CN114540073A - Method for removing catalyst particles in catalytic cracking slurry oil - Google Patents
Method for removing catalyst particles in catalytic cracking slurry oil Download PDFInfo
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Classifications
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G53/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes
- C10G53/02—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention relates to a method for removing catalyst particles in catalytic cracking slurry oil, which comprises the following steps: s1, preheating the catalytic cracking slurry oil to obtain thermal catalytic cracking slurry oil; s2, adding a flocculating agent and a weighting agent into solvent water to prepare a settling auxiliary agent, preheating the settling auxiliary agent, adding the preheated settling auxiliary agent into the thermocatalytically cracked oil slurry, mixing, and shearing to emulsify the mixture to obtain emulsified oil slurry; s3, the emulsified oil slurry is continuously subjected to static sedimentation separation at the temperature of 110-200 ℃ and under the pressure of 0.2-1.3MPa, and the mixture of the separated catalyst particles and water is discharged. The method of the invention reduces the types of the sedimentation auxiliary agents by means of heating and pressurizing auxiliary treatment, and greatly reduces the economic and labor cost of using the sedimentation auxiliary agents; the method is suitable for various oil slurries with different properties, has the advantages of small investment, low operation cost and high removal rate, and can reduce the ash content in the catalytic oil slurry to be less than 0.005 wt.%.
Description
Technical Field
The invention belongs to the technical field of solid-liquid separation, and particularly relates to a method for removing catalyst particles in catalytic cracking slurry oil.
Background
The catalytic cracking slurry oil is rich in polycyclic aromatic hydrocarbons, is an ideal raw material for producing products such as fuel oil, needle coke, carbon fiber materials, carbon black, plasticizers, petroleum resin and the like, but the slurry oil de-solidification is a great technical problem in the petrochemical industry of China, so that the development of a catalytic cracking slurry oil de-solidification process technology which is suitable for the national conditions of China is urgently needed.
At present, most of catalytic cracking oil slurry in China is directly used as heavy fuel oil or as a blending component of the fuel oil, but the utilization rate of the catalytic cracking oil slurry in the two ways to the oil slurry is low. This not only causes great economic loss, but also causes serious coking problem of the furnace tube due to the high content of catalyst particles in the slurry oil. Under the condition that the profit of the oil refining industry is gradually reduced, research and development of a high value-added utilization way of catalytic cracking slurry oil become the key for improving the economy of a catalytic cracking unit. Since the last decade, a great deal of research has been conducted on the technologies of removing solid particles from catalytic cracking slurry oil and comprehensively utilizing the solid particles, and at present, there are 5 main technologies for separating catalyst particles from slurry oil: natural sedimentation, centrifugal separation, filtration separation, sedimentation aid, and electrostatic separation. In recent years, there are also magnetic separation techniques and high-temperature ceramic membrane separation techniques.
In the traditional separation method, the separation process of the natural sedimentation method is generally carried out in a settler, and factors such as oil slurry density, oil slurry viscosity, particle size and density influence the sedimentation velocity of solid particles in the settler. Under certain temperature conditions, the settling velocity of the particles increases along with the increase of the size. However, in the catalyst slurry-particle dispersion system, the catalyst particles are very fine, and the asphaltene and colloid contained in the slurry affect the dispersion action at the time of particle settling, so that the effect of purification and separation is poor, and it is generally difficult to remove particles having a diameter of 20nm or less by gravity settling. Although the equipment is simple and the cost is low, the disadvantages are that the period is too long, the operation temperature is high, the de-solidification effect is not ideal, and the method is only effective for particles with the particle size of more than 20 nm.
The separation effect of the filtration method is not influenced by the property change of the raw materials or the operation condition of the catalytic cracking unit, the separation efficiency is stable, and the equipment is simple. The material of the filter element is porous metal or stainless steel powder sintered by a wire mesh, and the filtering pore diameter is controlled between 0.2 and 20 mu m. The filter element has the advantages of higher strength, higher pressure difference bearing capability and operation under high temperature conditions, and is simple to operate and low in investment, but the method needs long flushing time, has high resistance in the oil slurry filtering process and has poor separation effect on small-particle-size particles.
The viscosity, conductivity and dielectric constant of the oil slurry in the electrostatic separation method have great influence on the electrostatic separation effect, and when the factors are in a proper range, the effect is good, but the oil slurry with high content of colloid and asphaltene has poor separation effect, because the asphalt colloid can bring adverse effect to the separation
The centrifugal separation method has good separation effect on particles with the particle size of more than 10nm and wide operation temperature range, but the equipment is also complicated, so the investment cost is also high.
The magnetic separation technology is mainly used for regeneration and recovery of the waste catalyst, and the metal content is required to reach a certain degree, so that the application is limited. The high-temperature ceramic membrane separation technology has the advantages of remarkable separation effect, short separation time, high filtration precision, mild backwashing and the like, gradually draws attention of people, but the ceramic membrane has high manufacturing cost and complex process.
Compared with the method, the settling auxiliary agent method has higher separation efficiency, low agent adding cost and good economic benefit. USP5593572 discloses a process for removing spent catalyst fines from a catalytic slurry oil by adding a sufficient amount of an aliphatic polymer containing heteroatoms (N, S, O) to the slurry oil and performing a flocculation and sedimentation separation. USP6316685 discloses the use of unsaturated carboxylic acid polymers containing polyol and alkoxylated alkyl phenolic resin units as a settling aid. Patent USP5481059 describes the alkoxylation addition of acrylic acid with phenolic resins as a sedimentation aid. The above patents show that the settling of the auxiliary agent can greatly improve the settling effect and shorten the settling time, but even then, the settling time is about hours or even days, and the catalyst powder is concentrated in the oil slurry at the bottom of the container, and the catalyst powder is removed and the oil slurry is recovered by means of filtration, centrifugal separation and the like, which affect the treatment capacity and the treatment cost.
Patent CN101670199.A (200910190490.5) provides a method for capturing settling agent and removing catalyst solid powder in oil slurry. The trapping and settling agent comprises the following components in percentage by weight: 0-50% of alkyl R quaternary ammonium salt, 0-40% of flocculant solution and 0-100% of polyalcohol. The settling speed of the solid catalyst powder in the oil slurry is accelerated by adding the trapping settling agent, so that the ash content of the oil slurry is reduced to be below 0.05 wt.%. Patent No. 103265969.a (201310220492.0) discloses a novel catalytic slurry oil solids removal composition, which is prepared by adding the composition into slurry oil containing catalyst powder impurities for solid removal, so that the catalyst powder except the slurry oil is precipitated or enriched in another liquid phase, thereby reducing the ash content in the catalytic slurry oil to below 0.05 wt.%, and the catalyst powder removal rate is above 86%. Patent CN01205472.A discloses a composition for removing catalyst powder from slurry, which contains alkylphenol ethoxylate, alkyl sulfonate, alkyl sulfate wetting agent, alkoxylated alkylbenzene phenolic resin, and block copolymer demulsifier of polyalcohol polyoxyethylene polyoxypropylene; the invention also provides a method for removing catalyst powder in oil slurry by using the composition and application of the composition in removing catalyst powder in oil slurry. The ash content in the oil slurry after the catalyst powder is removed can be reduced to below 0.01 percent. However, the sedimentation aids used in these methods are all compositions, and the types of flocculants added are more, so that the cost and complexity of the aids are increased, and the removal rate is not ideal.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a method for removing catalyst particles in catalytic cracking slurry oil, which reduces the types of settling aids and greatly reduces the economic and labor cost of using the settling aids by means of heating and pressurizing auxiliary treatment; the method is suitable for various oil slurries with different properties, has the advantages of small investment, low operation cost and high removal rate, and can reduce the ash content in the catalytic oil slurry to be less than 0.005 wt.%.
Therefore, the invention provides a method for removing catalyst particles in catalytic cracking slurry oil, which is characterized by comprising the following steps:
s1, preheating the catalytic cracking slurry oil to obtain thermal catalytic cracking slurry oil;
s2, adding a flocculating agent and a weighting agent into solvent water to prepare a settling auxiliary agent, preheating the settling auxiliary agent, adding the preheated settling auxiliary agent into the thermocatalytically cracked oil slurry, mixing, and shearing or stirring to emulsify the mixture to obtain emulsified oil slurry;
s3, the emulsified oil slurry is continuously subjected to static sedimentation separation at the temperature of 100-200 ℃ and under the pressure of 0.2-1.3MPa, and the mixture of the separated catalyst particles and water is discharged.
Wherein, during static settlement separation, if the settlement temperature is lower than 100 ℃, the viscosity of the oil slurry is too high, and the settlement time is too long; if the temperature is higher than 200 ℃, the polymer settling aid is decomposed and cannot play a role in assisting settling. Since the polymer settling aid must be dissolved in water to function, water must be used as a solvent, but the water boils in the temperature range of 110-. And sedimentation is carried out in the heating and pressurizing process, the characteristic that the viscosity of the oil slurry is lower at high temperature is utilized, meanwhile, the solvent water does not boil, the high-molecular sedimentation auxiliary agent does not decompose, and the purpose of accelerating sedimentation is achieved.
The temperature for mixing the preheating of the catalytic cracking slurry oil and the settling auxiliary agent is not particularly limited in the invention as long as uniform mixing can be achieved. However, in order to prevent the mixing process from being too severe after the temperature exceeds the boiling point of water, the higher the temperature is, the more the viscosity of the slurry oil is decreased, the more the viscosity of the system is decreased, and the mixing efficiency is improved, considering that the viscosity of the slurry oil is decreased with the increase of the temperature. The method for removing the catalyst particles from the catalytic cracking slurry oil of the present invention is preferably that the catalytic cracking slurry oil is preheated to 90-100 ℃ and then mixed with the settling assistant, preferably preheated to 90-98 ℃.
The present invention is not limited to the shear emulsification method, as long as sufficient mixing can be achieved. In order to achieve better removal effect, the method for removing catalyst particles in catalytic cracking slurry oil of the invention preferably comprises the step of cutting or stirring at a speed of 6000rev/min-10000rev/min for 10-50min in step S2.
In the method for removing catalyst particles from catalytic cracking slurry oil, the emulsified slurry oil is preferably subjected to ultrasonic treatment and then to static settling separation. After the ultrasonic treatment is adopted for assistance, the method can reduce the types of the used sedimentation aids, greatly reduce the economic and labor cost of using the sedimentation aids, and ensure that the selection of the sedimentation aids is simpler.
The ultrasonic treatment condition is not limited in the invention, as long as the aim of strengthening mixing can be achieved, and in order to achieve better removal effect, the method for removing the catalyst particles in the catalytic cracking slurry oil disclosed by the invention is preferably used, wherein the ultrasonic treatment frequency is 80-240KHz, the time is 10min-50min, the temperature is 90-100 ℃, and the further preferred temperature is 90-98 ℃.
The method for removing the catalyst particles in the catalytic cracking slurry oil of the invention is preferably that the temperature of the static settling separation is 120-180 ℃, the pressure is 0.3-1.1MPa, and the time is 2-18 h.
In the method for removing catalyst particles from catalytic cracking slurry oil according to the present invention, preferably, the amount of the flocculant is 600-1200ppm of the weight of the catalytic cracking slurry oil, the amount of the solvent water is 4-10 wt% of the weight of the catalytic cracking slurry oil, and the weighting agent is 10-30 wt% of the weight of the solvent water.
The invention is not limited to the kind of the flocculant, and the flocculant may be dissolved in water to settle ash. In order to achieve a better removing effect, the method for removing catalyst particles from catalytic cracking slurry oil, provided by the invention, preferably comprises the step of selecting the flocculant from one or more of quaternary ammonium salt-fluorosilicone acrylate block copolymers, amphiphilic polysiloxane grafted quaternary ammonium salt block copolymers, polyether polysiloxane quaternary ammonium salt block copolymers, polyacrylamide, sodium polyacrylate, polyvinyl alcohol, ammonium sulfate, styrene sulfonate and lignosulfonate.
The present invention is not limited to the kind of weighting agent, and may be dissolved in water to increase the density of the aqueous solution. In order to achieve better removal effect, the method for removing catalyst particles in catalytic cracking slurry oil of the invention preferably comprises one or more of glucose, ammonium citrate, cellulose, starch and dextrin.
Compared with the prior preparation method, the invention has the beneficial effects that:
by means of ultrasonic assistance and heating and pressurizing treatment, the types of the sedimentation aids are reduced, and the sedimentation aids are low in cost, so that the sedimentation aids are simpler to select; the method is suitable for various oil slurries with different properties, has small investment, low operation cost and high removal rate, can reduce the ash content in the catalytic oil slurry to below 0.005 wt.%, and has the removal rate of catalyst particles of about 95 percent.
