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Coarse-grained sphere-like zirconium hydroxide with large specific surface area and preparation method of zirconium hydroxide

A technology of zirconium hydroxide and spherical shape, which is applied in chemical instruments and methods, inorganic chemistry, zirconium compounds, etc., can solve the problems of increased osmotic pressure and unfavorable hemodialysis, and achieve lower osmotic pressure, uniform particle size, and less impurity content Effect

Active Publication Date: 2016-04-20
JIANGXI KINGAN HI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing literature shows that zirconium hydroxide is mainly prepared by ammonia precipitation method. Although nano-scale powder zirconium hydroxide with large specific surface area can be prepared, when nano-powder is used as a dialysis material, it is easy to unite and increase the osmotic pressure. Good for hemodialysis

Method used

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  • Coarse-grained sphere-like zirconium hydroxide with large specific surface area and preparation method of zirconium hydroxide
  • Coarse-grained sphere-like zirconium hydroxide with large specific surface area and preparation method of zirconium hydroxide
  • Coarse-grained sphere-like zirconium hydroxide with large specific surface area and preparation method of zirconium hydroxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Prepare a 0.5mol / L zirconium oxychloride solution, add a dispersant sodium dodecylsulfonate, the mass ratio of the dispersant to zirconium oxychloride is 1:10000, settle for 0.5h and filter, The filtrate is ready for use;

[0022] (2), press Zr 4+ with SO 4 2- The molar ratio of the substances is 1:1 ratio and the solid sodium sulfate is added to the filtrate to react;

[0023] (3) After it fully reacts to form a sulfur-zirconium complex, add solid sodium hydroxide at 15°C, control the pH value at the end of the reaction at 7, and then age at 60°C for 24h;

[0024] (4) After the aging, directly filter the mixture at 60°C, and wash the filter residue 4 times with 3‰ (mass percent concentration) NaOH solution at 60°C;

[0025] (5) Add water to the filter residue and water at a ratio of 1:1 to make a slurry, and adjust the pH value of the slurry to 5.0 with 0.5mol / L dilute citric acid at 30°C. The filter residue was washed 4 times with water, and then dried at 120...

Embodiment 2

[0027] (1) Prepare a 0.8mol / L zirconium oxychloride solution, add polyethylene glycol as a dispersant, the mass ratio of dispersant to zirconium oxychloride is 1:1000, filter after settling for 1 hour, and use the filtrate for later use;

[0028] (2), press Zr 4+ with SO 4 2- The molar ratio of the substances is 1:1.2, and the concentrated sulfuric acid containing 98wt% is added to the zirconium oxychloride solution for reaction;

[0029] (3) After the sulfur-zirconium complex is fully reacted, add potassium hydroxide solid at 60°C, control the pH value at the end of the reaction at 10, and then age the mixture at 100°C for 1 hour;

[0030] (4) After the aging, control the mixture at 70°C and then filter it with suction, and wash the filter residue 3 times with 70°C 2‰ (mass percent concentration) NaOH solution;

[0031] (5) Add water to the filter residue and water at a ratio of 1:2 to make a slurry, and adjust the pH of the slurry to 4 with a mixed acid containing 2 mol o...

Embodiment 3

[0033] (1) Prepare a 1.5mol / L zirconium oxychloride solution, and add a dispersant sodium polyacrylate, the mass ratio of the dispersant to zirconium oxychloride is 1:100, settle for 3 hours and filter, and the filtrate is ready for use;

[0034] (2), press Zr 4+ with SO 4 2- The molar ratio of the substances is 1:1.1 and the mixed solution of 2mol / L magnesium sulfate and 2mol / L sodium sulfate is added to the zirconium oxychloride solution for reaction;

[0035] (3) Add a mixed solution of 2mol / L NaOH and 2mol / L KOH at 40°C after it fully reacts to form a sulfur-zirconium complex, control the pH value at the end of the reaction at 12, and then age the mixed solution at 120°C for 6h ;

[0036] (4) After aging, control the mixture to cool to 100°C and then filter it with suction, and wash the filter residue 5 times with 90°C 1‰ (mass percent concentration) NaOH solution;

[0037] (5) Add water to the filter residue and water at a ratio of 1:4 to make a slurry, and adjust the...

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Abstract

The invention discloses coarse-grained sphere-like zirconium hydroxide with large specific surface area. Zirconium hydroxide adopts a sphere-like structure in shape, the grain size D10 is larger than or equal to 8 mu m, the diameter D50 is larger than or equal to 30 mu m and smaller than or equal to 40 mu m, the diameter D90 is smaller than or equal to 80 mu m, the specific surface area is larger than or equal to 550 m<2> / g, the pore volume is 0.20-0.25 cm<3>, the pore diameter is 2.0-2.4 nm, and the phosphorus / sulfur dynamic adsorption capacity of zirconium hydroxide is larger than 1 mmol / g. The invention further provides a preparation method of coarse-grained sphere-like zirconium hydroxide with the large specific surface area. According to the method, zirconium oxychloride reacts with SO4<2->, a product reacts with potassium hydroxide or sodium hydroxide, and zirconium hydroxide is directly prepared; ammonium ions are avoided effectively, and the prepared product contains few impurities and is uniform in grain size, large in specific surface area and high in activity. With adoption of the coarse-grained sphere-like structure, the product can be applied to phosphorous removal through dynamic adsorption for hemodialysis and can effectively reduce osmotic pressure.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis of zirconium hydroxide, in particular to zirconium hydroxide with coarse grain size and large specific surface area and a preparation method thereof. Background technique [0002] Uremia is a chronic renal failure in which metabolic acidosis and water and electrolyte balance disorders occur in patients. Among them, metabolic acidosis refers to the retention of acid substances such as phosphoric acid in the blood due to metabolic disorders. Excessive phosphorus content in the blood can cause phosphorus and calcium metabolism disorders, excessive phosphorus and calcium deficiency, which is called hyperphosphatemia in medicine. At present, the main treatment method for uremia patients is to go to the hospital regularly for hemodialysis to maintain life. At present, the hemodialysis instrument uses the principle of semi-permeable membrane to purify the blood through diffusion, removing va...

Claims

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Application Information

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IPC IPC(8): C01G25/00
CPCC01G25/00C01P2004/03C01P2004/32C01P2004/51C01P2004/61C01P2006/12C01P2006/14C01P2006/16C01P2006/82
Inventor 李春邱才华陈孝伟陈双华陈浪
Owner JIANGXI KINGAN HI TECH
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