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High-content liquid sodium benzohydroxamic acid as well as preparation and application thereof

A technology of sodium benzohydroxamate and benzoate, applied in solid separation, organic chemistry, flotation and other directions, can solve problems such as increasing the difficulty of wastewater treatment, achieve high product utilization rate and effective content, and save production cost, the effect of improving utilization

Active Publication Date: 2019-05-28
湖南中科矿冶技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this way, in the process of alkali addition-acid addition-alkali addition, not only a large amount of acid and alkali are repeatedly consumed, but also a large amount of waste water treatment problems are caused, and the waste water contains a part of benzohydroxamic acid soluble in water, which is more serious. The difficulty of wastewater treatment has become a difficult problem for enterprises

Method used

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  • High-content liquid sodium benzohydroxamic acid as well as preparation and application thereof
  • High-content liquid sodium benzohydroxamic acid as well as preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Add 50 grams of methyl benzoate and 0.6 grams of phenylethylphenol formaldehyde resin polyoxyethylene ether (Xingtai Lantian Fine Chemical Co., Ltd., Nongru 400#) into a three-necked flask, stir evenly, add 55 grams of water, and stir to emulsify . Add hydroxylamine sulfate 33.6 grams, after dissolving, add dropwise the sodium hydroxide solution of 81 grams 40%, control reaction solution temperature during dropwise at 30-31 ℃, pH value is not more than 12, after dropwise addition (1.5 hours), Heat at 30-31°C for 3 hours, then raise the temperature to 40°C, and react for 3 hours. After the reaction was completed, the precipitated salt was removed by filtration to obtain a solution of uniform sodium benzohydroxamic acid. In terms of benzohydroxamic acid, the content of benzohydroxamic acid was 24%. The product is tracked by gas chromatography, and the product has good stability within 6 months without decomposition by-products.

Embodiment 2

[0047] Add 50 grams of methyl benzoate and 0.7 grams of phenylethylphenol formaldehyde resin polyoxyethylene ether (Xingtai Lantian Fine Chemical Co., Ltd., Nongru 400#) into a three-necked flask, stir evenly, add 55 grams of water, stir and emulsify . Add hydroxylamine sulfate 33.6 grams, after dissolving, add dropwise the sodium hydroxide solution of 81 grams 40%, control reaction solution temperature during dropwise at 30-31 ℃, pH value is not more than 12, after dropwise addition (1.5 hours), Heat at 30-31°C for 3 hours, then raise the temperature to 40°C, and react for 3 hours. After completion of the reaction, the precipitated salt was removed by filtration to obtain a solution of uniform sodium benzohydroxamic acid. In terms of benzohydroxamic acid, the content of benzohydroxamic acid was 23.9%. The product is tracked by gas chromatography, and the product has good stability within 6 months without decomposition by-products.

Embodiment 3

[0049] Add 50 grams of methyl benzoate and 0.6 grams of alkylphenol formaldehyde resin polyoxyethylene ether (Handan Xindia Chemical Co., Ltd., Nongru 700#) into a three-necked flask, stir evenly, add 55 grams of water, and stir to emulsify. Add hydroxylamine sulfate 33.6 grams, after dissolving, add dropwise the sodium hydroxide solution of 81 grams 40%, control reaction solution temperature during dropwise at 30-31 ℃, pH value is not more than 12, after dropwise addition (1.5 hours), Heat at 30-31°C for 3 hours, then raise the temperature to 40°C, and react for 3 hours. After the reaction was completed, the precipitated salt was removed by filtration to obtain a solution of uniform sodium benzohydroxamic acid. In terms of benzohydroxamic acid, the content of benzohydroxamic acid was 23.4%. The product is tracked by gas chromatography, and the product has good stability within 6 months without decomposition by-products.

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Abstract

The invention belongs to the field of preparation of flotation materials and specifically discloses a preparation method of liquid sodium benzohydroxamic acid. The preparation method comprises the following steps: carrying out a hydroxyl oximation reaction on benzoate and hydroxylamine sulfate in a solution containing a macromolecular emulsifier and alkali, then carrying out solid-liquid separation to obtain the liquid sodium benzohydroxamic acid, wherein the macromolecular emulsifier is at least one of pesticide emulsifier 400#, pesticide emulsifier 700#, APEP-108 and pesticide emulsifier 1602#. The invention further provides the liquid sodium benzohydroxamic acid prepared by adopting the method and application of the liquid sodium benzohydroxamic acid. According to the invention, the hydroxylamine sulfate is adopted as a hydroxylamine raw material and is matched with the macromolecular emulsifier involved in the invention to be subjected to the hydroxyl oximation reaction; and afterthe reaction, the liquid sodium benzohydroxamic acid with high effective solid content and good stability can be obtained through the simple solid-liquid separation.

Description

technical field [0001] The invention belongs to the field of flotation agents and relates to liquid sodium benzohydroxamate. Background technique [0002] The hydroxime group in benzohydroxamic acid contains N atom and O atom, they all have lone pair electrons, belong to weak electron donor, it is easy to form stable chelate with metal ion, and benzene ring itself can provide certain Hydrophobic. Therefore, benzohydroxamic acid has excellent chelation and collection performance, and is widely used in the flotation of various oxide ores and rare earths such as ilmenite, bastnaesite, niobasite, and niobium-tantalum ore. [0003] At present, the production of benzyl hydroxamic acid is mainly obtained by the hydroxamation reaction of methyl benzoate with hydroxylamine hydrochloride. There are mainly two methods for the hydroximation reaction. One is to use methanol as a solvent. After the reaction, the solvent is distilled off or filtered to obtain the product (Jiang Renwang, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C259/10B03D1/01B03D101/02
Inventor 李春林孙昱符剑刚蒋泽斌
Owner 湖南中科矿冶技术有限公司
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