Dechlorination reagent Ng131 as well as preparation method and application thereof

Abstract

The invention discloses a dechlorination reagent Ng131 as well as a preparation method and application thereof. The dechlorination reagent Ng131 is prepared from the following raw materials: tri-octyl decyl alkyl tertiary amine, bismuth molybdate and pine oil. The method comprises the following steps of: reacting the raw materials of tri-octyl decyl alkyl tertiary amine, bismuth molybdate and pine oil according to a formula ratio for 1-4 hours at the oxygen pressure of 0.5-1.0 KPa and the temperature of 200-300 DEG C; the application is the application of the dechlorination reagent Ng131 in a copper sulfate solution defluorination process. The dechlorination reagent Ng131 is stable in chlorine removal performance under high-acid and high-temperature conditions, and has efficient dechlorination performance.

Description

Technical Field

[0001] This invention belongs to the field of metallurgical technology, specifically relating to a dechlorination reagent Ng131, its preparation method, and its application. Background Technology

[0002] Zinc sulfate is an important raw material for electrolytic zinc production and is widely used in metallurgy, chemical industry, and electronics. However, during the production process of zinc sulfate, chlorine impurities are often present, which affect the purity and quality of zinc sulfate, thus limiting its application range and market value. To improve the quality of zinc sulfate, it is essential to effectively remove chlorine. Therefore, developing a method to solve the above-mentioned technical problems is crucial. Summary of the Invention

[0003] The first objective of this invention is to provide a dechlorination reagent Ng131; the second objective is to provide a method for preparing the dechlorination reagent Ng131; and the third objective is to provide applications of the dechlorination reagent Ng131.

[0004] The first objective of this invention is achieved by preparing the dechlorination reagent Ng131 from raw materials trioctyldecyl tertiary amine, bismuth molybdate, and pine oil.

[0005] Its technical principle is as follows: 1. Dehydration condensation reaction of pine oil The hydroxyl groups in pine oil undergo dehydration condensation with the hydroxyl groups on the surface of bismuth molybdate, forming chemical bonds: Bi-OH + HO-R′→Bi-OR′+ H2O 2. Oxygen pressure crosslinking reaction Under oxygen pressure conditions, alkyl chains undergo oxidative coupling: 2R-H + [O] → RR + H2O The second objective of this invention is achieved by reacting the raw materials trioctyldecyl tertiary amine, bismuth molybdate, and pine oil in the formula ratio at an oxygen pressure of 0.5~1.0 kPa and a temperature of 200~300°C for 1~4 hours.

[0006] The third objective of this invention is achieved by the application of the dechlorination reagent Ng131 in the dechlorination process of zinc sulfate solution.

[0007] The dechlorination reagent Ng131 of this invention is prepared by reacting trioctyldecyl tertiary amine, bismuth molybdate, and pine oil at an oxygen pressure of 0.5-1.0 kPa and a temperature of 200-300℃ for 1-4 hours. After the reaction stops, a chlorine-removing precipitant, Ng131, is obtained. The molar ratio of the tertiary amine, bismuth molybdate, and pine oil is 1-5:1-10:20-100. This precipitant exhibits stable chlorine removal performance under high acid and high temperature conditions, demonstrating highly efficient dechlorination. By adding the aforementioned dechlorination reagent Ng131 and adjusting reaction conditions such as pH, temperature, and time, the efficiency and stability of chlorine removal can be improved, ultimately achieving an environmentally friendly and economically feasible treatment solution. Detailed Implementation

[0008] The present invention will be further described below with reference to embodiments, but this is not intended to limit the present invention in any way. Any modifications or substitutions made based on the teachings of the present invention shall fall within the protection scope of the present invention.

[0009] The dechlorination reagent Ng131 described in this invention is prepared from raw materials trioctyldecyl tertiary amine, bismuth molybdate, and pine oil.

[0010] The molar ratio of the trioctyldecyl tertiary amine, bismuth molybdate, and pine oil is (1~5):(1~10):(20~100).

