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%。

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%.