Process for synthesizing calcium zirconate by liquid-phase and solid-phase mixed calcination method

A solid-phase calcining method and liquid-phase mixing technology, applied in zirconium compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of high equipment requirements, unrealistic large-scale production, and high cost, and achieve short production process flow and operation. Easy control and high product quality effect

Inactive Publication Date: 2011-04-06
JIANGXI KINGAN HI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The solid-phase high-temperature synthesis method generally uses zirconia and calcium oxide as raw materials with a molar ratio of 1:1 for mechanical mixing, and then calcines the materials at a high temperature of 1400°C-1700°C; this method not only has high energy consumption, but also has a particle size distribution Wide, weak activity
The hydrothermal method is to mix calcium salt or calcium hydroxide with zirconium oxychloride (molar ratio 2:1), adjust the pH>12 with KOH, put it into the reactor for a certain period of time, filter and wash, dry and calcinate (900°C- 1200℃) the quality of the calcium zirconate prepared is very good, but the requirements for the equipment are too high, the material waste is large, the cost is too high, and the scale production is unrealistic
Co-precipitation method is based on (NH 4 ) 2 C 2 o 4 Precipitated calcium, with NH 3 ·H 2 O precipitates zirconium to obtain mixed materials, which are also washed, dried and calcined, which is cumbersome and expensive.
From the current overall preparation method of calcium zirconate, it can be attributed to: high energy consumption, complicated operation, large amount of waste water, uneven particles, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] In the first step, put 20L of purified water into a 50L reactor and start stirring; in the second step, put 10KgZBC (39.5%ZrO 2 ) and 3.25Kg calcium carbonate (55.5%CaO) were put into the reaction kettle and stirred for 30 minutes; the third step was to put the slurry directly into the centrifuge for centrifugal dehydration for 5 minutes; the fourth step was to determine the water content of the material after preliminary dehydration 40%-50%, put it into a quartz crucible, send it into a tunnel kiln, and control the central temperature at 950°C-970°C; step 5, discharge after 16 hours, cool, ball mill for 30 minutes, and pack to get the finished product.

Embodiment 2

[0011] In the first step, put 22L of purified water into a 50L reactor and start stirring; in the second step, 10KgZBC (40.2%ZrO 2 ) and 3.3Kg calcium carbonate (55.5% CaO) were put into the reaction kettle and stirred for 40 min; in the third step, the slurry was directly put into the centrifuge for centrifugal dehydration for 15 min; in the fourth step, the water content of the material after preliminary dehydration was 45 %, put it into a quartz crucible, send it into a tunnel kiln, and control the central temperature at 930°C-960°C; the fifth step is to discharge the material after 17 hours, cool it, and ball mill it for 50 minutes, and then pack it to get the finished product.

Embodiment 3

[0013] In the first step, put 18L of purified water into a 50L reactor and start stirring; in the second step, put 10KgZOH (40.6%ZrO 2 ) and 3.3Kg calcium carbonate (55.8%CaO) were put into the reaction kettle and stirred for 32 min; the third step, the slurry was directly put into the centrifuge for centrifugal dehydration; the fourth step, the water content of the material after preliminary dehydration was 50 %, put it into a quartz crucible, send it into a tunnel kiln, and control the central temperature at 900°C-940°C; the fifth step, discharge after 20h, cool and pack to obtain the finished product.

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PUM

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Abstract

The invention relates to a process for synthesizing calcium zirconate by a liquid-phase and solid-phase mixed calcination method. The process comprises the following steps of: 1, mixing zirconium carbonate or zirconium hydroxide and CaCO3 or Ca (OH) 2 in a metallic oxide molar ratio of 1:1.0-1.2 by using refined water; 2, performing centrifugal separation and dehydration on the slurry; 3, loading the dehydrated mixture into a quartz crucible, feeding the quartz crucible into a tunnel kiln of which the central highest temperature is between 850 and 1,200 DEG C, and slowly warming up; and 4, discharging, cooling, crushing, and packing to obtain finished products. The moisture content of the dehydrated materials is between 40 and 50 percent. By the process, the defects of nonuniform mixing, incomplete reaction, nonuniform particles and super high energy consumption by a dry method are overcome, and the process problems of difficulty in cleaning impurities, a large amount of wastewater, drying and the like by a wet method are solved. The whole production process has short flow and simple equipment, is easy to operate and control, is suitable for large-scale production, and has high product quality and lower cost.

Description

technical field [0001] The invention relates to a synthesis process of calcium zirconate, in particular to a process for synthesizing calcium zirconate by a liquid-phase mixed solid-phase calcination method. Background technique [0002] At present, the preparation methods of calcium zirconate mainly include solid-phase high-temperature synthesis. [3-4] ,Hydrothermal [5] and co-precipitation [6-7] . The solid-phase high-temperature synthesis method generally uses zirconia and calcium oxide as raw materials with a molar ratio of 1:1 for mechanical mixing, and then calcines the materials at a high temperature of 1400°C-1700°C; this method not only has high energy consumption, but also has a particle size distribution Broad, weak activity. The hydrothermal method is to mix calcium salt or calcium hydroxide with zirconium oxychloride (molar ratio 2:1), adjust the pH>12 with KOH, put it into the reactor for a certain period of time, filter and wash, dry and calcinate (900°...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/00
Inventor 罗方承董雪平邱才华吴江陈忠锡
Owner JIANGXI KINGAN HI TECH
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