Being purified using valve tower is increased the production capacity of valve tower and reduces single during titanium tetrachloride
The method of position product energy consumption
Technical field
The invention belongs to smelting field of nonferrous metal, be related to raw material purification technique in titanium smelt production increase production capacity,
The method of operating of reducing energy consumption, increases production capacity and the reduction of valve tower during especially a kind of utilization valve tower purification titanium tetrachloride
The method of energy consumption of unit product.
Background technology
Titanium is a kind of corrosion resistant metal, is widely used in Aeronautics and Astronautics, navigation, chemical industry, oil, weaving, medicine equipment
And field of metallurgy.Titanium sponge is, using the titanium tetrachloride and magnesium metal of purification, under argon gas protection, to make magnesium metal and titanium tetrachloride
Reaction, production titanium sponge and magnesium chloride.Titanium sponge production is higher to titanium tetrachloride purity requirement, and titanium tetrachloride purification is to utilize four
Titanium chloride and the physical property of other impurity chlorides --- boiling point it is different, by making the anti-of titanium tetrachloride and impurity chlorides
Multiple gasification and condensation, finally make titanium tetrachloride sufficiently be separated with impurity chlorides.
At present, titanium tetrachloride purification generally single column purification is carried out using a valve tower, raw material is entered from tower, in tower with
On all tower sections be referred to as stripping section, following all tower sections are referred to as rectifying section in tower.Rectifying section is by titanium tetrachloride
And its gasification repeatedly of impurity and condensation, titanium tetrachloride is purified step by step, it is the necessaries for ensureing titanium tetrachloride quality;
Stripping section is step by step purified impurity chlorides by the gasification repeatedly to titanium tetrachloride and its impurity and condensation, is to ensure
The necessaries of the titanium tetrachloride rate of recovery.The purity of rectifying section outlet impurity chlorides is pure with stripping section middle outlet titanium tetrachloride
Degree is the contradictory relation of opposition, it is ensured that the purity of impurity chlorides, certainly will affect the purity of titanium tetrachloride, and then needs reduction to add
Doses, the yield of final impact titanium tetrachloride.
The content of the invention
The technical problem to be solved in the present invention is to find increase float valve during a kind of purification titanium tetrachloride using valve tower
The production capacity of tower and the method for reducing energy consumption of unit product, the method can increase by four while the rate of recovery of titanium tetrachloride is ensured
The yield of titanium chloride, and then the energy consumption of unit product titanium tetrachloride is reduced, reduce titanium tetrachloride cost for purification.
The present invention technical solution be:
The production capacity for increasing valve tower and the method for reducing energy consumption of unit product during a kind of utilization valve tower purification titanium tetrachloride,
It is comprised the following steps that:
1.1 carry out titanium tetrachloride purification using valve tower purification system, and the valve tower purification system has 2# valve towers and 1# floating
Valve tower, the bottom of towe discharging opening of the 2# valve towers is connected with titanium tetrachloride finished pot 4, the tower top of the 2# valve towers by pipeline
Discharging opening is connected by pipeline with the tower middle charging aperture of 1# valve towers, and the 2# valve towers, the tower top of 1# valve towers set respectively
The tower middle charging aperture for having overhead reflux valve II 7, overhead reflux valve I 6, the 2# valve towers is connected with four chlorinations by pipeline
Titanium material tank, is provided with material inlet valve II in tower, near 1# valve towers on the pipeline of the tower middle charging aperture near 2# valve towers
The pipeline of tower middle charging aperture be provided with material inlet valve I in tower, the pipeline between the 2# valve towers and 1# valve towers is provided with
Tower top effluent storage tank, the outlet at bottom of the 1# valve towers is connected with titanium tetrachloride head tank by pipeline;
Purification operations are carried out in 2# valve towers, the overhead reflux valve II of 2# valve towers is closed so that tower top temperature is increased to 70
DEG C~120 DEG C, material inlet valve II in tower is opened, make titanium tetrachloride raw material enter 2# valve towers by 2# valve tower towers middle charging aperture
In, being fed in tower by material inlet valve in control tower II, feeding quantity is single column purification 2 times~2.2 times of feeding quantity, the middle temperature of tower
Spend for 125~130 DEG C, in tower top an overhead is obtained, in sending into a tower top effluent recycling can, obtain in bottom of towe
Refined titanic chloride send into titanium tetrachloride finished pot in;
1.2nd, material inlet valve I in tower is opened, by an overhead of a tower top effluent recycling can collection, 1# is sent into and is floated
In valve tower, as secondary purification raw material, fed in tower by material inlet valve in control tower I, feeding quantity is single column purification charging
1/2~2/3 times of amount, opens the overhead reflux valve I of 1# valve towers, and the tower top temperature for making 1# valve towers is controlled 60 DEG C~90
DEG C, an overhead is carried out into purification & isolation again by 1# valve towers, secondary overhead is obtained, what bottom of towe was obtained
Titanium tetrachloride is sent in titanium tetrachloride head tank, is blended with titanium tetrachloride raw material, makes as the purification raw material of 2# valve towers
With.
