Alkyl thioether-based ethyl hydroxamic acid agent and preparation method and application thereof

A technology of ethyl ethyl hydroxamic acid and alkyl sulfide, which is applied in the field of alkyl sulfide ethyl hydroxamic acid and its preparation, can solve the problem of mineral floating without alkyl sulfide ethyl hydroxamic acid. Selecting collectors, weak collecting ability, etc., to achieve the effect of improving hydrophobic foaming performance, improving flotation recovery rate and enhancing effect

Active Publication Date: 2019-12-03
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These hydroxamic acids with short carbon chain structures generally have good selectivity, but weak collection ability
At present, there is no relevant report on the use of alkyl sulfide-based ethyl hydroxamic acid reagents as mineral flotation collectors

Method used

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  • Alkyl thioether-based ethyl hydroxamic acid agent and preparation method and application thereof
  • Alkyl thioether-based ethyl hydroxamic acid agent and preparation method and application thereof
  • Alkyl thioether-based ethyl hydroxamic acid agent and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Preparation of benzyl sulfide ethyl hydroxamic acid:

[0052] Add 18.93g of 96.15% benzyl thioether acetic acid, 16.16g of 99% methanol and 2.5g of 98% concentrated sulfuric acid into a 150mL three-necked flask, raise the temperature to 75°C for 5 hours, and after cooling to room temperature, add 4.2g of 98.5 % sodium bicarbonate solid, after no bubbles are released, filter, and distill off methanol under reduced pressure to obtain methyl benzyl sulfide acetate. Add 7.76g of 99.5% hydroxylamine hydrochloride into a 150mL three-neck flask, and add 30mL of distilled water to dissolve the hydroxylamine hydrochloride. Weigh 8.33g of 96% sodium hydroxide, dissolve it with 20mL of distilled water, then add the aqueous solution of sodium hydroxide dropwise to the aqueous solution of hydroxylamine hydrochloride in an ice bath, after the dropwise addition, add benzyl sulfide to the mixture Methyl acetic acid was heated to 40°C for 4 hours. After the reaction, it was acidified w...

Embodiment 2

[0064] Preparation of benzyl sulfide ethyl hydroxamic acid:

[0065] Add 9.47g of 96.15% benzyl thioether acetic acid, 8.08g of 99% methanol and 1.3g of 98% concentrated sulfuric acid into a 100mL three-necked flask, raise the temperature to 75°C for 5 hours, and after cooling to room temperature, add 2.1g of 98 .5% sodium bicarbonate solid, after no bubbles are released, filter, and distill under reduced pressure to remove methanol to obtain methyl benzyl sulfide acetate. Add 3.88g of 99.5% hydroxylamine hydrochloride into a 100mL three-necked flask, and add 30mL of distilled water to dissolve the hydroxylamine hydrochloride. Weigh 6.59g of 85.0% potassium hydroxide, dissolve it with 20mL of distilled water, then add the aqueous solution of potassium hydroxide dropwise to the aqueous solution of hydroxylamine hydrochloride under ice-cooling, after the dropwise addition, add benzyl Methyl thioether acetate was heated to 40°C for 4.5 hours. After the reaction, it was acidified...

Embodiment 3

[0067] Preparation of dodecyl sulfide ethyl hydroxamic acid:

[0068] Weigh 18.71g of 97.30% dodecyl sulfide acetic acid, 16.16g of 99% methanol and 2.5g of 98% concentrated sulfuric acid into a 150mL three-neck flask, heat to 75°C for 4.5h, and cool to room temperature , Add 4.2g of 98.5% sodium bicarbonate solid, after no bubbles are released, filter, and distill under reduced pressure to obtain methyl dodecyl sulfide group acetate. Add 7.76g of 99.5% hydroxylamine hydrochloride and 30mL of distilled water into a 150mL three-neck flask, mix 8.33g of 96% sodium hydroxide with 20mL of distilled water, then add the aqueous solution of sodium hydroxide dropwise to the aqueous solution of hydroxylamine hydrochloride in an ice bath After the dropwise addition, add methyl dodecyl sulfide ethyl acetate to the mixture, raise the temperature to 40°C and react for 4 hours, acidify with sulfuric acid after the reaction to obtain the product of dodecyl sulfide ethyl hydroxamic acid 17.20...

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Abstract

The invention discloses an alkyl thioether-based ethyl hydroxamic acid agent and a preparation method and application thereof. An alkyl thioether-based ethyl hydroxamic acid molecule simultaneously has two functional groups including a thioether group and a hydroxamic group, the alkyl thioether-based ethyl hydroxamic acid molecule is esterified by alkyl thioether-based acetic acid and methanol, and then hydroxamination is carried out by hydroxylamine and alkali to obtain the alkyl thioether-based ethyl hydroxamic acid agent. The alkyl thioether-based ethyl hydroxamic acid agent can be used asa collector for mineral flotation, the preparation method is simple, the yield is high, the thioether group and the hydroxamic acid group in the molecule have a synergistic effect, and the collectingperformance of the alkyl thioether-based ethyl hydroxamic acid agent can be effectively improved.

Description

technical field [0001] The invention belongs to the field of beneficiation agents, and in particular relates to a novel alkyl sulfide ethyl hydroxamic acid agent and its preparation method and application. Background technique [0002] Hydroxamic acid compounds are typical chelating agents 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 a stable chelate, which is formed by combining two O atoms in carbonyl and hydroxyl with metal cations five-membered ring structure. With such a special structure, hydroxamic acid compounds have been widely used in the fields of flotation of metal oxide ores, solvent extraction, wastewater treatment, and medicine. [0003] Wang et al. reported the flotation of fine-grained cassiterite by alkylhydroxamic acid and its solution chemical properties (structural formula a, PeipeiWang, Wenqing Qin, Liuyi Ren,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B03D1/012B03D101/02B03D103/02
CPCB03D1/012B03D2201/02B03D2203/02B03D1/008B03D1/01B03D2203/04C07C323/60
Inventor 钟宏孙青王帅
Owner CENT SOUTH UNIV
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