CN113270150A - Method for determining consistency of reaction acid concentration in titanium dioxide acidolysis - Google Patents

Method for determining consistency of reaction acid concentration in titanium dioxide acidolysis Download PDF

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Publication number
CN113270150A
CN113270150A CN202110447485.9A CN202110447485A CN113270150A CN 113270150 A CN113270150 A CN 113270150A CN 202110447485 A CN202110447485 A CN 202110447485A CN 113270150 A CN113270150 A CN 113270150A
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acid
concentration
reaction
acidolysis
waste
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王红青
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Anhui Annada Titanium Industry Co ltd
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Anhui Annada Titanium Industry Co ltd
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    • GPHYSICS
    • G16INFORMATION AND COMMUNICATION TECHNOLOGY [ICT] SPECIALLY ADAPTED FOR SPECIFIC APPLICATION FIELDS
    • G16CCOMPUTATIONAL CHEMISTRY; CHEMOINFORMATICS; COMPUTATIONAL MATERIALS SCIENCE
    • G16C20/00Chemoinformatics, i.e. ICT specially adapted for the handling of physicochemical or structural data of chemical particles, elements, compounds or mixtures
    • G16C20/10Analysis or design of chemical reactions, syntheses or processes
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00Compounds of titanium
    • C01G23/04Oxides; Hydroxides
    • C01G23/047Titanium dioxide
    • C01G23/053Producing by wet processes, e.g. hydrolysing titanium salts

Abstract

The invention discloses a method for determining the consistency of reaction acid concentration in titanium dioxide acidolysis, which comprises the following steps: in the acidolysis process, the original acid concentration and the reaction acid concentration are determined, then the weight of the added mineral powder, the acid-mineral ratio, the volume of sulfuric acid, the density of sulfuric acid, the specific gravity of waste acid and the concentration of waste acid are counted, and the waste acid amount is calculated according to the following formula: (weight of ore powder, acid-to-volume of sulfuric acid, density of sulfuric acid, concentration of reaction acid)/specific gravity of waste acid (concentration of reaction acid-concentration of waste acid) = amount of waste acid, and the amount of waste acid is adjusted according to the set concentration of reaction acid. The invention has the beneficial effect that the concentration of the acid in the acidolysis reaction is accurately controlled, so that the chronic diseases which disturb a large amount of solid-phase substances remained in the acidolysis pot in the titanium dioxide production are eliminated. The acidolysis pot basically realizes no solid matters, and a clear gas distribution plate can be seen in the acidolysis pot. And the improvement of the yield is guaranteed. A solid foundation is laid for improving the quality, and the acidolysis rate of the titanium ore is improved from the original less than 92.5 percent to be stabilized at more than 95.5 percent.

