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Organic precipitator as well as preparation method and application thereof

An organic precipitant and sediment technology, applied in the field of organic precipitants and their preparation, can solve the problems of poor selectivity, high content of non-rare earth impurities, adverse effects on the quality of production products, etc., and achieve high yield, fast precipitation, and structural stable effect

Active Publication Date: 2018-08-10
厦门熙途科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the poor selectivity of the existing precipitants to rare earth elements, the content of non-rare earth impurities (such as iron, aluminum, calcium, silicon, etc.) in the formed precipitate is particularly high, which will adversely affect subsequent production and product quality.

Method used

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  • Organic precipitator as well as preparation method and application thereof
  • Organic precipitator as well as preparation method and application thereof
  • Organic precipitator as well as preparation method and application thereof

Examples

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preparation example Construction

[0042] The present invention also provides a method for preparing the organic precipitating agent described in the above technical scheme, comprising the following steps:

[0043] Alkylphenoxyacetic acid and hydroxide are reacted to obtain an organic precipitant;

[0044] The hydroxide is selected from one or more of lithium hydroxide, sodium hydroxide, potassium hydroxide, calcium hydroxide, magnesium hydroxide and aluminum hydroxide.

[0045] The alkylphenoxyacetic acid includes one or more of the structural compounds of formula (IV)~formula (VI):

[0046]

[0047] Among them, R 1 , R 2 , R 3 and R' 3 independently selected from substituted straight chain alkyl groups with 1 to 10 carbon atoms, unsubstituted straight chain alkyl groups with 1 to 10 carbon atoms, substituted branched chain alkyl groups with 3 to 10 carbon atoms, An unsubstituted branched alkyl group having 3 to 10 carbon atoms, a substituted aryl group or an unsubstituted aryl group.

[0048] In the ...

Embodiment 1

[0066] 1) Preparation of 1,1,3,3-tetramethylbutylphenoxyacetic acid:

[0067] Add 100 grams of absolute ethanol and 48.4 grams (0.21 mol) of sodium 1,1,3,3-tetramethylbutylphenolate into the reaction vessel. Turn on stirring and heating, raise the temperature to 110° C., and slowly add 37.8 grams (0.32 mol) of sodium chloroacetate into the reaction vessel. After reacting for 1.5 hours, cool to room temperature, distill the solvent of the obtained reaction product under reduced pressure, and then add 50 mL of 6mol / L hydrochloric acid solution for acidification. The acidification temperature is 30°C, and the acidification time is 5 minutes. After three times, distillation under reduced pressure at 160°C gave 1,1,3,3-tetramethylbutylphenoxyacetic acid.

[0068] The 1,1,3,3-tetramethylbutylphenoxyacetic acid prepared in this example was subjected to acid-base titration and NMR detection, the purity was greater than 98%, and it had the structure of formula (IV). In formula (IV), R...

Embodiment 2

[0082] 1) the preparation of p-phenoxydiacetic acid:

[0083] Add 100 grams of absolute ethanol and 22.0 grams (0.20 mol) of hydroquinone into the reaction vessel. Turn on stirring and heating, raise the temperature to 110° C., and slowly add 58.3 grams (0.5 mol) of sodium chloroacetate into the reaction vessel. After reacting for 1.5 hours, cool to room temperature, distill the solvent of the obtained reaction product under reduced pressure, and then add 60 mL of 6mol / L hydrochloric acid solution for acidification. The acidification temperature is 30 ° C, and the acidification time is 5 minutes. After three times, distill under reduced pressure at 160°C to obtain p-phenoxydiacetic acid.

[0084] The p-phenoxydiacetic acid prepared in this example is subjected to acid-base titration and NMR detection, the purity is greater than 98.5%, and it has the structure of formula (V). In formula (V), R 2 Take hydrogen.

[0085] 2) preparation of p-ammonium phenoxydiacetate:

[0086]...

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Abstract

The invention belongs to the field of rare earth gathering, and particularly relates to an organic precipitator as well as a preparation method and application thereof. The organic precipitator provided by the invention is prepared from one or more of structural compounds of formula (I) to formula (III), wherein R1, R2, R3 and R'3 are independently selected from hydrogen, substituted or non-substituted linear chain alkyl with the number of carbon atoms of 1 to 10, substituted or non-substituted branched alkyl with the number of the carbon atoms of 3 to 10, and substituted or non-substituted aryl; n is a natural integer; and M<n+> indicates cations. The organic precipitator provided by the invention has good selectivity to the rare earth and is very suitable for gathering rare-earth elements in a low-concentration rare-earth solution. The experiment result shows that when the organic precipitator provided by the invention is used for gathering the rare earth in the low-concentration rare earth solution, the precipitation speed is high, the purity of the gathered rare earth product is greater than 96 percent, and the yield is greater than 95 percent. (The formula (I) to (III) are shown in the description).

Description

technical field [0001] The invention belongs to the field of rare earth enrichment, and in particular relates to an organic precipitant and its preparation method and application. Background technique [0002] Southern ion-type rare earth mines are extremely important strategic resources in my country, rich in medium and heavy rare earths. At present, the leaching processes of ion-type rare earth ores are mainly pool leaching and in-situ leaching. The concentration of the obtained rare earth solution is very low, and it needs to be enriched to a high concentration before it can enter the next step of the rare earth separation plant. In recent years, with the continuous expansion of mining efforts, the concentration of rare earth solutions has continued to decrease, the content of impurities has continued to increase, and the difficulty of enrichment has continued to increase. [0003] At present, the enrichment of low-concentration rare-earth solutions mainly adopts the pre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C51/02C07C59/70C22B3/44C22B59/00
CPCC07C51/02C07C51/367C07C51/412C07C59/70C22B3/44C22B59/00Y02P10/20
Inventor 孙晓琦王艳良周海月苏佳
Owner 厦门熙途科技有限公司
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