A kind of method for triethylamine recovery, phosphorus pollutant removal and phosphorus resource recovery in glyphosate mother liquor

A technology for glyphosate mother liquor and phosphorus pollutants, applied in chemical instruments and methods, water/sewage multi-stage treatment, water/sludge/sewage treatment, etc., can solve the problem of increasing the content of phosphorus pollutants in glyphosate mother liquor, which is difficult Obtain the problems of calcium chloride products, slow escape speed of triethylamine, etc., and achieve obvious economic and social benefits, shorten recovery time, and fast mass transfer speed

Inactive Publication Date: 2017-04-12
SICHUAN LECHUANG TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Though said method can improve triethylamine rate of recovery, reduce waste water amount, but there are following problems: 1. owing to adding calcium hydroxide aqueous solution in glyphosate acidic mother liquor and reacting at normal temperature, thereby be difficult to remove the phosphorus pollutant in mother liquor Transform as much as possible, still have higher concentration of phosphorus pollutants in the mother liquor; Poor, the escape rate of triethylamine is slow, so the distillation time is long, resulting in increased energy consumption
3. due to higher phosphorus pollutants are arranged in the glyphosate mother liquor after step (1) treatment, thereby if the mother liquor at the bottom of the distillation tower is reclaimed for preparing calcium hydroxide aqueous solution, the calcium oxide aqueous solution will contain phosphorus pollutants, Increase the content of phosphorus pollutants in the glyphosate mother liquor for subsequent treatment. If the mother liquor at the bottom of the distillation tower is subjected to solid-liquid separation to recover calcium chloride through distillation and dehydration, it will be difficult to obtain qualified calcium chloride products.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The operation of this embodiment is as follows:

[0024] (1) Glyphosate mother liquor 500mL is packed into flask, under stirring, add calcium hydroxide powder in glyphosate mother liquor and stir evenly, the add-on of calcium hydroxide powder should make the pH value of glyphosate mother liquor be 10.5, Then raise the temperature of the glyphosate mother liquor to 85°C and react under stirring for 3 hours. During the reaction, the temperature of the reaction system is maintained at 85°C and the pH value is 10.5. The triethylamine vapor generated during the reaction is collected and condensed to obtain triethylamine 6.0 g of amine solution;

[0025] (2) pass into water vapor to the solid-liquid mixture material that reaction forms and carry out stripping desorption, the gas that steam stripping desorption discharges obtains 87 grams of triethylamine solution through condensation, and the time of steam stripping desorption is 10 minutes;

[0026] (3) The above two parts ...

Embodiment 2

[0033] The operation of this embodiment is as follows:

[0034](1) Glyphosate mother liquor 500mL is packed into the flask, under stirring, add the calcium hydroxide emulsion of mass concentration 10% in glyphosate mother liquor and stir evenly, the add-on of calcium hydroxide emulsion should make the glyphosate mother liquor The pH value is 11, and then the glyphosate mother liquor is heated to 90°C and reacted for 2 hours under stirring. During the reaction, the temperature of the reaction system is maintained at 90°C and the pH value is 11, and the triethylamine vapor generated during the reaction is collected. And condensed to obtain 82.4 grams of triethylamine solution;

[0035] (2) pass into water vapor to the solid-liquid mixture material that reaction forms and carry out stripping desorption, the gas that steam stripping desorption discharges obtains 12 grams of triethylamine solutions through condensation, and the time of steam stripping desorption is 10 minutes;

[...

Embodiment 3

[0039] The operation of this embodiment is as follows:

[0040] (1) Glyphosate mother liquor 500mL is packed into flask, under stirring, add the calcium hydroxide emulsion of mass concentration 25% in glyphosate mother liquor and stir evenly, the add-on of calcium hydroxide emulsion should make the glyphosate mother liquor The pH value is 12.3, and then the glyphosate mother liquor is heated to 95°C and reacted for 0.5 hours under stirring. During the reaction, the temperature of the reaction system is maintained at 95°C and the pH value is 12.3, and the triethylamine vapor generated during the reaction is collected. And condensed to obtain 84.5 grams of triethylamine solution;

[0041] (2) pass into water vapor to the solid-liquid mixture material that reaction forms and carry out stripping desorption, the gas that steam stripping desorption discharges obtains 11.3 grams of triethylamine solutions through condensation, and the time of steam stripping desorption is 10 minutes;...

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Abstract

A method for recovering triethylamine, removing phosphorus pollutants and recovering phosphorus resources in glyphosate mother liquor comprises operation steps as follows: (1) calcium hydroxide powder or a calcium hydroxide emulsion is added to the glyphosate mother liquor, the mixture is evenly mixed, the calcium hydroxide powder or the calcium hydroxide emulsion is required to be added to enable the pH value of the glyphosate mother liquor to range from 10.5 to 12.3, then the glyphosate mother liquor is heated to the temperature higher than 85 DEG C for a reaction for 0.5-3 h while stirring is performed, triethylamine vapor produced in the reaction is collected and condensed, and a triethylamine solution is obtained; (2) a solid-liquid mixture formed through the reaction is subjected to water vapor gas-stripping desorption, a gas discharged through water vapor gas-stripping desorption is condensed, and a triethylamine solution is obtained; (3) the triethylamine is obtained through dehydration treatment of the obtained triethylamine solutions; (4) a coagulant is added to the solid-liquid mixture obtained after water vapor gas-stripping desorption while stirring is performed, the mixture is evenly mixed, then solid-liquid separation is performed after a reaction while stirring is performed, obtained solid substances are used as the phosphorus resources to be recycled, and an obtained liquid is collected for further treatment.

Description

technical field [0001] The invention belongs to the field of glyphosate mother liquor treatment and relates to a method for removing phosphorus pollutants from glyphosate mother liquor and recovering triethylamine and phosphorus resources. Background technique [0002] The mainstream process of glyphosate production in my country adopts the glycine method (also known as the alkyl ester method). After the synthesis reaction is completed, a large amount of acidic mother liquor (pH<1.0) will be produced when the glyphosate is extracted by solid-liquid separation. The acidic mother liquor Contains about 24% triethylamine hydrochloride, 1-3% glyphosate, glyphosate, methyl glyphosate, aminomethyl phosphoric acid, dimethyl phosphite, inorganic phosphate, etc. Since the mother liquor contains a large amount of organic phosphine and other pollutants, direct discharge into the environment will bring serious environmental problems. Before 2010, domestic enterprises basically adopted...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/05C07C209/86C02F9/10C02F103/36
Inventor 夏烈文姒俊吴泳霖曾陶
Owner SICHUAN LECHUANG TECH CO LTD
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