Method for reducing influence of high-phosphorus titanium concentrate on stability of titanium solution

Abstract

The invention relates to a method for reducing the influence of high-phosphorus titanium concentrates on the stability of a titanium solution, which comprises the following steps: grinding and sieving 30-specification high-phosphorus titanium concentrates and 10-specification titanium concentrates, and mixing the sieved test samples of the 30-specification high-phosphorus titanium concentrates and the 10-specification titanium concentrates in proportion to obtain a mixed test sample; placing the mixed test sample in a beaker, adding concentrated sulfuric acid, stirring, adding water, heating for reaction, covering the beaker above the beaker, stopping heating when volume expansion occurs, stopping stirring when volume expansion stops, carrying out curing reaction on the beaker, and cooling the beaker to room temperature; adding water into the beaker, setting temperature, stirring and leaching, adding iron powder, controlling Ti < 3 + > to be qualified, adding a flocculating agent, and continuously stirring; and naturally settling the mixed titanium solution, carrying out vacuum filtration, extracting a supernatant titanium solution, and measuring the stability and settling performance of the supernatant titanium solution. According to the method, the stability index required by the hydrolysis procedure can be guaranteed, the 30-specification high-phosphorus titanium concentrate and the 10-specification titanium concentrate are used for preparing and mixing, and the cost of titanium concentrate raw materials can be saved.

Description

Technical Field

[0001] The present invention relates to the field of titanium dioxide production methods, and more specifically, to a method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid. Background Art

[0002] Ilmenite, as a composite mineral, is mainly composed of titanium minerals, titanium iron oxides, phosphorus-containing fluorocarbon compounds, fluorine-containing magnesium silicate and other multi-minerals. Among them, the content of phosphorus has a significant impact on the production process of titanium dioxide. Specifically, excessive phosphorus content will directly damage the key quality indicators of titanium dioxide, including reduced whiteness, weakened stability, and decreased UV resistance. When the phosphorus content in ilmenite exceeds a certain threshold, phosphorus will react chemically with other mineral components to produce a series of phosphorus-containing compounds. During the slurry processing process, these compounds are deposited on the surface of the slurry due to gravity, which in turn increases the viscosity of the slurry and poses a challenge to subsequent separation and purification steps.

[0003] The presence of phosphate ions promotes the hydration reaction of phosphate on the surface of ilmenite, forming a stable phosphate layer. In titanium concentrate with a high phosphorus content, high concentrations of phosphate ions cause a dense phosphate film to form on the surface of water-insoluble ilmenite particles. This film is easily converted into tributyl phosphate under high temperature conditions, and decomposes into phosphorus oxychloride under acidic conditions. The presence of tributyl phosphate not only significantly affects the whiteness and tinting power of titanium dioxide, but also weakens its UV resistance, which is mainly attributed to its easy hydrolysis characteristics in acidic solutions and its influence on the surface charge distribution of titanium dioxide particles.

[0004] Therefore, with the increase of phosphorus content in ilmenite raw materials, the stability of titanium liquid shows a trend of gradual decline. At the same time, the micelles formed by these phosphorus-containing compounds and the accompanying organic impurities on the surface of titanium dioxide particles not only contain a large amount of organic matter that is difficult to dissolve in water, but also increase the energy barrier that needs to be overcome for the collision and dispersion between particles. When this energy demand exceeds the range that the particles themselves can bear, it will lead to the loss of stability of the particles, and then cause agglomeration, which will have an adverse effect on the final quality of titanium dioxide products.

[0005] Therefore, the prior art needs to be improved. Summary of the invention

[0006] The purpose of the present invention is to provide a method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid. The experiment is carried out by simulating the ball milling-acid hydrolysis-reduction-sedimentation process of sulfuric acid process titanium dioxide production. 30 specifications of high-phosphorus titanium concentrate and 10 specifications of titanium concentrate are used in different proportions. The acid hydrolysis tail gas is treated during the acid hydrolysis process, the flocculant is added in the reduction process and the iron powder is added at a rate, and the sedimentation is filtered to carry out stability test evaluation.

[0007] In order to solve the above technical problems or achieve the above objectives, the present invention adopts the following technical solutions, which are specifically described as follows: According to aspects of the present invention, there is provided a method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid, comprising the following steps: 1) Grind and sieve the 30-specification high-phosphorus titanium concentrate and the 10-specification titanium concentrate respectively, take the sieve-downs of each as their respective test samples, and mix the test sample of the 30-specification high-phosphorus titanium concentrate with the test sample of the 10-specification titanium concentrate in proportion to obtain a mixed titanium concentrate test sample; 2) Place the mixed titanium concentrate test sample in a beaker, add concentrated sulfuric acid to the beaker, stir evenly, add water and heat to react, and cover the beaker. When volume expansion occurs, stop heating, and stop stirring when the volume expansion stops. Then place the beaker in a drying oven for aging reaction. After the aging reaction is completed, cool the beaker to room temperature; 3) Add water to the cooled beaker and set the temperature for stirring and leaching. After the leaching is completed, add iron powder to the beaker to control the Ti 3+ If qualified, then add flocculant to the beaker and continue stirring; 4) After the stirring is completed, the mixed titanium liquid in the beaker is allowed to settle naturally, vacuum filtered and the supernatant titanium liquid is extracted to measure its stability and sedimentation performance.

