CN113281213A - Vanadium removal efficiency detection method and device - Google Patents
Vanadium removal efficiency detection method and device Download PDFInfo
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Abstract
本发明公开了一种除钒效率检测方法及装置，所述方法包括：将预定量的TiCl4原料置于反应器内加热至沸腾；向所述反应器内加入预定量的除钒试剂进行反应；对从所述反应器排出的蒸汽进行冷凝处理，并将冷凝液引导回所述反应器内进行加热及反应，如此循环；当反应进行预定时间之后，检测所述冷凝液中的钒杂质含量；以及基于反应后的钒杂质含量判断所述除钒试剂的除钒效率。本发明的除钒效率检测方法及装置能够帮助选择合适的除钒试剂。
The invention discloses a method and a device for detecting vanadium removal efficiency. The method comprises: placing a predetermined amount of TiCl4 raw material in a reactor and heating it to boiling; adding a predetermined amount of a vanadium removing reagent into the reactor for reaction ; Condensate the steam discharged from the reactor, and guide the condensate back into the reactor for heating and reaction, and circulate like this; when the reaction is carried out for a predetermined time, detect the vanadium impurity content in the condensate And judge the vanadium-removing efficiency of described vanadium-removing reagent based on the vanadium impurity content after the reaction. The vanadium removal efficiency detection method and device of the present invention can help to select a suitable vanadium removal reagent.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to a vanadium removal efficiency detection method and device.
Background
Titanium tetrachloride is the main raw material for preparing chlorination-process titanium dioxide, titanium sponge and other industrial products, the main production methods at home and abroad comprise a boiling chlorination process and a molten salt chlorination process, titanium tetrachloride is generated by the reaction of titanium dioxide-containing raw materials and chlorine at high temperature, and the titanium tetrachloride generated by the reaction contains more impurities, mainly VOCl3、FeCl3Etc. therefore, it is necessary toAnd (5) purifying in a refining system.
How to select a proper vanadium removal reagent has a great influence on the stability of the production quality of titanium products, so that a method for detecting the vanadium removal efficiency of the vanadium removal reagent and a related device are needed.
Disclosure of Invention
The invention mainly aims to provide a vanadium removal efficiency detection method and device, which can help select a proper vanadium removal reagent, so that effective impurity removal and purification can be carried out on titanium tetrachloride, and the production quality of subsequent titanium products can be ensured.
According to one aspect of the invention, a vanadium removal efficiency detection method is provided, which comprises the following steps: a predetermined amount of TiCl is added4Heating the raw materials in a reactor to boil; adding a predetermined amount of vanadium removal reagent into the reactor for reaction; condensing the steam discharged from the reactor, and guiding the condensate back to the reactor for heating and reaction, and circulating the steps; detecting the content of vanadium impurities in the condensate after the reaction is carried out for a preset time; and judging the vanadium removal efficiency of the vanadium removal reagent based on the content of the vanadium impurities after the reaction.
According to one embodiment of the invention, based on said TiCl4Amount of the starting materials, TiCl4Determining the dosage of the vanadium removal reagent according to the content of vanadium impurities in the raw materials and the first coefficient.
According to one embodiment of the invention, the TiCl is reacted4The mass of the starting material multiplied by the TiCl4VOCl in the raw material3And dividing the product by 2.5-3.5 to obtain the mass of the vanadium removal reagent.
According to one embodiment of the invention, the heating temperature is greater than 180 ℃; and/or the predetermined time is 15 to 20 minutes.
According to an embodiment of the invention, the method further comprises: after the vanadium removal reagent is added, the materials in the reactor are continuously stirred until the reaction is finished.
According to one embodiment of the invention, the VOCl in the condensate after the reaction is removed3And if the mass fraction is less than 0.0003%, judging that the vanadium removal efficiency of the vanadium removal reagent meets the standard.
According to another aspect of the present invention, a vanadium removal efficiency detection apparatus is provided, including: a reactor configured to contain TiCl4Raw materials and vanadium removal reagents; a feeding unit connected to the reactor and feeding a predetermined amount of a vanadium removal reagent into the reactor; a heating unit configured to heat the reactor; the condenser is connected to the reactor through an inlet pipe and an outlet pipe, the inlet pipe guides steam discharged from the reactor into the condenser, and the outlet pipe guides condensate back into the reactor for heating and reaction; and a detection unit configured to detect the content of vanadium impurities in the condensate after a predetermined time of reaction.
According to an embodiment of the invention, the apparatus further comprises: and the sampling unit is connected to the condenser and is configured to sample the condensate after the reaction.
According to one embodiment of the invention, the vanadium removal agent is used in an amount based on TiCl4Amount of the starting materials, TiCl4The content of vanadium impurities in the raw material and the first coefficient are determined.
