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Synthesis method of hydroxyoximate

A hydroxamate and synthesis method technology, applied in solid separation, organic chemistry, flotation, etc., can solve the problems of inability to precipitate hydroxamic acid, complicated operation, and increased cost, so as to avoid a large amount of acidic wastewater and improve synthesis yield rate, loss avoidance effect

Inactive Publication Date: 2015-03-25
BLUESTAR LEHIGH ENG INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During the acidification process, a large amount of acidic wastewater will be produced, and at the same time, some hydroxamic acid cannot be precipitated during the acidification process, which will greatly reduce the product yield
The solubility of hydroxamic acid in water is very small. When it is used in flotation industry, it needs to be dissolved by adding caustic alkali or ammonia water. The acidification precipitation and alkaline dissolution before and after this not only cause the loss of part of hydroxamic acid and the generation of a large amount of acidic wastewater, but also make The operation is complicated and the cost is greatly increased

Method used

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  • Synthesis method of hydroxyoximate

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Effect test

Embodiment 1

[0028] Embodiment 1, with reference to attached figure 1 , a kind of synthetic method of hydroxamate, this method uses fatty acid, short-chain alcohol, dodecylsulfonic acid, hydroxylamine hydrochloride and caustic alkali to divide into two steps and synthesize hydroxamate, and its concrete steps are as follows:

[0029] (1) Preparation of fatty acid ester: Add fatty acid, short-chain alcohol and dodecylsulfonic acid into the reactor, the ratio of the three substances is, fatty acid: short-chain alcohol: dodecylsulfonic acid=1: 3: 0.10, stirred and reacted at 75°C for 4 hours; the reactant was distilled under reduced pressure to obtain fatty acid ester, and unreacted alcohol was recovered;

[0030] (2) Preparation of hydroxamate: add hydroxylamine hydrochloride solution in another reactor, add caustic alkali in batches under stirring condition, the ratio of hydroxylamine hydrochloride to caustic alkali is 1:2, after adding caustic Stir and mix for 10 minutes after alkali; add ...

Embodiment 2

[0031] Embodiment 2, a kind of synthetic method of hydroxamate, this method uses fatty acid, short-chain alcohol, dodecylsulfonic acid, hydroxylamine hydrochloride and caustic alkali to synthesize hydroxamate in two steps, and its specific steps are as follows:

[0032] (1) Preparation of fatty acid ester: Add fatty acid, short-chain alcohol and dodecylsulfonic acid into the reactor, the ratio of the three substances is, fatty acid: short-chain alcohol: dodecylsulfonic acid=1: 8: 0.15, stirred and reacted at 100°C for 8 hours; the reactant was distilled under reduced pressure to obtain fatty acid ester, and unreacted alcohol was recovered;

[0033] (2) Preparation of hydroxamate: Add hydroxylamine hydrochloride solution in another reactor, add caustic alkali in batches under stirring condition, the ratio of hydroxylamine hydrochloride to caustic alkali is 1: 2.2, after adding Stir and mix for 20 minutes after the base; add fatty acid ester, the ratio of fatty acid ester to hyd...

Embodiment 3

[0034] Embodiment 3, a kind of synthetic method of hydroxamate, this method uses fatty acid, short-chain alcohol, dodecylsulfonic acid, hydroxylamine hydrochloride and caustic alkali to synthesize hydroxamate in two steps, and its specific steps are as follows:

[0035] (1) Preparation of fatty acid ester: Add fatty acid, short-chain alcohol and dodecylsulfonic acid into the reactor, the ratio of the three substances is, fatty acid: short-chain alcohol: dodecylsulfonic acid=1: 5: 0.12, stirred and reacted at 85°C for 6 hours; the reactant was distilled under reduced pressure to obtain fatty acid ester, and unreacted alcohol was recovered;

[0036] (2) Preparation of hydroxamate: add hydroxylamine hydrochloride solution in another reactor, add caustic alkali in batches under stirring condition, the ratio of hydroxylamine hydrochloride to caustic alkali is 1:2, after adding caustic Stir and mix for 15 minutes after alkali; add fatty acid ester, the ratio of fatty acid ester to h...

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Abstract

The invention relates to a synthesis method of hydroxamate. The hydroxamate is synthesized from fatty acid, short chain alcohol, dodecyl sulfonic acid, hydroxylamine hydrochloride and caustic alkali by two steps; and the synthesis method comprises the following steps of adding fatty acid, short chain alcohol and dodecyl sulfonic acid into a reactor, stirring and reacting at a constant temperature of 75 DEG C-100 DEG C; carrying out reduced pressure distillation on the reactants to obtain fatty acid ester; adding hydroxylamine hydrochloride into another reactor, adding caustic alkali in batches while stirring, and mixing; adding fatty acid ester and reacting for 3-5 hours at 40 DEG C-60 DEG C to obtain a hydroxamate solution; and rapidly cooling the hydroxamate solution to obtain the solid hydroxamate. By the synthesis method, the conversion between acid-alkali environment for the esterification and hydroximation two-step reaction is avoided, the synthesized product needs not to be subjected to processing steps such as acidification, impurity removal and purification and the obtained product can be organically combined with flotation industry. The synthesis method has the advantages that the operation is simple, the yield of the product is high, the generation of a large amount of acidic wastewater is avoided and the cost of chemical agents is effectively decreased.

Description

technical field [0001] The invention relates to a synthesis method of a high-efficiency chelation flotation collector, in particular to a synthesis method of a hydroxamate. Background technique [0002] The structural formula of hydroxamic acid molecule is RC(=O)NHOH, and the oxygen atom and nitrogen atom in the molecule have lone pairs of electrons, which can be combined with Fe 3+ 、Cu 2+ , Zn 2+ 、Ni 2+ Metal ions are combined into stable complexes, and hydroxamic acid has been successfully used in various mineral flotation separation tests. Hydroxamic acid has been used as a flotation collector for nearly 70 years, and has achieved good flotation results. It is widely used in the flotation of other mines. In the beneficiation test of complex polymetallic ore, using hydroxamic acid as a flotation collector has become the key to the success of many beneficiation processes. As a flotation collector for oxidized ore, hydroxamic acid has the advantages of high efficiency ...

Claims

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Application Information

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IPC IPC(8): C07C259/10C07C259/06B03D1/01B03D101/02
Inventor 刘养春徐会会宋文义刘升林刘星强
Owner BLUESTAR LEHIGH ENG INST CO LTD
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