阅读说明：本技术 一种费托合成过滤元件的再生方法 (Regeneration method of Fischer-Tropsch synthesis filter element ) 是由 杜冰 孟祥堃 卜亿峰 门卓武 李为真 于 2020-05-27 设计创作，主要内容包括：本发明属于再生领域,提供一种费托合成过滤元件的再生方法,该方法包括：(1)将待再生费托合成过滤原件卸出,安装到再生装置上；(2)在再生装置上对所述过滤元件进行预处理,去除残余的费托合成重质油；(3)用复合溶剂浸泡去重质油的过滤元件以溶解过滤元件上的残渣,然后用复合溶剂冲洗过滤元件；(4)对所述冲洗后的过滤元件进行超声处理,然后用清水冲洗过滤元件；(5)对所述步骤(4)处理完的过滤元件进行干燥。本发明的方法,将催化剂颗粒溶解或使其碎裂进而清除出去,从而实现过滤器有效再生。(The invention belongs to the field of regeneration, and provides a regeneration method of a Fischer-Tropsch synthesis filter element, which comprises the following steps: (1) unloading the Fischer-Tropsch synthesis filter element to be regenerated and installing the Fischer-Tropsch synthesis filter element on a regenerating device; (2) pretreating the filter element on a regeneration device to remove residual Fischer-Tropsch synthesis heavy oil; (3) soaking the heavy oil-removed filter element in a composite solvent to dissolve residues on the filter element, and then washing the filter element with the composite solvent; (4) carrying out ultrasonic treatment on the washed filter element, and then washing the filter element by using clean water; (5) and (4) drying the filter element treated in the step (4). The method of the invention dissolves or disintegrates the catalyst particles to remove them, thereby realizing effective regeneration of the filter.)

1. A method of regenerating a fischer-tropsch synthesis filter element, the method comprising:

(1) unloading the Fischer-Tropsch synthesis filter element to be regenerated and installing the Fischer-Tropsch synthesis filter element on a regenerating device;

(2) pretreating the filter element on a regeneration device to remove residual Fischer-Tropsch synthesis heavy oil;

(3) soaking the filter element for removing the heavy oil in a composite solvent to dissolve residues on the filter element, and then washing the filter element by the composite solvent;

(4) the rinsed filter element is sonicated and then rinsed with clean water.

2. The regeneration method according to claim 1, wherein,

the pretreatment uses high temperature gas to purge the filter element;

the high-temperature gas is at least one of nitrogen, air and water vapor;

the gas temperature is 100-500 deg.C, preferably 100-350 deg.C.

3. The regeneration method according to claim 1 or 2, wherein the complex solvent comprises: alkali, surfactant, corrosion inhibitor, assistant and chelating agent, based on the total weight of the composite solvent,

0.5-95 wt% of alkali, 0.1-10 wt% of surfactant, 0.1-8 wt% of corrosion inhibitor, 0.1-8 wt% of auxiliary agent and 0.1-8 wt% of chelating agent.

4. The regeneration method according to claim 1 or 2, wherein,

the alkali is one or more of alkali metal hydroxide, alkaline earth metal hydroxide, alkali metal carbonate and alkali metal bicarbonate, and is preferably sodium hydroxide and/or potassium hydroxide; and/or

The surfactant comprises one or more of an anionic surfactant, a cationic surfactant and a nonionic surfactant, preferably one or more of LAS, AOS and AEO type surfactants; and/or

The auxiliary agent is one or more of sodium chloride, potassium chloride, sodium carbonate and potassium carbonate; and/or

The corrosion inhibitor is a metal corrosion inhibitor, preferably sodium benzoate and/or sodium nitrite; and/or

The chelating agent is one or more of polyphosphate, aminocarboxylic acid, 1, 3-diketone, hydroxycarboxylic acid and polyamine.

5. The regeneration method according to claim 1 or 2, wherein,

the temperature for soaking the composite solvent is normal temperature to 150 ℃, preferably normal temperature to 120 ℃, and more preferably 25 ℃ to 100 ℃; and/or

The soaking time of the composite solvent is 0.1-24 hours, preferably 0.5-10 hours; and/or

The pressure for soaking the composite solvent is between normal pressure and 1.0 MPa, and preferably between normal pressure and 0.5 MPa.

6. The regeneration process according to claim 1 or 2, wherein the conditions of the sonication comprise: the temperature is 5-100 ℃.

7. The regeneration method according to claim 1 or 2, wherein the regeneration device includes:

a cleaning regeneration tank for installing the filter element to be regenerated and then carrying out the pretreatment and the composite solvent soaking and washing; and

a feed line and a discharge line for delivering pretreated feedstock and complex solvent to the cleaning regeneration tank; and

a composite solvent storage tank (E-1) which is communicated with a feed line of a composite solvent; and

a pressure pump for pumping the composite solvent from the composite solvent storage tank into the feed line; and

an ultrasonic processing unit for performing ultrasonic processing on the washed filter element, then washing the filter element with clean water, and then drying.

