CN104419463B - A kind of light ends fractionation hydrogenation test apparatus and method - Google Patents
A kind of light ends fractionation hydrogenation test apparatus and method Download PDFInfo
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- CN104419463B CN104419463B CN201310397829.5A CN201310397829A CN104419463B CN 104419463 B CN104419463 B CN 104419463B CN 201310397829 A CN201310397829 A CN 201310397829A CN 104419463 B CN104419463 B CN 104419463B
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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
- C10G67/00—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only
- C10G67/02—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only plural serial stages only
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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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1037—Hydrocarbon fractions
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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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/40—Characteristics of the process deviating from typical ways of processing
- C10G2300/4006—Temperature
Abstract
A kind of light ends fractionation hydrogenation test apparatus and method, belong to course of reaction and possess the assay device technical field of heating and heat-obtaining function.Described double tube reactor is divided into internal layer and outer layer, internal layer is reaction member, being provided with in reactor thermocouple is placed in catalyst and filler centre, outer layer is temperature control unit, it is divided into heating, constant temperature, cooling three sections, every section is provided with conduction oil entrance and conduction oil outlet, circulating heat conduction oil respectively above-mentioned three sections of heat supplies or heat-obtaining ensures the properly functioning of the low temperature strong exothermal reactions such as light ends fractionation hydrogenation and removing alkynes, alkene.Apparatus of the present invention adopt double tube reactor stability contorting catalyst bed reaction temperature, analoging industrial device practical condition can be used for, process conditions steadily control, product property is reliable and stable, and test data can be used for the thermodynamics and kinetics research of light ends fractionation hydrogenation and removing alkynes, olefins reaction process.
Description
Technical field
The present invention relates to a kind of light ends fractionation hydrogenation test apparatus and method, belong to course of reaction and possess the assay device technical field of heating and heat-obtaining function.
Background technology
Hydrogenation catalyst possesses oil product lighting in petroleum refining with chemical industry, clean and increase economic efficiency, the important function of enhancing efficiency by relying on tapping internal latent power, its exploitation needs to carry out substantial amounts of test evaluation work with performance test, hydropyrolysis experiment is to evaluate catalyst activity, the sole mode of selectivity and stability, the process conditions of hydrogenation, the difference that catalyst and the requirement to assay device are understood according to raw oil character and target product there are differences, such as, low pressure can be divided into according to pressure rating, middle pressure, high pressure and supertension hydrogenation, heat absorption can be divided into according to heat, heat release and strong exothermal reaction, therefore, hydrogenation plant there are differences according to technical process, the exploitation and performance evaluation of hydrogenation catalyst need to set up a set of reliable and stable assay device targetedly according to test requirements document.
Light ends fractionation is because of rich in one or more in the monoolefine of C2～C5, alkadienes and alkynes, can not effectively comprehensively utilize, there is bigger economic loss and environmental pollution, its selective hydrogenation or full unifining process can effectively remove undesirable components therein, the hydrogenation process of low carbon number unsaturated hydrocarbons mostly is strong exothermal reaction, it is generally adopted the noble metal catalyst low temperature hydrogenations such as Pd, Au, Pt, the control of catalyst bed reaction temperature is a difficult problem, therefore, it is necessary to set up a set of reliable and stable assay device targetedly according to test requirements document.
CN102491864A discloses a kind of hydrogenation test apparatus.This device is applicable to carbon two carbon three selective hydrogenation test, it is made up of line compression air distribution system, material distribution response system, tail gas recycle three part, owing to raw material is that after this device of low-pressure gaseous charging adopts air to drive compressor compresses raw material, Gaseous materials measures laggard system through mass-flow gas meter, plant running stationarity is high, each reactor content composition is completely the same, and device fabrication cost declines.
CN201424455Y discloses a kind of petroleum distillate hydrofinishing, hydrocracking tests device.This device is applicable to fraction oil hydrogenation refining, the hydrogenation high temperature endothermic reaction such as cracking or gasoline and diesel hydrogenation refining desulfurization, being made up of feed unit, reaction member, condensation recovery unit three part, the gas circuit of device, oil circuit, system response temperature and pressure all can be controlled by microcomputer.
CN201842823U discloses a kind of hydrogenation test apparatus.This device has installed an air and liquid mixer additional between high score gas water filling port and aeration tower, make that water is gentle to be sufficiently mixed in blender, then pass through the secondary gas washing of aeration tower, reach the purpose of H2S and NH3 etc. in abundant washing high score gas, thus solving the problem of NH4 salt blocking gas circuit pipeline in device operating.
