Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Pentaalkyl-diethylene-tri-tert-amine and its preparation method and use

A technology of pentaalkyl diethylene and tritertiary amine, applied in the field of metallurgy, can solve the problems of high cost, poor selectivity, high price, etc., and achieve the effects of simple operation, mild reaction conditions, and good extraction and separation effect.

Active Publication Date: 2015-01-28
CENT SOUTH UNIV
View PDF1 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] For the extractants of tungsten, molybdenum and vanadium in the prior art of this field, such as organic phosphoric acid such as P204, Cyanex272, neutral extractants such as TOPO and TBP, hydroximes such as LIX63, etc., there are poor selectivity, high price, high cost, etc. A series of defects, the object of the present invention is to provide a kind of pentaalkyldiethylene tri-tertiary amine compound with novel structure, which can be used for selective extraction and separation of tungsten, molybdenum and vanadium anions in aqueous solution

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

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Pentaalkyl-diethylene-tri-tert-amine and its preparation method and use
  • Pentaalkyl-diethylene-tri-tert-amine and its preparation method and use
  • Pentaalkyl-diethylene-tri-tert-amine and its preparation method and use

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] In a 250mL three-necked flask equipped with a stirrer, a reflux condenser, and a dropping funnel, add 0.1mol of diethylenetriamine, 0.5mol of anhydrous potassium carbonate, and 50mL of absolute ethanol, start the stirrer, heat, and keep the reaction temperature at 75 After ℃, start to add 0.5mol n-bromohexane dropwise, the dropping rate is 20-30 drops / min, stop after 12 hours of reaction, cool down, the mixture is filtered to obtain a bright yellow transparent solution, and distilled under reduced pressure to remove ethanol and a small amount of unreacted Bromo-n-hexane obtains the product after vacuum distillation, and the product after vacuum distillation is washed with 10% sodium hydroxide by mass fraction, and the solution is divided into three layers, the upper layer is a yellow oily liquid, the middle layer is reddish brown, and the lower layer is a colorless transparent liquid. Take out the middle and lower layers, add cyclohexane to extract three times, 5 mL each...

Embodiment 2

[0034] The feed liquid is pure molybdenum feed liquid in which ammonium molybdate is dissolved in deionized water, containing 4.93g L of molybdenum -1 , adjusted to pH=3 with sulfuric acid.

[0035] Organic phase: prepare four organic phases with numbers 1, 2, 3, and 4, the extractant of the organic phase is N, N, N', N", N"-pentahexyldiethylenetriamine, and the diluent is sulfonated Kerosene, the modifier is 2-octyl alcohol, the volume ratio of fixed 2-octanol to sulfonated kerosene is 1:2, and the No. 1 organic phase is 1% N,N,N',N",N"-pentahexyldiethylenetri Amine, 3% by volume of organic phase No. 2 N,N,N',N",N"-Pentahexyldiethylenetriamine, 5% by volume of organic phase No. 3N,N,N',N",N",N" - Pentahexyldiethylenetriamine, organic phase No. 4 is 7% by volume N,N,N',N",N"-pentahexyldiethylenetriamine.

[0036] The above four organic phases were acidified with sulfuric acid and then subjected to single-stage extraction under the condition of O / A (volume ratio of organic ph...

Embodiment 3

[0041] The feed liquid is a synthetic feed liquid in the laboratory, containing Mo 4.416g L -1 , Fe 2+ (Fe 3+ )1.119g L -1 、Ni 2+ 2.06g·L -1 , P 1.481g·L -1 , adjust the pH to 1.5 with sulfuric acid.

[0042] The composition of the organic phase is 7% by volume N,N,N',N",N"-pentahexyldiethylenetriamine + 31% by volume 2-octanol + 62% by volume sulfonated kerosene, after acidification with sulfuric acid, in O / A =1 / 4 for single-stage extraction, the temperature is 25°C, and the extraction time is 10min. The experimental results are shown in Table 2.

[0043] Table 2 N, N, N', N", N"-Pentahexyldiethylenetriamine Selective Extraction and Separation Effect of Molybdenum

[0044] the element

[0045] As shown in Table 2, the extraction rate of organic relative molybdenum is relatively high, but nickel is not extracted, so a higher separation effect of molybdenum and nickel can be achieved.

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 discloses pentaalkyl-diethylene-tri-tert-amine and its preparation method and use. The preparation method comprises that brominated C4-C8 alkane is slowly and dropwisely added into a diethylenetriamine-containing organic solution, the mixed solution is heated and undergoes a replacement reaction in the presence of anhydrous potassium carbonate, and the product is separated and purified to form the pentaalkyl-diethylene-tri-tert-amine having a novel structure. The preparation method has simple processes and mild reaction conditions. The pentaalkyl-diethylene-tri-tert-amine compound can be used as an extraction agent for effective extraction separation of molybdate, tungstateradicle or vanadate anions and widens an extraction agent selection range in the tungsten, molybdenum and vanadium extraction separation technology.

Description

technical field [0001] The invention relates to a pentaalkyldiethylene tritertiary amine, a preparation method and application thereof, and belongs to the technical field of metallurgy. Background technique [0002] Tungsten, molybdenum and vanadium are important strategic rare metals, which are widely used in industry. With the increase in demand for tungsten, molybdenum and vanadium, the development of tungsten, molybdenum and vanadium resources is no longer limited to some traditional resources, but also includes many secondary resources, extracting tungsten and molybdenum from solutions containing tungsten, molybdenum and vanadium , vanadium methods, including precipitation, ion exchange and solvent extraction, because solvent extraction has the advantages of easy continuous operation, good economic benefits, large capacity, and wide application sources, it has always been concerned by industry and scholars. [0003] The extractants for extracting tungsten, molybdenum a...

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
Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/08C07C211/14C22B3/28C22B34/36C22B34/34C22B34/22
CPCY02P10/20
Inventor 曹佐英周小舟肖连生关文娟李青刚张贵清曾理
Owner CENT SOUTH UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com