Preparation method for combined modified straw active particulate carbon adsorption material and use of same

Patent metadata

Field	Value
Publication number	US-11633714-B2
Application number	US-201816621621-A
Country	US
Kind code	B2
Filing date	Nov 26, 2018
Priority date	Dec 12, 2017
Publication date	Apr 25, 2023
Grant date	Apr 25, 2023

Abstract

A preparation method for a combined modified straw active particulate carbon adsorption material and use of same. The preparation method for the combined modified straw active particulate carbon adsorption material comprises the following steps: 1) mixing straw powders, distilled water, a binder and a composite mineral, then pelletizing same, and then placing same in a tube furnace for pyrolysis to prepare straw particulate carbon; 2) introducing an inert gas into a modification reagent, adjusting the pH value combined and 3) soaking the straw particulate carbon into the combined modification solution for 30 min, and performing cleaning and drying, so as to obtain a combined modified straw active particulate carbon adsorption material. The combined modified straw active particulate carbon has a good adsorption effect on phosphate group in low-pollution water.

First claim

The invention claimed is:

1. A preparation method of a combined modified straw activated granular carbon adsorption material for phosphorus removal, comprising the following steps:
1) mixing 100 pbw straw powder, 50-150 pbw distilled water, 10-100 pbw binder, and 0-25 pbw composite mineral for granulation, to obtain straw composite granules;
2) Loading the straw composite granules in a tubular furnace and carrying out pyrolysis at 350-750° C. for 1-6h, and then cooling, to obtain straw granular carbon with a particle size of 0.5-6 mm for later use;
3) Charging an inert gas into a modification reagent, which are at least one of metallic magnesium ion solution, metallic aluminum ion solution, or metallic iron ion solution and adding an alkaline solution in drops till the pH is 8-11; carrying out ultrasonic treatment for 5-30 minutes, keeping in a still state at 35-60° C. for 30-80 minutes, and then adding ferric nitrate solution for reaction for 5-10 minutes, to obtain a combined modified solution for later use;
4) Loading the straw granular carbon obtained in the step 2) into the combined modified solution obtained in the step 3) and soaking for 30 minutes, carrying out ultrasonic treatment at 1-8 MPa for 1-12h, and then centrifuging; next, drying at 105±2° C., firing in a muffle furnace at 200° C. for 2-8h, taking out and washing with 0.1 mol/L hydrochloric acid solution and deionized water in alternate till the supernatant is neutral, and then drying, so as to obtain the combined modified straw activated granular carbon adsorption material.

2. The method of claim 1 wherein the molar concentration of the modification reagent is 0.25-0.85 mol/L.

3. The preparation method of the combined modified straw activated granular carbon adsorption material according to claim 2 , wherein, in the step 1), the composite mineral comprises at least one of nano-montmorillonite and anion powder, the anion powder composed of tourmaline powder and lanthanide or rare earth elements.

4. The preparation method of the combined modified straw activated granular carbon adsorption material according to claim 3 , wherein, the molar concentration of the ferric nitrate solution added in the step 3) is 0.1 mol/L, and the mass of the ferric nitrate solution accounts for 10% of the mass of the modification reagent; the mass ratio of the straw granular carbon to the combined modified solution in the step 4) is 1:2-10.

5. The preparation method of the combined modified straw activated granular carbon adsorption material according to claim 4 , wherein, in the step 1), the binder is at least one of cellulose ether and its derivatives, natural polymer and its derivatives, polyvinyl alcohol, and beta-cyclodextrin;
wherein the cellulose ether and its derivatives comprise at least one of methyl cellulose, ethyl cellulose, methyl hydroxyethyl cellulose, hydroxyethyl cellulose, ethyl hydroxyethyl cellulose, carboxymethyl hydroxyethyl cellulose and methyl hydroxypropyl cellulose;
the natural polymer and its derivatives comprise at least one of starch, gelatin, sodium alginate, guar gum and Arabic gum.

6. The preparation method of the combined modified straw activated granular carbon adsorption material according to claim 5 , wherein, in the step 1), the straw powder comprises at least one of wheat straw powder, rice straw powder, corn straw powder, peanut straw powder, cassava straw powder, coconut shell powder and bamboo processing residue powder; the particle size of the straw powder is 40-60 mesh.

