CN101696021A - Method for separating ammonium chloride and methanol from mother liquor subjected to alcohol precipitation and separation of glycine - Google Patents

Abstract

The invention relates to a method for separating ammonium chloride and methanol from mother liquor subjected to alcohol precipitation and separation of glycine, which mainly provides a technical scheme for quickly extracting methanol and separating ammonium chloride. The method is characterized in that methanol and ammonium chloride mother liquor (aqueous solution) subjected to the alcohol precipitation and separation of glycine is filled into a distillation tower to distill and separate the methanol and the ammonium chloride, wherein the methanol can be recovered and recycled; an obtained ammonium chloride solution is steamed to dewater and heated up to 115 DEG C, and then the ammonium chloride is obtained through evaporating, filtering and dewatering.

Description

The partition method that glycine alcohol analyses, separate ammonium chloride and methyl alcohol in the mother liquor of back

Technical field

The invention discloses a kind of separation method of producing behind the glycine ammonium chloride and methyl alcohol in the surplus solution.

Background technology

The technical matters of traditional mode of production glycine after extracting glycine, contains a large amount of methyl alcohol and ammonium chloride in the mother liquor, can reuse behind the methyl alcohol distillation extraction, but the extraction of the ammonium chloride in the remaining liquid by solar evaporation moisture wherein, is the ammonium chloride spontaneous nucleation often.This method crystalline purity is higher, but because day illumination is shone, crystallization velocity is slower, can not join in the cycle production process sequence.Therefore a day illumination solarization method is not suitable for large-scale production.

Summary of the invention

The partition method that glycine alcohol analyses, separate ammonium chloride and methyl alcohol in the mother liquor of back mainly provides a kind of technical scheme that can extract methyl alcohol rapidly from mother liquor, isolate ammonium chloride.It is characterized in that: alcohol is analysed isolate the methyl alcohol ammonium chloride mother liquor (aqueous solution) that obtains behind the glycine and enter distillation tower fractionation by distillation methyl alcohol and ammonium chloride, the recyclable recycling of methyl alcohol, obtain ammonium chloride solution and open steam and dewater, be warming up to 115 ℃ through evaporation, filter, dehydration obtains ammonium chloride.Promptly in 1 cube of reactor, add 250KG urotropine solution, add water 170KG, driving ammonia valve, to transfer to PH be 7.3～7.6, the chloroacetic acid solution 650KG that dropping prepares, reaction solution temperature in mid-term is controlled at 79.5～80.5 ℃, and PH is controlled at 5.8～6.5, and the reaction end temp is controlled at 81.5～82.5 ℃, PH is controlled at 6.8～7.5, is discharged to alcohol and analyses the chamber.Per 5 cubes of alcohol are analysed and are added water 150KG, after having connect ammonia chloride liquid, stir and begin to drip the dilute methanol for preparing half an hour again, put fast rate of addition from slow to fast gradually, drip the water for cooling that drives a well after half an hour, drip off methyl alcohol and be cooled to 27 ℃, begin to filter, centrifugal, dry, sieve obtains the technical grade glycine after expecting.Alcohol is analysed and is separated the methyl alcohol aqueous ammonium chloride solution obtain and enter distillation tower fractionation by distillation methyl alcohol and ammonium chloride, and the recyclable recycling of methyl alcohol obtains ammonium chloride solution and opens steam and dewater, be warming up to 115 ℃ through evaporation, filter, dehydration obtains ammonium chloride.

Description of drawings

Referring to accompanying drawing, be process flow sheet of the present invention.

Embodiment

Below in conjunction with drawings and the specific embodiments technical characterictic of the present invention is described further, referring to accompanying drawing, calculate for convenient, with 1 cube of reactor is unit: add 250KG urotropine solution in 1 cube of reactor, add water 170KG, driving ammonia valve, to transfer to PH be 7.3～7.6, the chloroacetic acid solution 650KG that dropping prepares, reaction solution temperature in mid-term is controlled at 79.5～80.5 ℃, PH is controlled at 5.8～6.5, the reaction end temp is controlled at 81.5～82.5 ℃, and PH is controlled at 6.8～7.5, is discharged to alcohol and analyses the chamber.Per 5 cubes of alcohol are analysed and are added water 150KG, connect to open behind the ammonia chloride liquid and begun to drip the dilute methanol for preparing after stirring half an hour, put fast rate of addition from slow to fast gradually, drip the water for cooling that drives a well after half an hour, drip off methyl alcohol and be cooled to 27 ℃, begin to filter, centrifugal, dry, sieve expects to obtain the technical grade glycine.Alcohol is analysed and is separated the methyl alcohol aqueous ammonium chloride solution obtain and enter distillation tower fractionation by distillation methyl alcohol and ammonium chloride, and the recyclable recycling of methyl alcohol obtains ammonium chloride solution and opens steam and dewater, be warming up to 115 ℃ through evaporation, filter, dehydration obtains ammonium chloride.

Claims (1)

1. the partition method of ammonium chloride and methyl alcohol in the mother liquor of back is analysed, separated to glycine alcohol, it is characterized in that: alcohol is analysed isolate the methyl alcohol ammonium chloride mother liquor (aqueous solution) that obtains behind the glycine and enter distillation tower fractionation by distillation methyl alcohol and ammonium chloride, the recyclable recycling of methyl alcohol, obtain ammonium chloride solution and open steam and dewater, be warming up to 115 ℃ through evaporation, filter, dehydration obtains ammonium chloride.

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