Preparation method of trioctyl methyl ammonium oxalate

A technology of trioctylmethylammonium oxalate and trioctylmethylammonium chloride, which is applied in the field of preparation of trioctylmethylammonium oxalate, can solve the problems of weak extraction ability, high solvent content, polluted wastewater, etc. Achieve the effect of purity, green environmental protection, strong extraction ability, and avoid pollution

Pending Publication Date: 2021-04-06
JIANGXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this extractant also has a drawback, when the anionic group is Cl - It is exchanged into the raffinate, which contains a large amount of chloride ions, which makes the concentration of chloride ions in the extractant higher, forming difficult-to-treat and polluting wastewater
In the same way, when trioctylmethylammonium bromide and trioctylmethylammonium nitrate are used as extractants, polluted Br - and NO 3 - ions, resulting in difficult-to-treat, highly polluting wastewater
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Method used

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  • Preparation method of trioctyl methyl ammonium oxalate
  • Preparation method of trioctyl methyl ammonium oxalate
  • Preparation method of trioctyl methyl ammonium oxalate

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Example Embodiment

[0017] The invention provides a preparation method of trioctyl methyl ammonium oxalate.

[0018] In the method (1), trioctyl tertiary amine and isooctyl alcohol are mixed, placed in a vertical reactor, and then continuously fed with methyl chloride at a speed of 100-300 mL / min, and reacted at 100-200 ° C for 5- 10h, obtain trioctyl methyl ammonium chloride crude product;

[0019] (2) the trioctyl methyl ammonium chloride crude product is transferred to the falling film type liquid film distillation apparatus, and is distilled under 120~150 ℃ and 2~8mmHg column conditions, obtains trioctyl methyl ammonium chloride;

[0020] (3) Mix trioctylmethylammonium chloride with wet silver oxide, place in a reaction kettle, stir at 40-80°C for 2-6h, cool to room temperature and separate phases to obtain trioctylmethyl Ammonium hydroxide;

[0021] (4) Mix trioctylmethylammonium hydroxide and oxalic acid, place in a reaction kettle, stir at 30~60°C for 2~6h, cool to room temperature and s...

Example Embodiment

[0032] Example 1

[0033] A kind of synthetic method of trioctyl methyl ammonium oxalate. The synthetic method of trioctyl methyl ammonium oxalate described in the present embodiment is:

[0034] Step 1. According to the volume ratio of 1:(1.5~2), the trioctyl tertiary amine and isooctyl alcohol are mixed, placed in the vertical reactor, and then chloromethane is continuously fed at the speed of 100~200mL / min, Under the condition of 100~150℃, react for 5~8h to obtain the crude product of trioctylmethylammonium chloride;

[0035] Step 2. Transfer the crude product of trioctyl methyl ammonium chloride to a falling film liquid film distillation apparatus, and distill at 120-150° C. and 2-6 mm (Hg column) to obtain trioctyl methyl chloride Ammonium;

[0036] Step 3. According to the molar ratio of 1:(1~1.5), mix trioctylmethylammonium chloride and wet silver oxide, place in the reaction kettle, stir at 40~60℃ for 2~4h, cool down Phase separation after reaching room temperature...

Example Embodiment

[0043] Example 2

[0044] A kind of synthetic method of trioctyl methyl ammonium oxalate. The synthetic method of trioctyl methyl ammonium oxalate described in the present embodiment is:

[0045] Step 1. According to the volume ratio of 1:(2~2.5), the trioctyl tertiary amine and isooctanol are mixed, placed in the vertical reactor, and then the methyl chloride is continuously fed at the speed of 150~250mL / min, Under the condition of 130~180℃, react for 6~9h to obtain the crude product of trioctylmethylammonium chloride;

[0046] Step 2. Transfer the crude product of trioctyl methyl ammonium chloride to a falling film liquid film distillation apparatus, and distill under the conditions of 120-150° C. and 3-7 mm (Hg column) to obtain trioctyl methyl chloride Ammonium;

[0047] Step 3. According to the molar ratio of 1:(1.5~2.5), mix trioctylmethyl ammonium chloride and wet silver oxide, place in the reaction kettle, stir at 50~70℃ for 3~5h, cool down Phase separation after rea...

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Abstract

The invention provides a preparation method of trioctyl methyl ammonium oxalate, and belongs to the technical field of extraction agent synthesis. The method comprises the following steps: firstly, mixing trioctyl tertiary amine with isooctyl alcohol, putting the mixture into a vertical reactor, continuously introducing chloromethane, conducting reacting at 100-200 DEG C for 5-10 hours, then transferring the mixture into a falling film type liquid film distiller, and conducting distilling at 120-150 DEG C and under the condition of 2-8mm (Hg column) to obtain trioctyl methyl ammonium chloride; mixing the trioctyl methyl ammonium chloride with wet silver oxide, and conducting reacting in a reaction kettle to obtain trioctyl methyl ammonium hydroxide; and mixing the trioctyl methyl ammonium hydroxide with an oxalic acid solution, conducting reacting in a reaction kettle to obtain a trioctyl methyl ammonium oxalate crude product, conducting washing with deionized water, and carrying out vacuum drying to obtain the trioctyl methyl ammonium oxalate product. The trioctyl methyl ammonium oxalate synthesized by the method has the characteristics of strong extraction capability, high yield and environmental protection.

Description

technical field [0001] The invention relates to the technical field of extraction agent synthesis, in particular to a preparation method of trioctylmethylammonium oxalate. Background technique [0002] Quaternary ammonium salt is a good extractant, which mainly extracts metal ions in the form of anions. Commonly used quaternary ammonium salts are mainly trioctylmethylammonium chloride, followed by trioctylmethylammonium sulfate, trioctylmethylammonium bromide and trioctylmethylammonium nitrate. The quaternary ammonium salt extractant is usually a mixture mainly composed of octyl, and its molecular formula is R 3 NCH 3 Cl(R=C 8 -C 10 ), its molecular structure determines that it has three distinct characteristics: the molecule contains three long carbon chain alkyl groups, which make it have good oil solubility; the molecule contains a Cl that can be exchanged - , can be exchanged with other metal anions; unlike other amine extractants, quaternary ammonium salt extractan...

Claims

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Application Information

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IPC IPC(8): C07C209/68C07C211/63C07C51/41C07C55/07
CPCC07C209/68C07C51/412C07C211/63C07C55/07Y02P10/20
Inventor 刘子帅罗仙平汪金良周贺鹏
Owner JIANGXI UNIV OF SCI & TECH
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