Green preparation method for hydroxyl oxime acid rare-earth flotation agents

A flotation reagent and rare earth technology, which is applied in the preparation of carboxylic acid esters, the preparation of organic compounds, flotation, etc., can solve the problems of environmental protection pressure and governance problems of production enterprises, high industrial production costs, increased production costs, etc., to achieve flotation Excellent selection performance, improve the economic benefits of the enterprise, and reduce the effect of wastewater discharge

Active Publication Date: 2016-10-12
INST OF MULTIPURPOSE UTILIZATION OF MINERAL RESOURCES CHINESE ACAD OF GEOLOGICAL SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, the catalyst is expensive, resulting in high industrial production costs
[0007] The above cases show that a large amount of waste liquid will be produced in the traditional production of rare earth collectors, which is not friendly to the environment, will bring environmental protection pressure and governance problems to production enterprises, and increase production costs

Method used

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  • Green preparation method for hydroxyl oxime acid rare-earth flotation agents
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  • Green preparation method for hydroxyl oxime acid rare-earth flotation agents

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Process flow chart such as figure 2 shown.

[0041] Will C 5～7 Add 20kg of fatty acid, 10kg of o-hydroxynaphthoic acid and 10kg of methanol into the enamel reaction kettle. After stirring evenly, add 2.8kg of concentrated sulfuric acid. After installing the cooling reflux device, start heating and reflux reaction for 20 hours. After cooling to room temperature, add Add 15% hydroxylamine sulfate aqueous solution of 16.0kg hydroxylamine sulfate to the enamel reaction kettle, add dropwise a 35% sodium hydroxide aqueous solution while stirring, keep the pH value in the reactor not less than 10, control the reaction temperature at 35°C, hydrogen The amount of sodium oxide to be added is 19.0kg. After the dropwise addition, the reaction is continued for 4 hours, and the temperature is kept at 50°C for another 8 hours after the reaction. After the reaction is completed, the reaction product is neutralized with dilute sulfuric acid to a pH value of 5.0-6.0, and stirred After...

Embodiment 2

[0043] Process flow chart such as image 3 shown.

[0044] Will C 5～7 Add 20kg of fatty acid, 10kg of o-hydroxynaphthoic acid and 10kg of methanol into the enamel reaction kettle, stir evenly, add 2.8kg of concentrated sulfuric acid, install the cooling reflux device, start heating and reflux reaction for 20 hours, and the product is centrifuged to obtain a paste Mixed carboxylate, the liquid is stored for later use; the paste mixed carboxylate of gained and the 15% hydroxylammonium sulfate aqueous solution containing 16.0kg hydroxylammonium sulfate are added in the enamel reaction kettle, while stirring, the mass fraction is 35% hydrogen Sodium oxide aqueous solution, keep the pH value in the reaction kettle not less than 10, control the reaction temperature at 35°C, add 16.0kg of sodium hydroxide dropwise, react for 4 hours after the dropwise addition, keep warm for 8 hours after the reaction, and the temperature is 50°C ; After the reaction is completed, the waste liquid ...

Embodiment 3

[0046] Except C 5～7 Fatty acid obtains weight and is 50g, and the weight of o-hydroxy naphthoic acid is 30g, and the addition of the vitriol oil is 8g, and reflux time is 30 hours, and the molar number of 15~25% hydroxylamine sulfate aqueous solution is that molar number is C 5～7 Except 0.65 times of fatty acid and o-hydroxy naphthoic acid total molar number, all the other are consistent with embodiment 1.

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Abstract

The invention provides a green preparation method for hydroxyl oxime acid rare-earth flotation agents. The green preparation method comprises the steps of fatty acid esterification, fatty acid ester oximation and acidification. After the fatty acid esterification and before the fatty acid ester oximation, waste liquid is not treated, and a fatty acid esterification mixed product is totally added into a reaction kettle for performing oximation directly. The invention also provides another green preparation method for the hydroxyl oxime acid rare-earth flotation agents. The green preparation method comprises the steps of fatty acid esterification, fatty acid ester separation and purification, fatty acid ester oximation and acidification; when the step of fatty acid ester acidification is performed, the waste liquid obtained by separating and purifying the fatty acid ester is added. A hydroxyl oxime acid rare-earth collecting agent is synthesized by adopting the process provided by the invention, the waste water discharge during a synthesizing process can be reduced; the green preparation of the hydroxyl oxime acid rare-earth flotation agents can be realized; the economic benefit of an enterprise can be greatly improved; meanwhile, the flotation agents obtained by the method provided by the invention have excellent flotation performance.

Description

technical field [0001] The invention relates to the field of synthesis of flotation agents, in particular to a green preparation method of hydroxamic acid rare earth flotation agents. Background technique [0002] Hydroxamic acid (Hydroxamic Acid) and its salts are a new type of high-efficiency chelating agent. Its molecular formula is RCOHN-OH (wherein -R is an alkyl or aryl group), and it is a very active organic weak acid. Hydroxamic acid reacts on many metal ions (Cu 2+ 、Co 2+ 、Ni 2+ , Fe 3+ , Zn 2+ etc.) have strong chelating activity and can form stable four-membered ring and five-membered ring chelates, so hydroxamic acid is widely used in the mineral processing industry, such as in lead-zinc oxide ore, copper oxide ore and rare earth ore It is widely used as a collector in flotation, and hydroxamic acid is the most effective collector for the flotation of bastnaesite, niobium-tantalum ore, iron ore and tungsten ore. [0003] Hydroxamic acid is usually prepared ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C259/06B03D1/018B03D101/02
CPCY02P20/582C07C67/08B03D1/018B03D2201/02C07C259/06C07C69/003
Inventor 熊文良陈炳炎陈达邓杰邓善芝
Owner INST OF MULTIPURPOSE UTILIZATION OF MINERAL RESOURCES CHINESE ACAD OF GEOLOGICAL SCI
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