CN105271385A - Method of removing silicon in coarse titanium tetrachloride - Google Patents
Method of removing silicon in coarse titanium tetrachloride Download PDFInfo
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- CN105271385A CN105271385A CN201510750953.4A CN201510750953A CN105271385A CN 105271385 A CN105271385 A CN 105271385A CN 201510750953 A CN201510750953 A CN 201510750953A CN 105271385 A CN105271385 A CN 105271385A
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- Prior art keywords
- titanic chloride
- silicon
- titanium tetrachloride
- crude titanic
- tower top
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/02—Halides of titanium
- C01G23/022—Titanium tetrachloride
- C01G23/024—Purification of tetrachloride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention belongs to the field of titanium chemical industry and particularly relates to and aims at providing a method of removing silicon in coarse titanium tetrachloride. The method comprises the steps that the coarse titanium tetrachloride is rectified to obtain fine titanium tetrachloride; all parameters of a rectifying tower are controlled as follows: the feeding speed is between 6 t/h and 10 t/h, the feeding temperature is between 65 DEG C and 85 DEG C, the reflux ratio is between 50 and 80, the tower top temperature is between 125 DEG C and 132 DEG C, the temperature of reflux liquid is between 75 DEG C and 85 DEG C, and the tower top pressure is between minus 2 kPa and 5 kPa. By the adoption of the method, the silicon in the coarse titanium tetrachloride can be removed, so that the fine titanium tetrachloride with the silicon content ranging from 1 ppm to 3 ppm is obtained.
Description
Technical field
The invention belongs to titanium chemical field, be specifically related to a kind of method removing silicon in crude titanic chloride.
Background technology
Refined titanic chloride is the starting material producing titanium sponge and chloride process titanium dioxide.
The method of current production crude titanic chloride has three kinds, is respectively shaft chlorination, fluidizing chlorination and fused salt chlorimation, but no matter adopts which kind of chlorination method, and all containing a certain amount of impurity in crude titanic chloride, major impurity is FeCl
3, AlCl
3, VOCl
3, SiCl
4, TiOCl
2with solid formation etc., these impurity are very harmful to titanium tetrachloride and subsequent product thereof, so need removing before entering downstream production process.
For titanium sponge production process, silicon with 4 times of concentration enrichments in titanium sponge, can affect mechanical property and the mechanical property of titanium sponge Brinell hardness and follow-up titanium material.SiCl
4can with TiCl
4infinitely dissolve each other, boiling point is 57.6 DEG C, belongs to the low-boiling point material in impurity, adopts rectification method to remove in production.The crude titanic chloride desilication technique of current domestic employing is rectification method silica removal, the tower plate structure adopted mostly is valve tray column and sieve-tray tower, total silicone content (Σ Si content) in product how between 15 ~ 30ppm, thus constrains raising and the high-end applications of China's titanium sponge quality.
The present invention adopts based on solution the problem that in the refined titanic chloride of traditional control method production, silicone content is higher, proposes a kind of rectifying tower control method reducing silicone content.
Summary of the invention
The invention provides a kind of method removing silicon in crude titanic chloride.The method, on the basis of existing rectification process, optimizes rectifying tower control method and processing parameter, improves rectifying fractionation efficiency of tower, reduces silicone content in refined titanic chloride, improves quality product.
Technical problem to be solved by this invention is to provide a kind of method removing silicon in crude titanic chloride.This production method comprises the following steps: crude titanic chloride carries out rectifying and obtains refined titanic chloride; Controlling each parameter of rectifying tower is: input speed 6 ~ 10t/h, feeding temperature 65 ~ 85 DEG C, reflux ratio 50 ~ 80, tower top temperature 125 ~ 132 DEG C, phegma temperature 75 ~ 85 DEG C, tower top pressure-2 ~ 5kPa.
Preferably, in above-mentioned removing crude titanic chloride silicon method in, described input speed for control inlet amount error per hour be no more than ± 3%.
Preferably, in above-mentioned removing crude titanic chloride silicon method in, total silicone content≤500ppm in described crude titanic chloride.
