制在3~4万PPM。废催化剂中有害的高价铬还原成无害稳定的低价铬，同时低价氧化铬与催化剂的载体材料氧化铝进行固化反应形成铝铬固溶体；依据《GB 5085.3-2007 危险废物鉴别标准 浸出毒性鉴别》要求，按照HJ/T299进行固体废物浸出液，按照GB/T 15555.4对浸出液中的危害成分项目铬（六价）浓度进行测量，检测值小于危害成分浓度限值5mg/L，已经不属于危险废物，无害化处理效果明显。
进一步弱还原气氛烧结，氧化铬和氧化铝的固溶进一步强化，颗粒的强度得到提升。催化剂颗粒原为多孔结构，烧结完成后依然保持了部分多孔结构，形成了铬刚玉轻质骨料。
附图说明
图 1 铬刚玉轻质骨料显微结构图
实施方式
通过下面的实施例可以更详细的解释本发明。
实施例
Catofin丙烷脱氢废含铬催化剂，按照《国家危险废物名录（2021年版）》划分属于HW50废物。废催化剂处理前的运输、储运按照HJ 1091固体废物再生利用污染防治技术导则要求进行。
将废催化剂分装到匣钵内，匣钵的上沿有过气通道，匣钵堆叠在窑车上。窑车进入高温窑内进行无害化处理及铬刚玉轻质料的烧结。废催化剂表面结焦的烧失处理阶段，控制窑温在650℃，保持氧化气氛，该温度段维持时间70分钟，烧失催化剂表面的结焦；废催化剂的无害化处理阶段，温度控制在1100℃，还原气氛CO浓度控制在3.5万PPM；废催化剂的烧结阶段，温度控制在1400℃，还原气氛CO浓度控制在1万PPM，利用催化剂颗粒原为多孔结构，氧化铬和氧化铝的固溶进一步强化，形成了多孔的铬刚玉烧结料。 轻质铬刚玉烧结料的指标见表1,轻质烧结料的显微结构见图1。
实施例
Catofin丙烷脱氢废含铬催化剂，按照《国家危险废物名录（2021年版）》划分属于HW50废物。废催化剂处理前的运输、储运按照HJ 1091固体废物再生利用污染防治技术导则要求进行。
将废催化剂分装到匣钵内，匣钵的上沿有过气通道，匣钵堆叠在窑车上。窑车进入高温窑内进行无害化处理及铬刚玉轻质料的烧结。废催化剂表面结焦的烧失处理阶段，控制窑温在600℃，保持氧化气氛，该温度段维持时间75分钟，烧失催化剂表面的结焦；废催化剂的无害化处理阶段，温度控制在1000℃，还原气氛CO浓度控制在4万PPM；废催化剂的烧结阶段，温度控制在1450℃，还原气氛CO浓度控制在1.5万PPM，利用催化剂颗粒原为多孔结构，氧化铬和氧化铝的固溶进一步强化，形成了多孔的铬刚玉烧结料。 轻质铬刚玉烧结料的指标见表1。
实施例
Catofin丙烷脱氢废含铬催化剂，按照《国家危险废物名录（2021年版）》划分属于HW50废物。废催化剂处理前的运输、储运按照HJ 1091固体废物再生利用污染防治技术导则要求进行。
将废催化剂分装到匣钵内，匣钵的上沿有过气通道，匣钵堆叠在窑车上。窑车进入高温窑内进行无害化处理及铬刚玉轻质料的烧结。废催化剂表面结焦的烧失处理阶段，控制窑温在700℃，保持氧化气氛，该温度段维持时间60分钟，烧失催化剂表面的结焦；废催化剂的无害化处理阶段，温度控制在1200℃，还原气氛CO浓度控制在3万PPM；废催化剂的烧结阶段，温度控制在1350℃，还原气氛CO浓度控制在2万PPM，利用催化剂颗粒原为多孔结构，氧化铬和氧化铝的固溶进一步强化，形成了多孔的铬刚玉烧结料。 轻质铬刚玉烧结料的指标见表1。
表 1 轻质铬刚玉烧结料的指标
废催化剂的烧焦、无害化、烧结成耐火材料再利用，高温过程利用了现有高温窑炉及后续烟气处理装置，可在高温窑炉内直接进行无害化处理，处理过程中不产生二次固废、废液、废气等污染。
制备出来的烧结铬刚玉轻质骨料能够做为一种优级的耐火材料原料使用，去制备轻质耐火砖或轻质浇注料。制备出来的轻质骨料，依据《GB 5085.3-2007 危险废物鉴别标准 浸出毒性鉴别》要求，按照HJ/T299进行固体废物浸出液，按照GB/T 15555.4对浸出液中的危害成分项目铬（六价）浓度进行测量，检测值小于危害成分浓度限值5mg/L，已经不属于危险废物，无害化处理效果明显。通过本发明的方法能够高效率实现了废催化剂的资源化利用。
Claims (1)
1.一种丙烷脱氢废催化剂制备铬刚玉轻质骨料的方法，其特征在于：具体步骤如下：
废催化剂分装到匣钵内，匣钵的上沿设有过气通道，匣钵堆叠在窑车上，进入高温窑内进行无害化处理及烧结；
废催化剂表面结焦的烧失处理，控制窑温在600~700℃，保持氧化气氛，该温度段维持时间60~75分钟，烧失催化剂表面的结焦；
废催化剂烧焦完成后，继续升温，温度在1000~1200℃时，氧化气氛调整为还原气氛，还原气氛CO浓度控制在3~4万PPM； 还原气氛下将废催化剂中有害的高价铬还原成无害稳定的低价铬，同时低价氧化铬与催化剂的载体材料氧化铝进行固化反应形成铝铬固溶体；
无害化处理后的催化剂进一步升温，温度升到1350~1450℃，气氛保持弱还原气氛，还原气氛CO浓度控制在1~2万PPM；氧化铬和氧化铝的固溶进一步强化，形成了多孔的铬刚玉烧结料。
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