Description

Method for determining consistency of reaction acid concentration in titanium dioxide acidolysis
Technical Field
The invention relates to the field of a sulfuric acid method titanium dioxide production process, in particular to a method for determining the consistency of reaction acid concentration in titanium dioxide acidolysis.
Background
Titanium dioxide is known as titanium dioxide, is considered as a white pigment with the best performance in the world, and is widely applied to the industries of coatings, synthetic fibers, high-grade white paint, white rubber, printing, metallurgy and the like.
The acidolysis is a tap for titanium white production, and no stable process is used as a guarantee, so that the titanium white production cannot be carried out continuously and stably for a long time, the high acidolysis rate cannot be realized, and the production benefit is maximized. The existing acidolysis process generally adopts a solid phase method, sulfuric acid measured according to the ratio of mineral acid is put into an acidolysis pot from an acid adding pipe, the sulfuric acid can be called as original acid, an air draft system is started while compressed air is introduced for stirring, titanium ore powder is put into the acidolysis pot from an ore feeding port after the sulfuric acid is put into the acidolysis pot for a half, air blast stirring is continued until the titanium ore powder is completely and uniformly stirred, waste acid is added for initiating reaction, the waste acid can be called as initiation acid, after the main reaction is finished, the titanium ore is cured for a period of time, water (light titanium liquid) is added for leaching and dissolving, and after the iron powder is completely dissolved and the temperature is proper, the simple substance iron powder is added until the ferric iron in the solution is completely converted into the ferrous iron. Under the existing production mineral resources and technological conditions, the factors influencing the acidolysis reaction are more, and the factors mainly comprise: 1) titanium ore proportioning and stability of fineness of ore powder; 2) concentrating the original acid, and making the concentration of the acid; 3) the original acid concentration causes the fluctuation of the acid concentration; 4) the metering of leaching process water, and the like. The primary concern here is the original acid concentration, which triggers the impact of acid concentration formulation and fluctuations on the acidolysis reaction. As the original acid concentration causes formulation and fluctuation of the acid concentration, the phenomenon of scabbing and solid phase residue in the acidolysis pot is more prominent, as shown in figure 1; the acidolysis rate is low, which causes the increase of the manufacturing cost.
The concentration of the sulfuric acid added into an acidolysis pot when the original acid, namely acidolysis is started, can be accelerated if the concentration of the acid exceeds the process requirement, the reaction is accelerated rapidly by the dilution heat after the waste acid is added, the pot overflow phenomenon is easy to occur, and the tail gas can not be absorbed and discharged up to the standard. On the contrary, if the concentration of the original acid is low, the heat of dilution is insufficient, the reaction is slow, and the rate of acid hydrolysis is low.
The acid concentration during the reaction can influence the reaction speed of the concentrated acid and the ilmenite, and further influence a series of indexes such as acidolysis rate and the like. Meanwhile, after the original concentrated acid concentration is fixed, the reaction acid concentration determines the addition amount of the initiating waste acid, so that the water amount brought into the system is determined. The quality of the reaction of the whole system is determined.
Chinese utility model patent publication No. CN211470801U discloses a metering device is mixed in advance in continuous acidolysis of titanium white powder, adopts this metering device is mixed in advance in continuous acidolysis of titanium white powder can be in sulfuric acid process titanium white powder acidolysis process effectual control acid-mineral ratio and the concentration of reaction acid to reach the purpose of continuous acidolysis steady production. The purpose is realized by controlling the addition amount of sulfuric acid and ore powder through a mineral powder weighing metering tank and an electromagnetic flow meter, and the influence of the original acid concentration on the acidolysis reaction is not considered.
For another example, chinese patent publication No. CN102830200A discloses a method for detecting the acidolysis rate of a titanium-containing mineral, which calculates the acidolysis rate according to formula 1, wherein formula 1 is: the acid hydrolysis ratio = mA/(mA + mB) × 100%, where mA represents the mass of TiO2 in the titanium solution, and mB represents the mass of TiO2 in the residue. The method has accurate detection result and can objectively evaluate the acidolysis performance of ilmenite of different factories and mines, but the acidolysis rate is directly calculated according to the mass of TiO2 in titanium liquid and the mass of TiO2 in residues, and the influence of the initial acid concentration in the acidolysis process on the acidolysis reaction caused by the acid concentration is not considered.
Disclosure of Invention
The invention aims to solve the technical problem that the prior titanium dioxide acidolysis has influence on acidolysis due to the concentration of the original acid, and no special method is provided for ensuring the consistency of the original acid and the concentration of the trigger acid at present, so that the invention provides a method for determining the consistency of the reaction acid concentration in the titanium dioxide acidolysis.
And (3) concentration of reaction acid: is an important index for controlling the reaction state. And (3) inputting the parameters of the assay analysis into a calculation formula by an operator according to the ore feeding amount and the change of the concentration of the waste acid to calculate the consumption of the reaction waste acid in each batch. Thereby ensuring the consistency of the reaction acid concentration of each batch. Aiming at the different high iron content of the ore from each source, the concentration of the reaction acid needs to be adjusted in time for adaptation. If the concentration of the acid is high, the iron content of the ore is low, the amount of water generated by the reaction is small, that is, the amount of water evaporated by diffusion from the inside of the molecule or the inside of the ore powder particle, the formed solid phase is poor in porosity, and on the other hand, the high concentration of the reaction acid causes less water to be taken in, which is not good for forming the solid phase in a porous state. And under the condition of low reaction acid concentration, because the reaction condition is observed through the temperature of the tail gas, the reaction time is always continuous at a high point, and even secondary reaction occurs, so that the solubility of a solid phase substance is improved by proper reaction acid concentration.
Therefore, the invention designs a calculation formula for controlling the concentration of the reaction acid, and can ensure the consistency of the concentration of the reaction acid in each batch.
The technical scheme of the invention is as follows: the method for determining the consistency of the reaction acid concentration in the acidolysis of titanium dioxide comprises the following steps: in the acidolysis process, the original acid concentration and the reaction acid concentration are determined, then the weight of the added mineral powder, the acid-mineral ratio, the volume of sulfuric acid, the density of sulfuric acid, the specific gravity of waste acid and the concentration of waste acid are counted, and the waste acid amount is calculated according to the following formula:
