Preparation method of basic zirconium carbonate

A zirconium carbonate and basic technology, which is applied in the field of compound synthesis, can solve the problems of inability to realize industrial production, decomposition of basic zirconium carbonate, poor product consistency, etc., and achieve the effect of large output, high product activity and high solution concentration

Inactive Publication Date: 2014-01-01
JIANGXI KINGAN HI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because it is a solid phase reaction, the consistency of the product is poor, the activity is poor, and the reaction is an exothermic reaction, such as a large batch reaction, which will cause local overheating and cause the decomposition of basic zirconium carbonate, which cannot realize industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A kind of preparation method of basic zirconium carbonate, its processing step is:

[0018] a, the anhydrous sodium sulfate is made into the solution that mass ratio is 31.2%, the pH value of adjusting sodium sulfate solution with sodium hydroxide solution is 8, after settling for 0.5h, filter, and filtrate is standby;

[0019] b. Make zirconium oxychloride into a solution with a mass concentration of 282g / L. After heating the zirconium oxychloride solution to 73°C, add sodium sulfate solution while heating to keep the system temperature at 58-60°C. During the reaction The weight ratio of anhydrous sodium sulfate to zirconium oxychloride is 1:1.8;

[0020] c. After adding the sodium sulfate solution, raise the temperature to 88-90°C and keep it warm for 1h;

[0021] d. After the heat preservation is over, lower the temperature of the system to 50°C, and then add sodium bicarbonate solution to keep the system temperature at 50-55°C. After adding sodium bicarbonate, rais...

Embodiment 2

[0024] A kind of preparation method of basic zirconium carbonate, its processing step is:

[0025] a, the anhydrous sodium sulfate is made into the solution that mass ratio is 28%, the pH value of adjusting sodium sulfate solution with sodium hydroxide solution is 7, after settling for 1h, filter, and filtrate is standby;

[0026] b. Make zirconium oxychloride into a solution with a mass concentration of 301g / L. After heating the zirconium oxychloride solution to 80°C, add sodium sulfate solution while heating to keep the system temperature at 55-60°C. During the reaction The weight ratio of anhydrous sodium sulfate to zirconium oxychloride is 1:2;

[0027] c. After adding the sodium sulfate solution, raise the temperature to 85-90°C and keep it warm for 1.5h;

[0028] d. After the heat preservation is over, lower the temperature of the system to 55°C, and then add sodium bicarbonate solution to keep the system temperature at 55-60°C. After adding sodium bicarbonate, raise th...

Embodiment 3

[0031] A kind of preparation method of basic zirconium carbonate, its processing step is:

[0032] a, anhydrous sodium sulfate is made into the solution that mass ratio is 32%, the pH value of adjusting sodium sulfate solution with sodium hydroxide solution is 9, after settling for 0.75h, filter, and filtrate is standby;

[0033] b. Make zirconium oxychloride into a solution with a mass concentration of 320g / L. After heating the zirconium oxychloride solution to 85°C, add sodium sulfate solution while heating to keep the system temperature at 60-65°C. During the reaction The weight ratio of anhydrous sodium sulfate to zirconium oxychloride is 1:2.5;

[0034] c. After adding the sodium sulfate solution, raise the temperature to 85-90°C and keep it warm for 2 hours;

[0035] d. After the heat preservation is over, lower the temperature of the system to 65°C, and then add sodium bicarbonate solution to keep the system temperature at 60-65°C. After adding sodium bicarbonate, r...

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Abstract

The invention provides a preparation method of basic zirconium carbonate. The method comprises the following technical steps: a, adjusting the pH value of sodium sulfate liquor to be greater than 7, and settling for 0.5-5 hours and filtering, wherein the filtrate is for later use; b, preparing zirconium oxychloride into liquor with concentration of 280-320g / L, and adding the sodium sulfate liquor while heating after heating the zirconium oxychloride liquor to a temperature which is not lower than 70 DEG C, wherein the weight ratio of anhydrous sodium sulfate to zirconium oxychloride in reaction is 1:(1-4); c, after adding the sodium sulfate liquor, heating to 70-95 DEG C and insulating for 0.5-5 hours; d, after insulation, cooling the temperature of the system to 30-70 DEG C, then adding sodium hydrogen carbonate liquor, and heating the system to 60-90 DEG C and continuously insulating for 0.5-5 hours, wherein the weight ratio of anhydrous sodium sulfate to sodium hydrogen carbonate is 1:(0.8-3); e, after insulation, filtering, washing sulfate radicals by water till being qualified, preparing the material to slurry, dropwise adding acid with the acidity of 0.5-10N till the pH of the system is within 2-6, maintaining for 0.5-3 hours and filtering, washing for 3-7 times and centrifugalizing to obtain the basic zirconium carbonate. Compared with other methods, the method provided by the invention is high in product activity, high in concentration of liquor, great in output and high in yield.

Description

technical field [0001] The invention belongs to the field of compound synthesis, in particular to a preparation method of basic zirconium carbonate. Background technique [0002] Basic zirconium carbonate is the main raw material of organic zirconium salts and other zirconium products. It is widely used in cosmetics, paper chemicals, automobile purification treatment and paint additives and other industries. Due to the different methods and process conditions for preparing basic zirconium carbonate, the molar ratio of zirconium dioxide to carbon dioxide in its molecular formula varies between 4:1 and 1:1. At present, there are mainly one-step synthesis method, two-step synthesis method and solid-phase synthesis method for basic zirconium carbonate. [0003] Chinese patent application 01821766.4 "Sodium Zirconium Carbonate Basic and Zirconium Carbonate Basic and Preparation Method" is a one-step synthesis method in which zirconium oxychloride is mixed with soda ash and then ...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): C01G25/00
Inventor邱才华吴江陈忠锡张尚谌美玲
OwnerJIANGXI KINGAN HI TECH