Preferably, in above-mentioned removing crude titanic chloride silicon method in, rate of yield is 1 ~ 4% of input speed.
Preferably, in above-mentioned removing crude titanic chloride silicon method in, described tower top pressure-2 ~ 0kPa.
In order to solve the problem that in existing rectifying gained refined titanic chloride, silicone content is higher, the basis of contriver's silicon in existing rectifying separation removing crude titanic chloride reasonably controls the series of parameters such as content, input speed, reflux ratio, reflux temperature, tower top pressure of silicon in raw material through great many of experiments, these parameters complement each other, thus achieve SiCl in crude titanic chloride
4with TiCl
4good separation, finally obtains the refined titanic chloride of total silicone content at 1 ~ 3ppm.The refined titanic chloride quality that present method obtains is good, better for next process, can ensure that the quality of the finished product.
Embodiment
Crude titanic chloride is the product after rich titanium material chlorination, mainly containing SiCl
4, VOCl
3, AlCl
3, FeCl
3, TiOCl
2deng impurity.Wherein, SiCl
4can with TiCl
4infinitely dissolve each other, boiling point is 57.6 DEG C, belongs to the low-boiling point material in impurity, and tradition adopts rectification method removing silicon, but in the refined titanic chloride of gained, how total silicone content (Σ Si content) is between 15 ~ 30ppm, thus constrains raising and the application of China's titanium sponge quality.
In order to solve the problem, contriver has carried out the condition test at each reference mark, have studied the impact of each factor on silicone content in product, a large amount of experiments, summary, analysis are carried out, finally draw, on the basis of traditional rectification process, controlling each parameter of rectifying tower is input speed 6 ~ 10t/h, feeding temperature 65 ~ 85 DEG C, reflux ratio 50 ~ 80, tower top temperature 125 ~ 132 DEG C, phegma temperature 75 ~ 85 DEG C, after tower top pressure-2 ~ 5kPa carries out rectifying, the refined titanic chloride of low silicon content 1 ~ 3ppm can be obtained.This refined titanic chloride quality is good, can meet the need of production of titanium sponge and titanium white chloride well.Preferably, total silicone content≤500ppm in crude titanic chloride.Input speed for control inlet amount error per hour be no more than ± 3%.Rate of yield is 1 ~ 4% of input speed.Tower top pressure-2 ~ 0kPa.
The stage number of the rectifying tower adopted in the embodiment of the present invention 44 pieces, diameter 1200mm, tray spacing 300mm, but the present invention is not limited to this rectifying tower.
Embodiment 1
In crude titanic chloride, total silicone content (Σ Si content) is 180ppm, input speed is 7.8t/h, feeding temperature is 84.5 DEG C, reflux ratio is 65, tower top temperature is 129 ± 0.6 DEG C, phegma temperature is 83 ± 1.0 DEG C, and tower top pressure is 1.2kPa, and the rate of yield of tower top low boilers is 2.8% of feed material feed rates.
In the refined titanic chloride that the present embodiment obtains, total silicone content (Σ Si content) is 2ppm, and other index also meets member country of the Commonwealth of Independent States's 0 grade of refined titanic chloride standard.
Embodiment 2
In crude titanic chloride, total silicone content (Σ Si content) is 65ppm, input speed is 7.0t/h, feeding temperature is 80 DEG C, reflux ratio is 58, tower top temperature is 130 ± 0.5 DEG C, phegma temperature is 80 ± 0.6 DEG C, and tower top pressure is 1.6kPa, and tower top low boilers rate of yield is 3.2% of feed material feed rates.
In the refined titanic chloride that the present embodiment obtains, total silicone content (Σ Si content) is 1.5ppm, and other index also meets member country of the Commonwealth of Independent States's 0 grade of refined titanic chloride standard.
Comparative example 1
With the raw material of the same refined titanic chloride of the present invention, adopt traditional rectificating method to carry out rectifying, in gained refined titanic chloride, total silicone content (Σ Si content) is 12-15ppm.
