阅读说明：本技术 一种获取连续高温氯气的加热方法 (Heating method for obtaining continuous high-temperature chlorine ) 是由 温良英 王建鑫 周艾然 岳东 刘波 赵岩 于 2021-07-30 设计创作，主要内容包括：本发明涉及一种获取连续高温氯气的加热方法,包括如下步骤：1)向石墨管道中连续通入惰性气体,并利用感应加热器将石墨管道加热至800～1750℃；2)将连续通入石墨管道中的气体切换成氯气或混合气体,所述混合气体由氯气和惰性气体组成；3)利用感应加热器持续加热石墨管道,并调节感应加热器的输出功率,石墨管道连续输出700～1600℃的高温氯气或高温混合气体。本发明中,有效利用在700～1600℃下,氯气和石墨不反应以及石墨管道导热好的特性对氯气进行加热,通过调节气体流速和加热温度,从而获得温度和浓度可调的连续高温氯气；通入沸腾氯化炉后可提升分布板区附近的气速,从而提升流化质量,取得沸腾氯化炉可长周期、高效率稳定运行的效果。(The invention relates to a heating method for obtaining continuous high-temperature chlorine, which comprises the following steps: 1) continuously introducing inert gas into the graphite pipeline, and heating the graphite pipeline to 800-1750 ℃ by using an induction heater; 2) switching gas continuously introduced into the graphite pipeline into chlorine or mixed gas, wherein the mixed gas consists of chlorine and inert gas; 3) the graphite pipeline is continuously heated by the induction heater, the output power of the induction heater is adjusted, and the graphite pipeline continuously outputs high-temperature chlorine or high-temperature mixed gas at 700-1600 ℃. According to the invention, the chlorine gas is heated by effectively utilizing the characteristics that the chlorine gas and graphite do not react at 700-1600 ℃ and the graphite pipeline has good heat conduction, and the continuous high-temperature chlorine gas with adjustable temperature and concentration is obtained by adjusting the gas flow rate and the heating temperature; the gas velocity near the distribution plate area can be increased after the gas is introduced into the boiling chlorination furnace, so that the fluidization quality is improved, and the effect that the boiling chlorination furnace can stably run for a long period and with high efficiency is obtained.)

1. A heating method for obtaining continuous high-temperature chlorine gas is characterized in that: the method comprises the following steps:

1) continuously introducing inert gas into the graphite pipeline, and heating the graphite pipeline to 800-1750 ℃ by using an induction heater;

2) changing gas continuously introduced into the graphite pipeline into chlorine or mixed gas, wherein the mixed gas consists of chlorine and inert gas;

3) the graphite pipeline is continuously heated by the induction heater, and the output power of the induction heater is adjusted, so that the graphite pipeline continuously outputs high-temperature chlorine gas or high-temperature mixed gas at 700-1600 ℃.

2. The heating method for obtaining continuous high-temperature chlorine gas according to claim 1, characterized in that: after the step 3), the operation when the graphite pipeline needs to stop outputting the high-temperature chlorine or the high-temperature mixed gas comprises the following steps:

4) switching the gas introduced into the graphite pipeline into inert gas, and closing the induction heater after the design duration;

5) and stopping introducing the inert gas into the graphite pipeline when the temperature of the graphite pipeline is lower than 300 ℃.

3. The heating method for obtaining continuous high-temperature chlorine gas according to claim 1, characterized in that: the graphite pipeline is in a straight pipe, a tube array or a coil pipe structure.

4. The heating method for obtaining continuous high-temperature chlorine gas according to claim 1, characterized in that: the inert gas is one or more of nitrogen, helium, neon and argon.

5. The heating method for obtaining continuous high-temperature chlorine gas according to claim 1, characterized in that: the induction heater is a medium-frequency induction heater or a high-frequency induction heater.

6. The heating method for obtaining continuous high-temperature chlorine gas according to claim 1, characterized in that: the volume fraction of chlorine in the mixed gas is 0-100%, and the volume fraction of chlorine in the correspondingly obtained high-temperature mixed gas corresponds to the volume fraction of chlorine in the mixed gas.

7. The heating method for obtaining continuous high-temperature chlorine gas according to claim 3, characterized in that: the graphite pipeline is a straight pipe, the length of the straight pipe is 0.5-2 m, the inner diameter of the straight pipe is 20-50 mm, and the wall thickness of the straight pipe is 5-30 mm.

