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Method for recovering triethylamine, removing phosphorus pollutants and recovering phosphorus resources 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: 2015-12-09
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) Put 500mL of the glyphosate mother liquor into the flask, add calcium hydroxide powder to the glyphosate mother liquor under stirring and stir evenly. The amount of calcium hydroxide powder added should make the pH of the glyphosate mother liquor 10.5. Then the glyphosate mother liquor was heated to 85°C and reacted for 3 hours under stirring. During the reaction, the temperature of the reaction system was maintained at 85°C and the pH value was 10.5. The triethylamine vapor generated during the reaction was collected and condensed to obtain triethyl 6.0 grams of amine solution;

[0025] (2) Steam is introduced into the solid-liquid mixture formed by the reaction for gas stripping and desorption, the gas discharged by steam stripping and desorption is condensed to obtain 87 grams of triethylamine solution, and the time for steam stripping and desorption is 10 minutes;

[0026] (3) Combine the above-mentioned two par...

Embodiment 2

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

[0034] (1) Put 500mL of the glyphosate mother liquor into the flask, add calcium hydroxide emulsion with a mass concentration of 10% to the glyphosate mother liquor under stirring and stir evenly. The amount of calcium hydroxide emulsion added should be such that the glyphosate mother liquor The pH value is 11, 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 condense to obtain 82.4 g of triethylamine solution;

[0035] (2) Steam is introduced into the solid-liquid mixture formed by the reaction for gas stripping and desorption, the gas discharged by steam stripping and desorption is condensed to obtain 12 grams of triethylamine solution, and the time for steam stripping and desorption is 10 minutes;

[003...

Embodiment 3

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

[0040] (1) Put 500mL of the glyphosate mother liquor into the flask, add 25% calcium hydroxide emulsion with mass concentration to the glyphosate mother liquor under stirring and stir evenly. The amount of calcium hydroxide emulsion added should be such that the glyphosate mother liquor The pH value was 12.3, then the glyphosate mother liquor was heated to 95°C and reacted for 0.5 hours under stirring. During the reaction, the temperature of the reaction system was maintained at 95°C and the pH value was 12.3. The triethylamine vapor generated during the reaction was collected And condense to obtain 84.5 g of triethylamine solution;

[0041] (2) Steam is introduced into the solid-liquid mixture formed by the reaction for gas stripping and desorption. The gas discharged by steam stripping and desorption is condensed to obtain 11.3 grams of triethylamine solution. The time for steam stripping and desorption is 10 minutes;

[004...

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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 the glyphosate mother liquor and recovering triethylamine and phosphorus resources. Background technique [0002] The mainstream process for glyphosate production in my country is the glycine method (also known as the alkyl ester method). After the synthesis reaction is completed, solid-liquid separation and extraction of glyphosate will produce a large amount of acidic mother liquor (pH<1.0). It contains about 24% of triethylamine hydrochloride, 1-3% of glyphosate, as well as increased glyphosate, methyl glyphosate, aminomethyl phosphoric acid, dimethyl phosphite, inorganic phosphate, etc. Since the mother liquor contains a large amount of organic phosphines and other pollutants, direct discharge into the environment will cause serious environmental problems. Before 2010, domestic enterprises basically used the method...

Claims

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Application Information

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Patent Type & Authority Applications(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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