Drawings
FIG. 1 is a schematic process flow diagram of the method for removing catalyst particles from catalytic cracking slurry oil according to the present invention.
Detailed Description
The embodiments of the present invention will be described in detail below with reference to the accompanying drawings: the present example is carried out on the premise of the technical scheme of the present invention, and detailed embodiments and processes are given, but the scope of the present invention is not limited to the following examples, and experimental methods without specific conditions noted in the following examples are generally performed under conventional conditions.
Referring to fig. 1, the main process of the method for removing catalyst particles from catalytic cracking slurry oil of the present invention is: firstly, preparing an aqueous solution containing a flocculating agent and a weighting agent as a settling auxiliary agent, preheating catalytic cracking slurry oil to 90-98 ℃, and uniformly mixing the settling auxiliary agent and the thermal catalytic cracking slurry oil through a mixer to obtain emulsified slurry oil; then, the emulsified slurry oil enters a settling tank with an ultrasonic generator for settling. Wherein, the mixer can be a high-speed shearing emulsifying machine commonly used in laboratories, and can also be a static mixer commonly used in industry.
The removal effect in the examples was evaluated by ash, which was determined in GB508-65, and the ash content of the slurry before solids removal was compared each time. The removal rate (ash value of slurry after solid removal/ash value of slurry before solid removal) × 100%. The main properties of the slurries used in the following examples are shown in table 1 below.
TABLE 1 Properties of the catalytic cracking slurries for the experiments
Example 1
(1) 250g Liaohe catalytic cracking slurry oil is weighed and put into a three-neck flask, the three-neck flask is placed in an electric heating sleeve with a magnetic stirring and temperature control device, a condensing tube is connected, a power supply is turned on, and the temperature is adjusted to 90 ℃.
(2) Measuring solvent water with the mass of 4 wt.% of Liaohe catalytic cracking slurry oil by using a measuring cylinder, putting the solvent water into a beaker, heating the beaker to 90 ℃, stirring the solvent water, weighing a certain mass of flocculant ammonium sulfate (the addition is 600ppm of the Liaohe catalytic cracking slurry oil), adding the flocculant ammonium sulfate into the beaker, weighing a weighting agent ammonium citrate, pouring the weighting agent ammonium citrate into the beaker (the total addition is 30 wt.% of the water), and uniformly mixing to obtain a settling auxiliary agent, wherein the temperature is kept constant by using an electric heating mode in the process.
(3) Adding the prepared settling auxiliary agent into the catalytic cracking slurry oil preheated to the set temperature while the settling auxiliary agent is hot.
(4) And transferring the mixture to a high-speed shearing emulsifying machine, setting the rotating speed of the emulsifying machine at 6000r/min, keeping the mixing time at 50min, transferring the mixture to a settling tank with an ultrasonic generator, and settling (the ultrasonic frequency is 80KHz, the ultrasonic time is 50min, the ultrasonic temperature is kept at 90 ℃), the static settling pressure is 0.3MPa, the temperature is kept at 120 ℃, and the settling time is 18h, so that the settled oil slurry ash content is 88 ppm.
Example 2
(1) Weighing 250g of Jilin petrochemical catalytic cracking slurry oil, putting the weighed Jilin petrochemical catalytic cracking slurry oil into a three-neck flask, putting the three-neck flask into an electric heating sleeve with a magnetic stirring and temperature control device, connecting a condensing tube, turning on a power supply and adjusting the temperature to 91 ℃.
(2) Measuring solvent water with the mass of 5 wt.% of catalytic cracking slurry oil by using a measuring cylinder, putting the solvent water into a beaker, heating the beaker to 91 ℃, stirring the beaker simultaneously, weighing a certain mass of flocculant ammonium sulfate (the total addition is 700ppm of the catalytic cracking slurry oil), adding the flocculant ammonium citrate and glucose into the beaker according to the mass ratio of 1:1, pouring the weighting agents ammonium citrate and glucose into the beaker (the total addition is 28 wt.% of the solvent water), and uniformly mixing, wherein the temperature is kept constant by using an electric heating mode in the process.
(3) And adding the prepared settling assistant aqueous solution into the catalytic cracking slurry oil preheated to the set temperature while the solution is hot under the stirring state.
(4) And transferring the mixture to a high-speed shearing emulsifying machine, setting the rotating speed of the emulsifying machine to 6500r/min, keeping the mixing time to be 45min, transferring the mixture to a settling tank with an ultrasonic generator, and settling (the ultrasonic frequency is 100KHz, the ultrasonic time is 45min, the ultrasonic temperature is 91 ℃), the static settling pressure is 0.4MPa, the temperature is 130 ℃, and the settling time is 16h, so that the ash content of the clarified oil slurry is 142 ppm.
Example 3
(1) 250g Liaohe catalytic cracking slurry oil is weighed and put into a three-neck flask, the three-neck flask is placed in an electric heating sleeve with a magnetic stirring and temperature control device, a condensing tube is connected, a power supply is turned on, and the temperature is adjusted to 92 ℃.
(2) Measuring solvent water with the mass of 6 wt.% of catalytic cracking slurry oil by using a measuring cylinder, putting the solvent water into a beaker, heating the beaker to 92 ℃, stirring the beaker simultaneously, weighing a certain mass of flocculant quaternary ammonium salt-fluorosilicone acrylate block copolymer + polyacrylamide (with the molecular weight of 500 ten thousand) (the mass ratio of the two is 1:1) (the total addition amount is 800ppm of the catalytic cracking slurry oil), adding the flocculant quaternary ammonium salt-fluorosilicone acrylate block copolymer + polyacrylamide into the beaker, weighing a weighting agent ammonium citrate + glucose (the mass ratio of the two is 1:1), pouring the weighting agent ammonium citrate + glucose into the beaker (the total addition amount is 26 wt.% of water), and uniformly mixing, wherein the temperature is kept constant by using an electric heating mode in the process.
(3) And adding the prepared settling assistant aqueous solution into the catalytic cracking slurry oil preheated to the set temperature while the solution is hot under the stirring state.
