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Method for detecting iron content in lithium-loaded organic phase by ultraviolet-visible spectrophotometer

An organic phase and iron content technology, applied in the field of analysis and detection, can solve the problems of not being able to distinguish the existence of different forms of iron, and achieve the effects of high measurement accuracy and repeatability, small environmental interference, and easy operation

Inactive Publication Date: 2020-08-04
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above methods can only measure the total iron content in the sample, but cannot distinguish the different forms of iron

Method used

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  • Method for detecting iron content in lithium-loaded organic phase by ultraviolet-visible spectrophotometer
  • Method for detecting iron content in lithium-loaded organic phase by ultraviolet-visible spectrophotometer
  • Method for detecting iron content in lithium-loaded organic phase by ultraviolet-visible spectrophotometer

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Experimental program
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Embodiment approach

[0028] According to a preferred embodiment of the present invention, the iron-containing compound is FeCl 3 ·6H 2 O solid,

[0029] The solvent is selected from concentrated aqueous hydrochloric acid and / or MgCl 2 aqueous solution.

[0030] The method for detecting the iron content in the lithium-loaded organic phase of the present invention is mainly applicable to tributyl phosphate (TBP) extracting lithium-loaded organic phase with LiFeCl in the conventional extraction process of lithium extraction. 4 .2 Detection of iron content in complexed state of TBP.

[0031] The inventor has found through research that dissolving FeCl with concentrated hydrochloric acid 3 ·6H 2 O solid powder can provide a higher concentration of chloride ions for the dissolution of iron, ensuring that Fe is dissolved in the form of FeCl 4 - The form exists in concentrated hydrochloric acid, and H + combined to form HFeCl 4 , then HFeCl 4 The form of extraction is transferred to the organic ...

Embodiment 1

[0086] (1) Weigh 180g of FeCl 3 ·6H 2 O solid (analytically pure), it is dissolved in the concentrated hydrochloric acid aqueous solution of 500ml mass fraction 20%, obtains iron concentration and is the iron-containing hydrochloric acid aqueous solution of 1.3mol / L;

[0087] Get the tributyl phosphate (TBP) of 800ml, mix with 200ml sulfonated kerosene, obtain TBP organic solution;

[0088] The TBP organic solution of described 1000ml is mixed with the iron-containing hydrochloric acid aqueous solution of described 500ml, after static phase separation, get upper organic phase, obtain the standard solution of iron-containing lithium extraction organic phase, utilize atomic absorption spectrophotometer (AAS ), analyze the iron content in the lower floor water phase to be 0mol / L, then calculate and obtain the concentration of iron in the iron-containing lithium organic phase standard solution according to the formula to be 0.65mol / L.

[0089] Prepare the concentrated hydrochlor...

Embodiment 2

[0110] (1) Weigh 12g of FeCl 3 ·6H 2 O solid (analytically pure), it is dissolved in the concentrated hydrochloric acid aqueous solution of 500ml mass fraction 37%, obtains iron concentration and is the iron-containing hydrochloric acid aqueous solution of 0.086mol / L;

[0111] Get the tributyl phosphate (TBP) of 800ml, mix with 200ml sulfonated kerosene, obtain TBP organic solution;

[0112] The TBP organic solution of described 1000ml is mixed with the iron-containing hydrochloric acid aqueous solution of described 500ml, after static phase separation, get upper organic phase, obtain the standard solution of iron-containing lithium extraction organic phase, utilize atomic absorption spectrophotometer (AAS ), the analysis of the iron content in the lower floor water phase is 0mol / L, and then according to the formula, the concentration of iron in the iron-containing lithium extraction organic phase standard solution is 0.043mol / L;

[0113] Prepare the concentrated hydrochlori...

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Abstract

The invention discloses a method for detecting the content of iron in lithium extraction loaded organic phase. The method includes steps of preparing ferrous organic phase standard solution and non-ferrous blank organic phase corresponding to the ferrous organic phase standard solution; plotting absorption curves of ferrous organic phase and selecting measurement wavelengths; preparing ferrous organic phase standard solution with different degrees of iron concentration, measuring absorbance values of the ferrous organic phase standard solution under the condition of the measurement wavelengths, and plotting standard work curves for describing relations between the absorbance values and the concentration of iron in the ferrous organic phase standard solution; measuring absorbance values ofto-be-detected samples under the condition of the measurement wavelengths and computing the content of iron in the to-be-detected samples according to the standard work curves. The method has the advantages that the method is easy and convenient to operate, is speedy and is high in measurement accuracy and repeatability, and the content of the iron which is available in the lithium extraction loaded organic phase in specific forms can be quickly measured by the aid of the method.

Description

technical field [0001] The invention belongs to the field of analysis and detection, and in particular relates to a method for detecting iron content in an organic phase loaded with lithium extracted by tributyl phosphate with an ultraviolet-visible spectrophotometer. Background technique [0002] As a new strategic energy source, lithium is mainly used in fields such as batteries, nuclear power generation, aerospace, and medicine. Lithium resources exist in the form of solid ore and salt lake brine. my country's salt lakes are rich in lithium resources, and the extraction method is currently one of the most promising methods for extracting lithium from brine. In the process of extracting lithium from salt lake brine, it is usually necessary to add FeCl 3 As a co-extractant, tributyl phosphate (TBP) was then used as an extractant to extract lithium from salt lake brine. FeCl 4 - The form enters the organic phase of lithium extraction, and the Li in the brine + Ions com...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/31G01N21/33
CPCG01N21/31G01N21/33
Inventor 黄焜刘杰张开强刘会洲
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI