CN109382043A - The in situ regeneration method of Fischer-Tropsch synthesis device filter element and the F- T synthesis system of application in situ regeneration method - Google Patents
The in situ regeneration method of Fischer-Tropsch synthesis device filter element and the F- T synthesis system of application in situ regeneration method Download PDFInfo
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- CN109382043A CN109382043A CN201710666043.7A CN201710666043A CN109382043A CN 109382043 A CN109382043 A CN 109382043A CN 201710666043 A CN201710666043 A CN 201710666043A CN 109382043 A CN109382043 A CN 109382043A
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- filter
- filter element
- lye
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- nitrogen
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- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 81
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 81
- 238000011069 regeneration method Methods 0.000 title claims abstract description 53
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 190
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 96
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 95
- 239000003054 catalyst Substances 0.000 claims abstract description 79
- 239000002002 slurry Substances 0.000 claims abstract description 78
- 238000000034 method Methods 0.000 claims abstract description 38
- 230000008929 regeneration Effects 0.000 claims abstract description 31
- 238000010926 purge Methods 0.000 claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 238000007598 dipping method Methods 0.000 claims abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 271
- 239000003513 alkali Substances 0.000 claims description 50
- 239000002351 wastewater Substances 0.000 claims description 43
- 239000000243 solution Substances 0.000 claims description 24
- 238000003860 storage Methods 0.000 claims description 16
- 238000011010 flushing procedure Methods 0.000 claims description 13
- 238000007654 immersion Methods 0.000 claims description 10
- 238000002347 injection Methods 0.000 claims description 10
- 239000007924 injection Substances 0.000 claims description 10
- 229910052783 alkali metal Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 3
- 150000001340 alkali metals Chemical class 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 2
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- -1 alkali metal acid carbonate Chemical class 0.000 claims 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 238000001914 filtration Methods 0.000 description 51
- 239000003921 oil Substances 0.000 description 39
- 238000004140 cleaning Methods 0.000 description 12
- 230000004907 flux Effects 0.000 description 11
- 239000007788 liquid Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 238000011001 backwashing Methods 0.000 description 6
- 239000002585 base Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 239000008187 granular material Substances 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 238000010025 steaming Methods 0.000 description 3
- 239000006188 syrup Substances 0.000 description 3
- 235000020357 syrup Nutrition 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000012263 liquid product Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/005—Separating solid material from the gas/liquid stream
- B01J8/006—Separating solid material from the gas/liquid stream by filtration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/11—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with bag, cage, hose, tube, sleeve or like filtering elements
- B01D29/31—Self-supporting filtering elements
- B01D29/33—Self-supporting filtering elements arranged for inward flow filtration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/50—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with multiple filtering elements, characterised by their mutual disposition
- B01D29/52—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with multiple filtering elements, characterised by their mutual disposition in parallel connection
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/62—Regenerating the filter material in the filter
- B01D29/66—Regenerating the filter material in the filter by flushing, e.g. counter-current air-bumps
- B01D29/68—Regenerating the filter material in the filter by flushing, e.g. counter-current air-bumps with backwash arms, shoes or nozzles
- B01D29/688—Regenerating the filter material in the filter by flushing, e.g. counter-current air-bumps with backwash arms, shoes or nozzles with backwash arms or shoes acting on the cake side
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/20—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium
- B01J8/22—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid
- B01J8/224—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid the particles being subject to a circulatory movement
- B01J8/228—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid the particles being subject to a circulatory movement externally, i.e. the particles leaving the vessel and subsequently re-entering it
-
- 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
- C10G2/00—Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon
- C10G2/30—Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon from carbon monoxide with hydrogen
- C10G2/32—Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon from carbon monoxide with hydrogen with the use of catalysts
- C10G2/34—Apparatus, reactors
- C10G2/342—Apparatus, reactors with moving solid catalysts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2201/00—Details relating to filtering apparatus
- B01D2201/08—Regeneration of the filter
- B01D2201/085—Regeneration of the filter using another chemical than the liquid to be filtered
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2201/00—Details relating to filtering apparatus
- B01D2201/08—Regeneration of the filter
- B01D2201/087—Regeneration of the filter using gas bubbles, e.g. air
Abstract
The present invention relates to Fischer-Tropsch synthesis device filter element regeneration fields, disclose the in situ regeneration method of Fischer-Tropsch synthesis device filter element and the F- T synthesis system of application in situ regeneration method.This method comprises: (1) empties the catalyst slurry in the external filter being arranged in except Fischer-Tropsch synthesis device under production model, with nitrogen；(2) filter element in external filter is set with water vapor purging, removes remaining synthetic oil in the filter element, obtains filter element to be regenerated；(3) it with dipping by lye and rinses, wash with water the filter element to be regenerated again, obtain regeneration filter element；(4) it is dried up to obtain the external filter of regeneration filter element with hot nitrogen, and external filter pressurization is reached close to the pressure in Fischer-Tropsch synthesis device.The in-situ regeneration for not dismantling the filter element that filter element can be completed in external filter may be implemented.
Description
Technical field
The present invention relates to the regeneration fields of Fischer-Tropsch synthesis device filter element, and in particular to the filtering of Fischer-Tropsch synthesis device
The in situ regeneration method of element and the F- T synthesis system of application in situ regeneration method.
Background technique
It is iron-based and cobalt-base catalyst that syrup state bed Fischer Tropsch, which synthesizes common catalyst,.The main component of ferrum-based catalyst is
Iron, copper, potassium, silicon；Cobalt-base catalyst is that metallic cobalt is supported on aluminium oxide or silica support.In Fischer-Tropsch synthesis process
In, catalyst is tiny particle, it is mixed in solvent and the heavy product of synthesis, thus syrup state bed Fischer Tropsch synthesis will be reacted
Product needs to realize being separated by filtration for F- T synthesis heavy product and catalyst using filtration method.Common filter element is stainless
Steel wire sintered pipes or powder of stainless steel sintered pipes.During the filtration process, catalyst granules can gradually form filter cake in slurries side.