(4) And transferring the mixture to a high-speed shearing emulsifying machine, setting the rotating speed of the emulsifying machine to 7000r/min, keeping the mixing time to be 40min, transferring the mixture to a settling tank with an ultrasonic generator, and settling (the ultrasonic frequency is 120KHz, the ultrasonic time is 40min, the ultrasonic temperature is kept at 92 ℃), the static settling pressure is 0.5MPa, the temperature is kept at 140 ℃, and the settling time is 14h, so that the ash content of the clarified slurry is 58 ppm.
Example 4
(1) 250g of Jilin petrochemical catalytic cracking slurry oil is weighed and placed into a three-neck flask, the three-neck flask is placed into an electric heating sleeve with a magnetic stirring and temperature control device, a condensing tube is connected, a power supply is turned on, and the temperature is adjusted to 93 ℃.
(2) Measuring solvent water with 7 wt.% of the mass of the slurry oil by using a measuring cylinder, putting the solvent water into a beaker, heating the beaker to 93 ℃, stirring the beaker simultaneously, weighing a certain mass of flocculant quaternary ammonium salt-fluorosilicone acrylate block copolymer + polyacrylamide (with the molecular weight of 700 ten thousand) (the mass ratio of the two is 1:1) (the total addition is 900ppm of the catalytic slurry oil), adding the flocculant quaternary ammonium salt-fluorosilicone acrylate block copolymer + polyacrylamide into the beaker, weighing a weighting agent ammonium citrate + glucose (the mass ratio of the two is 1:1), pouring the weighting agent ammonium citrate + glucose into the beaker (the total addition is 24 wt.% of the mass of water), and uniformly mixing, wherein the temperature is kept constant by using an electric heating mode in the process.
(3) And adding the prepared aqueous solution into the catalytic cracking slurry oil preheated to the set temperature while the aqueous solution is hot under a stirring state.
(4) And transferring the mixture to a high-speed shearing emulsifying machine, setting the rotating speed of the emulsifying machine to 7500r/min, keeping the mixing time to 35min, transferring the mixture to a settling tank with an ultrasonic generator, and settling (the ultrasonic frequency is 140KHz, the ultrasonic time is 35min, the ultrasonic temperature is kept at 93 ℃), the static settling pressure is 0.6MPa, the temperature is kept at 150 ℃, and the settling time is 12h, so that the ash content of the obtained clarified oil slurry is 192 ppm.
Example 5
(1) 250g of Liaohe catalytic cracking slurry oil is weighed and put into a three-neck flask, the three-neck flask is placed in an electric heating sleeve with a magnetic stirring and temperature control device, a condensing tube is connected, a power supply is turned on, and the temperature is adjusted to 94 ℃.
(2) Measuring solvent water with the mass of 9 wt.% of the slurry oil by using a measuring cylinder, putting the solvent water into a beaker, heating the solvent water to 94 ℃, stirring the solvent water, weighing a flocculant quaternary ammonium salt-fluorosilicone acrylate block copolymer and polyacrylamide (with the molecular weight of 1400 ten thousand) with a certain mass (the mass ratio of the flocculant quaternary ammonium salt to the fluorosilicone acrylate block copolymer to the polyacrylamide is 1:1) (the total addition is 1000ppm of the catalytic slurry oil), adding the flocculant quaternary ammonium salt to the beaker, weighing a weighting agent ammonium citrate to the glucose (the mass ratio of the flocculant to the fluorosilicone acrylate block copolymer to the glucose is 1:1), pouring the weighting agent ammonium citrate to the beaker (the total addition is 22 wt.% of the water), and uniformly mixing the flocculant and the polyacrylamide with the slurry oil, wherein the temperature is kept constant by using an electric heating mode in the process.
(3) And adding the prepared aqueous solution into the catalytic cracking slurry oil preheated to the set temperature while the aqueous solution is hot under a stirring state.
(4) And transferring the mixture to a high-speed shearing emulsifying machine, setting the rotating speed of the emulsifying machine at 8000r/min, keeping the mixing time at 30min, transferring the mixture to a settling tank with an ultrasonic generator, and settling (ultrasonic frequency of 160KHz, ultrasonic time of 30min, ultrasonic temperature of 94 ℃), wherein the static settling pressure is 0.7MPa, the temperature is kept at 160 ℃, and the settling time is 10h, so that the ash content of the obtained clarified slurry is 181 ppm.
Example 6
(1) 250g of Jilin petrochemical catalytic cracking slurry oil is weighed and placed into a three-neck flask, the three-neck flask is placed into an electric heating sleeve with a magnetic stirring and temperature control device, a condensing tube is connected, a power supply is turned on, and the temperature is adjusted to 95 ℃.
(2) Measuring solvent water with 9 wt.% of the mass of the oil slurry by using a measuring cylinder, putting the solvent water into a beaker, heating the beaker to 95 ℃, stirring the beaker at the same time, weighing a certain mass of flocculant quaternary ammonium salt-fluorine-silicon acrylate block copolymer + polyacrylamide (with the molecular weight of 200-1400 ten thousand) (the mass ratio of the two is 1:1) (the total addition amount is 1050ppm of the catalytic oil slurry), adding the flocculant quaternary ammonium salt-fluorine-silicon acrylate block copolymer + polyacrylamide into the beaker, weighing a weighting agent ammonium citrate + cellulose (with the mass ratio of 1:1) and pouring the weighting agent ammonium citrate + cellulose (with the addition amount of 20 wt.% of water) into the beaker, and uniformly mixing the mixture, wherein the temperature is kept constant by using an electric heating mode in the process.
(3) Adding the prepared aqueous solution into the catalytic cracking slurry oil preheated to the set temperature while the aqueous solution is hot under the stirring state.
(4) And transferring the mixture to a high-speed shearing emulsifying machine, setting the rotating speed of the emulsifying machine to be 8500r/min, keeping the mixing time to be 25min, then transferring the mixture to a settling tank with an ultrasonic generator for settling (ultrasonic frequency is 180KHz, ultrasonic time is 25min, ultrasonic temperature is kept at 95 ℃), static settling pressure is 0.8MPa, temperature is kept at 165 ℃, settling time is 8h, and the ash content of the obtained clarified oil slurry is 89 ppm.
Example 7
(1) 250g of Liaohe catalytic cracking slurry oil is weighed and put into a three-neck flask, the three-neck flask is placed in an electric heating sleeve with a magnetic stirring and temperature control device, a condensing tube is connected, a power supply is turned on, and the temperature is adjusted to 96 ℃.
(2) Measuring solvent water with 10 wt.% of the mass of the oil slurry by using a measuring cylinder, putting the solvent water into a beaker, heating the beaker to 96 ℃, simultaneously stirring, weighing a certain mass of flocculant sodium styrene sulfonate (the total addition is 1100ppm of the catalytic oil slurry), adding the flocculant sodium styrene sulfonate into the beaker, weighing weighting agent starch, pouring the weighting agent starch into the beaker (the addition is 18 wt.% of the mass of the solvent water), and uniformly mixing, wherein the temperature is kept constant by using an electric heating mode in the process.
(3) And adding the prepared aqueous solution into the catalytic cracking slurry oil preheated to the set temperature while the aqueous solution is hot under a stirring state.
(4) And transferring the mixture to a high-speed shearing emulsifying machine, setting the rotating speed of the emulsifying machine at 9000r/min, keeping the mixing time at 20min, transferring the mixture to a settling tank with an ultrasonic generator, and settling (ultrasonic frequency of 200KHz, ultrasonic time of 20min, ultrasonic temperature of 96 ℃), wherein the static settling pressure is 0.9MPa, the temperature is kept at 170 ℃, and the settling time is 6h, so that the ash content of the clarified slurry is 120 ppm.
Example 8
(1) Weighing 250g of Jilin petrochemical catalytic cracking slurry oil, putting the weighed Jilin petrochemical catalytic cracking slurry oil into a three-neck flask, putting the three-neck flask into an electric heating sleeve with a magnetic stirring and temperature control device, connecting a condensing tube, turning on a power supply and adjusting the temperature to 97 ℃.
(2) Measuring solvent water with the weight of 10 wt.% of the oil slurry by using a measuring cylinder, putting the solvent water into a beaker, heating the beaker to 97 ℃, stirring the beaker at the same time, weighing flocculant lignosulfonate with a certain weight (the total addition is 1150ppm of the catalytic oil slurry), adding the flocculant lignosulfonate into the beaker, weighing weighting agent starch, pouring the weighting agent starch into the beaker (the addition is 16 wt.% of the water), and uniformly mixing, wherein the temperature is kept constant by using an electric heating mode in the process.
(3) And adding the prepared aqueous solution into the catalytic cracking slurry oil preheated to the set temperature while the aqueous solution is hot under a stirring state.
(4) Transferring the mixture to a high-speed shearing emulsifying machine, setting the rotating speed of the emulsifying machine to 9500r/min, keeping the mixing time to 15min, transferring the mixture to a settling tank with an ultrasonic generator, and settling (ultrasonic frequency of 220KHz, ultrasonic time of 15min, ultrasonic temperature of 97 ℃), wherein the static settling pressure is 1.0MPa, the temperature is kept to 175 ℃, and the settling time is 4h, so that the ash content of clarified slurry is 187 ppm.
Example 9
(1) 250g of Liaohe catalytic cracking slurry oil is weighed and put into a three-neck flask, the three-neck flask is placed in an electric heating sleeve with a magnetic stirring and temperature control device, a condensing tube is connected, a power supply is turned on, and the temperature is adjusted to 98 ℃.
(2) Measuring solvent water with the weight of 10 wt.% of the oil slurry by using a measuring cylinder, putting the solvent water into a beaker, heating the beaker to 98 ℃, stirring the beaker simultaneously, weighing a certain mass of flocculant sodium polyacrylate (the total addition is 1200ppm of the catalytic oil slurry), adding the flocculant sodium polyacrylate into the beaker, weighing weighting agent starch, pouring the weighting agent starch into the beaker (the addition is 14 wt.% of the water mass), and uniformly mixing, wherein the temperature is kept constant by using an electric heating mode in the process.
(3) And adding the prepared aqueous solution into the catalytic cracking slurry oil preheated to the set temperature while the aqueous solution is hot under a stirring state.
(4) And transferring the mixture to a high-speed shearing emulsifying machine, setting the rotating speed of the emulsifying machine to 10000r/min, keeping the mixing time to 10min, transferring the mixture to a settling tank with an ultrasonic generator, and settling (the ultrasonic frequency is 240KHz, the ultrasonic time is 10min, the ultrasonic temperature is 98 ℃), the static settling pressure is 1.1MPa, the temperature is 180 ℃, and the settling time is 2h, so that the ash content of the obtained clarified oil slurry is 110 ppm.
Example 10
(1) 250g of Jilin petrochemical catalytic cracking slurry oil is weighed and placed into a three-neck flask, the three-neck flask is placed into an electric heating sleeve with a magnetic stirring and temperature control device, a condensing tube is connected, a power supply is turned on, and the temperature is adjusted to 97.5 ℃.
(2) Measuring solvent water with the weight of 7 wt.% of the oil slurry by using a measuring cylinder, putting the solvent water into a beaker, heating the beaker to 97.5 ℃, simultaneously stirring, weighing a certain mass of flocculant polyamphiphilic polysiloxane grafted quaternary ammonium salt block copolymer (the total addition is 1000ppm of the catalytic oil slurry), adding the flocculant polyamphilic polysiloxane grafted quaternary ammonium salt block copolymer into the beaker, weighing weighting agents ammonium citrate and starch (the mass ratio of the flocculant polyamphilic polysiloxane grafted quaternary ammonium salt block copolymer to the starch is 1:1), pouring the weighting agents ammonium citrate and starch into the beaker (the addition is 12 wt.% of water), and uniformly mixing, wherein the temperature is kept constant by using an electric heating mode in the process.
(3) And adding the prepared aqueous solution into the catalytic cracking slurry oil preheated to the set temperature while the aqueous solution is hot under a stirring state.
(4) And transferring the mixture to a high-speed shearing emulsifying machine, setting the rotating speed of the emulsifying machine to 9750r/min, keeping the mixing time to 43min, transferring the mixture to a settling tank with an ultrasonic generator, and settling (the ultrasonic frequency is 230KHz, the ultrasonic time is 47.5min, the ultrasonic temperature is kept at 97.5 ℃), the static settling pressure is 1.3MPa, the temperature is kept at 200 ℃, and the settling time is 3h, so that the ash content of the obtained clarified oil slurry is 110 ppm.
Example 11
(1) 250g of Liaohe catalytic cracking slurry oil is weighed and put into a three-neck flask, the three-neck flask is placed in an electric heating sleeve with a magnetic stirring and temperature control device, a condensing tube is connected, a power supply is turned on, and the temperature is adjusted to 96.5 ℃.
(2) Measuring solvent water with 8 wt.% of the oil slurry by using a measuring cylinder, putting the solvent water into a beaker, heating the beaker to 96.5 ℃, simultaneously stirring, weighing a certain mass of flocculant polyether polysiloxane quaternary ammonium salt block copolymer (the total addition amount is 800ppm of catalytic oil slurry), adding the flocculant polyether polysiloxane quaternary ammonium salt block copolymer into the beaker, weighing weighting agents cellulose and starch (the mass ratio of the two is 1:1), pouring the weighting agents cellulose and starch into the beaker (the addition amount is 10 wt.% of water), and uniformly mixing, wherein the temperature is kept constant by using an electric heating mode in the process.
(3) And adding the prepared aqueous solution into the catalytic cracking slurry oil preheated to the set temperature while the aqueous solution is hot under a stirring state.
(4) And transferring the mixture to a high-speed shearing emulsifying machine, setting the rotating speed of the emulsifying machine to be 9250r/min, keeping the mixing time to be 37min, then transferring the mixture to a settling tank with an ultrasonic generator for settling (the ultrasonic frequency is 210KHz, the ultrasonic time is 42.5min, the ultrasonic temperature is kept at 96.5 ℃), keeping the static settling pressure to be 0.95MPa, keeping the temperature at 162 ℃, and keeping the settling time to be 5h, thus obtaining the clarified oil slurry ash content of 97 ppm.
Example 12
(1) 250g of Jilin petrochemical catalytic cracking slurry oil is weighed and placed into a three-neck flask, the three-neck flask is placed into an electric heating sleeve with a magnetic stirring and temperature control device, a condensing tube is connected, a power supply is turned on, and the temperature is adjusted to 95.5 ℃.
(2) Measuring solvent water with 8.5 wt.% of the mass of the oil slurry by using a measuring cylinder, putting the solvent water into a beaker, heating the beaker to 95.5 ℃, simultaneously stirring, weighing a certain mass of flocculant polyether polysiloxane quaternary ammonium salt block copolymer + polyvinyl alcohol (with the molecular weight of 10000) (the total addition is 1050ppm of the catalytic oil slurry), adding the flocculant polyether polysiloxane quaternary ammonium salt block copolymer + polyvinyl alcohol into the beaker, weighing weighting agent dextrin sugar, pouring the weighting agent dextrin sugar into the beaker (with the addition of 16 wt.% of water), and uniformly mixing, wherein the temperature is kept constant by using an electric heating mode in the process.
(3) And adding the prepared aqueous solution into the catalytic cracking slurry oil preheated to the set temperature while the aqueous solution is hot under a stirring state.
(4) And transferring the mixture to a high-speed shearing emulsifying machine, setting the rotating speed of the emulsifying machine to 8750r/min, keeping the mixing time to be 31min, transferring the mixture to a settling tank with an ultrasonic generator, and settling (the ultrasonic frequency is 190KHz, the ultrasonic time is 37.5min, the ultrasonic temperature is kept at 95.5 ℃), wherein the static settling pressure is 0.85MPa, the temperature is kept at 155 ℃, and the settling time is 7h, so that the ash content of the obtained clarified oil slurry is 105 ppm.
Example 13
(1) 250g Liaohe catalytic cracking slurry oil is weighed and put into a three-neck flask, the three-neck flask is placed in an electric heating sleeve with a magnetic stirring and temperature control device, a condensing tube is connected, a power supply is turned on, and the temperature is adjusted to 94.5 ℃.
(2) Measuring solvent water with the mass of 9 wt.% of the slurry oil by using a measuring cylinder, putting the solvent water into a beaker, heating the beaker to 94.5 ℃, simultaneously stirring, weighing a certain mass of flocculant polyether polysiloxane quaternary ammonium salt block copolymer and styrene sulfonate (the mass ratio of the flocculant polyether polysiloxane quaternary ammonium salt block copolymer to the styrene sulfonate is 1:1) (the total addition is 1100ppm of the catalytic slurry oil), adding the flocculant polyether polysiloxane quaternary ammonium salt block copolymer and the styrene sulfonate into the beaker, weighing weighting agent cellulose, pouring the weighting agent cellulose into the beaker (the addition is 20 wt.% of the mass of water), and uniformly mixing, wherein the temperature is kept constant by using an electric heating mode in the process.
(3) And adding the prepared aqueous solution into the catalytic cracking slurry oil preheated to the set temperature while the aqueous solution is hot under a stirring state.
(4) And transferring the mixture to a high-speed shearing emulsifying machine, setting the rotating speed of the emulsifying machine to 8250r/min, keeping the mixing time to 25min, transferring the mixture to a settling tank with an ultrasonic generator, and settling (the ultrasonic frequency is 170KHz, the ultrasonic time is 32.5min, the ultrasonic temperature is kept at 94.5 ℃), the static settling pressure is 0.75MPa, the temperature is kept at 145 ℃, and the settling time is 9h, so that the ash content of the obtained clarified oil slurry is 67 ppm.
Example 14
(1) 250g of Jilin petrochemical catalytic cracking slurry oil is weighed and placed into a three-neck flask, the three-neck flask is placed into an electric heating sleeve with a magnetic stirring and temperature control device, a condensing tube is connected, a power supply is turned on, and the temperature is adjusted to 93.5 ℃.
(2) Measuring solvent water with the weight of 10 wt.% of the oil slurry by using a measuring cylinder, putting the solvent water into a beaker, heating the beaker to 93.5 ℃, simultaneously stirring, weighing a certain mass of flocculant polyether polysiloxane quaternary ammonium salt block copolymer and lignosulfonate (the mass ratio of the two is 1:1) (the total addition is 700ppm of the catalytic oil slurry), adding the flocculant polyether polysiloxane quaternary ammonium salt block copolymer and lignosulfonate into the beaker, weighing weighting agent starch, pouring the weighting agent starch into the beaker (the addition is 24 wt.% of the water mass), and uniformly mixing, wherein the temperature is kept constant by using an electric heating mode in the process.
(3) And adding the prepared aqueous solution into the catalytic cracking slurry oil preheated to the set temperature while the aqueous solution is hot under a stirring state.
