CN103896336B - A kind of substep continuous decomposition method of zircon sand - Google Patents
A kind of substep continuous decomposition method of zircon sand Download PDFInfo
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- CN103896336B CN103896336B CN201210581451.XA CN201210581451A CN103896336B CN 103896336 B CN103896336 B CN 103896336B CN 201210581451 A CN201210581451 A CN 201210581451A CN 103896336 B CN103896336 B CN 103896336B
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Abstract
The present invention relates to zircon sand and decompose field, particularly, the present invention relates to a kind of substep continuous decomposition method of zircon sand.The substep continuous decomposition method of zircon sand of the present invention, comprises the following steps: 1) by zircon sand and alkali metal hydroxide by weight being 1:(0.3-0.8) ratio mix; 2) zircon sand step 1) obtained and the mixture of alkali metal hydroxide are delivered in horizontal stove, obtain intermediate calcination material; 3) by step 2) after the cooling of the intermediate calcination material that obtains, then by itself and alkali metal hydroxide 1:(0.3-1.0 by weight) ratio mix; 4) mass transport mixed step 3) obtained, in another horizontal stove, can obtain zirconates after reaction.The inventive method adopts substep to add alkali, can reduce the consumption of alkali, and effectively alleviate because single alkali number is too high, the sticky wall that material produces in rotary kiln or ring formation phenomenon, and the continous-stable that can realize zircon sand decomposes.
Description
Technical field
The present invention relates to zircon sand and decompose field, particularly, the present invention relates to a kind of substep continuous decomposition method of zircon sand.
Background technology
Zircon sand is a kind of with the silicate (ZrSiO of zirconium
4) be the main mineral formed, chemical stability is high, is difficult to decompose.Be that raw material can prepare multiple zirconates with zircon sand, wherein zirconium oxychloride (ZrOCl
28H
2o) be more important zirconates basic chemical industry product.Zirconium oxychloride can be used for separation of zirconium and hafnium and prepares atomic level zirconium hafnium, also can prepare other zirconium chemicalses such as zirconium white, zirconium sulfate, acetic acid zirconium, zirconium carbonate.At present, what domestic decomposing zircon sand mainly adopted is alkali fusion, and alkali fusion Ye Shi China produces the main method that zirconium oxychloride adopts.The method is that zircon sand and alkali (being mainly NaOH) are heated to about 700 DEG C fusion and decomposition in sintering pot, obtains zirconic acid sodium salt and silicate, then through washing the process removal of impurities such as transition, then crystallization can obtain zirconium oxychloride.In whole production process, the calcination of zircon sand and NaOH is an important step.
During existing zirconium oxychloride is produced, alkali fusion reaction is mainly carried out in sintering pot discontinuous, mainly has the following disadvantages: (1) thermo-efficiency is low, and decomposition course energy consumption is high, and zirconium oxychloride per ton needs consume mark 0.9 ton, coal or consume coal gas 2600 cubes; (2) Automation of Manufacturing Process degree is low; (3) pot body is heated uneven, and temperature is unstable, causes zirconium oxychloride unstable product quality; (4) operating process is open, and in environment, alkali mist is large; (5) production process generally adopts overhead traveling crane to fill the sintering pot handling repeatedly of high temperature alkaline solution, is unfavorable for safety in production.
Domestic patent 201010553198.8 once reported that the continuous alkali fusion adopting rotary kiln directly to carry out zircon sand decomposed, but because material alkalinity is high, at high temperature material is melting viscous pasty state, the inwall of the rotary kiln that very easily bonds, thus generation ring formation, be unfavorable for realizing large-scale industrial production.
Summary of the invention
The object of the invention is to, for solving the problem, improve the deficiency of traditional alkali fusion technique, a kind of novel method of continuous decomposition zircon sand is provided.By the application of novel method, the continous-stable that can realize alkali fusion process zircon sand decomposes, and increases substantially production efficiency and automatization level, improves operating environment.
The substep continuous decomposition method of zircon sand of the present invention, comprises the following steps:
1) by zircon sand and alkali metal hydroxide by weight being 1:(0.3-0.8) ratio mix;
2) zircon sand step 1) obtained and the mixture of alkali metal hydroxide are delivered in horizontal stove, successively by horizontal chamber oven preheating section of kiln, high temperature section and holding-zone, obtain intermediate calcination material;
3) by step 2) after the cooling of the intermediate calcination material that obtains, then by itself and alkali metal hydroxide 1:(0.3-1.0 by weight) ratio mix;
4) mass transport mixed step 3) obtained, in another horizontal stove, successively by horizontal chamber oven preheating section of kiln, high temperature section and holding-zone, obtains zirconates.
