Method for removing impurity mercury from crude selenium

Patent metadata

Field	Value
Publication number	US-2024375956-A1
Application number	US-202218691363-A
Country	US
Kind code	A1
Filing date	Mar 24, 2022
Priority date	Sep 13, 2021
Publication date	Nov 14, 2024
Grant date	—

Abstract

Disclosed is a method for removing impurity mercury from crude selenium. The method includes: mixing a vulcanizing agent with a crude selenium slag that is crushed to not more than 200 mesh uniformly, and performing briquetting to obtain a mixed material; adding the mixed material into a sealed furnace, and subjecting the mixed material to vulcanization by heating under an inert atmosphere to obtain a vulcanized selenium; subjecting the vulcanized selenium to primary vacuum distillation, such that selenium is converted into a gas phase and collected in a form of a volatile, and generated mercury sulfide and valuable elements are enriched in a resulting residue; and subjecting the selenium to secondary distillation to further remove mercury.

First claim

1 . A method for removing impurity mercury from crude selenium, comprising the following steps:
mixing a vulcanizing agent with a crude selenium slag that is crushed uniformly, and performing briquetting to obtain a mixed material; and adding the mixed material into a sealed furnace, and subjecting the mixed material to vulcanization by heating under an inert atmosphere to obtain a vulcanized selenium; subjecting the vulcanized selenium to primary vacuum distillation, such that selenium is converted into a gas phase and collected in a form of a volatile, and generated mercury sulfide and valuable elements are enriched in a resulting residue; and subjecting the selenium to secondary distillation.

2 . The method for removing impurity mercury from crude selenium according to claim 1 , wherein the crude selenium slag is crushed to a particle size of not more than 200 mesh, and the briquetting is conducted at a pressure of 4 MPa to 8 MPa.

3 . The method for removing impurity mercury from crude selenium according to claim 1 , wherein during the vulcanization, a molar ratio of mercury to the vulcanizing agent is in a range of 1:10 to 1:20; and the vulcanizing agent is selected from the group consisting of elemental sulfur and a sulfide.

4 . The method for removing impurity mercury from crude selenium according to claim 3 , wherein the sulfide is selected from the group consisting of sodium sulfide, ferric sulfide, and ferrous disulfide.

5 . The method for removing impurity mercury from crude selenium according to claim 1 , wherein the vulcanization by heating under an inert atmosphere is conducted at a temperature of 150°° C. to 300°° C. for 15 min to 60 min, with a heating rate of 5° C./min to 25° C./min.

6 . The method for removing impurity mercury from crude selenium according to claim 1 , wherein the vulcanization by heating is conducted with a heating rate of 5° C./min to 15° C./min.

7 . The method for removing impurity mercury from crude selenium according to claim 1 , wherein the vulcanization by heating under the inert atmosphere is conducted at a temperature of 200°° C. to 250° C. for 30 min to 45 min.

8 . The method for removing impurity mercury from crude selenium according to claim 1 , wherein the primary vacuum distillation is conducted at a temperature of 240° C. to 280° C. and a pressure of 1 Pa to 30 Pa for 20 min to 100 min, with a heating rate of 5° C./min to 25° C./min.

9 . The method for removing impurity mercury from crude selenium according to claim 1 , wherein the primary vacuum distillation temperature is conducted with a heating rate of 5° C./min to 15° C./min.

10 . The method for removing impurity mercury from crude selenium according to claim 1 , wherein the primary vacuum distillation is conducted at a temperature of 260°° C. to 280° C. and a pressure of 10 Pa to 20 Pa for 40 min to 80 min.

11 . The method for removing impurity mercury from crude selenium according to claim 1 , wherein the secondary distillation is a secondary vacuum distillation.

12 . The method for removing impurity mercury from crude selenium according to claim 11 , wherein the secondary vacuum distillation is conducted at a temperature of 200°° C. to 250° C. and a pressure of 1 Pa to 10 Pa for 30 min to 60 min, with a heating rate of 5° C./min to 25° C./min.

13 . The method for removing impurity mercury from crude selenium according to claim 11 , wherein the secondary vacuum distillation is conducted at a temperature of 220° C. to 230° C. and a pressure of 5 Pa to 10 Pa for 40 min to 50 min, with a heating rate of 10° C./min to 15° C./min.

14 . The method for removing impurity mercury from crude selenium according to claim 1 , wherein the crude selenium slag has Se with a mass fraction of 90% to 97%, Hg with a mass fraction of 3,200 ppm, and Pb with a mass fraction of 2% to 2.5%.

15 . The method for removing impurity mercury from crude selenium according to claim 5 , wherein the vulcanization by heating is conducted with a heating rate of 5° C./min to 15° C./min.

16 . The method for removing impurity mercury from crude selenium according to claim 5 , wherein the vulcanization by heating under the inert atmosphere is conducted at a temperature of 200°° C. to 250° C. for 30 min to 45 min.

17 . The method for removing impurity mercury from crude selenium according to claim 8 , wherein the primary vacuum distillation temperature is conducted with a heating rate of 5° C./min to 15° C./min.

18 . The method for removing impurity mercury from crude selenium according to claim 8 , wherein the primary vacuum distillation is conducted at a temperature of 260° C. to 280° C. and a pressure of 10 Pa to 20 Pa for 40 min to 80 min.

19 . The method for removing impurity mercury from crude selenium according to claim 12 , wherein the secondary vacuum distillation is conducted at a temperature of 220° C. to 230° C. and a pressure of 5 Pa to 10 Pa for 40 min to 50 min, with a heating rate of 10° C./min to 15° C./min.

Assignees

• Univ Kunming Science & Technology

Inventors

• Xu Baoqiang
• Luo Huan
• Yang Bin
• Jiang Wenlong
• Liu Lang
• Zha Guozheng
• Xiong Heng
• Tian Yang
• Kong Lingxin
• Li Yifu
• Wang Fei
• Yang Jia
• Qu Tao
• Liu Dachun

Classifications

• B01D3/143

  by two or more of a fractionation, separation or rectification step · CPC title

• B01D3/10

  Vacuum distillation (B01D3/12 takes precedence) · CPC title

• C01B19/02 Primary

  Elemental selenium or tellurium · CPC title

• Y02P10/20

  Recycling · CPC title