Method for extraction and separation of tungsten and molybdenum from tungsten and molybdenum mixed solution

A mixed solution, tungsten and molybdenum technology, applied in the field of chemical extraction, can solve the problems of large loss of tungsten co-extraction, large amount of tungsten co-extraction, large water solubility, etc., to achieve less loss of organic phase, small loss of tungsten co-extraction, and environmental pollution small effect

Active Publication Date: 2013-01-16
CENT SOUTH UNIV +1
View PDF8 Cites 39 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method is to add H to the acidic tungsten-molybdenum mixed solution 2 o 2 Make tungsten and molybdenum form peroxo complexes of tungsten and molybdenum respectively, and then use phosphoric acid ester (such as tributyl phosphate TBP) or trialkylphosphine oxide (such as tributylphosphine oxide TBPO, trioctylphosphine oxide TOPO ) or tertiary amines (such as trioctylamine TOA) or quaternary ammonium salts (such as tetraoctyl ammonium sulfate) and other extractants under certain conditions preferentially extract molybdenum peroxygen complexes and separate them from tungsten. This method can effectively remove tungsten molybdenum in acid salt, but the co-extraction amount of tungsten is relatively large, and the above-mentioned extractant requires a higher concentration of extractant to obtain a better separation effect, and the higher concentration of extractant leads to Difficulty with phase separation (U.S. Pat. No. 4,275,039)
U.S. Patent U.S.Pat.No.4,275,039, in order to improve the phase separation problem in the extraction process, use the three-component mixed extractant to replace the single-component extractant, that is, by D 2 EHPA, TBP, and TBPO are mixed in a certain proportion to form a t...

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Organic phase composition (volume percentage): 3%TRPO+60%TBP+37%sulfonated kerosene, among which TRPO is a mixed trialkylphosphine oxide of Cynex923 provided by Cytec Corporation of Canada.

[0023] Aqueous phase material liquid: prepared molybdenum-containing sodium tungstate solution, pH 10.3, adjusted to pH 3.5 with nitric acid, added 30% H 2 o 2 aqueous solution, H 2 o 2 The amount of addition is 1.0 times of the total amount of moles of tungsten and molybdenum, and then the pH value is adjusted to 1.5 with nitric acid solution to obtain the extraction material liquid, wherein WO 3 140.5g / L, Mo 16.3g / L, Mo / WO 3 =0.116.

[0024] Extraction and separation: the above-mentioned organic phase and aqueous phase feed liquid are subjected to 8-stage countercurrent extraction under the condition of ratio 2 / 1, and the loaded organic phase is subjected to single-stage back extraction under the condition of ratio 1 / 1 with 0.1mol / L NaOH aqueous solution , after...

Embodiment 2

[0027] Organic phase composition (volume percentage): 1%TRPO+40%TBP+59% aviation kerosene, wherein TRPO is a mixed trialkylphosphine oxide Cynex923 provided by Cytec Company.

[0028] Aqueous phase material liquid: an industrial actual molybdenum-containing ammonium tungstate solution produced by a company using an ion exchange process, the pH value is 9.5, the pH value is adjusted to 3.5 with hydrochloric acid, and 30% H is added to it 2 o 2 ,H 2 o 2 The addition amount is 1.5 times of the sum of the moles of tungsten and molybdenum, mix evenly, and then adjust the pH value to 2.5 with ammonia solution to obtain the extraction water phase complexing material liquid, wherein WO 3 180.2g / L, Mo 3.60g / L, Mo / WO 3 =0.020.

[0029] Extraction and separation: the organic phase and the aqueous phase feed liquid are subjected to 3-stage countercurrent extraction under the condition of a ratio of 4 / 3, and the loaded organic phase is subjected to single-stage stripping under...

Embodiment 3

[0032] Organic phase composition (volume percentage): 5%TRPO+80%TBP+15%sulfonated kerosene, wherein TRPO is a mixed trialkylphosphine oxide Cynex923 provided by Cytec Company.

[0033] Aqueous phase material liquid: an industrial actual molybdenum-containing ammonium tungstate solution produced by a company using a quaternary ammonium salt alkaline medium extraction process, with a pH value of 9.5, adjusted to pH 3.0 with sulfuric acid, and adding 30% H 2 o 2 ,H 2 o 2 The addition amount is 1.8 times of the sum of moles of tungsten and molybdenum, the pH value is 1.30, and then the pH value is adjusted to 1.8 with ammonia solution to obtain the extraction material liquid, wherein WO 3 140.2g / L, Mo17.5g / L, Mo / WO 3 =0.125.

[0034] Extraction and separation: the above-mentioned organic phase and the aqueous phase feed liquid are subjected to 15-stage countercurrent extraction under the condition of a ratio of 3 / 2, and the loaded organic phase is subjected to a 3-sta...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention provides a method for extraction and separation of tungsten and molybdenum. Hydrogen peroxide is filled in the tungsten and molybdenum mixed solution, the pH value is regulated to be acidic, and the acid tungsten mixed solution is taken as a water phase feed liquid to carry out extraction and separation with an organic phase. The organic phase comprises trialkylphosphine oxide, tributyl phosphate and a diluting agent; the organic phase conducts the multi-stage extraction with the water phase feed liquid, molybdenum is extracted into the organic phase, and tungsten is left in a raffinate, so that the separation of tungsten and molybdenum is achieved. The load-bearing organic phase adopts an alkaline back-extraction agent to carry out back-extraction to obtain a molybdenum-contained solution, and the organic phase subjected to the back-extraction returns to the extraction process. Tungsten and molybdenum are extracted and separated in the tungsten and molybdenum mixed solution containing H2O2 by adopting a novel binary mixture extracting agent, the method has the advantages that extraction and the back-extraction are high in split-phase speed, the separation effect of tungsten and molybdenum is good, the tungsten co-extraction loss is low, the loss of the organic phase as well as the environmental pollution is low, the industrialization is easy to realize, and the method is especially suitable for separating tungsten and molybdenum in the tungstate solution with high molybdenum content.

Description

technical field [0001] The invention relates to a method for extracting and separating tungsten and molybdenum from a tungsten and molybdenum mixed solution. The invention belongs to the technical field of chemical extraction. Background technique [0002] Tungsten and molybdenum are important strategic rare metals and have a wide range of uses in industry. Tungsten and molybdenum belong to group VIB in the periodic table of elements. Due to the contraction of lanthanide, tungsten and molybdenum have very similar properties and are difficult to separate. Molybdenum is often associated with tungsten minerals, and many secondary resources (such as waste petroleum hydrogenation catalysts, waste cemented carbide) also contain tungsten and molybdenum. However, molybdenum is an impurity element that needs to be strictly controlled in tungsten metallurgy. For example, my country's national standard GB10116-2007 stipulates that the molybdenum content in 0-grade ammonium paratungst...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C22B34/34C22B34/36C22B3/40
CPCY02P10/20
Inventor 张贵清吴文君关文娟张红卫肖连生李晓宇张启修张互标
Owner CENT SOUTH UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products