CN106770891A - Catalyst test apparatus and evaluation method - Google Patents
Catalyst test apparatus and evaluation method Download PDFInfo
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- CN106770891A CN106770891A CN201611252898.7A CN201611252898A CN106770891A CN 106770891 A CN106770891 A CN 106770891A CN 201611252898 A CN201611252898 A CN 201611252898A CN 106770891 A CN106770891 A CN 106770891A
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- gas
- liquid
- knockout drum
- pressure
- catalyst
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/10—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using catalysis
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/58—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to change the structural skeleton of some of the hydrocarbon content without cracking the other hydrocarbons present, e.g. lowering pour point; Selective hydrocracking of normal paraffins
- C10G45/60—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to change the structural skeleton of some of the hydrocarbon content without cracking the other hydrocarbons present, e.g. lowering pour point; Selective hydrocracking of normal paraffins characterised by the catalyst used
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/58—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to change the structural skeleton of some of the hydrocarbon content without cracking the other hydrocarbons present, e.g. lowering pour point; Selective hydrocracking of normal paraffins
- C10G45/68—Aromatisation of hydrocarbon oil fractions
-
- 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
- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/72—Controlling or regulating
-
- 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
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/02—Gasoline
Abstract
The present invention provides a kind of catalyst test apparatus and evaluation method, catalyst test apparatus include feed unit, reaction member and separative element, and feed unit includes hydrogen cylinder, feed naphtha tank, the first raw material pump, raw liquefied petroleum gas tank, the second raw material pump, the first preheater and the second preheater；Reaction member includes reactor, and the beds for loading catalyst to be evaluated are provided with reactor, and for preparing gasoline by raw material of the material from the second preheater；Separative element, for being separated to the product from the reactor, to obtain gaseous component and liquid phase component for sampling analysis.Catalyst test apparatus of the invention and evaluation method, can be used to mix the evaluating catalyst that isomerization/aromatisation prepares gasoline component, can evaluate catalysis activity of the catalyst under continuous state；And can realize evaluating the catalyst of differential responses system by the Push And Release of respective valves, it is applied widely.
Description
Technical field
The invention belongs to evaluating catalyst field, particularly catalyst test apparatus and evaluation method.
Background technology
Catalyst is important catalyst in chemical industry, and production capacity is govern to a certain extent.To urging for catalyst
Change the measurement of performance, mainly evaluated by the overall target to the active of catalyst, selectivity and life-span.It is existing to urge
Agent evaluating apparatus are only capable of evaluating the catalyst of single a certain reaction system, and applicability is limited.
Gasoline is one of important engine fuel, is widely used in the industries such as communications and transportation.With the hair of national economy
Exhibition, the demand to gasoline is growing, it is contemplated that domestic gasoline consumption is up to 1.7 hundred million tons within 2025.In face of so huge
Consumption, using light-hydrocarbon aromatized/aromatisation (isomerization/aromatisation of liquefied gas, light naphthar, condensate etc.) produce Gaoxin
The research of alkane value gasoline blending component has wide market prospects with application.And naphtha is the low octane rating based on alkane
Gasoline component, the method for improving its octane number is：Under catalyst action, by aromatisation or isomerization reaction by naphtha
Alkane transformations be aromatic hydrocarbons or isoparaffin.Meanwhile, olefin-containing liquefied gas, by aromatization technology, is sent out under catalyst action
High octane gasoline component is produced in the reactions such as raw cracking, oligomerisation, cyclisation, dehydrogenation, hydrogen migration, so as to improve the application valency of liquefied gas
Value.Contribute to understand and grasp the situation of the reaction system by the performance for evaluating the catalyst in the reaction system, and pass through
Adjusting process process improves reaction rate and production efficiency.But, existing catalyst test apparatus can not be used to mix
Isomerization/aromatisation prepares the evaluating catalyst of gasoline component, and major part is only directed to a certain reaction and designs, or by phase
The transformation answered could realize the evaluating catalyst of differential responses system, using there is many restrictions.
The content of the invention
It is an object of the invention to provide a kind of catalyst test apparatus, the catalyst test apparatus can be used to mix isomery
Change/aromatisation prepares the evaluating catalyst of gasoline component, can evaluate catalysis activity of the catalyst under continuous state；
Another object of the present invention is to provide using above-mentioned catalyst test apparatus to mixing isomerization/aromatisation system
The method that the catalyst of standby gasoline component carries out evaluating catalyst.
To realize one object of the present invention, using following technical scheme：
A kind of catalyst test apparatus, including：
Feed unit, the feed unit is including hydrogen cylinder, feed naphtha tank, for conveying the feed naphtha tank
The second of first raw material pump of middle material, raw liquefied petroleum gas tank, material for conveying the raw liquefied petroleum gas tank
Raw material pump, the first preheater and the second preheater；First preheater is used to heat the material from the first raw material pump,
To obtain the naphtha that gasifies, second preheater is used to heat from the hydrogen cylinder, the second raw material pump and the first preheating
The material of device；
Reaction member, the reaction member includes reactor, is provided with the reactor and loads urging for catalyst to be evaluated
Agent bed, and for preparing gasoline by raw material of the material from second preheater；
Separative element, for being separated to the product from the reactor, to obtain for sampling analysis
Gaseous component and liquid phase component.
