A method for accelerating the precipitation of solid suspended impurities in crude titanium tetrachloride

Abstract

This invention relates to the field of titanium chemical technology, specifically to a method for accelerating the precipitation of solid suspended impurities in crude titanium tetrachloride. A precipitation aid is added to the crude titanium tetrachloride. After reacting with titanium tetrachloride at room temperature, the precipitation aid generates a large amount of flocculent material, which adsorbs and rapidly precipitates the solid suspended impurities. The precipitation aid is a mixture of long-chain alkanes or olefins. This invention, by adding a precipitation aid to crude titanium tetrachloride, operates on a principle similar to flocculants precipitating solid suspended impurities in wastewater. The aid reacts with titanium tetrachloride at room temperature to generate a large amount of flocculent material, which adsorbs and rapidly precipitates the solid suspended impurities, increasing the precipitation rate of solid impurities in crude titanium tetrachloride, shortening the precipitation time, and reducing production costs. After adding the precipitation aid, the solid suspended impurities in crude titanium tetrachloride can be basically precipitated within five minutes, and become clear and transparent in about half an hour. This shortens the precipitation time, improves the efficiency of the settling tank, and also makes the vanadium slag after vanadium removal purer and more valuable.

Description

Technical Field

[0001] This invention relates to the field of titanium chemical technology, specifically to a method for accelerating the precipitation of solid suspended impurities in crude titanium tetrachloride. Background Technology

[0002] Titanium tetrachloride is an important intermediate raw material for the production of sponge titanium, and its quality significantly affects the quality of sponge titanium. The molten salt process for producing titanium tetrachloride begins by feeding titanium ore and chlorine gas into a chlorination furnace. Under high-temperature conditions, titanium tetrachloride is generated. The titanium tetrachloride vapor is then condensed to obtain crude titanium tetrachloride in liquid form. This crude titanium tetrachloride often contains a significant amount of solid insoluble impurities, which need to be precipitated before distillation to reduce the amount of solid impurities.

[0003] Currently, in the molten salt method for producing crude titanium tetrachloride, the slurry is first fed into a settling tank for precipitation. After solid impurities settle, the bottom slurry is returned to the chlorination furnace, while the clear liquid at the top is fed into a distillation system. A vanadium removal agent is added, and after distillation to remove solid impurities, the liquid continues into a rectification system to remove liquid and gaseous impurities with different boiling points, finally yielding refined titanium tetrachloride. Because the solid impurity particles in crude titanium tetrachloride are small and the settling time is long, the crude titanium tetrachloride entering the distillation system in actual production often still contains 0-50 g / L of solid impurities. After distillation, a large amount of solid residue remains in the distillation vessel, affecting production. Summary of the Invention

[0004] The purpose of this invention is to provide a method for accelerating the precipitation of solid suspended impurities in crude titanium tetrachloride, in order to solve the problems mentioned in the background art, such as the small particle size of solid impurities in crude titanium tetrachloride, the long precipitation time, and the fact that in actual production, crude titanium tetrachloride entering the distillation system often still contains 0-50 g / L of solid impurities.

[0005] To achieve the above objectives, the present invention provides the following technical solution:

[0006] A method for accelerating the precipitation of solid suspended impurities in crude titanium tetrachloride involves adding a precipitation aid to the crude titanium tetrachloride. The precipitation aid reacts with titanium tetrachloride at room temperature to generate a large amount of flocculent material, which adsorbs the solid suspended impurities and rapidly precipitates them. The precipitation aid is a mixture of long-chain alkanes or alkenes.

[0007] As a preferred option, the specific steps are as follows:

[0008] S10: Measure the temperature of the crude titanium tetrachloride container and ensure that the temperature is ≤65℃;

[0009] S20: Add crude titanium tetrachloride and precipitating agent from the bottom of the mixing tank in a certain proportion;

[0010] S30: While adding the precipitating agent and crude titanium tetrachloride into the mixing tank, turn on the stirrer at a speed of approximately 120 RPM.

[0011] S40: Open the overflow valve at the top of the stirring tank to the No. 1 sedimentation tank; after the No. 1 sedimentation tank reaches the specified liquid level, adjust the valve to allow it to overflow to the No. 2 sedimentation tank;

[0012] S50: During the receiving period of material in sedimentation tank #2, the material in sedimentation tank #1 settles and is prepared for discharge.