[0008] In one embodiment of the present invention, in step 1), before the 30-specification high-phosphorus titanium concentrate and the 10-specification titanium concentrate are ground and sieved respectively, the 30-specification high-phosphorus titanium concentrate and the 10-specification titanium concentrate are tested for trace elements respectively, and then the 30-specification high-phosphorus titanium concentrate and the 10-specification titanium concentrate are respectively placed in a sealed sample preparation machine for grinding 3-4 times and passed through a 325-mesh sieve, and the respective sieve-under materials are taken as respective test samples.

[0009] In one embodiment of the present invention, in step 1), the ratio of the test sample of 30 specification high phosphorus titanium concentrate to the test sample of 10 specification titanium concentrate is 1:4-1:9.

[0010] In one embodiment of the present invention, in step 2), timing is performed while heating for reaction, and when heating is stopped, the temperature is measured and the reaction time is recorded.

[0011] In one embodiment of the present invention, in step 2), the beaker is covered with 40%-80% coverage above the beaker.

[0012] In one embodiment of the present invention, in step 2), the drying oven is a forced air drying oven, the aging reaction temperature is 170-180° C., and the aging reaction time is 2-4 hours.

[0013] In one embodiment of the present invention, in step 3), the temperature is set to 60-70° C. and the stirring time is 1-2 h.

[0014] In one embodiment of the present invention, in step 3), iron powder is added to the beaker once, twice, three times or four times.

[0015] In one embodiment of the present invention, in step 3), Ti is controlled 3+ After passing the test, measure the temperature after adding iron powder.

[0016] In one embodiment of the present invention, in step 4), the natural sedimentation time is 10-60 minutes.

[0017] By adopting the above technical solution, the present invention has the following advantages compared with the prior art: The method of the present invention realizes the control of the process of using phosphorus titanium concentrate and ensures the stability index required by the hydrolysis process. Compared with the titanium liquid prepared from pure 10-specification titanium concentrate, the stability and sedimentation performance of the titanium liquid prepared by the method of the present invention are slightly lower, but the use of 30-specification high-phosphorus titanium concentrate and 10-specification titanium concentrate for preparation and mixing is conducive to saving the cost of titanium concentrate raw materials. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings in the following description are only some embodiments of the present invention. For ordinary technicians in this field, other embodiments can be obtained based on these drawings without paying creative work.

[0019] The above and / or additional aspects and advantages of the present invention will be more apparent and easily understood in the description of the embodiments in conjunction with the accompanying drawings, in which: Figure 1 A flow chart of a method provided by the present invention for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid is shown. DETAILED DESCRIPTION

[0020] It should be understood that the embodiments of the present invention shown in the exemplary embodiments are only illustrative. Although only a few embodiments are described in detail in the present invention, it is easy for those skilled in the art to appreciate that multiple modifications are feasible without actually departing from the teaching of the subject matter of the present invention. Accordingly, all such modifications should be included within the scope of the present invention. Without departing from the gist of the present invention, other replacements, modifications, changes and deletions may be made to the design, operating conditions and parameters of the following exemplary embodiments.

[0021] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the embodiments of the present invention are further described in detail below in combination with specific embodiments and with reference to the accompanying drawings.

[0022] like Figure 1 As shown, the present invention provides a method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid, comprising the following steps: S101: Grind and sieve the 30-specification high-phosphorus titanium concentrate and the 10-specification titanium concentrate respectively, take the sieve-downs of each as their respective test samples, and mix the test sample of the 30-specification high-phosphorus titanium concentrate with the test sample of the 10-specification titanium concentrate in proportion to obtain a mixed titanium concentrate test sample; S102: placing the mixed titanium concentrate test sample in a beaker, adding concentrated sulfuric acid to the beaker, stirring evenly, adding water and heating for reaction, and covering the beaker above the beaker. When volume expansion occurs, heating is stopped, and stirring is stopped when volume expansion stops. The beaker is then placed in a drying oven for aging reaction. After the aging reaction is completed, the beaker is cooled to room temperature. S103: Add water to the cooled beaker and set the temperature for stirring and leaching. After the leaching is completed, add iron powder to the beaker to control the Ti 3+ If qualified, then add flocculant to the beaker and continue stirring; S104: After the stirring is completed, the mixed titanium liquid in the beaker is naturally settled, vacuum filtered and the supernatant titanium liquid is extracted to measure its stability and sedimentation performance.

