CN108624756A - 一种低耗高效废汞触媒的回收工艺 - Google Patents
一种低耗高效废汞触媒的回收工艺 Download PDFInfo
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- 229910052753 mercury Inorganic materials 0.000 title claims abstract description 39
- 238000011084 recovery Methods 0.000 title claims abstract description 34
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- 238000010521 absorption reaction Methods 0.000 claims abstract description 12
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- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 5
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- 229910021389 graphene Inorganic materials 0.000 claims description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 4
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- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 3
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
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- 229910000831 Steel Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
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- VTIIJXUACCWYHX-UHFFFAOYSA-L disodium;carboxylatooxy carbonate Chemical compound [Na+].[Na+].[O-]C(=O)OOC([O-])=O VTIIJXUACCWYHX-UHFFFAOYSA-L 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G13/00—Compounds of mercury
- C01G13/04—Halides
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B43/00—Obtaining mercury
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/009—General processes for recovering metals or metallic compounds from spent catalysts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
本发明涉及一种低耗高效废汞触媒的回收工艺,包括内衬容器、分离、收集、吸附、活性炭吸附,所述内衬容器,用碱液清洗,加热至115℃,喷砂,涂布2.5mm厚的内涂层涂料,温度为95℃,干燥15min;所述分离,干馏炉内压力为0.5MPa,加热升温,加热速率为25℃/min,至480℃,保持15min后,继续加热至580℃;保持20min,降温,速率5℃/min,降至400℃,保持20min;所述收集,碳酸钠的浓度为0.5mol/L;本发明的回收工艺,采用干馏炉及其后续的尾气处理工艺,具有回收能耗低、设备成本低,回收彻底,氯化汞回收率高,环境无污染的优点,汞的回收率为99.94%,纯度达99.95%。
Description
技术领域
本发明涉及一种废汞触媒,具体地说,涉及一种废汞触媒回收工艺,属于废汞触媒回收氯化汞的生产技术领域。
背景技术
汞俗称“水银”,是地壳中相当稀少的一种元素。极少数的汞在自然中以纯金属的状态存在,是唯一的液体金属。朱砂、氯硫汞矿、硫锑汞矿和其它一些与朱砂的矿物是汞最常见的矿藏。
目前,废汞触媒回收通常是将废汞触媒先与石灰水一起蒸煮,使氯化汞转化为氧化汞,再经高温使氧化汞成为单质汞,该种方法回收率低,只有57%左右的回收率,并且废弃物对环境污染十分严重。
中国专利CN201210484615.7可以实现氯化汞的回收和活性炭的回收,且回收率高。但该工艺加热采用隔离式电加热,导致工艺耗能高,不利于低碳环保。
中国专利CN201310671649.1可以实现氯化汞的回收:回收的循环N2中氯化汞可以达到10ppm,回收工艺较简单,但对设备的要求较高,高度的HCl结合水蒸气形成酸雾,加之氯化汞蒸汽对设备的维护成本也高,导致成本高,不利于工业大规模生产。
在实现本发明的过程中,发明人发现现有技术中至少存在以下问题:回收不彻底,回收能耗高、成本高,污染环境。
发明内容
为了解决背景技术中存在的技术问题,本发明提供一种低耗高效废汞触媒的回收工艺,可以实现以下发明目的:
本发明的一种低耗高效的废汞触媒的回收工艺克服了现有回收工艺回收不彻底,回收能耗高、成本高、污染环境的缺陷,本发明采用干馏炉及其后续的尾气处理工艺,具有回收能耗低、设备成本低,回收彻底,氯化汞回收率高,环境无污染的优点。
为解决上述技术问题,采用以下技术方案:
一种低耗高效废汞触媒的回收工艺,其特征在于,包括内衬容器、分离、收集、吸附、活性炭吸附。
作为本发明优选的技术方案,所述内衬容器,用碱液清洗,加热至115℃去油、去锈,再加以喷砂,使被处理表面形成砂面,再涂布一层内涂层涂料,内涂层涂料的厚度为2.5mm,涂布温度为95℃,干燥15min。
作为本发明优选的技术方案,所述内衬容器,所需的内涂层涂料,由氧化硅溶胶65份、钛白颜料12份、聚氨酯改性环氧树脂25份、纳米补强剂12份、弹性微球10份、聚四氟乙烯65份、蓖麻油醇酸树脂20份、线性乙烯10份、氧化锌粉12份、短油度醇酸树脂12份、邻苯二甲酸二丁酯12份、流平剂12份、消泡剂15份、氧化锆45份、固化剂6份、二甲苯9份、石墨烯8份、乙二醇乙醚10份、润滑剂5份、酚醛树脂15份、氧化铝粉10份、烯丙基缩水甘油醚5份、成膜助剂12份、锂基膨润土3份、润湿剂15份组成。
作为本发明优选的技术方案,所述的锂基膨润土,表观粘度1205mPa.s,密度3.3g/cm3,蒙脱石含量91.6%;
所述润滑剂为聚醚改性二甲基硅氧烷共聚体溶液,其质量百分浓度为21%,溶剂为二甲苯;
所述润湿剂,为航空煤油与二甲苯的混合溶液,其中,航空煤油:二甲苯的质量比为5:117。
作为本发明优选的技术方案,所述分离,干馏炉内压力为0.5MPa,加热升温,加热速率为25℃/min,温度为480℃,氯化汞和活性炭开始分离;保持15min后,继续加热至580℃;保持20min后,开始降温处理,降温速率为5℃/min,降至400℃,保持20min;如此进行循环往复。
作为本发明优选的技术方案,所述收集,碳酸钠洗罐中碳酸钠水溶液的浓度为0.5mol/L。
作为本发明优选的技术方案,所述吸附,包括分子筛吸附,所述分子筛吸附,采用活性氧化铝分子筛,所述活性氧化铝分子筛,有效物质含量99.8%,堆积密度0.7g/ml,颗粒度为3-5mm,Al2O3含量≥95.6%,Fe2O3≤0.05%,抗压强度18.3KN/颗,耐酸度≥95.2%,显气孔率0.50%。
