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A kind of preparation method of hydroxamate collector

A hydroxamate and collector technology, which is applied in the field of mineral flotation collector preparation, can solve the problems that the influence of the environment cannot be ignored, the inconvenience of direct granulation, and large dust pollution, so as to eliminate pollution and shorten the reaction time , the effect of high production efficiency

Active Publication Date: 2019-12-20
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The traditional hydroxamic acid synthesis methods have their own advantages, but there are the following problems: 1) the traditional methods are generally carried out in a large amount of solvent systems, and the follow-up recovery treatment of the solvent is inevitably required; 2) the traditional methods generally use methyl monocarboxylate and other lower alcohol esters are raw materials, and volatile lower alcohols such as methanol are inevitably produced in the reaction process. The amount of methanol is small and difficult to collect, but the impact on the environment cannot be ignored; 3) due to the volatile characteristics of lower alcohols, traditional methods cannot The alcohols produced by the reaction are used as products, and the hydroxamic acid (salt) product obtained is a completely dry powder, which is not convenient for direct granulation, so that the dust pollution is large during the preparation and use, and the spilling and waste are serious

Method used

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  • A kind of preparation method of hydroxamate collector
  • A kind of preparation method of hydroxamate collector
  • A kind of preparation method of hydroxamate collector

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Taking 0.5mol diethylene glycol dibenzoate as a benchmark, put analytically pure diethylene glycol dibenzoate, hydroxylamine hydrochloride and sodium hydroxide in a molar ratio of 1:2.6:5.0 into SM-0.5L type agitating ball mill in turn, and stir The speed is 800r / min, react at the initial temperature of 32°C for 30min, and press the white solid product after the reaction on a 769YP-15A powder tablet press to obtain Φ5×8(mm) sodium benzohydroxamic acid particles. The yield of sodium benzohydroxamic acid was 86.41%. After acidifying the product, the UV spectrum was measured as figure 1 Shown; The product is directly measured by infrared spectrum as figure 2 shown.

Embodiment 2

[0057] Taking 1.0mol diethylene glycol dibenzoate as a benchmark, put technical grade diethylene glycol dibenzoate, hydroxylamine hydrochloride and sodium hydroxide into a WZM three-roller ball mill in a molar ratio of 1: 2.6: 5.0, and the stirring speed is 1400r / min, react at an initial temperature of 32°C for 40min, and press the white solid product after reaction on a 769YP-15A powder tablet press to obtain Φ5×8(mm) sodium benzohydroxamate particles. The yield of sodium benzohydroxamate was 80.21%.

Embodiment 3

[0059] Based on 0.05mol diethylene glycol dibenzoate, put analytically pure diethylene glycol dibenzoate, hydroxylamine hydrochloride and sodium hydroxide into the mortar in a molar ratio of 1:2.6:5.0, and start at 33°C Under high temperature, manually grind and react for 15 minutes, and press the white solid product after the reaction on a 769YP-15A powder tablet press to obtain Φ5×8 (mm) sodium benzohydroxamate particles. The yield of sodium benzohydroxamate was 88.91%. .

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Abstract

The invention provides a method for preparing hydroximic acid salt collector. Particularly, the method comprises the steps that grinding reaction is carried out on a di-esters compound shown in formula (I) and a hydroxylammonium salt compound shown in formula (II) under the action of alkali to prepare hydroximic acid salt shown in formula (III) and a dihydric alcohols compound shown in formula (IV); each R1 is independently aromatic base, naphthenic base or alkyl group; R2 is -(CH2)-n- or -(CH2)-n-O-(CH2)-n-; each n is independently 1-10; NH2OH M comprises hydroxylamine hydrochloride, hydroxylamine-O-sulfonate or hydroxylamine nitrate; the alkali comprises sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, dibasic sodium phosphate or sodium dihydrogen phosphate; Y<+> comprises sodium ion or potassium ion; alkyl group, aromatic base, naphthenic base, -(CH2)-n- or -(CH2)-n-O-(CH2)-n- can be optionally mono-substituted equally or differently polysubstituted by hydrogen, fluorine, chlorine, bromine, hydroxide radical, amidogen, carboxyl, alkyl group, alkoxy group or aromatic base. The method for preparing the hydroximic acid salt collector has the advantages that the processes are simple, the reaction time is short, the efficiency is high, and the hydroximic acid salt collector has no pollution.

Description

technical field [0001] The invention relates to the technical field of preparation of mineral flotation collectors, in particular to a preparation method of hydroxamate collectors. Background technique [0002] Hydroxamic acid is a common desilication flotation collector in industry. Due to the special structure of hydroxamic acid, it is easy to chelate with metal ions and has good selectivity to metal oxide ores. It is used in bauxite, ferro-titanium It is used in the flotation of ore, tin ore, copper oxide ore and other minerals. The synthesis methods of hydroxamic acid include hydroxylamine method, nitroalkane rearrangement method, nitroalkane reduction method, and reaction preparation method of nitroso compounds and aldehydes, among which the hydroxylamine method is the most commonly used in industrial production. The hydroxylamine method is based on carboxylic acid or its derivatives R-CO-L (L is OH, O, OR, Cl, Br, NH 2 etc.) and hydroxylamine as raw materials, the me...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C259/10C07C259/08C07C259/06B03D1/01
CPCB03D1/01B03D2201/02C07C259/06C07C259/08C07C259/10C07C2601/14
Inventor 钟宏刘威王帅
Owner CENT SOUTH UNIV
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