Preferably, the separative element includes：
Cooler, for receiving the product from the reactor and being cooled down to it；
High-pressure gas-liquid knockout drum, for receiving the material from the cooler and carrying out gas-liquid separation to it, obtains liquid
Phase material；
Low-pressure gas-liquid knockout drum, for receiving the liquid phase substance from the high-pressure gas-liquid knockout drum and carrying out gas-liquid to it
Separate, obtain gaseous component and liquid phase component..
Preferably, the catalyst test apparatus also include carrier gas unit, and the carrier gas unit includes nitrogen cylinder, first defeated
Gas pipeline, the second gas transmission line and the 3rd gas transmission line, wherein, the first gas transmission line is used to convey the nitrogen from the nitrogen cylinder
Gas is purged to the reaction member and separative element；Second gas transmission line is used to convey the nitrogen from the nitrogen cylinder
Gas carries out pressurising to the raw liquefied petroleum gas tank；3rd gas transmission line is used to convey the nitrogen from the nitrogen cylinder
Pressurising is carried out to the low-pressure gas-liquid knockout drum.
Preferably, the reaction member also includes heating furnace, and the reactor is tubular reactor, and the heating furnace is arranged
In on the reactor, for being heated to the reactor.
Preferably, the entrance for being exported to second preheater of the hydrogen cylinder is provided with hydrogen delivery tube line, institute
State hydrogen delivery tube line and be provided with first flowmeter；
First gas transmission line is provided with second flowmeter.
Preferably, the first gas phase export pipeline, described first are provided with the gaseous phase outlet of the high-pressure gas-liquid knockout drum
Counterbalance valve and wet flow indicator are disposed with gas phase export pipeline；
The second gas phase export pipeline, the second gas phase output are provided with the gaseous phase outlet of the low-pressure gas-liquid knockout drum
The gas phase sampling valve for sampling analysis is provided with pipeline；The gas phase sampling valve is triple valve；
The 3rd gas phase export pipeline is provided with the gas phase sampling valve to the outlet side pipeline of the counterbalance valve；It is described low
Liquid phase export pipeline is provided with the outlet at bottom for pressing knockout drum, is provided with the liquid phase export pipeline for sampling point
The liquid phase sampling valve of analysis.
To realize another object of the present invention, using following technical scheme：
It is a kind of the catalyst that mixing isomerization/aromatisation prepares gasoline component is entered using foregoing catalyst test apparatus
The method of row evaluating catalyst, the carrier gas unit includes nitrogen cylinder, the first gas transmission line, the second gas transmission line and the 3rd gas transmission
Pipeline；Methods described includes：
Before reaction, receive the nitrogen from nitrogen cylinder using the first gas transmission line and reaction member and separative element are blown
Sweep, to displace air, maintain the inert environments of system；
During the course of the reaction：
The raw liquefied petroleum gas tank is filled using the second gas transmission line nitrogen of the conveying from the nitrogen cylinder
Pressure；
Pressurising is carried out to the low-pressure gas-liquid knockout drum using the 3rd gas transmission line nitrogen of the conveying from the nitrogen cylinder.
Preferably, methods described also includes：
Before preheating raw material, after air is displaced completely, while heating system, continue to use nitrogen
Gas is purged to system, with the impurity on Removal of catalyst.
Preferably, the separative element includes cooler, high-pressure gas-liquid knockout drum and low-pressure gas-liquid knockout drum；Described first
Counterbalance valve is provided with gas phase export pipeline；The 3rd is provided with the gas phase sampling valve to the outlet side pipeline of the counterbalance valve
Gas phase export pipeline；Liquid phase export pipeline, the liquid phase efferent duct are provided with the outlet at bottom of the low-pressure gas-liquid knockout drum
The liquid phase sampling valve for sampling analysis is provided with line；Methods described also includes：
In the separative element：
The gasoline product from the reaction member is cooled down using cooler；
The material from the cooler is received using high-pressure gas-liquid knockout drum, then using described in the back pressure valve regulation
Pressure in high-pressure gas-liquid knockout drum is identical with the pressure of the reaction member, to carry out gas-liquid separation to it, empties gas gas-phase objects
Matter, obtains liquid phase substance；Then will be input into the low-pressure gas-liquid knockout drum to low-pressure gas-liquid point from the nitrogen in nitrogen cylinder
Pressure in tank is identical with the pressure in high-pressure gas-liquid knockout drum, nitrogen conveying is then cut off, so that high-pressure gas-liquid knockout drum
Liquid phase substance export downwards under gravity；
The liquid phase substance from the high-pressure gas-liquid knockout drum is received using low-pressure gas-liquid knockout drum and gas-liquid is carried out to it
Separate, obtain the gaseous component and liquid phase component for sampling analysis；Then gaseous component is passed through into gas phase sampling valve and the 3rd
It is 0.1-0.3MPa that gas phase export pipeline discharges a part to the pressure in the low-pressure gas-liquid knockout drum, then by gas phase
Sampling valve is sampled analysis to gaseous component；Then gaseous component is put by gas phase sampling valve and the 3rd gas phase export pipeline
Sky, then analysis is sampled to liquid phase component by liquid phase sampling valve.