[0023] The method of the present invention realizes the control of the process of using phosphorus titanium concentrate and ensures the stability index required by the hydrolysis process. Compared with the titanium liquid prepared from pure 10-specification titanium concentrate, the stability and sedimentation performance of the titanium liquid prepared by the method of the present invention are slightly lower, but the use of 30-specification high-phosphorus titanium concentrate and 10-specification titanium concentrate for preparation and mixing is conducive to saving the cost of titanium concentrate raw materials.

[0024] In a preferred embodiment of the above method, in step S101, before the 30-specification high-phosphorus titanium concentrate and the 10-specification titanium concentrate are ground and sieved respectively, the 30-specification high-phosphorus titanium concentrate and the 10-specification titanium concentrate are tested for trace elements respectively, and then the 30-specification high-phosphorus titanium concentrate and the 10-specification titanium concentrate are placed in a sealed sample making machine for grinding 3-4 times and passing through a 325-mesh sieve, and then the respective sieve-under materials are taken as respective test samples, preferably ground 3 times.

[0025] In a preferred embodiment of the above method, in step S101, the ratio of the test sample of 30 specification high phosphorus titanium concentrate to the test sample of 10 specification titanium concentrate is 1:4-1:9. The preferred ratio is 1:4 or 1:9.

[0026] In a preferred embodiment of the above method, in step S102, timing is performed while heating for reaction, and when heating is stopped, the temperature is measured and the reaction time is recorded.

[0027] In a preferred embodiment of the above method, in step S102, the beaker is covered with a 40%-80% covering method. Preferably, the beaker is covered with a 40% covering method or an 80% covering method.

[0028] In a preferred embodiment of the above method, in step S102, the drying oven is a forced air drying oven, the aging reaction temperature is 170-180° C., preferably 170° C., and the aging reaction time is 2-4 hours, preferably 2 hours.

[0029] In a preferred embodiment of the above method, in step S103, the temperature is set to 60-70°C, preferably 65°C, and the stirring time is 1-2h, preferably 2h.

[0030] In a preferred embodiment of the above method, in step S103, iron powder is added to the beaker once, twice, three times or four times.

[0031] In a preferred embodiment of the above method, in step S103, Ti is controlled 3+ After passing the test, measure the temperature after adding iron powder.

[0032] In a preferred embodiment of the above method, in step S104, the natural sedimentation time is 10-60 min, preferably 10 min, 30 min or 60 min.

[0033] The above technical solution of the present invention is described and explained in detail below through specific embodiments.

[0034] A method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid provided in an embodiment of the present invention comprises the following steps: (1) Grinding of titanium concentrate: Take the titanium concentrate raw material warehouse containing 30 specifications of high-phosphorus titanium concentrate and 10 specifications of titanium concentrate (both are tested for trace elements), put them into the sealed sample making machine for grinding 3-4 times, and then pass them through a 325-mesh sieve. The titanium concentrates under the sieve are used as their respective test samples, and the test samples of 30 specifications of high-phosphorus titanium concentrate and 10 specifications of titanium concentrate are mixed evenly according to different proportions.

[0035] (2) Acid hydrolysis initiation and main reaction: Add concentrated sulfuric acid to the mixed titanium concentrate test sample in a beaker, stir evenly, add distilled water, and start heating. Cover the beaker in different ways. When volume expansion occurs, stop heating, measure the temperature and record the reaction time. Stop stirring when volume expansion stops, and then place the beaker in a forced air drying oven at 170-180°C for aging reaction for 2-4 hours. After the aging reaction is completed, cool the beaker to room temperature.

[0036] (3) Leaching and reduction: Add water to the cooled beaker, set the temperature to 60-70℃ and keep warm, set the stirring time to 1-2h and a certain speed, and then add iron powder at different times to control Ti 3+ If qualified, measure the temperature after adding iron powder, then add the prepared flocculant into the beaker and continue stirring.

[0037] (4) After the stirring is completed, the mixed titanium liquid in the beaker is allowed to settle naturally, vacuum filtered and the supernatant titanium liquid is extracted to measure its stability and sedimentation performance.

[0038] in: In the above embodiment, preferably, in step (1), the ratio of 30 specification high-phosphorus titanium concentrate to 10 specification titanium concentrate is 1:4-1:9, preferably 1:4 or 1:9; in step (2), the beaker is covered with a 40%-80% covering method, preferably a 40% covering method or an 80% covering method; in step (3), iron powder is added once, twice, three times or four times (the total amount of iron powder is constant); in step (4), the natural sedimentation time is 10-60 min, preferably 10 min, 30 min or 60 min.

[0039] Example 1 A method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid, comprising the following steps: (1) Take the titanium concentrate raw material warehouse containing 30 specifications of high-phosphorus titanium concentrate and 10 specifications of titanium concentrate (both for trace element testing), put them into the sealed sample making machine for grinding three times, and then pass them through a 325-mesh sieve to sieve out the respective titanium concentrates as their respective test samples, and mix the test samples of 30 specifications of high-phosphorus titanium concentrate and 10 specifications of titanium concentrate evenly in a ratio of 1:4.

