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Alpha-hydroxy unsaturated alkylphosphonic acid compound as well as preparation method and application of alpha-hydroxy unsaturated alkylphosphonic acid compound

An alkyl phosphonic acid, unsaturated technology, applied in the field of mineral flotation collector compound and its preparation

Active Publication Date: 2014-03-05
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The chain hydrocarbon unsaturated hydroxy acid has a suitable hydrophobic carbon chain (C 8 ) and double-hydrophilic configuration, with a hydroxyl group and a phosphonic acid group in its molecule, it is a brand new compound, and there is no literature report on it

Method used

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  • Alpha-hydroxy unsaturated alkylphosphonic acid compound as well as preparation method and application of alpha-hydroxy unsaturated alkylphosphonic acid compound
  • Alpha-hydroxy unsaturated alkylphosphonic acid compound as well as preparation method and application of alpha-hydroxy unsaturated alkylphosphonic acid compound
  • Alpha-hydroxy unsaturated alkylphosphonic acid compound as well as preparation method and application of alpha-hydroxy unsaturated alkylphosphonic acid compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Example 1 Preparation of 1-hydroxyl-2-ethyl-2-hexene-1-phosphonous acid

[0032] Fully mix 4.4 parts of 2-ethyl-2-hexenal, 40 parts of 1,4-dioxane, 7 parts of hypophosphorous acid, and 2 parts of 20% dilute sulfuric acid, stir at 80°C for 5 hours, and use 1.4 parts of ethyl acetate Ester extraction of 1-hydroxy-2-ethyl-2-hexene-1-phosphonous acid, the extraction temperature is 30 ° C, extraction 3 times, liquid separation, take the upper liquid and distill under reduced pressure to remove ethyl acetate, the distillation temperature is 50 °C, the vacuum degree is 0.098MPa, the residue is 1-hydroxy-2-ethyl-2-hexene-1-phosphonous acid, and the yield is 75.2%.

Embodiment 2

[0033] Example 2 Preparation of 1-hydroxyl-2-ethyl-2-hexene-1-phosphonous acid

[0034] Fully mix 4.4 parts of 2-ethyl-2-hexenal, 40 parts of 1,4-dioxane, 7 parts of hypophosphorous acid, and 1 part of 37% concentrated hydrochloric acid, stir and react at 80°C for 5 hours, and use 1.4 parts of ethyl acetate Ester extraction of 1-hydroxy-2-ethyl-2-hexene-1-phosphonous acid, the extraction temperature is 30 ° C, extraction 3 times, liquid separation, take the upper liquid and distill under reduced pressure to remove ethyl acetate, the distillation temperature is 50 °C, the vacuum degree is 0.098MPa, the residue is 1-hydroxy-2-ethyl-2-hexene-1-phosphonous acid, and the yield is 83.5%.

Embodiment 3

[0035] Example 3 Preparation of 1-hydroxyl-2-ethyl-2-hexene-1-phosphonous acid

[0036]Mix 4.4 parts of 2-ethyl-2-hexenal, 40 parts of ethanol, 7 parts of hypophosphorous acid, and 1 part of hydrochloric acid, stir and react at 80°C for 5 hours, and extract 1-hydroxy-2-ethyl with 1.4 parts of ethyl acetate -2-hexene-1-phosphonous acid, the extraction temperature is 30°C, extract 3 times, separate the liquid, take the upper liquid and distill under reduced pressure to remove ethyl acetate, the distillation temperature is 55°C, the vacuum degree is 0.098MPa, the residue That is 1-hydroxy-2-ethyl-2-hexene-1-phosphonous acid with a yield of 70.6%.

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Abstract

The invention discloses an alpha-hydroxy unsaturated alkylphosphonic acid compound as well as a preparation method and application of the alpha-hydroxy unsaturated alkylphosphonic acid compound. The alpha-hydroxy unsaturated alkylphosphonic acid compound has the structural formula I as shown in the specification. The preparation method comprises the steps: subjecting 2-ethyl-2-hexenal and hypophosphorous acid or hypophosphite to addition reaction in the existence of an acid catalyst to generate 1-hydroxyl-2-ethyl-2-hexenyl-1-phosphorous acid; subjecting 1-hydroxyl-2-ethyl-2-hexenyl-1-phosphorous acid and an oxidizing agent to reaction to generate 1-hydroxyl-2-ethyl-2-hexenyl-1-phosphonic acid. 30-600g / t of 1-hydroxyl-2-ethyl-2-hexenyl-1-phosphonic acid is used as a flotation collector for bauxite, ilmenite, rutile, scheelite, wolframite, rare earth ores, tin ores, fluorite ores or lithium ores, and the pH value of a flotation solution is controlled at 4-12, so that a target ore and a gangue mineral can be effectively separated.

Description

technical field [0001] The invention belongs to the technical field of mineral processing, and relates to a new compound used as a mineral flotation collector and a preparation method thereof, and the compound is used in bauxite, ilmenite, rutile, scheelite, wolframite, rare earth The application as a collector in ore, tin ore, fluorite ore or lithium ore flotation. Background technique [0002] The collector with long carbon chain is an excellent collector for oxide ore due to its polar hydroxyl and phosphonic acid functional groups. Alkyl phosphonic acid has a weak ability to collect silicate minerals. At the same time of flotation, adding appropriate inhibitors, such as starch, dextrin, sodium humate or water glass, can successfully separate useful minerals from gangue. Mineral separation. Oleic acid and its modified products are currently the most commonly used collectors for oxidized ore in industrial flotation processes. Patents CN101648157A and CN101757983A disclos...

Claims

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Application Information

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IPC IPC(8): C07F9/38B03D1/014B03D101/02
Inventor 钟宏李方旭王帅黄志强刘广义曹占芳
Owner CENT SOUTH UNIV
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