8. The heating method for obtaining continuous high-temperature chlorine gas according to claim 3, characterized in that: the graphite pipeline is a coil pipe, the outer diameter of the coil pipe is 0.3-1 m, the total length of the coil pipe is 2-20 m, the inner diameter of the pipeline is 20-50 mm, and the wall thickness of the pipeline is 5-30 mm.

9. The heating method for obtaining continuous high-temperature chlorine gas according to claim 3, characterized in that: the graphite pipeline is a tube array, the outer diameter of the whole sleeve is 0.3-1 m, the total length of all the tube arrays is 2-50 m, the inner diameter of each tube array is 20-50 mm, and the wall thickness of the pipeline is 5-30 mm.

Technical Field

The invention belongs to the technical field of chlorination processes, and particularly relates to a heating method for obtaining continuous high-temperature chlorine.

Background

At present, titanium-containing slag, zircon sand, high-alumina fly ash and quartz sand are generally added into a boiling chlorination furnace in industry, then normal-temperature chlorine is introduced into the boiling chlorination furnace to perform a carbon-adding chlorination reaction to generate TiCl4, ZrCl4, AlCl3 and SiCl4 gases, and the gases are further reacted to produce products such as sponge titanium, sponge zirconium, aluminum silicate powder, white carbon black and the like.

Because the chlorine gas at normal temperature is not completely heated when entering the boiling chlorination furnace, and the temperature of the chlorine gas is lower, the operating gas velocity near a distribution plate area in the boiling chlorination furnace is lower, and particle dead zones are larger, so that the problems of poor fluidization quality, low chlorination rate, particle adhesion and loss flow and the like in the boiling chlorination furnace are caused, and the long-period, high-efficiency and stable operation of the boiling chlorination furnace is severely restricted.

The high-temperature chlorine gas is introduced into the boiling chlorination furnace, the operating gas speed near a distribution plate area in the boiling chlorination furnace can be effectively improved, the fluidization quality and the reaction efficiency can be improved, meanwhile, the high-temperature chlorine gas can supplement heat for the boiling chlorination furnace, and the condition that the chlorination reaction heat is insufficient is avoided. Chinese patent CN202022159981.8 discloses a heat exchanger for high-purity hydrogen chloride and chlorine, chinese patent CN201220389897.8 discloses a liquid chlorine gasification system, chinese patent CN201821804804.7 discloses a liquid chlorine vaporization heat exchanger, and chinese patent CN201620277906.2 discloses a device or method for chlorine heat exchange, chlorine vaporization or chlorine recovery in a high-temperature-resistant chlorine absorption tower, but does not relate to a method for obtaining continuous high-temperature chlorine.

Therefore, how to obtain continuous high-temperature chlorine gas, the high-temperature chlorine gas is introduced into the boiling chlorination furnace to improve the fluidization quality near the distribution plate area and supplement heat, which is a key problem for optimizing and developing the chlorination process.

Disclosure of Invention

Aiming at the defects in the prior art, the technical problem to be solved by the invention is to provide a heating method for obtaining continuous high-temperature chlorine, solve the problems of poor fluidization quality and low reaction efficiency caused by using normal-temperature chlorine for chlorination at present, and obtain the effect that a boiling chlorination furnace can stably run for a long period and with high efficiency.

In order to solve the technical problems, the invention adopts the following technical scheme: a heating method for obtaining continuous high-temperature chlorine gas comprises the following steps:

1) continuously introducing inert gas into the graphite pipeline, and heating the graphite pipeline to 800-1750 ℃ by using an induction heater;

2) switching gas continuously introduced into the graphite pipeline into chlorine or mixed gas, wherein the mixed gas consists of chlorine and inert gas;

3) the graphite pipeline is continuously heated by the induction heater, the output power of the induction heater is adjusted, and the graphite pipeline continuously outputs high-temperature chlorine or high-temperature mixed gas at 700-1600 ℃.

Further, after the step 3), the operation of stopping the graphite pipeline from outputting the high-temperature chlorine gas or the high-temperature mixed gas comprises the following steps:

4) switching the gas introduced into the graphite pipeline into inert gas, and closing the induction heater after a period of time;

5) and stopping introducing the inert gas into the graphite pipeline when the temperature of the graphite pipeline is lower than 300 ℃.