According to the substep continuous decomposition method of zircon sand of the present invention, described alkali metal hydroxide is NaOH.
According to the substep continuous decomposition method of zircon sand of the present invention, described horizontal chamber oven preheating section of kiln temperature controls at 300-650 DEG C, material stop 10-200 minute; High temperature section temperature controls at 650-950 DEG C, material stop 10-200 minute; Holding-zone temperature controls at 300-700 DEG C, material stop 10-200 minute.
According to the substep continuous decomposition method of the zircon sand that the present invention states, above-mentioned horizontal stove is preferably continuous rotary kiln.
According to the substep continuous decomposition method of zircon sand of the present invention, above-mentioned horizontal stove feeding manner, preferably adopts the helixes feed equipment containing feeding warehouse.
According to the substep continuous decomposition method of zircon sand of the present invention, described in the zirconates that obtains be sodium zirconate.
The inventive method, compared with conventional art, can realize the continuous prodution of alkali fusion process, improves heat utilization efficiency, reduces energy consumption; Improve production automation level, improve operating environment; Owing to adopting substep to add alkali, can reduce the consumption of alkali, and effectively alleviate because single alkali number is too high, the sticky wall that material produces in rotary kiln or ring formation phenomenon, the continous-stable that can realize zircon sand decomposes.
Embodiment
The substep continuous decomposition method of zircon sand of the present invention, is described in detail by following examples.
Embodiment 1
Zircon sand is mixed by weight 1:0.5 with sodium hydroxide, be delivered in rotary kiln by screw feeder, pass through preheating section successively, high temperature section, holding-zone, preheating section temperature is 450 DEG C, material stop entered high temperature section after 30 minutes, high temperature section temperature controls at 900 DEG C, material stop 50 minutes, then material enters holding-zone, temperature controls at 500 DEG C, stop and obtain intermediate calcination material after 80 minutes, after discharging, intermediate calcination material is mixed by with sodium hydroxide weight ratio 1:0.8, be delivered in another rotary kiln by screw feeder, control preheating section, high temperature section, the same single-revolution kiln of holding-zone temperature, the residence time of three periods is respectively 30 minutes, 30 minutes, 100 minutes, discharging can obtain sodium zirconate, zirconium rate of decomposition is 97% after tested.
Embodiment 2
Zircon sand is mixed by weight 1:0.8 with sodium hydroxide, be delivered in rotary kiln by screw feeder, pass through preheating section successively, high temperature section, holding-zone, preheating section temperature is 300 DEG C, material stop entered high temperature section after 80 minutes, high temperature section temperature controls at 700 DEG C, material stop 180 minutes, then material enters holding-zone, temperature is 300 DEG C, stop and obtain intermediate calcination material after 100 minutes, after discharging, intermediate calcination material is mixed by with sodium hydroxide weight ratio 1:0.6, be delivered in another rotary kiln by screw feeder, control preheating section, high temperature section, holding-zone temperature is 300 DEG C, 700 DEG C, 500 DEG C, the residence time is respectively 50 minutes, 50 minutes, 80 minutes, discharging can obtain sodium zirconate, zirconium rate of decomposition is 99% after tested.
Embodiment 3
Zircon sand is mixed by weight 1:0.3 with sodium hydroxide, be delivered in rotary kiln by screw feeder, pass through preheating section successively, high temperature section, holding-zone, preheating section temperature is 600 DEG C, material stop entered high temperature section after 100 minutes, high temperature section temperature controls at 900 DEG C, material stop 100 minutes, then material enters holding-zone, temperature is 400 DEG C, stop and obtain intermediate calcination material after 100 minutes, after discharging, intermediate calcination material is mixed by with sodium hydroxide weight ratio 1:1.0, be delivered in another rotary kiln by screw feeder, control preheating section, high temperature section, the same single-revolution kiln of holding-zone temperature, the residence time is respectively 60 minutes, 60 minutes, 80 minutes, discharging can obtain sodium zirconate, zirconium rate of decomposition is 98.8% after tested.
Embodiment 4
Zircon sand is mixed by weight 1:0.8 with sodium hydroxide, be delivered in rotary kiln by screw feeder, pass through preheating section successively, high temperature section, holding-zone, preheating section temperature is 300 DEG C, material stop entered high temperature section after 200 minutes, high temperature section temperature controls at 950 DEG C, material stop 10 minutes, then material enters holding-zone, temperature controls at 500 DEG C, stop and obtain intermediate calcination material after 200 minutes, after discharging, intermediate calcination material is mixed by with sodium hydroxide weight ratio 1:0.3, be delivered in another rotary kiln by screw feeder, control preheating section, high temperature section, the same single-revolution kiln of holding-zone temperature, the residence time of three periods is respectively 30 minutes, 30 minutes, 100 minutes, discharging can obtain sodium zirconate, zirconium rate of decomposition is 96.5% after tested.
