Resource cyclic utilization method of rhodium-containing waste liquid of butanol-octanol device

A recycling and waste liquid technology, applied in chemical instruments and methods, rhodium organic compounds, compounds containing elements of Group 8/9/10/18 of the periodic table, etc., can solve triphenylphosphine damage, waste of resources, etc. problems, to achieve the effect of high recovery rate, less three wastes and less investment

Active Publication Date: 2017-08-08
山东博苑医药化学股份有限公司
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  • Application Information

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Problems solved by technology

Triphenylphosphine is completely destroyed, causing waste of resources

Method used

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  • Resource cyclic utilization method of rhodium-containing waste liquid of butanol-octanol device

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) recovery of rhodium in reaction mother liquor

[0038] 10kg butanol device rhodium-containing waste liquid (rhodium content 0.15%) is adsorbed circularly with polystyrene resin containing active mercapto functional groups as the adsorption resin until the rhodium content in the solution is lower than 5ppm. Then the adsorption resin is eluted and analyzed with the prepared eluent, and the deliquified solution becomes a rhodium-containing solution. Add water and hydrochloric acid in rhodium-containing solution, reflux, rhodium complex hydrolyzes and generates rhodium sulfide to separate out, filters, and the filtered solid is added in 125g concentrated hydrochloric acid and refluxes to generate rhodium chloride, and refluxes until no hydrogen sulfide emerges (with Calcium hydroxide absorbs hydrogen sulfide), the rhodium chloride solution is concentrated and crystallized to separate out rhodium chloride hydrate, and the mother liquor is reserved for batch application. ...

Embodiment 2

[0050] (1) recovery of rhodium in reaction mother liquor:

[0051] a) 4000kg butanol device rhodium-containing waste liquid (0.15% rhodium content) is pumped into the rhodium adsorption device that the polystyrene resin that contains active mercapto functional group is housed as adsorption resin circulation from raw material storage tank, circulates Adsorption, until the content of rhodium in the solution is lower than 5ppm.

[0052] b) After the adsorption resin is eluted and analyzed with an eluent, the eluent becomes a rhodium-containing solution. Add water and hydrochloric acid in the rhodium-containing solution, reflux, the rhodium complex hydrolyzes and generates rhodium sulfide to separate out, filters, adds the filtered solid to 50kg concentrated hydrochloric acid and refluxes to generate rhodium chloride, and refluxes until no hydrogen sulfide emerges (with hydrogen Calcium oxide absorbs hydrogen sulfide), the rhodium chloride solution is concentrated and crystallize...

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Abstract

The invention relates to a resource cyclic utilization method of rhodium-containing waste liquid of a butanol-octanol device. The cyclic utilization of effective sources, namely rhodium and triphenylphosphine is ensured and a useless resource, namely a waste solvent, is combusted and converted into energy for production, so that materials are put into the best use; tail gas generated by combustion is subjected to desulfurization treatment and denitration treatment and is discharged after reaching standards, so that the discharged gas is pollution-free and environment-friendly resource cyclic utilization is realized. In an important link of recycling of the rhodium, an absorption method is adopted and a loading type rhodium ligand and a waste rhodium catalyst are mixed and alternately used for absorbing; then the rhodium is displaced from a triphenylphosphine ligand. The method is little in investment, environmentally friendly and high in rhodium recycling rate; the triphenylphosphine is sufficiently recycled and economic benefits and market competitiveness are greatly improved.

Description

technical field [0001] The invention relates to a resource comprehensive utilization technology of waste liquid, in particular to a resource recycling method for rhodium-containing waste liquid of a butanol plant. Background technique [0002] The rhodium-phosphine complex catalyst system is widely used in the low-pressure carbonylation of propylene to butyl-octyl alcohol. Due to the presence of various high-boiling point by-products and oxygen, chlorine, and sulfur impurities in the raw materials during the carbonylation reaction, part of the catalyst in the reaction system loses Active, the recovery of precious metal rhodium in catalyst waste liquid has aroused widespread concern. The current representative recycling methods are as follows. [0003] 1. Incineration and ashing method: The method introduced in Chinese patent CN 1414125 uses carbonates of alkali metals or alkaline earth metals as additives to incinerate and ash the waste catalyst residue at 650°C-700°C, and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/53C07F9/50C07F15/00C01G55/00B01J31/24
CPCB01J31/2495B01J2531/0213B01J2531/822C01G55/005C07F9/5022C07F9/5325C07F15/008
Inventor 李成林于国清舒瑞友
Owner 山东博苑医药化学股份有限公司
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