The hydrogenation test apparatus that above prior art relates to is not suitable for the strong exothermal reaction of light ends fractionation hydrogenation cold-starting, it is hydrogenated with for light ends fractionation, beds temperature rise is uncontrollable, the practical situation of the analoging industrial device production run that its technological process and hydrogenation process can not be similar to.
Summary of the invention
In order to overcome the deficiencies in the prior art, the present invention provides a kind of light ends fractionation hydrogenation test apparatus and method, it is hydrogenated with the strong exothermal reaction of cold-starting suitable in light ends fractionation, is specially lab scale or the pilot-plant of light ends fractionation selective hydrogenation or full hydrogenation effectively elimination wherein unsaturated hydro carbons undesirable components.
A kind of light ends fractionation hydrogenation test method, containing following steps；
In feed unit, hydrogen is pressed into double tube reactor by mass flowmenter metering after air relief valve reduces pressure；Light ends fractionation raw oil storage tank Raw is measured by electronic scale, air-actuated feeding pump squeeze into double tube reactor, and air-actuated feeding pump is to be driven by 0.2～0.5Mpa air；Double tube reactor 1 is divided into internal layer and outer layer, internal layer is used for loading catalyst and filler and is provided with the interior thermocouple of multiple mensuration bed temperature, outer layer is divided into preheating, constant temperature, cooling three sections, adopts circulating heat conduction oil respectively above-mentioned three sections of heat supplies or heat-obtaining from thermostatic bath to ensure the stability contorting of catalyst bed reaction temperature in hydrogenation process；Product by double tube reactor out after through condenser condense, and enter knockout drum separate, isolated gas is reduced pressure by system back pressure valve, and through wet gas flow meter measure after emptying；Level of condensate in liquid level shaker associating liquid level pneumatic control valve regulation knockout drum；The product liquid discharged by liquid level pneumatic control valve enters product storage tank, and can be sampled by fast sampling mouth；In process of the test, control whole system pressure with mass-flow gas meter and system back pressure valve, control the ratio of the alkene in hydrogen and reaction oil or reaction oil and/or alkynes with mass-flow gas meter and pneumatic feed pump；
The technological parameter index controlled is:
Single reactor catalyst loadings: 20mL-200mL, dilutes with inert ceramic balls；
Air speed: 0.5-10h-1；
Bed temperature: 5-250 DEG C；
Pressure: 0.5-5.0Mpa
Hydrogen and oil or hydrogen and wherein unsaturated hydrocarbons mol ratio: 1:1-50:1
Adopting double tube reactor reaction bed temperature to control, strong exothermal reaction carries out on hotbed waiting, removes alkynes for C-4-fraction low temperature hydrogenation and alkadienes is tested, at the catalyst stability of 500h, reaction pressure 2.0Mpa, feed volume air speed 2.5h-1, hydrogen/(alkynes+alkadienes) mol ratio 2～5, bed reaction temperature 28～32 DEG C, thermostatic bath the circulating heat conduction oil temperature controlled is 25～28 DEG C, and in whole process of the test, the fluctuating margin of reaction bed temperature is less than 0.5 DEG C.
A kind of light ends fractionation hydrogenation test apparatus, including feed unit, reaction and temperature control unit, gas-liquid separation unit, product sampling and recovery unit,
(1) in the feed unit described in, hydrogen feed system includes successively, air relief valve, hydrogen quality effusion meter, hydrogen gas buffer, check valve；Lighter hydrocarbons feed system includes successively, electronic scale, light hydrocarbon feedstocks tank, filter, air-actuated feeding pump；
The particular content of feed unit is, hydrogen quality effusion meter range is 0～16L/h, for small-range effusion meter；Electronic scale range is 0～30Kg, and precision is not less than 5g；Air-actuated feeding pump needs 0.2～0.5Mpa air to drive, and range ability is 0～600g/h；
(2) reaction described in and temperature control unit include thermocouple in double tube reactor, reactor, conduction oil entrance, conduction oil outlet, thermostatic bath；
The structure of reaction and temperature control unit is, double tube reactor is divided into internal layer and outer layer, internal layer is reaction member, being provided with in reactor thermocouple is placed in catalyst and filler centre, outer layer is temperature control unit, being divided into heating, constant temperature, cooling three sections, every section is provided with conduction oil entrance and conduction oil outlet；
The number of described double tube reactor is 1-5, can adopt connection in series or in parallel between reactor, and the low temperature hydrogenation parallel test of the light-end products generally parallel waies adopting two reactors connect more；
Described circulating heat conduction oil is by thermostatic bath regulating and controlling temperature, and conduction oil flows out from thermostatic bath, conduction oil entrance respectively enter the bringing-up section of double tube reactor, constant temperature zone and/or cooling section, and flowed back to thermostatic bath by conduction oil outlet；