8. The regeneration method according to claim 7, wherein,

the feed line for cleaning the regeneration tank includes: a gas feed line (P-3), a vapor inlet pipe (P-2), a composite solvent feed line (P-1) and a composite solvent feed line (P-4);

the discharge line that washs the regenerator tank includes: a waste water discharge line (P-7), a solvent discharge line (P-6) and a waste steam discharge line (P-15);

the pressure pump comprises a compound solvent pump (E-2) and a solvent circulating pump (E-5); the composite solvent pump (E-2) is arranged between the composite solvent feeding pipeline (P-1) and the composite solvent storage tank (E-1);

the ultrasonic treatment unit comprises an ultrasonic device (E-6) for mounting and ultrasonic treatment after the filter element is unloaded from the cleaning regeneration tank;

the feed line of the ultrasonic device comprises: a solvent feed line (P-11), a solvent feed line (P-8), a feed line (P-12) and a dry gas feed line (P-13);

the discharge line of the ultrasonic device comprises: a wastewater discharge line (P-14), a solvent discharge line (P-9) and a solvent discharge line (P-10);

the solvent circulating pump (E-5) is arranged between the composite solvent feeding pipeline (P-4) and the solvent discharging pipeline (P-10) and is communicated with the discharge hole of the cleaning regeneration tank and the solvent feeding pipeline (P-11);

the solvent discharge pipeline (P-9) is communicated with the composite solvent storage tank (E-1),

the dry gas feed line (P-13) is connected to the complex solvent pump (E-2).

9. The regeneration method of claim 8, wherein the method comprises:

the Fischer-Tropsch synthesis filter pipe (E-4) to be regenerated is arranged in a cleaning regeneration tank (E-3), water vapor with the temperature of 300 ℃ is introduced from a steam inlet pipe (P-2) at the top of the cleaning regeneration tank, the water vapor enters the interior of the filter pipe and passes through the pores of the filter pipe, the Fischer-Tropsch synthesis heavy oil remaining in the filter pipe is blown out and is discharged from a steam outlet pipe (P-15) at the bottom of the cleaning regeneration tank;

closing valves of a steam inlet pipe (P-2) and a steam outlet pipe (P-15), starting a composite solvent pump (E-2), pumping the composite solvent in a composite solvent storage tank (E-1) into a cleaning regeneration tank along a pipeline (P-1) to enable the composite solvent to overflow a filter pipe to be regenerated, soaking the filter pipe to be regenerated in the composite solvent for 0.5-10h at the temperature of normal temperature to 100 ℃, and enabling a blocked catalyst in the filter pipe to react with the composite solvent to dissolve catalyst particles;

starting a composite solvent circulating pump (E-5), circulating the composite solvent in the cleaning regeneration tank for 0.5-10h along a pipeline (P-4), and in the circulation process of the composite solvent, enabling the composite solvent to flow to the outer side of the filter pipe from the pores penetrating through the filter pipe in the filter pipe and carrying out the catalyst particle dissolved in the composite solvent;

then the composite solvent in the cleaning regeneration tank is put into a composite solvent storage tank E-1 through a pipeline (P-6), clear water is introduced from the pipeline (P-3) to flush the residual composite solvent in the filter tube, the flushing water is discharged out of the cleaning regeneration tank through a pipeline (P-7), and the regenerated filter tube is discharged out of the cleaning regeneration tank for later use.

The filter pipe is detached from the cleaning regeneration tank (E-3) and then is installed in the ultrasonic device (E-6), firstly, the composite solvent pump (E-2) is started, the composite solvent in the composite solvent storage tank is pumped into the ultrasonic device (E-6) along a pipeline (P-8), so that the composite solvent is submerged in the filter pipe to be regenerated, the switch of the ultrasonic device (E-6) is turned on, and ultrasonic treatment is carried out for 1-5 hours;

starting a composite solvent circulating pump (E-5), and circulating the composite solvent in the cleaning regeneration tank along the pipelines (P-10) and (P-11); after the ultrasonic treatment is finished, putting the composite solvent in the cleaning regeneration tank into a composite solvent storage tank through a pipeline (P-9), introducing clear water from the pipeline (P-12), and stopping water washing when the pH value of the clear water discharged from the cleaning regeneration tank is 7-8;

air is introduced through the line (P-13) to blow the filter tubes dry, and the regenerated filter tubes are discharged from the cleaning regeneration tank for later use.

10. The regeneration method of claim 1, wherein the method further comprises: and (4) drying the filter element treated in the step (4).

Technical Field

The invention relates to a regeneration method of a Fischer-Tropsch synthesis filter element.

Background

The catalyst commonly used in slurry bed Fischer-Tropsch synthesis is an iron-based catalyst and a cobalt-based catalyst, the main components of the iron-based catalyst are iron, copper, potassium and silicon, the cobalt-based catalyst is metal cobalt loaded on an alumina or silica carrier, the slurry bed Fischer-Tropsch synthesis generally adopts a filtration method to realize the filtration and separation of a Fischer-Tropsch synthesis heavy product and the catalyst, and a commonly used filter element is a stainless steel wire mesh sintered pipe or a stainless steel powder sintered pipe. During the filtering process, a filter cake is gradually formed on the slurry side, the filtering pressure drop is gradually increased, and the back washing of the cleaning solution is periodically adopted. However, in the long-term use process, the catalyst fine powder gradually enters the inside of the pore channel of the filter element and is clamped in the pore channel of the filter element, and the fine powder cannot be washed out during backwashing, so that the filter element is blocked.

CN102688724B discloses a Fischer-Tropsch wax and catalyst filtering and back flushing method in a Fischer-Tropsch synthesis slurry bed reactor, which comprises the following steps: step 1: in the production mode, a clear liquid extraction system is started, and Fischer-Tropsch wax is extracted into a crude wax product buffer tank with set pressure; step 2: in the production mode, when the backflushing time interval value reaches a set value, a backflushing system is started to backflush the filter element; and step 3: and when the backflushing time reaches a set value, closing the backflushing system, and starting to extract clear liquid for delaying.

CN104606945A discloses a chemical cleaning device and a cleaning method for a filter element, wherein a to-be-cleaned recycling filter element is placed in a soaking tank, and is soaked with hydrogen peroxide of a predetermined concentration, so as to remove macromolecular organic matters adhered to the inside of the to-be-cleaned recycling filter element, so that the to-be-cleaned recycling filter element can be reused, and the cost increase caused by frequent replacement is avoided. This method has a problem that the filter tube containing the inorganic substance or metal oxide catalyst cannot be regenerated.

