CN103030665A - Water-washing purification method of chlorpyrifos - Google Patents

Abstract

The invention discloses a water-washing purification method of chlorpyrifos, comprising the following steps of: adding lauryl sodium sulfate into an oil-water system obtained by condensing through a water-phase method to separate water; firstly washing a separated oil phase by water with a suitable temperature and then carrying out acid washing by using an acid with a suitable temperature; and finally, dehydrating separated crude oil and drying to obtain a chlorpyrifos raw medicine finished product with the content of being more than 98%. According to the water-washing purification method of chlorpyrifos disclosed by the invention, a traditional separation process is improved and optimized, so that a complicated re-crystallization step is not operated, and demulsification and acid washing steps are increased; and the water-washing purification method is simple and reliable and is convenient to operate, and the product yield and purity can be improved to be more than 98%.

Description

The washing method of purification of a kind of Chlorpyrifos 94

Technical field

The present invention relates to chemical purification field, exactly is the washing method of purification of a kind of Chlorpyrifos 94.

Background technology

Chlorpyrifos 94, chemical name O, O-diethyl-O-(3,5,6-trichloro-2-pyridyl) thiophosphatephosphorothioate, its molecular formula is C ₉H ₁₁Cl ₃NO ₃PS.Chlorpyrifos 94 as the organophosphorus desinsection kill to expire that agent has efficiently, wide spectrum and hypotoxicity, be the contour malicious organic phosphorous insecticide first-selection kind of alternative acephatemet, thiophos that the current pesticide structure of China is adjusted.Its mechanism of action is acetylcholine esterase inhibition, have tag, stomach toxicity and stifling three kinds of modes of action, can effectively prevent eliminating aphis, snout moth's larva, mythimna separata, tortrix moth, scale insect, leafhopper and do harm to the over one hundred kind of insect such as mite and mite class.The synthetic method of Chlorpyrifos 94 is mainly Double solvent method and water method according to the solvent difference of reacting.It is reaction system that Double solvent method adopts water and organic solvent, and wherein organic solvent is volatile, toxicity is high, operational hazards, loss are many, is unfavorable for environment protection and safety in production.Common water method is that 3,5,6-trichloropyridine-2-sodium alkoxide is added to the water, and adds catalyzer, O, and O-o,o-diethylthiophosphoryl chloride and PH conditioning agent, decrease temperature crystalline directly obtain the former powder of Chlorpyrifos 94.Recrystallization complex operation in this method is awkward, and yield is not ideal enough 92% ~ 95%.

Technical problem to be solved by this invention provides refining separation and the method for purification that a kind of water legal system gets Chlorpyrifos 94, and operation is simple and reliable, and cost is lower, and yield and purity are high.

Summary of the invention

The object of the present invention is to provide the washing method of purification of a kind of Chlorpyrifos 94, it is improved on traditional separating technology and is optimized the synthetic Chlorpyrifos 94 of water method, thus the high purity of obtaining, high yield the former medicine finished product of Chlorpyrifos 94.

Above-mentioned purpose realizes by following scheme:

The washing method of purification of a kind of Chlorpyrifos 94 is characterized in that: may further comprise the steps:

(1) breakdown of emulsion divides water: add sodium lauryl sulphate in the condensation of water method obtains the profit system of Chlorpyrifos 94, content is controlled at 250 ~ 300ppm, at the 45-50 ℃ of lower 0.8-1.2h that stirs, leaves standstill minute water behind the 1.8-2.2h, is discharged to washing kettle;

(2) washing: add the boiling water of 3-4 times of volume in the washing kettle, be heated to and finish after stirring washing 0.8-1.2h under the 80-85 ℃ of condition, minute water discharges water automotive gasoline bright stock after washing to the pickling still;

(3) pickling: add 2-3 times of volume 15-20% aqueous hydrochloric acid in the pickling still, be heated to 65-75 ℃, finish behind the stirring washing 0.8-1.2h, a minute water blowing is transferred to the alkali cleaning still;