[0040] (2) Add 160g of concentrated sulfuric acid (content ≥98%) to a certain amount of mixed titanium concentrate test sample in a beaker, stir evenly, add 26g of distilled water, start heating, cover the beaker with a 40% cover, and stop heating when volume expansion occurs. Measure the temperature and record the reaction time. Stop stirring when volume expansion stops, and then place the beaker in a forced air drying oven at an aging temperature of 170°C for 2h. After aging, take it out and cool it naturally to room temperature. (3) Add 300g of water to the cooled beaker, set the temperature to 65℃, stir for 2h, and add iron powder (the total amount of iron powder is constant) to the beaker twice. 3+ If qualified, measure the temperature after adding iron powder, then add the prepared flocculant into the beaker and continue stirring.

[0041] (4) After the stirring is completed, pour the mixed titanium liquid in the beaker into a 500 ml measuring cylinder, let it settle naturally for 30 minutes, vacuum filter and extract the supernatant titanium liquid, observe the height of the supernatant, and judge the stability and sedimentation performance of the titanium liquid from the acid hydrolysis of titanium concentrate.

[0042] In the above Example 1, after testing, the temperature after adding the iron powder was measured to be 74° C., the stability of the prepared titanium liquid was 360 ml, and the filtration time was 12 minutes and 10 seconds.

[0043] Example 2 A method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid, comprising the following steps: (1) Take the titanium concentrate raw material warehouse containing 30 specifications of high-phosphorus titanium concentrate and 10 specifications of titanium concentrate (both for trace element testing), put them into the sealed sample making machine for grinding three times, and then pass them through a 325-mesh sieve to sieve out the respective titanium concentrates as their respective test samples, and mix the test samples of 30 specifications of high-phosphorus titanium concentrate and 10 specifications of titanium concentrate evenly in a ratio of 1:9.

[0044] (2) Add 160g of concentrated sulfuric acid (content ≥98%) to a certain amount of mixed titanium concentrate test sample in a beaker, stir evenly, add 26g of distilled water, start heating, cover the beaker with a 40% cover, and stop heating when volume expansion occurs. Measure the temperature and record the reaction time. Stop stirring when volume expansion stops, and then place the beaker in a forced air drying oven at an aging temperature of 170°C for 2h. After aging, take it out and cool it naturally to room temperature. (3) Add 300g of water to the cooled beaker, set the temperature to 65℃, stir for 2h, and add iron powder (the total amount of iron powder is constant) to the beaker twice. 3+ If qualified, measure the temperature after adding iron powder, then add the prepared flocculant into the beaker and continue stirring.

[0045] (4) After the stirring is completed, pour the mixed titanium liquid in the beaker into a 500 ml measuring cylinder, let it settle naturally for 30 minutes, vacuum filter and extract the supernatant titanium liquid, observe the height of the supernatant, and judge the stability and sedimentation performance of the titanium liquid from the acid hydrolysis of titanium concentrate.

[0046] In the above Example 2, after testing, the temperature after adding the iron powder was measured to be 72° C., the stability of the prepared titanium liquid was 420 ml, and the filtration time was 5 minutes and 10 seconds.

[0047] Example 3 A method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid, comprising the following steps: (1) Take the titanium concentrate raw material warehouse containing 30 specifications of high-phosphorus titanium concentrate and 10 specifications of titanium concentrate (both for trace element testing), put them into the sealed sample making machine for grinding three times, and then pass them through a 325-mesh sieve to sieve out the respective titanium concentrates as their respective test samples, and mix the test samples of 30 specifications of high-phosphorus titanium concentrate and 10 specifications of titanium concentrate evenly in a ratio of 1:9.

[0048] (2) Add 160g of concentrated sulfuric acid (content ≥98%) to a certain amount of mixed titanium concentrate test sample in a beaker, stir evenly, add 26g of distilled water, start heating, cover the beaker with 80% coverage, and stop heating when volume expansion occurs. Measure the temperature and record the reaction time. Stop stirring when volume expansion stops, and then place the beaker in a forced air drying oven at an aging temperature of 170°C for 2h. After aging, take it out and cool it naturally to room temperature. (3) Add 300g of water to the cooled beaker, set the temperature to 65℃, stir for 2h, and add iron powder (the total amount of iron powder is constant) to the beaker twice. 3+ If qualified, measure the temperature after adding iron powder, then add the prepared flocculant into the beaker and continue stirring.

[0049] (4) After the stirring is completed, pour the mixed titanium liquid in the beaker into a 500 ml measuring cylinder, let it settle naturally for 30 minutes, vacuum filter and extract the supernatant titanium liquid, observe the height of the supernatant, and judge the stability and sedimentation performance of the titanium liquid from the acid hydrolysis of titanium concentrate.

[0050] In the above Example 3, after testing, the temperature after adding the iron powder was measured to be 72° C., the stability of the prepared titanium liquid was 390 ml, and the filtration time was 6 minutes and 56 seconds.

[0051] Example 4 A method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid, comprising the following steps: (1) Take the titanium concentrate raw material warehouse containing 30 specifications of high-phosphorus titanium concentrate and 10 specifications of titanium concentrate (both for trace element testing), put them into the sealed sample making machine for grinding three times, and then pass them through a 325-mesh sieve to sieve out the respective titanium concentrates as their respective test samples, and mix the test samples of 30 specifications of high-phosphorus titanium concentrate and 10 specifications of titanium concentrate evenly in a ratio of 1:9.

[0052] (2) Add 160g of concentrated sulfuric acid (content ≥98%) to a certain amount of mixed titanium concentrate test sample in a beaker, stir evenly, add 26g of distilled water, start heating, cover the beaker with a 40% cover, and stop heating when volume expansion occurs. Measure the temperature and record the reaction time. Stop stirring when volume expansion stops, and then place the beaker in a forced air drying oven at an aging temperature of 170°C for 2h. After aging, take it out and cool it naturally to room temperature. (3) Add 300g of water to the cooled beaker, set the temperature to 65℃, stir for 1h, and then add iron powder (the total amount of iron powder is constant) to the beaker twice. 3+ If qualified, measure the temperature after adding iron powder, then add the prepared flocculant into the beaker and continue stirring.

[0053] (4) After the stirring is completed, pour the mixed titanium liquid in the beaker into a 500 ml measuring cylinder, let it settle naturally for 30 minutes, vacuum filter and extract the supernatant titanium liquid, observe the height of the supernatant, and judge the stability and sedimentation performance of the titanium liquid from the acid hydrolysis of titanium concentrate.

[0054] In the above-mentioned Example 4, after testing, the temperature after adding the iron powder was measured to be 69° C., the stability of the prepared titanium liquid was 430 ml, and the filtration time was 5 minutes and 25 seconds.

[0055] Example 5 A method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid, comprising the following steps: (1) Take the titanium concentrate raw material warehouse containing 30 specifications of high-phosphorus titanium concentrate and 10 specifications of titanium concentrate (both for trace element testing), put them into the sealed sample making machine for grinding three times, and then pass them through a 325-mesh sieve to sieve out the respective titanium concentrates as their respective test samples, and mix the test samples of 30 specifications of high-phosphorus titanium concentrate and 10 specifications of titanium concentrate evenly in a ratio of 1:9.

[0056] (2) Add 160g of concentrated sulfuric acid (content ≥98%) to a certain amount of mixed titanium concentrate test sample in a beaker, stir evenly, add 26g of distilled water, start heating, cover the beaker with a 40% cover, and stop heating when volume expansion occurs. Measure the temperature and record the reaction time. Stop stirring when volume expansion stops, and then place the beaker in a forced air drying oven at an aging temperature of 170°C for 2h. After aging, take it out and cool it naturally to room temperature. (3) Add 300g of water to the cooled beaker, set the temperature to 65℃, stir for 2h, and add iron powder (a certain amount of iron powder) to the beaker at once. 3+ If qualified, measure the temperature after adding iron powder, then add the prepared flocculant into the beaker and continue stirring.

[0057] (4) After the stirring is completed, pour the mixed titanium liquid in the beaker into a 500 ml measuring cylinder, let it settle naturally for 30 minutes, vacuum filter and extract the supernatant titanium liquid, observe the height of the supernatant, and judge the stability and sedimentation performance of the titanium liquid from the acid hydrolysis of titanium concentrate.

[0058] In the above Example 5, after testing, the temperature after adding the iron powder was measured to be 80° C., the stability of the prepared titanium liquid was 380 ml, and the filtration time was 7 minutes and 25 seconds.

[0059] Example 6 A method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid, comprising the following steps: (1) Take the titanium concentrate raw material warehouse containing 30 specifications of high-phosphorus titanium concentrate and 10 specifications of titanium concentrate (both for trace element testing), put them into the sealed sample making machine for grinding three times, and then pass them through a 325-mesh sieve to sieve out the respective titanium concentrates as their respective test samples, and mix the test samples of 30 specifications of high-phosphorus titanium concentrate and 10 specifications of titanium concentrate evenly in a ratio of 1:9.

[0060] (2) Add 160g of concentrated sulfuric acid (content ≥98%) to a certain amount of mixed titanium concentrate test sample in a beaker, stir evenly, add 26g of distilled water, start heating, cover the beaker with a 40% cover, and stop heating when volume expansion occurs. Measure the temperature and record the reaction time. Stop stirring when volume expansion stops, and then place the beaker in a forced air drying oven at an aging temperature of 170°C for 2h. After aging, take it out and cool it naturally to room temperature. (3) Add 300g of water to the cooled beaker, set the temperature to 65℃, stir for 2h, and then add iron powder (the total amount of iron powder is constant) to the beaker four times. 3+ If qualified, measure the temperature after adding iron powder, then add the prepared flocculant into the beaker and continue stirring.

