CN112110499A - Method for recovering nano nickel titanate and high-purity tungsten slag from waste SCR denitration catalyst - Google Patents
Method for recovering nano nickel 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 nickel 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 recovery, tungsten slag treatment and the like, high-value nano nickel titanate and high-purity tungsten slag products can be recovered through the recovery process, the element recovery rate is high, the product purity meets industrial application, the recovery process is simple and feasible, and the method is a novel efficient recovery process of titanium and tungsten elements in the waste SCR denitration catalyst.
Description
Technical Field
The invention belongs to the field of non-ferrous metal recovery, and particularly relates to a method for recovering nano nickel titanate and high-purity tungsten slag from a waste SCR denitration catalyst.
Background
Titanium and tungsten are rare metal elements, are distributed in nature in a relatively dispersed manner, have relatively low content and relatively high extraction and utilization difficulty, and require a large amount of investment. The content of precious metal resources in the solid waste is often far higher than that in natural ores, and the types of impurity elements are relatively few. Therefore, the method has the advantages that precious metal resources are recovered from the solid wastes in a specific form according to specific requirements, the complexity and difficulty of the recovery process are greatly reduced, and meanwhile, the mass production cost is saved. The waste SCR denitration catalyst is solid waste rich in precious metal resources, wherein the content of titanium dioxide can reach more than 70%, and the content of tungsten trioxide can reach more than 5%, so that the recovery value of the waste SCR denitration catalyst is approved by industry people and relevant research is carried out in recent years.
In addition, as a special solid waste, the waste SCR denitration catalyst also has the characteristics of high yield, great harm and the like, and the efficient harmless treatment of the waste SCR denitration catalyst is not only considered from the viewpoint of precious metal resource recovery. If a large amount of waste SCR denitration catalysts are treated in a simple mode of random stacking or landfill in the past, a large amount of highly toxic elements such as vanadium, arsenic, mercury, selenium and the like contained in the waste catalysts enter the environment, harm is caused to soil, underground water and the surrounding living environment, and the living environment and health of human beings are seriously influenced. Meanwhile, a large amount of waste SCR denitration catalysts are improperly treated, and adverse effects and cost loss are caused to enterprises certainly.
The recovery of titanium and tungsten elements from the waste SCR denitration catalyst has important significance in resource saving and environmental protection, and related recovery processes are developed domestically. Chinese patent application CN201010254247.8 discloses a method for recovering metal oxides from waste flue gas denitration catalysts, which comprises the steps of mixing and roasting a waste catalyst and sodium carbonate to separate titanium and tungsten elements, respectively obtaining sodium salt precipitate of titanic acid and tungsten-containing solution, recovering the sodium salt of titanic acid by acid pickling treatment to obtain titanium dioxide, and recovering the tungsten-containing solution to obtain tungsten trioxide by calcium salt precipitation, acid pickling, roasting and the like. Chinese patent application CN201310467454.5 discloses a method for recovering SCR waste flue gas denitration catalyst, in which elements of titanium and tungsten are separated by dissolving with strong alkali to obtain sodium salt precipitate of titanic acid and tungsten-containing solution, the sodium salt of titanic acid is subjected to acid leaching, water washing, roasting and other steps to recover titanium dioxide, and for the element of tungsten, sodium chloride is added into the tungsten-containing solution, and sodium tungstate is recovered by crystallization.
The existing titanium and tungsten element recovery process in the waste SCR denitration catalyst generally has the defects of low element recovery rate, single recovered product, low recovered product value and the like, so that a more efficient novel titanium and tungsten element recovery process 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 form of nano nickel titanate and high-purity tungsten slag is a novel process for realizing the efficient disposal of the waste SCR denitration catalyst.
The invention aims to provide a method for recovering nano nickel titanate and high-purity tungsten slag from a waste SCR denitration catalyst. According to the invention, the high-quality nano nickel titanate and the high-purity tungsten slag are obtained by recovering through a specific recovery process aiming at the existence form and the 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 nickel titanate
Adding a precipitator into the titanium liquid obtained in the step (2), fully reacting, filtering to obtain a precipitate, and sequentially washing, drying and roasting the precipitate to recover the precipitate to obtain nano nickel 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-.
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), the precipitant is an ethanol solution of nickel chloride and polyacrylic acid, wherein the concentration of nickel chloride is 1.5-3mol/L, and the concentration of polyacrylic acid is 0.05-0.25 mol/L.
Preferably, in the step (3), the molar ratio of the nickel chloride to the titanium element in the precipitant is (1-2): 1.
Preferably, in the step (3), the reaction temperature is 70-90 ℃ and the reaction time is 15-45 min.
