CN109821859B - Method for treating waste fluid catalytic cracking catalyst - Google Patents
Method for treating waste fluid catalytic cracking catalyst Download PDFInfo
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Abstract
The invention provides a method for treating a fluid catalytic cracking waste catalyst, which comprises the following steps: 1) preparing the screened waste fluid catalytic cracking catalyst into slurry; 2) under certain hydrothermal conditions, carrying out hydrothermal reaction on the slurry, and naturally cooling after the hydrothermal reaction is finished to obtain a reactant A; 3) and mixing the reactant A with water, stirring at room temperature, filtering, washing and drying to obtain the harmless fluid catalytic cracking waste catalyst. The method realizes the reconstruction of the structure of the fluid catalytic cracking waste catalyst by a hydrothermal method, and in the reconstruction process, heavy metals such as Ni, V and the like are immobilized in the reconstructed structure of the fluid catalytic cracking waste catalyst, so that the toxicity of the catalyst is greatly reduced, and the environmental pollution is further prevented, wherein the leaching toxicity of the nickel element and the vanadium element can be respectively as low as 0.089mg/L and 0.076mg/L, which is far lower than the requirement of < 5mg/L in GB5085.3-2007 'hazardous waste identification Standard leaching toxicity identification'.
Description
Technical Field
The invention relates to the technical field of industrial waste treatment, in particular to a method for treating a fluid catalytic cracking waste catalyst.
Background
The Fluid Catalytic Cracking (FCC) catalyst is one of the most used catalysts in petroleum processing links, and due to the large deposition of carbon deposits on the surface of the catalyst in the catalytic cracking process, the damage of steam to active components at high temperature, and the adsorption and reaction of heavy metals (Ni, V, Fe, etc.) in crude oil with the active sites of the FCC catalyst, the FCC catalyst is greatly deactivated, and the rejection amount of the FCC catalyst is gradually increased. The current global production of spent catalyst is reported to exceed 60 million tons, approaching 20 million tons domestically.
In 2016, 8, 1 and newly released 'national records of dangerous wastes', the FCC waste catalyst is listed in the records of dangerous wastes and classified as HW 50-class dangerous wastes. Because a large amount of toxic and harmful components, mainly heavy metal elements, are accumulated in the FCC spent catalyst, random discharge can not only cause environmental pollution, but also harm human health, and how to treat the components becomes a problem to be solved urgently. Because the recovery and utilization of the waste FCC catalyst are still in the exploration and testing stage, the most important treatment mode of the waste FCC catalyst is still landfill, and the landfill of the waste FCC catalyst is a simple and easy method, the waste FCC catalyst with lost activity is usually landfill treated according to the designated waste site. In foreign countries, the waste catalyst can be landfilled to meet a certain standard, for example, in the United states, the environmental protection method has strict limits on the landfilling of the waste catalyst, and toxic substances must be converted into non-toxic substances before the landfilling of the waste catalyst. With the increasing national environmental standards, domestic environmental problems are also receiving more and more attention from people. After the land resource and environment management department approves and permits the landfill, the land resource and environment management department evaluates and identifies the landfill to confirm that the landfill of the waste catalyst is approved after being harmless to the land and the environment, and the landfill treatment is carried out in a certain mode. Therefore, before landfilling, it is necessary to perform harmless treatment on toxic and harmful components (mainly heavy metal elements) in the FCC waste catalyst.
Currently, the methods for harmless treatment of FCC spent catalyst mainly include chemical methods, incineration methods, thermal plasma methods, and the like. The chemical method is to contact the waste FCC catalyst with chemicals and react with harmful metals such as vanadium, nickel, iron, sodium and the like deposited on the catalyst to clean out the harmful metals or reduce the toxicity of the harmful metals. According to the regulations of the general rules of hazardous waste identification, the waste after the treatment of hazardous waste with one or more hazardous characteristics such as toxicity (including leaching toxicity, acute toxicity and other toxicity) and infectivity still belongs to hazardous waste. Therefore, the spent FCC catalyst after chemical treatment is still a hazardous waste and has not been rendered harmless. The incineration method is to incinerate the FCC waste catalyst at high temperature to remove the carbon deposit, and to carry out structural recombination on the toxic and harmful components (mainly heavy metal elements) in the FCC waste catalyst by high-temperature calcination to immobilize the components, but the method has low harmless efficiency, needs high-temperature treatment, and has danger, safety and high economic cost. The thermal plasma process is a new development in recent years for the treatment of particularly delicate hazardous waste, which, although it has unique advantages for the treatment of this particular class of toxic waste, is too expensive in terms of economic cost; the plasma process requires more process control parameters, requires a high degree of automation, still lacks a solid engineering foundation for large-scale equipment, and has low feasibility of industrial operation.
Therefore, the development of an efficient, safe, convenient and harmless treatment mode of the FCC spent catalyst, which can be industrially operated, has very important significance.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for treating a spent fcc catalyst, so as to solve the problems of low treatment efficiency, insecurity and high cost of the existing spent fcc catalyst, such that the spent fcc catalyst is not easy to be applied industrially.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a method for treating a spent fluid catalytic cracking catalyst, comprising the steps of:
1) preparing the screened waste fluid catalytic cracking catalyst into slurry;
2) under a certain hydrothermal condition, carrying out hydrothermal reaction on the slurry, and naturally cooling after the hydrothermal reaction is finished to obtain a reactant A;
3) and mixing the reactant A with water, stirring at room temperature, filtering, washing and drying to obtain the harmless fluid catalytic cracking waste catalyst.
Optionally, the sieve pore size of the sieving treatment in the step 1) is less than or equal to 100 meshes.
Optionally, the solid content of the slurry in step 1) is 15-20%.
Optionally, the hydrothermal conditions in step 2) are:
hydrothermal temperature: 120-200 ℃;
hydrothermal heat preservation time: 2-4 h;
hydrothermal stirring speed: 180-220 r/min.
Optionally, the amount of the water used in the step 3) is 5 to 10 times of the amount of the reactant a.
Optionally, the stirring speed in the step 3) is 200-300r/min, and the stirring time is 20-60 min.
Optionally, the drying temperature for drying in the step 3) is 100 ℃ to 120 ℃.
Compared with the prior art, the method for treating the waste fluid catalytic cracking catalyst has the following advantages:
1. the treatment method of the waste fluid catalytic cracking catalyst realizes the reconstruction of the structure of the waste fluid catalytic cracking catalyst by a hydrothermal method, and in the reconstruction process, heavy metals such as Ni, V and the like are immobilized in the reconstructed structure of the waste fluid catalytic cracking catalyst, so that the toxicity of the waste fluid catalytic cracking catalyst is greatly reduced, and the pollution to the environment is further prevented, wherein the leaching toxicity of the nickel element and the vanadium element can be respectively as low as 0.089mg/L and 0.076mg/L, which is far lower than the requirement of < 5mg/L in the leaching toxicity identification of GB5085.3-2007 hazardous waste identification standard.
2. The method for treating the fluid catalytic cracking waste catalyst by adopting the hydrothermal method is simple, the treatment efficiency is high, the water for washing and filtering can be repeatedly used, and the water after being repeatedly used can be concentrated, so that the method has no by-product which pollutes the environment, is green and environment-friendly, has low economic cost, has mild reaction conditions, is safe and reliable, and is easy for industrial application.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The present invention will be described in detail with reference to examples.
Example 1
A treatment method of a fluid catalytic cracking waste catalyst specifically comprises the following steps:
1) screening the waste FCC catalyst by using a sieve with 100-mesh sieve pore size, mixing 1.2kg of the waste FCC catalyst with 100-mesh sieve pore size with tap water to prepare slurry with 15% of solid content;
2) feeding the slurry into a hydrothermal reaction kettle with the hydrothermal temperature of 160 ℃, stirring at a hydrothermal stirring speed of 180r/min, carrying out hydrothermal heat preservation for 2 hours, carrying out hydrothermal reaction on the slurry, and naturally cooling to room temperature after the hydrothermal reaction is finished to obtain a reactant A;
3) mixing the reactant A with water, wherein the using amount (mass) of the water is 5 times of that of the reactant A, stirring at the stirring speed of 200r/min for 20min at room temperature, filtering, washing, and drying at 120 ℃ to obtain the harmless fluid catalytic cracking waste catalyst.
The leaching toxicity of the harmless fcc waste catalyst of this example was tested according to GB5085.3-2007 "hazardous waste identification standard leaching toxicity identification", and compared with the same batch of fcc waste catalyst that was not treated by the treatment method of this example, wherein the testing instrument for the leaching toxicity was inductively coupled plasma atomic emission spectroscopy (ICP-AES).
Tests show that the leaching toxicity of the nickel element and the vanadium element of the harmless fluid catalytic cracking waste catalyst in the embodiment is respectively 0.189mg/L and 0.255mg/L, which is far lower than the requirement of < 5mg/L in GB5085.3-2007 'hazardous waste identification standard leaching toxicity identification', while the leaching toxicity of the nickel element and the vanadium element of the same batch of fluid catalytic cracking waste catalyst which is not treated by the treatment method in the embodiment is 50.436mg/L and 37.574mg/L, which is far higher than the requirement of < 5mg/L in GB5085.3-2007 'hazardous waste identification standard leaching toxicity identification'.