[0013] S60: When discharging, open the bottom valve of the No. 1 sedimentation tank and the valve leading to the mud tank to discharge the bottom mud. Through the glass window on the pipe, when the material becomes clear, close the valve leading to the mud tank and open the valve leading to the pre-distillation storage tank to discharge the upper clear liquid to the pre-distillation storage tank until it is empty, and prepare to receive the material.

[0014] S70: After the No. 2 sedimentation tank reaches the specified liquid level, switch the valve to make the material in the stirring tank flow to the No. 1 sedimentation tank, and the No. 2 sedimentation tank will settle and prepare for discharge.

[0015] S80: Discharging material from sedimentation tank #2 is the same as in step S70;

[0016] S90: The sedimentation tank and the No. 2 sedimentation tank alternately operate for receiving and discharging materials.

[0017] Preferably, the amount of precipitation aid added in step S20 is 2‰-9‰ of the mass of crude titanium tetrachloride.

[0018] Preferably, the precipitation aid in step S20 comprises the following raw materials by weight percentage: stearic acid 4%-10%, oleic acid 70%-80%, linoleic acid 10%-20%, and linolenic acid 0%-5%.

[0019] Preferably, the precipitation aid in step S20 comprises the following raw materials in percentage weight: stearic acid 6.52%, oleic acid 76.85%, linoleic acid 15.83%, and linolenic acid 0.8%.

[0020] Preferably, the linoleic acid is obtained by extracting a solution containing linoleic acid from corn bran, extracting with an organic solvent, concentrating to obtain crude linoleic acid oil, and then purifying it to obtain high-purity linoleic acid.

[0021] Preferably, the organic solvent is ethanol.

[0022] Preferably, the purification is performed using the urea encapsulation method.

[0023] Preferably, the specific steps of the urea inclusion method purification are as follows: urea and methanol are added to the crude linoleic acid fraction in a ratio of 1:9:30, the reaction temperature is 75°C, the reaction time is 50 min, the inclusion temperature is 25°C, and the inclusion time is 26 hours.

[0024] Preferably, the linolenic acid is α-linolenic acid or γ-linolenic acid.

[0025] Compared with the prior art, the beneficial effects of this invention are as follows: This method for accelerating the precipitation of solid suspended impurities in crude titanium tetrachloride involves adding a precipitation aid to the crude titanium tetrachloride. The principle is similar to that of flocculants precipitating solid suspended impurities in wastewater. After reacting with titanium tetrachloride at room temperature, the aid generates a large amount of flocculent material, which adsorbs the solid suspended impurities and rapidly precipitates them, thereby increasing the precipitation rate of solid impurities in crude titanium tetrachloride, shortening the precipitation time, and reducing production costs. After adding the precipitation aid, the solid suspended impurities in crude titanium tetrachloride can be basically precipitated within five minutes, and become clear and transparent in about half an hour, greatly shortening the precipitation time, improving the efficiency of the settling tank, and also making the vanadium slag after vanadium removal purer and more valuable. Attached Figure Description

[0026] The accompanying drawings are provided to further illustrate the invention and form part of the specification. They are explained in detail together with the embodiments of the invention, but do not constitute a limitation thereof.

[0027] Figure 1 This is a schematic diagram of the process for accelerating the precipitation of solid suspended impurities in crude titanium tetrachloride according to the present invention. Detailed Implementation

[0028] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0029] Example 1

[0030] A method for accelerating the precipitation of solid suspended impurities in crude titanium tetrachloride involves adding a precipitation aid to the crude titanium tetrachloride. The precipitation aid reacts with titanium tetrachloride at room temperature to generate a large amount of flocculent material, which adsorbs the solid suspended impurities and precipitates them rapidly. The precipitation aid is a mixture of long-chain alkanes or alkenes.

[0031] like Figure 1 As shown, the specific steps are as follows:

[0032] S10: Measure the temperature of the crude titanium tetrachloride container and ensure that the temperature is ≤65℃;

[0033] S20: Add crude titanium tetrachloride and precipitating agent from the bottom of the mixing tank in a certain proportion;

[0034] S30: While adding the precipitating agent and crude titanium tetrachloride into the mixing tank, turn on the stirrer at a speed of approximately 120 RPM.

