An optimized method for the synthesis of diglyphosate from iminodiacetonitrile

A technology of iminodiacetonitrile and bisphosphonate is applied in chemical instruments and methods, organic chemistry, compounds of elements of Group 5/15 of the periodic table, etc. time, improved yield, and high economic efficiency

Active Publication Date: 2012-02-08
SHANDONG WEIFANG RAINBOW CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This route needs to control the lye concentration at about 20% during the alkaline hydrolysis process, so a large amount of water must be poured into the liquid caustic soda to dilute the liquid caustic soda, but high-quality synthetic diglyphosate requires IDA concentration at 25% Above, so methods such as evaporation should be adopted to remove part of the water in the system after the alkali hydrolysis is completed, and the amount of dehydrated water is at least 40%-50% of the amount of water added, and dehydration takes up a lot of time, so in terms of energy consumption and There are major disadvantages in terms of production capacity
In terms of process route optimization, relevant research units and production companies have conducted a lot of research, but there are few studies and reports on reducing the cost of diglyphosate from the perspective of reducing energy consumption and increasing production capacity in the alkaline hydrolysis process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Take 115g of sodium hydroxide solution with a mass fraction of 32%, and 32g of water to form an alkali solution, add it to a 500ml flask, heat up to 40°C, start to slowly add iminodiacetonitrile (92% mass fraction), first add 80g, and take 1 Hour. Then add 160g of 32% sodium hydroxide solution, and then add 23g of iminodiacetonitrile for 0.5 hours. After the addition, the temperature is raised to 82°C, kept for 1 hour, ammonia is discharged for 0.5 hours, and 40g of 30% hydrochloric acid is added at 78°C. Keep warm for 10-20 minutes, then filter to obtain 414.6 g of filtrate. Transfer the filtrate to a 1000ml flask and add 163.3g of phosphorus trichloride dropwise at 40-50°C for 1.5 hours, then raise the temperature to reflux and add 105g of formaldehyde (36.5%) dropwise. 70g, add 57.8g sodium hydroxide (32%) to adjust the pH, lower the temperature, crystallize, filter with suction, wash with 400g water, and dry to obtain 204.4g of bisglyphosate with a content of 98.3%...

Embodiment 2

[0020] Take 131.5g of sodium hydroxide solution with a mass fraction of 32%, and 80g of water to form an alkali solution, add it to a 500ml flask, heat up to 60°C, start to slowly add iminodiacetonitrile (92%), first add 51.5g, and take 1 hour, then add 50g of 32% sodium hydroxide, and then add 51.5g of iminodiacetonitrile for 0.5 hours, then add 81.5g of 32% sodium hydroxide solution, heat up to 85°C, keep warm for 1.5 hours, and discharge ammonia for 0.5 hour, cooled to about 78°C and added 40g of 30% hydrochloric acid, then filtered, the filtrate was 455.1g. Transfer the filtrate to a 1000ml flask and add 153g of phosphorus trichloride dropwise at 40-50°C for 1 hour, then raise the temperature to reflux and add 115g of formaldehyde (36.5%) dropwise. , add 58g of sodium hydroxide (32%) to adjust the pH, lower the temperature, crystallize, filter with suction, wash with 400g of water, and dry to obtain 205.1g of bisglyphosate with a content of 98.3% and a solid yield of 88.8%...

Embodiment 3

[0022] Take 104g of sodium hydroxide solution with a mass fraction of 32%, and 64g of water to form an alkali solution, add it to a 500ml flask, heat up to 40°C, start to slowly add iminodiacetonitrile (92%), and add a total of 103g for 1 hour. Then add 156g of 32% sodium hydroxide, heat up to 90°C, keep warm for 2 hours, discharge ammonia for 0.5 hour, cool down to 83°C and add 40g of 30% hydrochloric acid, then filter, the filtrate is 432.9g. Transfer the filtrate to a 1000ml flask and add 165g of phosphorus trichloride dropwise at 40-50°C for 1 hour, then warm up to reflux and add 105g of formaldehyde (36.5%) dropwise. Add 60.3g of sodium hydroxide (32%) to adjust the pH, lower the temperature, crystallize, filter with suction, wash with 400g of water, and dry to obtain 204.9g of bisglyphosate with a content of 98.6% and a solid yield of 89.0%.

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Abstract

The invention discloses a method for synthesizing bisglyphosate from iminodiacetonitrile. The following steps are adopted: firstly, part of the high-concentration liquid alkali is made into a 20%-25% alkali solution, the temperature is raised to 40-60°C, and then slowly Dosing of iminodiacetonitrile, 1-2 hours after the addition, add the remaining amount of liquid alkali during or after the addition of iminodiacetonitrile; raise the temperature to 80-95°C, keep it warm for 1-2 hours, deamination for half an hour , add hydrochloric acid to adjust the pH, and obtain iminodiacetic acid and its sodium salt solution; filter, and react the filtrate with phosphorus trichloride and formaldehyde to generate diglyphosate wet material and waste water. The invention is simple and easy to implement, reduces the water consumption during alkaline hydrolysis, saves the alkaline hydrolysis dehydration process, improves the deammonization efficiency, reduces energy consumption, increases the content of iminodiacetic acid, improves the yield of diglyphosate, and has the advantages of Higher economic benefit.

Description

technical field [0001] The invention relates to a method for synthesizing diglyphosate from iminodiacetonitrile, in particular to a production method for synthesizing diglyphosate by reducing energy consumption and improving production capacity. Background technique [0002] The iminodiacetic acid (IDA) method was developed in the late 1990s and realized industrialized production. The iminodiacetonitrile method (IDAN) is mainly used in this process in China. Due to the advantages of cheap and easy-to-obtain raw materials such as iminodiacetonitrile, good catalyst selectivity and higher yield for glyphosate oxidation, the production cost is lower, and the degree of cleaner production is higher than that of the glycine method. Mainstream technology. [0003] In the route of synthesizing bis-glyphosate by iminodiacetonitrile now, iminodiacetonitrile all is to carry out alkaline hydrolysis in dilute lye (alkali content about 20%), after alkaline hydrolysis is finished, first de...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38
Inventor 陈桂元孙国庆陈琦侯永生孙文萍赵超
Owner SHANDONG WEIFANG RAINBOW CHEM
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