Cerium sulfate chelated sulfur dioxide, a preparation method and a use thereof

Patent metadata

Field	Value
Publication number	US-10899628-B2
Application number	US-201816094939-A
Country	US
Kind code	B2
Filing date	Mar 15, 2018
Priority date	Nov 27, 2017
Publication date	Jan 26, 2021
Grant date	Jan 26, 2021

Abstract

The disclosure discloses cerium sulfate chelated sulfur dioxide, a preparation method and a use thereof. The cerium sulfate chelated sulfur dioxide has a molecular formula of Ce[SO4][SO2].2H2O. It is a white crystal and the preparation method thereof may comprise the following steps: adding anhydrous cerium sulfate to dilute sulfuric acid with stirring for dissolvation; adding a solvent followed by refluxing at 45-50° C. for 2.0-2.5 h; heating the reaction product to remove the solvent, cooling to 20° C. or lower, and adding dilute sulfuric acid to allow precipitation of all crystals; cooling down the product followed by suction filtration, washing the obtained crystals by the solvent, so that crude cerium sulfate chelated sulfur dioxide can be obtained. The solubility of the cerium sulfate chelated sulfur dioxide of the disclosure has been significantly improved compared to the anhydrous cerium sulfate. The obtained solution is colorless and transparent, so that the cerium sulfate chelated sulfur dioxide can be used as a better titrant with wide application and supreme performance.

First claim

What is claimed is:

1. A preparation method of cerium sulfate chelated sulfur dioxide, characterized in that it comprises the following steps:
adding anhydrous cerium sulfate to dilute sulfuric acid with stirring for dissolvation, adding a solvent followed by refluxing at 45-50° C. for 2.0-2.5 h, heating the reaction product to remove the solvent, cooling to 20° C. or lower, and adding dilute sulfuric acid to allow precipitation of all crystals, cooling down the product followed by suction filtration, washing the obtained crystals by the solvent, so that the crude cerium sulfate chelated sulfur dioxide can be obtained.

2. The preparation method of cerium sulfate chelated sulfur dioxide as claimed in claim 1 , characterized in that it further comprises adding dilute sulfuric acid to the crude cerium sulfate chelated sulfur dioxide for recrystallization, then cooling down the product followed by suction filtration, and drying the product under vacuum to obtain a pure cerium sulfate chelated sulfur dioxide crystallized product.

3. The preparation of cerium sulfate chelated sulfur dioxide as claimed in claim 1 , the solvent is methanol.

4. The preparation method of cerium sulfate chelated sulfur oxide as claimed in claim 1 , characterized in that the dilute sulfuric acid is diluted from concentrated sulfuric acid to a 30% by mass sulfuric acid aqueous solution.

5. The preparation method of cerium sulfate chelated sulfur dioxide as claimed in claim 1 , characterized in that a mass ratio of the anhydrous cerium sulfate to the concentrated sulfuric acid is 1:2 to 1:3.

6. The preparation method of cerium sulfate chelated sulfur dioxide as claimed in claim 2 , characterized in that the dilute sulfuric acid is diluted from concentrated sulfuric acid to a 30% by mass sulfuric acid aqueous solution.

7. A method of preparing cerium sulfate chelated sulfur dioxide comprising:
adding anhydrous cerium sulfate to dilute sulfuric acid;
adding a solvent followed by refluxing at a predetermined temperature for a predetermined period;
heating a reaction product to remove the solvent, then cooling to about 20° C.;
adding dilute sulfuric acid to allow precipitation of crystals;
cooling down the product;
inducing suction, filtration; and
washing the crystals by the solvent to create crude cerium sulfate chelated sulfur oxide.

8. The method as claimed in claim 7 , wherein the predetermined temperature is about 45° C.-50° C.

9. The method as claim in claim 7 , wherein the predetermined period is about 2.0 hours to 2.5 hours.

10. The method as claimed in claim 7 , further comprising:
adding dilute sulfuric acid to the crude cerium sulfate chelated sulfur dioxide for recrystallization;
cooling the product followed by suction filtration; and
drying the product under vacuum to obtain a pure cerium sulfate chelated sulfur dioxide crystallized product.

11. The method as claimed in claim 7 , wherein the solvent is methanol.

12. The method as claimed in claim 7 , wherein the dilute sulfuric acid is diluted from concentrated sulfuric acid to about 30% by mass sulfuric acid aqueous solution.

13. The method as claimed in claim 7 , wherein a mass ratio of the anhydrous cerium sulfate to the concentrated sulfuric acid is about 1:2 to 1:3.

14. The method as claimed in claim 7 , wherein the cerium sulfate chelated sulfur dioxide is used as a titrant in determining the content of titanium, iron or antimony.

15. The method as claimed in claim 7 , wherein the cerium sulfate chelated sulfur dioxide is a white crystal.

Assignees

• Univ South China Normal

Inventors

• Huang Ruqiang
• Wang Qian
• Wang Guanghua
• Wang Jinghui
• Gao Linlin
• Zhang Jingwen

Classifications

• C01F17/282 Primary

  Sulfates · CPC title

• C01P2002/76

  by a space-group or by other symmetry indications · CPC title

• C01P2002/84

  by UV- or VIS- data · CPC title

• C01P2002/82

  by IR- or Raman-data · CPC title

• C01P2002/88

  by thermal analysis data, e.g. TGA, DTA, DSC · CPC title