Further, temperature is 125 DEG C~130 DEG C in the tower of 2# valve towers.
Further, temperature is 110 DEG C~120 DEG C in the tower of 1# valve towers.
Further, the specification of 2# valve towers isWhen, the feeding quantity of 2# valve towers in 4 hours by
2.91 ton hours are gradually increased to 6.25 ton hours.
Further, the specification of 1# valve towers isWhen, the feeding quantity of 1# valve towers be 1.1 ton hours~
2 ton hours.
The invention has the beneficial effects as follows:
1st, the overhead reflux valve of 2# valve towers is closed, it is to avoid it is cold that the titanium tetrachloride of rectifying section and impurity chlorides carry out repeatedly
Solidifying and gasification, energy saving;
2nd, the impurity chlorides total amount and material total amount of charging column plate are reduced, is ensureing that titanium tetrachloride reaches the same of same purity
When, feeding quantity can be significantly improved, be multiplied yield, and energy consumption of unit product is reduced;
3rd, reduce charging column plate impurity chlorides total amount, feeding quantity increase by 2 times -2.2 times while, product percent of pass by
85% brings up to 98%, reduces product secondary purification total amount, reduces energy consumption of unit product;
4th, a tower top effluent need to carry out secondary purification, although increase part energy consumption, but it is total only to account for 10%, Jing of reducing energy consumption
Body examination is calculated, and due to the effective lifting being multiplied with product percent of pass of yield, energy consumption of unit product lowers 45%.
Description of the drawings
Fig. 1 is the schematic diagram of valve tower purification system of the present invention.
In figure:1-1# valve towers, 2-2# valve towers, 3- titanium tetrachloride head tanks, 4- titanium tetrachloride finished pots, tower of 5-
Top effluent storage tank, 6- overhead reflux valve Is, 7- overhead refluxes valve II, material inlet valve I in 8- towers, material inlet valve in 9- towers
II, 10- bottom of towe outlet valve I, 11- bottom of towe outlet valve II.
Specific embodiment
Embodiment 1
As illustrated, carrying out titanium tetrachloride purification using valve tower purification system, the valve tower purification system has 2# valve towers 2
With 1# valve towers 1, the bottom of towe discharging opening of the 2# valve towers 2 is connected with titanium tetrachloride finished pot 4, the 2# float valves by pipeline
The tower top discharging opening of tower 2 is connected by pipeline with the tower middle charging aperture of 1# valve towers 1, the 2# valve towers 2,1# valve towers 1
Tower top be respectively equipped with overhead reflux valve II 7, overhead reflux valve I 6, the tower middle charging aperture of the 2# valve towers 2 is by pipe
Road is connected with titanium tetrachloride head tank 3, and material inlet valve II in tower is provided with the pipeline of the tower middle charging aperture near 2# valve towers 2
9, material inlet valve I 8, the 2# valve towers 2 and 1# float valves in tower is provided with the pipeline of the tower middle charging aperture near 1# valve towers 1
Pipeline between tower 1 is provided with a tower top effluent storage tank 5, outlet at bottom and the titanium tetrachloride raw material of the 1# valve towers 1
Tank 3 is connected by pipeline;The discharging of bottom of towe outlet valve II 11, bottom of towe is respectively equipped with the bottom of towe of 2# valve towers 2,1# valve towers 1
Valve I 10.
The increase valve tower production capacity, the method for operating for reducing energy consumption of unit product, comprise the following steps that:
1st, on the basis of normally having overhead reflux operation, by 2# valve towers 2Overhead reflux valve II 7 is closed
Close, it is to avoid overhead flows back into 2# valve towers 2, cause the evaporation repeatedly and condensation of rectifying section;
2nd, material inlet valve II 9 in tower is opened, the titanium tetrachloride raw material of titanium tetrachloride head tank 3 is sent in 2# valve towers 2, passed through
Material inlet valve II 9 incrementally increases feeding quantity in tower in control tower, and by 2.91 ton hours, (feeding quantity is feeding quantity in 4 hours
Single column purifies feeding quantity) it is gradually increased to 6.25 ton hours;
3rd, temperature drops to 125 DEG C~130 DEG C for 137 DEG C by original (single column purification) in tower;Tower top temperature is by original (single column
Purification) 60 DEG C~90 DEG C be increased to 70 DEG C~120 DEG C;
4th, purification is completed, bottom of towe outlet valve II 11 is opened, (after testing, purity is 99.8%) to send into by the refined titanic chloride of bottom of towe
Titanium tetrachloride finished pot 4, tower top obtains an overhead, and in sending into a tower top effluent recycling can 5, one time tower top evaporates
Go out thing total amount increases to 27 tons/month by original (single column purification) 9 tons/month, and impurity chlorides content is reduced to 20% by 50%,
Titanium tetrachloride primary recovery reaches 99.4%;Titanium tetrachloride product comprehensive energy consumption is that 10kg marks coal/t;
5th, material inlet valve I 8 in tower is opened, using an overhead as raw material, by a tower top effluent recycling can 5 again
Enter 1# valve towers 1Feeding quantity is controlled for 2 ton hours by material inlet valve in control tower I 8;
6th, opening overhead reflux valve I 6,110 DEG C~120 DEG C of temperature in control 1# valve towers 1,60 DEG C~80 DEG C of tower top temperature,
It is 98% to obtain titanium tetrachloride purity, and this stage is without titanium tetrachloride product output;Secondary tower top impurity chlorides purity is 60%,
Discharge standard can be reached;
7th, the bottom of towe of 1# valve towers 1 obtains purity for 98% titanium tetrachloride, the feeding titanium tetrachloride head tank of opening bottom of towe outlet valve I 10
The mixing of 3 titanium tetrachloride raw materials is sent into 2# valve towers 2 and is used as the continuation blending of tower raw material is entered, and titanium tetrachloride secondary returning yield reaches
99.65%.Titanium tetrachloride product comprehensive energy consumption is that 16kg marks coal/t, (this stage 2# valve towers 2 and 1# valve towers 1 have energy consumption,
But 1# valve towers 1 are without product output);By calculating, valve tower containing 1# 1 is without energy consumption during titanium tetrachloride output, product synthesis
Energy consumption is that 12kg marks coal/ton.
