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Method for producing high-grade zircon sand

A zircon sand, high-grade technology, applied in chemical instruments and methods, zirconium compounds, inorganic chemistry, etc., can solve the problem of high production costs, difficult environmental pollution control, and product quality that cannot meet the quality standards of high-purity zirconium oxychloride, etc. problems, to achieve the effect of high product quality, small footprint, and large operating load flexibility

Inactive Publication Date: 2016-04-20
郭志斌
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Zirconium oxychloride products are widely used and are the basic raw materials of zirconium chemical industry. The market demand is large. In 2014, it reached 240,000 tons. However, domestic zirconium oxychloride is produced by "alkali fusion method". Pollution control is very difficult, and the product quality cannot meet the quality standard of high-purity zirconium oxychloride

Method used

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  • Method for producing high-grade zircon sand
  • Method for producing high-grade zircon sand
  • Method for producing high-grade zircon sand

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] Method for producing high-grade zircon sand by submerging and burning zircon sand

[0075] 1. First add a certain concentration and a certain amount of fresh sulfuric acid liquid, recovered acid liquid and a certain amount of water into the acid mixing tank, mix to obtain 70% sulfuric acid, and then pump 70% sulfuric acid into the submerged combustion reactor Then add zircon sand, the liquid-solid ratio is 0.5:1, and then pass through natural gas combustion and heating to obtain the flue gas obtained after high-temperature combustion at 800-1000 ° C. The high-temperature flue gas passes through heat transfer with sulfuric acid in the reactor, and then Heat the zircon sand and sulfuric acid in the kettle, and adjust the temperature of the sulfuric acid by adjusting the intake of high-temperature combustion gas. According to the process requirements, first heat the sulfuric acid to 240°C-260°C, keep it warm for 2 hours, then heat it to 260°C-320°C, and keep it warm for 2 ...

Embodiment 2

[0097] Method for producing high-purity zirconium oxychloride

[0098] 1. Chlorination reaction

[0099] The raw material zircon sand, calcined petroleum coke and silicon carbide are added to the mixer according to the mass ratio of zircon sand: calcined coke: silicon carbide = 1:0.22:0.34, and the materials are mixed, and then added to the front of the furnace The silo is continuously fed into the chlorination furnace through a screw conveyor.

[0100] Chlorine gas produced by electrolysis of hydrochloric acid is fed into the bottom of the chlorination furnace, and the weight of the feed is zircon sand: chlorine gas = 1: 2.78, so that chlorine gas enters the reaction section through the distributor to react with raw materials, and the reaction temperature is controlled at 1170 ° C, and the furnace pressure is controlled. Within 3000Pa, at the same time determine the slag removal time of the chlorination furnace according to the furnace pressure, control the chlorine gas flow...

Embodiment 3

[0138] After the reaction in the reaction kettle in Example 1, the zircon sand is stirred and washed, filtered by a belt filter, and the filtered mother liquor is mixed with the primary mother liquor and the washing liquid for washing crystals in Example 2 and introduced into the mother liquor evaporator, and the mother liquor is evaporated by steam heating Evaporate the mother liquor, control the heating vapor pressure to 0.3-0.5MPa, the secondary pressure of the evaporator is at 0.2MPa-0.3MPa, evaporate to the zirconium dioxide concentration at 180-200g / l, and then follow the method described in the above-mentioned embodiment 2 Carry out crystallization, filtration, washing, re-dissolving the obtained crystals, evaporate and crystallize together with the solid hydrolyzate, filter, wash, and separate to obtain high-purity zirconium oxychloride products) to obtain zirconium oxychloride with a direct crystallization rate of more than 90% crystals.

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Abstract

The invention relates to a method for preparing zircon sand, in particular to a method for producing high-grade zircon sand. The method comprises the following steps: adding zircon sand and sulfuric acid at the mass ratio of (0.4-0.9): 1 into an immersion combustion reaction still; introducing smoke at 800-1000 DEG C after natural gas combustion to enable a chemical reaction to be carried out for 6-8 hours at 100-350 DEG C in the reaction still; removing impurities in the zircon sand; then carrying out stirring washing; filtering, washing and drying to obtain the high-grade zircon sand. High-purity zirconium oxychloride, gas-phase method silicon dioxide and high-grade zircon sand can be co-produced by using the production method disclosed by the invention, the method is a green, cyclic and economical industry chain, and the obtained product is good in quality, low in production cost and free of pollution.

Description

technical field [0001] The invention relates to a method for preparing zircon sand, in particular to a method for producing high-grade zircon sand. Background technique [0002] Zirconium oxychloride products are widely used and are the basic raw materials of zirconium chemical industry. The market demand is large. In 2014, it reached 240,000 tons. However, domestic zirconium oxychloride is produced by "alkali fusion method". Pollution control is very difficult, and the product quality cannot reach the quality standard of high-purity zirconium oxychloride. [0003] Fumed silicon dioxide is widely used and is a high-grade industrialized nano-material. The main raw material is silicon tetrachloride, and the main source of silicon tetrachloride is the by-product of the polysilicon industry or the by-product of the organic silicon industry. [0004] In recent years, in order to reduce production costs, polysilicon enterprises have developed silicon tetrachloride cold hydrogenat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/20C01B33/107C01G25/00C01B33/12C01B7/03C25B1/26C25B1/02
CPCC01B33/20C01B7/035C01B33/10721C01B33/12C01G25/00C01P2006/80C25B1/02C25B1/26
Inventor 郭志斌李毅南江红兵赵成飞董法强
Owner 郭志斌
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