[0011] The preparation method of the dechlorination reagent Ng131 of the present invention involves reacting the raw materials trioctyldecyl tertiary amine, bismuth molybdate and pine oil in the formula ratio at an oxygen pressure of 0.5~1.0 kPa and a temperature of 200~300℃ for 1~4 h.

[0012] The application of the dechlorination reagent Ng131 described in this invention is its application in the dechlorination process of zinc sulfate solution.

[0013] The zinc sulfate dechlorination process includes pretreatment and main reaction steps, specifically including: A. Pretreatment: Adjust the pH of the zinc sulfate solution to be treated to 1-3 to obtain material a; B. Main reaction: Add dechlorination reagent Ng131 to material a and stir to obtain dechlorinated zinc sulfate solution.

[0014] The chloride ion content in the zinc sulfate solution to be treated in step A is 0.5~0.7 g / L.

[0015] The amount of dechlorination reagent added in step B is 4.5~6.5 g / L.

[0016] In step B, the stirring speed for the reaction is 100~200 r / min.

[0017] The temperature for stirring the reaction in step B is 50~80℃.

[0018] The stirring reaction time in step B is 1-3 hours.

[0019] The present invention will be further described below with reference to specific embodiments: Example 1

[0020] The raw materials trioctyldecyl tertiary amine, bismuth molybdate, and pine oil in a molar ratio of 1:1:20 were reacted at an oxygen pressure of 0.5~0.8 kPa and a temperature of 200~220 °C for 5 h to obtain the target dechlorination reagent Ng131.

[0021] Example 2

[0022] The raw materials trioctyldecyl tertiary amine, bismuth molybdate, and pine oil in a molar ratio of 5:10:100 were reacted at an oxygen pressure of 0.8~1.0 kPa and a temperature of 280~300 °C for 2 h to obtain the target dechlorination reagent Ng131.

[0023] Example 3

[0024] The raw materials trioctyldecyl tertiary amine, bismuth molybdate, and pine oil in a molar ratio of 3:5:60 were reacted at an oxygen pressure of 0.6~0.8 kPa and a temperature of 220~240 °C for 3 h to obtain the target dechlorination reagent Ng131.

[0025] Example 4

[0026] The raw materials trioctyldecyl tertiary amine, bismuth molybdate, and pine oil in a molar ratio of 4:8:50 were reacted at an oxygen pressure of 0.7~0.9 kPa and a temperature of 220~260 °C for 4 h to obtain the target dechlorination reagent Ng131.

[0027] Example 5

[0028] The raw materials trioctyldecyl tertiary amine, bismuth molybdate and pine oil in a molar ratio of 3:7:80 were reacted at an oxygen pressure of 0.7~1.0 kPa and a temperature of 230~260 °C for 3 h to obtain the target dechlorination reagent Ng131.

[0029] Example 6

[0030] The raw materials trioctyldecyl tertiary amine, bismuth molybdate and pine oil in a molar ratio of 4:3:30 were reacted at an oxygen pressure of 0.6~0.8 kPa and a temperature of 210~230 °C for 4 h to obtain the target dechlorination reagent Ng131.

[0031] Example 7

[0032] The raw materials trioctyldecyl tertiary amine, bismuth molybdate and pine oil in a molar ratio of 2:9:70 were reacted at an oxygen pressure of 0.5~0.9 kPa and a temperature of 230~260 °C for 3 h to obtain the target dechlorination reagent Ng131.

[0033] Example 8

[0034] The raw materials trioctyldecyl tertiary amine, bismuth molybdate and pine oil in a molar ratio of 5:8:60 were reacted at an oxygen pressure of 0.6~0.8 kPa and a temperature of 200~230℃ for 3 h to obtain the target dechlorination reagent Ng131.

[0035] Example 9

[0036] The dechlorination reagent Ng131 prepared in Example 3 was used in the experiment, and the specific operation is as follows: Take 200 ml of zinc sulfate solution with a chloride ion content of 0.68 g / L, adjust the pH value to 2, add 4.5 g of the dechlorination reagent Ng131 prepared in Example 3, heat to 55~65℃, react for 2 h, and after the reaction is completed, separate the solid and liquid. The filter residue is bismuth oxychloride precipitate, and the chloride content in the filtrate is 36.82 mg / L, that is, the chloride removal rate in zinc sulfate solution is 94.23%.

