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Amino phosphonic acid compound and preparation method and application thereof

An aminophosphonic acid and compound technology, which is applied in the field of aminophosphonic acid compounds, can solve the problems of complex preparation process, low synthesis yield and insignificant effect, etc., and achieves easy industrial production, high product yield and good water solubility. Effect

Active Publication Date: 2018-12-04
BLUESTAR LEHIGH ENG INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These organic phosphonic acid compounds are used as flotation collectors, and the sorting is good, but the preparation process of these compounds is complicated, the synthesis yield is low, and the environmental pollution is relatively large in the preparation process. Used as a collector in iron ore, bauxite, phosphate rock and other mines, the effect is not obvious and the selectivity is poor

Method used

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  • Amino phosphonic acid compound and preparation method and application thereof
  • Amino phosphonic acid compound and preparation method and application thereof
  • Amino phosphonic acid compound and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1, an aminophosphonic acid compound, the general formula of the compound is shown in (I):

[0023]

[0024] Wherein: R is H, F, Cl or Br.

[0025] Its preparation method includes the following steps: add aniline or aniline containing substituents, phosphorous acid solution and an acidic catalyst in a reaction kettle, raise the temperature of the reaction system to 80°C, and slowly add 3,7-dimethyl Base-2,6-octadienal, after the dropwise addition, raise the temperature of the reaction system to 110°C, react at this temperature, and obtain a white solid after cooling. The reaction time was 1 hour. The acidic catalyst used in the reaction is selected from one of hydrochloric acid, sulfuric acid, nitric acid, hydrofluoric acid or phosphoric acid; the reaction raw material is 3,7-dimethyl-2,6-octadienal, aniline or aniline containing substituents The molar ratio of phosphorous acid and acidic catalyst is 1:1:1:0.02. Aminophosphonic acid compounds are used as...

Embodiment 2

[0026] Embodiment 2, an aminophosphonic acid compound, the general formula of the compound is shown in (I):

[0027]

[0028] Where: R is C 1~6 Hydrocarbyl.

[0029] Its preparation method comprises the following steps: adding aniline or aniline containing substituents, phosphorous acid solution and an acidic catalyst into a reaction kettle, raising the temperature of the reaction system to 100°C, and slowly adding 3,7-dimethyl Base-2,6-octadienal, after the dropwise addition, raise the temperature of the reaction system to 160°C, react at this temperature, and obtain a white solid after cooling. The reaction time was 4 hours. The acid catalyst used in the reaction is selected from oxalic acid, citric acid, tartaric acid, glycolic acid, phthalic acid, sulfamic acid or p-toluenesulfonic acid. The molar ratio of the reaction raw materials 3,7-dimethyl-2,6-octadienal, aniline or aniline containing substituents, phosphorous acid and acidic catalyst is 1: 2: 3: 0.08. Aminoph...

Embodiment 3

[0030] Embodiment 3, an aminophosphonic acid compound, the general formula of the compound is shown in (I):

[0031]

[0032] Where: R is H.

[0033] Its preparation method includes the following steps: add aniline or aniline containing substituents, phosphorous acid solution and an acidic catalyst in a reaction kettle, raise the temperature of the reaction system to 90°C, and slowly add 3,7-dimethyl Base-2,6-octadienal, after the dropwise addition, raise the temperature of the reaction system to 130°C, react at this temperature, and obtain a white solid after cooling. The reaction time was 1.5 hours. The acid catalyst used in the reaction is selected from oxalic acid, citric acid, tartaric acid, glycolic acid, phthalic acid, sulfamic acid or p-toluenesulfonic acid. The molar ratio of the reaction raw materials 3,7-dimethyl-2,6-octadienal, aniline or aniline containing substituents, phosphorous acid and acidic catalyst is 1:1:1:0.05. Aminophosphonic acid compounds are us...

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Abstract

The invention discloses an amino phosphonic acid compound and further discloses a preparation method of the amino phosphonic acid compound. The general formula of the compound is shown as the formula(I) (Please see the specifications for the formula). The amino phosphonic acid compound is prepared through the mode that 3,7-dimethyl-2,6-octadienal, aniline or aniline containing a substituent group, and phosphorous acid are subjected to a Mannich reaction under the action of acid catalysts. The amino phosphonic acid compound can be used as a floatation collector of ilmenite, bauxite, fluorite ores, rare earth ores or collophanite and has the characteristics of good selectivity, high water solubility, good dispersibility and the like, and the flotation recovery rate can be increased by 2-16percent points. The preparation method adopts a one-pot synthesis method, operation is easy to control, the product yield is high, and industrial production is easy.

Description

technical field [0001] The invention belongs to the field of mineral flotation, and relates to an aminophosphonic acid compound. The invention also relates to its preparation method and its application in flotation of ilmenite, bauxite, rare earth ore, fluorite ore or phosphate rock. Background technique [0002] Oleic acid and its modified products are the most commonly used mineral processing collectors in the flotation process of oxidized ore. Acid is used as a collector, which can effectively improve the grade of iron ore concentrate; Chinese published patent literature (publication number: CN101585016) uses oleic acid as a collector in the low-grade fluorite-barite flotation separation method, and water glass is siliceous and calcium Flotation separation of high quality mineral inhibitors; Chinese published patent literature (publication number: CN101712014A) multi-type impurity single-type fluorite ore beneficiation method uses alkaline oleic acid, neutral oleic acid a...

Claims

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Application Information

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IPC IPC(8): B03D1/014B03D101/02B03D103/06B03D103/04
CPCB03D1/014B03D2201/02B03D2203/04B03D2203/06
Inventor 刘养春宋文义杨勇刘国举徐会会张晓梅
Owner BLUESTAR LEHIGH ENG INST CO LTD
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