7. The preparation method of the combined modified straw activated granular carbon adsorption material according to claim 5 , wherein, the mass ratio of the nano-montmorillonite to the anion powder is 1-1.5:1.

8. The preparation method of the combined modified straw activated granular carbon adsorption material according to claim 2 , wherein, in the step 1), the straw powder comprises at least one of wheat straw powder, rice straw powder, corn straw powder, peanut straw powder, cassava straw powder, coconut shell powder and bamboo processing residue powder; the particle size of the straw powder is 40-60 mesh.

9. The preparation method of the combined modified straw activated granular carbon adsorption material according to claim 2 , wherein, in the step 1), the composite mineral comprises at least one of nano-montmorillonite and anion powder.

10. The preparation method of the combined modified straw activated granular carbon adsorption material according to claim 2 , wherein, the inert gas in the step 3) is N 2 or Ar, and the alkaline solution in the step 3) is ammonia water or sodium hydroxide solution.

11. The preparation method of the combined modified straw activated granular carbon adsorption material according to claim 3 , wherein, in the step 1), the straw powder comprises at least one of wheat straw powder, rice straw powder, corn straw powder, peanut straw powder, cassava straw powder, coconut shell powder and bamboo processing residue powder; the particle size of the straw powder is 40-60 mesh.

12. The preparation method of the combined modified straw activated granular carbon adsorption material according to claim 3 , wherein, the mass ratio of the nano-montmorillonite to the anion powder is 1-1.5:1.

13. The preparation method of the combined modified straw activated granular carbon adsorption material according to claim 3 , wherein, the inert gas in the step 3) is N 2 or Ar, and the alkaline solution in the step 3) is ammonia water or sodium hydroxide solution.

14. The preparation method of the combined modified straw activated granular carbon adsorption material according to claim 4 , wherein, in the step 1), the straw powder comprises at least one of wheat straw powder, rice straw powder, corn straw powder, peanut straw powder, cassava straw powder, coconut shell powder and bamboo processing residue powder; the particle size of the straw powder is 40-60 mesh.

15. The preparation method of the combined modified straw activated granular carbon adsorption material according to claim 4 , wherein, the mass ratio of the nano-montmorillonite to the anion powder is 1-1.5:1.

16. The preparation method of the combined modified straw activated granular carbon adsorption material according to claim 1 , wherein, in the step 1), the straw powder comprises at least one of wheat straw powder, rice straw powder, corn straw powder, peanut straw powder, cassava straw powder, coconut shell powder and bamboo processing residue powder; the particle size of the straw powder is 40-60 mesh.

17. The preparation method of the combined modified straw activated granular carbon adsorption material according to claim 1 , wherein, the mass ratio of the nano-montmorillonite to the anion powder is 1-1.5:1.

18. The preparation method of the combined modified straw activated granular carbon adsorption material according to claim 1 , wherein, the inert gas in the step 3) is N 2 or Ar, and the alkaline solution in the step 3) is ammonia water or sodium hydroxide solution.

19. The preparation method of the combined modified straw activated granular carbon adsorption material according to claim 1 , wherein, in the step 1), the temperature rise rate of the tubular furnace is 5-10° C./minute.

Assignees

• Jiangsu Acad Agricultural Sci

Inventors

• Sun Enhui
• Huang Hongying
• Jin Hongmei
• Wu Guofeng
• Chang Zhizhou
• Ye Xiaomei
• Xu Yueding
• Yong Cheng

Classifications

• C02F1/283

  using coal, charred products, or inorganic mixtures containing them · CPC title

• B01J20/20 Primary

  comprising free carbon; comprising carbon obtained by carbonising processes · CPC title

• B01J20/305

  Addition of material, later completely removed, e.g. as result of heat treatment, leaching or washing, e.g. for forming pores · CPC title

• B01J20/3085

  Chemical treatments not covered by groups B01J20/3007 - B01J20/3078 · CPC title

• B01J20/3078 Primary

  Thermal treatment, e.g. calcining or pyrolizing · CPC title