CN113184900B - Titanium tetrachloride production method and system and raw material ratio adjusting method - Google Patents
Titanium tetrachloride production method and system and raw material ratio adjusting method Download PDFInfo
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- CN113184900B CN113184900B CN202110515530.XA CN202110515530A CN113184900B CN 113184900 B CN113184900 B CN 113184900B CN 202110515530 A CN202110515530 A CN 202110515530A CN 113184900 B CN113184900 B CN 113184900B
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- C01G23/022—Titanium tetrachloride
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Abstract
The invention discloses a titanium tetrachloride production method, a titanium tetrachloride production system and a raw material ratio adjusting method. According to the invention, the chlorine concentration detection device is added behind the leaching system to adjust the addition of the chlorine and the addition of the titanium-containing raw material, so that the adjustment precision and time can be greatly improved, the reaction efficiency is improved, the consumption of the chlorine and the raw material is reduced, and the alkali liquor consumption of the tail gas treatment system is reduced.
Description
Technical Field
The invention relates to the technical field of titanium white chloride production, in particular to a titanium tetrachloride production method, a titanium tetrachloride production system and a method for adjusting the proportion of chlorine and a titanium-containing raw material in a titanium tetrachloride chlorination system.
Background
Titanium tetrachloride is the main raw material of titanium dioxide, titanium sponge and other industrial products in chlorination process, two main production methods at home and abroad are boiling chlorination and molten salt chlorination, titanium-containing raw materials and chlorine react at high temperature to generate titanium tetrachloride, wherein the proportion of the chlorine and the raw materials is the key point to be controlled, and the adjustment of the chlorine amount in the existing boiling chlorination or molten salt chlorination is mainly realized by sampling and detecting the Ti component of materials in a reactor, adjusting the adding amount of the raw materials and relatively delaying the adjustment.
Based on this, the prior art still remains to be improved.
Disclosure of Invention
In order to solve the technical problems, the embodiment of the invention provides a titanium tetrachloride production method, a titanium tetrachloride production system and a method for adjusting the proportion of chlorine and a titanium-containing raw material in a titanium tetrachloride chlorination system. The technical problems of complex and lagging adjusting method in the prior art are solved. By adding the chlorine concentration detection device behind the reactor, the adjustment precision and time can be greatly improved, the reaction efficiency is improved, the consumption of chlorine and raw materials is reduced, and the alkali liquor consumption of a tail gas treatment system is reduced.
On one hand, according to the method for adjusting the proportion of chlorine and the titanium-containing raw material in the chlorination system disclosed by the embodiment of the invention, the concentration of chlorine in the leached tail gas is detected to obtain the detection concentration of chlorine, and the addition of chlorine and the addition of the titanium-containing raw material are adjusted according to the detection concentration of chlorine.
And further, determining an adjustment scheme of the addition of the chlorine and the addition of the titanium-containing raw material according to the detection concentration of the chlorine and the height of the bed layer in the chlorination furnace.
Further, the height of the bed in the chlorination furnace is determined by measuring the temperature at different heights in the chlorination furnace.
Further, when the chlorine detection concentration is in the range of 0.5-5% and the height of the bed layer is not lower than 80% of the total height of the chlorination furnace, the addition amount of the chlorine and the addition amount of the titanium-containing raw material are not adjusted.
Further, when the chlorine detection concentration is lower than 0.5% and the height of the bed layer is not lower than 80% of the total height of the chlorination furnace, gradually increasing the adding amount of the chlorine until the chlorine detection concentration reaches 0.5-5%.
Further, the adding amount of the chlorine gas which is gradually increased is 50-100kg/h per time.
Further, when the chlorine detection concentration is higher than 5% and the bed height is lower than 80% of the total height of the chlorination furnace, gradually increasing the adding amount of the titanium-containing raw material until the bed height is not lower than 80% of the total height of the chlorination furnace;
at this time, if the chlorine detection concentration is recovered to 0.5-5%, the adjustment is stopped, and if the chlorine detection concentration is higher than 5%, the adding amount of the chlorine is gradually reduced until the chlorine detection concentration is recovered to 0.5-5%.