According to an embodiment of the invention, the heating unit is configured to provide a heating temperature of more than 180 ℃.
In the vanadium removal efficiency detection method according to the embodiment of the invention, the vanadium removal reagent and TiCl can be ensured by cyclically condensing the steam discharged from the reactor and guiding the condensate back to the reactor for heating and reaction4Fully reacting vanadium impurities in the raw materials; by adding a predetermined amount of TiCl4The raw materials and the vanadium removal reagent with the preset amount are subjected to reaction in preset time, the vanadium removal efficiency of the vanadium removal reagent can be judged based on the content of vanadium impurities after the reaction, and whether the detected vanadium removal reagent can be used for effectively removing vanadium is judged according to the vanadium removal efficiency, so that the selection of a proper vanadium removal reagent is facilitated, and effective impurity removal and purification are performed.
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 shows a flow diagram of a vanadium removal efficiency detection method according to an exemplary embodiment of the present invention; and
fig. 2 shows a schematic diagram of a vanadium removal efficiency detection apparatus according to an exemplary 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.
Fig. 1 shows a flowchart of a vanadium removal efficiency detection method according to an exemplary embodiment of the present invention, and as shown in fig. 1, the vanadium removal efficiency detection method includes the following steps:
s105, adding a predetermined amount of TiCl4Heating the raw materials in a reactor to boil;
s110, adding a predetermined amount of vanadium removal reagent into the reactor for reaction;
s115, condensing the steam discharged from the reactor, and guiding the condensate back to the reactor for heating and reaction, and circulating the steps;
s120, detecting the content of vanadium impurities in the condensate after the reaction is carried out for a preset time; and S125, judging the vanadium removal efficiency of the vanadium removal reagent based on the content of the vanadium impurities after the reaction.
In the vanadium removal efficiency detection method according to the embodiment of the invention, the vanadium removal reagent and TiCl can be ensured by cyclically condensing the steam discharged from the reactor and guiding the condensate back to the reactor for heating and reaction4Vanadium impurities in the raw materials react fully and quickly, the required operation is simple and convenient, and the corresponding device is simple; by adding a predetermined amount of TiCl4Raw materials and predetermined amount of removalThe vanadium reagent is subjected to reaction in a preset time, the vanadium removal efficiency of the vanadium removal reagent can be judged based on the content of vanadium impurities after the reaction, and whether the detected vanadium removal reagent can be used for effectively removing vanadium is judged, so that the selection of a proper vanadium removal reagent is facilitated, and effective impurity removal and purification are performed.
In step S105, the heating temperature may be greater than 180 ℃. And in the reaction process, the reactor is continuously heated to ensure that the vanadium removing reagent and TiCl4The vanadium impurities in the starting materials continue to react and TiCl4Can be continuously boiled to form steam. It can be appreciated that in the production of titanium tetrachloride, the heating temperature of the vanadium removal process is generally at TiCl4Between 136.4 ℃ and 150 ℃. Different from the method, the method is used for detecting the vanadium removal efficiency of the vanadium removal reagent, and the higher heating temperature (more than 180 ℃) is selected so as to accelerate the reaction rate, thereby being capable of quickly detecting the vanadium removal efficiency. The heating mode can be oil bath heating to ensure the uniformity of heating.
In step S110, TiCl boiling into the reactor4Adding a predetermined amount of a vanadium-removing reagent to the reaction mixture so that the vanadium-removing reagent is mixed with TiCl4The vanadium impurities in the vanadium-containing catalyst react to realize the purpose of impurity removal and purification. In the examples of the invention, it is possible to base on TiCl4Amount of starting material TiCl4Determining the dosage of the vanadium removal reagent according to the content of vanadium impurities in the raw materials and the first coefficient. Wherein the first coefficient represents the proportional relationship between the amount of vanadium impurities and the amount of vanadium removal reagent required to be consumed. The first coefficient is a constant set according to the detection effect. The first coefficient may be 2.5 to 3.5, for example, TiCl may be used4The mass of the starting material multiplied by TiCl4VOCl in the raw material3And dividing the product by 2.5-3.5 to obtain the mass of the vanadium removal reagent. A larger first factor indicates that less vanadium removal reagent is required and the vanadium removal efficiency is higher. In the embodiment of the invention, if the first coefficient is set to be too small, the vanadium removal efficiency of the screened vanadium removal reagent is too low, and the requirement cannot be met; however, the first coefficient is also not possible and is not necessarily set to infinity, and if it is set too large, it will cause the screening condition to be imposedBecomes too harsh to select a suitable vanadium removal reagent. In the embodiment of the invention, when the range of the first coefficient is set to be 2.5-3.5, the vanadium removal efficiency of the vanadium removal reagent screened according to the method can meet the requirement, namely, the numerical range of 2.5-3.5 can be used for properly and effectively detecting the vanadium removal efficiency of the vanadium removal reagent. In a preferred embodiment, the first coefficient may be 3. For example, TiCl is mixed with4The mass of the starting material multiplied by TiCl4VOCl in the raw material3And dividing the product by 3 to obtain the mass of the vanadium removal reagent.