But with continuous deposition filter cake, filtering pressure drop is gradually increased influence filter process, needs periodically to adopt and be rinsed with Cheongju liquid.
CN104606945A discloses a kind of filter core chemically-cleaning device and cleaning method, comprising: by circulation benefit to be cleaned
It is put into and is impregnated in tub with filter core；Water inlet pipe is opened, deionized water is injected to the immersion tub, until flooding described to be cleaned
Recycle filter core predetermined altitude；Chemicals quality control is opened, hydrogen peroxide is injected to the immersion tub, until the immersion tub
Interior hydrogen peroxide reaches predetermined concentration；The filter core to be cleaned that recycles is set to impregnate the predetermined time.This method is only by filter core
It disassembles and is cleaned by way of immersion, cannot be removed effectively the inorganic matter or metal oxidation that catalyst filtration pipe contains
Object.
CN102688724B discloses Fischer-Tropsch wax and catalyst filtration and recoil in a kind of F- T synthesis paste state bed reactor
Method, comprising: 1) under production model, open clear liquid and extract system out, Fischer-Tropsch wax oil is drawn to the waxy stone production for having set pressure
In object surge tank；2) under production model, when back flushing between spacing value when reaching setting value, open backpurge system filter core is carried out it is anti-
Punching；3) when back flushing between when reaching setting value, close the backpurge system, start clear liquid extraction delay；When the clear liquid is extracted out
Delay reaches setting value, opens the clear liquid extraction system, and the Fischer-Tropsch wax oil is drawn to and has set the described thick of pressure
In wax Product Surge Tank.This method provides the method for backwash realize to the filter in F- T synthesis paste state bed reactor into
Row cleaning.But since the hole of screen pipe is not straight hole, after some tiny catalyst granules enter in filtering pore, it is easy card
In hole, it can not be developed when can neither pass through screen pipe, thus backwash, these fine particles are more long-pending in hole
It is more, cause filtering blockage.Therefore there is the particle cleaning that these cannot be stuck in screen pipe in this method actual use
Defect out.
In addition, syrup state bed Fischer Tropsch synthetic catalyst and heavy synthetic oil are separated by filtration mode, interior filtration method can be used,
Outer filtration method can be used.Filter element is mounted in reactor by interior filtration method, and heavy synthetic oil passes through filtering outside screen pipe
Layer enters in pipe, is then out reactor, catalyst stays in reactor.When interior filtration method replacement filter element, need to react
Device parking.Filter element is mounted in the filter outside paste state bed reactor by outer filtration method, catalyst and heavy synthetic oil
Slurries from reactor draw enter external filter.In external filter, heavy synthetic oil passed through outside screen pipe filter layer into
Enter in pipe, be then out filter, remaining catalyst slurry is recirculated back to paste state bed reactor.Outside paste state bed reactor
Two or more external filters can be set, due to there is spare external filter, when outer filtration method replaces filter element, do not need anti-
It answers device to stop, but needs for filter to be isolated from paste state bed reactor system, and need to dismantle filter for filter element
It draws off, replaces with new filter element.Therefore, in order to which outer filtration method more simply and effectively cleans screen pipe, filtering is not removed
Device needs better method.
Summary of the invention
The purpose of the invention is to overcome the cleaning of the outer screen pipe of F- T synthesis paste state bed reactor inconvenient, tiny
Grain cleans halfway problem, provides the in situ regeneration method of Fischer-Tropsch synthesis device filter element and applies in-situ regeneration side
The F- T synthesis system of method, this method can make outer filtration method with disassembly filter is not required to, and screen pipe cleaning effect is more preferable, letter
Just the advantages of.
To achieve the goals above, the first aspect of the present invention provides a kind of original of Fischer-Tropsch synthesis device filter element
Position regeneration method, comprising:
(1) under production model, the catalyst in the external filter except Fischer-Tropsch synthesis device will be set with nitrogen
Slurries are emptied；
(2) filter element in external filter is set with water vapor purging, removes remaining conjunction in the filter element
At oil, filter element to be regenerated is obtained；
(3) it with dipping by lye and rinses, wash with water the filter element to be regenerated again, obtain regeneration filter element；
(4) it is dried up to obtain the external filter of regeneration filter element with hot nitrogen, and external filter pressurization is reached and is connect
Pressure in nearly Fischer-Tropsch synthesis device.
The second aspect of the present invention provides a kind of in-situ regeneration using Fischer-Tropsch synthesis device filter element of the invention
The F- T synthesis system of method, the system include:
Fischer-Tropsch synthesis device E-1, multiple external filter E-2 with multiple filter element E-3, NaOH solution circulating pump E-4,
Alkali liquor storage tank E-5 and lye pump E-6；Wherein,
Multiple external filter E-2 are parallel with one another, and pass through catalyst slurry intake pipeline P-1 and catalyst slurry discharge pipe
Line P-9 is connected with Fischer-Tropsch synthesis device E-1；
Alkali liquor storage tank E-5 is connected to by lye discharge pipe P-8 with the bottom of external filter E-2, and passes through lye pump E-6
Enter the top that pipeline P-6 is connected to external filter E-2 with lye, for realizing immersion of the lye to filter element E-3 is used；
NaOH solution circulating pump E-4 is connected to the bottom of external filter E-2, and passes through lye pipeloop P-7 and external filter E-2
Top connection, for realizing flushing of the lye to filter element E-3 is used；
The nitrogen that outer company is additionally provided at the top of external filter E-2 enters pipeline P-2, water vapour enters pipeline P-3, water into
Enter pipeline P-4 and synthetic oil export pipeline P-5；
The bottom of external filter E-2 is additionally provided with the wastewater discharge pipe line P-10 and nitrogen outlet pipeline P-11 of outer company；
Enter pipeline P-2 by nitrogen, water vapour enters pipeline P-3, water enters pipeline P-4, synthetic oil export pipeline P-
5, wastewater discharge pipe line P-10 and nitrogen outlet pipeline P-11 realizes emptying and drying to external filter E-2, and to mistake
It the water vapor purging of filtering element E-3 and washs with water.