CN102688724B discloses a Fischer-Tropsch wax and catalyst filtering and back flushing method in a Fischer-Tropsch synthesis slurry bed reactor, wherein the Fischer-Tropsch synthesis catalyst and heavy synthetic oil are filtered and separated by using a filtering method, and when the filtering flux is reduced and the filtering pressure drop is increased, the Fischer-Tropsch synthesis catalyst and the heavy synthetic oil are regenerated by using a back flushing method. Because the holes of the filter pipe are not straight holes, some fine catalyst particles are easy to be blocked in the holes after entering the holes of the filter pipe, and can not pass through the filter pipe, and can not be washed out during back washing, and the fine catalyst particles can be accumulated more and more in the holes to cause the blockage of the filter pipe, so the defect is that the particles blocked in the filter pipe can not be cleaned out.

Disclosure of Invention

The research of the above documents finds that the prior art mainly adopts a backwashing method to regenerate the filter element, and because the filter pores of the filter element are not straight pores, and after fine catalyst particles enter the pores of the filter element, part of the fine catalyst particles are clamped in the filter element, the catalyst particles cannot be washed out by backwashing, and thus the backwashing effect is poor.

Aiming at the defects in the prior art, the invention proposes a method for regenerating a filter element, which comprises the steps of pretreating the filter element, dissolving or crushing residual oil wax and catalyst fine powder in the filter element, and treating the filter element by using ultrasonic equipment to remove residues such as catalyst powder blocked in the filter element.

In a preferred embodiment, the composite solvent is used for dissolving or crushing, the composite solvent comprises alkali, an additive and the like, wherein the alkali chemically reacts with silicon dioxide in an iron-based Fischer-Tropsch synthesis catalyst or chemically reacts with aluminum oxide in a cobalt-based Fischer-Tropsch synthesis catalyst to generate a water-soluble substance, so that fine catalyst powder blocked in pores of the filter element is dissolved or cracked, the particle size is further reduced, the residual oil wax in the filter element is further dissolved by the composite solvent, and then ultrasonic treatment is carried out to remove the crushed fine catalyst particles from the pores of the filter tube, so that the regeneration of the filter element is realized.

The method adopted by the invention can completely dissolve or completely crack the catalyst particles, thereby effectively realizing the regeneration of the filter.

Accordingly, the present invention provides a method for regenerating a fischer-tropsch synthesis filter element, the method comprising:

(1) unloading the Fischer-Tropsch synthesis filter element to be regenerated and installing the Fischer-Tropsch synthesis filter element on a regenerating device;

(2) pretreating the filter element on a regeneration device to remove residual Fischer-Tropsch synthesis heavy oil;

(3) soaking the filter element for removing the heavy oil in a composite solvent to dissolve residues on the filter element, and then washing the filter element by the composite solvent;

(4) the rinsed filter element is sonicated and then rinsed with clean water.

Preferably, the pre-treatment uses a high temperature gas to purge the filter element.

Preferably, the high temperature gas is at least one of nitrogen, air and water vapor.

Preferably, the gas temperature is from 100 ℃ to 500 ℃, preferably 100 ℃ to 350 ℃.

Preferably, the complex solvent includes: the composite solvent comprises 0.5-95 wt% of alkali, 0.1-10 wt% of surfactant, 0.1-8 wt% of corrosion inhibitor, 0.1-8 wt% of assistant and 0.1-8 wt% of chelating agent, based on the total weight of the composite solvent.

Preferably, the base is one or more of an alkali metal hydroxide, an alkaline earth metal hydroxide, an alkali metal carbonate and an alkali metal bicarbonate, preferably sodium hydroxide and/or potassium hydroxide.

Preferably, the surfactant comprises one or more of an anionic surfactant, a cationic surfactant and a non-ionic surfactant, preferably one or more of LAS, AOS, AEO type surfactants.

Preferably, the auxiliary agent is one or more of sodium chloride, potassium chloride, sodium carbonate and potassium carbonate.

Preferably, the corrosion inhibitor is a metal corrosion inhibitor, preferably sodium benzoate and/or sodium nitrite.

Preferably, the chelating agent is one or more of a polyphosphate, an aminocarboxylic acid, a 1, 3-dione, a hydroxycarboxylic acid, and a polyamine.

Preferably, the temperature for soaking the composite solvent is between normal temperature and 150 ℃, preferably between normal temperature and 120 ℃, and more preferably between 25 and 100 ℃.

Preferably, the soaking time of the composite solvent is 0.1-24 hours, and preferably 0.5-10 hours.

Preferably, the pressure for soaking the composite solvent is between normal pressure and 1.0 MPa, and preferably between normal pressure and 0.5 MPa.

Preferably, the conditions of the sonication include: the temperature is 5-100 ℃.

Preferably, the regeneration device includes:

a cleaning regeneration tank for installing the filter element to be regenerated and then carrying out the pretreatment and the composite solvent soaking and washing; and

a feed line and a discharge line for delivering pretreated feedstock and complex solvent to the cleaning regeneration tank; and

the composite solvent storage tank is communicated with a feed pipeline of the composite solvent; and

a pressure pump for pumping the composite solvent from the composite solvent storage tank into the feed line; and

an ultrasonic processing unit for performing ultrasonic processing on the washed filter element, then washing the filter element with clean water, and then drying.

Preferably, the feed line for cleaning the regeneration tank comprises: a gas feed line, a vapor inlet pipe, a composite solvent feed line, and a composite solvent feed line;

the discharge line that washs the regenerator tank includes: a waste water discharge line, a steam outlet pipe, a solvent discharge line and a waste steam discharge line;

the pressure pump comprises a composite solvent pump and a solvent circulating pump; the composite solvent pump is arranged between the composite solvent feeding pipeline and the composite solvent storage tank;

the ultrasonic treatment unit comprises an ultrasonic device E-6 which is used for mounting and ultrasonic treatment after the filter element is unloaded from the cleaning regeneration tank;

the feed line of the ultrasonic device comprises: a solvent feed line, a feed line, and a dry gas feed line;

the discharge line of the ultrasonic device comprises: a wastewater discharge line, a solvent discharge line;

the solvent circulating pump is arranged between the composite solvent feeding pipeline and the solvent discharging pipeline and is communicated with a discharging port of the cleaning regeneration tank and the solvent feeding pipeline;

the solvent discharge pipeline is communicated with the composite solvent storage tank,

the dry gas feed line is connected to a complex solvent pump.

Preferably, the method comprises:

installing a Fischer-Tropsch synthesis filter pipe to be regenerated into a cleaning regeneration tank, introducing water vapor at the temperature of 120-300 ℃ from a steam inlet pipe at the top of the cleaning regeneration tank, allowing the water vapor to enter the inside of the filter pipe, penetrating through the pores of the filter pipe, blowing out Fischer-Tropsch synthesis heavy oil remaining in the filter pipe, and discharging the Fischer-Tropsch synthesis heavy oil from a steam outlet pipe at the bottom of the cleaning regeneration tank;

closing valves of a steam inlet pipe and a steam outlet pipe, starting a composite solvent pump, pumping the composite solvent in a composite solvent storage tank into a cleaning regeneration tank along a pipeline, so that the composite solvent is submerged in a filter pipe to be regenerated, soaking the filter pipe to be regenerated in the composite solvent for 0.5-10h at the normal temperature of-100 ℃, and reacting a catalyst blocked in the filter pipe with the composite solvent to dissolve catalyst particles;

starting a composite solvent circulating pump, circulating the composite solvent in the cleaning regeneration tank for 0.5-10h along a pipeline, and in the circulation process of the composite solvent, enabling the composite solvent to flow to the outer side of the filter pipe from the pores penetrating through the filter pipe in the filter pipe and taking out the catalyst particle part dissolved by the composite solvent;

and then putting the composite solvent in the cleaning regeneration tank into a composite solvent storage tank through a pipeline, introducing clean water from the pipeline to flush the residual composite solvent in the filter pipe, discharging the flushing water out of the cleaning regeneration tank from the pipeline, and discharging the regenerated filter pipe out of the cleaning regeneration tank for later use.

The method comprises the following steps of (1) after a filter pipe is detached from a cleaning regeneration tank, installing the filter pipe into an ultrasonic device, firstly starting a composite solvent pump, pumping a composite solvent in a composite solvent storage tank into the ultrasonic device along a pipeline to enable the composite solvent to submerge the filter pipe to be regenerated, turning on a switch of the ultrasonic device at a proper temperature, and carrying out ultrasonic treatment for 1-5 hours;

starting a composite solvent circulating pump, and cleaning the composite solvent in the regeneration tank to circulate along the pipeline; after the ultrasonic treatment is finished, putting the composite solvent in the cleaning regeneration tank into a composite solvent storage tank through a pipeline, introducing clean water from the pipeline, and stopping water washing when the pH value of the clean water discharged from the cleaning regeneration tank is 7-8;

introducing hot air from the pipeline to blow the filter pipe dry, and discharging the regenerated filter pipe from the cleaning regeneration tank for later use.

Preferably, the method further comprises: and (4) drying the filter element treated in the step (4).

The main differences between the invention and the prior art are as follows:

the prior art mainly adopts a backwashing method to regenerate the filter element, and because the filter holes of the filter element are not straight holes, and after fine catalyst particles enter the holes of the filter element, part of the fine catalyst particles are clamped in the filter element, the catalyst particles cannot be washed out by backwashing, so the backwashing effect is poor. The method of the invention dissolves or disintegrates the catalyst particles to remove them, thereby realizing filter regeneration.

Drawings

FIG. 1 is a schematic view of the process for regenerating a Fischer-Tropsch synthesis filter element of the present invention.

Description of the reference numerals

E-1 composite solvent storage tank; an E-2 complex solvent pump; e-3, cleaning a regeneration tank; e-4 filtering pipes; e-5 composite solvent circulating pump; e-6 ultrasonic device.

Detailed Description

The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.

The invention is described in detail with reference to the accompanying drawings, and provides a method for regenerating a Fischer-Tropsch synthesis filter element, which comprises the following steps: (1) unloading the Fischer-Tropsch synthesis filter element to be regenerated and installing the Fischer-Tropsch synthesis filter element on a regenerating device; (2) pretreating the filter element on a regeneration device to remove residual Fischer-Tropsch synthesis heavy oil; (3) soaking the filter element for removing the heavy oil in a composite solvent to dissolve residues on the filter element, and then washing the filter element by the composite solvent; (4) the rinsed filter element is sonicated and then rinsed with clean water.

The prior art mainly adopts a backwashing method to regenerate the filter element, and because the filter holes of the filter element are not straight holes, and after fine catalyst particles enter the holes of the filter element, part of the fine catalyst particles are clamped in the filter element, the catalyst particles cannot be washed out by backwashing, so the backwashing effect is poor. The method of the invention dissolves or disintegrates the catalyst particles to remove them, thereby realizing filter regeneration.

The purpose of the pre-treatment is to remove residual fischer-tropsch synthesis heavy oil, which according to a preferred embodiment of the invention uses high temperature gas to purge the filter elements.

The high temperature gas may be selected from a wide variety of types, such as inert gas, oxygen-containing gas, and water vapor, and according to a preferred embodiment of the present invention, the high temperature gas is at least one of nitrogen, air, and water vapor.

According to a preferred embodiment of the invention, the gas temperature is between 100 ℃ and 500 ℃, preferably between 100 ℃ and 350 ℃.

The composite solvent is used for dissolving residues on the filter element, and according to a preferred embodiment of the invention, the composite solvent comprises: the composite solvent comprises 0.5-95 wt% of alkali, 0.1-10 wt% of surfactant, 0.1-8 wt% of corrosion inhibitor, 0.1-8 wt% of assistant and 0.1-8 wt% of chelating agent, based on the total weight of the composite solvent.

According to a preferred embodiment of the present invention, the base is, for example, one or more of alkali metal hydroxide, alkaline earth metal hydroxide, alkali metal carbonate and alkali metal bicarbonate, and the kinds of the alkali metal hydroxide, alkaline earth metal hydroxide, alkali metal carbonate and alkali metal bicarbonate are wide in selection range and can be applied to the present invention.

According to a preferred embodiment of the present invention, the surfactant includes one or more of anionic surfactants, cationic surfactants and nonionic surfactants, and the kinds of the anionic surfactants, the cationic surfactants and the nonionic surfactants can be selected from a wide range, the anionic surfactants are, for example, carboxylates, sulfonates, sulfate salts, phosphate salts and the like, the cationic surfactants are, for example, amine salt cationic surfactants, quaternary ammonium salt cationic surfactants and heterocyclic cationic surfactants and the like, and the nonionic surfactants are, for example, fatty alcohol polyoxyethylene ethers, fatty acid methyl ester polyoxyethylene ethers, fatty acid polyoxyethylene ether series and the like (sodium dodecylbenzene sulfonate).

According to a preferred embodiment of the present invention, preferably one or more of LAS, AOS, AEO type surfactants.

According to a preferred embodiment of the invention, the adjuvant is one or more of sodium chloride, potassium chloride, sodium carbonate and potassium carbonate.

According to a preferred embodiment of the invention, the corrosion inhibitor is a metal corrosion inhibitor, preferably a phosphate, chromate, phosphate, nitrite, silicate or the like.

According to a preferred embodiment of the present invention, the chelating agent is one or more of polyphosphate, aminocarboxylic acid, 1, 3-dione, hydroxycarboxylic acid, and polyamine.

According to a preferred embodiment of the present invention, the temperature for soaking the composite solvent is between room temperature and 150 ℃, preferably between room temperature and 120 ℃, and more preferably between 25 ℃ and 100 ℃.

According to a preferred embodiment of the present invention, the time for soaking the composite solvent is 0.1 to 24 hours, preferably 0.5 to 10 hours.

According to a preferred embodiment of the present invention, the pressure of the composite solvent soaking is normal pressure to 1.0 mpa, preferably normal pressure to 0.5 mpa.

According to a preferred embodiment of the present invention, the conditions of the ultrasonic treatment include: the temperature is 5-100 ℃.

According to a preferred embodiment of the invention, the filter element is first purged with water vapor at a high temperature of 150 ℃ to remove oil wax from the surface. And then soaking the filter element to be regenerated by using a composite solvent solution with the mass fraction of 20-60%, wherein the conditions are that the temperature is 5-100 ℃, the pressure is normal, and the soaking and repeated washing time is 0.5-10 hours. Discharging the solvent, treating with ultrasonic equipment for 2-10h, and repeatedly washing with composite solvent during ultrasonic treatment. And after the ultrasonic treatment is finished, washing the substrate with clear water until the pH value is 7-8.

According to a preferred embodiment of the present invention, preferably, the regeneration device includes:

a cleaning regeneration tank for installing the filter element to be regenerated and then carrying out the pretreatment and the composite solvent soaking and washing; and

a feed line and a discharge line for delivering pretreated feedstock and complex solvent to the cleaning regeneration tank; and

the composite solvent storage tank E-1 is communicated with a feed pipeline of the composite solvent; and

a pressure pump for pumping the composite solvent from the composite solvent storage tank into the feed line; and

an ultrasonic processing unit for performing ultrasonic processing on the washed filter element, then washing the filter element with clean water, and then drying.

Preferably, the feed line for cleaning the regeneration tank comprises: a gas feed line P-3, a vapor inlet pipe P-2, a composite solvent feed line P-1 and a composite solvent feed line P-4;

the discharge line that washs the regenerator tank includes: a waste water discharge pipeline P-7, a steam outlet pipe P-5 and a waste steam discharge pipeline P-15;

the pressure pump comprises a compound solvent pump E-2 and a solvent circulating pump E-5; the composite solvent pump E-2 is arranged between the composite solvent feeding pipeline P-1 and the composite solvent storage tank E-1;

the ultrasonic treatment unit comprises an ultrasonic device E-6 which is used for mounting and ultrasonic treatment after the filter element is unloaded from the cleaning regeneration tank;

the feed line of the ultrasonic device comprises: a solvent feed line P-11, a solvent feed line P-8, a feed line P-12, and a dry gas feed line P-13;

the discharge line of the ultrasonic device comprises: a wastewater discharge line P-14, a solvent discharge line P-9 and a solvent discharge line P-10;

the solvent circulating pump E-5 is arranged between the composite solvent feeding pipeline P-4 and the solvent discharging pipeline P-10 and is communicated with a discharging hole of the cleaning regeneration tank and the solvent feeding pipeline P-11;

the solvent discharge pipeline P-9 is communicated with the composite solvent storage tank E-1,

the dry gas feed line P-13 is connected to a complex solvent pump E-2.

Preferably, the method comprises:

the Fischer-Tropsch synthesis filter pipe E-4 to be regenerated is arranged in a cleaning regeneration tank E-3, water vapor with the temperature of 300 ℃ of 120-;

closing valves of a steam inlet pipe P-2 and a steam outlet pipe P-15, starting a composite solvent pump E-2, pumping the composite solvent in a composite solvent storage tank E-1 into a cleaning regeneration tank along a pipeline P-1 to enable the composite solvent to overflow a filter pipe to be regenerated, soaking the filter pipe to be regenerated in the composite solvent for 0.5-10h at the normal temperature of-100 ℃, and enabling a catalyst blocked in the filter pipe to react with the composite solvent to dissolve catalyst particles;

starting a composite solvent circulating pump E-5, circulating the composite solvent in the cleaning regeneration tank for 0.5-10h along a pipeline P-4, wherein in the circulation process of the composite solvent, the composite solvent flows to the outer side of the filter pipe from the pores penetrating through the filter pipe in the filter pipe, and the catalyst particles dissolved by the composite solvent are partially carried out;

then the composite solvent in the cleaning regeneration tank is put into a composite solvent storage tank E-1 through a pipeline P-6, clear water is introduced from a pipeline P-3 to flush the residual composite solvent in the filter pipe, the flushing water is discharged out of the cleaning regeneration tank through a pipeline P-7, and the regenerated filter pipe is discharged from the cleaning regeneration tank for later use.

The filter pipe is detached from the cleaning regeneration tank E-3 and then is installed in an ultrasonic device E-6, firstly, a compound solvent pump E-2 is started, the compound solvent in a compound solvent storage tank is pumped into the ultrasonic device E-6 along a pipeline P-8, so that the compound solvent is submerged in the filter pipe to be regenerated, a switch of the ultrasonic device E-6 is turned on at a proper temperature, and ultrasonic treatment is carried out for 1-10 hours;

starting a composite solvent circulating pump E-5, and circulating the composite solvent in the cleaning regeneration tank along pipelines P-10 and P-11; after the ultrasonic treatment is finished, putting the composite solvent in the cleaning regeneration tank into a composite solvent storage tank through a pipeline P-9, introducing clear water from a pipeline P-12, and stopping water washing when the pH value of the clear water discharged from the cleaning regeneration tank is 7-8;

hot air is introduced through the line P-13 to blow the filter tubes dry, and the regenerated filter tubes are discharged from the cleaning regeneration tank for later use.

According to the invention, preferably the method further comprises: and (4) drying the filter element treated in the step (4).

According to the invention, the filter element to be regenerated refers to a filter element which is discharged from a slurry bed Fischer-Tropsch synthesis catalyst and a heavy synthetic oil filter and blocks the internal filter holes due to fine catalyst particles.

According to the invention, the catalyst commonly used in slurry bed Fischer-Tropsch synthesis is an iron-based catalyst and a cobalt-based catalyst, the main components of the iron-based catalyst are iron, copper, potassium and silicon, the cobalt-based catalyst is metal cobalt loaded on an alumina or silica carrier, the slurry bed Fischer-Tropsch synthesis generally adopts a filtration method to realize the filtration and separation of a Fischer-Tropsch synthesis heavy product and the catalyst, and the commonly used filter element is a stainless steel wire mesh sintered pipe or a stainless steel powder sintered pipe. During the filtering process, a filter cake is gradually formed on the slurry side, the filtering pressure drop is gradually increased, and the back washing of the cleaning solution is periodically adopted. However, in the long-term use process, the catalyst fine powder gradually enters the inside of the pore channel of the filter element and is clamped in the pore channel of the filter element, and the fine powder cannot be washed out during backwashing, so that the filter element is blocked.

The present invention provides a regeneration method for regeneration of a filter element. The process of the present invention is described in detail below with reference to the accompanying drawings.

According to a preferred embodiment of the present invention, the process of the Fischer-Tropsch synthesis filter element regeneration method provided by the present invention is shown in FIG. 1. The Fischer-Tropsch synthesis filter pipe E-4 to be regenerated is installed in a cleaning regeneration tank E-3, water vapor with the temperature of 300 ℃ is introduced from a steam inlet pipe P-2 at the top of the cleaning regeneration tank, the water vapor enters the inside of the filter pipe and passes through the pores of the filter pipe, and Fischer-Tropsch synthesis heavy oil remaining in the filter pipe is blown out and discharged from a steam outlet pipe P-15 at the bottom of the cleaning regeneration tank.

The valves of the steam inlet pipe P-2 and the steam outlet pipe P-15 are closed. Starting a composite solvent pump E-2, pumping the composite solvent in a composite solvent storage tank E1 into a cleaning regeneration tank along a pipeline P-1 to enable the composite solvent to submerge a filter pipe to be regenerated, soaking the filter pipe to be regenerated in the composite solvent for 0.5-10h at the normal temperature of-100 ℃, and enabling a catalyst blocked in the filter pipe to react with the composite solvent to dissolve catalyst particles.

And starting the composite solvent circulating pump E-5, circulating the composite solvent in the cleaning regeneration tank for 0.5-10h along a pipeline P-4, wherein in the circulation process of the composite solvent, the composite solvent flows to the outer side of the filter pipe from the pores penetrating through the filter pipe in the filter pipe, and the catalyst particles dissolved by the composite solvent are partially carried out.

Then the composite solvent in the cleaning regeneration tank is put into a composite solvent storage tank E-1 through a pipeline P-6, clear water is introduced from a pipeline P-3 to flush the residual composite solvent in the filter pipe, the flushing water is discharged out of the cleaning regeneration tank through a pipeline P-7, and the regenerated filter pipe is discharged from the cleaning regeneration tank for later use.

The filter tube is detached from the cleaning regeneration tank E-3 and then installed in the ultrasonic device E-6. Firstly, starting a compound solvent pump E-2, pumping the compound solvent in a compound solvent storage tank into an ultrasonic device E-6 along a pipeline P-8, enabling the compound solvent to submerge a filter pipe to be regenerated, turning on a switch of the ultrasonic device E-6 at a proper temperature, and carrying out ultrasonic treatment for 1-10 h.

And starting the compound solvent circulating pump E-5, and circulating the compound solvent in the cleaning regeneration tank along the pipelines P-10 and P-11. And after the ultrasonic treatment is finished, putting the composite solvent in the cleaning regeneration tank into a composite solvent storage tank through a pipeline P-9, introducing clean water from a pipeline P-12, and stopping washing when the pH value of the clean water discharged from the cleaning regeneration tank through P14 is 7-8.

Hot air is introduced through the line P-13 to blow the filter tubes dry, and the regenerated filter tubes are discharged from the cleaning regeneration tank for later use.

Example 1

2 filter pipes to be regenerated are arranged in a cleaning regeneration tank, the filter pipes are stainless steel wire mesh sintered pipes, the diameter is 25.4 mm, the length is 1.2 m, and the pore diameter is 15 microns, the 2 filter pipes are used for 1500 hours in a slurry bed Fischer-Tropsch synthesis internal filter using an iron-based Fischer-Tropsch synthesis catalyst, the back washing time interval is shortened to 5 minutes under the filtration pressure drop of 0.1 MPa at most, and the filter flux is 0.08m under the filtration pressure drop of 0.05 MPa³/m²·h。

Introducing 250 ℃ steam from a steam inlet pipe at the top of the cleaning regeneration tank, introducing the steam into the interior of the filter pipe, penetrating through the pores of the filter pipe, blowing out the Fischer-Tropsch synthesis heavy oil remaining in the filter pipe, and discharging from a steam outlet pipe at the bottom of the cleaning regeneration tank. The steam inlet valve and the steam outlet valve were closed after 20 minutes of steam purging. Pumping a composite solvent water solution with the mass fraction of 35% into the cleaning regeneration tank by using a pump to ensure that the composite solvent submerges the filter pipe to be regenerated, and soaking the filter pipe to be regenerated in the composite solvent for 6 hours at the temperature of 60 ℃. And starting the composite solvent circulating pump to circulate the composite solvent in the cleaning regeneration tank, wherein the composite solvent flows to the outer side of the filter pipe from the pores penetrating through the filter pipe in the filter pipe. And (4) emptying the composite solvent in the cleaning regeneration tank after the composite solvent is circulated for 20 minutes. And adding clear water from the top of the cleaning regeneration tank to flush the residual composite solvent in the filter pipe.

The specific weight formula of the composite solvent aqueous solution is as follows: 81% NaOH; 6% fatty alcohol polyoxyethylene ether; 5% NaCl; 8% of 1, 3-propanedione.

The filter tube is removed from the cleaning regeneration tank and installed in the ultrasonic device. Firstly, starting a compound solvent pump E-2, pumping the compound solvent in a compound solvent storage tank into an ultrasonic device along a pipeline to enable the compound solvent to submerge a filter pipe to be regenerated, turning on a switch of the ultrasonic device at 15 ℃, and carrying out ultrasonic treatment for 6 hours. At the same time, the compound solvent circulating pump is started, and the compound solvent in the regeneration tank circulates along the pipeline. And after the ultrasound is finished, putting the composite solvent in the cleaning regeneration tank into a composite solvent storage tank through a pipeline, introducing clean water from the pipeline, and stopping washing when the pH value of the clean water discharged from the cleaning regeneration tank is 7-8. Then hot air is introduced from the pipeline to blow the filter pipe dry, and the regenerated filter pipe is discharged from the cleaning regeneration tank for standby.

Discharging the regenerated filter pipe from the cleaning regeneration tank, installing the filter pipe into a slurry bed Fischer-Tropsch synthesis inner filter using an iron-based Fischer-Tropsch synthesis catalyst, filtering and separating the catalyst and heavy synthetic oil, wherein the back wash time interval is 50 minutes under the filtering pressure drop of 0.1 MPa at most, the filtering flux is 0.46m under the filtering pressure drop of 0.05 MPa³/m²H. Indicating that the regeneration effect is good.

Example 2

3 filter pipes to be regenerated are arranged in a cleaning regeneration tank, the filter pipes are stainless steel wire mesh sintered pipes, the diameter of each filter pipe is 25.4 millimeters, the length of each filter pipe is 1.2 meters, the pore diameter of each filter pipe is 15 micrometers, and the 3 filter pipes use iron-based Fischer-Tropsch synthesisThe catalyst-forming slurry bed Fischer-Tropsch synthesis internal filter is used for 1500 hours, the back washing time interval is shortened to 5 minutes under the filtration pressure drop of 0.1 MPa at most, and the filtration flux is 0.08m under the filtration pressure drop of 0.05 MPa³/m²·h。

Introducing 250 ℃ steam from a steam inlet pipe at the top of the cleaning regeneration tank, introducing the steam into the interior of the filter pipe, penetrating through the pores of the filter pipe, blowing out the Fischer-Tropsch synthesis heavy oil remaining in the filter pipe, and discharging from a steam outlet pipe at the bottom of the cleaning regeneration tank. The steam inlet valve and the steam outlet valve were closed after 20 minutes of steam purging. Pumping a composite solvent water solution with the mass fraction of 35% into the cleaning regeneration tank by using a pump to ensure that the composite solvent submerges the filter pipe to be regenerated, and soaking the filter pipe to be regenerated in the composite solvent for 4 hours at the temperature of 80 ℃. And starting the composite solvent circulating pump to circulate the composite solvent in the cleaning regeneration tank, wherein the composite solvent flows to the outer side of the filter pipe from the pores penetrating through the filter pipe in the filter pipe. And (4) emptying the composite solvent in the cleaning regeneration tank after the composite solvent is circulated for 30 minutes. And adding clear water from the top of the cleaning regeneration tank to flush the residual composite solvent in the filter pipe.

The concrete formula of the composite solvent water solution is as follows: 88% K₂CO₃(ii) a 6% anionic polyacrylamide; 2% KCl; 4% polyphosphate.

The filter tube is removed from the cleaning regeneration tank and installed in the ultrasonic device. Firstly, starting a composite solvent pump E-2, pumping the composite solvent in a composite solvent storage tank into an ultrasonic device along a pipeline to enable the composite solvent to submerge a filter pipe to be regenerated, turning on a switch of the ultrasonic device at 90 ℃, and carrying out ultrasonic treatment for 4 hours. At the same time, the compound solvent circulating pump is started, and the compound solvent in the regeneration tank circulates along the pipeline. And after the ultrasound is finished, putting the composite solvent in the cleaning regeneration tank into a composite solvent storage tank through a pipeline, introducing clean water from the pipeline, and stopping washing when the pH value of the clean water discharged from the cleaning regeneration tank is 7-8. Then hot air is introduced from the pipeline to blow the filter pipe dry, and the regenerated filter pipe is discharged from the cleaning regeneration tank for standby.

Discharging the regenerated filter pipe from the cleaning regeneration tank, and mountingFiltering and separating the catalyst and heavy synthetic oil in a slurry bed Fischer-Tropsch synthesis inner filter using an iron-based Fischer-Tropsch synthesis catalyst, wherein the back washing time interval is 50 minutes under the filtering pressure drop of 0.1 MPa at most, and the filtering flux is 0.43m under the filtering pressure drop of 0.05 MPa³/m²H. Indicating that the regeneration effect is good.

Example 3

3 filter pipes to be regenerated are arranged in a cleaning regeneration tank, the filter pipes are stainless steel wire mesh sintered pipes, the diameter is 25.4 mm, the length is 1.2 m, and the pore diameter is 15 microns, the 3 filter pipes are used for 1500 hours in a slurry bed Fischer-Tropsch synthesis internal filter using an iron-based Fischer-Tropsch synthesis catalyst, the back washing time interval is shortened to 5 minutes under the filtration pressure drop of 0.1 MPa at most, and the filter flux is 0.08m under the filtration pressure drop of 0.05 MPa³/m²·h。

Introducing 250 ℃ steam from a steam inlet pipe at the top of the cleaning regeneration tank, introducing the steam into the interior of the filter pipe, penetrating through the pores of the filter pipe, blowing out the Fischer-Tropsch synthesis heavy oil remaining in the filter pipe, and discharging from a steam outlet pipe at the bottom of the cleaning regeneration tank. The steam inlet valve and the steam outlet valve were closed after 20 minutes of steam purging. Pumping a composite solvent water solution with the mass fraction of 35% into the cleaning regeneration tank by using a pump to ensure that the composite solvent submerges the filter pipe to be regenerated, and soaking the filter pipe to be regenerated in the composite solvent for 6 hours at 50 ℃. And starting the composite solvent circulating pump to circulate the composite solvent in the cleaning regeneration tank, wherein the composite solvent flows to the outer side of the filter pipe from the pores penetrating through the filter pipe in the filter pipe. And (4) emptying the composite solvent in the cleaning regeneration tank after the composite solvent is circulated for 30 minutes. And adding clear water from the top of the cleaning regeneration tank to flush the residual composite solvent in the filter pipe.

The concrete formula of the composite solvent water solution is as follows: 88% KOH; 3% diethanolamine; 4% KHCO₃(ii) a 7% hydroxycarboxylic acid.

The filter tube is removed from the cleaning regeneration tank and installed in the ultrasonic device. Firstly, starting a composite solvent pump E-2, pumping the composite solvent in a composite solvent storage tank into an ultrasonic device along a pipeline to enable the composite solvent to submerge a filter pipe to be regenerated, turning on a switch of the ultrasonic device at 90 ℃, and carrying out ultrasonic treatment for 4 hours. At the same time, the compound solvent circulating pump is started, and the compound solvent in the regeneration tank circulates along the pipeline. And after the ultrasound is finished, putting the composite solvent in the cleaning regeneration tank into a composite solvent storage tank through a pipeline, introducing clean water from the pipeline, and stopping washing when the pH value of the clean water discharged from the cleaning regeneration tank is 7-8. Then hot air is introduced from the pipeline to blow the filter pipe dry, and the regenerated filter pipe is discharged from the cleaning regeneration tank for standby.

Discharging the regenerated filter pipe from the cleaning regeneration tank, installing the filter pipe into a slurry bed Fischer-Tropsch synthesis inner filter using an iron-based Fischer-Tropsch synthesis catalyst, filtering and separating the catalyst and heavy synthetic oil, wherein the back wash time interval is 50 minutes under the filtering pressure drop of 0.1 MPa at most, the filtering flux is 0.45m under the filtering pressure drop of 0.05 MPa³/m²H. Indicating that the regeneration effect is good.

Comparative example 1

According to the method of the embodiment 3, except that the component of the composite solvent aqueous solution is only NaOH solution, the regenerated filter pipe is discharged from the cleaning regeneration tank and is installed in a slurry bed Fischer-Tropsch synthesis inner filter using an iron-based Fischer-Tropsch synthesis catalyst, the filtration and separation of the catalyst and the heavy synthetic oil are carried out, the back washing time interval is 50 minutes under the filtration pressure drop of 0.1 MPa at most, and the filtration flux is 0.30m under the filtration pressure drop of 0.05 MPa³/m²·h。

The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.