CN112110482B - Method for recovering nano strontium titanate and high-purity tungsten slag from waste SCR denitration catalyst - Google Patents
Method for recovering nano strontium titanate and high-purity tungsten slag from waste SCR denitration catalyst Download PDFInfo
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Abstract
The invention belongs to the field of non-ferrous metal recovery, and particularly relates to a method for recovering nano strontium titanate and high-purity tungsten slag from a waste SCR denitration catalyst. The recovery method mainly comprises the steps of waste catalyst pretreatment, acid dissolution, titanium precipitation and the like, high-value nano strontium titanate and high-purity tungsten slag products can be recovered and obtained through the recovery process, the process steps are simple, the value of the recovered products is high, and reasonable and efficient treatment of the waste SCR denitration catalyst can be realized.
Description
Technical Field
The invention belongs to the field of non-ferrous metal recovery, and particularly relates to a method for recovering nano strontium titanate and high-purity tungsten slag from a waste SCR denitration catalyst.
Background
Due to successful application experience in the field of denitration in the thermal power industry, with increasingly strict environmental requirements of various industries, the application range of the SCR denitration catalyst is more and more extensive, and the SCR denitration catalyst becomes the first choice for denitration in multiple industries such as thermal power, steel, cement and the like. The SCR denitration catalyst has a certain service life, generally becomes a waste catalyst after 3-5 years, the corresponding waste SCR denitration catalyst also synchronously increases along with the continuous increase of the using amount, and statistically, more than 82 ten thousand tons of waste SCR denitration catalysts need to be treated in 2025 nationwide.
The waste SCR denitration catalyst is a special solid waste, has the characteristics of great harm, difficult treatment, high yield and the like, and simultaneously contains a large amount of precious metal resources, wherein TiO is2、WO3、MoO3And V2O5Are very expensive high value-added components. Therefore, the recovery of components such as titanium, tungsten and vanadium from the waste SCR denitration catalyst not only can realize the recycling of resources, but also can treat a large amount of accumulated waste catalyst, and has very important significance in the aspects of resource saving, environmental protection and the like. TiO 22And WO3Is the most used carrier and active auxiliary agent in the SCR denitration catalyst, has higher content, and is TiO in the waste SCR denitration catalyst2The content can reach more than 70 percent, WO3The content can also reach about 5 percent, so the titanium and the tungsten are always high value-added elementsThe focus of the collection.
In China, more researches are made on recovery processes of titanium and tungsten elements in waste SCR denitration catalysts. Chinese patent application CN201310063440.7 discloses a method for recovering tungsten component from selective catalytic reduction denitration catalyst, which comprises mixing and roasting waste catalyst and sodium carbonate, soaking in water to separate tungsten element from waste catalyst, obtaining tungsten solution, and finally recovering tungsten product with purity of 42-53% by extraction and back extraction processes. Chinese patent application CN201510943530.4 discloses a method and a system for comprehensively recycling waste SCR denitration catalysts. The existing recovery method of titanium and tungsten also has obvious defects of low product purity, complex process and the like, and an efficient and reasonable recovery scheme is urgently needed to be developed.
Disclosure of Invention
The total content of titanium dioxide and tungsten trioxide in the waste SCR denitration catalyst can reach more than 75%, and the efficient recovery of titanium and tungsten elements in the forms of nano strontium titanate and high-purity tungsten slag is an ideal way for realizing reasonable treatment of the waste SCR denitration catalyst.
The invention aims to provide a method for recovering nano strontium titanate and high-purity tungsten slag from a waste SCR denitration catalyst. According to the invention, high-quality nanometer strontium titanate and high-purity tungsten slag are obtained by recovering through a specific recovery process according to the existence form and chemical characteristics of titanium and tungsten elements in the waste SCR denitration catalyst.