Further, the adding amount of the titanium-containing raw material is gradually increased to be 0.5 to 1t/h each time; the gradual reduction of the addition of the chlorine gas is 50-100kg/h each time.
On the other hand, the embodiment of the invention also discloses a production method of titanium tetrachloride, which adopts the adjusting method to adjust the adding amount of chlorine and the adding amount of the titanium-containing raw material.
In a third aspect, the embodiment of the invention also discloses a titanium tetrachloride production system, which comprises a chlorination furnace, a cyclone separator, a leaching system, a tail gas detection device, a titanium-containing raw material adding device and a chlorine adding device which are sequentially connected,
the tail gas detection device is used for detecting the concentration of chlorine in the tail gas passing through the leaching system; a bed height detection device is arranged in the chlorination furnace; the titanium-containing raw material adding device is communicated with a titanium-containing raw material adding port of the chlorination furnace; the chlorine adding device is communicated with a chlorine adding port of the chlorination furnace;
the titanium-containing raw material adding device and the chlorine adding device adjust the adding amount of the titanium-containing raw material and the chlorine based on the detection result of the tail gas detection device and the detection result of the bed height detection device.
By adopting the technical scheme, the invention at least has the following beneficial effects:
according to the invention, the chlorine concentration detection device is added behind the leaching system to adjust the addition of the chlorine and the addition of the titanium-containing raw material, so that the adjustment precision and time can be greatly improved, the reaction efficiency is improved, the consumption of the chlorine and the raw material is reduced, and the alkali liquor consumption of the tail gas treatment system is reduced.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a schematic structural view of a titanium tetrachloride production system according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following embodiments of the present invention are described in further detail with reference to the accompanying drawings.
It should be noted that all expressions using "first" and "second" in the embodiments of the present invention are used for distinguishing two entities with the same name but different names or different parameters, and it should be noted that "first" and "second" are merely for convenience of description and should not be construed as limitations of the embodiments of the present invention, and they are not described in any more detail in the following embodiments.
As shown in figure 1, some embodiments of the invention disclose a titanium tetrachloride production system, which comprises a chlorination furnace 3, a cyclone separator 4, a leaching system 5, a tail gas detection device 6, a titanium-containing raw material adding device 1 and a chlorine adding device 2 which are sequentially connected,
the tail gas detection device 6 is used for detecting the concentration of chlorine in the tail gas passing through the leaching system 5; a bed height detection device is arranged in the chlorination furnace 3; the titanium-containing raw material adding device 1 is communicated with a titanium-containing raw material adding port of the chlorination furnace 3; the chlorine adding device 2 is communicated with a chlorine adding port of the chlorination furnace 3;
the titanium-containing raw material adding device 1 and the chlorine adding device 2 adjust the adding amount of the titanium-containing raw material and the chlorine based on the detection result of the tail gas detection device 6 and the detection result of the bed height detection device.
The titanium tetrachloride production system that this embodiment provided through increase chlorine concentration detection device behind the reactor, can improve the adjustment precision and the time of chlorine addition and titanium-containing raw materials addition greatly, improve reaction efficiency, reduce chlorine and titanium-containing raw materials consumption, reduce tail gas processing system's alkali lye consumption simultaneously.
Based on the system, the embodiment of the invention also discloses a titanium tetrachloride production method and a method for adjusting the proportion of chlorine and a titanium-containing raw material in a chlorination system. Specifically, when the concentration of chlorine in the leached tail gas is higher than the preset value, the addition proportion of chlorine is considered to be too large, and at the moment, the addition amount of chlorine is properly reduced or the addition amount of the titanium-containing raw material is increased. When the concentration of the chlorine in the leached tail gas is lower than the preset value, the adding proportion of the chlorine is considered to be too small, and at the moment, the adding amount of the chlorine can be properly increased or the adding amount of the titanium-containing raw material can be reduced. The chlorine content in the tail gas is continuously monitored or monitored at preset time intervals, so that the adjustment of the chlorine adding amount and the titanium-containing raw material adding amount can be realized in time.
