CN102435463A - Online acquisition system and method for catalyst slurry - Google Patents
Online acquisition system and method for catalyst slurry Download PDFInfo
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- CN102435463A CN102435463A CN2011103385619A CN201110338561A CN102435463A CN 102435463 A CN102435463 A CN 102435463A CN 2011103385619 A CN2011103385619 A CN 2011103385619A CN 201110338561 A CN201110338561 A CN 201110338561A CN 102435463 A CN102435463 A CN 102435463A
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Abstract
The invention relates to an online acquisition system and an online acquisition method for catalyst slurry. The online acquisition system for the catalyst slurry comprises (A) a sampling system, and (B) an inert medium injection system, wherein the sampling system comprises a first sampling pipeline (14), a second sampling pipeline (16) and a catalyst slurry collecting container (11); the first end of the first sampling pipeline (14) extends into a slurry reactor (8); the first sampling pipeline (14) is provided with a first valve (6); the second end of the second sampling pipeline (16) is connected to the second end of the first sampling pipeline; the second sampling pipeline (16) is provided with a second valve (7) and a third valve (10); the catalyst slurry collecting container (11) is connected to the first end of the second sampling pipeline (16); the inert medium injection system comprises an inert liquid medium supply device (1) and a fourth pipeline (12); and the inert liquid medium supply device (1) is connected to the second ends of the first sampling pipeline (14) and the second sampling pipeline (16). The system can easily acquire catalyst slurry on line.
Description
Technical field
The present invention relates to a kind of catalyst slurry on-line acquisition system and method, relate in particular to catalyst slurry on-line acquisition system and method in the Fischer-Tropsch synthetic pulp state bed reactor.
Background technology
Fischer-Tropsch is synthetic to be meant under certain conditions synthetic gas CO and H
2The reaction of synthetic hydrocarbon under the effect of catalyzer.From the 1950's, Sasol company has realized coal-based synthetic liquid fuel heavy industrialization (Dry, M.E., Catalysis Today, 1990,6 (3) 183-206) in South Africa.What Fischer-Tropsch synthesized normal employing is cobalt-base catalyst and ferrum-based catalyst, and the reactor of employing has fixed bed reactors, flowing bed reactor and paste state bed reactor.Cobalt-base catalyst is applicable to more that based on to the hydrogen-carbon ratio requirement in the synthetic gas rock gas is that the Fischer-Tropsch that synthesizes source of the gas synthesizes.Ferrum-based catalyst all can use for the fischer-tropsch reaction that synthesizes source of the gas rock gas or coal owing to possess the water-gas shift activity.Because paste state bed reactor has higher production efficiency, catalyzer is easy to load and unload and can directly be used for the lower coal based synthetic gas of hydrogen-carbon ratio, demonstrates bigger advantage, be the synthetic liquid fuel technology of giving priority to both at home and abroad at present.
The ferrum-based catalyst that is used for paste state bed reactor must possess certain particle size and wear strength, could in the fischer-tropsch reaction process, keep certain stability to separate with one-tenth wax with being beneficial to the main reaction product.In recent years; Most research work all concentrates on the prescription and the technology of preparing of catalyzer; The preparation method of syrup state bed Fischer Tropsch synthesis iron base catalyst is disclosed in patent WO99/49965 like South Africa Sasol company; Group of Shenhua discloses the formulation adjuvant research and the fabricating technology research of slurry attitude bed catalyst ferrum-based catalyst in patents such as CN101293206B, CN101298046A and CN101884926A, the purpose of these researchs all is for improving the abrasion resistance of catalyzer.Simultaneously; With regard to ferrum-based catalyst activating process and technique for applying in slurry attitude bed; Also done a large amount of work both at home and abroad, disclose the activating process parameter to Effect on Performance such as the oily space-time yield of catalyzer, deactivation rates like one Chinese patent application CN1583274, CN101796166A and CN10189206A etc.
But very complicated variation until inactivation, has all taken place from appearance, size and phase from reduction, reaction in ferrum-based catalyst in paste state bed reactor.Therefore will improve catalyzer resistance to abrasion and stability in slurry attitude bed, must gather the catalyzer in the course of reaction, the physicochemical property of following the tracks of catalyzer changes.And in the research work both at home and abroad, little report Fischer-Tropsch synthetic pulp attitude bed catalyst method of sampling and system.
The patent No. is that the Chinese patent that the name of ZL90214227.5 (CN2072151U) is called " a kind of high temperature, high-pressure sampling container " discloses a kind of sampling equipment that can be used for high temperature, high pressure and deep well sampling; But this sampling equipment only is applicable to the steam sampling of high temperature, high pressure and deep well, does not contain solid particle in its appearance of getting, and can not cause wearing and tearing to sampler; And it is simple in structure; Therefore, in the syrup state bed Fischer Tropsch synthetic reaction process, can't take a sample with said sampling container.