作为本发明优选的技术方案,所述低耗高效废汞触媒的回收工艺,汞的回收率为99.94%,纯度达99.95%。
本发明采用以上技术方案,与现有技术相比,具有以下优点:
本发明的一种低耗高效废汞触媒的回收工艺,采用干馏炉及其后续的尾气处理工艺,具有回收能耗低、设备成本低,回收彻底,氯化汞回收率高,环境无污染的优点,汞的回收率为99.94%,纯度达99.95%。
具体实施方式
实施例1一种低耗高效废汞触媒的回收工艺
本发明的一种低耗高效的废汞触媒回收工艺,主要包括以下步骤:
(1)内衬容器:
将干馏炉、冷凝器、洗罐、隔网板以及管道内部表面用碱液清洗,并加热至115℃去油、去锈,再加以喷砂,使被处理表面形成砂面,再涂布一层内涂层涂料,内涂层涂料的厚度为2.5mm,涂布温度为95℃,干燥15min。
所述的内涂层涂料,由氧化硅溶胶65份、钛白颜料12份、聚氨酯改性环氧树脂25份、纳米补强剂12份、弹性微球10份、聚四氟乙烯65份、蓖麻油醇酸树脂20份、线性乙烯10份、氧化锌粉12份、短油度醇酸树脂12份、邻苯二甲酸二丁酯12份、流平剂12份、消泡剂15份、氧化锆45份、固化剂6份、二甲苯9份、石墨烯8份、乙二醇乙醚10份、润滑剂5份、酚醛树脂15份、氧化铝粉10份、烯丙基缩水甘油醚5份、成膜助剂12份、锂基膨润土3份、润湿剂15份组成。
所述的锂基膨润土,表观粘度1205mPa.s,密度3.3g/cm3,蒙脱石含量91.6%;
所述润滑剂为聚醚改性二甲基硅氧烷共聚体溶液,其质量百分浓度为21%,溶剂为二甲苯;
所述润湿剂,为航空煤油与二甲苯的混合溶液,其中,航空煤油:二甲苯的质量比为5:117;
所述流平剂为聚丙烯酸含氟酯,所述消泡剂为聚醚改性硅油;
所述烯丙基缩水甘油醚,购自上海昊化化工有限公司。
内涂层涂料,其制备方法,步骤如下:
第一,将氧化铝粉、锂基膨润土和氧化锆研磨粉碎至200目,第二,向搅拌容器中加入氧化硅溶胶65份、钛白颜料12份、聚氨酯改性环氧树脂25份、纳米补强剂12份、聚四氟乙烯65份、蓖麻油醇酸树脂20份、线性乙烯10份、短油度醇酸树脂12份、邻苯二甲酸二丁酯12份、流平剂12份、消泡剂15份、氧化锆45份、二甲苯9份、石墨烯8份、乙二醇乙醚10份、润滑剂5份、酚醛树脂15份、氧化铝粉10份、烯丙基缩水甘油醚5份、锂基膨润土3份、润湿剂15份,120℃下搅拌混合8h;然后加入氧化锌粉12份、弹性微球10份、成膜助剂12份,升温至150℃搅拌2.5h;最后加入固化剂6份,降温至45℃搅拌1.5h即可。
所述干馏炉的内部结构,包括一隔网板,隔网板为网孔设计,网孔大小为4-5mm,隔网板设置于干馏炉高度的三分之一处,以形成两个相对封闭的空间。
本步骤中涂布的内涂层涂料,提高了容器表面的平整度,不仅有效抵制强腐蚀烟气(如HCl等气体)对钢质内壁的腐蚀,有效抵制强腐蚀性液体等强腐蚀性物质的腐蚀,同时所形成的漆膜具有很高的耐磨性、耐温性(可耐900℃高温不融化、不滴漆、不挥发)及耐冷热震荡性,具有低张力、不发热、稳定性高等特性,不粘壁,使用寿命长,可以完全代替之前的钛材容器,大大节省成本,并提高工效。
(2)分离:
称取2kg废汞触媒放置在隔网板上,先通入氮气置换出干馏炉内的空气,干馏炉内压力保持为0.5MPa,然后将干馏炉进行加热升温,加热速率为25℃/min,温度为480℃,氯化汞和活性炭开始分离;
保持15min后,继续加热至580℃;
保持20min后,开始降温处理,降温速率为5℃/min,降至400℃,保持20min;
如此进行循环往复。
废汞触媒中氯化汞含量为4.5%,活性炭灰份2.2 %、机械强度95%、堆积密度420g/L。
(3)收集:
混合气体经过两组冷却器冷却,氯化汞粉末从冷却器底部收集到盛有酸液的溶解槽中,剩余尾气经过碳酸钠洗罐进行洗涤,得到的氧化汞沉淀通过碳酸钠洗罐底部的过滤装置分离。
其中,碳酸钠洗罐中碳酸钠水溶液的浓度为0.5mol/L。
(4)吸附:
剩余尾气继续经过碱洗罐进行碱洗中和后进入分子筛吸附罐,以除去二氧化碳气体和氯化氢气体,以及水雾。
