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Collecting agent as well as preparation method and application thereof

A collector and reaction technology, applied in solid separation, flotation, etc., can solve problems such as insufficient collection force, and achieve the effects of small dosage of chemicals, convenient operation and simple process

Active Publication Date: 2018-10-19
INST OF RESOURCES UTILIZATION & RARE EARTH DEV GUANGDONG ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the hydroxamic acids in the application market are mainly benzohydroxamic acid, salicylic hydroxamic acid and C 5-9 Alkyl hydroxamic acid, which has good flotation selectivity for oxide ore, but the collection capacity is slightly insufficient

Method used

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  • Collecting agent as well as preparation method and application thereof
  • Collecting agent as well as preparation method and application thereof
  • Collecting agent as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Add 0.05mol decyl salicylic acid, 0.1mol methanol, and 0.0005mol concentrated sulfuric acid into the reactor, and stir and react at 80°C for 9 hours to obtain methyl decyl salicylate. According to the national standard GB / T12717-2007, The measured esterification rate was 75.2%. Take 0.041mol hydroxylamine hydrochloride, 0.15mol sodium hydroxide, decyl methyl salicylate obtained from the above reaction and 40mL water, control the reaction temperature at 40°C, react for 6 hours, acidify with concentrated sulfuric acid, remove the reaction solvent to obtain a collector 13.9g. The content of decyl salicylic hydroxamic acid in this embodiment is 61.5% as measured by the Kjeldahl method. Infrared spectrum see figure 1 , 3292cm -1 and N-H and -OH stretching vibration peaks, 2928 and 2852cm -1 for -CH 3 and -CH 2 -Asymmetric stretching vibration peak, 1658cm -1 For the carbon base (C=0) stretching vibration peaks, 1604 and 1490cm -1 It is the swing peak of the skeleton ...

Embodiment 2

[0039] Add 0.05mol decyl salicylic acid, 0.2mol methanol, and 0.005mol benzenesulfonic acid into the reactor, stir and react at 100°C for 6 hours to obtain methyl decyl salicylate, according to the national standard GB / T12717-2007 , The measured esterification rate was 85.2%. Take 0.051mol hydroxylamine hydrochloride, 0.16mol sodium hydroxide, decyl salicylate methyl ester obtained from the above reaction and 40mL methanol solvent, control the reaction temperature at 50°C, react for 4.5 hours, acidify with concentrated sulfuric acid, remove the reaction solvent to collect Dose 14.5g. The content of decyl salicyl hydroxamic acid in this embodiment was 76.1% by Kjeldahl method. Infrared spectrum see figure 2 , 3291cm -1 and stretching vibration peaks of N-H and -OH, 2930 and 2859 cm -1 for -CH 3 and -CH 2 -Asymmetric stretching vibration peak, 1658cm -1 For the carbon base (C=0) stretching vibration peaks, 1602 and 1489cm -1 It is the swing peak of the skeleton of the b...

Embodiment 3

[0041] Add 0.05mol decyl salicylic acid, 0.4mol methanol, and 0.01mol p-toluenesulfonic acid to the reactor, stir and react at 120°C for 3 hours to obtain methyl decyl salicylate, according to the national standard GB / T12717- In 2007, the measured esterification rate was 86.7%. Mix 0.056 mol of hydroxylamine hydrochloride, 0.175 mol of sodium hydroxide, decyl salicylate methyl ester obtained from the above reaction and 40 mL of ethanol solvent, control the reaction temperature at 60°C, react for 3 hours, acidify with concentrated sulfuric acid, remove the reaction solvent and collect Dose 14.2g. The content of decyl salicyl hydroxamic acid in this embodiment is 69.4% by Kjeldahl method. Infrared spectrum see image 3 , 3292cm -1 and N-H and -OH stretching vibration peaks, 2928 and 2852cm -1 for -CH 3 and -CH 2 -Asymmetric stretching vibration peak, 1652cm-1 For the carbon base (C=0) stretching vibration peaks, 1604 and 1495cm -1 It is the swing peak of the skeleton of t...

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Abstract

The invention discloses a collecting agent as well as a preparation method and application thereof. The collecting agent is composed of decyl salicylhydroxamic acid, methyl decyl salicylate and decylsalicylic acid, is in a brown yellow viscous state at the normal temperature, can be dispersed in an alkali solution, and has relatively strong collecting capacity on non-ferrous metal oxide ores. Thecollecting agent can be prepared by a one-pot method and is simple in process. The preparation method of the collecting agent comprises the following steps that the decyl salicylic acid and methanolare mixed, a catalyst is added, and the methyl decyl salicylate is generated under stirring through the reaction; the methyl decyl salicylate and the hydroxylamine hydrochloride are mixed with alkali,water, the methanol or ethanol is taken as a solvent, and the collecting agent being the mixture of the decyl salicylhydroxamic acid, the methyl decyl salicylate and the decyl salicylic acid is obtained through the reaction and acidifying. The collecting agent is applied to beneficiation of tungsten ores, rare earth ores and tin ores.

Description

technical field [0001] The invention belongs to the field of flotation agent and its preparation, and mainly relates to a collector, its preparation method and application. Background technique [0002] Hydroxamic acid (Hydroxamic acid) has a strong chelating ability to metal ions (Cu, Cr, Co, Fe, Mn, W, Sn), and is usually used as copper oxide ore, black and white tungsten ore, rare earth and tin ore in mineral engineering The flotation collector is used. Because hydroxamic acid is expensive to prepare and has good selectivity, it is usually compounded with other agents to reduce cost pressure and optimize flotation indicators. [0003] CN101579653A discloses a method for beneficiating fine-grained tungsten ore in fine-grained tungsten ore in scheelite heating and beneficiation of scheelite hydroxamic acid and sulfated oleic acid soap as collectors. The addition of sulfated oleic acid soap can make up for the insufficient collection capacity of benzohydroxamic acid. CN10...

Claims

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Application Information

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IPC IPC(8): B03D1/001B03D101/02B03D103/02
CPCB03D1/001B03D2201/02B03D2203/02
Inventor 李方旭张发明林日孝刘进齐越超张辉蒋海勇郑少冰陈志杰
Owner INST OF RESOURCES UTILIZATION & RARE EARTH DEV GUANGDONG ACAD OF SCI
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