The Chinese patent that the name of number of patent application 96193860.9 (CN1184529A) is called " sampling method and device " discloses the method and apparatus of taking a sample in the streaming suspension of a kind of polymer beads from olefinic polymerization and hydrocarbon diluent formation; But this method only is applicable to the situation that temperature and pressure is lower; Be not suitable for the situation of the synthetic middle temperature of Fischer-Tropsch, middle pressure; Therefore; In the syrup state bed Fischer Tropsch synthetic reaction process, can't carry out the sampling of catalyst slurry with said sampling method and system equally.
Therefore, need a kind of in the syrup state bed Fischer Tropsch synthetic reaction process online method and system of carrying out the sampling of catalyst slurry.
Summary of the invention
The present invention relates to a kind of catalyst slurry on-line acquisition system, wherein catalyst slurry is contained in the paste state bed reactor (8), comprising:
(A) sampling system comprises:
(A1) the first sampling pipeline has first end and second end, and first end of the first sampling pipeline extend into slurry attitude bed
In the reactor, wherein, the first sampling pipeline is provided with first valve;
(A2) the second sampling pipeline has first end and second end, and second end of the second sampling pipeline is connected to first and adopts
Second end of appearance pipeline; Wherein, be provided with second valve, first of the second sampling pipeline at the second end place of the second sampling pipeline
The end place is provided with the 3rd valve;
(A3) catalyst slurry collection container, be connected to second the sampling pipeline first end;
(B) inert media injected system comprises:
(B1) inertia liquid medium feeding mechanism; With
(B2) the 4th pipeline is connected to second end of the first sampling pipeline and second end of the second sampling pipeline with inertia liquid medium feeding mechanism, and wherein the 4th pipeline is provided with the 4th valve.
Preferably, (A) sampling system further comprises: (A4) pressure monitoring device is connected on the sampling of second between second valve and the 3rd valve pipeline through the 3rd pipeline.
Preferably, be provided with the U-shaped pipe in the 3rd pipeline, fill the inertia liquid medium in the U-shaped pipe.
Preferably, the inert media injected system further comprises: (B3) pump is arranged between the 4th valve and the inertia liquid medium feeding mechanism.
Preferably, (B) the inert media injected system further comprises: (B4) pressure monitoring device is arranged between pump and the 4th valve.
Preferably, the catalyst slurry on-line acquisition system further comprises:
(C) purging system comprises:
(C1) inert blowing gas sweeping device, through the 5th pipeline be connected to second the sampling pipeline second end;
(C2) the 5th valve is arranged on the 5th pipeline.
Preferably, (A) pipeline and the valve in the sampling system is wear-resistant pipeline and wear-resistant valve.
Preferably, (B) pressure monitoring device in the inert media injected system is a tensimeter with pressure monitoring device in (A) sampling system.
Preferably, (A) in sampling system, (B) inert media injected system the outer pipeline of paste state bed reactor be provided with heating arrangement or accompany thermic devices with valve.
Preferably, paste state bed reactor is a Fischer-Tropsch synthetic pulp state bed reactor; Inertia liquid medium feeding mechanism is a liquid wax feeding mechanism.
The invention still further relates to a kind of catalyst slurry online acquisition method, carry out through system of the present invention, this method comprises:
(a) close the 3rd valve, open first valve and second valve, make catalyst slurry in the paste state bed reactor get into (A1) the first sampling pipeline and (A2) the second sampling pipeline;
(b) close second valve, open the 3rd valve, catalyst slurry is collected in (A3) catalyst slurry collection container;
Alternatively, (c) repeating step (a) to (b).
Preferably, reaction medium or the product in inertia liquid medium and the paste state bed reactor is identical.
Preferably, the pressure in the paste state bed reactor is greater than external environment condition pressure, and preferably, with respect to external environment condition pressure, the pressure in the paste state bed reactor is 0.4-3.5MPa, is preferably 0.5-3.0MPa.
Preferably, temperature is 200～320 ℃ in the paste state bed reactor, preferred 200-300 ℃, and more preferably 235～275 ℃.
Preferably, further comprise: in step (a) before, (a ') is injected in the paste state bed reactor the first end preset distance H that in paste state bed reactor liquid level is higher than the first sampling pipeline through (B) inert media injected system with inert media.
Preferably, when system has heating arrangement or companion during thermic devices, the heating-up temperature of heating arrangement or companion's thermic devices or to accompany hot temperature be 100～200 ℃.
Preferably, this method further comprises: (d) cleaning step: in the first sampling pipeline and the second sampling pipeline, inject the inertia liquid medium through (B) inert media injected system, clean.
Preferably, when the catalyst slurry on-line acquisition system comprised (C) purging system, this method further comprised: (e) purge step: through purging system the second sampling pipeline (is purged.
Preferably, the mode of collection catalyst slurry is a batch (-type).