(weight of ore powder, acid-to-volume of sulfuric acid, density of sulfuric acid, concentration of reaction acid)/specific gravity of waste acid (concentration of reaction acid-concentration of waste acid) = amount of waste acid, and the amount of waste acid is adjusted according to the set concentration of reaction acid.
The formula for calculating the volume of sulfuric acid in the above scheme is as follows: sulfuric acid volume = mineral fines weight acid-to-mineral ratio/sulfuric acid concentration sulfuric acid density.
In the scheme, the weight of the ore powder is 25.66t, the acid-ore ratio is 1.12, the sulfuric acid concentration is 98.20%, the sulfuric acid density is 1.83g/cm for thin film plantation, the reaction acid concentration is 82.70%, the specific gravity of the waste acid is 1.24%, and the concentration of the waste acid is 54.61%.
The calculation formula of the waste acid amount in the scheme is input by DCS and the result is displayed.
The formula for calculating the volume of the sulfuric acid in the scheme is input by DCS and the result is displayed.
The invention has the beneficial effect that the concentration of the acid in the acidolysis reaction is accurately controlled, so that the chronic diseases which disturb a large amount of solid-phase substances remained in the acidolysis pot in the titanium dioxide production are eliminated. The acidolysis pot basically realizes no solid matters, and a clear gas distribution plate can be seen in the acidolysis pot. And the improvement of the yield is guaranteed. A solid foundation is laid for the improvement of the quality, and the technology is in the leading level in the titanium dioxide industry; the acidolysis rate of the titanium ore is improved from the original less than 92.5 percent to be stabilized at more than 95.5 percent.
Drawings
FIG. 1 is a photograph after an acidolysis reaction in an acidolysis pot in the prior art;
FIG. 2 is a photograph after the acidolysis reaction in the acidolysis pot according to the present invention.
Detailed Description
The technical scheme in the embodiment of the invention is clearly and completely described below by combining the embodiment. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments based on the embodiments in the present invention, without any inventive work, will be apparent to those skilled in the art from the following description.
One embodiment of the invention is as follows: the method for determining the consistency of the reaction acid concentration in the acidolysis of titanium dioxide comprises the following steps: in the acidolysis process, the original acid concentration and the reaction acid concentration are determined, then the weight of the added mineral powder, the acid-mineral ratio, the volume of sulfuric acid, the density of sulfuric acid, the specific gravity of waste acid and the concentration of waste acid are counted, and the waste acid amount is calculated according to the following formula:
(weight of ore fines acid-ore ratio-volume of sulfuric acid-density of reaction acid)/specific gravity of waste acid (concentration of reaction acid-concentration of waste acid) = amount of waste acid. Wherein sulfuric acid volume = mineral fines weight acid-mineral ratio/sulfuric acid concentration sulfuric acid density.
In the formula, the weight of the mineral powder is 25.66t, the acid-mineral ratio is 1.12, the sulfuric acid concentration is 98.20%, the sulfuric acid density is 1.83g/cm for high-speed thin-wall cultivation, the reaction acid concentration is 82.70%, the specific gravity of the waste acid is 1.24, and the concentration of the waste acid is 54.61%.
By adopting the method for operation, the economic benefits are calculated according to the annual production of 5 ten thousand tons in a single production line and the production time of 330 days:
1) the increase of the acidolysis rate produces economic benefits
The acidolysis rate of the titanium ore is improved from the original less than 92.5 percent to be stabilized at more than 95.5 percent. 187237 tons of ore are charged in the year 2020, and the benefit is 842.6 ten thousand yuan calculated according to the average price of ore sources of 1500 yuan/ton.
[ 187237X 47.5% × (95.5% -92.5%)/47.5% ]X1500 Yuan/ton 842.6 Van Yuan, wherein 47.5% refers to the grade of the ore.
The acid concentration during the reaction can be attributed to the reaction rate of sulfuric acid with ilmenite. The acidolysis rate, the solid residue in the pot and titanium are influencedA series of problems of liquid index. Meanwhile, after the concentration of the fed ortho-acid is determined, the concentration of the reaction acid also determines the amount of the added initiating waste acid. The amount of water carried away in the acidolysis reaction system was also determined. Ultimately determining the mass of the solid phase (titanium sulfate) formed by the reaction. The quality here refers to the ease of dissolution of the solid phase during leaching. The acidolysis rate and the total titanium and F value index are controlled. The reaction acid concentration in the current domestic titanium dioxide production is generally controlled to be 81-88%, which is caused by the great difference due to the different types of the titanium concentrates used by people. For example, the West Chang mine has fine particle size distribution, and 60 percent of the rest of 320 meshes of the ore pass through the sieve. The MgO content is also high. Fe2O3The content is low, so that the reaction acid concentration must be controlled to be about 80 percent of the bottom line. The solid phase obtained by the acidolysis reaction has good porosity and is easy to leach and dissolve. And low MgO content Fe in Vietnam ore2O3The content is high. High reaction acid concentrations are required. Due to the change of mineral resources, the currently used mines of the company have 6 kinds of mines such as West Chang, Vietnam, Chengde, Yishui, Sri Lanka, south Africa and the like. In order to stabilize and increase the acidolysis yield. The target task of yield is realized, and the scab of solid-phase substances in the acidolysis pot is avoided. The titanium liquid index qualification rate is improved, a calculation formula of the reaction acid concentration is designed, engineering technicians input different reaction acid concentrations according to different ore sources used for acidolysis, and the usage amount of 55% waste acid required for initiating the main reaction is calculated quickly. The concentration of the reaction acid is tracked and finely adjusted by operators according to the residual amount of solid phase substances in the acidolysis pot and the Baume concentration of the leached titanium solution, so that the acidolysis reaction condition achieves an optimal effect.
In order to facilitate the operation, the preferred embodiment of the invention is operated on DCS by the formula calculation, a calculation formula of the reaction acid concentration is designed on DCS, and engineering technicians input different reaction acid concentrations on DCS according to different mineral sources used for acidolysis, so that the usage amount of 55% waste acid required for initiating the main reaction can be calculated quickly. The concentration of the reaction acid is tracked and finely adjusted on DCS according to the solid phase residue amount in the acidolysis pot by operators according to the Baume concentration of the leaching titanium solution, so that the acid liberation condition achieves an optimal effect.
As shown in figure 2, the acidolysis pot after acidolysis reaction basically realizes no solid matters through controlling the concentration of the reaction acid, and a clear gas distribution plate can be seen in the acidolysis pot.