(4) And transferring the mixture to a high-speed shearing emulsifying machine, setting the rotating speed of the emulsifying machine to 7750r/min, keeping the mixing time to 20min, transferring the mixture to a settling tank with an ultrasonic generator, and settling (the ultrasonic frequency is 150KHz, the ultrasonic time is 27.5min, the ultrasonic temperature is kept at 93.5 ℃), wherein the static settling pressure is 0.65MPa, the temperature is kept at 135 ℃, and the settling time is 11h, so that the ash content of the obtained clarified oil slurry is 140 ppm.
Example 15
(1) 250g Liaohe catalytic cracking slurry oil is weighed and put into a three-neck flask, the three-neck flask is placed in an electric heating sleeve with a magnetic stirring and temperature control device, a condensing tube is connected, a power supply is turned on, and the temperature is adjusted to 92.5 ℃.
(2) Measuring solvent water with 10 wt.% of the oil slurry by using a measuring cylinder, putting the solvent water into a beaker, heating the beaker to 92.5 ℃, simultaneously stirring, weighing a certain mass of flocculant amphiphilic polysiloxane grafted quaternary ammonium salt block copolymer and polyacrylamide (the mass ratio of the flocculant amphiphilic polysiloxane grafted quaternary ammonium salt block copolymer to the polyacrylamide is 1:1) (the total addition amount is 1200ppm of the catalytic oil slurry), adding the flocculant amphiphilic polysiloxane grafted quaternary ammonium salt block copolymer and the polyacrylamide into the beaker, weighing a weighting agent ammonium citrate and cellulose (the mass ratio of the flocculant amphiphilic polysiloxane grafted quaternary ammonium salt block copolymer to the cellulose is 1:1), pouring the weighting agent ammonium citrate to the beaker (the addition amount is 26 wt.% of water), and uniformly mixing, wherein the temperature is kept constant by using an electric heating mode in the process.
(3) And adding the prepared aqueous solution into the catalytic cracking slurry oil preheated to the set temperature while the aqueous solution is hot under a stirring state.
(4) And transferring the mixture to a high-speed shearing emulsifying machine, setting the rotating speed of the emulsifying machine at 7250r/min, keeping the mixing time at 15min, transferring the mixture to a settling tank with an ultrasonic generator, and settling (the ultrasonic frequency is 130KHz, the ultrasonic time is 22.5min, the ultrasonic temperature is kept at 92.5 ℃), wherein the static settling pressure is 0.2MPa, the temperature is kept at 110 ℃, and the settling time is 13h, so that the ash content of the obtained clarified oil slurry is 170 ppm.
Comparative example:
in order to further illustrate that the technical scheme of the invention has substantial technical effects compared with the prior art, the invention provides the following comparative examples:
comparative example 1:
the treatment processes (1) to (3) in the catalytic cracking slurry oil de-solidification process in the comparative example are completely the same as those in example 3;
the difference from the embodiment 3 is that: after the steps (1) to (3),
(4) and transferring the mixture to a high-speed shearing emulsifying machine, setting the rotating speed of the emulsifying machine to 7000r/min, keeping the mixing time to be 40min, transferring the mixture to a settling tank with an ultrasonic generator, and settling (the ultrasonic frequency is 120KHz, the ultrasonic time is 40min, the ultrasonic temperature is kept at 92 ℃), the static settling pressure is normal pressure, the temperature is kept at 92 ℃, and the settling time is 14h, so that the ash content of the clarified slurry is 330 ppm.
In the comparative example, the final clarified slurry ash content was 330ppm, which was 469% higher than the comparative ratio, and the ash content of the clarified slurry was >100ppm, and thus the ash content could not be used as a raw material for producing high-quality carbon materials such as needle coke.
Therefore, the viscosity of the oil slurry can be effectively reduced through heating, pressurizing and settling, the ash settling speed is accelerated, and the clarified oil slurry meeting the production requirement can be obtained in a short time. Therefore, the ash removal process of the present invention has substantial technical effects over the prior art.
Comparative example 2
The treatment processes (1) to (3) in the catalytic cracking slurry oil de-solidification process in the comparative example are completely the same as those in example 3;
the difference from the embodiment 3 is that: after the steps (1) to (3),
(4) and transferring the mixture to a high-speed shearing emulsifying machine, setting the rotating speed of the emulsifying machine to 7000r/min, keeping the mixing time to be 40min, then directly entering a settling tank for settling, wherein the static settling pressure is 0.5MPa, the temperature is kept at 140 ℃, and the settling time is 18h, so that the ash content of the obtained clarified oil slurry is 410 ppm.
In the comparative example, the ash content of the final clarified slurry was 410ppm, which was increased by 607% compared with the comparative ratio, and the ash content of the clarified slurry was >100ppm, and thus the ash content could not be used as a raw material for producing high-quality carbon materials such as needle coke.
Therefore, the sedimentation auxiliary agent can be effectively dispersed through ultrasonic treatment, the contact between the flocculating agent and ash particles is accelerated, the sedimentation efficiency is improved, and the clarified oil slurry meeting the production requirement can be obtained in a short time.
Comparative example 3
The treatment processes (1), (3) and (4) in the catalytic cracking slurry oil de-solidification process in the comparative example are completely the same as those in the example 3;
the difference from the embodiment 3 is that: step (2)
(2) Measuring solvent water with the mass of 6 wt.% of the slurry oil by using a measuring cylinder, putting the solvent water into a beaker, heating the beaker to 92 ℃, stirring the beaker simultaneously, weighing a certain mass of flocculant quaternary ammonium salt-fluorosilicone acrylate block copolymer + polyacrylamide (with the molecular weight of 500 ten thousand) (the mass ratio of the two is 1:1) (the total addition amount is 800ppm of the catalytic slurry oil), adding the flocculant quaternary ammonium salt-fluorosilicone acrylate block copolymer + polyacrylamide into the beaker, uniformly mixing, and keeping the temperature constant by using an electric heating mode in the process.
The ash content of the clarified slurry obtained by the above steps (1) to (4) was 378 ppm.
In the comparative example, the ash content of the final clarified slurry is 378ppm, the water and slurry are not obviously layered, the water and slurry are mutually interspersed, the comparative ratio of the upper clarified slurry is increased by 552%, and the ash content of the clarified slurry is more than 100ppm, so that the ash content of the upper clarified slurry cannot be used as a raw material for producing high-quality carbon materials such as needle coke and the like.
Therefore, the addition of the weighting agent can accelerate the downward sedimentation speed of the flocculating agent and the like dissolved in the water phase, improve the sedimentation efficiency and obtain the clarified oil slurry meeting the production requirement in a short time.
Comparative example 4
The treatment processes (1) to (3) in the catalytic cracking slurry oil de-solidification process in the comparative example are completely the same as those in example 3;
the difference from the embodiment 3 is that: after the steps (1) to (3),
(4) and transferring the mixture to a high-speed shearing emulsifying machine, setting the rotating speed of the emulsifying machine to 7000r/min, keeping the mixing time to be 40min, transferring the mixture to a settling tank with an ultrasonic generator, and settling (the ultrasonic frequency is 120KHz, the ultrasonic time is 40min, the ultrasonic temperature is kept at 92 ℃), the static settling pressure is 2MPa, the temperature is kept at 250 ℃, and the settling time is 14h, so that the ash content of the clarified slurry is 470 ppm.
Because the settling temperature is too high, the polymer settling agent is decomposed, and the aim of auxiliary settling cannot be achieved, the ash content of the final clarified slurry in the comparative example is 470ppm, which is increased by 710% compared with the comparative ratio, and the ash content of the clarified slurry is more than 100ppm, so that the clarified slurry cannot be used as a high-quality carbon material raw material for producing needle coke and the like. The invention can prevent the setting agent from decomposing by controlling the highest temperature of the setting, and improve the setting effect.
Comparative example 5
The treatment processes (1) to (3) in the catalytic cracking slurry oil de-solidification process in the comparative example are completely the same as those in example 3;
the difference from the embodiment 3 is that: after the steps (1) to (3),
(4) and transferring the mixture to a high-speed shearing emulsifying machine, setting the rotating speed of the emulsifying machine to 7000r/min, keeping the mixing time to be 40min, transferring the mixture to a settling tank with an ultrasonic generator, and settling (the ultrasonic frequency is 120KHz, the ultrasonic time is 40min, the ultrasonic temperature is kept at 92 ℃), the static settling pressure is normal pressure, the temperature is kept at 140 ℃, and the settling time is 14h, so that the ash content of the obtained clarified oil slurry is 512 ppm.
Because the water solution is boiled due to the fact that the pressurizing operation is not carried out in the heating and settling process, the ash content is distributed in the whole settler due to the fact that the back mixing is carried out in a large amount in the settler, the purpose of effective settling cannot be achieved, the ash content of the finally clarified oil slurry in the comparative example is 512ppm, the comparative proportion is increased by 782%, and the ash content of the clarified oil slurry is greater than 100ppm, so that the finally clarified oil slurry cannot be used as a high-quality carbon material for producing needle coke and the like. The heating and pressurizing process can prevent the boiling of the aqueous solution from causing the back mixing of the oil slurry system, and improve the sedimentation effect.
The present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof, and it is therefore intended that all such changes and modifications as fall within the true spirit and scope of the invention be considered as within the following claims.
Claims (9)
1. A method for removing catalyst particles in catalytic cracking slurry oil is characterized by comprising the following steps:
s1, preheating the catalytic cracking slurry oil to obtain thermal catalytic cracking slurry oil;
s2, adding a flocculating agent and a weighting agent into solvent water to prepare a settling auxiliary agent, preheating the settling auxiliary agent, adding the preheated settling auxiliary agent into the thermocatalytically cracked oil slurry, mixing, and shearing or stirring to emulsify the mixture to obtain emulsified oil slurry;
s3, the emulsified oil slurry is continuously subjected to static sedimentation separation at the temperature of 110-200 ℃ and under the pressure of 0.2-1.3MPa, and the mixture of the separated catalyst particles and water is discharged.
2. The method for removing catalyst particles from catalytically cracked slurry oil according to claim 1, wherein the catalytically cracked slurry oil is preheated to 90-100 ℃ and then mixed with the settling aid, preferably preheated to 90-98 ℃.
3. The method for removing catalyst particles from catalytic cracking slurry oil of claim 1, wherein in step S2, the shearing or stirring speed is 6000rev/min-10000rev/min and the time is 10-50 min.
4. The method for removing catalyst particles from catalytic cracking slurry oil according to claim 1, wherein the emulsified slurry oil is subjected to ultrasonic treatment and then to the static settling separation.
5. The method for removing catalyst particles from catalytic cracking slurry oil according to claim 4, wherein the ultrasonic treatment is performed at a frequency of 80-240KHz, for a time of 10min-50min, and at a temperature of 90-100 ℃, preferably 90-98 ℃.
6. The method as claimed in claim 1, wherein the temperature of the static settling separation is 120-180 ℃, the pressure is 0.3-1.1MPa, and the time is 2-18 h.
7. The method for removing catalyst particles from catalytic cracking slurry oil according to claim 1, wherein the flocculant is used in an amount of 600-1200ppm by weight of the catalytic cracking slurry oil, the solvent water is used in an amount of 4-10 wt.% by weight of the catalytic cracking slurry oil, and the weighting agent is used in an amount of 10-30 wt.% by weight of the solvent water.
8. The method for removing catalyst particles from catalytic cracking slurry oil according to claim 1, wherein the flocculant is one or more selected from quaternary ammonium salt-fluorosilicone acrylate block copolymer, amphiphilic polysiloxane grafted quaternary ammonium salt block copolymer, polyether polysiloxane quaternary ammonium salt block copolymer, polyacrylamide, sodium polyacrylate, polyvinyl alcohol, ammonium sulfate, styrene sulfonate and lignosulfonate.
9. The method for removing catalyst particles from catalytic cracking slurry oil according to claim 1, wherein the weighting agent is one or more selected from glucose, ammonium citrate, cellulose, starch and paste sugar.
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| CN115011377A (en) * | 2022-07-01 | 2022-09-06 | 中国海洋石油集团有限公司 | Method for separating solid in catalytic cracking slurry oil |
| CN115433605A (en) * | 2022-09-05 | 2022-12-06 | 茂名市鹰鹏机电设备有限公司 | Medium-low temperature catalytic slurry removal process |
| CN116333780A (en) * | 2023-03-24 | 2023-06-27 | 广东石油化工学院 | Separation process of catalytic cracking slurry concentrate |
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