[0061] (4) After the stirring is completed, pour the mixed titanium liquid in the beaker into a 500 ml measuring cylinder, let it settle naturally for 30 minutes, vacuum filter and extract the supernatant titanium liquid, observe the height of the supernatant, and judge the stability and sedimentation performance of the titanium liquid from the acid hydrolysis of titanium concentrate.

[0062] In the above Example 6, after testing, the temperature after adding the iron powder was measured to be 70° C., the stability of the prepared titanium liquid was 420 ml, and the filtration time was 5 minutes.

[0063] Example 7 A method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid, comprising the following steps: (1) Take the titanium concentrate raw material warehouse containing 30 specifications of high-phosphorus titanium concentrate and 10 specifications of titanium concentrate (both for trace element testing), put them into the sealed sample making machine for grinding three times, and then pass them through a 325-mesh sieve to sieve out the respective titanium concentrates as their respective test samples, and mix the test samples of 30 specifications of high-phosphorus titanium concentrate and 10 specifications of titanium concentrate evenly in a ratio of 1:9.

[0064] (2) Add 160g of concentrated sulfuric acid (content ≥98%) to a certain amount of mixed titanium concentrate test sample in a beaker, stir evenly, add 26g of distilled water, start heating, cover the beaker with a 40% cover, and stop heating when volume expansion occurs. Measure the temperature and record the reaction time. Stop stirring when volume expansion stops, and then place the beaker in a forced air drying oven at an aging temperature of 170°C for 2h. After aging, take it out and cool it naturally to room temperature. (3) Add 300g of water to the cooled beaker, set the temperature to 65℃, stir for 2h, and then add iron powder (the total amount of iron powder is constant) to the beaker four times. 3+ If qualified, measure the temperature after adding iron powder, then add the prepared flocculant into the beaker and continue stirring.

[0065] (4) After the stirring is completed, pour the mixed titanium liquid in the beaker into a 500 ml measuring cylinder, let it settle naturally for 10 minutes, vacuum filter and extract the supernatant titanium liquid, observe the height of the supernatant, and judge the stability and sedimentation performance of the titanium liquid from the acid hydrolysis of titanium concentrate.

[0066] In the above Example 7, after testing, the temperature after adding the iron powder was measured to be 71° C., the stability of the prepared titanium liquid was 410 ml, and the filtration time was 8 minutes and 30 seconds.

[0067] Example 8 A method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid, comprising the following steps: (1) Take the titanium concentrate raw material warehouse containing 30 specifications of high-phosphorus titanium concentrate and 10 specifications of titanium concentrate (both for trace element testing), put them into the sealed sample making machine for grinding three times, and then pass them through a 325-mesh sieve to sieve out the respective titanium concentrates as their respective test samples, and mix the test samples of 30 specifications of high-phosphorus titanium concentrate and 10 specifications of titanium concentrate evenly in a ratio of 1:9.

[0068] (2) Add 160g of concentrated sulfuric acid (content ≥98%) to a certain amount of mixed titanium concentrate test sample in a beaker, stir evenly, add 26g of distilled water, start heating, cover the beaker with a 40% cover, and stop heating when volume expansion occurs. Measure the temperature and record the reaction time. Stop stirring when volume expansion stops, and then place the beaker in a forced air drying oven at an aging temperature of 170°C for 2h. After aging, take it out and cool it naturally to room temperature. (3) Add 300g of water to the cooled beaker, set the temperature to 65℃, stir for 2h, and add iron powder (the total amount of iron powder is constant) to the beaker twice. 3+ If qualified, measure the temperature after adding iron powder, then add the prepared flocculant into the beaker and continue stirring.

[0069] (4) After the stirring is completed, pour the mixed titanium liquid in the beaker into a 500 ml measuring cylinder, let it settle naturally for 60 minutes, vacuum filter and extract the supernatant titanium liquid, observe the height of the supernatant, and judge the stability and sedimentation performance of the titanium liquid from the acid hydrolysis of titanium concentrate.

[0070] In the above-mentioned Example 8, after testing, the temperature after adding the iron powder was measured to be 71° C., the stability of the prepared titanium liquid was 420 ml, and the filtration time was 5 minutes and 10 seconds.

[0071] Example 9 A method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid, comprising the following steps: (1) Take the titanium concentrate raw material warehouse containing 30 specifications of high-phosphorus titanium concentrate and 10 specifications of titanium concentrate (both for trace element testing), put them into the sealed sample making machine for grinding 4 times, and then pass them through a 325-mesh sieve. The titanium concentrates of each specification are sieved as their respective test samples, and the test samples of the 30 specifications of high-phosphorus titanium concentrate and the test samples of the 10 specifications of titanium concentrate are evenly mixed in a ratio of 1:6.