In summary it can be seen, the inventive method is by reasonably controlling each parameter of rectifying tower, and can produce and obtain silicon content is 1 ~ 3ppm refined titanic chloride, has the technique effect higher than existing traditional rectificating method.
Claims (5)
1. remove a method for silicon in crude titanic chloride, it is characterized in that: comprise the following steps: crude titanic chloride carries out rectifying and obtains refined titanic chloride; Controlling each parameter of rectifying tower is: input speed 6 ~ 10t/h, feeding temperature 65 ~ 85 DEG C, reflux ratio 50 ~ 80, tower top temperature 125 ~ 132 DEG C, phegma temperature 75 ~ 85 DEG C, tower top pressure-2 ~ 5kPa.
2. the method for silicon in removing crude titanic chloride according to claim 1, is characterized in that: described input speed is no more than for controlling inlet amount error per hour ± and 3%.
3. the method for silicon in removing crude titanic chloride according to claim 1, is characterized in that: total silicone content≤500ppm in described crude titanic chloride.
4. the method for silicon in removing crude titanic chloride according to claim 1, is characterized in that: rate of yield is 1 ~ 4% of input speed.
5. the method for silicon in removing crude titanic chloride according to claim 1, is characterized in that: described tower top pressure is-2 ~ 0kPa.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510750953.4A CN105271385B (en) | 2015-11-06 | 2015-11-06 | A kind of method of silicon in removing crude titanic chloride |
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|---|---|---|---|
| CN201510750953.4A CN105271385B (en) | 2015-11-06 | 2015-11-06 | A kind of method of silicon in removing crude titanic chloride |
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| Publication Number | Publication Date |
|---|---|
| CN105271385A true CN105271385A (en) | 2016-01-27 |
| CN105271385B CN105271385B (en) | 2017-03-29 |
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| CN201510750953.4A Active CN105271385B (en) | 2015-11-06 | 2015-11-06 | A kind of method of silicon in removing crude titanic chloride |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106834747A (en) * | 2017-01-18 | 2017-06-13 | 贵州大学 | A kind of method for preparing titanium sponge |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2370525A (en) * | 1942-11-16 | 1945-02-27 | Pittsburgh Plate Glass Co | Purification of titanium tetrachloride |
| CN201144153Y (en) * | 2007-12-15 | 2008-11-05 | 遵义钛业股份有限公司 | Device for recovering SiCl4 in TiCl4 refining process |
| CN201704087U (en) * | 2010-05-04 | 2011-01-12 | 山东鲁北企业集团总公司 | Fast heating and distilling device in process of refining titanium tetrachloride |
| CN103011268A (en) * | 2012-12-21 | 2013-04-03 | 天津大学 | Titanium tetrachloride purification system and method |
| CN104118905A (en) * | 2014-08-06 | 2014-10-29 | 攀钢集团攀枝花钢铁研究院有限公司 | Refining process of crude titanium tetrachloride |
-
2015
- 2015-11-06 CN CN201510750953.4A patent/CN105271385B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2370525A (en) * | 1942-11-16 | 1945-02-27 | Pittsburgh Plate Glass Co | Purification of titanium tetrachloride |
| CN201144153Y (en) * | 2007-12-15 | 2008-11-05 | 遵义钛业股份有限公司 | Device for recovering SiCl4 in TiCl4 refining process |
| CN201704087U (en) * | 2010-05-04 | 2011-01-12 | 山东鲁北企业集团总公司 | Fast heating and distilling device in process of refining titanium tetrachloride |
| CN103011268A (en) * | 2012-12-21 | 2013-04-03 | 天津大学 | Titanium tetrachloride purification system and method |
| CN104118905A (en) * | 2014-08-06 | 2014-10-29 | 攀钢集团攀枝花钢铁研究院有限公司 | Refining process of crude titanium tetrachloride |
Non-Patent Citations (1)
| Title |
|---|
| 莫畏等: "《钛冶炼》", 31 July 2011 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106834747A (en) * | 2017-01-18 | 2017-06-13 | 贵州大学 | A kind of method for preparing titanium sponge |
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|---|---|
| CN105271385B (en) | 2017-03-29 |
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