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Preparation method of sulfated zirconia

A technology of zirconium oxide and zirconium hydroxide, applied in chemical instruments and methods, catalyst activation/preparation, chemical/physical processes, etc., can solve problems such as high pollution, high corrosion, and use restrictions, and achieve good technical effects. The effect of increasing the sulfur content and increasing the specific surface area

Pending Publication Date: 2020-05-05
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The early acidic catalysts were based on HF, H 2 SO 4 Such liquid acids are used as catalysts. This type of catalyst is still used in some industrial reactions. Due to the defects of high corrosion, high pollution, and high cost of separation and treatment, the use of this type of liquid acid is increasingly restricted.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh zirconium oxychloride (ZrOCl 2 ·8H 2 O) 64g, dissolved in 500mL deionized water, high-speed shear machine speed 15000rpm, drop 25% ~ 28% NH 3 ·H 2 O, to PH=10~11, stop the dropwise addition, continue to stir at high speed for 30min; age at room temperature; wash the precipitate repeatedly with deionized water to make the pH=6~7, and use 0.1mol / L AgNO 3 Solution detection Cl-free - residue, dried in an oven, and ground into fine powder; impregnated zirconium hydroxide fine powder with 0.5mol / L dilute sulfuric acid in a high-speed shearing machine at 2000rpm; filtered, dried, and roasted at 650°C for 5h to obtain SO 4 2- / ZrO 2 . The measured specific surface area is 288m 2 / g, sulfur content 1.43%.

Embodiment 2

[0025] Weigh zirconium oxychloride (ZrOCl 2 ·8H 2 O) 64g, dissolved in 500mL deionized water, high-speed shear machine speed 11000rpm, drop 25% ~ 28% NH 3 ·H 2 O, to PH=10~11, stop the dropwise addition, continue to stir at high speed for 30min; age at room temperature; wash the precipitate repeatedly with deionized water to make the pH=6~7, and use 0.1mol / L AgNO 3 Solution detection Cl-free - residue, dried in an oven, and ground into fine powder; impregnated zirconium hydroxide fine powder with 0.3mol / L dilute sulfuric acid at a high speed shearing machine at 1000rpm; filtered, dried, and roasted at 550°C for 3h to obtain SO 4 2- / ZrO 2 . The measured specific surface area is 258m 2 / g, sulfur content 1.04%.

Embodiment 3

[0027] Weigh zirconium oxychloride (ZrOCl 2 ·8H 2 O) 64g, dissolved in 500mL deionized water, high-speed shear machine speed 13000rpm, drop 25% ~ 28% NH 3 ·H 2 O, to PH=10~11, stop the dropwise addition, continue to stir at high speed for 30min; age at room temperature; wash the precipitate repeatedly with deionized water to make the pH=6~7, and use 0.1mol / L AgNO 3 Solution detection Cl-free - residue, dried in an oven, and ground into fine powder; impregnated zirconium hydroxide fine powder with 0.7mol / L dilute sulfuric acid at a speed of 3000rpm in a high-speed shearing machine; filtered, dried, and roasted at 650°C for 5h to obtain SO 4 2- / ZrO 2 . The measured specific surface area is 278m 2 / g, sulfur content 1.33%.

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Abstract

The invention relates to a preparation method of sulfated zirconia. The method comprises the following steps: preparing a zirconium oxychloride aqueous solution with a certain concentration, adjustingthe pH value to 10-11 with concentrated ammonia water to obtain a zirconium hydroxide precipitate, repeatedly washing until no chloride ion is detected, drying, impregnating with a dilute sulfuric acid solution with a certain concentration, filtering, drying, and roasting to obtain sulfated zirconia. Sulfated zirconia belongs to solid superacid and has excellent catalytic performance in the aspects of conversion and utilization of biodiesel, isomerization of n-butane and the like.

Description

technical field [0001] The invention relates to a preparation method of sulfuric acid zirconia, which belongs to the field of preparation of solid super acid. Background technique [0002] With the continuous emphasis on the environment in China, the environmental protection standards in the chemical and oil refining industries are becoming increasingly stringent. Currently, acidic catalysts are used in many industrial reactions and occupy an important position. The early acidic catalysts were based on HF, H 2 SO 4 Such liquid acids are used as catalysts. This type of catalyst is still used in some industrial reactions. Due to the defects of high corrosion, high pollution, and high cost of separation and treatment, the use of this type of liquid acid is increasingly restricted. [0003] The industry is in urgent need of new green environmental protection catalysts to replace, and solid acid catalysts have the following advantages in industrial applications: first, continu...

Claims

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Application Information

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IPC IPC(8): B01J27/053B01J37/02B01J37/03B01J35/10
CPCB01J27/053B01J37/0201B01J37/031B01J35/615
Inventor 马夏坪金照生吕建刚周海春孙兰萍
Owner CHINA PETROLEUM & CHEM CORP
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