Example 2
A treatment method of a fluid catalytic cracking waste catalyst specifically comprises the following steps:
1) screening the waste FCC catalyst by using a sieve with 100-mesh sieve pore size, mixing 1.2kg of the waste FCC catalyst with 100-mesh sieve pore size with tap water to prepare slurry with 15% of solid content;
2) feeding the slurry into a hydrothermal reaction kettle with the hydrothermal temperature of 170 ℃, stirring at the hydrothermal stirring speed of 200r/min and carrying out hydrothermal heat preservation for 3 hours to enable the slurry to carry out hydrothermal reaction, and naturally cooling to room temperature after the hydrothermal reaction is finished to obtain a reactant A;
3) mixing the reactant A with water, wherein the using amount (mass) of the water is 5 times of that of the reactant A, stirring at the stirring speed of 220r/min for 20min at room temperature, filtering, washing, and drying at 120 ℃ to obtain the harmless fluid catalytic cracking waste catalyst.
The leaching toxicity of the harmless fcc waste catalyst of this example was tested according to GB5085.3-2007 "hazardous waste identification standard leaching toxicity identification", and compared with the same batch of fcc waste catalyst that was not treated by the treatment method of this example, wherein the testing instrument for the leaching toxicity was inductively coupled plasma atomic emission spectroscopy (ICP-AES).
Tests show that the leaching toxicity of the nickel element and the vanadium element of the harmless fluid catalytic cracking waste catalyst in the embodiment is respectively 0.126mg/L and 0.184mg/L, which is far lower than the requirement of < 5mg/L in GB5085.3-2007 'hazardous waste identification standard leaching toxicity identification', while the leaching toxicity of the nickel element and the vanadium element of the same batch of fluid catalytic cracking waste catalyst which is not treated by the treatment method in the embodiment is 46.892mg/L and 36.568mg/L, which is far higher than the requirement of < 5mg/L in GB5085.3-2007 'hazardous waste identification standard leaching toxicity identification'.
Example 3
A treatment method of a fluid catalytic cracking waste catalyst specifically comprises the following steps:
1) screening the waste FCC catalyst by using a sieve with 100-mesh sieve pore size, mixing 1.2kg of the waste FCC catalyst with 100-mesh sieve pore size with tap water to prepare slurry with 15% of solid content;
2) feeding the slurry into a hydrothermal reaction kettle with the hydrothermal temperature of 180 ℃, stirring at a hydrothermal stirring speed of 200r/min, carrying out hydrothermal heat preservation for 3 hours, carrying out hydrothermal reaction on the slurry, and naturally cooling to room temperature after the hydrothermal reaction is finished to obtain a reactant A;
3) mixing the reactant A with water, wherein the using amount (mass) of the water is 5 times of that of the reactant A, stirring at the stirring speed of 240r/min for 20min at room temperature, filtering, washing, and drying at 120 ℃ to obtain the harmless fluid catalytic cracking waste catalyst.
The leaching toxicity of the harmless fcc waste catalyst of this example was tested according to GB5085.3-2007 "hazardous waste identification standard leaching toxicity identification", and compared with the same batch of fcc waste catalyst that was not treated by the treatment method of this example, wherein the testing instrument for the leaching toxicity was inductively coupled plasma atomic emission spectroscopy (ICP-AES).
Tests show that the leaching toxicity of the nickel element and the vanadium element of the harmless fluid catalytic cracking waste catalyst in the embodiment is respectively 0.096mg/L and 0.197mg/L, which are far lower than the requirement of < 5mg/L in GB5085.3-2007 'hazardous waste identification standard leaching toxicity identification', while the leaching toxicity of the nickel element and the vanadium element of the same batch of fluid catalytic cracking waste catalyst which is not treated by the treatment method in the embodiment is 47.453mg/L and 35.865mg/L, which are far higher than the requirement of < 5mg/L in GB5085.3-2007 'hazardous waste identification standard leaching toxicity identification'.
Example 4
A treatment method of a fluid catalytic cracking waste catalyst specifically comprises the following steps:
1) screening the waste FCC catalyst by using a sieve with 100-mesh sieve pore size, mixing 1.2kg of the waste FCC catalyst with 100-mesh sieve pore size with tap water to prepare slurry with 15% of solid content;
2) feeding the slurry into a hydrothermal reaction kettle with the hydrothermal temperature of 160 ℃, stirring at a hydrothermal stirring speed of 220r/min, carrying out hydrothermal heat preservation for 4 hours, carrying out hydrothermal reaction on the slurry, and naturally cooling to room temperature after the hydrothermal reaction is finished to obtain a reactant A;
3) mixing the reactant A with water, wherein the using amount (mass) of the water is 5 times of that of the reactant A, stirring at the stirring speed of 260r/min for 20min at room temperature, filtering, washing, and drying at 120 ℃ to obtain the harmless fluid catalytic cracking waste catalyst.
