Method of preparation and application of ion-keeper adsorbent

Patent metadata

Field	Value
Publication number	US-11071967-B2
Application number	US-201715776985-A
Country	US
Kind code	B2
Filing date	Mar 2, 2017
Priority date	Mar 25, 2016
Publication date	Jul 27, 2021
Grant date	Jul 27, 2021

Abstract

The invention belongs to the field of chemical separation, hydrometallurgy and resource recovery and provides a method for preparing and applying of ion-keeper adsorbent. By adjusting the pH to selective oxidation to achieve the oxidation of ferrous iron into ferric iron. Separates the iron after the hydrothermal reaction; By using of ion imprint “ion keeper” effect and biomass as raw materials, to prepare the adsorbent with internal rules, hierarchical pores and high selectivity. It can be used for deep purification of chromium solution, such as iron, aluminum, vanadium and other impurities in the solution; After the deep purification of chromium solution, then adjusting the pH, adding appropriate hydrating agent, by hydrothermal precipitation treatment of chrome, filtration, acid washing and calcination to obtain chromium oxide crystal. It achieves the purification of chromium, iron, aluminum and chromium. The recycling and comprehensive utilization of waste resources are also realized. The process is simple, the iron, aluminum, vanadium and other impurities are in the selective adsorption. Chromium solution after deep purification can be processed for high purity chromium products to provide technical support.

First claim

We claim:

1. A preparation method of ion-keeper adsorbent, comprising:
(1) providing a chromate solution having a concentration of 0.1˜1.5 mol/L, wherein the pH of the chromate solution is adjusted to 2˜6;
(2) washing, breaking and soaking a biomass in the chromate solution for 2˜36 h to obtain a mixture of biomass chromate; a mass ratio of mass the biomass to the chromate solution is 1: 2˜8;
(3) transferring the biomass chromate mixture obtained in step (2) into a reaction kettle and aged-aging for 2˜8 hours at a temperature of 120 to 220° C. to obtain a chromium-keeper adsorbent, which is ion-keeper adsorbent.

2. The preparation method claim 1 , wherein the biomass is one or more of a kelp, a straw, a sawdust, a leaf or a peel.

3. An application method of the ion-keeper obtained in the preparation method of claim 1 , comprising:
(1) dissolving a chromium-containing solid or chromium-containing solution in an acid solution, and a pH is adjusted to 0.5˜4.5, an insoluble material is filtered to obtain a chromium liquid 1 ; pickling the insoluble material obtained by filtration until the chromium content in line with the national environmental protection standard;
(2) a pH of the chromium liquid 1 obtained in the step (1) is adjusted to 0.5˜6.0, adding a reducing agent, and the pH is adjusted to 1.0˜5.0, obtaining a separated ferrochrome qualified liquid; adding oxidant to obtain a mixed solution of trivalent iron, trivalent chromium and trivalent aluminum; the mixed solution is subjected to hydrothermal reaction, and the reaction is accompanied by constant stirring; after the reaction is finished, a filtrate and Fe-containing sediment are obtained; the pH of filtrate is adjusted to 0.5 to 3.5 and a chrome storage solution is gotten, that is chromium liquid 2 ; hydrothermal conditions are in the range of 50˜150° C. and 0.5Mpa˜2.5 Mpa for 0.5˜10 hours;
(3) adding the ion keeper adsorbent to the chromium liquid 2 obtained in the step (2) or passing the chromium liquid 2 through a fixed bed equipped with the ion-keeper adsorbent; a ratio of the ion-keeper adsorbent and the chromium liquid 2 is 1:150˜500 and then shock or stirring 5˜24 hours, get sinking a chrome qualified liquid 3 ;
(4) high temperature hydrothermal: the chrome qualified liquid 3 and hydrating agent is placed in a closed reactor hydrothermal reaction, heated to 150˜400° C,the pressure of 0.5 Mpa˜4.5 Mpa, insulation 1 to 5 hours; a reaction product is filtered, washed with acidic liquid and dried to obtain green filter cake which is high purity chromium compound, calcined at 500˜1200° C. and transformed into nano-chromium oxide solid.

4. The preparation method of claim 3 , wherein the reducing agent is methanol, ethanol and straw or two of the above mixture.

5. The preparation method of claim 3 , wherein an oxidizing agent is selected from the group consisting of oxygen, air, hydrogen peroxide, ozone or sulfuric acid radicals.

6. The preparation method of claim 4 , wherein an oxidizing agent is selected from the group consisting of oxygen, air, hydrogen peroxide, ozone or sulfuric acid radicals.

7. The preparation method of claim 3 , wherein the hydrating agent is selected from oxalic acid, cellulose, methanol, formaldehyde, formic acid, ethanol or glucose.

Assignees

• Univ Dalian Tech

Inventors

• Ma Wei
• Duan Shibo
• Yu Shuangen
• Meng Fanqing
• Wang Ren
• Xu Jun
• Guo Liyan
• Wu Lei
• Liu Zhuo
• Tan Dazhi

Classifications

• C22B3/24

  by adsorption on solid substances, e.g. by extraction with solid resins · CPC title

• B01J20/24 Primary

  Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives · CPC title

• B01J20/3021

  Milling, crushing or grinding · CPC title

• Y02P10/20

  Recycling · CPC title

• B01J2220/4843

  Algae, aquatic plants or sea vegetals, e.g. seeweeds, eelgrass · CPC title