Preferably, catalyst slurry online acquisition method is the catalyst slurry online acquisition method in fischer-tropsch synthetic catalyst reduction phase or Fischer-Tropsch synthesis stage.
This system is the catalyst slurry in the online acquisition paste state bed reactor easily.
Description of drawings
Fig. 1 is the synoptic diagram of a kind of preferred implementation of sampling system of the present invention.
Embodiment
In the present invention, under the situation of not contradiction or conflict, all embodiment of the present invention, embodiment and characteristic can make up each other.
In the present invention, conventional unit, parts etc. both can be purchased, also can be according to content self-control disclosed by the invention.
In the present invention, for outstanding emphasis of the present invention, the omission that some conventional operations and unit, parts are carried out, or only do simple description.
In the present invention, " with ... link to each other " or " being connected to " or " connections ", both can be that the two directly links to each other, also can across common parts or device (for example valve, pump, heat interchanger etc.) links to each other or connection.
In the present invention, term " on-line acquisition system " is meant the system that equipment is gathered under the situation of operation, for example under the situation of ordinary production, like fischer-tropsch synthetic catalyst reduction phase or Fischer-Tropsch synthesis stage.
One aspect of the present invention relates to the catalyst slurry on-line acquisition system in the paste state bed reactor, and this system comprises:
(A) sampling system comprises:
(A1) the first sampling pipeline has first end and second end, and first end of the first sampling pipeline extend in the paste state bed reactor, and wherein, the first sampling pipeline is provided with first valve;
(A2) the second sampling pipeline has first end and second end, and second end of the second sampling pipeline is connected to second end of the first sampling pipeline; Wherein, be provided with second valve at the second end place of the second sampling pipeline, the first end place of the second sampling pipeline is provided with the 3rd valve;
(A3) catalyst slurry collection container, be connected to second the sampling pipeline first end.
Preferably, sampling system further comprises: (A4) pressure monitoring device is connected to the second sampling pipeline between second valve and the 3rd valve through the 3rd pipeline.Preferably, (A4) pressure monitoring device is a tensimeter.
Preferably, be provided with the U-shaped pipe in the 3rd pipeline, fill the inertia liquid medium in the U-shaped pipe.Can prevent that like this slurries get into the preceding pipeline of pressure monitoring device in the sampling process, result in blockage.
Preferably, (A3) the catalyst slurry collection container is the catalyst slurry holding tank.
Between first end and second end of the first sampling pipeline, be provided with first valve.Preferably, first valve and/or second valve are ball valve.Preferably, the 3rd valve is a stop valve.
Preferably, (A) pipeline and the valve on the sampling system all has abrasion resistance.(A) pipeline on the sampling system and valve adopt wear-resistant pipeline and valve, can increase the service life, and save maintenance cost.
Preferably, the pressure in the paste state bed reactor is greater than external environment condition pressure.
Preferably, paste state bed reactor is a Fischer-Tropsch synthetic pulp state bed reactor.
Preferably, the system that line acquisition system of the present invention is gathered the catalyzer of the reduction or the stage of reaction, the system that the catalyzer of the synthetic reduction of preferred especially Fischer-Tropsch or the stage of reaction is gathered.
Preferably, temperature is 200～320 ℃ in the paste state bed reactor, preferred 200-300 ℃, and more preferably 235～275 ℃.Preferably, pressure is 0.4-3.5MPa in the paste state bed reactor, is preferably 0.5-3.0MPa (relative pressure, gauge pressure).With respect to external environment condition pressure, relative pressure in the paste state bed reactor (gauge pressure) is 0.4-3.5MPa, is preferably 0.5-3.0MPa.Preferably, temperature is 200～320 ℃ when reduction of paste state bed reactor inner catalyst or reaction, preferred 200-300 ℃, and more preferably 235～275 ℃.Preferably, pressure is 0.4-3.5MPa when reduction of paste state bed reactor inner catalyst or reaction, is preferably 0.5-3.0MPa.
The major product (hydrocarbon products) that Fischer-Tropsch synthetic pulp state bed reactor of the present invention is produced is hydrocarbon gas (containing low-carbon alkene), light naphthar and heavy naphtha, diesel oil distillate, wax and synthetic water, especially with naphtha, diesel oil distillate and wax primary product.When producing, paste state bed reactor top is gas phase zone, and the bottom is slurry attitude bed district.
The wax of producing in the Fischer-Tropsch synthesis device is discharged as product through after the filtrator that is provided with in the reactor and the catalyst separation, also can through the slurries in the extraction reactor through external equipment for separating liquid from solid with obtain after catalyst granules separates.Under the external filtrator situation, separate the catalyst granules that obtains and loop back reactor continuation participation reaction again.
Preferably, (A3) the catalyst slurry collection container is a high-temperature resistant container, for example stainless steel or glass container.
Preferably, on-line acquisition system of the present invention further comprises:
(B) inert media injected system comprises:
(B1) inertia liquid medium feeding mechanism; With
(B2) the 4th pipeline is connected to second end of the first sampling pipeline and second end of the second sampling pipeline with inertia liquid medium feeding mechanism, and wherein the 4th pipeline is provided with the 4th valve.
Preferably, (B) the inert media injected system further comprises: (B3) pump is arranged between the 4th valve and the inertia liquid medium feeding mechanism.Preferably, (B3) pump is a reciprocating pump.
Preferably, the inert media injected system further comprises: (B4) pressure monitoring device is arranged between (B3) pump and the 4th valve.(B4) pressure monitoring device is used for measuring the pressure of the 4th pipeline.Preferably, (B4) pressure monitoring device is a tensimeter.Preferably, (B4) pressure monitoring device is arranged on (B3) delivery side of pump place.
Preferably, the 4th valve is a ball valve.Preferably, between (B4) pressure monitoring device and the 4th valve, be provided with the 6th valve.Preferably, the 6th valve is a stop valve.
Preferably, reaction medium (for example solvent) or the product in inertia liquid medium and the paste state bed reactor is identical.Like this, when slurry attitude bed district liquid level that just can be in paste state bed reactor is low, in paste state bed reactor, injects the inertia liquid medium and do not influence reaction, reduce or avoid polluting reaction, need not to separate in addition the inertia liquid medium.
(B1) inertia liquid medium feeding mechanism is used to supply liquid medium.For example, (B1) inertia liquid medium feeding mechanism is the liquid medium storage device of inertia, and the liquid medium memory jar of inertia for example is like liquid wax storage tank.
Preferably, the inertia liquid medium is a liquid wax.Preferably, (B1) inertia liquid medium feeding mechanism is a liquid wax feeding mechanism.When paste state bed reactor was Fischer-Tropsch synthetic pulp state bed reactor, because product comprises wax, preferred especially inertia liquid medium was a liquid wax.
Preferably, on-line acquisition system of the present invention further comprises:
(C) purging system comprises:
(C1) inert blowing gas sweeping device, through the 5th pipeline be connected to second the sampling pipeline second end;
(C2) the 5th valve is arranged on the 5th pipeline.
Preferably, (C1) the inert blowing gas sweeping device is connected to second end of the first sampling pipeline and second end of the second sampling pipeline through the 5th pipeline.
Preferably, part, second sampling pipeline, three pipeline, first valve, second valve and three valve of the first sampling pipeline outside reactor is provided with heating arrangement or companion's thermic devices, preferred electric tracing device, for example electric-heating belt.When the composition in the catalyst slurry or inertia liquid medium at normal temperature (for example 20～30 ℃) down when solid-state, when for example the inertia liquid medium was liquid wax, heating arrangement or companion's thermic devices can prevent that solution stopping wax condenses in the place of flowing through or solidifies.Therefore, preferably, in this case, pipeline that all reactors of the liquid MEDIA FLOW warp of inertia are outer or equipment are provided with above-mentioned heating arrangement or companion's thermic devices.Preferably, outer pipeline and the valve of all reactors of on-line acquisition system of the present invention is provided with above-mentioned heating arrangement or companion's thermic devices.Preferably, except purging system, pipeline that all reactors of on-line acquisition system of the present invention are outer and valve are provided with above-mentioned heating arrangement or companion's thermic devices.For example, (A) in sampling system, (B) inert media injected system the outer pipeline of all reactors be provided with above-mentioned heating arrangement or accompany thermic devices with valve.
Preferably, the heating-up temperature of heating arrangement or companion's thermic devices or to accompany hot temperature be 100～200 ℃.
The present invention relates to use system of the present invention on the other hand to the catalyst slurry online acquisition method in the paste state bed reactor, may further comprise the steps:
(a) the 3rd valve cuts out, open first valve and second valve, make catalyst slurry in the paste state bed reactor get into (A1) the first sampling pipeline and (A2) the second sampling pipeline;
When (b) treating that the interior pressure of the second sampling pipeline is identical with the paste state bed reactor internal pressure, close second valve, open the 3rd valve, catalyst slurry is collected in (A3) catalyst slurry collection container.
Alternatively, (c) repeating step (a) to (b).
For successfully sampling, (A1) port of first end of the first sampling pipeline should be lower than the liquid level certain distance in the paste state bed reactor, for example preset distance H.For example, preset distance H=15～50mm, preferred 15～30mm, for example about 20mm.
Preferably; When the port of first end of (A1) first sampling pipeline and the distance between the liquid level in the paste state bed reactor do not reach when requiring; First end that for example is higher than the first sampling pipeline (14) is higher than liquid level; Though perhaps first end of the first sampling pipeline is lower than liquid level; But during less than preset distance H, through (B) inert media injected system inert media is injected in the paste state bed reactor that liquid level reaches requirement in paste state bed reactor, for example is higher than the first end preset distance H of the first sampling pipeline (14).
Therefore, preferably, method of the present invention further comprises: in step (a) before,
(a ') is injected into inert media in the paste state bed reactor through (B) inert media injected system that liquid level reaches requirement in paste state bed reactor, for example is higher than distance H.
Preferably; Step (a ') comprising: close first valve, second valve and the 5th valve (if existence); Start (B3) pump, treat that pressure in the 4th pipeline is higher than paste state bed reactor (for example about 0.5MPa) after, open first valve; In paste state bed reactor, inject the inertia liquid medium, liquid level reaches requirement in paste state bed reactor.
Preferably, in step (a) before, preferably before, confirm whether heating arrangement or the companion's thermic devices in (A) sampling system reaches design temperature in step (a ').When the composition in the catalyst slurry or or the inertia liquid medium at normal temperature (for example 20～30 ℃) down when solid-state, before sampling, need to confirm whether (A) sampling system and heating arrangement or companion's thermic devices in (B) the inert media injected system reach design temperature.
Preferably, method of the present invention further comprises:
(d) cleaning step: in the first sampling pipeline and the second sampling pipeline, inject the inertia liquid medium through (B) inert media injected system, clean.
Preferably, (d) cleaning step comprises: start (B3) pump, open the 6th valve (if existence), the 4th valve, second valve, the 3rd valve, in the first sampling pipeline and the second sampling pipeline, inject whiteruss, clean.
Preferably, after (d) cleaning step, also comprise purge step.Therefore, preferably, method of the present invention further comprises:
(e) purge step: the second sampling pipeline is purged through purging system.
After the cleaning, stop (B3) pump, close the 4th valve,, the sampling pipeline is purged (for example 5 minutes) through purging inert gas (for example nitrogen) from the 5th valve through purging system.
After purging finishes, close the 5th valve and the 3rd valve.
With reference to the accompanying drawings, being example with Fischer-Tropsch synthetic pulp state bed reactor describes in detail to the system and method for online acquisition catalyst slurry of the present invention.
The present invention relates to a kind of method of Fischer-Tropsch synthetic pulp state bed reactor online acquisition catalyst slurry, it is characterized in that the catalyzer of the synthetic reduction of Fischer-Tropsch or the stage of reaction is gathered, the physicochemical property of following the tracks of catalyzer changes.Under certain temperature, pressure and catalyst slurry concentration, in reaction gas, feed unstripped gas, make catalyst reduction or Fischer-Tropsch synthesis takes place; Reaction product and unreacted gas get into piece-rate system and separate through behind the still internal filter; In reduction or the course of reaction,, gather catalyst slurry through sampling apparatus and system.
As shown in Figure 1, a kind of preferred embodiment in, catalyst slurry acquisition system provided by the invention comprises:
(A) sampling system comprises: the first sampling pipeline 14 and on the 5th valve (ball valve) 5 and first valve (ball valve) 6, the second sampling pipeline 16 and on second valve (ball valve) 7, the 3rd valve (stop valve) 10 and tensimeter 18, catalyst slurry holding tank 11.Preferably, part, first valve (ball valve) 6, second sampling pipeline 16, second valve (ball valve) 7 and three valve (stop valve) 10 of the first sampling pipeline 14 outside reactor all adds electric-heating belt.Preferably, filled with liquid paraffin in the U type pipe before the tensimeter 18 prevents that the preceding pipeline of slurries entering tensimeter results in blockage in the sampling process.
(B) liquid wax injected system comprises: the 6th valve (stop valve) 3, the 4th valve (ball valve) 4 and tensimeter 17 on liquid wax accumulator tanks 1, liquid wax injection pump 2, the 4th pipeline (liquid wax injects pipeline) the 12 and the 4th pipeline 12.
Preferably, catalyst slurry acquisition system of the present invention further comprises:
(C) purging system comprises:
(C1) the inert blowing gas sweeping device 202, are connected to second end of the second sampling pipeline 16 through the 5th pipeline;
(C2) the 5th valve 5 is arranged on the 5th pipeline.
Preferably, catalyst slurry acquisition system of the present invention further comprises:
(D) slurry attitude bed reactive system, it comprises: the reaction product discharging pipeline 15 that unstripped gas injects pipeline 13, stirred tank reactor 8, still internal filter 9 and is attached thereto.
Among Fig. 1 alphabetical A through arrow labeled the liquid level in the stirred tank reactor 8.
