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6-aliphatic hydrocarbon amido hexyl hydroximic acid collecting agent and preparation and application methods thereof

A technology of base hexyl hydroxamic acid and base hexyl hydroxamic acid salt, which is applied to 6-aliphatic hydrocarbon amido hexyl hydroxamic acid collector and its preparation and application fields, can solve the problem of low product yield, amide bond cleavage, Acyl chloride is highly toxic, and the flotation recovery rate is improved, the chelation capacity is strong, and the flotation separation effect is high.

Active Publication Date: 2013-09-18
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The shortcoming of this method is: the toxicity of acyl chloride is big, easily hydrolyzes, hydroximation reaction needs to react under the condition of heating and strong alkali, easily causes the breakage of amide bond in the molecule, and product yield is lower

Method used

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  • 6-aliphatic hydrocarbon amido hexyl hydroximic acid collecting agent and preparation and application methods thereof
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  • 6-aliphatic hydrocarbon amido hexyl hydroximic acid collecting agent and preparation and application methods thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0044] Embodiment 1: the preparation of 6-nordecyl amidohexyl hydroxamic acid

[0045] Add 11.32 parts of caprolactam with a purity of 99% and 6.95 parts of hydroxylamine hydrochloride with a purity of 99% into the reactor, add 34.64 parts of toluene as a solvent, heat to 105°C under stirring, and react for 3 hours, distill out the solvent for recovery; then Add 17.26 parts of n-decanoic acid into the above reactor, heat to 120° C. under stirring, and react for 1 to 4 hours to obtain the desired 6-n-decylamidohexyl hydroxamic acid product. Analysis showed that the purity of 6-n-decylamidohexyl hydroxamic acid was 90.3%, and the yield was 92.4%. Product Mr: 300.24, detected by mass spectrometry MS: 286.15 [M-15] (see figure 1 ), which is the peak of demethylation. NMR analysis and infrared spectrum analysis spectra are shown in Figure 5 with Figure 8 , see Table 1 and Table 2 for the data.

Embodiment 2

[0046] Embodiment 2: the preparation of 6-n-octylaminohexyl hydroxamic acid

[0047] 17.26 parts of n-decanoic acid in Example 1 were changed to 14.42 parts of n-octanoic acid, and other conditions were unchanged, the purity of the 6-n-octylamidohexyl hydroxamic acid obtained was 91.4%, and the yield was 93.2%. Product Mr: 272.21, detected by mass spectrometry MS: 258.10 [M-15] (see figure 2 ), is the peak of methyl removal. NMR analysis and infrared spectrum analysis spectra are shown in Image 6 with Figure 9 , see Table 1 and Table 2 for the data.

Embodiment 3

[0048] Embodiment 3: Preparation of 6-isooctylamidohexyl hydroxamic acid

[0049] 17.26 parts of n-decanoic acid in Example 1 were changed to 14.42 parts of isooctanoic acid, and other conditions were unchanged, the purity of the obtained 6-isooctylamidohexyl hydroxamic acid was 89.4%, and the yield was 91.2%. Product Mr: 272.21, detected by mass spectrometry MS: 244.15 [M-29] (see image 3 ), is the peak of dropping the branched ethyl group; 258.05[M-15] is the peak of dropping the methyl group. NMR analysis spectrum see Figure 7 , see Table 2 for the data.

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Abstract

A structural formula of a 6-aliphatic hydrocarbon amido hexyl hydroximic acid collecting agent is represented by a formula (I), wherein R represents C2-C18 aliphatic hydrocarbon group. The preparation method comprises the steps as follows: caprolactam and hydroxylamine hydrochloride or hydroxylamine sulphate are taken as raw materials, methylbenzene is taken as a solvent, the reaction temperature ranges from 80 DEG C to 110 DEG C, the reaction lasts for 1-4 hours, and 6-amino hexyl hydroximic acid is generated; 6-amino hexyl hydroximic acid reacts with C2-C18 fat carboxylic acid at the reaction temperature ranging from 100 DEG C to 160 DEG C for 1-4 hours to generate 6-aliphatic hydrocarbon amido hexyl hydroximic acid, and the product yield can be higher than 91%; and 6-aliphatic hydrocarbon amido hexyl hydroximic acid used in flotation of scheelite, wolframite, tombarthite ore, tin ore, bauxite, titanic iron ore or fluorite ore is taken as the collecting agent, so that the flotation recovery rate can be increased by 3%-10%.

Description

technical field [0001] The present invention relates to 6-aliphatic amidohexyl hydroxamic acid and its use as a collector in the flotation of scheelite, wolframite, rare earth ore, tin ore, bauxite, ilmenite or fluorite ore Methods and Preparations. Background technique [0002] Hydroxamic acid and its salts are known flotation collectors for froth flotation of oxide minerals, often used in the flotation of metals or minerals, such as fluorspar, wolframite, wolframite, cassiterite, muscovite , phosphatite, hematite, pyrolusite, rhodonite, chrysocolla, malachite, barite, calcite and rare earths. Hydroxamic acids are generally more potent and selective than conventional fatty acids, aliphatic amines, petroleum sulfonates, and alkyl sulfates. [0003] At present, the hydroxamic acid collectors used in mineral flotation mainly include aliphatic hydroxamic acid collectors and benzyl hydroxamic acid collectors. Patent CN101816980A discloses a C 5～9 Alkyl hydroxamic acid (see s...

Claims

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Application Information

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IPC IPC(8): B03D1/016B03D101/02
Inventor 钟宏邓兰青王帅黄志强刘广义曹占芳
Owner CENT SOUTH UNIV
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