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Purifying method of propoxur

A purification method, propoxur technology, applied in chemical instruments and methods, organic chemistry, preparation of organic compounds, etc., can solve problems such as difficult to achieve purification effect, unpleasant special smell, etc., achieve white color, avoid decomposition, and simple operation Effect

Active Publication Date: 2018-02-09
HUNAN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although propoxur has a melting point of 91°C, it is theoretically suitable for this purification technology, but actual research has found that it is difficult to achieve the purification effect by using this technology, and the product still contains 0.3% 1,2-diisopropoxybenzene and has an unpleasant smell. special smell

Method used

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  • Purifying method of propoxur

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 214.4g propoxur (97.5%) and 8.5g petroleum ether into a 500mL three-neck flask with cooling tube, thermometer and stirring, stir and heat to 95°C until completely melted, and control the temperature of the system to slowly drop to 85°C (cooling rate 0.1°C / min) and maintained for 1 h, standing still for crystallization. A small amount of yellow liquid appeared in the kettle floating above the white solid, which was removed from the system. The white solid was heated and melted and sliced ​​to obtain 205.2 g of white, odorless propoxur (liquid chromatography, external standard) with a content of 99.3% and a yield of 97.5%. The mass of the yellow liquid removed from the system was 15.8 g, which was analyzed as a 32.5% solution of propoxur in petroleum ether, in which 1,2-diisopropoxybenzene and 1-isopropoxy-2-methoxybenzene were also dissolved. 6g of petroleum ether can be recovered by simple distillation, and the remaining oily residue after distillation can be inci...

Embodiment 2

[0030] Add 214.4g propoxur (97.5%) and 6g petroleum ether into a 500mL three-neck flask with cooling tube, thermometer and stirring, stir and heat to 100°C until completely melted, and control the temperature of the system to slowly drop to 90°C (cooling rate 0.1°C / min ) and maintain 1h, static crystallization. A small amount of yellow liquid appeared in the kettle floating above the white solid, which was removed from the system. The white solid was heated and melted and sliced ​​to obtain 206.5 g of white, odorless propoxur (liquid chromatography, external standard) with a content of 99.1% and a yield of 97.9%. The mass of the yellow liquid removed from the system was 12.0 g, which was analyzed to be a 36.2% solution of propoxur in petroleum ether, in which 1,2-diisopropoxybenzene and 1-isopropoxy-2-methoxybenzene were also dissolved. 3g of petroleum ether can be recovered by simple distillation, and the remaining oily residue after distillation can be incinerated.

Embodiment 3

[0032] Add 214.4g of propoxur (97.5%) and 4.2g of petroleum ether into a 500mL three-neck flask with a cooling tube, thermometer, and stirring, stir and heat to 100°C until completely melted, and control the temperature of the system to slowly drop to 85°C (cooling rate 0.1°C / min) and maintained for 2h, standing still for crystallization. A small amount of yellow liquid appeared in the kettle floating above the white solid, which was removed from the system. The white solid was heated and melted and sliced ​​to obtain 208.2 g of 98.8% white, odorless propoxur (liquid chromatography, external standard), with a yield of 98.4%. The mass of the yellow liquid removed from the system was 8.4 g, which was analyzed as a 39.5% solution of propoxur in petroleum ether, in which 1,2-diisopropoxybenzene and 1-isopropoxy-2-methoxybenzene were also dissolved. 2g of petroleum ether can be recovered by simple distillation, and the remaining oily residue after distillation can be incinerated....

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Abstract

The invention discloses a purifying method of propoxur. The purifying method of propoxur comprises following steps: 1, a propoxur solid mixture containing impurities is mixed with an inert solvent, and an obtained mixture is heated until the propoxur solid mixture is melted completely so as to obtain a mixed system; and 2, the mixed system is cooled slowly to the melting-crystal temperature of propoxur, and is allowed to stand until the mixed system is converted into crystal and liquid floating on the crystal completely, and the liquid floating on the crystal is removed so as to obtain purified propoxur. The purifying method is capable of removing impurities 1,2-diisopropoxybenzene and 1-isopropoxy-2-metoxybenzene, operation is simple, and equipment requirement is low.

Description

technical field [0001] The invention belongs to the technical field of organic matter purification, and in particular relates to a method for purifying propoxur. Background technique [0002] Proxacarb (2-isopropoxyphenyl methyl carbamate) is a non-systemic insecticide with contact killing, stomach poisoning and fumigation effects, and is effective against ectoparasites, household hygiene pests (mosquitoes, flies, cockroaches, etc.) and The storage pests are knocked down quickly and have a long lasting effect. Its structural formula: [0003] [0004] Promoxur itself is odorless, but there are about 1% of 1,2-diisopropoxybenzene and 0.1% of 1-isopropoxy-2-methoxybenzene and other aromatic ethers in the original drug of propoxur ( Both come from the main raw material 2-isopropoxyphenol) has an unpleasant special smell, which affects the indoor use of propoxur as a high-grade sanitary insecticide, so it is necessary to develop a simple and effective separation technology ...

Claims

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Application Information

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IPC IPC(8): C07C269/08C07C271/44
CPCC07C269/08C07C271/44
Inventor 王宇蒋彪陈明王胜得杨彬刘伟
Owner HUNAN CHEM RES INST
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