Collecting system prepared from W/O/W multiphase emulsion as well as preparation method and application thereof

A multi-phase emulsion and system technology, applied in solid separation, flotation, etc., can solve the problems of large pollution, large amount of hydroxylamine, low yield of benzyl hydroxamic acid, etc., achieve high yield and accelerate the rate of oximation reaction , The effect of drug cost reduction

Active Publication Date: 2019-08-20
INST OF RESOURCES UTILIZATION & RARE EARTH DEV GUANGDONG ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to overcome the defects and deficiencies that hydroxylamine will decompose in a strong alkali environment in the existing production process of benzohydroxamic acid, the amount of hydroxylamine is large, the productive rate of benzohydroxamic acid is low, and the pollution is large, and provide a A kind of W / O / W multiphase emulsion prepares the method for collection system

Method used

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  • Collecting system prepared from W/O/W multiphase emulsion as well as preparation method and application thereof
  • Collecting system prepared from W/O/W multiphase emulsion as well as preparation method and application thereof
  • Collecting system prepared from W/O/W multiphase emulsion as well as preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] This embodiment provides a collection system, which is prepared by the following method.

[0036] In a 250 mL three-necked double-necked reaction flask equipped with a condenser, a stirrer and a thermometer, 20.0 g of methyl benzoate and 0.2 g of Span-80 were mixed, and 26 mL of 40% aqueous hydroxylamine hydrochloride was added dropwise. After the system is uniformly dispersed to form a water-in-oil emulsion, gradually add 24mL of 50% sodium hydroxide to form a W / O / W multi-phase emulsion system, control the temperature to 40±1°C, and react for 4h. After the reaction, add concentrated sulfuric acid until the pH of the solution is about 6, leave standstill to obtain 82.4g of product, obtain the content of benzohydroxamic acid of product by Kjeldahl method and be 22.5%, and the yield of benzohydroxamic acid is 93.4% %.

Embodiment 2

[0038] This embodiment provides a collection system, which is prepared by the following method.

[0039]In a 250 mL three-necked double-layer reaction flask equipped with a condenser, a stirrer and a thermometer, 20.0 g of methyl benzoate and 0.8 g of dodecyl glucoside were mixed, and 27 mL of 40% hydroxylamine hydrochloride aqueous solution was added dropwise. After the system is uniformly dispersed to form a water-in-oil emulsion, gradually add 25 mL of 50% sodium hydroxide to form a W / O / W multi-phase emulsion system, control the temperature at 42±1°C, and react for 3 hours. After the reaction finished, add concentrated sulfuric acid to the solution pH is about 6, leave standstill to obtain benzohydroxamic acid thick product 85.6g, obtain the content of the benzohydroxamic acid of product by the Kjeldahl nitrogen method be 21.7%, benzylhydroxamic acid The yield of xamic acid was 93.5%.

Embodiment 3

[0041] This embodiment provides a collection system, which is prepared by the following method.

[0042] In a 250 mL three-necked double-necked reaction flask equipped with a condenser, a stirrer and a thermometer, 20.0 g of methyl benzoate and 1.6 g of Triton X-200 were mixed, and 28 mL of a 40% aqueous solution of hydroxylamine hydrochloride was added dropwise. After the system is uniformly dispersed to form a water-in-oil emulsion, gradually add 29 mL of 50% sodium hydroxide to form a W / O / W multi-phase emulsion system, control the temperature at 45±1°C, and react for 2.5 hours. After the reaction finished, add concentrated sulfuric acid to the solution pH is about 6, leave standstill to obtain benzohydroxamic acid thick product 88.4g, obtain the content of the benzohydroxamic acid of product by Kjeldahl method be 20.3%, benzylhydroxamic acid The yield of xamic acid was 90.4%.

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Abstract

The invention relates to a collecting system prepared from W / O / W multiphase emulsion as well as a preparation method and application thereof. The method comprises the following steps: adding a hydroxylamine water solution into a methyl benzoate and surfactant system; after the system is uniformly dispersed to form water-in-oil microemulsion, adding alkali and neutralizing to form the water-in-oil-in-water W / O / W multiphase emulsion; carrying out oximation reaction; then dropwise adding concentrated sulfuric acid to obtain the collecting system. The collecting system provided by the invention selects water as a solvent and is green and environmentally friendly; the W / O / W multiphase emulsion is constructed so that the utilization rate of hydroxylamine is improved and the reaction of the hydroxylamine is accelerated; and the yield of benzohydroxamic acid is high and the energy consumption is low. The collecting system prepared by the method contains the benzohydroxamic acid, a surfactant and other impurity components; the surfactant can have a foaming effect and can be used for reducing the dosage of a foaming agent when being applied to mineral dressing engineering; and in a floatation process, the cost of medicaments is reduced and the collecting effect is relatively good.

Description

technical field [0001] The invention relates to the field of flotation reagents, more specifically, to a collection system prepared from a W / O / W multiphase emulsion, a preparation method and application thereof. [0002] technical background [0003] Hydroxamic acid (Hydroxamic acid) has a strong chelating ability to metal ions Cu, Cr, Co, Fe, Mn, W, Sn, etc., and is usually used as a floating material for black and white tungsten ore, copper oxide ore and tin ore in mineral engineering. Choose a collector to use. Taking benzohydroxamic acid as an example, it has the advantages of good selectivity and strong collection capacity when applied to rare metal beneficiation. Dai Zilin (Research on the flotation of fine-grained wolframite with benzyl hydroxamic acid[J]. Mining and Metallurgy Engineering, 1995,15(2):20-23.) reported the separation of wolframite and wolframite with benzyl hydroxamic acid stone and calcite. Sun Wei, (Research on the application and mechanism of benz...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B03D1/018B03D101/02B03D101/04B03D103/02
CPCB03D1/018B03D2201/02B03D2201/04B03D2203/02
Inventor 李方旭张发明林日孝
Owner INST OF RESOURCES UTILIZATION & RARE EARTH DEV GUANGDONG ACAD OF SCI
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