The beneficial effects of the present invention are：
(1) catalyst test apparatus of the invention, can be used to mix the catalyst that isomerization/aromatisation prepares gasoline component
Evaluate, catalysis activity of the catalyst under continuous state can be evaluated；And can be realized to not by the Push And Release of respective valves
Evaluated with the catalyst of reaction system, it is applied widely；
(2) side that evaluating catalyst is carried out to the catalyst that mixing isomerization/aromatisation prepares gasoline component of the invention
Method, it is simple to operation.
Brief description of the drawings
Fig. 1 is catalyst test apparatus of the invention schematic diagram in one embodiment.
Specific embodiment
Technical solution of the present invention and its effect are described further below by way of specific embodiment.Implementation below
Present disclosure is merely to illustrate, the protection domain being not intended to limit the invention.Using design of the invention to the present invention
The simple change for carrying out is all in the scope of protection of present invention.
As shown in figure 1, catalyst test apparatus of the invention, including：
Feed unit, the feed unit is including hydrogen cylinder 12, feed naphtha tank 1, for conveying the naphtha original
First raw material pump 2 of material, raw liquefied petroleum gas tank 3, the thing for conveying the raw liquefied petroleum gas tank 3 in batch can 1
The second raw material pump 4, the first preheater 5 and the second preheater 6 expected；First preheater 5 is used to heat from described first
The material of raw material pump 2, to obtain the naphtha that gasifies, second preheater 6 is used to heat from the original of the hydrogen cylinder 12, second
Expect the material of the preheater 5 of pump 4 and first；The hydrogen cylinder 12, for providing hydrogen, preferably high-purity hydrogen；Can also be used for again
Reaction advance row air tightness test；
Reaction member, the reaction member includes being provided with filling catalyst to be evaluated in reactor 7, the reactor 7
Beds, and for preparing gasoline by raw material of the material from second preheater 6；The catalyst to be evaluated
Catalyst is filled with bed；It is preferred that the top and bottom of the beds are equipped with ceramic packing, the ceramics of lower end are filled out
Expect that the ceramic packing of upper end is for making the catalyst distribution of filling uniform for supporting beds；It is further preferably described
Filtering meshes are provided between ceramic packing and catalyst, for separating filler and catalyst；Further preferably, positioned at lower end
The lower end of ceramic packing is also equipped with filtering meshes, i.e. filling order is followed successively by ceramic packing, filtering meshes, urges from top to bottom
Agent, filtering meshes, ceramic packing, filtering meshes；This type of feed is conducive to catalyst to be separated with ceramic packing, filtering
Stratum reticulare can also prevent the catalyst crushed or ceramic packing from entering the outlet line of reaction system, prevent pipeline from blocking；
Separative element, for being separated to the product from the reactor 7, to obtain for sampling analysis
Gaseous component and liquid phase component.
Catalyst test apparatus of the invention, can be used to mixing isomerization/aromatisation and prepare the catalyst of gasoline component and comment
Valency, can evaluate catalysis activity of the catalyst under continuous state；And can be realized to difference by the Push And Release of respective valves
The catalyst of reaction system is evaluated, applied widely.
In one embodiment, the separative element includes：
Cooler 9, for receiving the product from the reactor 7 and being cooled down to it；It is preferred that the cooling
Device 9 is coiled pipe cooler, and cooling medium is deionized water, distilled water or running water；
High-pressure gas-liquid knockout drum 10, for receiving the material from the cooler 9 and carrying out gas-liquid separation to it, obtains
Liquid phase substance；
Low-pressure gas-liquid knockout drum 11, for receiving the liquid phase substance from the high-pressure gas-liquid knockout drum 10 and being carried out to it
Gas-liquid separation, obtains gaseous component and liquid phase component.
The specific setting of separative element, contributes to the gaseous component and liquid phase component of system product at preferably separation, with
It is easy to be sampled it analysis, it is ensured that the accuracy of sampling analysis.
In one embodiment, the catalyst test apparatus also include carrier gas unit, and the carrier gas unit includes nitrogen
Gas cylinder 13, the first gas transmission line 14, the second gas transmission line 19 and the 3rd gas transmission line 18, wherein, the first gas transmission line 14 is used for
Nitrogen of the conveying from the nitrogen cylinder 13 is purged to the reaction member and separative element；Second gas transmission line 19
Pressurising is carried out to the raw liquefied petroleum gas tank 3 so that liquefied gas material liquid for conveying the nitrogen from the nitrogen cylinder 13
Change；3rd gas transmission line 18 is used for nitrogen of the conveying from the nitrogen cylinder 13 to be carried out to the low-pressure gas-liquid knockout drum 11
Pressurising.The nitrogen cylinder 13 can also be used for carrying out air tightness test before the reaction.
It is to use nitrogen displacement reaction member and separative element that purging is carried out to reaction member and separative element before reaction
In air, the air in system is driven out of, maintenance system is reacted and is separated in an inert atmosphere.And by air
After replacing completely, continuation is purged with nitrogen to system while heating to system, will be adsorbed on a catalyst
Impurity removal.In course of reaction nitrogen can be provided with or without according to reaction needs.
In one embodiment, the reaction member also includes heating furnace 8, and the reactor is tubular reactor, institute
State heating furnace 8 to be sheathed on the reactor 7, for heating the reactor 7.
