2-丙基庚醇生产工业催化剂溶液中铑含量测定

doi:10.19964/j.issn.1006-4990.2024-0053

Abstract

Abstract:

Using a mixture of butene and synthesis gas（H₂/CO） as raw materials，rhodium/diphosphine ligand was used as a catalyst to generate the intermediate product valeraldehyde through carbonylation reaction.The valeraldehyde is then condensed and hydrogenated to produce the environmentally friendly plasticizer alcohol 2-propylheptanol.This process had the characteristics of low concentration of precious metal rhodium，high aspect ratio of the product，fast reaction，and mild conditions.However，the rhodium concentration in the reaction solution was an important factor affecting the low-pressure carbonylation synthesis reaction.By establishing a method for treating the reaction solution of 2-propylheptanol containing rhodium catalyst and determining the rhodium content in it，the reaction conditions for separating rhodium by extraction method were studied.The rhodium content determination methods under different extraction conditions were compared，and compared with the traditional digestion method and atomic absorption method for directly determining rhodium in organic liquids.The method had the characteristics of mild reaction conditions，convenient processing，and good reproducibility.The results showed that at 80 ℃，5.000 0 g of rhodium containing waste liquid treated with 10.0 mL of nitric acid（1+4），10.0 mL of hydrogen peroxide aqueous solution（H₂O₂ mass fraction of 30%），and 4.0 mL of toluene for 1 hour，after separation，the rhodium was extracted and separated，and the rhodium was transferred from the oil phase to the water phase.After reaching a constant volume，the rhodium content in the water phase was determined by ICP-AES，with a relative standard deviation（RSD，n=6） of 0.6% and standard recovery rates ranging from 96.80% to 101.19%.

Key words: analytical chemistry, extraction method, determination, reaction solution of rhodium compound, rhodium

CLC Number:

TQ138.22

WANG Yong, LI Jixia, ZHANG Guisheng, WANG Pengfei, WANG Benlei. Determination of rhodium for catalyst solution of 2-Propylheptanol[J]. Inorganic Chemicals Industry, 2024, 56(9): 142-146.

Figures/Tables 6

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References 13

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编号	样品含铑量/μg	加入的铑量/μg	铑测量值/μg	铑回收率/%
1	1 860.1	1 000	2 894.1	101.19
2	1 860.1	2 000	3 736.6	96.80
3	1 860.1	4 000	5 713.6	97.50
4	1 860.1	6 000	7 671.4	97.60

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National Inorganic Salts Information Center

Inorganic Acid-Base-Salt Committee of CIESC

Determination of rhodium for catalyst solution of 2-Propylheptanol

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