The leaching toxicity of the harmless fcc waste catalyst of this example was tested according to GB5085.3-2007 "hazardous waste identification standard leaching toxicity identification", and compared with the same batch of fcc waste catalyst that was not treated by the treatment method of this example, wherein the testing instrument for the leaching toxicity was inductively coupled plasma atomic emission spectroscopy (ICP-AES).
Tests show that the leaching toxicity of the nickel element and the vanadium element of the harmless fluid catalytic cracking waste catalyst in the embodiment is respectively 0.093mg/L and 0.122mg/L, which is far lower than the requirement of < 5mg/L in GB5085.3-2007 'hazardous waste identification standard leaching toxicity identification', while the leaching toxicity of the nickel element and the vanadium element of the same batch of fluid catalytic cracking waste catalyst which is not treated by the treatment method in the embodiment is 50.436mg/L and 37.574mg/L, which is far higher than the requirement of < 5mg/L in GB5085.3-2007 'hazardous waste identification standard leaching toxicity identification'.
Example 5
A treatment method of a fluid catalytic cracking waste catalyst specifically comprises the following steps:
1) screening the waste FCC catalyst by using a sieve with 100-mesh sieve pore size, mixing 1.2kg of the waste FCC catalyst with 100-mesh sieve pore size with tap water to prepare slurry with 15% of solid content;
2) feeding the slurry into a hydrothermal reaction kettle with the hydrothermal temperature of 170 ℃, stirring at the hydrothermal stirring speed of 180r/min, carrying out hydrothermal heat preservation for 4 hours, carrying out hydrothermal reaction on the slurry, and naturally cooling to room temperature after the hydrothermal reaction is finished to obtain a reactant A;
3) mixing the reactant A with water, wherein the using amount (mass) of the water is 5 times of that of the reactant A, stirring at the stirring speed of 280r/min for 20min at room temperature, filtering, washing, and drying at 120 ℃ to obtain the harmless fluid catalytic cracking waste catalyst.
The leaching toxicity of the harmless fcc waste catalyst of this example was tested according to GB5085.3-2007 "hazardous waste identification standard leaching toxicity identification", and compared with the same batch of fcc waste catalyst that was not treated by the treatment method of this example, wherein the testing instrument for the leaching toxicity was inductively coupled plasma atomic emission spectroscopy (ICP-AES).
Tests show that the leaching toxicity of the nickel element and the vanadium element of the harmless fluid catalytic cracking waste catalyst in the embodiment is respectively 0.089mg/L and 0.076mg/L, which is far lower than the requirement of < 5mg/L in GB5085.3-2007 'hazardous waste identification standard leaching toxicity identification', while the leaching toxicity of the nickel element and the vanadium element of the same batch of fluid catalytic cracking waste catalyst which is not treated by the treatment method in the embodiment is respectively 46.892mg/L and 36.568mg/L, which is far higher than the requirement of < 5mg/L in GB5085.3-2007 'hazardous waste identification standard leaching toxicity identification'.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. A method for treating a fluid catalytic cracking spent catalyst is characterized by comprising the following steps:
1) mixing the screened waste fluid catalytic cracking catalyst with tap water to prepare slurry;
2) under a certain hydrothermal condition, carrying out hydrothermal reaction on the slurry, and naturally cooling after the hydrothermal reaction is finished to obtain a reactant A;
3) mixing the reactant A with water, stirring at room temperature, filtering, washing and drying to obtain a harmless fluid catalytic cracking waste catalyst;
the aperture of the sieve pores subjected to screening treatment in the step 1) is less than or equal to 100 meshes;
the solid content of the slurry in the step 1) is 15-20%;
the hydrothermal conditions in the step 2) are as follows:
hydrothermal temperature: 120-200 ℃;
hydrothermal heat preservation time: 2-4 h;
hydrothermal stirring speed: 180-220 r/min.
2. The method for treating spent fluidized catalytic cracking catalyst according to claim 1, wherein the amount of the water used in the step 3) is 5 to 10 times the amount of the reactant a.
3. The method as claimed in claim 1, wherein the stirring speed in step 3) is 200-300r/min, and the stirring time is 20-60 min.
4. The method as claimed in claim 1, wherein the drying temperature of the drying in step 3) is 100-120 ℃.
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| CN111763069B (en) * | 2020-07-10 | 2021-12-07 | 武汉理工大学 | Waste FCC catalyst ceramic membrane support and preparation method and application thereof |
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| CN102125872B (en) * | 2011-01-17 | 2013-05-29 | 湖南聚力催化剂股份有限公司 | Method for synthesizing porous microsphere material containing NaY zeolite by waste FCC (fluid catalytic cracking) catalyst |
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