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CN-121972140-A - Glyphosate adsorption material and preparation method and application thereof

CN121972140ACN 121972140 ACN121972140 ACN 121972140ACN-121972140-A

Abstract

The invention discloses a glyphosate adsorption material with salt tolerance and wide pH application range, which is prepared by taking D202 macroporous strong alkali II type styrene anion exchange resin as a carrier and loading metal oxide, and the preparation method comprises the steps of respectively preprocessing the D202 macroporous strong alkali II type styrene anion exchange resin by adopting ethanol, distilled water, sodium hydroxide solution and sodium chloride solution, drying, preparing metal salt solution, loading metal salt into pores of the exchange resin by a dipping-steaming method, dispersing the metal salt solution into alkaline solution for stirring reaction, filtering and washing, and drying to obtain the glyphosate adsorption material.

Inventors

  • DONG ZHEN
  • KANG XINCHENG
  • YANG MIAO
  • XIA TAO

Assignees

  • 武汉理工大学

Dates

Publication Date
20260505
Application Date
20260204

Claims (10)

  1. 1. A glyphosate adsorption material with salt tolerance and wide pH application range is characterized in that D202 macroporous strong base II type styrene anion exchange resin is used as a carrier, and metal oxide is loaded to prepare the glyphosate adsorption material.
  2. 2. The method for preparing the glyphosate adsorbing material as set forth in claim 1, comprising the steps of: (1) Pretreating D202 macroporous strong base II type styrene anion exchange resin by respectively adopting ethanol, distilled water, sodium hydroxide solution and sodium chloride solution, and drying; (2) Preparing a metal salt solution, and loading the metal salt into pores of the exchange resin through a dipping-steaming method; (3) Dispersing the mixture into alkaline solution, stirring the mixture for reaction, filtering, washing and drying the mixture to obtain the glyphosate adsorption material.
  3. 3. The process for preparing glyphosate adsorbing material as set forth in claim 2, wherein in step (1), the D202 macroporous strong base type II styrene anion exchange resin has a particle size of 0.315-1.25mm, a volume exchange capacity of 1.0mmol/mL or more, and a wet true density of 1.07-1.12g/mL.
  4. 4. The method for preparing a glyphosate adsorbing material according to claim 2, wherein the pretreatment in step (1) comprises immersing in distilled water, sodium hydroxide solution and sodium chloride solution at 20-40 ℃ for 10-30min, wherein the concentration of the sodium hydroxide solution is 3-5wt% and the concentration of the sodium chloride solution is 7-10wt%.
  5. 5. A process for preparing a glyphosate adsorbing material as set forth in claim 2, wherein said impregnating-evaporating method of step (2) comprises immersing said exchange resin in said metal salt solution, heating and stirring until the solution evaporates.
  6. 6. The method for preparing a glyphosate adsorbing material according to claim 2, wherein said metal salt in step (2) is one or more of iron salt, lanthanum salt, cerium salt, neodymium salt, and yttrium salt.
  7. 7. The process for preparing glyphosate adsorbing material as set forth in claim 2, wherein said metal salt solution in step (2) is ethanol/water solution as solvent, the preparation temperature is 50-60 ℃, and the stirring speed is 300-400rpm.
  8. 8. The process for preparing a glyphosate adsorbing material as set forth in claim 2, wherein said alkaline solution in step (3) is an aqueous solution of sodium hydroxide or potassium hydroxide at a concentration of 0.1 to 1M.
  9. 9. The process for preparing glyphosate adsorbing material as set forth in claim 2, wherein the stirring reaction temperature in step (3) is 20-50 ℃ and the reaction time is 24-48 hours.
  10. 10. The use of the glyphosate adsorbing material of claim 1 in a glyphosate separation process comprising directly separating and recovering glyphosate from an acidic glyphosate mother liquor, an alkaline glyphosate mother liquor or a glyphosate contaminated wastewater.

Description

Glyphosate adsorption material and preparation method and application thereof Technical Field The invention belongs to the technical field of composite materials, and particularly relates to a glyphosate adsorption material, and preparation and application thereof. Background Glyphosate is currently the most widely used herbicide worldwide due to its broad spectrum and high efficacy with low toxicity. On the one hand, the glyphosate after use has higher water solubility, enters the human body through water and food chains, and has toxic action on the nervous and endocrine systems. On the other hand, in the industrial production process of glyphosate, in order to realize crystallization separation and purification of a target product, the process is often accompanied by acidification, alkalization and multi-step salting out/crystallization operation, and two typical mother solutions with common characteristics of high salinity, extreme pH and high concentration glyphosate are finally produced, namely an acidic mother solution and an alkaline mother solution. The existing mother liquor treatment technology generally converts organic phosphine into inorganic phosphorus for recovery through a deep oxidation technology, the selling price of the organic phosphine in the waste liquid is far higher than that of the inorganic phosphate, but few reports are given to the recovery of high-value organic phosphine in the mother liquor. Therefore, the method is oriented to the resource treatment of the organic phosphine in the acid and alkaline glyphosate mother liquor, and has important environmental significance and economic value. Although used for the separation of glyphosate by different classes of adsorbents, such as inorganic materials (activated carbon, graphene), natural polymers (nanocellulose), commercial resins (D201, D301) and new materials such as MOF, etc. However, a large amount of acidic or alkaline mother liquor generated in the glyphosate production process has the characteristics of extreme pH, high salt and ion strength, complex coexisting components and the like, and is easy to cause the limitations of insufficient selectivity, reduced adsorption capacity or strict pH condition requirement of the conventional adsorption material. In the existing engineering treatment, the mother liquor is often required to be subjected to neutralization, desalination or multi-step pretreatment, and then the units such as precipitation/membrane separation/oxidation are matched to realize load reduction and standard emission, but the problems of large medicament consumption, increased salt load and secondary wastewater, long flow, high running cost and the like generally exist in the mode. Therefore, a material and a method which can adapt to the complex working condition of the glyphosate acid-base production mother solution, can be directly added for use and realize efficient adsorption and recovery are needed, so as to reduce the treatment cost and improve the recycling level. Disclosure of Invention A large amount of acidic or alkaline mother solution generated in the glyphosate production process has the characteristics of extreme pH, high salt and ion strength, complex coexisting components and the like, and is easy to cause the limitations of insufficient selectivity, reduced adsorption capacity or strict pH condition requirement of the conventional adsorption material. In the existing engineering treatment, the mother liquor is often required to be subjected to neutralization, desalination or multi-step pretreatment, and then the units such as precipitation/membrane separation/oxidation are matched to realize load reduction and standard emission, but the problems of large medicament consumption, increased salt load and secondary wastewater, long flow, high running cost and the like generally exist in the mode. Aiming at the situation that no glyphosate adsorbent capable of directly treating glyphosate mother liquor exists in the market, the invention provides the glyphosate adsorption material with salt tolerance and wide pH effect and the preparation method thereof, which can directly treat glyphosate acid-base amphoteric mother liquor. A glyphosate adsorbing material with high salt tolerance and wide pH range is prepared from D202 macroporous strong alkali type II styrene anion exchange resin as carrier and loaded metal oxide. The invention also provides a preparation method of the glyphosate adsorption material, which comprises the following steps: (1) Pretreating D202 macroporous strong base II type styrene anion exchange resin by distilled water, sodium hydroxide solution and sodium chloride solution respectively, and drying; (2) Preparing a metal salt solution, and loading the metal salt into pores of the exchange resin through a dipping-steaming method; (3) Dispersing the mixture into alkaline solution, stirring the mixture for reaction, filtering, washing and drying the mixture to obtain the glyphosate