As shown in Figure 1, a kind of system of fischer-tropsch synthetic catalyst evaluating apparatus online acquisition catalyst slurry comprises:
Liquid wax injected system: liquid wax accumulator tanks 1, liquid wax injection pump 2, liquid wax inject the 6th valve (stop valve) 3 on the 4th pipeline 12 and the 4th pipeline 12, the 4th valve (ball valve) 4 and tensimeter 17, the first sampling pipeline 14 with and on first valve (ball valve) 6 (also using this pipeline and valve when gathering still inner catalyst slurries);
The stirred tank reactive system: unstripped gas injected system 13, stirred tank reactor 8, still internal filter 9 reach reaction product discharging pipeline 15 with it;
The catalyst slurry acquisition system: the first sampling pipeline 14 and on the 5th valve (ball valve) 5 and first valve (ball valve) 6, the second sampling pipeline 16 and on second valve (ball valve) 7, the 3rd valve (stop valve) 10 and tensimeter 18, slurries holding tank 11.
Preferably, unstripped gas is synthetic gas (CO and H
2) or pure H
2, pure CO, the gas agent is than for 1000-10000ml/g-cat./h.
Preferably, the concentration of stirred tank inner catalyst slurries is 2-20wt%.
Preferably, temperature is 200-300 ℃ when stirred tank inner catalyst reduction or reaction.
Preferably, pressure is 0.5-3.0MPa when stirred tank inner catalyst reduction or reaction.
Preferably, the mode of collection catalyst slurry is a batch (-type).
Preferably, pipeline on the catalyst slurry acquisition system and valve all add electric tracing, and accompanying hot temperature is 100-200 ℃.
Preferably, the catalyst slurry holding tank is resistant to elevated temperatures stainless steel or glass container.
Preferably, pipeline and valve all have certain abrasion resistance on the catalyzer sampling system.
Preferably, the internal diameter of the internal diameter of part and still exterior portions is identical or different in the catalyzer sampling pipeline agitated reactor.
Further specify the working method that patent of the present invention provides method below in conjunction with accompanying drawing 1, but therefore the present invention does not receive any restriction.
A kind of preferred embodiment in, the method for sampling of the present invention, being divided into is three steps: sampling is prepared, cleaning and purging after the sampling, sampling.
(a ') the sampling preparation
1, confirms whether the electric tracing temperature on the sampling first sampling pipeline 14 and 16 reaches normal design temperature;
2, through drawing temperature (assaying reaction temperature in the kettle) to confirm, liquid level is higher than the sampling first sampling pipeline 14 lower port in the agitated reactor 8, at the built-in filter lower end, guarantees that promptly liquid level is higher than the about 20mm of first sampling pipeline 14 lower port; If liquid level is lower, start pump 2, close the 5th valve 5, first valve 6 and second valve 7, treat that pump discharge pressure table 17 shows that pressure is higher than agitated reactor 8 about 0.5MPa after, open first valve 6, injection liquid wax in agitated reactor, liquid level reaches requirement in still.
In the sampling preparatory stage, the preparation of sampling instrument, protective gloves, safety goggles and slurries holding tank etc. need be ready to before sampling.
(a) sampling
(1) common, sampling needs two operator's compounding practices, people nurse, people sampling;
(2) open first valve 6 and second valve 7; Close the 3rd valve 10; Catalyst slurry in the agitated reactor is got in the first sampling pipeline 14 and 16, treat that tensimeter 18 shows when pressure is identical with reacting kettle inner pressure, closes second valve 7; Slowly open the 3rd valve 10, catalyst slurry is collected in the serum pot 11;
(3) repeat aforesaid operations 2-3 time, collect required slurries after, close first valve 6, open second valve 7 and the 3rd valve 10.
(c) clean and (d) purge
(1) start pump 2, open valve 3,4,7,10 injects whiteruss in sampling pipeline 14,16, clean;
(2) clean up after, termination of pumping 2, shut-off valve 4 connects from the 5th valve 5 and to purge low pressure N
2, the sampling pipeline was purged about 5 minutes;
(3) after purging finishes, close the 5th valve 5 and the 3rd valve 10.
This system is the catalyst slurry in the online acquisition paste state bed reactor easily.
Embodiment
In this embodiment, be the applicable cases of method provided by the present invention in the syrup state bed Fischer Tropsch synthesis iron base catalyst R&D work.
SFT418 fischer-tropsch synthetic catalyst and the certain amount of fluid paraffin that 35g is had a group of Shenhua is packed into behind the slurry attitude bed agitated reactor 8; Reductase 12 is 4 hours under the condition of 250 ℃, 0.5MPa, pure hydrogen atmosphere (the gas agent is than being 2000ml/g-cat./h); After reduction finishes; Switch under the condition of 265 ℃, 2.3MPa, synthetic gas (hydrogen-carbon ratio is 1.5, and the gas agent is than being 2000ml/g-cat./h) and react 500h.Wherein at when reduction, reaction 100h, 200h, gathered catalyst slurry at 300 o'clock.Sampling during reduction and in the course of reaction is slightly had any different.
1. the slurries collection in the reduction process
Owing to do not produce liquid wax product in the reduction process, the liquid level when reduction finishes in the agitated reactor possibly be lower than sampling pipeline 6 lower port, need in still, inject certain amount of fluid paraffin.Concrete steps are following:
(1) confirms that the electric tracing temperature on the sampling first sampling pipeline 14 and 16 reaches 150 ℃ of normal design temperatures;
(2) through drawing temperature (assaying reaction temperature in the kettle) to confirm, liquid level is lower than the about 10mm of first sampling pipeline 14 lower port in the agitated reactor 8; Start pump 2, close the 5th valve 5, first valve 6 and second valve 7, treat that pump discharge pressure table 17 shows that pressure is higher than agitated reactor 8 about 0.5MPa after, open first valve 6, in agitated reactor, inject liquid wax, behind the about 200g of injection liquid wax, first valve 6 is closed in termination of pumping 2 simultaneously;
(3) draw temperature (assaying reaction temperature in the kettle) once more, after liquid levels are higher than the about 20mm of first sampling pipeline 14 lower port in the affirmation agitated reactor 8, open first valve 6 and second valve 7; Close the 3rd valve 10; Catalyst slurry in the agitated reactor is got in the pipeline 14 and 16, treat that tensimeter 18 shows when pressure is identical with reacting kettle inner pressure, closes second valve 7; Slowly open the 3rd valve 10, catalyst slurry is collected in the serum pot 11;
(4) repeat above-mentioned 3) operation 2-3 time, collect about 60g slurries after, close first valve 6, open second valve 7 and the 3rd valve 10.
(5) start pump 2, open valve 3,4,7,10 injects whiteruss in the sampling pipeline, clean;
(6) clean up after, termination of pumping 2, shut-off valve 4 connects from the 5th valve 5 and to purge low pressure N
2, the sampling pipeline was purged about 5 minutes;
(7) after purging finishes, close the 5th valve 5 and the 3rd valve 10.
2. the catalyst slurry collection in the course of reaction
In the fischer-tropsch reaction process, produce product liquid, liquid level is higher than the first sampling pipeline, 14 lower port in the agitated reactor 8, need in still, not inject whiteruss, and concrete sampling step is following:
(1) confirms that the electric tracing temperature on the first sampling pipeline 14 and 16 reaches 150 ℃ of normal design temperatures;
(2) through drawing temperature (assaying reaction temperature in the kettle) to confirm, liquid level is higher than the about 20mm of first sampling pipeline 14 lower port in the agitated reactor 8;
(3) open first valve 6 and second valve 7, close the 3rd valve 10, the catalyst slurry in the agitated reactor is got in the pipeline 14 and 16; Treat that tensimeter 18 shows when pressure is identical with reacting kettle inner pressure; Close second valve 7, slowly open the 3rd valve 10, catalyst slurry is collected in the serum pot 11;
(4) repeat above-mentioned 3) operation 2-3 time, collect about 60g slurries after, close first valve 6, open second valve 7 and the 3rd valve 10.
(5) start pump 2, open valve 3,4,7,10 injects whiteruss in the sampling pipeline, clean;
(6) clean up after, termination of pumping 2, shut-off valve 4 connects from the 5th valve 5 and to purge low pressure N
2, the sampling pipeline was purged about 5 minutes;
(7) after purging finishes, close the 5th valve 5 and the 3rd valve 10.
3. the property analysis of catalyzer in the slurries
With the catalyzer of gathering out, after the xylene extracting, carry out sreen analysis through Ma Erwen 2000 particle size distribution analysis appearance again, the granularity in differential responses stage is seen table 1.
The sreen analysis of table 1 different phase catalyzer
Annotate: D50 and be meant when making particle size distribution analysis that the catalyst granules granularity of 50% volume is more than this is worth;
＜50 microns, be meant the percent by volume of granularity less than 50 microns catalyst granules.
Certainly, the present invention also can have other embodiments, more than is merely preferred implementation of the present invention, is not to be used for limiting protection scope of the present invention; Under the situation that does not deviate from spirit of the present invention, those of ordinary skills are every to make various corresponding variations and modification according to content of the present invention, all belongs to the protection domain of claim of the present invention.
Claims (20)
1. catalyst slurry on-line acquisition system, wherein said catalyst slurry is contained in the paste state bed reactor (8), it is characterized in that, comprising:
(A) sampling system comprises:
(A1) the first sampling pipeline (14) has first end and second end, and first end of the said first sampling pipeline (14) extend in the said paste state bed reactor (8), and wherein, the said first sampling pipeline (14) is provided with first valve (6);
(A2) the second sampling pipeline (16) has first end and second end, and second end of the said second sampling pipeline (16) is connected to second end of the said first sampling pipeline (14); Wherein, be provided with second valve (7) at the second end place of the said second sampling pipeline (16), the first end place of the said second sampling pipeline (16) is provided with the 3rd valve (10);
(A3) catalyst slurry collection container (11), be connected to said second the sampling pipeline (16) first end;
(B) inert media injected system comprises:
(B1) inertia liquid medium feeding mechanism (1); With
(B2) the 4th pipeline (12) is connected to second end of the said first sampling pipeline (14) and second end of the said second sampling pipeline (16) with said inertia liquid medium feeding mechanism (1), and wherein said the 4th pipeline is provided with the 4th valve (4).
2. the catalyst slurry on-line acquisition system in the paste state bed reactor according to claim 1, wherein, said (A) sampling system further comprises:
(A4) pressure monitoring device (18) is connected on the said second sampling pipeline (16) between said second valve (7) and said the 3rd valve (10) through the 3rd pipeline.
3. catalyst slurry on-line acquisition system according to claim 2 wherein, is provided with the U-shaped pipe in said the 3rd pipeline, fills the inertia liquid medium in the U-shaped pipe.
4. catalyst slurry on-line acquisition system according to claim 1, wherein, said (B) inert media injected system further comprises:
(B3) pump (2) is arranged between said the 4th valve (4) and the said inertia liquid medium feeding mechanism (1).
5. catalyst slurry on-line acquisition system according to claim 4, wherein, said (B) inert media injected system further comprises:
(B4) pressure monitoring device (17) is arranged between said pump (2) and said the 4th valve (4).
6. catalyst slurry on-line acquisition system according to claim 1 further comprises:
(C) purging system comprises:
(C1) inert blowing gas sweeping device (202), through the 5th pipeline be connected to said second the sampling pipeline (16) second end;
(C2) the 5th valve (5) is arranged on said the 5th pipeline.
7. catalyst slurry on-line acquisition system according to claim 1, wherein, pipeline in said (A) sampling system and valve are wear-resistant pipeline and wear-resistant valve.
8. catalyst slurry on-line acquisition system according to claim 5, wherein, said pressure monitoring device (17) in said (B) inert media injected system and the said pressure monitoring device (18) in said (A) sampling system are tensimeter.
9. catalyst slurry on-line acquisition system according to claim 1, pipeline that paste state bed reactor (8) described in said (A) sampling system, said (B) inert media injected system is outer and valve are provided with heating arrangement or companion's thermic devices.
10. according to each described catalyst slurry on-line acquisition system of claim 1 to 9, wherein, said paste state bed reactor (8) is a Fischer-Tropsch synthetic pulp state bed reactor; Said inertia liquid medium feeding mechanism (1) is a liquid wax feeding mechanism.
11. a catalyst slurry online acquisition method, through carrying out according to each described system of claim 1 to 10, this method comprises:
(a) close said the 3rd valve (10), open said first valve (6) and said second valve (7), make the catalyst slurry in the said paste state bed reactor (8) get into said (A1) first sampling pipeline (14) and said (A2) second sampling pipeline (16);
(b) close said second valve (7), open said the 3rd valve (10), said catalyst slurry is collected in said (A3) the catalyst slurry collection container (11);
Alternatively, (c) repeating step (a) to (b).
12. method according to claim 11, wherein, reaction medium or product in said inertia liquid medium and the said paste state bed reactor (8) are identical.
13. according to claim 11 or 12 described methods, wherein, the pressure in the said paste state bed reactor (8) is greater than external environment condition pressure; Preferably; With respect to external environment condition pressure, the pressure in the said paste state bed reactor (8) is 0.4-3.5MPa, is preferably 0.5-3.0MPa.
14. according to each described method of claim 11 to 13, wherein, temperature is 200～320 ℃ in the said paste state bed reactor (8), preferred 200-300 ℃, and more preferably 235～275 ℃.
15. according to each described method of claim 11 to 14; Wherein, Further comprise: in step (a) before, (a ') through said (B) inert media injected system with inert media be injected in the said paste state bed reactor (8) until said paste state bed reactor (8) in liquid level be higher than said first sample pipeline (14) the first end preset distance H.
16. according to each described method of claim 11 to 15, wherein, when said catalyst slurry on-line acquisition system has said heating arrangement or companion during thermic devices, the heating-up temperature of said heating arrangement or companion's thermic devices or to accompany hot temperature be 100～200 ℃.
17., further comprise according to each described method of claim 11 to 16:
(d) cleaning step: in said first sampling pipeline (14) and the said second sampling pipeline (16), inject the inertia liquid medium through said (B) inert media injected system, clean.
18. according to each described method of claim 11 to 17, wherein, when said catalyst slurry on-line acquisition system comprised (C) purging system, this method further comprised:
(e) purge step: the said second sampling pipeline (16) is purged through said (C) purging system.
19. according to each described method of claim 11 to 18, wherein, the mode of gathering said catalyst slurry is a batch (-type).
20. according to each described method of claim 11 to 19, wherein, said catalyst slurry online acquisition method is the catalyst slurry online acquisition method in fischer-tropsch synthetic catalyst reduction phase or Fischer-Tropsch synthesis stage.
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