(4), alkali cleaning: in the alkali cleaning still, add 2-3 times of volume 15-20% aqueous sodium hydroxide solution, be heated to 45-55 ℃, finish minute water blowing behind the stirring washing 0.8-1.2h;

(4) drying: the former medicine finished product of Chlorpyrifos 94 that the former oil drying after step (3) the gained alkali cleaning can be obtained high-content.Beneficial effect of the present invention is: the present invention improves traditional separating technology and optimizes, and has saved the re-crystallization step of complex operation, increases breakdown of emulsion and acid pickling step, and is simple and reliable, convenient operation, and product yield and purity all can be brought up to more than 98%.

Embodiment

In the enamel glass reactor of 3000L, add 1100Kg water and 220Kg 3,5,6-trichloropyridine-2-sodium alkoxide is after stirring, add successively 5Kg Trimethylamine 99 30% aqueous solution, 0.5Kg4-Dimethylamino pyridine and 207Kg O, the O-o,o-diethylthiophosphoryl chloride drips 10% sodium hydroxide solution adjusting PH=9 ~ 10, is warming up to 60 ℃ of reaction 1.5h and finishes, reaction solution is changed in minute flow container, obtain the profit system of Chlorpyrifos 94;

The washing method of purification of a kind of Chlorpyrifos 94 may further comprise the steps:

(1) breakdown of emulsion divides water: add sodium lauryl sulphate in the condensation of above-mentioned water method obtains the profit system of Chlorpyrifos 94, content is controlled at 300ppm, at 50 ℃ of lower 0.8-1.2h that stir, leaves standstill minute water behind the 1.8-2.2h, is discharged to washing kettle;

(2) washing: add the boiling water of 4 times of volumes in the washing kettle, be heated to and finish after stirring washing 0.8-1.2h under 85 ℃ of conditions, minute water discharges water automotive gasoline bright stock after washing to the pickling still;

(3) pickling: add 3 times of volume 15% aqueous hydrochloric acids in the pickling still, be heated to 75 ℃, finish behind the stirring washing 0.8-1.2h, a minute water blowing is transferred to the alkali cleaning still;

(4), alkali cleaning: in the alkali cleaning still, add 2 times of volume 15% aqueous sodium hydroxide solutions, be heated to 55 ℃, finish minute water blowing behind the stirring washing 0.8-1.2h;

(4) drying: the former oil drying after step (3) the gained alkali cleaning can be obtained the former medicine finished product of Chlorpyrifos 94 of high-content, yield 98.2%, content 98.3%(liquid phase chromatography).

Claims (1)

1. the washing method of purification of a Chlorpyrifos 94 is characterized in that: may further comprise the steps:

(1) breakdown of emulsion divides water: add sodium lauryl sulphate in the condensation of water method obtains the profit system of Chlorpyrifos 94, content is controlled at 250 ~ 300ppm, at the 45-50 ℃ of lower 0.8-1.2h that stirs, leaves standstill minute water behind the 1.8-2.2h, is discharged to washing kettle;

(2) washing: add the boiling water of 3-4 times of volume in the washing kettle, be heated to and finish after stirring washing 0.8-1.2h under the 80-85 ℃ of condition, minute water discharges water automotive gasoline bright stock after washing to the pickling still;

(3) pickling: add 2-3 times of volume 15-20% aqueous hydrochloric acid in the pickling still, be heated to 65-75 ℃, finish behind the stirring washing 0.8-1.2h, a minute water blowing is transferred to the alkali cleaning still;

(4), alkali cleaning: in the alkali cleaning still, add 2-3 times of volume 15-20% aqueous sodium hydroxide solution, be heated to 45-55 ℃, finish minute water blowing behind the stirring washing 0.8-1.2h;

(4) drying: the former medicine finished product of Chlorpyrifos 94 that the former oil drying after step (3) the gained alkali cleaning can be obtained high-content.