Embodiment 5
Zircon sand is mixed by weight 1:0.8 with sodium hydroxide, be delivered in rotary kiln by screw feeder, pass through preheating section successively, high temperature section, holding-zone, preheating section temperature is 650 DEG C, material stop entered high temperature section after 10 minutes, high temperature section temperature controls at 650 DEG C, material stop 200 minutes, then material enters holding-zone, temperature is 700 DEG C, stop and obtain intermediate calcination material after 10 minutes, after discharging, intermediate calcination material is mixed by with sodium hydroxide weight ratio 1:0.6, be delivered in another rotary kiln by screw feeder, control preheating section, high temperature section, holding-zone temperature is 450 DEG C, 800 DEG C, 600 DEG C, the residence time is respectively 60 minutes, 60 minutes, 100 minutes, discharging can obtain sodium zirconate, zirconium rate of decomposition is 97.5% after tested.
Claims (6)
1. a substep continuous decomposition method for zircon sand, comprises the following steps:
1) by zircon sand and alkali metal hydroxide by weight being 1:(0.3-0.8) ratio mix;
2) zircon sand step 1) obtained and the mixture of alkali metal hydroxide are delivered in horizontal stove, successively by horizontal chamber oven preheating section of kiln, high temperature section and holding-zone, obtain intermediate calcination material;
3) by step 2) after the cooling of the intermediate calcination material that obtains, then by itself and alkali metal hydroxide 1:(0.3-1.0 by weight) ratio mix;
4) mass transport mixed step 3) obtained, in another horizontal stove, successively by horizontal chamber oven preheating section of kiln, high temperature section and holding-zone, obtains zirconates after reaction.
2. the substep continuous decomposition method of zircon sand according to claim 1, is characterized in that, described alkali metal hydroxide is NaOH.
3. the substep continuous decomposition method of zircon sand according to claim 1, is characterized in that, described horizontal chamber oven preheating section of kiln temperature controls at 300-650 DEG C, material stop 10-200 minute; High temperature section temperature controls at 650-950 DEG C, material stop 10-200 minute; Holding-zone temperature controls at 300-700 DEG C, material stop 10-200 minute.
4. the substep continuous decomposition method of the zircon sand according to any one of claim 1-3, is characterized in that, described horizontal stove is continuous rotary kiln.
5. the substep continuous decomposition method of the zircon sand according to any one of claim 1-3, is characterized in that, described horizontal stove feeding manner adopts the helixes feed equipment containing feeding warehouse.
6. the substep continuous decomposition method of the zircon sand according to any one of claim 1-3, is characterized in that, described in the zirconates that obtains be sodium zirconate.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2280897A (en) * | 1993-08-09 | 1995-02-15 | Frank Pitts | Extraction of zirconium values from zircon |
| CN101723451A (en) * | 2009-12-16 | 2010-06-09 | 北京有色金属研究总院 | Method for decomposing zirconite |
| CN101746730A (en) * | 2009-12-16 | 2010-06-23 | 北京有色金属研究总院 | Process for decomposing zircon by alkali fusion |
| CN102060326A (en) * | 2010-11-22 | 2011-05-18 | 北京有色金属研究总院 | Alkali fusion continuous decomposing process method of zirconite |
-
2012
- 2012-12-27 CN CN201210581451.XA patent/CN103896336B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2280897A (en) * | 1993-08-09 | 1995-02-15 | Frank Pitts | Extraction of zirconium values from zircon |
| CN101723451A (en) * | 2009-12-16 | 2010-06-09 | 北京有色金属研究总院 | Method for decomposing zirconite |
| CN101746730A (en) * | 2009-12-16 | 2010-06-23 | 北京有色金属研究总院 | Process for decomposing zircon by alkali fusion |
| CN102060326A (en) * | 2010-11-22 | 2011-05-18 | 北京有色金属研究总院 | Alkali fusion continuous decomposing process method of zirconite |
Non-Patent Citations (2)
| Title |
|---|
| "用碱分解锆英砂制备ZrO2工艺中放射性的分布、处理和回收研究";林振汉等;《稀有金属快报》;20071231;第26卷(第1期);第106-114页 * |
| "用锆英砂制备锆铁红";钟清莲等;《中国陶瓷》;20031231;第39卷(第6期);第52-54页 * |
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