Through the above technical solutions, the external filter of the Fischer-Tropsch synthesis device for slurry bed system, may be implemented not dismantle
The situ cleaning of filter element can be completed in filter element.In method provided by the invention, under production model, in external filter
In the case where online, successively external filter progress catalyst slurry emptied, water vapor purging, then impregnated using lye
And flushing, then wash with water, the small catalyst particles in filter element preferably can be dissolved or be made its fragmentation, thus real
Existing filter element is more cleaned, so that filter element realizes in-situ regeneration.
Detailed description of the invention
Fig. 1 is the schematic diagram of the in situ regeneration method of Fischer-Tropsch synthesis device filter element of the invention.
Description of symbols
E-1 Fischer-Tropsch synthesis device E-2 external filter E-3 filter element
E-4 NaOH solution circulating pump E-5 alkali liquor storage tank E-6 lye pump
P-1 catalyst slurry intake pipeline P-2 nitrogen enters pipeline P-3 water vapour and enters pipeline
P-4 water enters pipeline P-5 synthetic oil export pipeline P-6 lye and enters pipeline
P-7 circulation alkali liquor enters pipeline P-8 lye discharge pipe P-9 catalyst slurry discharge pipe
P-10 wastewater discharge pipe line P-11 nitrogen outlet pipeline
Specific embodiment
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
The first aspect of the present invention provides the in situ regeneration method of Fischer-Tropsch synthesis device filter element E-3 a kind of, such as
Shown in Fig. 1, comprising:
(1) under production model, will be arranged in the external filter E-2 except Fischer-Tropsch synthesis device E-1 with nitrogen
Catalyst slurry is emptied；
(2) the filter element E-3 in external filter E-2 is set with water vapor purging, removes residual in the filter element
The synthetic oil stayed obtains filter element to be regenerated；
(3) it with dipping by lye and rinses, wash with water the filter element to be regenerated again, obtain regeneration filter element；
(4) it is dried up to obtain the external filter of regeneration filter element with hot nitrogen, and external filter pressurization is reached and is connect
Pressure in nearly Fischer-Tropsch synthesis device E-1.
Method provided by the invention is for the filter element in the external filter of the Fischer-Tropsch synthesis device of slurry bed system form
Cleaning and regeneration.In Fischer-Tropsch synthesis device, under the action of the fischer-tropsch synthetic catalyst of fine-powdered, reaction synthesizes synthesis gas
To liquid product, wherein being mixed with catalyst, become catalyst slurry.The catalyst slurry is directed to Fischer-Tropsch synthesis device
Except external filter in, being separated by filtration for liquid product and catalyst is carried out by filter element.After one section of duration of runs, mistake
Filtering element is by the catalyst blockage under filtering.Generally, there are two above external filters for Fischer-Tropsch synthesis device, can use
Method realization of the invention is alternately cleaned, and the production model of F- T synthesis continues to carry out.Side provided by the invention
Method does not need because filter will be cleaned by catalyst granules blocking and stop reacting；Meanwhile each external filter can be each
From the in-situ regeneration for being filtered element, it is also not required to disassembly external filter, the cleaning of filter element can be realized.
In the present invention, refer to that Fischer-Tropsch synthesis device does not stop Fischer-Tropsch synthesis under production model.Only F- T synthesis
One in multiple external filters of reactor connection carries out the in-situ regeneration mode of filter element as shown in Figure 1.Outer filtering
Multiple pipelines are connected on device E-2: catalyst slurry intake pipeline P-1, nitrogen enter pipeline P-2, water vapour enters pipeline P-
3, water enter pipeline P-4, synthetic oil export pipeline P-5, lye enter pipeline P-6, circulation alkali liquor enters pipeline P-7, lye row
Pipeline P-8, catalyst slurry discharge pipe P-9, wastewater discharge pipe line P-10, nitrogen outlet pipeline P-11 out.On above-mentioned pipeline
Controlled valve is all respectively set, controls and inputs or export various objects to external filter by respective lines under different operation step
Material, completes the cleaning of each step.Such as injection point valve is set on catalyst slurry intake pipeline P-1, enter pipe in nitrogen
Nitrogen is arranged on line P-2 to enter valve, enter setting steam entry valve on pipeline P-3 in water vapour, enters pipeline P-4 in water
Synthetic oil outlet valve is arranged on synthetic oil export pipeline P-5, enters on pipeline P-6 in lye and sets for upper setting clear water inlet valve
Alkali liquor inlet valve is set, enters setting circulation alkali liquor inlet valve on pipeline P-7 in circulation alkali liquor, is set on lye discharge pipe P-8
Lye export valve is set, slurry outlet valve is set on catalyst slurry discharge pipe P-9, is arranged on wastewater discharge pipe line P-10
Waste gas outlet valve is arranged in wastewater outlet valve on nitrogen outlet pipeline P-11.
In accordance with the present invention it is preferred that the process emptied described in step (1) includes: the slurries for closing the external filter
Inlet valve and synthetic oil outlet valve, it is with the nitrogen of 3~5MPa that the catalyst slurry indentation slurry bed system in the external filter is anti-
After answering device, stops nitrogen and be passed through and close the slurry outlet valve of the external filter.During being emptied described in progress, only nitrogen
Enter the slurry outlet valve on valve and catalyst slurry discharge pipe P-9 into the nitrogen on pipeline P-2 to open, remaining is respectively managed
Valve on line is to close.After emptying described in completion, slurry outlet valve is closed, and is opened useless on nitrogen outlet pipeline P-11
Pressure in the external filter is down to normal pressure, is then shut off nitrogen and enters valve by gas outlet valve.
