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A kind of method of bisglyphosate mother liquor recycling

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: 2018-05-22
BEIJING ZIGUANG YINGLI CHEM TECH CO LTD
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  • Summary
  • 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 of waste salt, and difficulty in utilization.
There is no good method for the treatment of wastewater and mother liquor produced in the dinitrile process. Although there are membrane technologies for wastewater treatment and desalination processes, there are large initial investment, frequent clogging and damage of membranes, short service life, and high operating costs. The high problem has not yet been well resolved
This process saves the consumption of alkali and hydrochloric acid, but increases the consumption of ammonia and the refining of crude products. The process is longer and the investment is relatively large.

Method used

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  • A kind of method of bisglyphosate mother liquor recycling
  • A kind of method of bisglyphosate mother liquor recycling
  • A kind of method of bisglyphosate mother liquor recycling

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

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

Embodiment 2

[0072] Example 2 Alkaline hydrolysis of iminodiacetonitrile and addition of iminodiacetate hydrochloride crude product condensation example

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

Embodiment 3

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

[0075] Take 200 g of the disodium salt feed liquid after the alkaline hydrolysis of iminodiacetonitrile in the workshop, in which the content of iminodiacetic acid is 25.09%; take 17.30 g of the crude product of diacid, in which the content of IDA is 48.38%, mix the two into 500 mL In a four-neck flask, gradually raise the temperature to 100-110°C for deamination, deamination to steam pH = 7-7.5, then 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 solution is at 60-70°C Slowly add 72.30 g of 98.26% phosphorus trichloride solution dropwise during heat preservation, and keep warm for 30 minutes a...

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Abstract

The invention relates to a kind of using iminodiacetonitrile as the main raw material, through alkali hydrolysis or acid hydrolysis and alkali hydrolysis combined process, adding ammonium salt and heating deamination double decomposition reaction, recovering ammonia gas or / and regenerated diacid monosodium salt, through Diglyphosate mother liquor is directly hydrolyzed and hydrogen chloride is precipitated by the same ion effect to separate qualified sodium chloride by-products. The acid mother liquor can be recycled. The mother liquor, mother liquor that cannot be applied mechanically and washing water can be completely separated by adding calcium hydroxide. The aqueous alkali solution can regenerate raw materials and products, which can be used mechanically or separately to synthesize bisglyphosate, and the regenerated calcium hydroxide can be used repeatedly. The new process can realize the clean production of diglyphosate and the recycling and high value-added utilization of by-products.

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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Patent Type & Authority Patents(China)
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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