[0035] S40: Open the overflow valve at the top of the stirring tank to the No. 1 sedimentation tank; after the No. 1 sedimentation tank reaches the specified liquid level, adjust the valve to allow it to overflow to the No. 2 sedimentation tank;

[0036] S50: During the receiving period of material in sedimentation tank #2, the material in sedimentation tank #1 settles and is prepared for discharge.

[0037] S60: When discharging, open the bottom valve of the No. 1 sedimentation tank and the valve leading to the mud tank to discharge the bottom mud. Through the glass window on the pipe, when the material becomes clear, close the valve leading to the mud tank and open the valve leading to the pre-distillation storage tank to discharge the upper clear liquid to the pre-distillation storage tank until it is empty, and prepare to receive the material.

[0038] S70: After the No. 2 sedimentation tank reaches the specified liquid level, switch the valve to make the material in the stirring tank flow to the No. 1 sedimentation tank, and the No. 2 sedimentation tank will settle and prepare for discharge.

[0039] S80: Discharging material from sedimentation tank #2 is the same as in step S70;

[0040] S90: The sedimentation tank and the No. 2 sedimentation tank alternately operate for receiving and discharging materials.

[0041] In this embodiment, the amount of precipitation aid added in step S20 is 5‰ of the mass of crude titanium tetrachloride. The precipitation aid in step S20 includes the following raw materials by weight percentage: stearic acid 6.52%, oleic acid 76.85%, linoleic acid 15.83%, and linolenic acid 0.8%.

[0042] Linoleic acid is obtained by extracting a solution containing linoleic acid from corn bran. The solution is extracted with an organic solvent and concentrated to obtain crude linoleic acid oil. After purification, high-purity linoleic acid is obtained. The organic solvent is ethanol. The purification is carried out by urea inclusion method. The specific steps of urea inclusion method purification are as follows: urea and methanol are added to the crude linoleic acid fraction in a ratio of 1:9:30. The reaction temperature is 75℃, the reaction time is 50 min, the inclusion temperature is 25℃, and the inclusion time is 26 hours.

[0043] In addition, linolenic acid is either α-linolenic acid or γ-linolenic acid.

[0044] Example 2

[0045] A method for accelerating the precipitation of solid suspended impurities in crude titanium tetrachloride involves adding a precipitation aid to the crude titanium tetrachloride. The precipitation aid reacts with titanium tetrachloride at room temperature to generate a large amount of flocculent material, which adsorbs the solid suspended impurities and precipitates them rapidly. The precipitation aid is a mixture of long-chain alkanes or alkenes.

[0046] like Figure 1 As shown, the specific steps are as follows:

[0047] S10: Measure the temperature of the crude titanium tetrachloride container and ensure that the temperature is ≤65℃;

[0048] S20: Add crude titanium tetrachloride and precipitating agent from the bottom of the mixing tank in a certain proportion;

[0049] S30: While adding the precipitating agent and crude titanium tetrachloride into the mixing tank, turn on the stirrer at a speed of approximately 120 RPM.

[0050] S40: Open the overflow valve at the top of the stirring tank to the No. 1 sedimentation tank; after the No. 1 sedimentation tank reaches the specified liquid level, adjust the valve to allow it to overflow to the No. 2 sedimentation tank;

[0051] S50: During the receiving period of material in sedimentation tank #2, the material in sedimentation tank #1 settles and is prepared for discharge.

[0052] S60: When discharging, open the bottom valve of the No. 1 sedimentation tank and the valve leading to the mud tank to discharge the bottom mud. Through the glass window on the pipe, when the material becomes clear, close the valve leading to the mud tank and open the valve leading to the pre-distillation storage tank to discharge the upper clear liquid to the pre-distillation storage tank until it is empty, and prepare to receive the material.

[0053] S70: After the No. 2 sedimentation tank reaches the specified liquid level, switch the valve to make the material in the stirring tank flow to the No. 1 sedimentation tank, and the No. 2 sedimentation tank will settle and prepare for discharge.

