CN112745699A - Preparation method of titanium dioxide for extinction of spandex fibers - Google Patents
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
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Abstract
The invention discloses a preparation method of titanium dioxide for extinction of spandex fibers, which comprises the following steps of crushing titanium-rich ore, introducing chlorine gas, adding artificial or natural rutile for chlorination to obtain crude titanium tetrachloride, precipitating and filtering residues to remove waste materials, refining and purifying filtrate in a filtering and rectifying mode to obtain refined titanium tetrachloride, sequentially adding aluminum trioxide, preheating, introducing oxygen for oxidation and carrying out gas-solid separation to obtain crude titanium dioxide, pulping, dispersing, carrying out water separation and grading to obtain relatively pure titanium dioxide, and then coating, washing, drying and carrying out superfine grinding to obtain the titanium dioxide; compared with the titanium dioxide prepared by the traditional process, the titanium dioxide prepared by the preparation method has more excellent optical property, covering power, decoloring power and weather resistance; and the regeneration and utilization of chlorine can be realized in the preparation process, the three-waste discharge of a factory is effectively reduced, and the environment protection is facilitated.
Description
Technical Field
The invention belongs to the technical field of textile raw materials, and particularly relates to a preparation method of titanium dioxide for extinction of spandex fibers.
Background
Spandex, which is the most rapidly developed synthetic fiber in the world, is often blended with fibers such as polyester, cotton, wool and the like or applied to textiles in the form of core spun yarns and the like. Because of the high elasticity of the spandex, a small amount of spandex can ensure that yarns, fabrics and clothes have good elasticity, so the spandex is widely applied to textiles.
In the case of spandex fibers, a white pigment is added to improve the optical properties of the spandex fibers before spinning, and the process is called spinning matting, and the added white pigment is called a "matting agent". Anatase titanium dioxide has a good refractive index and sufficient hardness, is strong in adhesion, stable in properties, and high in melting point, and is considered to be the best white pigment in the world today. Can be widely applied to the industries of paint, plastic, rubber, cosmetics and chemical fiber. Anatase titanium dioxide is commonly used as a delustering agent in the chemical fiber industry. The average addition amount of the titanium dioxide for fiber-grade extinction is 0.3 percent of the total amount of the fiber, the market gap is large, and most of the titanium dioxide depends on import.
The preparation method of the titanium dioxide comprises a chlorination method, wherein natural rutile, artificial rutile or high titanium slag is used as a raw material in the chlorination method, and a finished product is prepared by chlorination, refining, oxidation and surface treatment. The process has the characteristics of short production flow, continuous operation, large scale of single-series devices and less discharge of three wastes; however, the production process of titanium dioxide by a chlorination process relates to multiple subjects and professions such as chemical industry, metallurgy, materials, machinery, control, fluid and the like, the technical difficulty is high, and key equipment is complex.
For a long time, the process of producing titanium dioxide in China is laggard, the product quality is unstable, and the grade is low. The paint has the advantages of poor weather resistance, poor dispersibility, low decoloring force, low covering power and high oil absorption amount in the application of textile raw materials.
Disclosure of Invention
The invention aims to: the preparation method of the titanium dioxide for extinction of the spandex fiber is provided, and the titanium dioxide prepared by the preparation method has more excellent optical performance, covering power, color reducing power and weather resistance than the titanium dioxide prepared by the traditional process; and the regeneration and utilization of chlorine can be realized in the preparation process, the three-waste discharge of a factory is effectively reduced, and the environment protection is facilitated.
The technical scheme adopted by the invention is as follows:
a preparation method of titanium dioxide for extinction of spandex fibers comprises the following steps of crushing titanium-rich ores, introducing chlorine gas, adding artificial or natural rutile for chlorination to obtain crude titanium tetrachloride, precipitating and filtering residues to remove waste materials, refining and purifying filtrate in a filtering and rectifying mode to obtain refined titanium tetrachloride, sequentially adding aluminum trioxide, preheating, introducing oxygen for oxidation and carrying out gas-solid separation to obtain crude titanium dioxide, pulping, dispersing, carrying out water separation and grading to obtain pure titanium dioxide, and then coating, washing, drying and carrying out superfine grinding to obtain the titanium dioxide.
Wherein, chlorine generated in the gas-solid separation process is supplemented to the chlorination stage.
In the chlorination process, the titanium-rich ore, rutile powder and petroleum coke are mixed and added into a fluidized bed furnace, chlorine is introduced upwards from the bottom of the furnace, and the temperature in the furnace is kept at 950-1000 ℃.
Wherein, in the oxidation process, the refined titanium tetrachloride and the aluminum trioxide are moderated and then put into an oxidation reactor for reaction; and (3) generating gas with titanium dioxide particles through reaction, cooling the gas by using chlorine after the gas is led out, reducing the temperature of the gas to 400-600 ℃, cooling the gas to 170-190 ℃ by using a cooling pipeline, and dechlorinating the titanium dichloride by using a separator and a collector.
In the coating process, an aluminum sulfate solution and a sodium silicate mixed solution are dropwise added into titanium dioxide slurry, the molecular weight ratio of the aluminum sulfate solution to the sodium silicate mixed solution is 3: 1-4: 1, the pH is adjusted by alkali or acid and kept at 8-10, the dropwise adding time is 3-5 hours, and then heat preservation and aging are carried out; after the completion, adjusting the pH value to 6-7 and washing with water; and then adding one or more of organic amine, polyol or organic silicon at the normal temperature, wherein the weight percentage of the organic amine is 0.04-0.08%.
Wherein the aluminum sulfate solution is prepared into 150-180 g/L solution according to TiO23.0-6.0 wt% of Al2O3Meter) is added to the titanium dioxide slurry.
Wherein the alkali metal ion concentration (as Na) of the sodium silicate solution is maintained2Calculated by O) is 0.2 to 0.4MoL/L in terms of TiO20.5-2% of mass (as SiO)2Amount) was added to the titanium dioxide slurry.
In the preparation method of the titanium dioxide, a pneumatic conveying system is adopted for conveying the powdery material; the pneumatic conveying system comprises a pneumatic conveying pipeline, and the pneumatic conveying pipeline comprises an inner pipe and an outer pipe sleeved outside the inner pipe; a plurality of annular fluid mechanics bodies with smooth arc-shaped axial sections are continuously arranged on the inner wall of the inner pipe along the axial direction of the inner pipe; for any one fluid mechanical body, an annular air inlet slit and an annular air outlet slit are respectively formed on the inner pipe at the intersection of the two ends of the fluid mechanical body and the inner pipe along the edge of the fluid mechanical body; the relative positions of the annular air inlet slit and the annular air outlet slit are respectively positioned at the upstream and the downstream of the powder conveying direction; the annular air inlet slit and the annular air outlet slit are respectively and smoothly connected with the fluid mechanics body and tangent to the cambered surface at the connection part of the fluid mechanics body; the outer tube is the annular duct, annular air inlet slit communicates with the outer tube through annular air inlet chamber respectively, and the pressurized gas stream passes through outer tube, annular air inlet chamber and annular air inlet slit flow out.
The annular air outlet seam is communicated with the annular air inlet slit of the adjacent fluid mechanics body, and the outlet of the annular air outlet seam faces the outlet direction of the annular air inlet slit.
The flow direction of the pressurized air flow in the outer pipe is opposite to the powder conveying direction, the axial section of the annular air inlet cavity is arc-shaped, and the pressurized air flow is guided to enter the annular air inlet slit after being swirled.
The invention has the following beneficial effects:
1. compared with titanium dioxide prepared by the traditional process, the titanium dioxide prepared by the preparation method disclosed by the invention has more excellent optical property, covering power, decoloring power and weather resistance, and can realize the regeneration and use of chlorine in the preparation process, thereby effectively reducing the three-waste discharge of a factory and being beneficial to environmental protection.
2. The oxidation process can quickly and uniformly convert titanium tetrachloride into titanium dioxide, utilizes chlorine to cool, is convenient for subsequent separation and reuse, does not introduce other elements to influence the purity of the product, is linked with the whole process, and reduces the mixing of additional elements.
3. According to the invention, the inorganic coating is carried out by adopting the mixed solution of the aluminum sulfate solution and the sodium silicate in the coating process, so that the effective complementary action is realized, the surface defect generated by a single coating is compensated, the titanium dioxide has a good photocatalysis shielding effect, and the weather resistance and the acid solubility of the titanium dioxide are improved by blocking and covering the lattice defect of the titanium dioxide and reducing the direct contact of the titanium dioxide and light; and the rheological property, the dispersion and the wetting property of the titanium dioxide in an organic medium are effectively improved by carrying out organic coating for the second time.
