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

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

Inactive Publication Date: 2012-11-07
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

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 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 and 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 pearlescent luster; 4) heat the zinc oxalate powder in a tubular calciner to 420°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.

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 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 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 oxide fine powder with pearlescent luster, in particular, using oxalate as a precipitating agent to controlly precipitate soluble zinc salt into tablets under the action of citrate and other dispersants. Zinc oxalate with pearlescent luster and zinc oxide micropowder with pearlescent luster after 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 characteristics become the main control indicators. Around t...

Claims

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Application Information

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