Preferably, in the step (3), the roasting temperature is 950-.
The invention has the beneficial effects that:
according to the invention, titanium and tungsten elements in the waste SCR denitration catalyst are efficiently recovered, and high-quality nano nickel titanate and high-purity tungsten slag are obtained. Wherein the purity of the nickel titanate is more than 98 percent, the content of the tungsten trioxide in the tungsten slag can reach more than 96 percent, and the recovery rates of titanium and tungsten elements respectively reach more than 90 percent and 97 percent. The method is mainly realized by the following aspects:
(1) the recovered titanium product has higher value. Titanium dioxide and coarse titanium slag are the main forms of titanium element recovery of the existing waste SCR denitration catalyst, wherein the price of the titanium dioxide is about 1.5 ten thousand yuan/ton, and the price of the coarse titanium slag is less than 5000 yuan/ton. Nickel titanate is widely used in semiconductor rectifiers, hydrocarbon dehydrogenation and sulfur addition catalysts, dyeing mixtures and other industrial fields, and recently, nickel titanate has been reported to have good performance in the field of photocatalysis. Due to excellent application prospect and higher preparation cost, the market price of the nickel titanate is far higher than that of the titanium dioxide and the coarse titanium slag. Therefore, the method has more ideal economic benefit for recovering the titanium element in the form of nickel titanate.
(2) The recovery rate of titanium element and the purity of the product have obvious advantages. When the conventional waste SCR denitration catalyst titanium element recovery process is used for recovering titanium dioxide, the recovered titanium dioxide often contains a large amount of sodium salt impurities of titanic acid due to the limit value of the process and the factors of the material, the purity is about 90% at most, and the element recovery rate is difficult to exceed 70%. 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, ethanol and polyacrylic acid in the precipitating agent used in the precipitating process have the effect of regulating and controlling the morphology of precipitate, wherein polyacrylic acid can also play a role in promoting the precipitation of titanium element and inhibiting the precipitation of impurity elements such as calcium, magnesium and silicon, and the stronger acidity of the solution can further ensure that other impurity elements are retained in the solution and separated from the titanium element. By the recovery process, the recovery rate of the titanium element can be ensured to reach more than 90%, and the purity of the recovered nickel titanate can reach more than 98%.
(3) The tungsten element recovery process is simpler, and the product purity is higher. In the waste SCR denitration catalyst components, only the tungsten trioxide component is insoluble in a sulfuric acid solution, and aiming at the existence form and the chemical characteristics of the tungsten element, the invention efficiently separates the tungsten element in the waste catalyst through an acid dissolving step, thereby greatly reducing the interference of other impurity elements on the tungsten recovery product and overcoming the problem of low purity of the tungsten recovery product in the prior art. Meanwhile, the tungsten element recovery process is very simple, the tungsten element loss caused by complicated and fussy recovery steps is effectively avoided, and the tungsten element recovery rate can reach more than 97%.
(4) The method has simple process steps, only comprises four processes of pretreatment, acid dissolution, titanium recovery and tungsten slag treatment, and is simple and conventional physical and chemical operation flows, thereby greatly reducing the difficulty of process implementation and the cost investment in the implementation process and having remarkable advantages in industrial application.
Detailed Description
The invention provides a method for recovering nano nickel titanate and high-purity tungsten slag from a waste SCR denitration catalyst, and the invention is further explained by combining a specific embodiment.
Example 1
Embodiment 1 describes a method for recovering nano nickel titanate and high-purity tungsten slag from a waste SCR denitration catalyst, which comprises the following specific 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 nickel titanate
Dissolving nickel chloride and polyacrylic acid by using ethanol, preparing a precipitator with the concentration of nickel chloride of 1.5mol/L and the concentration of polyacrylic acid of 0.05mol/L, adding the precipitator into the titanium liquid obtained in the step (2), ensuring the molar ratio of Ni/Ti =2, heating the solution to 70 ℃, stirring for 45min, and standing for 6h in a room-temperature environment after the reaction is finished. Then filtering to obtain a precipitate, washing with water, drying, and roasting at 950 ℃ for 6 hours to obtain the nano nickel 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 titanium element is 94.15%, and the recovery rate of tungsten element is 97.21%; the purity of the recovered nano nickel titanate is 98.06%, and the content of tungsten trioxide in the recovered tungsten slag is 96.75%.
Example 2
Embodiment 2 describes a method for recovering nano nickel titanate and high-purity tungsten slag from a waste SCR denitration catalyst, which comprises the following specific 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 a titanium solution and tungsten slag.