In the above-described embodiment, the adjustment of the amount of chlorine gas to be added and the amount of the raw material containing titanium to be added are further determined based on the detected concentration of chlorine gas in combination with the height of the bed in the chlorination furnace 3. Specifically, the bed height in the chlorination furnace 3 can be determined by measuring the temperature at different heights in the chlorination furnace 3. Temperature detection devices 7 can be arranged at different heights in the chlorination furnace 3 to monitor different temperatures, and the bed height is judged according to the temperature of each height. When the height of the bed layer is higher than a preset value and the concentration of chlorine in the tail gas is too high, the adding proportion of chlorine and the titanium-containing raw material is generally adjusted only by reducing the adding amount of chlorine; when the height of the bed layer is lower than a set value and the concentration of the chlorine is too high, the adding proportion of the chlorine and the titanium-containing raw material can be adjusted by increasing the amount of the titanium-containing principle, and the adding proportion of the chlorine and the titanium-containing raw material can be adjusted by combining the adding amount of the titanium-containing principle with the adding amount of the chlorine, so that the adding proportion of the chlorine and the titanium-containing raw material can be adjusted. Further, the adjustment of the chlorine and titanium containing principles is effectively quantitative batch-wise adjusted.
In some embodiments, as shown in FIG. 1, the bed height is determined by the temperature of a thermometer (T1-T5) at different positions, and if the corresponding temperature indicates that the reaction temperature is reached (above 400 ℃), the bed level is determined to have reached the height, T1 corresponds to 10% level, and T2-T5 correspond to 20% -80% level, respectively.
Specifically, according to the method for adjusting the ratio of chlorine to the titanium-containing raw material in the chlorination system disclosed in some embodiments of the present invention, when the detected concentration of chlorine is in the range of 0.5% to 5% and the height of the bed layer is not lower than 80% of the total height of the chlorination furnace, the addition amount of chlorine and the addition amount of the titanium-containing raw material are not adjusted, wherein the total height of the chlorination furnace refers to the height of the chlorination furnace for reaction, rather than the total height of the chlorination furnace;
when the chlorine detection concentration is lower than 0.5% and the height of the bed layer is not lower than 80% of the total height of the chlorination furnace, gradually increasing the addition of the chlorine until the chlorine detection concentration reaches 0.5-5%, so that the reaction rate of the raw materials can be gradually adjusted to an optimal state, and the utilization rate of the raw materials is improved;
the adding amount of the chlorine gas is gradually increased to 50-100kg/h each time;
when the chlorine detection concentration is higher than 5% and the bed height is lower than 80% of the total height of the chlorination furnace, gradually increasing the addition of the titanium-containing raw material until the bed height is not lower than 80% of the total height of the chlorination furnace;
at the moment, if the chlorine detection concentration is recovered to 0.5-5%, stopping adjustment, and if the chlorine detection concentration is higher than 5%, gradually reducing the addition of chlorine until the chlorine detection concentration is recovered to 0.5-5%, so that the chlorine content level can be reduced and controlled within a controllable range, and the subsequent tail gas system alkali liquor consumption is reduced.
In some preferred embodiments, the stepwise increase in the amount of titaniferous feed material added is from 0.5 to 1t/h per increase; the gradual reduction of the addition of the chlorine gas is 50-100kg/h each time.
The embodiment of the invention discloses a titanium tetrachloride production system, which comprises the following main process flows:
in the production process of the chlorination furnace, when a chlorine concentration detector (tail gas detection device) detects that the chlorine concentration in the tail gas is increased or reduced, the addition of chlorine or raw materials is adjusted according to the height of a bed layer in the chlorination furnace, and the method specifically comprises the following steps:
1. when the detected chlorine concentration is 0.5-5%, the height of the bed layer is more than 80% of the total height of the chlorination furnace (total height in the furnace) without adjustment.
2. When the concentration of the chlorine is lower than 0.5% and the height of the inner bed layer of the chlorination furnace is higher than 80% of the total height of the chlorination furnace, gradually increasing the addition amount of the chlorine by 50-100kg/h each time until the concentration of the chlorine is restored to be within the range of 0.5-5%.