[0054] S80: Discharging material from sedimentation tank #2 is the same as in step S70;

[0055] S90: The sedimentation tank and the No. 2 sedimentation tank alternately operate for receiving and discharging materials.

[0056] In this embodiment, the amount of precipitation aid added in step S20 is 9‰ of the mass of crude titanium tetrachloride. The precipitation aid in step S20 includes the following raw materials by weight percentage: stearic acid 4.5%, oleic acid 75.5%, linoleic acid 15%, and linolenic acid 5%.

[0057] Linoleic acid is obtained by extracting a solution containing linoleic acid from corn bran, followed by extraction with an organic solvent, concentration to obtain crude linoleic acid oil, and purification to obtain high-purity linoleic acid. The organic solvent is ethanol.

[0058] Specifically, the purification was carried out using the urea inclusion method. The specific steps of the urea inclusion method were as follows: urea and methanol were added to the crude linoleic acid fraction in a ratio of 1:9:30, the reaction temperature was 75℃, the reaction time was 50 min, the inclusion temperature was 25℃, and the inclusion time was 26 hours.

[0059] In addition, linolenic acid is either α-linolenic acid or γ-linolenic acid.

[0060] Example 3

[0061] A method for accelerating the precipitation of solid suspended impurities in crude titanium tetrachloride involves adding a precipitation aid to the crude titanium tetrachloride. The precipitation aid reacts with titanium tetrachloride at room temperature to generate a large amount of flocculent material, which adsorbs the solid suspended impurities and precipitates them rapidly. The precipitation aid is a mixture of long-chain alkanes or alkenes.

[0062] like Figure 1 As shown, the specific steps are as follows:

[0063] S10: Measure the temperature of the crude titanium tetrachloride container and ensure that the temperature is ≤65℃;

[0064] S20: Add crude titanium tetrachloride and precipitating agent from the bottom of the mixing tank in a certain proportion;

[0065] S30: While adding the precipitating agent and crude titanium tetrachloride into the mixing tank, turn on the stirrer at a speed of approximately 120 RPM.

[0066] S40: Open the overflow valve at the top of the stirring tank to the No. 1 sedimentation tank; after the No. 1 sedimentation tank reaches the specified liquid level, adjust the valve to allow it to overflow to the No. 2 sedimentation tank;

[0067] S50: During the receiving period of material in sedimentation tank #2, the material in sedimentation tank #1 settles and is prepared for discharge.

[0068] S60: When discharging, open the bottom valve of the No. 1 sedimentation tank and the valve leading to the mud tank to discharge the bottom mud. Through the glass window on the pipe, when the material becomes clear, close the valve leading to the mud tank and open the valve leading to the pre-distillation storage tank to discharge the upper clear liquid to the pre-distillation storage tank until it is empty, and prepare to receive the material.

[0069] S70: After the No. 2 sedimentation tank reaches the specified liquid level, switch the valve to make the material in the stirring tank flow to the No. 1 sedimentation tank, and the No. 2 sedimentation tank will settle and prepare for discharge.

[0070] S80: Discharging material from sedimentation tank #2 is the same as in step S70;

[0071] S90: The sedimentation tank and the No. 2 sedimentation tank alternately operate for receiving and discharging materials.

[0072] In this embodiment, the amount of precipitation aid added in step S20 is 2‰ of the mass of crude titanium tetrachloride. The precipitation aid in step S20 includes the following percentage weight of raw materials: 10% stearic acid, 80% oleic acid, and 10% linoleic acid.

[0073] Linoleic acid is obtained by extracting a solution containing linoleic acid from corn bran, extracting with organic solvents, concentrating to obtain crude linoleic acid oil, and then purifying it to obtain high-purity linoleic acid.

[0074] Specifically, the organic solvent is ethanol, and the purification process uses urea inclusion method.

[0075] In addition, the specific steps of the urea inclusion method purification are as follows: urea and methanol are added to the crude linoleic acid fraction in a ratio of 1:9:30, the reaction temperature is 75℃, the reaction time is 50 min, the inclusion temperature is 25℃, and the inclusion time is 26 hours.