其中,碱洗罐内采用浓度10%的氢氧化钾溶液,该溶液碱洗性能与氢氧化钠相比略强,并且使用该溶液与氯化氢反应生成的浓度6%-8%的氯化钾溶液,其内部杂质少,可以作为低汞触媒生产的一种添加剂使用;
分子筛吸附罐中采用活性氧化铝分子筛进行除水,活性氧化铝分子筛吸附水分饱和后,再通过蒸发器进行高温复活,可重复使用。
本发明所采用的活性氧化铝分子筛,有效物质含量99.8%,堆积密度0.7g/ml,颗粒度为3-5mm,Al2O3含量≥95.6%,Fe2O3≤0.05%,抗压强度18.3KN/颗,耐酸度≥95.2%,显气孔率0.50%。
(5)活性炭吸附:
分子筛吸附完成后依次进入一级活性炭吸附罐和二级活性炭吸附罐,得到循环氮气,返回到干馏炉循环使用,形成闭循环。
经检测,25℃、0.5MPa下,循环氮气中氯化汞含量≤1ppm,水分含量≤1ppm。
将本发明的氯化汞粉末和氧化汞沉淀分别干燥至恒重,称量(氯化汞粉末89.10g,氧化汞沉淀0.7204g)、计算汞的回收率,汞的回收率为99.94%,测定纯度达99.95%。
以上述依据本发明的理想实施例为启示,通过上述的说明内容,相关工作人员完全可以在不偏离本项发明技术思想的范围内,进行多样的变更以及修改。本项发明的技术性范围并不局限于说明书上的内容,必须要根据权利要求范围来确定其技术性范围。
Claims (8)
1.一种低耗高效废汞触媒的回收工艺,其特征在于,包括内衬容器、分离、收集、吸附、活性炭吸附。
2.根据权利要求1所述的一种低耗高效废汞触媒的回收工艺,其特征在于,
所述内衬容器,用碱液清洗,加热至115℃去油、去锈,再加以喷砂,使被处理表面形成砂面,再涂布一层内涂层涂料,内涂层涂料的厚度为2.5mm,涂布温度为95℃,干燥15min。
3.根据权利要求1所述的一种低耗高效废汞触媒的回收工艺,其特征在于,
所述内衬容器,所需的内涂层涂料,由氧化硅溶胶65份、钛白颜料12份、聚氨酯改性环氧树脂25份、纳米补强剂12份、弹性微球10份、聚四氟乙烯65份、蓖麻油醇酸树脂20份、线性乙烯10份、氧化锌粉12份、短油度醇酸树脂12份、邻苯二甲酸二丁酯12份、流平剂12份、消泡剂15份、氧化锆45份、固化剂6份、二甲苯9份、石墨烯8份、乙二醇乙醚10份、润滑剂5份、酚醛树脂15份、氧化铝粉10份、烯丙基缩水甘油醚5份、成膜助剂12份、锂基膨润土3份、润湿剂15份组成。
4.根据权利要求3所述的一种低耗高效废汞触媒的回收工艺,其特征在于,
所述的锂基膨润土,表观粘度1205mPa.s,密度3.3g/cm3,蒙脱石含量91.6%;
所述润滑剂为聚醚改性二甲基硅氧烷共聚体溶液,其质量百分浓度为21%,溶剂为二甲苯;
所述润湿剂,为航空煤油与二甲苯的混合溶液,其中,航空煤油:二甲苯的质量比为5:117。
5.根据权利要求1所述的一种低耗高效废汞触媒的回收工艺,其特征在于,
所述分离,干馏炉内压力为0.5MPa,加热升温,加热速率为25℃/min,温度为480℃,氯化汞和活性炭开始分离;保持15min后,继续加热至580℃;保持20min后,开始降温处理,降温速率为5℃/min,降至400℃,保持20min;如此进行循环往复。
6.根据权利要求1所述的一种低耗高效废汞触媒的回收工艺,其特征在于,
所述收集,碳酸钠洗罐中碳酸钠水溶液的浓度为0.5mol/L。
7.根据权利要求1所述的一种低耗高效废汞触媒的回收工艺,其特征在于,
所述吸附,包括分子筛吸附,所述分子筛吸附,采用活性氧化铝分子筛,所述活性氧化铝分子筛,有效物质含量99.8%,堆积密度0.7g/ml,颗粒度为3-5mm,Al2O3含量≥95.6%,Fe2O3≤0.05%,抗压强度18.3KN/颗,耐酸度≥95.2%,显气孔率0.50%。
8.根据权利要求1所述的一种低耗高效废汞触媒的回收工艺,其特征在于,
所述低耗高效废汞触媒的回收工艺,汞的回收率为99.94%,纯度达99.95%。
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