Therefore, no matter the induction heater is firstly closed after the step 3), or the introduction of chlorine gas into the graphite pipeline is firstly stopped, chlorine gas which is not effectively heated can enter the boiling chlorination furnace or a certain amount of chlorine gas remains in the graphite pipeline, and when the graphite pipeline is used next time, chlorine gas which is not effectively heated can still enter the boiling chlorination furnace; and through the step 4) and the step 5), the chlorine gas introduced into the boiling chlorination furnace can be guaranteed to be high-temperature chlorine gas after being effectively heated, and the chlorine gas in the graphite pipeline can be completely emptied, so that the next use is facilitated.

Further, the graphite pipeline is in a straight pipe, a tube array or a coil pipe structure.

Like this, use graphite material pipeline, have good heat conductivility, effectively heat the graphite pipeline and give chlorine with heat transfer through induction heater to obtain continuous high temperature chlorine.

Further, the inert gas is one or more of nitrogen, helium, neon and argon.

Thus, inert gas is used as gas which is introduced into the graphite pipeline at the beginning and the end, and unheated chlorine gas is prevented from entering the boiling chlorination furnace.

Further, the induction heater is a medium frequency induction heater or a high frequency induction heater.

Therefore, the medium-frequency or high-frequency induction heater is used for heating, the chlorine temperature can be adjusted by adjusting the output power of the induction heater, the operation is simple and convenient, and the control is reliable.

Further, the volume fraction of chlorine in the mixed gas is 0-100%.

Therefore, the volume fraction of the chlorine is adjusted by adjusting the flow rates of the inert gas and the chlorine, so that high-temperature chlorine with different concentrations is output to meet the production requirement.

Compared with the prior art, the invention has the following beneficial effects:

1. according to the invention, continuous high-temperature chlorine can be obtained; the characteristic that chlorine and graphite do not react under 700 ~ 1600 ℃ high temperature has effectively been utilized, uses graphite material pipeline, has good heat conductivility, effectively heats the graphite pipeline and gives chlorine with heat transfer through induction heater to obtain continuous high temperature chlorine.

2. In the invention, the temperature of the high-temperature chlorine gas is adjustable; the chlorine gas temperature can be adjusted by adjusting the output power of the induction heater by using a medium-frequency or high-frequency induction heater for heating, and the device is simple and convenient to operate and reliable to control.

3. In the invention, the concentration of the high-temperature chlorine is adjustable; the inert gas and the chlorine are heated in the graphite pipeline, the high-temperature chlorine concentration adjustment is realized by adjusting the flow rate of the inert gas or the chlorine, the operation is simple and convenient, and the control is reliable.

4. In the invention, beneficial reference is provided for the process optimization of the boiling chlorination furnace; the high-temperature chlorine gas is introduced into the boiling chlorination furnace, so that the gas velocity near the distribution plate area can be increased, and the fluidization quality is further improved; meanwhile, the heat can be supplemented to the chlorination furnace with insufficient reaction heat, and the establishment of steady-state heat balance is facilitated.

Drawings

FIG. 1 is a schematic process diagram of a heating method for obtaining continuous high temperature chlorine gas according to an embodiment;

FIG. 2 is a block flow diagram of a heating process for obtaining continuous high temperature chlorine gas according to an embodiment;

the induction heating device comprises an induction heater 1 and a graphite pipeline 2.

Detailed Description

The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.

The first embodiment is as follows:

referring to fig. 1 and 2, firstly, a graphite pipeline 2 with a length of 0.5-2 m, an inner diameter of 20-50 mm and a wall thickness of 5-30 mm is taken, the graphite pipeline 2 is placed in a heating coil of a medium-frequency induction heater 1, and two ends of the graphite pipeline 2 extend out of the heating coil;

then, continuously introducing nitrogen with the flow speed of 5-10 m3/h from one end of the graphite pipeline 2, allowing the nitrogen to flow out from the other end (for introducing into a boiling chlorination furnace), and starting the induction heater 1 to continuously heat the graphite pipeline 2 to 1000 ℃;

then, the induction heater 1 continuously heats the graphite pipeline 2, chlorine gas and nitrogen gas with the flow speed of 5-10 m3/h are mixed and continuously introduced from one end of the graphite pipeline 2, and then flow out from the other end of the heated graphite pipeline 2 to obtain continuous high-temperature chlorine gas;

wherein the flow rate of the nitrogen and the flow rate of the chlorine can be respectively adjusted to obtain high-temperature chlorine with the volume fraction of the chlorine being 0-40%; the output power of the induction heater 1 can be adjusted to obtain high-temperature chlorine gas at 700-1200 ℃;

finally, before stopping obtaining the high-temperature chlorine gas, firstly adjusting the flow speed of the nitrogen gas to 5-10 m³Stopping introducing chlorine slowly; when the chlorine completely stops being introduced into the graphite pipeline 2 for a period of time, the induction heater 1 is stopped, so that the high-temperature chlorine is stopped being output; and finally, when the temperature of the graphite tube is lower than 300 ℃, closing the nitrogen introduction.