4. The invention applies the pneumatic conveying system in the preparation method of titanium dioxide, the pneumatic conveying system adopts airflow diaphragm formed by using coanda effect, the relay mode is adopted to drive the material distribution to move along the conveying direction while isolating the material distribution, and the relay mode is adopted, so the conveying process is stable, the defects that the existing pneumatic conveying system for material distribution needs to introduce large-flow airflow at the end part of a pipeline are avoided, the defects comprise extremely large required airflow, no longer conveying distance, high energy consumption, unstable conveying, serious friction and collision of powder and the pipe wall, high dust content in the surrounding environment and the like, and the defects can be obviously improved by the pneumatic conveying system.
5. According to the invention, the wind film is formed on the surface of the fluid mechanical body through the coanda effect, the wind film drives the powder to move towards the conveying direction on one hand, and the direct contact between the powder and the inner wall of the pipeline is isolated on the other hand, so that the friction is reduced, the arc-shaped structure of the fluid mechanical body is utilized to enable the powder to cross the annular air outlet seam under the action of the inertia of the powder, and the airflow tightly attached to the surface of the fluid mechanical body flows into the annular air outlet seam under the coanda effect, so that the solid-gas separation is realized, and the powder is prevented from also entering the annular air outlet seam; the air flow dissipated from the lower part of the powder resistance to the middle part of the inner pipe can support the powder to disperse the powder, so that the powder is more uniformly pushed by the air flow, and the conveying efficiency is obviously improved.
6. The invention utilizes the circular structure of the pipeline to ensure that the annular air inlet slit and the fluid mechanical body are also annular, and the closed-loop fluid is formed by matching air outlet, so that the rear air is driven to uniformly move forwards according to the Bernoulli principle, and an air amplification effect is formed, thereby the material distribution in the middle of the pipeline is also driven forwards in an air flow relay and uniform manner.
7. The annular air outlet seam of the invention is internally communicated with the annular air inlet slit of the adjacent fluid mechanics body, the opening direction faces to the fluid direction of the annular air inlet slit, the structure utilizes the residual air after the adjacent fluid mechanics body at the upstream completes the wind film task to increase the wind power of the air outlet of the annular air inlet slit, simultaneously, the wind speed of the airflow in the annular air inlet slit is larger, and the negative pressure is formed between the airflow and the annular air outlet slit according to the Bernoulli principle, so that the air of the annular air outlet slit can be sucked in, the negative pressure at the opening of the annular air outlet slit is increased, thus the airflow after the wind film task is completed on the fluid mechanics body can more easily enter the annular air outlet slit, only the caliber of the annular air outlet slit and the annular air inlet slit is designed, the proper solid-gas separation can be realized by matching with the proper air inlet pressure, and the communication structure of the annular air outlet slit and the annular air inlet slit also enables even a small amount of powder to enter the, can also enter the inner pipe through the annular air inlet slit.
Drawings
FIG. 1 is a schematic process diagram of the present invention;
FIG. 2 is a schematic structural view of a pneumatic conveying pipeline according to the present invention;
fig. 3 is a partial structure schematic view of the pneumatic conveying pipeline of the invention.
The labels in the figure are:
1-inner tube, 2-outer tube, 3-fluid mechanics body, 4-annular air inlet slit, 5-annular air outlet slit, 6-annular air inlet cavity.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The procedures in the method are not specifically described and only need to be implemented according to the existing mature technology and process, and the laboratory verifies that the process which is not specifically mentioned in the invention has stronger flexibility, and the implementation of the existing relevant mature process has no obvious adverse effect on the final effect of the preparation method.
Referring to fig. 1, scheme one:
a preparation method of titanium dioxide for extinction of spandex fibers comprises the following steps of crushing titanium-rich ores, introducing chlorine gas, adding artificial or natural rutile for chlorination to obtain crude titanium tetrachloride, precipitating and filtering residues to remove waste materials, refining and purifying filtrate in a filtering and rectifying mode to obtain refined titanium tetrachloride, sequentially adding aluminum trioxide, preheating, introducing oxygen for oxidation and carrying out gas-solid separation to obtain crude titanium dioxide, pulping, dispersing, carrying out water separation and grading to obtain pure titanium dioxide, and then coating, washing, drying and carrying out superfine grinding to obtain the titanium dioxide.
Chlorine generated in the gas-solid separation process is supplemented to the chlorination stage.