According to the present invention there is provided a method comprising the steps of:
(1) pretreatment of
Treating the waste SCR denitration catalyst through roasting, soot blowing and crushing steps in sequence to obtain waste catalyst powder with the particle size of less than 300 meshes;
(2) acid soluble
Dissolving titanium element in the waste catalyst by using a sulfuric acid solution, and then filtering to obtain a titanium solution and a tungsten slag precipitate;
(3) recovery of strontium titanate
Adding a mixed solution of strontium nitrate and oxalic acid into the titanium liquid obtained in the step (2), fully reacting, filtering to obtain strontium titanyl oxalate precipitate, and sequentially washing, drying and roasting to recover to obtain nano strontium titanate;
(4) recovery of high purity tungsten slag
And (3) cleaning the tungsten slag obtained in the step (2) by using a dilute hydrochloric acid solution with the volume concentration of 5%, and finally, washing, drying and recycling to obtain the high-purity tungsten slag.
Preferably, in the step (1), the waste SCR denitration catalyst is eliminated V for industrial flue gas denitration2O5-WO3/TiO2The catalyst comprises TiO2、WO3、V2O5、Al2O3、SiO2、CaO。
Preferably, in the step (1), the roasting temperature is 550-750 ℃ and the roasting time is 3-6 h.
Preferably, in the step (2), the volume concentration of the sulfuric acid solution is 70-90%, and the liquid-solid mass ratio of the sulfuric acid solution to the waste catalyst powder is (5-10): 1.
Preferably, in the step (2), the reaction temperature is 80-120 ℃ and the reaction time is 1.5-4 h.
Preferably, in the step (3), in the mixed solution of strontium nitrate and oxalic acid, the concentration of strontium nitrate is 0.75-1.5mol/L, and the concentration of oxalic acid is 1.5-3 mol/L.
Preferably, in the step (3), the molar ratio of strontium nitrate to titanium element is (1-1.5): 1, and the molar ratio of oxalic acid to titanium element is (2-3): 1.
Preferably, in the step (3), the reaction temperature is 60-85 ℃ and the reaction time is 25-45 min.
Preferably, in the step (3), the calcination temperature is 650 ℃ and the calcination time is 3-6 h.
The invention has the beneficial effects that:
the invention efficiently recovers titanium and tungsten elements in the waste SCR denitration catalyst, and obtains high-quality nanometer strontium titanate and high-purity tungsten slag. Wherein the purity of strontium titanate is more than 99%, the content of tungsten trioxide in tungsten slag can reach more than 97%, and the recovery rates of titanium and tungsten elements respectively reach more than 93% and 97%. The method is mainly realized by the following aspects:
(1) the titanium element recovery form has higher value. Titanium element in the waste SCR denitration catalyst is usually recovered in the form of titanium dioxide or coarse titanium slag, wherein the price of the titanium dioxide is about 1.5 ten thousand yuan/ton, and the price of the coarse titanium slag is often less than 5000 yuan/ton. Strontium titanate is a precious electronic functional ceramic material and has very wide application in the electronic, mechanical and ceramic industries; meanwhile, strontium titanate is also widely used in the field of catalysis due to its good photocatalytic activity, electromagnetic properties and redox catalytic activity; in addition, strontium titanate is an ideal substitute for diamond. The price of the high-purity nanometer strontium titanate prepared by controlling the titanium precipitation condition and the roasting process is more than 5 times of the price of titanium dioxide and more than 15 times of the price of coarse titanium slag.
(2) According to the invention, titanium element is recovered by means of dissolving and then precipitating, in the acid dissolving step, titanium dioxide component can almost completely enter the solution from the fine waste catalyst powder, and the final recovery rate of titanium element can be ensured to be more than 93%. The titanium liquid obtained after acid dissolution has strong acidity, and when the mixed solution of strontium nitrate and oxalic acid is added to precipitate the titanium element, other components can not be precipitated under the acidic condition, so that the purity of the recovered strontium titanate can reach more than 99%. And other common titanium element recovery processes mostly obtain insoluble sodium titanate by adding sodium hydroxide or sodium carbonate for mixed roasting, and further recover titanium dioxide on the basis, or directly recover titanium dioxide in the form of coarse titanium slag, wherein the recovered product usually contains a large amount of sodium titanate and has low product value. The method provided by the invention is simple to operate, and the recovery rate of the titanium element and the purity of the product are more ideal.
(3) The waste SCR denitration catalyst is complex in component and is usually interfered by impurity elements in the process of recovering tungsten elements, so that the final recovered product is low in purity. In the invention, after the waste catalyst is pretreated, the tungsten element is directly separated by acid dissolution, and because only the tungsten trioxide component in the waste SCR denitration catalyst is insoluble in sulfuric acid solution, almost all other elements except the tungsten element enter the solution after the acid dissolution step, so that more than 97 percent of finally recovered tungsten slag is tungsten trioxide. In addition, the tungsten slag obtained after acid dissolution is extremely simple to treat, and a large amount of loss of tungsten element due to a complicated recovery process is avoided, so that the total recovery rate of the tungsten element can reach more than 97%.
(4) The method has very simple process steps, only comprises four processes of pretreatment, acid dissolution, titanium recovery and tungsten slag treatment, and is a simple and conventional physical and chemical operation flow, thereby greatly reducing the difficulty of process implementation and the cost investment in the implementation process, and being very suitable for industrial application.
Detailed Description
The invention provides a method for recovering nano strontium titanate and high-purity tungsten slag from a waste SCR denitration catalyst, which is further explained by combining a specific embodiment mode.
Example 1
Embodiment 1 describes a method for recovering nano strontium titanate and high-purity tungsten slag from a waste SCR denitration catalyst, which specifically comprises the following steps:
(1) pretreatment of
Roasting the waste SCR denitration catalyst for 6 hours at 550 ℃, and then blowing and crushing the waste catalyst to obtain waste catalyst powder below 300 meshes.
(2) Acid soluble
Preparing a sulfuric acid solution with the volume concentration of 90%, adding waste catalyst powder according to the liquid-solid mass ratio of 5:1, heating the solution to 80 ℃, stirring for 1.5h, cooling the solution after the reaction is finished, and filtering to obtain titanium liquid and tungsten slag.
(3) Recovery of strontium titanate
Preparing a mixed solution of strontium nitrate and oxalic acid, wherein the concentration of the strontium nitrate is 0.75mol/L, the concentration of the oxalic acid is 1.5mol/L, adding the mixed solution into the titanium solution obtained in the step (2), ensuring the molar ratio of Sr/Ti =1.5 and the oxalic acid/Ti =3, heating the solution to 60 ℃, stirring for 25min, and standing for 6h at room temperature after the reaction is finished. Then filtering to obtain strontium titanyl oxalate precipitate, washing with water, drying, and roasting at 450 deg.C for 6h to obtain nanometer strontium titanate.
(4) Recovery of high purity tungsten slag
And (3) cleaning the tungsten slag precipitate obtained in the step (2) by using a dilute hydrochloric acid solution with the volume concentration of 5%, and then washing and drying the tungsten slag precipitate to obtain the high-purity tungsten slag.
By the embodiment 1, the recovery rate of the titanium element is 93.35 percent, and the recovery rate of the tungsten element is 97.18 percent; the purity of the recovered nano strontium titanate is 99.06%, and the content of tungsten trioxide in the recovered tungsten slag is 97.89%.
Example 2
Embodiment 2 describes a method for recovering nano strontium titanate and high-purity tungsten slag from a waste SCR denitration catalyst, which specifically comprises the following steps:
(1) pretreatment of
Roasting the waste SCR denitration catalyst for 3 hours at 750 ℃, and then blowing and crushing the waste catalyst to obtain waste catalyst powder below 300 meshes.
(2) Acid soluble
Preparing a sulfuric acid solution with the volume concentration of 70%, adding waste catalyst powder according to the liquid-solid mass ratio of 10:1, heating the solution to 120 ℃, stirring for 4 hours, cooling the solution after the reaction is finished, and filtering to obtain titanium liquid and tungsten slag.
(3) Recovery of strontium titanate
Preparing a mixed solution of strontium nitrate and oxalic acid, wherein the concentration of the strontium nitrate is 1.5mol/L, the concentration of the oxalic acid is 3mol/L, adding the mixed solution into the titanium solution obtained in the step (2), ensuring that the molar ratio of Sr/Ti =1 and the oxalic acid/Ti =2, heating the solution to 85 ℃, stirring for 45min, and standing for 12h in a room temperature environment after the reaction is finished. Then filtering to obtain strontium titanyl oxalate precipitate, washing with water, drying, and roasting at 650 ℃ for 3h to obtain the nano strontium titanate.
(4) Recovery of high purity tungsten slag
And (3) cleaning the tungsten slag precipitate obtained in the step (2) by using a dilute hydrochloric acid solution with the volume concentration of 5%, and then washing and drying the tungsten slag precipitate to obtain the high-purity tungsten slag.
Through example 2, the recovery rate of titanium element is 93.67%, and the recovery rate of tungsten element is 98.09%; the purity of the recovered nano strontium titanate is 99.12%, and the content of tungsten trioxide in the recovered tungsten slag is 97.67%.
Example 3
Example 3 describes another method for recovering nano strontium titanate and high-purity tungsten slag from waste SCR denitration catalyst, which comprises the following specific steps:
(1) pretreatment of
Roasting the waste SCR denitration catalyst for 6 hours at 650 ℃, and then performing soot blowing and crushing treatment on the waste catalyst to obtain waste catalyst powder with the particle size of less than 300 meshes.
(2) Acid soluble
Preparing a sulfuric acid solution with the volume concentration of 80%, adding waste catalyst powder according to the liquid-solid mass ratio of 7:1, heating the solution to 90 ℃, stirring for 3 hours, cooling the solution after the reaction is finished, and filtering to obtain a titanium liquid and tungsten slag.
(3) Recovery of strontium titanate
Preparing a mixed solution of strontium nitrate and oxalic acid, wherein the concentration of the strontium nitrate is 1mol/L, the concentration of the oxalic acid is 2mol/L, adding the mixed solution into the titanium solution obtained in the step (2), ensuring the molar ratio of Sr/Ti =1.25 and the oxalic acid/Ti =2.5, heating the solution to 70 ℃, stirring for 30min, and standing for 8h in a room-temperature environment after the reaction is finished. Then filtering to obtain strontium titanyl oxalate precipitate, washing with water, drying, and roasting at 550 ℃ for 5h to obtain the nano strontium titanate.
(4) Recovery of high purity tungsten slag
And (3) cleaning the tungsten slag precipitate obtained in the step (2) by using a dilute hydrochloric acid solution with the volume concentration of 5%, and then washing and drying the tungsten slag precipitate to obtain the high-purity tungsten slag.
By the example 3, the recovery rate of the titanium element is 93.99 percent, and the recovery rate of the tungsten element is 98.11 percent; the purity of the recovered nano strontium titanate is 99.23%, and the content of tungsten trioxide in the recovered tungsten slag is 98.17%.
Example 4
Embodiment 4 describes another method for recovering nano strontium titanate and high-purity tungsten slag from a waste SCR denitration catalyst, which specifically comprises the following steps:
(1) pretreatment of
And roasting the waste SCR denitration catalyst for 3.5 hours at 700 ℃, and then performing soot blowing and crushing treatment on the waste catalyst to obtain waste catalyst powder with the particle size of below 300 meshes.
(2) Acid soluble
Preparing a sulfuric acid solution with the volume concentration of 88%, adding waste catalyst powder according to the liquid-solid mass ratio of 8:1, heating the solution to 115 ℃, stirring for 2 hours, cooling the solution after the reaction is finished, and filtering to obtain titanium liquid and tungsten slag.
(3) Recovery of strontium titanate
Preparing a mixed solution of strontium nitrate and oxalic acid, wherein the concentration of the strontium nitrate is 1.25mol/L, the concentration of the oxalic acid is 2.5mol/L, adding the mixed solution into the titanium solution obtained in the step (2), ensuring the molar ratio of Sr/Ti =1.3 and the oxalic acid/Ti =2.6, heating the solution to 65 ℃, stirring for 35min, and standing for 10h at room temperature after the reaction is finished. Then filtering to obtain strontium titanyl oxalate precipitate, washing with water, drying, and roasting at 600 ℃ for 3.5h to obtain the nano strontium titanate.