[0072] (2) Add 160g of concentrated sulfuric acid (content ≥98%) to a certain amount of mixed titanium concentrate test sample in a beaker, stir evenly, add 26g of distilled water, start heating, cover the beaker with a 60% cover, and stop heating when volume expansion occurs. Measure the temperature and record the reaction time. Stop stirring when volume expansion stops, and then place the beaker in a forced air drying oven at an aging temperature of 180°C for 3h. After aging, take it out and cool it naturally to room temperature. (3) Add 300g of water to the cooled beaker, set the temperature to 60℃, stir for 1.5h, and then add iron powder (the total amount of iron powder is constant) to the beaker twice. 3+ If qualified, measure the temperature after adding iron powder, then add the prepared flocculant into the beaker and continue stirring.

[0073] (4) After the stirring is completed, pour the mixed titanium liquid in the beaker into a 500 ml measuring cylinder, let it settle naturally for 30 minutes, vacuum filter and extract the supernatant titanium liquid, observe the height of the supernatant, and judge the stability and sedimentation performance of the titanium liquid from the acid hydrolysis of titanium concentrate.

[0074] In the above Example 9, after testing, the temperature after adding the iron powder was measured to be 73° C., the stability of the prepared titanium liquid was 375 ml, and the filtration time was 8 minutes and 12 seconds.

[0075] Example 10 A method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid, comprising the following steps: (1) Take the titanium concentrate raw material warehouse containing 30 specifications of high-phosphorus titanium concentrate and 10 specifications of titanium concentrate (both for trace element testing), put them into the sealed sample making machine for grinding 4 times, and then pass them through a 325-mesh sieve to sieve out the respective titanium concentrates as their respective test samples, and mix the test samples of 30 specifications of high-phosphorus titanium concentrate and 10 specifications of titanium concentrate evenly in a ratio of 1:8.

[0076] (2) Add 160g of concentrated sulfuric acid (content ≥98%) to a certain amount of mixed titanium concentrate test sample in a beaker, stir evenly, add 26g of distilled water, start heating, cover the beaker with a 50% cover, and stop heating when volume expansion occurs. Measure the temperature and record the reaction time. Stop stirring when volume expansion stops, and then place the beaker in a forced air drying oven at an aging temperature of 175°C for 4h. After aging, take it out and cool it naturally to room temperature. (3) Add 300g of water to the cooled beaker, set the temperature to 70℃, stir for 2h, and then add iron powder (the total amount of iron powder is constant) to the beaker three times. 3+ If qualified, measure the temperature after adding iron powder, then add the prepared flocculant into the beaker and continue stirring.

[0077] (4) After the stirring is completed, pour the mixed titanium liquid in the beaker into a 500 ml measuring cylinder, let it settle naturally for 45 minutes, vacuum filter and extract the supernatant titanium liquid, observe the height of the supernatant, and judge the stability and sedimentation performance of the titanium liquid from the acid hydrolysis of titanium concentrate.

[0078] In the above Example 10, after testing, the temperature after adding the iron powder was measured to be 74° C., the stability of the prepared titanium liquid was 370 ml, and the filtration time was 10 minutes and 35 seconds.

[0079] Comparative Example A method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid, comprising the following steps: (1) Take pure 10-specification titanium concentrate (for trace element testing), put it into a sealed sample preparation machine and grind it three times. After grinding, pass it through a 325-mesh sieve and the 10-specification titanium concentrate that falls under the sieve is used as the respective test sample.

[0080] (2) Add 160g of concentrated sulfuric acid (content ≥98%) to a certain amount of 10-specification titanium concentrate test sample in a beaker, stir evenly, add 26g of distilled water, and start heating. Cover the beaker with a 40% cover. When volume expansion occurs, stop heating, measure the temperature and record the reaction time. Stop stirring when volume expansion stops, and then place the beaker in a forced air drying oven at an aging temperature of 170°C for 2h. After aging, take it out and cool it naturally to room temperature. (3) Add 300g of water to the cooled beaker, set the temperature to 65℃, stir for 2h, and add iron powder (the total amount of iron powder is constant) to the beaker twice. 3+ If qualified, measure the temperature after adding iron powder, then add the prepared flocculant into the beaker and continue stirring.

[0081] (4) After the stirring is completed, pour the mixed titanium liquid in the beaker into a 500 ml measuring cylinder, let it settle naturally for 30 minutes, vacuum filter and extract the supernatant titanium liquid, observe the height of the supernatant, and judge the stability and sedimentation performance of the titanium liquid from the acid hydrolysis of titanium concentrate.

[0082] In the above comparative example, after testing, the temperature after adding iron powder was measured to be 71° C., the stability of the prepared titanium liquid was 440 ml, and the filtration time was 2 minutes and 10 seconds.