In one embodiment, the outlet of the nitrogen cylinder 13 is additionally provided with gas transmission line 13 ', the gas transmission line
13 ' the port of export respectively with the entrance point phase of first gas transmission line 14, the second gas transmission line 19 and the 3rd gas transmission line 18
Connection；The 4th valve 131 ' and the 4th pressure-reducing valve 132 ' are disposed with the gas transmission line 13 '.4th pressure-reducing valve 132 '
It is provided for maintaining pressure constant, it is stable to ensure the nitrogen flow for being input into follow-up system.
In one embodiment, the entrance for being exported to second preheater 6 of the hydrogen cylinder 12 is provided with hydrogen
Letter shoot line 15, first flowmeter 153 is provided with the hydrogen delivery tube line 15；First gas transmission line 14 is provided with
Second flowmeter 141.
The amount for being provided for controlling the raw material in hydrogen cylinder 12 to participate in reaction as needed of first flowmeter 153, to have
Pointedly the catalyst in certain reaction system is evaluated；Being provided for of second flowmeter 141 controls as needed
Flow when being purged to system with the nitrogen in nitrogen cylinder 13, with targetedly to the catalyst in certain reaction system
Evaluated.
It is appreciated that the 3rd valve 151 and the 3rd pressure-reducing valve 152 are additionally provided with hydrogen delivery tube line 15, described first
The 8th valve 142 is additionally provided with gas transmission line 14.
In one embodiment, it is provided with the first gas phase efferent duct at the gaseous phase outlet of the high-pressure gas-liquid knockout drum 10
Line 21, is disposed with counterbalance valve 211 and wet flow indicator 212, for working as high pressure gas on the first gas phase export pipeline 21
Pressure in liquid knockout drum 10 higher than the reactor 7 and the cooler 9 pressure when, discharge one by counterbalance valve 211
Divide the gaseous substance from the high-pressure gas-liquid knockout drum 10, to maintain the pressure in high-pressure gas-liquid knockout drum 10 with the reaction
Device 7 is identical with the pressure of the cooler 9；Pressure in high-pressure gas-liquid knockout drum 10 should be 0.8-1MPa；
The second gas phase export pipeline 22, second gas phase are provided with the gaseous phase outlet of the low-pressure gas-liquid knockout drum 11
The gas phase sampling valve 221 for sampling analysis is provided with export pipeline 22, is controlled to intermittently release out from the low-pressure gas-liquid
The gaseous component of knockout drum 11 is used for sampling analysis；The gas phase sampling valve 221 is triple valve；
The 3rd gas phase export pipeline is provided with the gas phase sampling valve 221 to the outlet side pipeline of the counterbalance valve 211
23, for the gaseous phase outlet of low-pressure gas-liquid knockout drum 11 to be connected with the 3rd gas phase export pipeline 23 when gas phase sampling valve 221
When, the gas phase of low-pressure gas-liquid knockout drum 11 is vented；And work as gas phase sampling valve 221 by the gaseous phase outlet of low-pressure gas-liquid knockout drum 11
When being connected with the second gas phase export pipeline 22, the gas phase to low-pressure gas-liquid knockout drum 11 is sampled analysis；
Liquid phase export pipeline 24, the liquid phase export pipeline are provided with the outlet at bottom of the low-pressure gas-liquid knockout drum 11
The liquid phase sampling valve 241 for sampling analysis is provided with 24, is controlled to intermittently release out from the low-pressure gas-liquid knockout drum 11
Liquid phase component be used for sampling analysis.
In one embodiment, the entrance for being exported to first preheater 5 from the first raw material pump 2 is provided with
First feedstock transportation pipeline 16, is provided with the first valve 161, for controlling as needed on the first feedstock transportation pipeline 16
Whether the raw material in feed naphtha tank 1 participates in reaction, targetedly to comment the catalyst in certain reaction system
Valency；
The entrance for being exported to second preheater 6 of the second raw material pump 4 is provided with the second feedstock transportation pipeline
17, the second valve 171 is provided with the second feedstock transportation pipeline 17, for controlling raw liquefied petroleum gas tank as needed
Whether the raw material in 3 participates in reaction, targetedly to evaluate the catalyst in certain reaction system.
In one embodiment, the 5th valve 181 is provided with the 3rd gas transmission line 18, for being as needed
It is no to being filled with nitrogen to improve pressure in low-pressure gas-liquid knockout drum 11；The 6th valve is provided with second gas transmission line 19
191, for being filled with nitrogen to pressurize to the intermittent of raw liquefied petroleum gas tank 3 as needed, gas raw material is liquefied；From
The outlet at bottom of the high-pressure gas-liquid knockout drum 10 to the top inlet of the low-pressure gas-liquid knockout drum 11 is provided with material conveying
Pipeline 20, is provided with the 7th valve 201 on the Location Detection of Medium Transportation Pipeline 20, be used to control the bottoms of high-pressure gas-liquid knockout drum 10
In material (liquid phase substance) input low-pressure gas-liquid knockout drum 11.