[0076] The present invention provides a method for accelerating the precipitation of solid suspended impurities in crude titanium tetrachloride. This method employs the concept of flocculation for water purification, which differs from the simple sedimentation of traditional methods. Specifically, a precipitation aid is added to the crude titanium tetrachloride. The principle is similar to that of flocculants for precipitating solid suspended impurities in wastewater. After reacting with titanium tetrachloride at room temperature, the aid generates a large amount of flocculent material, which adsorbs and rapidly precipitates the solid suspended impurities. This increases the precipitation rate of solid impurities in crude titanium tetrachloride, shortens the sedimentation time, and reduces production costs. After adding the precipitation aid, the solid suspended impurities in crude titanium tetrachloride can be basically precipitated within five minutes, and become clear and transparent in about half an hour. This significantly shortens the sedimentation time, improves the efficiency of the settling tank, and also makes the vanadium slag after vanadium removal purer and more valuable.

[0077] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely preferred examples and are not intended to limit the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the present invention as claimed. The scope of protection of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for accelerating the precipitation of solid suspended impurities in crude titanium tetrachloride, characterized in that: A precipitating agent is added to crude titanium tetrachloride. The precipitating agent reacts with titanium tetrachloride at room temperature to generate a large amount of flocculent material, which adsorbs and rapidly precipitates solid suspended impurities. The specific steps are as follows: S10: Measure the temperature of the crude titanium tetrachloride container and ensure that the temperature is ≤65℃; S20: Add crude titanium tetrachloride and precipitating agent from the bottom of the mixing tank in a certain proportion; S30: While adding the precipitating agent and crude titanium tetrachloride into the mixing tank, turn on the stirrer at a stirring rate of 120 RPM. S40: Open the overflow valve at the top of the stirring tank to the No. 1 sedimentation tank; after the No. 1 sedimentation tank reaches the specified liquid level, adjust the valve to make it overflow to the No. 2 sedimentation tank; S50: During the receiving period of material in sedimentation tank #2, the material in sedimentation tank #1 settles and is prepared for discharge. S60: When discharging, open the bottom valve of the No. 1 sedimentation tank and the valve leading to the mud tank to discharge the bottom mud. Through the glass window on the pipe, when the material becomes clear, close the valve leading to the mud tank and open the valve leading to the pre-distillation storage tank to discharge the upper clear liquid to the pre-distillation storage tank until it is empty, and prepare to receive the material. S70: After the No. 2 sedimentation tank reaches the specified liquid level, switch the valve to make the material in the stirring tank flow to the No. 1 sedimentation tank, and the No. 2 sedimentation tank will settle and prepare for discharge. S80: Discharge of material from sedimentation tank #2 is the same as in step S60; S90: Settling tank #1 and settling tank #2 operate alternately for receiving and discharging materials; The amount of precipitation aid added in step S20 is 2‰-9‰ of the mass of crude titanium tetrachloride; The precipitation aid mentioned in step S20 comprises the following raw materials by weight percentage: stearic acid 4%-10%, oleic acid 70%-80%, linoleic acid 10%-20%, and linolenic acid 0%-5%.

2. The method for accelerating the precipitation of solid suspended impurities in crude titanium tetrachloride according to claim 1, characterized in that: The precipitation aid mentioned in step S20 comprises the following raw materials by weight percentage: stearic acid 6.52%, oleic acid 76.85%, linoleic acid 15.83%, and linolenic acid 0.8%.

3. The method for accelerating the precipitation of solid suspended impurities in crude titanium tetrachloride according to claim 1, characterized in that: The linoleic acid is obtained by extracting a solution containing linoleic acid from corn bran, followed by organic solvent extraction, concentration to obtain crude linoleic acid oil, and purification to obtain high-purity linoleic acid.

4. The method for accelerating the precipitation of solid suspended impurities in crude titanium tetrachloride according to claim 3, characterized in that: The organic solvent is ethanol.

5. The method for accelerating the precipitation of solid suspended impurities in crude titanium tetrachloride according to claim 3, characterized in that: The purification process employed a urea encapsulation method.

6. The method for accelerating the precipitation of solid suspended impurities in crude titanium tetrachloride according to claim 1, characterized in that: The linolenic acid is α-linolenic acid or γ-linolenic acid.

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