2-ethyl-2-hexenyl hydroximic acid as well as combined collector thereof and application of 2-ethyl-2-hexenyl hydroximic acid and combined collector

A technology of hexenyl hydroxamic acid and combined collectors, applied in solid separation, organic chemistry, flotation, etc., can solve the problems of limited popularization and application, weak collection capacity, etc.

Active Publication Date: 2014-09-03
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN103301953A discloses a collector of 6-aryl amidohexyl hydroxamic acid, which overcomes the problem of amide breakage caused by traditional hydroximation reactions under heating and strong alkali conditions, and prepares Synthetic amidohydroxamic acid collector, which has strong collection ability for minerals such as tungsten ore, rare earth ore, tin ore or bauxite
[0004] At present, the hydroxamic acids for industrial application are mainly benzohydroxamic acid, salicylic hydroxamic acid and C 5～9 Alkyl hydroxamic acid, etc., have good selectivity. Although the collection capacity is constantly improving, the collection capacity is always weak, and the preparation process needs to be acidified first and then saponified, which limits their popularization and application.

Method used

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  • 2-ethyl-2-hexenyl hydroximic acid as well as combined collector thereof and application of 2-ethyl-2-hexenyl hydroximic acid and combined collector
  • 2-ethyl-2-hexenyl hydroximic acid as well as combined collector thereof and application of 2-ethyl-2-hexenyl hydroximic acid and combined collector
  • 2-ethyl-2-hexenyl hydroximic acid as well as combined collector thereof and application of 2-ethyl-2-hexenyl hydroximic acid and combined collector

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Embodiment 1 Preparation of alkenyl hydroxamic acid combination collector 1 and 2-ethyl-2-hexenyl hydroxamic acid

[0041] Add 7.1 parts of 2-ethyl-2-hexenoic acid, 9.6 parts of methanol, and 1.0 parts of concentrated sulfuric acid into a reactor with a stirring device, and react at 80°C for 6 hours to obtain 2-ethyl-2-hexene According to the method of national standard GB / T12717-2007, the esterification rate is 94.32%. Dissolve 3.83 parts of hydroxylamine hydrochloride and 4.4 parts of sodium hydroxide in 50.5 parts of methanol, add 13.8 parts of the 2-ethyl-2-hexenoic acid methyl ester product prepared by the previous step reaction, stir and control the temperature at 50oC, and react 3 hours, distilled to obtain the alkenyl hydroxamic acid combined collector, wherein the mass percentage of 2-ethyl-2-hexenyl hydroxamic acid is 71.2%. The 2-ethyl-2-hexenyl hydroxamic acid obtained by the separation and purification of the combined collector through silica gel column ch...

Embodiment 2

[0042] The preparation of embodiment 2 alkenyl hydroxamic acid combined collector 2

[0043] Add 7.1 parts of 2-ethyl-2-hexenoic acid, 9.6 parts of methanol, and 1.0 parts of dodecylbenzenesulfonic acid into a reactor with a stirring device, and react at 80°C for 6 hours to obtain 2-ethyl -2-hexenyl methyl ester product, the esterification rate is 92.58%. Dissolve 3.83 parts of hydroxylamine hydrochloride and 4.4 parts of sodium hydroxide in 45.8 parts of ethanol, add 13.8 parts of 2-ethyl-2-hexenoic acid methyl ester product prepared by the previous step reaction, stir and control the temperature at 50oC, reaction 3 Hours, distilled to obtain alkenyl hydroxamic acid combined collector, wherein the mass percentage of 2-ethyl-2-hexenyl hydroxamic acid is 73.5%.

Embodiment 3

[0044] The preparation of embodiment 3 alkenyl hydroxamic acid combined collector 3

[0045] Add 7.1 parts of 2-ethyl-2-hexenoic acid, 8 parts of methanol, and 1.0 parts of concentrated sulfuric acid into a reactor with a stirring device, and react at 80°C for 6 hours to obtain 2-ethyl-2-hexene Methyl ester product, the esterification rate is 90.65%. Dissolve 3.83 parts of hydroxylamine hydrochloride and 4.4 parts of sodium hydroxide in 48 parts of ethanol, add 13.8 parts of the 2-ethyl-2-hexenoic acid methyl ester product prepared in the previous step reaction, stir and control the temperature at 50oC, and react for 3.5 hours , Distilled to obtain the alkenyl hydroxamic acid combined collector, wherein the mass percentage of 2-ethyl-2-hexenyl hydroxamic acid is 71.7%.

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Abstract

The invention discloses 2-ethyl-2-hexenyl hydroximic acid as well as a combined collector thereof and an application of 2-ethyl-2-hexenyl hydroximic acid and the combined collector. The combined collector of 2-ethyl-2-hexenyl hydroximic acid consists of 2-ethyl-2-hexenyl hydroximic acid, 2-ethyl-2-methyl hexenoate and 2-ethyl-2-hexenoic acid, wherein the mass percentage of 2-ethyl-2-hexenyl hydroximic acid is not less than 60%. The combined collector is liquid at normal temperature, and has the characteristics of low freezing point, good dispersing performance in ore pulp, strong collector performance and the like. Hexenyl hydroximic acid and the combined collector of hexenyl hydroximic acid are obtained by performing esterification on 2-ethyl-2-hexenoic acid and methanol and then performing hydroxyl oximation with hydroxylamine, are mild in preparation condition, do not need to be acidified, and can not generate wastewater.

Description

technical field [0001] The invention belongs to the field of flotation agent and its preparation, and mainly relates to a novel alkenyl hydroxamic acid and its combined collector and their application. Background technique [0002] Hydroxamic acid is a typical chelating agent with high selectivity for metal ions. Oxygen and nitrogen containing lone pairs of electrons and close to each other in its molecular structure enable it to chelate with metal ions to form stable chelates. The practice at home and abroad has proved that hydroxamic acid has the advantages of strong collection ability, good selectivity, low toxicity, etc., and it is used in the flotation of ores such as tungsten ore, rare earth ore, tin ore and ilmenite, and has achieved ideal results. Sorting effect, it is a kind of oxide ore collector with development prospect. [0003] In my country, most sulfide deposits have oxidation zones on the upper part, and some deposits are oxidized to become medium-sized ox...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C259/06B03D1/018B03D1/01B03D101/02
Inventor 钟宏王帅唐清曹占芳刘广义许海峰黄志强
Owner CENT SOUTH UNIV
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