In the chlorination process, the titanium-rich ore, rutile powder and petroleum coke are mixed and added into a fluidized bed furnace, chlorine is introduced upwards from the bottom of the furnace, and the temperature in the furnace is kept at 950-1000 ℃.
In the oxidation process, the refined titanium tetrachloride and the aluminum trioxide are put into an oxidation reactor for reaction after being moderated; and (3) generating gas with titanium dioxide particles through reaction, cooling the gas by using chlorine after the gas is led out, reducing the temperature of the gas to 400-600 ℃, cooling the gas to 170-190 ℃ by using a cooling pipeline, and dechlorinating the titanium dichloride by using a separator and a collector.
In the coating process, a mixed solution of aluminum sulfate and sodium silicate is dropwise added into titanium dioxide slurry, the molecular weight ratio of the aluminum sulfate solution to the sodium silicate solution is 3:1, the pH is adjusted and maintained at 8 by alkali or acid, the dropwise adding time is 5 hours, and then the mixture is subjected to heat preservation and aging; after the completion, adjusting the pH value to 7 and washing with water; then adding 0.08 wt% of a mixture of organic amine, polyhydric alcohol and organic silicon at normal temperature, wherein the mixing ratio is 1:2: 1.
Preparing 150g/L solution of aluminum sulfate according to TiO26.0% of the mass (in terms of Al)2O3Meter) is added to the titanium dioxide slurry.
Maintaining the alkali metal ion concentration (as Na) of the sodium silicate solution2Calculated as O) is 0.4MoL/L, calculated as TiO 22% by mass (in SiO)2Amount) was added to the titanium dioxide slurry.
Scheme II:
the difference between the second scheme and the first scheme is that:
in the oxidation process, the refined titanium tetrachloride and the aluminum trioxide are put into an oxidation reactor for reaction after being moderated; and (3) generating gas with titanium dioxide particles through reaction, cooling the gas by using chlorine after the gas is led out, reducing the temperature of the gas to 400-600 ℃, cooling the gas to 170-190 ℃ by using a cooling pipeline, and dechlorinating the titanium dichloride by using a separator and a collector.
In the coating process, a mixed solution of aluminum sulfate and sodium silicate is dropwise added into titanium dioxide slurry, the molecular weight ratio of the aluminum sulfate solution to the sodium silicate solution is 4:1, the pH is adjusted and maintained at 10 by alkali or acid, the dropwise adding time is 3 hours, and then the heat preservation and aging are carried out; after the completion, adjusting the pH value to 6 and washing with water; then 0.04 wt% of organic amine is added at normal temperature.
Preparing the aluminum sulfate solution into 180g/L solution according to TiO23.0% of the mass (in terms of Al)2O3Meter) is added to the titanium dioxide slurry.
Maintaining the alkali metal ion concentration (as Na) of the sodium silicate solution2Calculated as O) is 0.2MoL/L, calculated as TiO20.5% of mass (in SiO)2Amount) was added to the titanium dioxide slurry.
The third scheme is as follows:
the difference between the third scheme and the first scheme is that:
in the oxidation process, the refined titanium tetrachloride and the aluminum trioxide are put into an oxidation reactor for reaction after being moderated; and (3) generating gas with titanium dioxide particles through reaction, cooling the gas by using chlorine after the gas is led out, reducing the temperature of the gas to 400-600 ℃, cooling the gas to 170-190 ℃ by using a cooling pipeline, and dechlorinating the titanium dichloride by using a separator and a collector.
In the coating process, a mixed solution of aluminum sulfate and sodium silicate is dropwise added into titanium dioxide slurry, the molecular weight ratio of the aluminum sulfate solution to the sodium silicate solution is 7:2, the pH is adjusted and maintained at 9 by alkali or acid, the dropwise adding time is 4 hours, and then the heat preservation and aging are carried out; after the completion, adjusting the pH value to 7 and washing with water; then 0.06 wt% of silicone was added at normal temperature.
The aluminum sulfate solution is prepared into 170g/L solution according to TiO25.0% by mass (in terms of Al)2O3Meter) is added to the titanium dioxide slurry.
Maintaining the alkali metal ion concentration (as Na) of the sodium silicate solution2Calculated as O) is 0.3MoL/L, calculated as TiO21.5% of the mass (in SiO)2Amount) was added to the titanium dioxide slurry.
Mixing the titanium dioxide prepared by the three methods with TiO imported from a certain date2Product (control 1) and chemical fiber grade TiO of a company in China2The product (control 2) was quality compared. The test results are summarized below:
the test result shows that compared with the control 1 and the control 2, the titanium dioxide prepared by the method has the advantages that the overall quality is obviously improved, the iron content is slightly different, the water content is slightly higher than that of the control 1 but is obviously lower than that of the control 2, the overall particle size distribution is reasonable in the aspect of particle size distribution, the particle size is close to or even exceeds that of the control 1, and the particle size is obviously improved compared with that of the control 2; the specific surface area already slightly exceeded control 1 and more than control 2.
The titanium dioxide prepared by the three methods is applied to the production of spandex chemical fiber together with an imported model TiO2 product (contrast 1) at a certain day and a chemical fiber grade TiO2 product (contrast 2) of a certain company in China, the fiber quality (filament) is detected, and the test results are summarized as follows:
| 22.2dtex | example one | Example two | EXAMPLE III | Control 1 | |
| Breaking strength/(cN.dtex)-1) | 1.38 | 1.33 | 1.35 | 1.22 | 1.08 |
| Elongation at break/% | 713.3 | 721.2 | 715.6 | 731.2 | 634.4 |
| Defect/(mg.0.01.g)-1) | 0 | 0 | 0 | 0 | 0 |
| Breaking Strength/cN | 30.23 | 30.43 | 31.22 | 30.11 | 29.32 |
| Powder/(mg.0.01.g)-1) | 4 | 4 | 4 | 5 | 8 |
| Linear density deviation ratio/%) | 3 | 2 | 2 | 2 | 1 |
The test result shows that compared with the comparison 1 and the comparison 2, the titanium dioxide prepared by the three methods is qualified in the quality of fiber filament products applied to spandex chemical fiber production as the delustering agent, the elongation at break of the filament added with the titanium dioxide of the first to third embodiments is improved to a certain extent, the powder is low, and the method is environment-friendly.
Referring to fig. 2 and 3, further, in the method for preparing titanium dioxide, a pneumatic conveying system is adopted for conveying the powdery material; the pneumatic conveying system comprises a pneumatic conveying pipeline, and the pneumatic conveying pipeline comprises an inner pipe 1 and an outer pipe 2 sleeved outside the inner pipe 1; a plurality of annular fluid mechanics bodies 3 with smooth arc-shaped axial sections are continuously arranged on the inner wall of the inner pipe 1 along the axial direction; for any one fluid mechanical body 3, an annular air inlet slit 4 and an annular air outlet slit 5 are respectively arranged on the inner pipe 1 at the intersection of the two ends of the fluid mechanical body 3 and the inner pipe 1 along the edge of the fluid mechanical body 3; the relative positions of the annular air inlet slit 4 and the annular air outlet slit 5 are respectively positioned at the upstream and the downstream of the powder conveying direction; the annular air inlet slit 4 and the annular air outlet slit 5 are respectively and smoothly connected with the fluid mechanics body 3 and tangent to the cambered surface at the connection part of the fluid mechanics body 3; the outer pipe 2 is an annular pipeline, the annular air inlet slits 4 are respectively communicated with the outer pipe 2 through an annular air inlet cavity 6, and pressurized air flows out through the outer pipe 2, the annular air inlet cavity 6 and the annular air inlet slits 4.
Furthermore, annular air-out slit 5 is in with adjacent hydrodynamics body 3's annular air inlet slit 4 inside intercommunication, 5 exit orientations of annular air-out slit 4 of annular air inlet slit.
Furthermore, the flow direction of the pressurized air flow in the outer pipe 2 is opposite to the powder conveying direction, the axial section of the annular air inlet cavity 6 is arc-shaped, and the pressurized air flow is guided to flow back to swirl and then enters the annular air inlet slit 4.
The pneumatic conveying system is applied in the preparation method of titanium dioxide, the coanda effect is utilized to form the airflow diaphragm, the relay mode is adopted to drive the separated material to move along the conveying direction while the separated material is isolated, and the relay mode is adopted, so that the conveying process is stable, the defects that the existing pneumatic conveying system for separated material needs to introduce large-flow airflow at the end part of a pipeline are avoided, the defects comprise that the required airflow is extremely large, the conveying distance cannot be far, the energy consumption is large, the conveying is unstable, the friction and collision of powder and the pipe wall are serious, the dust content in the surrounding environment is high, and the like.
The air film is formed on the surface of the fluid mechanics body through the coanda effect, the air film drives the powder to move towards the conveying direction on one hand, and on the other hand, the direct contact between the powder and the inner wall of the pipeline is isolated, so that the friction is reduced, the arc-shaped structure of the fluid mechanics body 3 is utilized to enable the powder to cross the annular air outlet seam 5 under the action of the inertia of the powder, and the airflow tightly attached to the surface of the fluid mechanics body 3 flows into the annular air outlet seam 5 under the coanda effect, so that the solid-air separation is realized, and the powder is prevented from also entering the annular air outlet seam 5; the air flow which escapes from the lower part of the powder resistance to the middle part of the inner pipe 1 can support the powder to disperse the powder, so that the powder is more uniformly pushed by the air flow, and the conveying efficiency is obviously improved.
The circular structure of the inner tube 1 is utilized, the annular air inlet slit 4 and the fluid mechanical body 3 are also in an annular shape, closed-loop fluid is formed by matching air outlet, and according to the Bernoulli principle, rear air is driven to move forwards uniformly, an air amplification effect is formed, and therefore powder in the middle of the inner tube 1 is driven forwards uniformly in an air flow relay mode.
The annular air outlet slit 5 is communicated with the annular air inlet slit 4 of the adjacent fluid mechanics body 3 inside, the opening direction faces the fluid direction of the annular air inlet slit 4, the structure reuses the residual air after the adjacent fluid mechanics body 3 at the upstream completes the air film task to increase the air outlet wind power of the annular air inlet slit 4, meanwhile, the air speed of the air flow in the annular air inlet slit 4 is larger, and according to the Bernoulli principle, negative pressure is formed between the annular air outlet slit 4 and the annular air outlet slit 5, so that the air of the annular air outlet slit 5 can be sucked, the negative pressure at the opening of the annular air outlet slit 5 is increased, the air flow after the air film task is completed on the fluid mechanics body 3 can more easily enter the annular air outlet slit 5, only the calibers of the annular air outlet slit 5 and the annular air inlet slit 4 are designed, and proper air inlet pressure is matched, proper solid-gas separation can be realized, and even though a small amount of powder enters the annular air outlet slit 5 through the communication structure of the annular air outlet And can also return to the inner pipe through the annular air inlet slit 4.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. A preparation method of titanium dioxide for extinction of spandex fiber is characterized by comprising the following steps: crushing titanium-rich ore, introducing chlorine gas, adding artificial or natural rutile for chlorination to obtain crude titanium tetrachloride, precipitating filter residue to remove waste, refining the filtrate in a filtering and rectifying manner to obtain refined titanium tetrachloride, sequentially adding aluminum trioxide, preheating, introducing oxygen for oxidation and carrying out gas-solid separation to obtain crude titanium dioxide, pulping, dispersing, carrying out water separation and grading to obtain relatively pure titanium dioxide, and then coating, washing, drying and carrying out superfine grinding to obtain the titanium dioxide.
2. The preparation method of the titanium dioxide for extinction of the spandex fiber, according to claim 1, is characterized in that: chlorine generated in the gas-solid separation process is supplemented to the chlorination stage.
3. The preparation method of the titanium dioxide for extinction of the spandex fiber, according to claim 1, is characterized in that: in the chlorination process, the titanium-rich ore, rutile powder and petroleum coke are mixed and added into a fluidized bed furnace, chlorine is introduced upwards from the bottom of the furnace, and the temperature in the furnace is kept at 950-1000 ℃.
4. The preparation method of the titanium dioxide for extinction of the spandex fiber, according to claim 1, is characterized in that: in the oxidation process, the refined titanium tetrachloride and the aluminum trioxide are put into an oxidation reactor for reaction after being moderated; and (3) generating gas with titanium dioxide particles through reaction, cooling the gas by using chlorine after the gas is led out, reducing the temperature of the gas to 400-600 ℃, cooling the gas to 170-190 ℃ by using a cooling pipeline, and dechlorinating the titanium dichloride by using a separator and a collector.
5. The preparation method of the titanium dioxide for extinction of the spandex fiber, according to claim 1, is characterized in that: in the coating process, a mixed solution of aluminum sulfate and sodium silicate is dropwise added into titanium dioxide slurry, the molecular weight ratio of the aluminum sulfate solution to the sodium silicate solution is 3: 1-4: 1, the pH is adjusted by alkali or acid and kept at 8-10, the dropwise adding time is 3-5 hours, and then heat preservation and aging are carried out; after the completion, adjusting the pH value to 6-7 and washing with water; and then adding one or more of organic amine, polyol or organic silicon at the normal temperature, wherein the weight percentage of the organic amine is 0.04-0.08%.
6. A method for preparing titanium dioxide for extinction of spandex fiber according to claim 5, characterized in that: preparing the aluminum sulfate solution into a 150-180 g/L solution according to TiO23.0-6.0 wt% of Al2O3Meter) is added to the titanium dioxide slurry.
7. A method for preparing titanium dioxide for extinction of spandex fiber according to claim 5, characterized in that: maintaining the alkali metal ion concentration (as Na) of the sodium silicate solution2Calculated by O) is 0.2 to 0.4MoL/L in terms of TiO20.5-2% of mass (as SiO)2Amount) was added to the titanium dioxide slurry.
8. The method for preparing titanium dioxide for matting acrylic chemical fiber as claimed in any one of claims 1 to 7, characterized in that: in the preparation method of the titanium dioxide, a pneumatic conveying system is adopted for conveying the powdery material; the pneumatic conveying system comprises a pneumatic conveying pipeline, and the pneumatic conveying pipeline comprises an inner pipe (1) and an outer pipe (2) sleeved outside the inner pipe (1); a plurality of annular fluid mechanics bodies (3) with smooth arc-shaped axial sections are continuously arranged on the inner wall of the inner pipe (1) along the axial direction; for any one fluid mechanical body (3), an annular air inlet slit (4) and an annular air outlet slit (5) are respectively formed on the inner pipe (1) at the intersection of the two ends of the fluid mechanical body and the inner pipe (1) along the edge of the fluid mechanical body (3); the relative positions of the annular air inlet slit (4) and the annular air outlet slit (5) are respectively positioned at the upstream and the downstream of the powder conveying direction; the annular air inlet slit (4) and the annular air outlet slit (5) are respectively and smoothly connected with the fluid mechanics body (3) and tangent to the cambered surface at the connection part of the fluid mechanics body (3); the outer tube (2) is an annular pipeline, the annular air inlet slits (4) are communicated with the outer tube (2) through annular air inlet cavities (6) respectively, and pressurized air flows pass through the outer tube (2), the annular air inlet cavities (6) and the annular air inlet slits (4) to flow out.
9. The method for preparing titanium dioxide for matting acrylic chemical fiber as claimed in claim 8, wherein: annular air-out seam (5) is in with annular air inlet slit (4) of adjacent fluid mechanics body (3) annular air inlet slit (4) inside intercommunication, and annular air-out seam (5) exit is towards the export direction of annular air inlet slit (4).
10. The method for preparing titanium dioxide for delustering acrylic fiber as claimed in claim 9, characterized in that: the flow direction of the pressurized air flow in the outer pipe (2) is opposite to the powder conveying direction, the axial section of the annular air inlet cavity (6) is arc-shaped, and the pressurized air flow is guided to flow back to swirl and then enters the annular air inlet slit (4).
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4759800A (en) * | 1986-02-27 | 1988-07-26 | Kronos Titan, Gmbh | Process for the improvement of titanium dioxide pigments by post-treatment |
| CN102320474A (en) * | 2011-06-15 | 2012-01-18 | 何智 | material-in-air conveying theory principle and technical scheme of conveying material by fluid |
| CN107758738A (en) * | 2017-11-29 | 2018-03-06 | 广西雅照钛白有限公司 | A kind of titanium dioxide chloridising production technology |
-
2020
- 2020-12-30 CN CN202011604837.9A patent/CN112745699A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4759800A (en) * | 1986-02-27 | 1988-07-26 | Kronos Titan, Gmbh | Process for the improvement of titanium dioxide pigments by post-treatment |
| CN102320474A (en) * | 2011-06-15 | 2012-01-18 | 何智 | material-in-air conveying theory principle and technical scheme of conveying material by fluid |
| CN107758738A (en) * | 2017-11-29 | 2018-03-06 | 广西雅照钛白有限公司 | A kind of titanium dioxide chloridising production technology |
Non-Patent Citations (2)
| Title |
|---|
| 王杏等: "《纳米二氧化钛的生产与应用》", 31 July 2014, 贵阳：贵州科技出版社 * |
| 邓科等: "氯化法钛白粉的生产工艺与技术经济分析", 《中国氯碱》 * |
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