Recycling method for mother liquor of N-(phosphonomethyl)iminodiacetic acid

A technology of bisglyphosate mother and bisglyphosate, which is applied in the direction of chemical instruments and methods, preparation of organic compounds, compounds of Group 5/15 elements of the periodic table, etc., can solve the problems of increasing crude product purification, frequent membrane clogging and damage, Problems such as short service life

Active Publication Date: 2016-03-30
BEIJING ZIGUANG YINGLI CHEM TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has too many times of solid-liquid separation, and the yield of diacid is only about 80%. A large amount of diacid waste water containing salt is concentrated and desalted, and the method of regeneration of evaporative condensate is used. The energy consumption is high, and the quality of salt is poor, so it is difficult to use.
[0007] At present, most enterprises adopt the method of desalting concentrated diglyphosate wastewater and regenerating evaporative condensate, but the existence of formaldehyde leads to biochemical difficulties, and there are problems such as high energy consumption, poor quality o

Method used

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  • Recycling method for mother liquor of N-(phosphonomethyl)iminodiacetic acid
  • Recycling method for mother liquor of N-(phosphonomethyl)iminodiacetic acid
  • Recycling method for mother liquor of N-(phosphonomethyl)iminodiacetic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069] Example 1 The acid solution of iminodiacetonitrile is applied mechanically to prepare the crude product of iminodiacetic acid hydrochloride.

[0070] Add 300g of 32% hydrochloric acid and 50g of water into a 500mL four-necked flask, and preheat it to 60-80°C, add 50g of 95% iminodiacetonitrile solid or solution to the preheated hydrochloric acid at a uniform speed within 30min, and the addition is complete Insulate at 95-120°C for 30 minutes, cool down and crystallize and separate to obtain 101g of crude iminodiacetate hydrochloride, 295g of acidolysis mother liquor; add 50g of water to the acidolysis mother liquor, pass in 55g of HCl gas, and preheat to 60 -80°C, add 50g of 95% iminodiacetonitrile solid or solution to the preheated acidolysis mother liquor with HCl gas at a uniform speed within 30 minutes, after adding, keep it warm at 95-120°C for 30 minutes, cool down to crystallize and separate, Obtained 151g of iminodiacetate hydrochloride crude product, 296g of a...

Embodiment 2

[0072] Example 2 Alkaline hydrolysis of iminodiacetonitrile and addition of iminodiacetochloride hydrochloride crude product condensation embodiment

[0073] Mix 44g of 96% sodium hydroxide and 150g of water into a 500mL four-neck flask, stir and maintain the temperature at 50-80°C, add 50g of 95% iminodiacetonitrile solid or solution into the sodium hydroxide solution at a uniform speed, and add The time is 0.5-1h. After the feeding is completed, keep the temperature at 50-80°C for 30min, and gradually raise the temperature of the alkaline solution to 100-110°C for deamination for about 1h. Add 38g (IDA%=40.36%, acidity is 50% based on HCl) mixed iminodiacetic acid hydrochloride crude product in Example 1, partially acidify the alkaline solution and continue heating for deamination until the steam pH=7 Sampling after -7.5 to track the determination of free ammonia and free NH 3 -N%=0.03%, after deamination, add 60g of hydrochloric acid (37%) to continue to acidify the syst...

Embodiment 3

[0074] Example 3 Condensation of crude product of iminodiacetonitrile disodium salt by adding iminodiacetate hydrochloride

[0075] Take 200g of the disodium salt feed solution after the alkaline hydrolysis of iminodiacetonitrile in the workshop, in which the iminodiacetic acid content is 25.09%; take 17.30g of the crude diacid product, in which the IDA content is 48.38%, and mix the two into 500mL four-port In the flask, gradually increase the temperature to 100-110°C for deamination, after deamination to steam pH=7-7.5, take samples to track and measure free ammonia and free NH 3 -N%=0.01%, after the deamination is completed, replenish water until the concentration of iminodiacetic acid is 27.5%, add hydrogen peroxide and activated carbon, and keep warm at 80-100°C for 30 minutes for decolorization, and the decolorized feed liquid is between 60-70°C Keep warm and slowly add 72.30g of 98.26% phosphorus trichloride solution dropwise. After the dropwise addition, keep warm fo...

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Abstract

The invention relates to a recycling method for mother liquor of N-(phosphonomethyl)iminodiacetic acid. According to the invention, with iminodiacetonitrile as a main raw material, through an alkaline hydrolysis process or an acidolysis and alkaline hydrolysis combined process, ammonia gas is recycled or/and monosodium diacid salt is generated by addition of ammonium salt and double decomposition reaction of deamination under heating; a qualified sodium chloride by-product is precipitated and separated through direct hydrolysis of the mother liquor of N-(phosphonomethyl)iminodiacetic acid and common-ion effect of hydrogen chloride; acidic mother liquor can be recycled; the mother liquor, the mother liquor incapable of being reused and washing water can be completely precipitated and separated through the addition of calcium hydroxide; the obtained precipitate can regenerate raw materials and products through an aqueous solution of acid or alkali; N-(phosphonomethyl)iminodiacetic acid is reused or separately synthesized; and the regenerated calcium hydroxide can be repeatedly reused. The novel recycling method provided by the invention can realize clean production of N-(phosphonomethyl)iminodiacetic acid and cyclic utilization of by-products with high added value.

Description

technical field [0001] The invention relates to a clean production process of a glyphosate intermediate diglyphosate, in particular to a method for recycling a diglyphosate mother liquor, and belongs to the technical field of pesticides and fine chemicals. Background technique [0002] Diglyphosate is an intermediate for the preparation of glyphosate, a broad-spectrum herbicide with the largest global consumption. The chemical name of glyphosate is N-phosphonomethylglycine. The control of deep-rooted malignant weeds is very effective. In recent years, the sales volume has gradually increased. It ranks first among the 50 largest pesticide varieties in the world. The market size exceeds 10 billion US dollars. It has been registered and widely used in more than 130 countries around the world. [0003] The industrial production of bisglyphosate is obtained by using iminodiacetic acid, phosphorous acid and formaldehyde under the catalysis of hydrochloric acid, heating to reflux c...

Claims

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Application Information

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IPC IPC(8): C07F9/38C07C229/16C07C227/40C07C227/18
Inventor 孙响响李宇航杨少梅韩田田孙瑞黄仁兵廖翠莺崔建斌张海双
Owner BEIJING ZIGUANG YINGLI CHEM TECH CO LTD
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