During the course of the reaction, the 7th valve 201 is closed, when the product of reaction generation is input into the high-pressure gas-liquid
After knockout drum 10, pressure and the reactor 7 and the institute in the high-pressure gas-liquid knockout drum 10 are adjusted by counterbalance valve 211 first
The pressure for stating cooler 9 is identical, then opens the 5th valve 181, will be from nitrogen cylinder 13 by the 3rd gas transmission line 18
In nitrogen be input into the low-pressure gas-liquid knockout drum 11 so that the pressure in low-pressure gas-liquid knockout drum 11 is separated with high-pressure gas-liquid
Pressure in tank 10 is identical, is then shut off the cut-out nitrogen of the 5th valve 181 and conveys and open the 7th valve 201 so that from height
Pressing the liquid phase substance of knockout drum 10 to be input under gravity carries out gas-liquid separation again in low-pressure gas-liquid knockout drum 11, treat
The 7th valve 201 is closed after pressure balance, the gaseous component from low-pressure gas-liquid knockout drum 11 is then passed through into gas phase sampling valve
221 and pipeline 23 to discharge a part to the pressure in low-pressure gas-liquid knockout drum 11 be 0.2MPa or so, then taken by gas phase
The gas phase export pipeline 22 of sample valve 221 and second is sampled analysis to gaseous component, then by gas phase sampling valve 221 and pipeline
23 are vented gaseous component, and analysis is then sampled to liquid phase component by liquid phase sampling valve 241, so as to realize that interval is separated
Analyzed with intermittent sampling.
The present invention is also provided and prepares gasoline component to mixing isomerization/aromatisation using foregoing catalyst test apparatus
The method that catalyst carries out evaluating catalyst,
The carrier gas unit includes nitrogen cylinder 13, the first gas transmission line 14, the second gas transmission line 19 and the 3rd gas transmission line
18；Methods described includes：
Before reaction, receive the nitrogen from nitrogen cylinder 13 using the first gas transmission line 14 and reaction member and separative element are entered
Row purging, to displace air, maintains the inert environments of system；
During the course of the reaction：
The nitrogen from the nitrogen cylinder 13 is conveyed using the second gas transmission line 19 to enter the raw liquefied petroleum gas tank 3
Row pressurising；
The nitrogen from the nitrogen cylinder 13 is conveyed using the 3rd gas transmission line 18 to enter the low-pressure gas-liquid knockout drum 11
Row pressurising.
In one embodiment, methods described also includes：
Before preheating raw material, after air is displaced completely, while heating system, continue to use nitrogen
Gas is purged to system, with the impurity on Removal of catalyst.
In one embodiment,
It is described including cooler 9, high-pressure gas-liquid knockout drum 10 and low-pressure gas-liquid knockout drum 11；The first gas phase efferent duct
Counterbalance valve 211 is provided with line 21；Is provided with the gas phase sampling valve 221 to the outlet side pipeline of the counterbalance valve 211
Three gas phase export pipelines 23；Liquid phase export pipeline 24, the liquid are provided with the outlet at bottom of the low-pressure gas-liquid knockout drum 11
The liquid phase sampling valve 241 for sampling analysis is provided with phase export pipeline 24；Methods described also includes：
In the separative element：
Cooled down using 9 pairs of gasoline products from the reaction member of cooler；
The material from the cooler 9 is received using high-pressure gas-liquid knockout drum 10, is then adjusted using the counterbalance valve 211
The pressure saved in the high-pressure gas-liquid knockout drum 10 is identical with the pressure of the reaction member, and gas-liquid separation is carried out with to it, row
Empty gaseous substance, obtains liquid phase substance；Then will be input into the low-pressure gas-liquid knockout drum 11 from the nitrogen in nitrogen cylinder 13
Pressure into low-pressure gas-liquid knockout drum 11 is identical with the pressure in high-pressure gas-liquid knockout drum 10, is then cut off nitrogen conveying, with
The liquid phase substance of high-pressure gas-liquid knockout drum 10 is set to export downwards under gravity；
Then the liquid phase substance from the high-pressure gas-liquid knockout drum 10 is received and to it using low-pressure gas-liquid knockout drum 11
Gas-liquid separation is carried out, gaseous component and liquid phase component for sampling analysis is obtained；Then gaseous component is sampled by gas phase
It is 0.1- that the gas phase export pipeline 23 of valve 221 and the 3rd discharges a part to the pressure in the low-pressure gas-liquid knockout drum 11
0.3MPa, is then sampled analysis to gaseous component by gas phase sampling valve 221；Then by gas phase sampling valve 221 and the
Be vented for gaseous component by three gas phase export pipelines 23, then analysis is sampled to liquid phase component by liquid phase sampling valve 241, so that
Realize that the interval of gas-liquid phase component is separated and intermittent sampling analysis.
When the catalyst that catalyst test apparatus of the invention are prepared gasoline component for mixing isomerization/aromatisation is commented
During valency, the material in feed naphtha tank 1 is naphtha, and the material in raw liquefied petroleum gas tank 3 is the liquefied gas of olefin-containing,
And this reaction is faced hydrogen and is reacted for pressurization.Now, the running of catalyst test apparatus is as follows：
The valve 131 ' of valve the 4th and the 4th pressure-reducing valve 132 ', the 8th valve 142, second flowmeter 141 are first turned on, will
High pure nitrogen from the nitrogen cylinder 13 is input into the second preheater 6 and is preheated, and then sequentially inputs reaction tube 7, cooling
Purged to reaction system and piece-rate system without air in device 9, high-pressure gas-liquid knockout drum 10 and low-pressure gas-liquid knockout drum 11；
Operation heating furnace 8 is heated to system while then proceeding to purging, and the beds in question response pipe 7 reach reaction temperature
After degree, the 7th valve 201 is closed, counterbalance valve 211 is adjusted to system demand pressure, then proceeded to be passed through nitrogen and be forced into close to system
The reaction pressure of system, closes the 4th valve 131 ', the 4th pressure-reducing valve 132 ', the 8th valve 142 and second flowmeter 141, if instead
During should carrying out, system pressure has declined, and is intermittently passed through nitrogen and ensures that system pressure is constant；Then will be from the stone brain
The liquid feedstock of oily head tank 1 is input into first preheater 5 through the first raw material pump 2 carries out preheating generation gasification naphtha,
Gas feed from the raw liquefied petroleum gas tank 3, the vaporization raw material from first preheater 5 and from the hydrogen
The hydrogen of gas cylinder 12 is input into the second preheater 6 and is preheated respectively, the control hydrogen input flow rate of first flowmeter 153；Come from
The material of the second preheater 6 is input into the reaction tube 7 and react being produced under the reaction temperature that heating furnace 8 is provided
Thing, is cooled down in the product input cooler 9 from reaction tube 7, and being then input into high-pressure gas-liquid knockout drum 10 carries out gas-liquid
Separate, isolate gaseous substance and liquid phase substance；Gaseous substance from high-pressure gas-liquid knockout drum 10 is through the first gas phase efferent duct
Line 21 and the counterbalance valve 211 being set in turn on the first gas phase export pipeline 21 discharge a part to maintain high-pressure gas-liquid point
Pressure in tank 10 is identical with the pressure of reactor 7 and the cooler 9；Then by the 3rd gas transmission line 18 to described low
Pressure knockout drum 11 in be input into nitrogen so that the pressure in low-pressure gas-liquid knockout drum 11 rise to in high-pressure gas-liquid knockout drum 10
Pressure it is identical, close the 5th valve 181 cut-out nitrogen conveying, open the 7th valve 201, from high-pressure gas-liquid knockout drum 10
Liquid phase substance is input under gravity carries out gas-liquid separation in low-pressure gas-liquid knockout drum 11, after closing the 7th after pressure balance
Valve 201, obtains gaseous component and liquid phase component；Then low-pressure gas-liquid knockout drum 11 is obtained by gas phase by gas phase sampling valve 221
Outlet and the UNICOM of the 3rd gas phase export pipeline 23, are then sampled the gaseous component from low-pressure gas-liquid knockout drum 11 by gas phase
Pressure in valve 221 and pipeline 23 to low-pressure gas-liquid knockout drum 11 is 0.1-0.3MPa (such as 0.2MPa), then by gas phase
The gas phase export pipeline 22 of sampling valve 221 and second is sampled analysis to gaseous component, then by gas phase sampling valve 221 and pipe
Be vented for gaseous component by line 23, and the reading of wet flow indicator 212 is used for computing system material balance；Then through liquid phase export pipeline 24
On liquid phase sampling valve 241 analysis is sampled to liquid phase component, and then by the intermittence to gaseous component and liquid phase component
Sampling analysis evaluation mixing isomerization/aromatisation prepares the catalyst of gasoline component.By continuous feed, realize to the catalyst
Activity and the life-span evaluation.
Mixing isomerization/aromatisation prepares the standard of the evaluating catalyst of gasoline component：
Continuous three times of olefin(e) centent then judges catalyst inactivation more than 20wt% in gas phase sampling, now needs to being catalyzed
Agent is regenerated or is changed；
The height of the selectivity of catalyst is judged by the content of isoparaffin/aromatic hydrocarbons in liquid phase sampling.
When catalyst test apparatus of the invention to be used for the evaluating catalyst of methanol oxidation alkene, feed naphtha
Liquid feedstock in tank 1 is the mixture of the methyl alcohol and water prepared in proportion, and raw liquefied petroleum gas tank 3 is not opened (need not
Gas feed).This reaction is reacted for normal pressure non-hydrogen.The running of catalyst test apparatus is as follows：
It is first shut off the 6th valve 191 and the second valve 171, opens the 4th valve 131 ' and the 4th pressure-reducing valve 132 ', the
Eight valves 142, second flowmeter 141, will be pre- from being carried out in the high pure nitrogen of the nitrogen cylinder 13 the second preheater 6 of input
Heat, then sequentially input purged in reaction tube 7, cooler 9, high-pressure gas-liquid knockout drum 10 and low-pressure gas-liquid knockout drum 11 to
Without air in reaction system and piece-rate system, due to being synthesis under normal pressure, therefore the 7th valve 201 is normally opened, and counterbalance valve 211 is not carried on the back
Pressure；Operation heating furnace 8 is heated to system while then proceeding to purging, and the beds in question response pipe 7 reach instead
After answering temperature, the 4th valve 131 ', the 4th pressure-reducing valve 132 ', the 8th valve 142 and second flowmeter 141 are closed；From described
The liquid feedstock of feed naphtha tank 1 is input into first preheater 5 through the first raw material pump 2 and is preheated, then is input into second
It is preheated in preheater 6 (wherein the first preheater 5 does not work)；Material input from the second preheater 6 is described anti-
Should react obtaining product in pipe 7 and under the reaction temperature that heating furnace 8 is provided, the product input cooling from reaction tube 7
Cooled down in device 9, being then input into high-pressure gas-liquid knockout drum 10 carries out gas-liquid separation, isolates gaseous substance and liquid phase thing
Matter；Gaseous substance from high-pressure gas-liquid knockout drum 10 is through the first gas phase export pipeline 21 and is arranged at the first gas phase output
Counterbalance valve 211 on pipeline 21 is vented；Liquid phase substance from high-pressure gas-liquid knockout drum 10 enters into low-pressure gas-liquid knockout drum 11
Row gas-liquid separation, obtains gaseous component and liquid phase component；Then gas phase sampling valve 221 is passed through by the gas of low-pressure gas-liquid knockout drum 11
Mutually outlet and the UNICOM of the second gas phase export pipeline 22, analysis is sampled to gaseous component through gas phase sampling valve 221, is then passed through
Be vented for gaseous component by gas phase sampling valve 221 and pipeline 23, and the reading of wet flow indicator 212 is used for computing system material balance；Through
Liquid phase sampling valve 241 on liquid phase export pipeline 24 is sampled analysis to liquid phase component, and then evaluates methanol oxidation alkene
Catalyst.
When catalyst test apparatus of the invention to be used for the evaluating catalyst of other reaction systems, it is only necessary to according to feelings
Condition is changed charging, is opened and the corresponding valve of closing, the corresponding charging of realization and pressure, you can carries out it according to actual conditions and urges
Agent is evaluated.
Catalyst test apparatus of the invention, have the advantage that：
(1) process is simple, easy to operate, control is steady, can simulate the industrial processes of respective reaction system, evaluates
It is more accurate；
(2) can be reacted by continuous feed, realize the continuous evaluation to the catalyst activity and life-span of respective reaction system；
(3) feed arrangement of multiple parallel connections is provided with due to feed system, such that it is able to pass through to control corresponding valve reality
Now to the switching of feed system, meet single feedstock and plurality of raw materials mixed feeding, optionally carry out facing hydrogen reaction with
Non-hydrogen reacts, and the evaluating catalyst of the reaction system of reaction etc. under pressurization and normal pressure, flexibility is strong；
(4) the evaluating catalyst work of polytype catalystic converter system is capable of achieving, such as methanol oxidation alkene, benzene add
Isomerization/aromatisation of hydrogen, aromatics isomerization, gasoline and diesel component etc. is reacted, such as prepared by mixing isomerization/aromatisation
The evaluating catalyst of gasoline component.
Claims (9)
1. a kind of catalyst test apparatus, it is characterised in that the catalyst test apparatus include：
Feed unit, the feed unit is including hydrogen cylinder (12), feed naphtha tank (1), for conveying the naphtha original
First raw material pump (2) of material, raw liquefied petroleum gas tank (3) in batch can (1), for conveying the raw liquefied petroleum gas tank
(3) the second raw material pump (4) of material, the first preheater (5) and the second preheater (6)；First preheater (5) is for adding
Material of the heat from the first raw material pump (2), to obtain the naphtha that gasifies, second preheater (6) comes from for heating
The material of the hydrogen cylinder (12), the second raw material pump (4) and the first preheater (5)；
Reaction member, the reaction member includes being provided with filling catalyst to be evaluated in reactor (7), the reactor (7)
Beds, and for preparing gasoline by raw material of the material from second preheater (6)；
Separative element, for being separated to the product from the reactor (7), to obtain the gas for sampling analysis
Phase component and liquid phase component.
2. catalyst test apparatus according to claim 1, it is characterised in that
The separative element includes：
Cooler (9), for receiving the product from the reactor (7) and being cooled down to it；
High-pressure gas-liquid knockout drum (10), for receiving the material from the cooler (9) and carrying out gas-liquid separation to it, obtains
Liquid phase substance；
Low-pressure gas-liquid knockout drum (11), for receiving the liquid phase substance from the high-pressure gas-liquid knockout drum (10) and being carried out to it
Gas-liquid separation, obtains gaseous component and liquid phase component.
3. catalyst test apparatus according to claim 2, it is characterised in that the catalyst test apparatus also include carrying
Gas unit, the carrier gas unit includes nitrogen cylinder (13), the first gas transmission line (14), the second gas transmission line (19) and the 3rd gas transmission
Pipeline (18), wherein, the first gas transmission line (14) is for conveying the nitrogen from the nitrogen cylinder (13) to the reaction member
Purged with separative element；Second gas transmission line (19) is for conveying the nitrogen from the nitrogen cylinder (13) to described
Raw liquefied petroleum gas tank (3) carries out pressurising；3rd gas transmission line (18) is for conveying from the nitrogen cylinder (13)
Nitrogen carries out pressurising to the low-pressure gas-liquid knockout drum (11).
4. catalyst test apparatus according to claim any one of 1-3, it is characterised in that the reaction member also includes
Heating furnace (8), the reactor (7) is tubular reactor, and the heating furnace (8) is sheathed on the reactor (7), for right
The reactor (7) is heated.
5. catalyst test apparatus according to claim 4, it is characterised in that be exported to institute from the hydrogen cylinder (12)
The entrance for stating the second preheater (6) is provided with hydrogen delivery tube line (15), and the hydrogen delivery tube line (15) is provided with first-class
Gauge (153)；
First gas transmission line (14) is provided with second flowmeter (141).
