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Production process for preparing disodium hydrogen phosphate from EOC method glyphosate mother liquor

A technology of disodium hydrogen phosphate and glyphosate mother liquor, applied in phosphorus compounds, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problems of easy poisoning and low service life of catalysts, Achieve the effects of increasing yield, reducing degradation cost, improving efficiency and conversion rate

Active Publication Date: 2021-11-26
ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a kind of production technique of EOC method glyphosate mother liquor to produce disodium hydrogen phosphate, produce the production technique of disodium hydrogen phosphate from glyphosate mother liquor, improve the recycling rate of glyphosate mother liquor, solve In the existing catalytic oxidation step, the catalyst is easily poisoned and the service life is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Mesoporous silica-supported iron was fabricated by the following steps:

[0028] S1. At room temperature, dissolve 2 mmol of sodium lauryl sarcosine in 30 mL of deionized water. After completely dissolving, add 12 mL of hydrochloric acid solution and stir at 400 r / min for 50 min to obtain solution A; 4 mL of tetraethyl orthosilicate and 0.2 Mix mL3-aminopropyltriethoxysilane evenly to obtain solution B; drop solution B into solution A at a rate of 1 drop / second, stir at 400r / min for 15min, then let it settle at room temperature for 24h, and place it at 73°C Set aside to settle, centrifuged, washed twice with deionized water, and dried in vacuo to obtain an intermediate product; 2 g of the intermediate product was dissolved in 20 mL of a mixed solution of ethanol and ethanolamine (volume ratio 3:1), refluxed for 12 h, and centrifuged. Wash the precipitate twice with ethanol, and dry it in vacuum to constant weight to obtain amino mesoporous silica;

[0029] S2. Add 12g ...

Embodiment 2

[0032] Mesoporous silica-supported iron was fabricated by the following steps:

[0033] S1, with step S1 in embodiment 1;

[0034] S2. Add 14g of amino mesoporous silica into 100mL of anhydrous dichloromethane, and ultrasonically disperse for 15 minutes, then add 30g of chlorosulfonic acid, and when no bubbles are generated by ultrasonication, stop ultrasonication, centrifuge, wash with deionized water, and heat at 30°C Vacuum drying to constant weight to obtain sulfonic acid-based mesoporous silica;

[0035] S3. Add 23g of sulfonic acid-based mesoporous silica into 70mL of deionized water, and ultrasonically disperse for 10-20min, then add 3g of ferric chloride, stir at 300r / min for 5h to obtain a mixture, transfer the mixture to a reaction kettle, and Stand at 82°C for 2h, cool to room temperature, centrifuge, vacuum dry, grind, place in a muffle furnace and heat up to 400°C at 5°C / min and bake for 6h to obtain iron supported on mesoporous silica.

Embodiment 3

[0037] S1, with step S1 in embodiment 1;

[0038] S2. Add 16g of amino mesoporous silica into 100mL of anhydrous dichloromethane, and ultrasonically disperse for 20min, then add 32g of chlorosulfonic acid, and when no bubbles are generated by ultrasonication, stop ultrasonication, centrifuge, wash with deionized water, 30°C Vacuum drying to constant weight to obtain sulfonic acid-based mesoporous silica;

[0039]S3. Add 26g of sulfonic acid-based mesoporous silica into 70mL of deionized water, and ultrasonically disperse for 10-20min, then add 3g of ferric sulfate, stir at 300r / min for 5h to obtain a mixture, transfer the mixture to a reaction kettle, and Stand at ℃ for 2 hours, cool to room temperature, centrifuge, vacuum dry, grind, place in a muffle furnace and heat up to 400 ℃ at 5 ℃ / min and bake for 6 hours to obtain iron supported on mesoporous silica.

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Abstract

The invention discloses a production process for preparing disodium hydrogen phosphate from glyphosate mother liquor through an EOC method, and belongs to the technical field of glyphosate mother liquor treatment. The production process comprises the following steps: 1, catalytic degradation of mother liquor: adjusting the pH value of the glyphosate mother liquor to 5-6, and then performing air oxidation under the action of mesoporous silica loaded iron to obtain oxidized mother liquor; 2, performing extraction to obtain mother liquor containing inorganic phosphorus salt; 3, carrying out solid-liquid separation to obtain a crude disodium hydrogen phosphate solid and a separation liquid; 4, membrane treatment: obtaining a crude disodium hydrogen phosphate solid again; 5, recrystallizing the solution to obtain a disodium hydrogen phosphate solid. According to the invention, mesoporous silica loaded iron is used as a catalyst, and the catalyst takes an iron compound as a precursor and mesoporous silica as a carrier, has high catalytic activity and stability, can be repeatedly used, and solves the problems of easy poisoning and short service life of the catalyst in the prior art.

Description

technical field [0001] The invention belongs to the technical field of glyphosate mother liquor treatment, and in particular relates to a production process for preparing disodium hydrogen phosphate from glyphosate mother liquor by EOC method. Background technique [0002] Glyphosate is a high-efficiency, low-toxicity, low-residue, and broad-spectrum herbicide for post-emergent herbicides. It has good systemic and conductive properties. It is one of the herbicide varieties with the largest consumption, the fastest growth momentum and the most market competitiveness in the world today. But at the same time, the production of glyphosate is also accompanied by the production of a large amount of glyphosate mother liquor. Glyphosate mother liquor has the characteristics of high COD, high phosphorus content, refractory degradation, and high biological toxicity. It is difficult to process and expensive to process. If these phosphorus-containing wastewater is discharged directly ...

Claims

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Application Information

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IPC IPC(8): C02F9/04C01B25/30B01J23/745C02F101/30
CPCC02F9/00C01B25/30B01J23/745C02F1/66C02F1/725C02F1/74C02F1/26C02F1/001C02F1/442C02F2101/306C02F2209/06C02F2301/08C02F2209/02C02F2209/03
Inventor 黄中桂雷忠裕王彪汪志成
Owner ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD