CN101844802B - Rapidly heating distillation device in titanium tetrachloride refining process - Google Patents
Rapidly heating distillation device in titanium tetrachloride refining process Download PDFInfo
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- CN101844802B CN101844802B CN2010101615132A CN201010161513A CN101844802B CN 101844802 B CN101844802 B CN 101844802B CN 2010101615132 A CN2010101615132 A CN 2010101615132A CN 201010161513 A CN201010161513 A CN 201010161513A CN 101844802 B CN101844802 B CN 101844802B
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Abstract
The invention belongs to the technical field of titanium sponge production by a magnesium method and in particular relates to a rapidly heating distillation device in a titanium tetrachloride refining process. The invention adopts a technical scheme that: the rapidly heating distillation device in the titanium tetrachloride refining process comprises a distillation still, a distillation tower, a cooler, a respiration tank, a ground tank and a finished product storage tank which are connected with one another sequentially through pipelines. The rapidly heating distillation device has the advantages of raising the temperature uniformly and stably, realizing automation easily, increasing production yield by 30 percent, reducing energy consumption by 15 percent, greatly improving the purity of the products, saving energy and reducing consumption, greatly improving the quality of the products and protecting the surrounding environment, along with simple and rapid operation, stable production, good separation effect and low production cost.
Description
Technical field
The invention belongs to magnesium method production technical field of titanium sponge, particularly a kind of rapidly heating distillation device in process of refining titanic chloride.
Background technology
In the titanium tetrachloride treating process, according to the boiling point of the high boiling point in the crude titanic chloride and lower-boiling impurity and titanium tetrachloride or the characteristics that relative volatility differs greatly, with distillation method or rectification method removing foreign matter.Adopt distillation method to separate for segregative high-boiling-point impurity, the lower-boiling impurity of difficulty adopts rectification method to separate for separating.The distillation operation is carried out in distillation tower, and control base product temperature partly vaporizes the volatile components titanium tetrachloride a little more than the boiling point (about 140-145 ℃) of titanium tetrachloride; Volatilizations such as difficult volatiles FeCl3 are little and residue at the bottom of the tower, even a small amount of volatilization is arranged, the phlegma condensation that also possibly fallen and returning again falls within the bottom of the tower.The control tower top temperature is at TiC14 boiling point (about 137 ℃), owing to have a little thermograde in the tower, the steam of TiCl4 forms internal recycle in tower, contacts between the steam that makes progress and the drop of whereabouts, has carried out heat and mass transfer process, has increased separating effect.In this process; High-boiling-point impurities such as FeCl3 along in the TiCl4 steam of tower rising reduce gradually, and pure TiCl4 steam is overflowed from cat head, becomes distillate through condenser condenses; And the continuous enrichment of high-boiling-point impurities such as FeCl3 in the cauldron bottom residue is regularly discharged and is made it separation.
The distillatory major equipment is still kettle, distillation tower and condensing surface.During distillation, common way is to adopt the mode of heating to make the feed liquid vaporization in the still kettle, and the steam in the still kettle gets in the distillation tower along vapour pipe, and the tower steam of effusion becomes distillate through condenser condenses, and TiCl4 liquid can get in the still along return line at the bottom of the tower.The heating of titanium tetrachloride is adopted the electromagnetism tube to twine nickel outward usually and is pressed against the direct and titanium tetrachloride Contact Heating vaporization of silk in the still kettle, and there is following shortcoming in this heating means in actual production process:
1, because the electromagnetism tube twines nickel outward presses against silk heating and must be immersed in the TiCl4 liquid, burn nickel easily and press against silk once long as exposing the liquid level time a little, must stop and change, otherwise can't produce, cause the start-stop car frequent, the driving rate reduction, production yields poorly.
2, in repair demolition or when changing nickel on the electromagnetism tube and pressing against thread, violent reaction will take place after overflowing and meeting the air contact in the TiCl4 in the still, generates TiO2 and HCl gas; Form a large amount of acid mists around; Not only corrode buildings and equipment, also can serious environment pollution, operator are damaged.
3, the electromagnetism tube twines nickel outward to press against silk little with TiCl4 liquid contact area, and TiCl4 liquid reaches 6 hours from the TRT that normal temperature reaches evaporation conditions in the still, causes power consumption high, and cost is high.
Summary of the invention
The objective of the invention is to, overcome the deficiency of prior art, a kind of rapidly heating distillation device in process of refining titanic chloride is provided; TiCl4 liquid is shortened from the TRT that normal temperature reaches evaporation conditions greatly; Not only help saving energy and reduce the cost, owing to need not to contact TiCl4 liquid, avoid contacting of TiCl4 liquid and air in maintenance or when changing globars; To avoid environmental pollution and, to have improved worker's operating environment greatly to personnel's injury.
For solving the problems of the technologies described above; Technical scheme of the present invention is: the rapidly heating distillation device in process of refining titanic chloride; Comprise the still kettle that connects successively through pipeline, distillation tower, water cooler, breather tank, jar and finished product storage tank; Described still kettle comprises: weigh column distillation still, light column distillation still and remove alum column distillation still; Described distillation tower comprises: heavy ends column, light fraction tower and remove alum cut tower, and described water cooler comprises: heavily tower cooler device, light tower cooler device and remove alum tower cooler device; Described heavy column distillation still, heavy ends column are connected through pipeline with heavy tower cooler device successively; Said light column distillation still, light fraction tower and light tower cooler device are complied with through pipeline and are connected; Said remove alum column distillation still, remove alum cut tower and remove alum tower cooler device be connected successively through pipeline; The bottom of said heavy tower cooler device is connected through materail tube with the top of light fraction tower; The top of said light column distillation still with remove alum column distillation still and be connected through materail tube, said bottom except that alum tower cooler device is connected with finished product storage tank.
Rapidly heating distillation device in process of refining titanic chloride of the present invention; Described still kettle comprises distillation kettle and the piezometric tube and the temperature tube that are positioned on the distillation kettle; Also comprise at least two heating units that are positioned at the still kettle internal upper part; Be parallel connection between heating unit, there is heating muff in each heating unit outside.
Heating unit of the present invention is a globars.Described heating unit is preferably 3-9.
Heating unit of the present invention uniform distribution in still kettle.
After adding material by rules to still kettle, press the startup knob of two groups of elema heaters of still kettle, begin to the still kettle feeding temperature-raising.When the still temperature rise was above to specified temperature, floating cutting down in the tower should have sound of movement sound, the existing backflow in the visor under the observing tower, and the venting port of condensing surface has gas to discharge, and tower top temperature begins to rise.Bound set(ting)value and the adjustment feeding quantity of setting the tower top temperature meter through adjustment make system reach optimal operational condition, remove heavy fractionated Ticl4 and get into light fraction tower and further purify and lower-boiling impurity such as remove; Material adds behind the tower still temperature that is heated to regulation with globars; Material in the tower still overflows to except that adopting same heating way in the alum still, and the heating kettle temperature is to the temperature of regulation, and the Ticl4 liquid that steams entering removes the alum tower and contacts with copper ball; At this moment the Vocl3 in the gas is reduced; Reduzate is deposited on the copper wire surface, and gas Ticl4 is come out to obtain smart Ticl4 after the back gets into the water cooler cooling by cat head, and rare gas element is through the breather tank emptying.
Heating unit globars of the present invention has following precaution when installing:
1) mode of connection of globars element; Adopt the parallelly connected mode of connection; Can regulate load unbalanced factor, the pin of globars electrical heating element is all used the ceramic fibre sleeving pipe insulation, and the ceramic fiber sleeve pipe not only plays a part electric insulation but also plays the fixedly effect of globars.
(2) in order to make every globars can both be in normal and the ideal working order, before installing globars is by the gross measured its resistance value, with its classification, resistance value is close is contained in same adjustment district, and it is close to make it working power.
(3) in order to check whether works fine of every globars electrical heating element, can measure electric current one by one with clamp on amperemeter during energizing test.The same area requires electric current close under the voltage that equates, deviation does not exceed 10%, should further check replacing if exceed 10%.
(4) globars electrical heating element matter is crisp easily broken, and is the most fragile in threaded position especially, installs and want SC; Handle with care; To pay special attention to never to allow monolateral stressed during installation, use heat resisting pipe and entangle globars and push gently and extract steel pipe socket then, set up sheath and fix.
The invention has the beneficial effects as follows:
Through with the transformation of cover production equipment to devices such as this titanium tetrachloride rapidly heating distillation device and heavy tower still, light tower stills, every globars electrical heating element heats up uniform and stable, simple and quick; Be prone to realize robotization; Production output improves 30%, and energy consumption reduces by 15%, produces stable; Good separating effect, product gas purity improves greatly.Both energy-saving and cost-reducing after the embodiment of the present invention, production cost is low, and quality product improves greatly, the environment around having protected again.
Because the 316L stainless steel cylinder contacts with TiCl4 liquid, when repair demolition or replacing globars, need not to contact the TiCl4 liquid in the still, stop the injury of waste gas to human body.Avoid bringing into impurity simultaneously, make the product that obtains purer.This TiCl4 rapid heating rectifier unit has rectification efficiency height, throughput is strong, turndown ratio is big characteristics.
Description of drawings
Fig. 1 is a structural representation of the present invention,
Fig. 2 is a still kettle structure for amplifying synoptic diagram,
Fig. 3 is along the cross-sectional view of A-A direction among Fig. 2.
Among the figure: the heavy column distillation still of 1-, the 2-heavy ends column, 3-is the tower cooler device heavily, the light column distillation still of 4-; The 5-light fraction tower, the light tower cooler device of 6-, 7-removes alum column distillation still, and 8-removes alum cut tower; 9-removes alum tower cooler device, 10-breather tank, 11-finished product storage tank; 12-ground jar, 13-materail tube, 14-piezometric tube, 15-heating unit, 16-heating muff, 17-temperature tube, 18-distillation kettle, 19-riser, 20-spoil disposal cinder notch, 21-refluxing opening, 22-vapour outlet.
Below in conjunction with accompanying drawing and embodiment the present invention is done further explain:
Embodiment
Be further described in conjunction with producing the embodiment contrast accompanying drawing of 5000 tons of titanium tetrachloride production equipments per year a kind of rapidly heating distillation device in process of refining titanic chloride of the present invention:
According to Fig. 1, Fig. 2 and shown in Figure 3; A kind of rapidly heating distillation device in process of refining titanic chloride; Comprise the still kettle that connects successively through pipeline, distillation tower, water cooler, breather tank 10, jars 12 and finished product storage tank 11; Still kettle comprises: heavy column distillation still 1, light column distillation still 4 and remove alum column distillation still 7, and distillation tower comprises: heavy ends column 2, light fraction tower 5 and remove alum cut tower 8, water cooler comprises: heavily tower cooler device 3, light tower cooler device 6 and remove alum tower cooler device 9; Heavy column distillation still 1, heavy ends column 2 and heavy tower cooler device 3 are connected through pipeline successively; Light column distillation still 4, light fraction tower 5 and light tower cooler device 6 are complied with through pipeline and are connected; Remove alum column distillation still 7, remove alum cut tower 8 and remove alum tower cooler device 9 and be connected successively through pipeline; Heavily the bottom of tower cooler device 3 is connected through materail tube 13 with the top of light fraction tower 5, the top of light column distillation still 4 with remove alum column distillation still 7 and be connected through materail tube 13, except that the bottom of alum tower cooler device 9 is connected with finished product storage tank 11.
Still kettle comprises distillation kettle 18 and the piezometric tube 14, temperature tube 17, riser 19, spoil disposal cinder notch 20, refluxing opening 21, the vapour outlet 22 that are positioned on the distillation kettle 18; Still kettle also comprises six heating units 15 that are positioned at the still kettle internal upper part; 15 of heating units are parallel connection; There is heating muff 16 in each heating unit 15 outside, and heating unit 15 is a globars, uniform distribution in still kettle.
The crude titanic chloride of being brought by chlorination pumps into high level tank through metering inflow heavy ends column 2 epimeres; Open double distilled return-flow system valve Ticl4 liquid and get into heavy column distillation still 1; Behind the heavy column distillation still 1 usefulness globars heating heating muff 16; The boiling point of the Ticl4 in a little higher than still heats up; Part Ticl4 vaporized gas is expelled to heavy ends column 2 through vapour outlet 22, the 3rd block of column plate in heavy ends column 2 bottoms along column plate along on the top, rise with heavy ends column 2 in the Ticl4 phlegma meet and carry out heat and mass transfer, Ticl4 liquid gives heat to the temperature of stipulating at this Ticl4 gas that is steamed by heavy ends column 2 tops through the heavy inner sleeve of tower cooler device 3; Get into the 7th block of column plate in the heavy ends column 2; Carry out rectifying at heavy ends column 2 towers and remove high-boiling-point impurity, impurity is expelled to ground jars 12 by still kettle 1 bottom spoil disposal cinder notch 20, and the thick Ticl4 that gets off from heavy tower cooler device 3 is by the 18 block of column plate in certain reflux ratio to the heavy ends column 2; Along column plate along linking to each other with heavy column distillation still refluxing opening 21 to the bottom overflow, another part remove heavy fractionated phlegma send into light fraction tower 5 through with above-mentioned flow process after further rectification and purification remove lower-boiling impurities such as Sicl4.
The Ticl4 that gets off of tower cooler device 6 is by the 18 block of column plate in certain reflux ratio to the light fraction tower 5 on the lenient side; Link to each other with light column distillation still refluxing opening 21 to the bottom overflow along the column plate edge; Another part is removed light fractionated phlegma and is sent into except that alum cut tower 8 through light column distillation still riser 19 and contact with copper ball; At this moment the Vocl3 in the gas is reduced, and reduzate is deposited on the copper wire surface, and gas Ticl4 ejects the back to get into except that alum water cooler 9 by removing alum cut tower 8; Rare gas element obtains smart Ticl4 and sends into the 11 confession sale uses of finished product basin after metering through breather tank 10 emptyings.
The heating muff of heating distilling device of the present invention is evenly distributed six stainless steel cylinders at distillation kettle top; Place one group of globars in each stainless steel cylinder; As the production equipment still kettle internal diameter of producing 5000 tons per year is 1400mm, and single stainless steel cylinder body diameter is 219mm, and the central point of stainless steel cylinder is evenly distributed on the circumference that the still kettle internal diameter is 800mm; Make that the still kettle internal heating is even, heats is good.
In same production equipment still kettle under the situation of equivalent material; The globars of equal-wattage and nickel reeling are compared; When beginning to be warming up to the temperature that reaches specified requirement, 2.5 hours globars heat temperature raising time, then need 6 hours with the nickel reeling heat temperature raising time.Burn heating unit cause the stopping production generation of phenomenon owing to adopting the globars heating needn't worry that liquid level is low; When the charging volume in the still kettle accounts for still volumetrical 50-60%; Could guarantee like this has bigger space on the liquid level in the still, and the steam that gasification is produced has sufficient chance and liquid separation that it is got in the still kettle, influences distillation efficiency; Thereby make that production is more stable, good separating effect.
Claims (3)
1. the rapidly heating distillation device in process of refining titanic chloride; Comprise the still kettle that connects successively through pipeline, distillation tower, water cooler, breather tank, jar and finished product storage tank; It is characterized in that: described still kettle comprises: weigh column distillation still, light column distillation still and remove alum column distillation still; Described distillation tower comprises: heavy ends column, light fraction tower and remove alum cut tower, and described water cooler comprises: heavily tower cooler device, light tower cooler device and remove alum tower cooler device; Described heavy column distillation still, heavy ends column are connected through pipeline with heavy tower cooler device successively; Said light column distillation still, light fraction tower and light tower cooler device are connected through pipeline successively; Said remove alum column distillation still, remove alum cut tower and remove alum tower cooler device be connected successively through pipeline; The bottom of said heavy tower cooler device is connected through materail tube with the top of light fraction tower; The top of said light column distillation still with remove alum column distillation still and be connected through materail tube, said bottom except that alum tower cooler device is connected with finished product storage tank; Described still kettle comprises distillation kettle and the piezometric tube and the temperature tube that are positioned on the distillation kettle; Described still kettle also comprises at least two heating units that are positioned at the still kettle internal upper part; Be parallel connection between heating unit, it is globars that there are heating muff, described heating unit in each heating unit outside.
2. the rapidly heating distillation device in process of refining titanic chloride according to claim 1 is characterized in that: described heating unit is preferably 3-9.
3. the rapidly heating distillation device in process of refining titanic chloride according to claim 1 is characterized in that: described heating unit uniform distribution in still kettle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101615132A CN101844802B (en) | 2010-05-04 | 2010-05-04 | Rapidly heating distillation device in titanium tetrachloride refining process |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010101615132A CN101844802B (en) | 2010-05-04 | 2010-05-04 | Rapidly heating distillation device in titanium tetrachloride refining process |
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| CN101844802A CN101844802A (en) | 2010-09-29 |
| CN101844802B true CN101844802B (en) | 2012-06-27 |
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| CN2010101615132A Expired - Fee Related CN101844802B (en) | 2010-05-04 | 2010-05-04 | Rapidly heating distillation device in titanium tetrachloride refining process |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102476826A (en) * | 2010-11-29 | 2012-05-30 | 贵阳铝镁设计研究院有限公司 | Method for reducing loss during titanium tetrachloride production process and device thereof |
| CN103011268A (en) * | 2012-12-21 | 2013-04-03 | 天津大学 | Titanium tetrachloride purification system and method |
| CN112412047B (en) * | 2020-10-15 | 2022-02-01 | 中国水利水电第九工程局有限公司 | Self-heating vibrating rod for concrete tamping drum |
| CN113912107B (en) * | 2021-11-08 | 2023-03-28 | 贵州威顿晶磷电子材料股份有限公司 | High-purity titanium tetrachloride purification manufacturing process |
| CN114797139B (en) * | 2022-03-09 | 2023-05-12 | 洛阳双瑞万基钛业有限公司 | Crude titanium tetrachloride electric heating device and distillation system containing high-concentration solid particles |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3963585A (en) * | 1973-05-22 | 1976-06-15 | Bayer Aktiengesellschaft | Distillation of titanium tetrachloride in solution with selected amines |
| CN1927723A (en) * | 2006-06-12 | 2007-03-14 | 北京有色金属研究总院 | Method of removing vanadium from titanium tetrachloride by aluminum powder as direct reducer |
| CN101549885A (en) * | 2009-05-27 | 2009-10-07 | 北京大学 | Method of refining titanium tetrachloride by using aluminium powder and vash oil mixture |
| 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 |
-
2010
- 2010-05-04 CN CN2010101615132A patent/CN101844802B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3963585A (en) * | 1973-05-22 | 1976-06-15 | Bayer Aktiengesellschaft | Distillation of titanium tetrachloride in solution with selected amines |
| CN1927723A (en) * | 2006-06-12 | 2007-03-14 | 北京有色金属研究总院 | Method of removing vanadium from titanium tetrachloride by aluminum powder as direct reducer |
| CN101549885A (en) * | 2009-05-27 | 2009-10-07 | 北京大学 | Method of refining titanium tetrachloride by using aluminium powder and vash oil mixture |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 李宏伟等.为精制提供优质四氯化钛的简易方法.《轻金属》.2004,(第9期),第45-46页. * |
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