[0083] It can be seen that in the method of reducing the influence of high-phosphorus titanium concentrate on the stability of titanium dioxide of the present invention, when the proportion of 30-specification high-phosphorus titanium concentrate and 10-specification titanium concentrate is appropriate, the sedimentation performance and stability of the titanium liquid are slightly reduced compared with the pure 10-specification titanium concentrate. However, the introduction of 30-specification high-phosphorus titanium concentrate is inexpensive, and this suitable ore raw material ratio is worth further exploration in production. In the above embodiment of the present invention, during the acidolysis reaction, the phosphorus-containing gas generated can be extracted in time, which is beneficial to the sedimentation performance and stability of the titanium liquid; the leaching time is related to the yield of the titanium liquid process. Too long time affects production, and too short time affects the yield. The time is reasonably adjusted according to production needs; iron powder is added in batches, and Ti is adjusted in time. 3+ , avoid premature hydrolysis caused by high temperature in summer during the reduction process, which will lead to poor sedimentation effect; the sedimentation time has a significant impact on the sedimentation effect, and the sedimentation time should not be ignored for the sake of production progress.

[0084] In summary, the method of the present invention realizes the control of the process of using phosphorus titanium concentrate and ensures the stability index required by the hydrolysis process. Compared with the titanium liquid prepared from pure 10-specification titanium concentrate, the stability and sedimentation performance of the titanium liquid prepared by the method of the present invention are slightly lower, but the use of 30-specification high-phosphorus titanium concentrate and 10-specification titanium concentrate for mixing is conducive to saving the cost of titanium concentrate raw materials.

[0085] It should be noted that, in this article, relational terms such as "first" and "second" are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusions, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to the process, method, article or device. In the absence of further restrictions, the elements defined by the sentence "including a..." do not exclude the presence of other identical elements in the process, method, article or device including the elements.

[0086] The technical features of the above embodiments may be combined arbitrarily. To make the description concise, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0087] The above-mentioned embodiments only express several implementation methods of the present invention, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the invention patent. It should be pointed out that, for ordinary technicians in this field, several variations and improvements can be made without departing from the concept of the present invention, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be subject to the attached claims.

Claims

1. A method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid, characterized in that: The following steps are involved: 1) Grind and sieve the 30-specification high-phosphorus titanium concentrate and the 10-specification titanium concentrate respectively, take the sieve-downs of each as their respective test samples, and mix the test sample of the 30-specification high-phosphorus titanium concentrate with the test sample of the 10-specification titanium concentrate in proportion to obtain a mixed titanium concentrate test sample; 2) Place the mixed titanium concentrate test sample in a beaker, add concentrated sulfuric acid to the beaker, stir evenly, add water and heat to react, and cover the beaker. When volume expansion occurs, stop heating, and stop stirring when the volume expansion stops. Then place the beaker in a drying oven for aging reaction. After the aging reaction is completed, cool the beaker to room temperature; 3) Add water to the cooled beaker and set the temperature for stirring and leaching. After the leaching is completed, add iron powder to the beaker to control the Ti 3+ If qualified, then add flocculant to the beaker and continue stirring; 4) After the stirring is completed, the mixed titanium liquid in the beaker is allowed to settle naturally, vacuum filtered and the supernatant titanium liquid is extracted to measure its stability and sedimentation performance.

2. The method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid according to claim 1, characterized in that: In step 1), before the 30-specification high-phosphorus titanium concentrate and the 10-specification titanium concentrate are ground and sieved respectively, the 30-specification high-phosphorus titanium concentrate and the 10-specification titanium concentrate are tested for trace elements respectively, and then the 30-specification high-phosphorus titanium concentrate and the 10-specification titanium concentrate are respectively placed in a sealed sample preparation machine for grinding 3-4 times and passed through a 325-mesh sieve, and the respective sieve-under materials are taken as respective test samples.

3. The method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid according to claim 1, characterized in that: In step 1), the ratio of the test sample of 30 specification high phosphorus titanium concentrate to the test sample of 10 specification titanium concentrate is 1:4-1:

9.

4. The method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid according to claim 1, characterized in that: In step 2), the timing is performed while the reaction is heated, and when the heating is stopped, the temperature is measured and the reaction time is recorded.

5. The method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid according to claim 1, characterized in that: In step 2), the beaker is covered with 40%-80% coverage above the beaker.

6. The method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid according to claim 1, characterized in that: In step 2), the drying oven is a forced air drying oven, the aging reaction temperature is 170-180° C., and the aging reaction time is 2-4 h.

7. The method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid according to claim 1, characterized in that: In step 3), the temperature is set to 60-70°C and the stirring time is 1-2h.

8. The method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid according to claim 1, characterized in that: In step 3), iron powder is added to the beaker once, twice, three times or four times.

9. The method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid according to claim 1, characterized in that: In step 3), control Ti 3+ After passing the test, measure the temperature after adding iron powder.

10. The method for reducing the influence of high-phosphorus titanium concentrate on the stability of titanium liquid according to claim 1, characterized in that: In step 4), the natural sedimentation time is 10-60 minutes.

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