Example two:

firstly, taking a graphite coil (a disc-shaped graphite pipeline 1) with the outer diameter of 0.3-1 m, the total length of the pipeline of 2-20 m, the inner diameter of the pipeline of 20-50 mm and the wall thickness of 5-30 mm, placing the graphite coil in a heating coil of a medium-frequency or high-frequency induction heater 1, and extending two ends of the graphite coil out of the heating coil;

then, the flow rate is set to be 5-10 m³Continuously introducing nitrogen gas from one end of the graphite coil pipe, enabling the nitrogen gas to flow out from the other end of the graphite coil pipe, and starting the induction heater 1 to continuously heat the graphite coil pipe to 1200 ℃;

then, the induction heater 1 continuously heats the graphite coil pipe, and the flow velocity is 5-10 m³Mixing chlorine gas and nitrogen gas for continuous introduction from one end of the graphite coil pipe, and then flowing out from the other end of the heated graphite coil pipe to obtain continuous high-temperature chlorine gas;

wherein the flow rate of the nitrogen and the flow rate of the chlorine can be respectively adjusted to obtain high-temperature chlorine with the volume fraction of the chlorine being 30-70%; the output power of the induction heater 1 can be adjusted to obtain high-temperature chlorine gas at 1000-1400 ℃;

finally, before stopping obtaining the high-temperature chlorine gas, firstly adjusting the flow speed of the nitrogen gas to 5-10 m³Stopping introducing chlorine slowly; when the chlorine completely stops being introduced into the graphite coil for a period of time, stopping the induction heater 1, and stopping outputting the high-temperature chlorine; and finally, when the temperature of the graphite coil is lower than 300 ℃, closing the nitrogen introduction.

Example three:

firstly, taking a set of graphite tubes (a graphite pipeline 1 in a row shape), wherein the outer diameter of the whole set of tubes is 0.3-1 m, the total length of all the tubes is 2-50 m, the inner diameter of each tube is 20-50 mm, the wall thickness of each tube is 5-30 mm, the whole set of graphite tubes are placed in a heating coil of a medium-frequency or high-frequency induction heater 1, and two ends of the whole set of graphite tubes extend out of the heating coil;

continuously introducing nitrogen with the flow rate of 5-10 m3/h from one end of the whole set of graphite tubes, allowing the nitrogen to flow out from the other end of the whole set of graphite tubes, and starting the induction heater 1 to continuously heat the whole set of graphite tubes to 1400 ℃;

the induction heater 1 continuously heats the whole set of graphite array tubes, and the flow velocity is 5-10 m³Mixing chlorine gas and nitrogen gas, continuously introducing the chlorine gas and the nitrogen gas from one end of the graphite tube array, and then flowing out from the other end of the heated graphite tube array to obtain continuous high-temperature chlorine gas;

adjusting the flow rate of the nitrogen and the flow rate of the chlorine respectively to obtain high-temperature chlorine with the volume fraction of the chlorine being 60-100%; the output power of the induction heater 1 can be adjusted to obtain high-temperature chlorine gas at 1000-1600 ℃;

finally, before stopping obtaining the high-temperature chlorine gas, firstly adjusting the flow speed of the nitrogen gas to 5-10 m³Stopping introducing chlorine slowly; when the chlorine completely stops being introduced into the graphite tube nest for a period of time, stopping the induction heater 1, and stopping outputting the high-temperature chlorine; and finally, when the temperature of the graphite tube is lower than 300 ℃, closing the nitrogen introduction.

The method can obtain continuous, temperature-adjustable and concentration-adjustable high-temperature chlorine gas, and provides beneficial reference for the process optimization of the boiling chlorination furnace; the high-temperature chlorine gas is introduced into the boiling chlorination furnace, so that the gas velocity near the distribution plate area can be increased, and the fluidization quality is further improved; meanwhile, the heat can be supplemented to the chlorination furnace with insufficient reaction heat, and the establishment of steady-state heat balance is facilitated.

Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.