In accordance with the present invention it is preferred that the process of water vapor purging described in step (2) includes: to open the external filter
Steam entry valve and wastewater outlet valve, be passed through water vapour in Xiang Suoshu external filter；It is closed after removing remaining synthetic oil
Steam entry valve and wastewater outlet valve；The water vapor purging time is 10~30min, and the temperature of water vapour is 120~200 DEG C.
During carrying out the water vapor purging, only water vapour enters the steam entry valve on pipeline P-3 and the discharge of steam waste water
Wastewater outlet valve on pipeline P-10 is to open, and the valve on remaining each pipeline is to close.After completing the water vapor purging,
Steam entry valve and wastewater outlet valve are also all closed.
In accordance with the present invention it is preferred that the process of dipping by lye described in step (3) includes: to open the external filter
Alkali liquor inlet valve submerges the filter element with lye, and impregnates at 25~150 DEG C the filter element 0.1~for 24 hours.It can
Entered in pipeline P-6 addition external filter E-2 with starting lye pump E-6 for the lye in alkali liquor storage tank by lye, is only opened
Lye enters the alkali liquor inlet valve on pipeline P-6.After the lye being added in the external filter has submerged the filter element,
Stop lye pump E-6, and closes alkali liquor inlet valve.Preferably, dipping by lye temperature is 25~100 DEG C.Soaking time is 0.5
~10h.
In accordance with the present invention it is preferred that the process of flushing described in step (3) includes: starting NaOH solution circulating pump E-4, by alkali
Liquid circulates through the filter element and is backwashed, and lye circulation time is 0.5~2h.During the flushing, only
Starting NaOH solution circulating pump E-4 and circulation alkali liquor enter the circulation alkali liquor inlet valve on pipeline P-7, make to impregnate in external filter E-2
The lye of the filter element can circulate, and lye can use lye at the filter element is continuously fluidly passed through
The hole of the filter element is rinsed, is especially backwashed, i.e., lye, which passes through the direction of the filter element, is
From the interior side of the filter element to the outside of the filter element, this is urged with when carrying out catalyst slurry filtration catalytic agent particle
The flow direction of agent slurries is opposite from the outer side of the filter element to the inside of the filter element.It can be preferably
With the catalyst fine particle deposited in the hole of filter element described in base extraction, regenerated effect is improved.
In accordance with the present invention it is preferred that the lye is selected from the hydroxide of alkali metal, the hydroxide of alkaline-earth metal, alkali
The aqueous solution of the acid carbonate of the carbonate or alkali metal of metal；It is preferred that the lye is sodium hydroxide solution or hydroxide
Potassium solution.
In accordance with the present invention it is preferred that the mass fraction of the lye is 0.5~35 weight %, preferably 2~20 weights
Measure %, more preferably 5~15 weight %；The gauge of the dipping by lye is 0~1MPa, preferably 0~0.3MPa.
In accordance with the present invention it is preferred that the process washed with water described in step (3) includes: to introduce the water into the filtering
Element is rinsed or backwashes, until the pH value of discharge water is 7~8.During the cleaning, water is only entered into pipeline
Wastewater outlet valve on clear water inlet valve and wastewater discharge pipe line P-10 on P-4 is opened, and rinses the external filter with clear water
Inside, remove remaining lye.And determine that stopping is described clear to detect the pH value of discharge water at wastewater discharge pipe line P-10
It washes.
In accordance with the present invention it is preferred that the process of step (4) includes: to be filled with the nitrogen of 90~150 DEG C of 0.1~3MPa
0.5~3h is dried in the external filter.The nitrogen that nitrogen enters on pipeline P-2 only can be entered into valve and nitrogen goes out
Waste gas outlet valve on mouth pipeline P-11 is opened, and the valve on remaining each pipeline is to close.Nitrogen can be exported by measurement
In water content determine the drying for completing the external filter.
The second aspect of the present invention provides a kind of in-situ regeneration using Fischer-Tropsch synthesis device filter element of the invention
The F- T synthesis system of method, the system include:
Fischer-Tropsch synthesis device E-1, multiple external filter E-2 with multiple filter element E-3, NaOH solution circulating pump E-4,
Alkali liquor storage tank E-5 and lye pump E-6；Wherein,
Multiple external filter E-2 are parallel with one another, and pass through catalyst slurry intake pipeline P-1 and catalyst slurry discharge pipe
Line P-9 is connected with Fischer-Tropsch synthesis device E-1；
Alkali liquor storage tank E-5 is connected to by lye discharge pipe P-8 with the bottom of external filter E-2, and passes through lye pump E-6
Enter the top that pipeline P-6 is connected to external filter E-2 with lye, for realizing immersion of the lye to filter element E-3 is used；
NaOH solution circulating pump E-4 is connected to the bottom of external filter E-2, and passes through lye pipeloop P-7 and external filter E-2
Top connection, for realizing flushing of the lye to filter element E-3 is used；
The nitrogen that outer company is additionally provided at the top of external filter E-2 enters pipeline P-2, water vapour enters pipeline P-3, water into
Enter pipeline P-4 and synthetic oil export pipeline P-5；
The bottom of external filter E-2 is additionally provided with the wastewater discharge pipe line P-10 and nitrogen outlet pipeline P-11 of outer company；
Enter pipeline P-2 by nitrogen, water vapour enters pipeline P-3, water enters pipeline P-4, synthetic oil export pipeline P-
5, wastewater discharge pipe line P-10 and nitrogen outlet pipeline P-11 realizes emptying and drying to external filter E-2, and to mistake
It the water vapor purging of filtering element E-3 and washs with water.
According to the present invention, Fischer-Tropsch synthesis device may include external filter described at least two, alternately in situ again
It is raw.It can guarantee being carried out continuously for Fischer-Tropsch synthetic reaction process, not need to stop reactor, also do not need to dismantle the outer filtering
Device is filtered the cleaning of element.
In the present invention, regenerated effect can be determined by measuring the filtration flux (Q) of the filter element.Specific method
It can be with are as follows: for the filter element of known filter area (S), in 200~250 DEG C of temperature, filter the condition of pressure drop 0.05MPa
Under, carry out the filter operation of synthetic oil catalyst slurries, the synthesis oil volume (V) that metering certain time (t) filters out, under
Formula obtains filtration flux (Q):
According to Fig. 1, the implementation process of method provided by the invention be can be such that
It is defeated by catalyst slurry that the catalyst slurry that Fischer-Tropsch synthesis obtains is carried out in Fischer-Tropsch synthesis device E-1
Enter pipeline P-1 to convey into external filter E-2, be passed through from filter element E-3, the catalyst granules isolated is in the outer of filter element
Side obtains synthetic oil on the inside of filter element and is discharged from synthetic oil export pipeline P-5.After a period of time, filter element E-3
Filtration flux decline, needs to regenerate, and the catalyst slurry conversion of Fischer-Tropsch synthesis device E-1 discharge is output to other outer mistake
Filter, external filter to be regenerated start to carry out in-situ regeneration.
Fischer-Tropsch synthesis device E-1 is closed on the catalyst slurry pipeline P-1 of external filter E-2 conveying catalyst slurry
Injection point valve, close external filter E-2 synthetic oil export pipeline P-5 on synthetic oil outlet valve；Nitrogen is opened to enter
Nitrogen on pipeline P-2 enters valve, the nitrogen of 3~5MPa is introduced into external filter E-2, by urging in external filter E-2
Agent slurries are pressed into Fischer-Tropsch synthesis device E-1 by catalyst slurry discharge pipe P-9, empty urging in external filter E-2
Agent slurries close the slurry outlet valve on catalyst slurry discharge pipe P-9；It closes nitrogen and enters valve, open nitrogen and go out
Nitrogen outlet valve on mouth pipeline P-11, is down to normal pressure for the pressure of external filter, and close nitrogen outlet valve.
It opens water vapour and enters the steam inlet valve on pipeline P-3,120~200 DEG C of water is passed through into external filter E-2
Steam, water vapour pass through the hole on filter element, synthetic oil remaining in filter element are blown out, from wastewater discharge pipe P-10
Discharge；Steam off inlet valve and wastewater outlet valve after 10~30min of water vapor purging.
It opens lye and enters the alkali liquor inlet valve on pipeline P-6, start lye pump E-6, by the alkali in alkali liquor storage tank E-5
Liquid is squeezed into external filter E-2, and lye is made to submerge filter element E-3, stops lye pump E-6, closes alkali liquor inlet valve, incited somebody to action
Filtering element E-3 impregnates 0.1-24h at 25~150 DEG C in lye, is destroyed in the hole of filter element E-3 and is blocked using lye
Catalyst.
The circulation alkali liquor inlet valve on lye pipeloop P-7 is opened, starts NaOH solution circulating pump E-4, by external filter E-2
In lye recycled, in lye cyclic process, keep lye outer from the inside of filter element E-3 to filter element E-3
Side passes through the hole of filter element E-3, and being backwashed will be taken out of by the catalyst granules that lye destroys in hole, thus real
Existing screen pipe regeneration；Lye circulation time is 0.5~2h, stops NaOH solution circulating pump E-4, closes circulation alkali liquor inlet valve.
The lye export valve on lye discharge pipe P-8 is opened, the lye in external filter E-2 is vented to alkali liquor storage tank
In E-5, it is then shut off circulation alkali liquor inlet valve.
It opens water and enters the clear water inlet valve on pipeline P-4 and introduce clear water to external filter E-2, it is residual in washing and filtering element
Remaining lye；Open wastewater discharge pipe line P-10 on wastewater outlet valve flushing water is discharged, until discharge water pH value be 7~
8 close clear water inlet valve and wastewater outlet valve.
The nitrogen outlet valve that the nitrogen that nitrogen enters on pipeline P-2 enters on valve and nitrogen outlet pipeline P-11 is opened, is drawn
The nitrogen for entering 90~150 DEG C of 0.1~3MPa enters 0.5~3h of external filter E-2 purging and is dried, and completes regeneration.
After completing regeneration, nitrogen outlet valve is closed, external filter is forced into and the pressure in Fischer-Tropsch synthesis device E-1
Power is close, closes nitrogen inlet valve.
Open the slurry on the injection point valve and catalyst slurry discharge pipe P-9 on catalyst slurry intake pipeline P-1
Catalyst slurry is introduced external filter E-2, and opened on the synthetic oil export pipeline P-5 of external filter E-2 by liquid outlet valve
Synthetic oil outlet valve, come into operation external filter E-2.
The present invention will be described in detail by way of examples below.In following embodiment, filtration flux passes throughIt measures.
Embodiment 1
The present embodiment is used to illustrate the in situ regeneration method of F- T synthesis filter element of the invention.
In F- T synthesis system, expense is carried out using iron-base fischer-tropsch synthesis catalyst in slurry bed ft synthetic reactor E-1
Hold in the palm synthetic reaction.It is connected to there are two external filter E-2 with Fischer-Tropsch synthesis device E-1 in system, pacifies in each external filter E-2
2 filter element E-3 are filled, screen pipe E-3 is stainless steel cloth sintered pipes, diameter 25.4mm, length 1.2m, 15 μm of aperture.
Filter element E-3 in one of external filter E-2 uses 1500h, in the filtering pressure drop of highest 0.1MPa
Under, backwashing time interval has shortened to 5min, falls in the filtration pressure of 0.05MPa, filtration flux is down to 0.08m3/m2·h。
External filter E-2 needs are regenerated under production model, as shown in Figure 1.
(1) the injection point valve on catalyst slurry pipeline P-1 is closed, the synthesis on synthetic oil export pipeline P-5 is closed
Oil export valve；It opens the nitrogen that nitrogen enters on pipeline P-2 and enters valve, the nitrogen of 3.2MPa is introduced into external filter, it will
Catalyst slurry in external filter is pressed into Fischer-Tropsch synthesis device E-1 by catalyst slurry discharge pipe P-9；
It closes slurry outlet valve and nitrogen enters valve, open the nitrogen outlet valve on nitrogen outlet pipeline P-11, it will be outer
The pressure of filter is down to normal pressure.
(2) it opens water vapour and enters the wastewater outlet on the steam inlet valve on pipeline P-3 and wastewater discharge pipe line P-10
Valve enters pipeline P-3 through water vapour and carries out purging 20min to the water vapour that external filter E-2 is passed through 150 DEG C, is then shut off steaming
Vapour inlet valve and wastewater outlet valve.
(3) it opens lye and enters the alkali liquor inlet valve on pipeline P-6, start lye pump E-6, it will be in alkali liquor storage tank E-5
Sodium hydroxide solution (concentration is 15 weight %) is squeezed into external filter E-2, so that lye is submerged filter element E-3, is stopped lye
E-6 is pumped, alkali liquor inlet valve, the lower immersion 4h by filter element E-3 at 80 DEG C are closed.
(4) the circulation alkali liquor inlet valve on lye pipeloop P-7 is opened, starts NaOH solution circulating pump E-4, by external filter
Lye in E-2 carries out circulation 30min, stops NaOH solution circulating pump E-4, closes circulation alkali liquor inlet valve；Open lye discharge pipe
Lye export valve on line P-8, the lye in external filter E-2 is vented into alkali liquor storage tank E-5, circulation alkali liquor is then shut off
Inlet valve.
(5) it opens the clear water inlet valve that water enters on pipeline P-4 to be rinsed to external filter E-2 introducing clear water, open
Flushing water is discharged wastewater outlet valve on wastewater discharge pipe line P-10, until closing clear water inlet valve when the pH value of discharge water is 8
With wastewater outlet valve.
(6) nitrogen outlet valve that the nitrogen that nitrogen enters on pipeline P-2 enters on valve and nitrogen outlet pipeline P-11 is opened,
The nitrogen of 90 DEG C of 0.1MPa is entered external filter E-2 purging 3.0h to be dried, completes regeneration.
(7) nitrogen outlet valve is closed, continues to be passed through nitrogen to external filter, when pressure ratio F- T synthesis is anti-in external filter
When answering in device the low 0.3MPa of pressure, nitrogen inlet valve is closed.
(8) it opens on the injection point valve and catalyst slurry discharge pipe P-9 on catalyst slurry intake pipeline P-1
Catalyst slurry is introduced external filter E-2, and opened on the synthetic oil export pipeline P-5 of external filter E-2 by slurry outlet valve
Synthetic oil outlet valve, come into operation external filter E-2.
Filtration pressure of the filter element E-3 in highest 0.1MPa to be detected to fall, backwashing time interval is improved to 70min,
It filters under pressure drop 0.05MPa, filtration flux is improved to 0.47m3/m2·h；Regeneration effect is good.
Embodiment 2
In F- T synthesis system, expense is carried out using iron-base fischer-tropsch synthesis catalyst in slurry bed ft synthetic reactor E-1
Hold in the palm synthetic reaction.It is connected to there are three external filter E-2 with Fischer-Tropsch synthesis device E-1 in system, pacifies in each external filter E-2
2 filter element E-3 are filled, screen pipe E-3 is stainless steel cloth sintered pipes, diameter 25.4mm, length 1.2m, 15 μm of aperture.
Filter element E-3 in one of external filter E-2 uses 1500h, in the filtering pressure drop of highest 0.1MPa
Under, backwashing time interval has shortened to 5min, falls in the filtration pressure of 0.05MPa, filtration flux is down to 0.08m3/m2·h。
External filter E-2 needs are regenerated under production model, as shown in Figure 1.
(1) the injection point valve on catalyst slurry pipeline P-1 is closed, the synthesis on synthetic oil export pipeline P-5 is closed
Oil export valve；It opens the nitrogen that nitrogen enters on pipeline P-2 and enters valve, the nitrogen of 4.0MPa is introduced into external filter, it will
Catalyst slurry in external filter is pressed into Fischer-Tropsch synthesis device E-1 by catalyst slurry discharge pipe P-9；
It closes slurry outlet valve and nitrogen enters valve, open the nitrogen outlet valve on nitrogen outlet pipeline P-11, it will be outer
The pressure of filter is down to normal pressure.
(2) it opens water vapour and enters the wastewater outlet on the steam inlet valve on pipeline P-3 and wastewater discharge pipe line P-10
Valve enters pipeline P-3 through water vapour and carries out purging 10min to the water vapour that external filter E-2 is passed through 200 DEG C, is then shut off steaming
Vapour inlet valve and wastewater outlet valve.
(3) it opens lye and enters the alkali liquor inlet valve on pipeline P-6, start lye pump E-6, it will be in alkali liquor storage tank E-5
Sodium hydroxide solution (concentration is 10 weight %) is squeezed into external filter E-2, so that lye is submerged filter element E-3, is stopped lye
E-6 is pumped, alkali liquor inlet valve, the lower immersion 8h by filter element E-3 at 50 DEG C are closed.
(4) the circulation alkali liquor inlet valve on lye pipeloop P-7 is opened, starts NaOH solution circulating pump E-4, by external filter
Lye in E-2 carries out circulation 100min, stops NaOH solution circulating pump E-4, closes circulation alkali liquor inlet valve；Open lye discharge pipe
Lye export valve on line P-8, the lye in external filter E-2 is vented into alkali liquor storage tank E-5, circulation alkali liquor is then shut off
Inlet valve.
(5) it opens the clear water inlet valve that water enters on pipeline P-4 to be rinsed to external filter E-2 introducing clear water, open
Flushing water is discharged wastewater outlet valve on wastewater discharge pipe line P-10, until closing clear water entrance when the pH value of discharge water is 7.5
Valve and wastewater outlet valve.
(6) nitrogen outlet valve that the nitrogen that nitrogen enters on pipeline P-2 enters on valve and nitrogen outlet pipeline P-11 is opened,
The nitrogen of 150 DEG C of 0.5MPa is entered external filter E-2 purging 0.5h to be dried, completes regeneration.
(7) nitrogen outlet valve is closed, continues to be passed through nitrogen to external filter, when pressure ratio F- T synthesis is anti-in external filter
When answering in device the low 0.3MPa of pressure, nitrogen inlet valve is closed.
(8) it opens on the injection point valve and catalyst slurry discharge pipe P-9 on catalyst slurry intake pipeline P-1
Catalyst slurry is introduced external filter E-2, and opened on the synthetic oil export pipeline P-5 of external filter E-2 by slurry outlet valve
Synthetic oil outlet valve, come into operation external filter E-2.
Filtration pressure of the filter element E-3 in highest 0.1MPa to be detected to fall, backwashing time interval is improved to 80min,
It filters under pressure drop 0.05MPa, filtration flux is improved to 0.50m3/m2·h；Regeneration effect is good.
Embodiment 3
In F- T synthesis system, expense is carried out using iron-base fischer-tropsch synthesis catalyst in slurry bed ft synthetic reactor E-1
Hold in the palm synthetic reaction.It is connected to there are four external filter E-2 with Fischer-Tropsch synthesis device E-1 in system, pacifies in each external filter E-2
2 filter element E-3 are filled, screen pipe E-3 is stainless steel cloth sintered pipes, diameter 25.4mm, length 1.2m, 15 μm of aperture.
Filter element E-3 in one of external filter E-2 uses 1500h, in the filtering pressure drop of highest 0.1MPa
Under, backwashing time interval has shortened to 5min, falls in the filtration pressure of 0.05MPa, filtration flux is down to 0.08m3/m2·h。
External filter E-2 needs are regenerated under production model, as shown in Figure 1.
(1) the injection point valve on catalyst slurry pipeline P-1 is closed, the synthesis on synthetic oil export pipeline P-5 is closed
Oil export valve；It opens the nitrogen that nitrogen enters on pipeline P-2 and enters valve, the nitrogen of 5.0MPa is introduced into external filter, it will
Catalyst slurry in external filter is pressed into Fischer-Tropsch synthesis device E-1 by catalyst slurry discharge pipe P-9；
It closes slurry outlet valve and nitrogen enters valve, open the nitrogen outlet valve on nitrogen outlet pipeline P-11, it will be outer
The pressure of filter is down to normal pressure.
(2) it opens water vapour and enters the wastewater outlet on the steam inlet valve on pipeline P-3 and wastewater discharge pipe line P-10
Valve enters pipeline P-3 through water vapour and carries out purging 30min to the water vapour that external filter E-2 is passed through 120 DEG C, is then shut off steaming
Vapour inlet valve and wastewater outlet valve.
(3) it opens lye and enters the alkali liquor inlet valve on pipeline P-6, start lye pump E-6, it will be in alkali liquor storage tank E-5
Potassium hydroxide solution (concentration is 6 weight %) is squeezed into external filter E-2, so that lye is submerged filter element E-3, is stopped lye pump
E-6 closes alkali liquor inlet valve, the lower immersion 10h by filter element E-3 at 100 DEG C.
(4) the circulation alkali liquor inlet valve on lye pipeloop P-7 is opened, starts NaOH solution circulating pump E-4, by external filter
Lye in E-2 carries out circulation 60min, stops NaOH solution circulating pump E-4, closes circulation alkali liquor inlet valve；Open lye discharge pipe
Lye export valve on line P-8, the lye in external filter E-2 is vented into alkali liquor storage tank E-5, circulation alkali liquor is then shut off
Inlet valve.
(5) it opens the clear water inlet valve that water enters on pipeline P-4 to be rinsed to external filter E-2 introducing clear water, open
Flushing water is discharged wastewater outlet valve on wastewater discharge pipe line P-10, until closing clear water inlet valve when the pH value of discharge water is 7
With wastewater outlet valve.
(6) nitrogen outlet valve that the nitrogen that nitrogen enters on pipeline P-2 enters on valve and nitrogen outlet pipeline P-11 is opened,
The nitrogen of 120 DEG C of 0.3MPa is entered external filter E-2 purging 1.5h to be dried, completes regeneration.
(7) nitrogen outlet valve is closed, continues to be passed through nitrogen to external filter, when pressure ratio F- T synthesis is anti-in external filter
When answering in device the low 0.3MPa of pressure, nitrogen inlet valve is closed.
(8) it opens on the injection point valve and catalyst slurry discharge pipe P-9 on catalyst slurry intake pipeline P-1
Catalyst slurry is introduced external filter E-2, and opened on the synthetic oil export pipeline P-5 of external filter E-2 by slurry outlet valve
Synthetic oil outlet valve, come into operation external filter E-2.
Filtration pressure of the filter element E-3 in highest 0.1MPa to be detected to fall, backwashing time interval is improved to 60min,
It filters under pressure drop 0.05MPa, filtration flux is improved to 0.42m3/m2·h；Regeneration effect is good.
From above-described embodiment as can be seen that using in situ regeneration method provided by the invention, Fischer-Tropsch provided by the invention is closed
Effectively filter element can be cleaned in the case where not dismantling external filter at system, restore the mistake of filter element
Effect is filtered, before filtration flux is compared to regeneration, improves 5.25~6.25 times.
It is described the prefered embodiments of the present invention in detail above in conjunction with attached drawing, still, the present invention is not limited thereto.At this
, can be with various simple variants of the technical solution of the present invention are made in the range of the technology design of invention, including each technical characteristic
It is combined with any other suitable method, these simple variants and combination equally should be considered as in disclosed in this invention
Hold, all belongs to the scope of protection of the present invention.
Claims (10)
1. a kind of in situ regeneration method of Fischer-Tropsch synthesis device filter element, comprising:
(1) under production model, the catalyst slurry in the external filter except Fischer-Tropsch synthesis device will be set with nitrogen
It is emptied；
(2) filter element in external filter is set with water vapor purging, removes remaining synthetic oil in the filter element,
Obtain filter element to be regenerated；
(3) it with dipping by lye and rinses, wash with water the filter element to be regenerated again, obtain regeneration filter element；
(4) it is dried up to obtain the external filter of regeneration filter element with hot nitrogen, and external filter pressurization is reached close to expense
Hold in the palm the pressure in synthesis reactor.
2. regeneration method according to claim 1, wherein the process emptied described in step (1) includes: to close outside described
The injection point valve and synthetic oil outlet valve of filter, with the nitrogen of 3~5MPa by the catalyst slurry in the external filter
After being pressed into paste state bed reactor, stops nitrogen and be passed through and close the slurry outlet valve of the external filter.
3. regeneration method according to claim 1, wherein the process of water vapor purging described in step (2) includes: to open
The steam entry valve and wastewater outlet valve of the external filter are passed through water vapour in Xiang Suoshu external filter；It removes remaining
Steam entry valve and wastewater outlet valve are closed after synthetic oil；The water vapor purging time is 10~30min, and the temperature of water vapour is
120~200 DEG C.
4. regeneration method according to claim 1, wherein the process of dipping by lye described in step (3) includes: to open institute
The alkali liquor inlet valve for stating external filter submerges the filter element with lye, and impregnates the filter element at 25~150 DEG C
0.1~for 24 hours.
5. regeneration method according to claim 1, wherein the process of flushing described in step (3) includes: that starting lye follows
Ring pump, circulates through the filter element for lye and backwashes, and lye circulation time is 0.5~2h.
6. according to claim 1, regeneration method described in any one of 4 and 5, wherein the lye is selected from the hydrogen of alkali metal
Oxide, the hydroxide of alkaline-earth metal, the carbonate of alkali metal or alkali metal acid carbonate aqueous solution；It is preferred that institute
Stating lye is sodium hydroxide solution or potassium hydroxide solution.
7. regeneration method according to claim 6, wherein the mass fraction of the lye is 0.5~35 weight %, preferably
For 2~20 weight %, more preferably 5~15 weight %；The gauge of the dipping by lye be 0~1MPa, preferably 0~
0.3MPa。
8. regeneration method according to claim 1, wherein the process washed with water described in step (3) includes: to draw water
Enter and the filter element is rinsed or is backwashed, until the pH value of discharge water is 7~8.
9. regeneration method according to claim 1, wherein the process of step (4) include: by the 0.1 of 90~150 DEG C~
The nitrogen of 3MPa is filled with 0.5~3h in the external filter and is dried.
10. a kind of in-situ regeneration side using Fischer-Tropsch synthesis device filter element described in any one of claim 1-9
The F- T synthesis system of method, the system include:
Fischer-Tropsch synthesis device (E-1), multiple external filters (E-2), the NaOH solution circulating pump for having multiple filter elements (E-3)
(E-4), alkali liquor storage tank (E-5) and lye pump (E-6)；Wherein,
Multiple external filters (E-2) are parallel with one another, and pass through catalyst slurry intake pipeline (P-1) and catalyst slurry discharge pipe
Line (P-9) is connected with Fischer-Tropsch synthesis device (E-1)；
Alkali liquor storage tank (E-5) is connected to by lye discharge pipe (P-8) with the bottom of external filter (E-2), and passes through lye pump
(E-6) and lye enters the top that pipeline (P-6) is connected to external filter (E-2), for realizing use lye to filter element
(E-3) immersion；
NaOH solution circulating pump (E-4) is connected to the bottom of external filter (E-2), and passes through lye pipeloop (P-7) and external filter
(E-2) top connection, for realizing flushing of the lye to filter element (E-3) is used；
The nitrogen that outer company is additionally provided at the top of external filter (E-2) enters pipeline (P-2), water vapour enters pipeline (P-3), water
Into pipeline (P-4) and synthetic oil export pipeline (P-5)；
The bottom of external filter (E-2) is additionally provided with the wastewater discharge pipe line (P-10) and nitrogen outlet pipeline (P-11) of outer company；
Enter pipeline (P-2) by nitrogen, water vapour enters pipeline (P-3), water enters pipeline (P-4), synthetic oil export pipeline
(P-5), wastewater discharge pipe line (P-10) and nitrogen outlet pipeline (P-11) realize emptying and drying to external filter (E-2),
And it to the water vapor purging of filter element (E-3) and washs with water.
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| CN113731023A (en) * | 2020-05-27 | 2021-12-03 | 国家能源投资集团有限责任公司 | Regeneration method of Fischer-Tropsch synthesis filter element |
| CN113926244A (en) * | 2021-10-09 | 2022-01-14 | 上海卫星装备研究所 | Combined liquid nitrogen pump inlet filtering and online regenerating device and using method |
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Application publication date: 20190226 |