(4) Recovery of high purity tungsten slag
And (3) cleaning the tungsten slag precipitate obtained in the step (2) by using a dilute hydrochloric acid solution with the volume concentration of 5%, and then washing and drying the tungsten slag precipitate to obtain the high-purity tungsten slag.
By the embodiment 4, the recovery rate of the titanium element is 93.67 percent, and the recovery rate of the tungsten element is 97.79 percent; the purity of the recovered nano strontium titanate is 99.34%, and the content of tungsten trioxide in the recovered tungsten slag is 98.29%.
It should be understood that the above-mentioned embodiments are only for illustrating the technical idea and features of the present invention, and are intended for those skilled in the art to understand the content of the present invention and to implement the present invention, and are not exhaustive of the specific embodiments, and the protection scope of the present invention is not limited thereby. Modifications and equivalents may be made thereto without departing from the spirit and scope of the present invention, which is set forth in the following claims.
Claims (6)
1. A method for recovering nanometer strontium titanate and high-purity tungsten slag from a waste SCR denitration catalyst comprises the following steps:
(1) preparation of waste catalyst powder by pretreatment
Roasting the waste catalyst, blowing off dust on the surface of the catalyst by using compressed air after the catalyst is cooled, and then crushing the waste catalyst to be less than 300 meshes;
(2) acid soluble
Adding the waste catalyst powder into a sulfuric acid solution with the volume concentration of 70-90%, heating to 80-120 ℃, stirring for 1.5-4h, and filtering to obtain a titanium liquid and a tungsten slag precipitate after the solution is cooled;
(3) recovery of strontium titanate
Adding a mixed solution of strontium nitrate and oxalic acid into the solution obtained in the step (2), heating the solution to 60-85 ℃, stirring for 25-45min, placing the solution in a room temperature environment for 6-12h after the reaction is finished, and then filtering to obtain strontium titanyl oxalate precipitate; finally, washing, drying and roasting in sequence to recover and obtain the nanometer strontium titanate, wherein in the mixed solution of the strontium nitrate and the oxalic acid, the concentration of the strontium nitrate is 0.75-1.5mol/L, and the concentration of the oxalic acid is 1.5-3 mol/L;
(4) recovery of high purity tungsten slag
And (3) cleaning the tungsten slag obtained in the step (2) by using a dilute hydrochloric acid solution with the volume concentration of 5%, and then sequentially washing, drying and recycling to obtain the high-purity tungsten slag.
2. The method for recovering nano strontium titanate and high-purity tungsten residues from waste SCR denitration catalyst according to claim 1, wherein the waste SCR denitration catalyst in the step (1) is eliminated V for industrial flue gas denitration2O5-WO3/TiO2The catalyst comprises TiO2、WO3、V2O5、Al2O3、SiO2、CaO。
3. The method for recovering the nano strontium titanate and the high-purity tungsten slag from the waste SCR denitration catalyst as recited in claim 1, wherein the calcination temperature in the step (1) is 550-750 ℃, and the calcination time is 3-6 h.
4. The method for recovering the nano strontium titanate and the high-purity tungsten slag from the waste SCR denitration catalyst according to claim 1, wherein the liquid-solid mass ratio of the sulfuric acid solution to the waste catalyst powder in the step (2) is (5-10): 1.
5. The method for recovering the nano strontium titanate and the high-purity tungsten slag from the waste SCR denitration catalyst according to claim 1, wherein in the step (3), the molar ratio of strontium nitrate to titanium elements is (1-1.5): 1, and the molar ratio of oxalic acid to titanium elements is (2-3): 1.
6. The method for recovering the nano strontium titanate and the high-purity tungsten slag from the waste SCR denitration catalyst as recited in claim 1, wherein the calcination temperature in the step (3) is 650 ℃ and the calcination time is 3-6 h.
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