Method for preparing zinc oxalate with pearl luster and zinc oxide powder with pearl luster

A technology of zinc oxide powder and zinc oxalate, which is applied in carboxylate preparation, zinc oxide/zinc hydroxide, organic chemistry, etc., can solve the problems of no pearly luster and harsh conditions, and achieve excellent UV shielding effect

Inactive Publication Date: 2011-08-24
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods mostly use hydrothermal crystallization or high-temperature reduction, and the conditions are relatively harsh. Although the flaky zinc oxide powder is obtained, the appearance of pearlescent color is not observed.

Method used

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  • Method for preparing zinc oxalate with pearl luster and zinc oxide powder with pearl luster
  • Method for preparing zinc oxalate with pearl luster and zinc oxide powder with pearl luster
  • Method for preparing zinc oxalate with pearl luster and zinc oxide powder with pearl luster

Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach 1

[0016] 1) Take 100ml of 0.05mol / L zinc nitrate solution and store it in the reactor, add 0.1g / L citric acid, start stirring, and adjust its pH=2.5; 2) Take 100ml of 0.06mol / L ammonium oxalate solution , adjust the pH=6.0; 3) Put the above two solutions into the reactor at a speed of 2mL / min and drop them into the reactor. After washing 4-5 times, send it to a drying oven for drying to obtain a flake zinc oxalate powder product with pearlescent luster; 4) heat the zinc oxalate powder in a tubular calciner to 480°C for 1 After one hour, take it out and air-cool it directly to obtain flaky zinc oxide powder with pearlescent luster. The morphology and other characteristics of the powder were characterized by a scanning electron microscope (JEOL JSM-5600LV type), see attached figure 1 with 2 .

Embodiment approach 2

[0018] 1) Take 100ml of 0.10mol / L zinc nitrate solution and store it in the reactor, add 0.3g / L sodium citrate, start stirring, and adjust its pH=2.5; 2) Take 100ml of 0.12mol / L ammonium oxalate solution, adjust the pH=6.0; 3) The above two solutions are dripped into the reactor at a speed of 2mL / min. Repeated washing 4-5 times, sent to drying oven to dry, you can get flake zinc oxalate powder product with pearl luster; 4) heat the zinc oxalate powder in a tubular calciner to 420°C After 1 hour, take it out and air-cool directly to obtain flaky zinc oxide powder with pearlescent luster. The morphology and other characteristics of the powder are similar to those of Embodiment 1.

Embodiment approach 3

[0020]1) Take 100ml of 0.20mol / L zinc nitrate solution and store it in the reactor, add 0.35g / L ammonium citrate, start stirring, and adjust its pH=3.0; 2) Take 100ml of 0.24mol / L ammonium oxalate solution, adjust the pH=7.0; 3) The above two solutions are dripped into the reactor at a speed of 5mL / min. Repeated washing 4-5 times, sent to the drying oven to dry, you can get flaky zinc oxalate powder product with pearl luster; 4) Heat the zinc oxalate powder in a tubular calciner to 450°C for heat preservation After 1 hour, take it out and air-cool directly to obtain flaky zinc oxide powder with pearlescent luster. The morphology and other characteristics of the powder are similar to those of Embodiment 1.

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Abstract

The invention belongs to the field of inorganic materials, and relates to a method for preparing zinc oxalate with pearl luster and zinc oxide microfine powder with pearl luster. The method comprises the following steps of: (1) storing 100ml of solution of zinc nitrate at the concentration of 0.05 and 0.20mol/L in a reactor, adding citric acid or citrate at the concentration of between 0.05 and 0.50g/L, stirring, and regulating the pH value to be between 1.5 and 5.0; (2) taking 100ml of solution of ammonium oxalate at the concentration of between 0.06 and 0.24mol/L, and regulating the pH value to be between 5.0 and 7.0; (3) dripping the two kinds of solution into the reactor at the speed of between 2 and 10mL/min, continuing to stir and age for 30 minutes after feed liquid is added, immediately performing centrifugal separation or suction filtration separation, repeatedly washing for 4 to 5 times, and drying in a drying oven to obtain a flaky zinc oxalate powder product with pearl luster; and (4) heating a tubular calcination furnace to raise the temperature of the zinc oxalate powder in the furnace to the temperature above 380 DEG C, keeping the temperature for 1 hour, and directly taking the zinc oxalate powder out for air cooling to obtain flaky zinc oxide powder with pearl luster. The flaky ZnO prepared by the method may have a more excellent ultraviolet shielding function; and due to a unique pearlized effect of the flaky ZnO, the flaky ZnO may be developed into a novel sunscreen product which integrates beauty and practicability into a whole, or is taken as a matrix material to be subjected to treatment such as doping, coating and the like so as to form a novel pearl pigment.

Description

technical field [0001] The invention belongs to the field of inorganic materials, and relates to a method for preparing zinc oxalate and zinc oxide fine powders with pearlescent luster, especially using oxalate as a precipitating agent to control the soluble zinc salt under the action of citrate and other dispersants. A method of depositing zinc oxalate in flake form and emitting a remarkable pearlescent luster and zinc oxide micropowder with pearlescent luster after being calcined and decomposed. Background technique [0002] Zinc oxide (ZnO) is an important semiconductor material, which has a wide range of applications in the fields of photocatalysis, sensitive ceramics, magnetic materials, cosmetics, coatings and pigments. The physical characteristics of ZnO powder, such as particle size and morphology, have a very important impact on the performance of its applied products. Therefore, in the process of powder preparation, its particle size and morphology and other charac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G9/02C07C55/07C07C51/41
Inventor 黄凯朱鸿民侯军刚焦树强王维
Owner UNIV OF SCI & TECH BEIJING
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