6. catalyst test apparatus according to any one of claim 2,3 or 5, it is characterised in that
The first gas phase export pipeline (21), first gas phase are provided with the gaseous phase outlet of the high-pressure gas-liquid knockout drum (10)
Counterbalance valve (211) and wet flow indicator (212) are disposed with export pipeline (21)；
The second gas phase export pipeline (22), second gas phase are provided with the gaseous phase outlet of the low-pressure gas-liquid knockout drum (11)
The gas phase sampling valve (221) for sampling analysis is provided with export pipeline (22)；The gas phase sampling valve (221) is threeway
Valve；
The 3rd gas phase export pipeline is provided with the gas phase sampling valve (221) to the outlet side pipeline of the counterbalance valve (211)
(23)；Liquid phase export pipeline (24), the liquid phase efferent duct are provided with the outlet at bottom of the low-pressure gas-liquid knockout drum (11)
The liquid phase sampling valve (241) for sampling analysis is provided with line (24).
7. a kind of catalyst test apparatus using as described in claim any one of 1-6 are prepared to mixing isomerization/aromatisation
The method that the catalyst of gasoline component carries out evaluating catalyst, it is characterised in that the carrier gas unit includes nitrogen cylinder (13), the
One gas transmission line (14), the second gas transmission line (19) and the 3rd gas transmission line (18)；Methods described includes：
Before reaction, receive the nitrogen from nitrogen cylinder (13) using the first gas transmission line (14) and reaction member and separative element are entered
Row purging, to displace air, maintains the inert environments of system；
During the course of the reaction：
Using the second gas transmission line (19) nitrogen of the conveying from the nitrogen cylinder (13) to the raw liquefied petroleum gas tank (3)
Carry out pressurising；
Using the 3rd gas transmission line (18) nitrogen of the conveying from the nitrogen cylinder (13) to the low-pressure gas-liquid knockout drum (11)
Carry out pressurising.
8. method according to claim 7, it is characterised in that methods described also includes：
Before being preheated to raw material, after air is displaced completely, while heating to system, continuation nitrogen pair
System is purged, with the impurity on Removal of catalyst.
9. method according to claim 8, it is characterised in that the separative element includes cooler (9), high-pressure gas-liquid point
From tank (10) and low-pressure gas-liquid knockout drum (11)；Counterbalance valve (211) is provided with the first gas phase export pipeline (21)；It is described
The 3rd gas phase export pipeline (23) is provided with gas phase sampling valve (221) to the outlet side pipeline of the counterbalance valve (211)；It is described
Liquid phase export pipeline (24) is provided with the outlet at bottom of low-pressure gas-liquid knockout drum (11), is set on the liquid phase export pipeline (24)
It is equipped with the liquid phase sampling valve (241) for sampling analysis；Methods described also includes：
In the separative element：
The gasoline product from the reaction member is cooled down using cooler (9)；
The material from the cooler (9) is received using high-pressure gas-liquid knockout drum (10), then using the counterbalance valve (211)
The pressure adjusted in the high-pressure gas-liquid knockout drum (10) is identical with the pressure of the reaction member, to carry out gas-liquid point to it
From, gaseous substance is emptied, obtain liquid phase substance；Then the low-pressure gas-liquid will be input into from the nitrogen in nitrogen cylinder (13) to separate
It is identical with the pressure in high-pressure gas-liquid knockout drum (10) to the pressure in low-pressure gas-liquid knockout drum (11) in tank (11), it is then cut off
Nitrogen is conveyed, so that the liquid phase substance of high-pressure gas-liquid knockout drum (10) is exported downwards under gravity；
The liquid phase substance from the high-pressure gas-liquid knockout drum (10) is received using low-pressure gas-liquid knockout drum (11) and it is carried out
Gas-liquid separation, obtains the gaseous component and liquid phase component for sampling analysis；Then gaseous component is passed through into gas phase sampling valve
(221) and the 3rd gas phase export pipeline (23) discharge a part to the pressure in the low-pressure gas-liquid knockout drum (11) be 0.1-
0.3MPa, is then sampled analysis to gaseous component by gas phase sampling valve (221)；Then gas phase sampling valve (221) is passed through
Gaseous component is vented with the 3rd gas phase export pipeline (23), then liquid phase component is sampled by liquid phase sampling valve (241)
Analysis.
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| CN107632098A (en) * | 2017-08-31 | 2018-01-26 | 天津市鹏翔科技有限公司 | Continuous catalytic reaction dynamic monitor |
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| CN107831234A (en) * | 2017-12-01 | 2018-03-23 | 钦州学院 | Laboratory prepares the experimental provision of isooctane |
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| CN111965001A (en) * | 2019-05-20 | 2020-11-20 | 内蒙古伊利实业集团股份有限公司 | Liquid sample heat treatment device and method |
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| CN111983136A (en) * | 2020-07-30 | 2020-11-24 | 青岛惠城环保科技股份有限公司 | Melamine catalyst performance evaluation equipment |
| CN114609323A (en) * | 2020-12-09 | 2022-06-10 | 中国石油天然气集团有限公司 | Method for evaluating continuous reforming catalyst |
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