Claims (5)

1. The method for determining the consistency of the reaction acid concentration in the acidolysis of titanium dioxide is characterized by comprising the following steps of: in the acidolysis process, the original acid concentration and the reaction acid concentration are determined, then the weight of the added mineral powder, the acid-mineral ratio, the volume of sulfuric acid, the density of sulfuric acid, the specific gravity of waste acid and the concentration of waste acid are counted, and the waste acid amount is calculated according to the following formula:
(weight of ore powder, acid-to-volume of sulfuric acid, density of sulfuric acid, concentration of reaction acid)/specific gravity of waste acid (concentration of reaction acid-concentration of waste acid) = amount of waste acid, and the amount of waste acid is adjusted according to the set concentration of reaction acid.
2. The method for determining the consistency of the reaction acid concentration in the acidolysis of titanium dioxide as claimed in claim 1, which is characterized in that: the formula for the volume of sulfuric acid is as follows: sulfuric acid volume = mineral fines weight acid-to-mineral ratio/sulfuric acid concentration sulfuric acid density.
3. The method for determining the consistency of the reaction acid concentration in the acidolysis of titanium dioxide as claimed in claim 1, which is characterized in that: the weight of the ore powder is 25.66t, the acid-ore ratio is 1.12, the sulfuric acid concentration is 98.20%, the sulfuric acid density is 1.83g/cm through high-speed dry-mass production, the reaction acid concentration is 82.70%, the waste acid specific gravity is 1.24, and the waste acid concentration is 54.61%.
4. The method for determining the consistency of the reaction acid concentration in the acidolysis of titanium dioxide as claimed in claim 1, which is characterized in that: and the calculation formula of the waste acid amount is input by the DCS and displays the result.
5. The method for determining the consistency of the reaction acid concentration in the acidolysis of titanium dioxide as claimed in claim 2, which is characterized in that: the calculation formula of the volume of the sulfuric acid is input by DCS and the result is displayed.
CN202110447485.9A 2021-04-25 2021-04-25 Method for determining consistency of reaction acid concentration in titanium dioxide acidolysis Pending CN113270150A (en)

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