In step S115, the condensation of the vapor discharged from the reactor and the introduction of the condensate back into the reactor for heating and reaction are cyclically performed. TiCl in the reactor4The method comprises the steps of heating and boiling raw materials to form steam for discharging, wherein a vanadium removal reagent and vanadium impurities are not completely reacted at first, the discharged steam possibly contains more vanadium impurities, the steam containing the vanadium impurities is condensed into condensate and then flows back into a reactor, the condensate is heated again and reacts with the vanadium removal reagent in the reactor, and therefore in the circulating process of discharging the steam and refluxing the condensate, the reaction process is continuously promoted to reduce the content of the impurities and improve the distribution uniformity of the vanadium impurities in the condensate until the reaction is stopped after a preset time.
In the embodiment of the invention, the predetermined time may be 15 to 20 minutes. Similarly, a shorter time for the reaction to proceed indicates a higher vanadium removal efficiency of the vanadium removal reagent. In the embodiment of the invention, if the preset time is set to be too long, the vanadium removal efficiency of the screened vanadium removal reagent is too low, and the requirement cannot be met; however, the predetermined time is not possible and is not necessarily set to be infinitely short, and if the predetermined time is set to be too short, the screening conditions become too severe, and it is difficult to select a suitable usable vanadium removal reagent. In the embodiment of the invention, when the predetermined time is set to be in the range of 15-20 minutes, the vanadium removal efficiency of the vanadium removal reagent screened according to the method can meet the requirement, namely, the numerical range of 15-20 minutes can be used for properly and effectively detecting the vanadium removal efficiency of the vanadium removal reagent. Therefore, the vanadium removal efficiency of the vanadium removal reagent can be detected after 15-20 minutes of reaction, so that rapid detection can be realized, the consumed time is short, and the efficiency is high. In a preferred embodiment, the predetermined time may be 15 minutes.
The invention combines the preset dosage of the vanadium removal reagent and the preset reaction time to detect the vanadium removal efficiency, thereby forming the standard of the vanadium removal efficiency detection method. The above criteria are references that the inventors of the present invention have determined after studies that can be used to effectively and accurately and rapidly judge the vanadium removal efficiency of the vanadium removal reagent. In embodiments of the invention, one criterion may be VOCl3The ratio of the mass to the consumption mass of the vanadium removing reagent is more than or equal to 3, and qualified TiCl is obtained4The time of the concentrate is less than or equal to 15 minutes. Wherein the qualified TiCl4The concentrate can be represented as VOCl3The mass fraction is less than 0.0003 percent. Accordingly, in step S125, if VOCl in the condensate after the reaction is present3And if the mass fraction is less than 0.0003%, judging that the vanadium removal efficiency of the vanadium removal reagent meets the standard, namely the vanadium removal reagent can effectively remove vanadium, and is suitable for impurity removal and purification processes in the production process.
In an embodiment of the present invention, the method may further include: after the vanadium removal reagent is added, the contents of the reactor are continuously stirred until the reaction is complete. The vanadium removal reagent and TiCl can be promoted by stirring4The contact of the raw materials improves the reaction rate.
The vanadium removal reagent for detection of the invention can be organic matter, such as fatty acid, mineral oil and the like. The invention carries out cooling collection by means of indirect condensation, and cooling media can include but are not limited to circulating cooling water and other cooling liquids.
Fig. 2 shows a schematic diagram of a vanadium removal efficiency detection apparatus 100 according to an exemplary embodiment of the present invention, and as shown in fig. 2, the vanadium removal efficiency detection apparatus 100 includes: a reactor 10 configured to contain TiCl4Raw materials and vanadium removal reagents; a feeding unit 20 connected to the reactor 10 and feeding a predetermined amount of a vanadium removing reagent into the reactor 10; a heating unit 30 configured to heat the reactor 10; a condenser 40 connected to the reactor 10 through an inlet pipe 42 and an outlet pipe 44, the inlet pipe 42 guiding the steam discharged from the reactor 10 into the condenser 40, the outlet pipe 44 condensing the steamThe liquid is guided back into the reactor 10 for heating and reaction; and a detection unit configured to detect the content of vanadium impurities in the condensate after a predetermined time of reaction.