When tower top has reflux operation, the production capacity of 2# valve towers 2 is 70 ton days, and product comprehensive energy consumption marks coal/t by 22kg, without tower
During the reflux operation of top, idle 1# valve towers 1 (2# valve towers 2 significantly improve production capacity, and 1# valve towers 1 are left unused) are needed to carry out
Coordinate, product comprehensive energy consumption is reduced to 12kg mark coal/t.
Embodiment 2
As illustrated, carrying out titanium tetrachloride purification using valve tower purification system, valve tower purification system is with embodiment 1.
The increase valve tower production capacity, the method for operating for reducing energy consumption of unit product, comprise the following steps that:
1st, opening tower operational procedure by valve tower carries out opening tower operation, starts 2# valve towers 2Close tower top to return
Stream valve II 7, when tower top temperature is increased to 60 DEG C, opens material inlet valve II 9 in tower, by the tetrachloro of titanium tetrachloride head tank 3
Change titanium material to send in 2# valve towers 2;
2nd, feeding quantity in tower is incrementally increased by material inlet valve in control tower II 9, in 4 hours feeding quantity by 3 ton hours gradually
Bring up to 6 ton hours;
3rd, in the tower of 2# valve towers 2 temperature control at 125 DEG C~130 DEG C;Tower top temperature is controlled 70 DEG C~120;
4th, purification is completed, bottom of towe outlet valve II 11 is opened, (after testing, purity is 99.8%) to send into by the refined titanic chloride of bottom of towe
Titanium tetrachloride finished pot 4, tower top obtains an overhead, and in sending into a tower top effluent recycling can 5, one time tower top evaporates
It is 27.4 tons/month to go out thing total amount, wherein, impurity chlorides are 20% in an overhead, titanium tetrachloride primary recovery
Reach 99.28%;Titanium tetrachloride product comprehensive energy consumption is that 10kg marks coal/t;
5th, material inlet valve I 8 in tower is opened, using an overhead as raw material, by a tower top effluent recycling can 5 again
Enter 1# valve towers 1Feeding quantity is controlled for 1.1 ton hours by material inlet valve in control tower I 8;
6th, opening overhead reflux valve I 6,110 DEG C~120 DEG C of temperature in control 1# valve towers 1,60 DEG C~80 DEG C of tower top temperature,
It is 98% to obtain titanium tetrachloride purity, and this stage is without titanium tetrachloride product output;Secondary tower top impurity chlorides purity is 60%,
Discharge standard can be reached;
7th, the bottom of towe of 1# valve towers 1 obtains purity for 98% titanium tetrachloride, the feeding titanium tetrachloride head tank of opening bottom of towe outlet valve I 10
The mixing of 3 titanium tetrachloride raw materials is sent into 2# valve towers 2 and is used as the continuation blending of tower raw material is entered, and titanium tetrachloride secondary returning yield reaches
99.65%;Titanium tetrachloride product comprehensive energy consumption is that 16kg marks coal/t, (this stage 2# valve towers 2 and 1# valve towers 1 have energy consumption,
But 1# valve towers 1 are without product output);By calculating, valve tower containing 1# 1 is without energy consumption during titanium tetrachloride output, product synthesis
Energy consumption is that 12kg marks coal/ton.
When tower top has reflux operation, the production capacity of 2# valve towers 2 is 70 ton days, and product comprehensive energy consumption marks coal/t by 22kg, without tower
During the reflux operation of top, idle 1# valve towers 1 (2# valve towers 2 significantly improve production capacity, and 1# valve towers 1 are left unused) are needed to carry out
Coordinate, product comprehensive energy consumption is reduced to 12kg mark coal/t.
The specific embodiment of the present invention is these are only, the present invention is not limited to, for those skilled in the art
For member, the present invention can have various modifications and variations.All any modifications within the spirit and principles in the present invention, made,
Equivalent, improvement etc., should be included within the scope of the present invention.