(3) Recovery of nickel titanate
Dissolving nickel chloride and polyacrylic acid by using ethanol, preparing a precipitator with the concentration of nickel chloride of 3mol/L and the concentration of polyacrylic acid of 0.25mol/L, adding the precipitator into the titanium solution obtained in the step (2), ensuring the molar ratio of Ni/Ti =1, heating the solution to 90 ℃, stirring for 15min, and standing for 12h in a room temperature environment after the reaction is finished. Then filtering to obtain a precipitate, washing with water, drying, and roasting at 1100 ℃ for 3h to obtain the nano nickel 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 2, the recovery rate of the titanium element is 93.57 percent, and the recovery rate of the tungsten element is 97.11 percent; the purity of the recovered nano nickel titanate is 98.12%, and the content of tungsten trioxide in the recovered tungsten slag is 96.15%.
Example 3
Example 3 describes another method for recovering nano nickel 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 4 hours at 650 ℃, 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 75%, adding waste catalyst powder according to the liquid-solid mass ratio of 7:1, heating the solution to 110 ℃, stirring for 3 hours, cooling the solution after the reaction is finished, and filtering to obtain a titanium solution and tungsten slag.
(3) Recovery of nickel titanate
Dissolving nickel chloride and polyacrylic acid by using ethanol, preparing a precipitator with the concentration of nickel chloride of 2mol/L and the concentration of polyacrylic acid of 0.15mol/L, adding the precipitator into the titanium solution obtained in the step (2), ensuring that the molar ratio of Ni/Ti =1.5, heating the solution to 80 ℃, stirring for 30min, and standing for 8h in a room-temperature environment after the reaction is finished. Then filtering to obtain a precipitate, washing with water, drying, and roasting at 1000 ℃ for 4h to obtain the nano nickel 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 3, the recovery rate of the titanium element is 94.23 percent, and the recovery rate of the tungsten element is 97.62 percent; the purity of the recovered nano nickel titanate is 98.09%, and the content of tungsten trioxide in the recovered tungsten slag is 96.35%.
Example 4
Embodiment 4 describes another method for recovering nano nickel titanate and high-purity tungsten slag from a waste SCR denitration catalyst, which comprises the following specific steps:
(1) pretreatment of
Roasting the waste SCR denitration catalyst for 5 hours at 700 ℃, 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 85%, 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 nickel titanate
Dissolving nickel chloride and polyacrylic acid by using ethanol, preparing a precipitator with the concentration of nickel chloride of 2.5mol/L and the concentration of polyacrylic acid of 0.10mol/L, adding the precipitator into the titanium liquid obtained in the step (2), ensuring that the molar ratio of Ni/Ti =1.8, heating the solution to 85 ℃, stirring for 25min, and standing for 7h in a room-temperature environment after the reaction is finished. Then filtering to obtain a precipitate, washing with water, drying, and roasting at 1050 ℃ for 4h to obtain the nano nickel 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 4, the recovery rate of the titanium element is 93.89%, and the recovery rate of the tungsten element is 97.01%; the purity of the recovered nano nickel titanate is 98.46%, and the content of tungsten trioxide in the recovered tungsten slag is 96.37%.
It should be understood that the above-mentioned embodiments are only for illustrating the technical concept and features of the present invention, and are not intended to be exhaustive or to limit the scope of the present invention, for providing those skilled in the art with understanding the present invention and implementing the same. 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 (7)
1. A method for recovering nano nickel 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 below 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 nickel titanate
Dissolving nickel chloride and a small amount of polyacrylic acid by using ethanol to prepare a precipitator, adding the prepared precipitator into the titanium liquid obtained in the acid dissolving step, heating the solution to 70-90 ℃, stirring for 15-45min, placing the solution in a room temperature environment for 6-12h after the reaction is finished, and then filtering to obtain a precipitate; washing, drying and roasting the precipitate in sequence to complete the recovery of the nickel 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 then sequentially washing, drying and recycling to obtain the high-purity tungsten slag.
2. The method for recovering nano nickel titanate and high-purity tungsten slag 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 nickel 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 nickel 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 nano nickel titanate and high-purity tungsten slag from the waste SCR denitration catalyst according to claim 1, wherein the concentration of each component of the precipitant in the step (3) is 1.5-3mol/L of nickel chloride and 0.05-0.25mol/L of polyacrylic acid.
6. The method for recovering the nano nickel titanate and the high-purity tungsten slag from the waste SCR denitration catalyst according to claim 1, wherein the molar ratio of nickel chloride to titanium in the precipitator in the step (3) is (1-2): 1.
7. The method for recovering nano nickel titanate and high-purity tungsten slag from the waste SCR denitration catalyst as claimed in claim 1, wherein the calcination temperature in the step (3) is 950-.
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