Preparation method of propylene hydroximic acid

A technology of propylene hydroxamic acid and methyl acrylate, applied in the direction of organic chemistry, etc., can solve the problems of few preparation methods of propylene hydroxamic acid, waste of raw materials, low yield, etc., to reduce energy consumption, improve purity, and improve utilization rate effect

Active Publication Date: 2012-07-18
DONGYING BAOMO ENVIRONMENT ENG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there are not many preparation methods of acrylhydroxamic acid. There are reports in the literature that acryl

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Example 1: Control the temperature of the constant temperature water bath at about 20°C, add 86g of methyl acrylate and 300g of distilled water to a 1000mL three-necked round-bottomed flask equipped with a condenser, a thermometer, and an agitator in sequence, and start the agitator to make it rotate at 400r Stir at a constant speed of about 20 minutes per minute to disperse methyl acrylate evenly in the aqueous solution, then add 83.4 g of hydroxylammonium hydrochloride (the molar ratio of hydroxylamine hydrochloride to methyl acrylate in this example is 1.2:1), and continue stirring to dissolve it Completely, when the temperature of the reaction system is stabilized at about 20°C, slowly add 150g of ionic membrane liquid alkali with a mass percentage concentration of 32% to the reaction system slowly with a dropping funnel, and keep the reaction system in the whole dropping process. The temperature shall not exceed 25°C, and the dropping time shall be controlled at abo...

Embodiment 2

[0019] Example 2: Control the temperature of the constant temperature water bath at 20°C, add 86g of methyl acrylate and 300g of distilled water to a 1000mL three-necked round-bottomed flask equipped with a condenser, a thermometer, and an agitator in sequence, and start the agitator to make it rotate at 400r / Stir at a constant speed for about 20 minutes, so that the methyl acrylate is uniformly dispersed in the aqueous solution, and then add 104 g of hydroxylammonium hydrochloride (the molar ratio of hydroxylamine hydrochloride to methyl acrylate in this example is 1.5:1), and continue to stir to dissolve it completely. When the temperature of the reaction system is stabilized at about 20°C, slowly add 187.5g of ionic membrane liquid caustic soda with a mass percentage concentration of 32% to the reaction system slowly with a dropping funnel, and keep the temperature of the reaction system during the whole dropping process. If the temperature exceeds 25°C, the dropping time s...

Embodiment 3

[0020] Example 3: Control the temperature of the constant temperature water bath at 20°C, add 86g of methyl acrylate and 300g of distilled water to a 1000mL three-necked round-bottomed flask equipped with a condenser, a thermometer, and an agitator, and start the agitator to make it rotate at 400r / Stir at a constant speed for about 30 minutes, so that the methyl acrylate is uniformly dispersed in the aqueous solution, and then add 104 g of hydroxylammonium hydrochloride (the molar ratio of hydroxylamine hydrochloride to methyl acrylate in this example is 1.5:1), and continue to stir to dissolve it completely. When the temperature of the reaction system is stabilized at about 20°C, slowly add 187.5g of ionic membrane liquid alkali with a mass percentage concentration of 32% to the reaction system slowly with a dropping funnel, and keep the temperature of the reaction system during the entire dropping process The temperature shall not exceed 25°C, and the dropping time shall be ...

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PUM

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Abstract

The invention discloses a preparation method of propylene hydroximic acid, wherein the temperature of the reaction is controlled by a thermostatic waterbath, a certain amount of methyl acrylate and pure water are added into a reaction vessel, the quality of the pure water is 3-4 times that of the methyl acrylate, the mixture is quickly stirred to enable the methyl acrylate to be uniformly dispersed, then hydroxylamine hydrochloride with the weight being 1.2-1.5 times that of the methyl acrylate is added into a three-opening round bottomed flask, the mixture is constantly stirred to dissolve the mixture, when the system temperature is kept stable at 20 DEG C, ionic membrane caustic soda liquid with the weight being equal to that of hydroxylamine hydrochloride,is added into the mixture by using a dripping method so as to enable the reaction to perform smoothly, meanwhile, the temperature of a reaction system is kept to be not more than 25 DEG C, low-pressure distillation is performed after the reaction to remove dissociated unreacted hydroxylamine and a by-product methyl alcohol, cooling and suction filtration are performed to remove the precipitated salinity, and the final product is a water solution of propylene hydroximic acid. The reaction is controlled to be carried out slowly by adopting a method of dripping ionic membrane caustic soda liquid, so that the dissociated hydroxylamine is prevented from being decomposed and volatilized due to rapid temperature increment, and the utilization ratio of raw materials is further improved.

Description

technical field [0001] The invention relates to a preparation method of an organic chelating agent propylene hydroxamic acid. The chelating agent belongs to hydroxamic acid compounds and is the most promising collector for oxidized ore flotation in recent years. Background technique [0002] Propylene hydroxamic acid is an organic chelating agent, which belongs to hydroxamic acid compounds, and can be combined with Cu + ,Co 2+ , Ni 2+ , Fe 3+ , Zn 2+ The plasma forms stable metal chelates. Therefore, the hydroxime group of hydroxamic acid cooperates with the metal ions on the mineral surface to form a stable chelate, which is adsorbed on the mineral surface, thus acting as a collector. Since the 1960s, mineral processing workers have done a lot of research on the use of hydroxamic acid and its salts as mineral processing flotation agents, and have also achieved good results. In terms of application, we have done a long period of work and achieved good results. In addi...

Claims

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Application Information

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IPC IPC(8): C07C259/06
Inventor 张洪松李岳军刘皓徐坤王曰鹏曹卫广
Owner DONGYING BAOMO ENVIRONMENT ENG CO LTD
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