无机盐工业
主管:中海油天津化工研究设计院有限公司
主办:中海油天津化工研究设计院有限公司
   中海油炼油化工科学研究院(北京)有限公司
   中国化工学会无机酸碱盐专业委员会
ISSN 1006-4990 CN 12-1069/TQ

无机盐工业 ›› 2023, Vol. 55 ›› Issue (6): 104-108.doi: 10.19964/j.issn.1006-4990.2022-0761

• 环境·健康·安全 • 上一篇    下一篇

羰基合成废铑液焙烧回收铑制备三氯化铑工艺研究

王本雷1,2(), 张桂生3, 蒋凌云1,2, 李晨1,2, 王鹏飞1,2, 李继霞1,2, 臧甲忠1,2   

  1. 1.中海油天津化工研究设计院有限公司,天津 300131
    2.天津市炼化催化工程技术中心 ; 天津 300131
    3.国能包头煤化工有限责任公司,内蒙古 包头 014020
  • 收稿日期:2022-12-30 出版日期:2023-06-10 发布日期:2023-06-14
  • 作者简介:王本雷(1989— ),男,硕士,工程师,主要研究方向为化工材料领域贵金属催化剂及工艺开发;E-mail:wang-benlei@163.com
  • 基金资助:
    中国海洋石油集团有限公司科技项目(CNOOC-KJ 135 ZDXM 32 TJY 002 TJY 2020)

Study on preparation process of rhodium trichloride by roasting recovery technology from waste rhodium solution of carbonyl synthesis

WANG Benlei1,2(), ZHANG Guisheng3, JIANG Lingyun1,2, LI Chen1,2, WANG Pengfei1,2, LI Jixia1,2, ZANG Jiazhong1,2   

  1. 1. CenerTech Tianjin Chemical Research and Design Institute Co. , Ltd, Tianjin 300131, China
    2. Tianjin Refining and Catalytic Technology Engineering Center, Tianjin 300131, China
    3. Guoneng Baotou Coal Chemical Co. , Ltd, baotou 014020, China
  • Received:2022-12-30 Published:2023-06-10 Online:2023-06-14

摘要:

铑资源稀少、价格昂贵,三氯化铑是制备铑催化剂等铑化合物的基础原料,羰基合成废铑液中铑含量通常在102~103 mg/kg,回收其中铑制备三氯化铑具有重要意义。目前废铑液回收铑主要采用焚烧法,此方法存在铑损失大、铑过烧及后续处理困难等问题。为解决这些问题,探索了一种羰基合成废铑液加入木炭粉先有氧后无氧的两段式焙烧回收工艺,该回收工艺操作简单,回收率高。主要流程为:废铑液蒸馏浓缩后得到浓缩铑渣,浓缩铑渣加入m(炭粉)/m(铑渣)=0.6的木炭粉后焙烧,室温升至600 ℃有氧焙烧,600 ℃保持3 h后,无氧条件下升温至1 100 ℃保持1 h后降至室温,得到活性铑灰,活性铑灰经酸浸溶、除杂浓缩得到三氯化铑,铑收率高于99.0%。

关键词: 羰基合成废铑液, 焙烧, 铑回收, 木炭粉

Abstract:

Rhodium resources are scarce and the price of rhodium is expensive.Rhodium trichloride is the raw material of rhodium catalyst and other rhodium compounds.The content of rhodium in waste rhodium solution of carbonyl synthesis is usually several hundred to several thousand milligrams per kilogram,the recovery of rhodium to prepare rhodium trichloride is of great significance.At present,the recovery of rhodium from waste rhodium liquid mainly adopts the incineration method,which has large rhodium loss and rhodium overfiring,subsequent processing difficulties and other problems.In order to solve these problems,a two-stage roasting process for recovery of rhodium from carbonyl synthesis by adding charcoal powder from aerobic roasting to oxygen-free roasting was explored.The process was simple and had a high recovery rate.The main process could be summarized as follows:the waste rhodium solution was distilled to obtain concentrated rhodium slag,and the rhodium slag was added with 0.6 times of charcoal powder,and roasted from room temperature to 600 ℃ under aerobic conditions.After being roasted at 600 ℃ for 3 h,the roasting temperature was rosed to 1 100 ℃ under the condition of no oxygen and remained at 1 100 ℃ for 1 h,the active rhodium ash was obtained when the temperature was lowered to room temperature.Then the active rhodium ash was dissolved in the acid.Finally,rhodium trichloride was obtained by purification and concentration,yield was higher than 99.0%.

Key words: waste rhodium solution of carbonyl synthesis, roasting, rhodium recovery, charcoal powder

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