The reactor 10 may be a flask or other reactor capable of reacting the vanadium removal reagent with TiCl4The feedstock provides a vessel of reaction environment. The feeding unit 20 may be a burette for accurately feeding a predetermined amount of the vanadium removal reagent, and the feeding of the vanadium removal reagent may be controlled by a valve of the burette. As mentioned above, the vanadium-removing agent can be used in an amount based on TiCl4Amount of starting material TiCl4The content of vanadium impurities in the raw material and the first coefficient are determined. For example, TiCl may be reacted4The mass of the starting material multiplied by TiCl4VOCl in the raw material3And dividing the product by 2.5-3.5 to obtain the mass of the vanadium removal reagent. The vanadium removal reagent may be organic.
The heating unit 30 may be an oil bath for providing a uniform heating effect to the reactor 10. The heating unit 30 may continuously heat the reactor 10 before the reaction is finished. The heating unit 30 is configured to provide a heating temperature greater than 180 ℃ to promote rapid reaction between the vanadium removal reagent and the vanadium impurities, thereby speeding up the detection of the vanadium removal efficiency.
The condenser 40 may cool the steam by a cooling medium including circulating cooling water or other cooling liquid, and collect the cooled condensed water. A condensing tower head may be provided between the introduction pipe 42, the discharge pipe 44, and the reactor 10. The detection unit can be any device capable of detecting the content of vanadium impurities.
The apparatus 100 may further comprise: and a sampling unit 50 connected to the condenser 40 and configured to sample the condensate after the reaction. The sampling unit 50 may comprise a conduit connected to the condenser 40 and a valve for controlling whether condensate flows out of the condenser 40 through the conduit. Since the steam and the condensate are continuously flowing and switching between the reactor 10 and the condenser 40, the content of vanadium impurities in the condensate in the condenser 40 is uniform after the reaction is finished for a predetermined time. Therefore, the result of sampling detection is very representative. The reaction time is 15 to 20 minutes.
The apparatus 100 may further comprise a stirring unit for continuously stirring the contents of the reactor after the vanadium removal reagent is added until the reaction is completed. The vanadium removal reagent and TiCl can be promoted by stirring4The contact of the raw materials improves the reaction rate. The stirring unit may be a stirring magneton.
The vanadium removal efficiency detection method and device are suitable for TiCl4The refining system in the production industry can help select a proper and effective vanadium removal reagent, the stability of the production quality of the titanium product is favorably ensured, and the detection method can be carried out quickly and consumes short time.
The following description is based on specific examples.
Example 1
The vanadium removal efficiency of the fatty acid is detected, and the detection method comprises the following steps:
weighing TiCl with a mass of 0.3kg4The starting material was placed in a flask with TiCl4VOCl in the raw material3The mass fraction of (A) is 1%;
placing the flask in an oil bath, and heating to boiling, wherein the temperature of the oil bath is 180 ℃;
the flask was charged, via a burette, with a vanadium removal reagent having a mass of 0.3kg × 1%/3 ═ 1g to react with TiCl4VOCl in the starting Material3Reacting, and stirring for 15min by using stirring magnetons; during the period, the steam discharged from the flask is condensed by a condenser, and the condensate is led back to the flask for heating and reaction, and the process is circulated;
then, a valve on the condenser is opened, and the VOCl in the condensate after the reaction is sampled and detected3The mass fraction of the vanadium removing reagent is 0.0007 percent and is more than 0.0003 percent, and the vanadium removing efficiency of the vanadium removing reagent is judged to be not in accordance with the standard, namely the vanadium can not be effectively removed.
Example 2
The method for detecting the vanadium removal efficiency of the mineral oil comprises the following steps:
weighing TiCl with a mass of 0.3kg4The starting material was placed in a flask with TiCl4VOCl in the raw material3The mass fraction of (A) is 1%;
placing the flask in an oil bath, and heating to boiling, wherein the temperature of the oil bath is 180 ℃;
the flask was charged, via a burette, with a vanadium removal reagent having a mass of 0.3kg × 1%/3 ═ 1g to react with TiCl4VOCl in the starting Material3Reacting, and stirring for 15min by using stirring magnetons; during the period, the steam discharged from the flask is condensed by a condenser, and the condensate is led back to the flask for heating and reaction, and the process is circulated;
then, a valve on the condenser is opened, and the VOCl in the condensate after the reaction is sampled and detected3The mass fraction of the vanadium removing reagent is 0.0001 percent and less than 0.0003 percent, and the vanadium removing efficiency of the vanadium removing reagent is judged to meet the standard, namely the vanadium can be effectively removed.
According to the embodiments, the vanadium removal efficiency detection method can quickly and effectively detect the vanadium removal efficiency of different vanadium removal reagents, so that a proper vanadium removal reagent can be screened out for industrial production.
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.
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