3. When the concentration of chlorine is more than 5% and the height of the bed layer in the chlorination furnace is lower than 80% of the total height of the chlorination furnace, increasing the adding amount of the titanium-containing raw material by 0.5-1t/h every time until the height of the bed layer is recovered to be not lower than 80% of the total height of the chlorination furnace, stopping adjustment if the chlorine is recovered to be 0.5-5%, and gradually reducing the adding amount of the chlorine by 50-100kg/h every time until the detection concentration is recovered to be lower than 5% if the height of the bed layer is not lower than 80% of the total height of the chlorination furnace and still exceeds 5%.
In summary, the titanium tetrachloride production system, the titanium tetrachloride production method, and the chlorine and titanium-containing raw material ratio adjusting method of the chlorination system disclosed in the embodiments of the present invention are suitable for titanium tetrachloride production systems in the titanium white chloride industry or the titanium sponge industry. The whole system comprises a chlorine pipeline, an adjusting system (namely a chlorine adding device), a raw material feeding system (namely a titanium-containing raw material adding device), a chlorination furnace, a thermometer (for detecting the temperatures of different heights in the chlorination furnace), a cyclone (for realizing the separation after the discharge of the chlorination furnace), a leaching system, a chlorine detecting device (namely a tail gas detecting device), a fan 8 and the like. The fan can be arranged at the downstream of the tail gas detection device, and the tail gas is discharged after passing through the fan 8. And the tail gas detection system detects the concentration of chlorine in the tail gas after the chlorination furnace flue gas is subjected to leaching. Determining the height of a bed layer in the chlorination furnace according to thermometers with different heights in the chlorination furnace, if the height of the bed layer is abnormal, and simultaneously detecting that the concentration of chlorine exceeds a control range, adjusting the addition amount of the raw materials, and if the height of the bed layer is normal, adjusting the addition amount of the chlorine.
It should be particularly noted that the various components or steps in the above embodiments can be mutually intersected, replaced, added or deleted, and therefore, the combination formed by the reasonable permutation and combination conversion shall also belong to the protection scope of the present invention, and the protection scope of the present invention shall not be limited to the embodiments.
The above is an exemplary embodiment of the present disclosure, and the order of disclosure of the above embodiment of the present disclosure is only for description and does not represent the merits of the embodiment. It should be noted that the discussion of any embodiment above is exemplary only, and is not intended to intimate that the scope of the disclosure, including the claims, of embodiments of the invention is limited to those examples, and that various changes and modifications may be made without departing from the scope, as defined in the claims. The functions, steps and/or actions of the method claims in accordance with the disclosed embodiments described herein need not be performed in any particular order. Furthermore, although elements of the disclosed embodiments of the invention may be described or claimed in the singular, the plural is contemplated unless limitation to the singular is explicitly stated.
Those of ordinary skill in the art will understand that: the discussion of any embodiment above is meant to be exemplary only, and is not intended to intimate that the scope of the disclosure, including the claims, of embodiments of the invention is limited to these examples; within the idea of an embodiment of the invention, also technical features in the above embodiment or in different embodiments may be combined and there are many other variations of the different aspects of an embodiment of the invention as described above, which are not provided in detail for the sake of brevity. Therefore, any omissions, modifications, substitutions, improvements, and the like that may be made without departing from the spirit and principles of the embodiments of the present invention are intended to be included within the scope of the embodiments of the present invention.
Claims (5)
1. A method for adjusting the proportion of chlorine and a titanium-containing raw material in a chlorination system is characterized in that the concentration of chlorine in tail gas after washing is detected to obtain the detection concentration of chlorine, and the addition of the chlorine and the addition of the titanium-containing raw material are adjusted according to the detection concentration of the chlorine;
determining an adjustment scheme of the addition of the chlorine and the addition of the titanium-containing raw material according to the detection concentration of the chlorine and the height of the bed layer in the chlorination furnace;
the bed height in the chlorination furnace is determined by measuring the temperature at different heights in the chlorination furnace;
when the chlorine detection concentration is within the range of 0.5-5% and the height of the bed layer is not lower than 80% of the total height of the chlorination furnace, the addition amount of the chlorine and the addition amount of the titanium-containing raw material are not adjusted;
when the chlorine detection concentration is lower than 0.5% and the height of the bed layer is not lower than 80% of the total height of the chlorination furnace, gradually increasing the addition of the chlorine until the chlorine detection concentration reaches 0.5-5%;
when the chlorine detection concentration is higher than 5% and the bed height is lower than 80% of the total height of the chlorination furnace, gradually increasing the addition of the titanium-containing raw material until the bed height is not lower than 80% of the total height of the chlorination furnace;
at this time, if the chlorine detection concentration is recovered to 0.5-5%, the adjustment is stopped, and if the chlorine detection concentration is higher than 5%, the adding amount of the chlorine is gradually reduced until the chlorine detection concentration is recovered to 0.5-5%.