[0037] Example 10

[0038] The dechlorination reagent Ng131 prepared in Examples 1, 2, 4, 5, 6, 7, and 8 were tested respectively, using the same method as in Example 9. The results showed that when 200 mL of zinc sulfate solution with a chloride ion content of 0.5-0.7 g / L was taken, the pH was adjusted to 1-3, 4.5-6.5 g of dechlorination reagent Ng131 was added with stirring, the temperature was raised to 50-80℃, and the reaction was allowed to proceed for 1-3 hours. After the reaction was completed, the solid and liquid were separated, and the filter residue was bismuth oxychloride precipitate. The chloride content in the filtrate was 30-40 mg / L, which means that the chloride removal rate in the zinc sulfate solution was 92.0-95.7%.

[0039] Comparative Example 1 Chinese patent CN108220599A discloses a method for self-purification and dechlorination of zinc sulfate solution, which involves 1m 3 Zinc electrolyte is added to the reaction tank, and Zn in the zinc electrolyte... 2+ Concentration of 56~g58 / L, Mn 7+ Concentration of 0.4~0.6 g / L, Cl -The concentration of the slag was 0.4~0.6 g / L, the concentration of suspended solids was 0.05~0.07 g / L, and the rest was impurities or water. Copper slag with a particle size of 180~325 mesh was selected, of which 60% was copper slag with a particle size of 325 mesh. The copper content in the copper slag was 45.03%, and the copper oxide content in the copper slag was 5~6%. 8.5 kg of fresh copper slag was slurried and added evenly to the reaction tank within 10 minutes. The temperature of the reaction tank was controlled at 30~40℃. The self-purification dechlorination reaction time was 2.5~3.5 h. Filtration was started 0.3 h after the start of the self-purification dechlorination reaction and ended when the reaction ended. The chloride ion content in the filtrate was 63.23 mg / L, and the chloride ion removal rate could only reach 84.58%.

Claims

1. A dechlorination reagent Ng131, characterized in that, The dechlorination reagent Ng131 is prepared from raw materials trioctyldecyl tertiary amine, bismuth molybdate and pine oil.

2. The dechlorination reagent Ng131 according to claim 1, characterized in that, The molar ratio of the trioctyldecyl tertiary amine, bismuth molybdate, and pine oil is (1~5):(1~10):(20~100).

3. A method for preparing the dechlorination reagent Ng131 according to claim 1 or 2, characterized in that, The raw materials, trioctyldecyl tertiary amine, bismuth molybdate, and pine oil, are reacted in the formula ratio at an oxygen pressure of 0.5~1.0 kPa and a temperature of 200~300℃ for 1~4 hours.

4. The application of the dechlorination reagent Ng131 according to claim 1 or 2, characterized in that, The application of the dechlorination reagent Ng131 in the dechlorination process of zinc sulfate solution.

5. The application according to claim 4, characterized in that, The zinc sulfate dechlorination process includes pretreatment and main reaction steps, specifically including: A. Pretreatment: Adjust the pH of the zinc sulfate solution to be treated to 1-3 to obtain material a; B. Main reaction: Add dechlorination reagent Ng131 to material a and stir to obtain dechlorinated zinc sulfate solution.

6. The application according to claim 5, characterized in that, The chloride ion content in the zinc sulfate solution to be treated in step A is 0.5~0.7 g / L.

7. The application according to claim 5, characterized in that, The amount of dechlorination reagent added in step B is 4.5~6.5 g / L.

8. The application according to claim 5, characterized in that, In step B, the stirring speed for the reaction is 100~200 r / min.

9. The application according to claim 5, characterized in that, The temperature for stirring the reaction in step B is 50~80℃.

10. The application according to claim 5, characterized in that, The stirring reaction time in step B is 1-3 hours.