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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
However, trioctylmethylammonium sulfate has weak extraction ability and low extraction rate relative to trioctylmethylammonium chloride.
In addition, the existing preparation method of trioctylmethylammonium chloride is complicated, and the organic phase separation is difficult, and the amount of solvent added is high, and trioctylmethylammonium chloride will be dissolved in the solvent, resulting in the synthesis of trioctylmethylammonium chloride. Low yield of octylmethylammonium chloride

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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preparation example Construction

[0017] The invention provides a preparation method of trioctylmethylammonium oxalate.

[0018] The method (1) mixes trioctyl tertiary amine and isooctyl alcohol, puts it in a vertical reactor, then continuously feeds methyl chloride at a rate of 100-300mL / min, and reacts at 100-200°C for 5- 10h, obtain trioctyl methyl ammonium chloride crude product;

[0019] (2) The crude product of trioctylmethyl ammonium chloride is transferred to a falling film liquid film distillation apparatus, and distilled at 120~150°C and 2~8mmHg column conditions to obtain trioctylmethyl ammonium chloride;

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

Embodiment 1

[0033] A method for synthesizing trioctylmethylammonium 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), trioctyl tertiary amine and isooctyl alcohol are mixed, placed in a vertical reactor, and then continuously fed into methyl chloride at a speed of 100~200mL / min, React at 100-150°C for 5-8 hours to obtain the crude product of trioctylmethylammonium chloride;

[0035] Step 2, transfer the crude product of trioctylmethyl ammonium chloride to a falling film liquid film distillation apparatus, and distill at 120~150°C and 2~6mm (Hg column) conditions to obtain trioctylmethyl ammonium chloride Ammonium;

[0036] Step 3. According to the molar ratio of 1: (1-1.5), mix trioctylmethylammonium chloride with wet silver oxide, place in a reaction kettle, stir at 40-60°C for 2-4 hours, and cool After reaching room temperature, the phases were separated to obtain tri...

Embodiment 2

[0044] A method for synthesizing trioctylmethylammonium 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), trioctyl tertiary amine and isooctyl alcohol are mixed, placed in a vertical reactor, and then continuously fed into methyl chloride at a speed of 150~250mL / min, React at 130-180°C for 6-9 hours to obtain the crude product of trioctylmethylammonium chloride;

[0046] Step 2, transfer the crude product of trioctylmethyl ammonium chloride to a falling film liquid film distillation apparatus, and distill at 120~150°C and 3~7mm (Hg column) conditions to obtain trioctylmethyl ammonium chloride Ammonium;

[0047] Step 3. According to the molar ratio of 1: (1.5-2.5), mix trioctylmethylammonium chloride with wet silver oxide, place in a reaction kettle, stir at 50-70°C for 3-5 hours, and cool After reaching room temperature, the phases were separated to obtain tri...

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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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