2. The process according to claim 1, wherein the stepwise increase in chlorine is carried out in an amount of 50 to 100kg/h per increase.
3. The process according to claim 1, wherein the stepwise increase of the amount of titaniferous feed material added is from 0.5 to 1t/h per increase; the gradual reduction of the addition of the chlorine gas is 50-100kg/h each time.
4. A process for producing titanium tetrachloride, characterized in that the amount of chlorine gas to be added and the amount of the titanium-containing raw material to be added are adjusted by the adjustment method as set forth in any one of claims 1 to 3.
5. A titanium tetrachloride production system is characterized by comprising a chlorination furnace, a cyclone separator, a leaching system, a tail gas detection device, a titanium-containing raw material adding device and a chlorine adding device which are sequentially connected,
the tail gas detection device is used for detecting the concentration of chlorine in the tail gas passing through the leaching system; a bed height detection device is arranged in the chlorination furnace; the titanium-containing raw material adding device is communicated with a titanium-containing raw material adding port of the chlorination furnace; the chlorine adding device is communicated with a chlorine adding port of the chlorination furnace;
the titanium-containing raw material adding device and the chlorine adding device adjust the adding amount of the titanium-containing raw material and the chlorine on the basis of the detection result of the tail gas detection device and the detection result of the bed height detection device; the bed height in the chlorination furnace is determined by measuring the temperature at different heights in the chlorination furnace;
when the chlorine detection concentration is within the range of 0.5-5% and the height of the bed layer is not lower than 80% of the total height of the chlorination furnace, the addition amount of the chlorine and the addition amount of the titanium-containing raw material are not adjusted;
when the chlorine detection concentration is lower than 0.5% and the height of the bed layer is not lower than 80% of the total height of the chlorination furnace, gradually increasing the addition of the chlorine until the chlorine detection concentration reaches 0.5-5%;
when the chlorine detection concentration is higher than 5% and the bed height is lower than 80% of the total height of the chlorination furnace, gradually increasing the addition of the titanium-containing raw material until the bed height is not lower than 80% of the total height of the chlorination furnace;
at this time, if the chlorine detection concentration is recovered to 0.5-5%, the adjustment is stopped, and if the chlorine detection concentration is higher than 5%, the adding amount of the chlorine is gradually reduced until the chlorine detection concentration is recovered to 0.5-5%.
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| CN113651355B (en) * | 2021-09-13 | 2023-01-24 | 攀钢集团钒钛资源股份有限公司 | Titanium dioxide production system and method for distributing chlorine |
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| JP3734687B2 (en) * | 2000-07-05 | 2006-01-11 | 東邦チタニウム株式会社 | Method for producing aqueous titanium tetrachloride solution |
| US7182931B2 (en) * | 2003-02-25 | 2007-02-27 | Tronox Llc | Process for making titanium dioxide |
| CN201538690U (en) * | 2009-10-27 | 2010-08-04 | 攀钢集团研究院有限公司 | Boiling chloridizing furnace feeding device |
| CN103121709A (en) * | 2011-11-18 | 2013-05-29 | 攀钢集团研究院有限公司 | Method for stirring boiling chlorination furnace and method for preparing titanium tetrachloride |
| CN103058270B (en) * | 2012-12-26 | 2014-08-06 | 攀钢集团攀枝花钢铁研究院有限公司 | Control system and control method for low temperature fluidizing chlorination furnace |
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| CN103880076B (en) * | 2013-12-09 | 2016-01-20 | 云南新立有色金属有限公司 | Prepare the system of titanium dioxide |
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