Constant temperature zone bath and cooling section bath can be merged use when adopting single reactor by described thermostatic bath, at least need 2 baths, at least need 3 baths when adopting two reactor parallel connections；
(3) gas-liquid separation unit described in includes, condenser, system back pressure valve, knockout drum, liquid level shaker, liquid level pneumatic control valve；
The structure of gas-liquid separation unit is, the material outlet of double tube reactor is sequentially connected with condenser, knockout drum, material is divided into gas circuit and oil circuit after knockout drum, and gas circuit is controlled by system back pressure valve, and oil circuit is jointly controlled by liquid level pneumatic control valve and liquid level shaker；
(4) the product sampling described in includes with recovery unit, fast sampling mouth, product storage tank, wet gas flow meter；
Wet gas flow meter, the emptying after wet gas flow meter measures of test tail gas it is connected to after described system back pressure valve；
The concrete structure of product sampling and recovery unit is be connected to product storage tank after described liquid level pneumatic control valve, and product storage tank is provided with atmospheric valve, is provided with snap joint sample tap before material enters product storage tank；
By computer aided control system, hydrogen quality effusion meter, system back pressure valve, liquid level pneumatic control valve are controlled；
Pressure hydrogen quality effusion meter and system back pressure valve control；
Described reaction temperature thermostatic bath control；
Described feed volume air speed air-actuated feeding pump controls；
The mol ratio hydrogen quality effusion meter of described hydrogen and alkynes and pneumatic feed pump control.
It is an advantage of the invention that the low temperature hydrogenation strong exothermal reaction for light ends fractionation, solve and beds big with the conventional hydro device charging poor stability of heating furnace, system pressure fluctuation and cause especially greatly because of temperature rise the reaction temperature cannot the problem such as stability contorting.
Apparatus of the present invention adopt double tube reactor stability contorting catalyst bed reaction temperature, analoging industrial device practical condition can be used for, process conditions steadily control, product property is reliable and stable, and test data can be used for the thermodynamics and kinetics research of light ends fractionation hydrogenation and removing alkynes, olefins reaction process.
Accompanying drawing explanation
When considered in conjunction with the accompanying drawings, by referring to detailed description below, can more completely be more fully understood that the present invention and easily learn the advantage that many of which is adjoint, but accompanying drawing described herein is used for providing a further understanding of the present invention, constitute the part of the present invention, the schematic description and description of the present invention is used for explaining the present invention, is not intended that inappropriate limitation of the present invention, such as figure wherein:
Fig. 1 is the structural representation of the present invention.
Fig. 2 is the structural representation of the present invention.
Below in conjunction with drawings and Examples, the present invention is further described.
Detailed description of the invention
Obviously, the many modifications and variations that those skilled in the art do based on the objective of the present invention belong to protection scope of the present invention.
Embodiment 1: as shown in Figure 1 and Figure 2, a kind of light ends fractionation hydrogenation test apparatus, double tube reactor 1；Thermocouple 2 in reactor；Conduction oil entrance 3；Conduction oil outlet 4；Thermostatic bath 5；Air relief valve 6；Hydrogen quality effusion meter 7；Hydrogen gas buffer 8；Check valve 9；Suspended body flowmeter 10；Electronic scale 11；Light hydrocarbon feedstocks tank 12；Filter 13；Air-actuated feeding pump 14；Condenser 15；System back pressure valve 16；Wet gas flow meter 17；Knockout drum 18；Liquid level shaker 19；Liquid level pneumatic control valve 20；Fast sampling mouth 21；Product storage tank 22.
The light ends fractionation hydrogenation test apparatus of the present invention is achieved in that
A kind of light ends fractionation hydrogenation test apparatus that is used for includes feed unit, reaction and temperature control unit, gas-liquid separation unit, product sampling and recovery unit successively, it is characterised in that:
(1) in the feed unit described in, hydrogen feed system includes successively, air relief valve 6, hydrogen quality effusion meter 7, hydrogen gas buffer 8, check valve 9；Lighter hydrocarbons feed system includes successively, electronic scale 11, light hydrocarbon feedstocks tank 12, filter 13, air-actuated feeding pump 14.
The particular content of feed unit is, hydrogen quality effusion meter 7 range is 0～16L/h, for small-range effusion meter；Electronic scale 11 range is 0～30Kg, and precision is not less than 5g；Air-actuated feeding pump 14 needs 0.2～0.5Mpa air to drive, and range ability is 0～600g/h.
(2) reaction described in and temperature control unit include, thermocouple 2, conduction oil entrance 3, conduction oil outlet 4, thermostatic bath 5 in double tube reactor 1, reactor.
The particular content of reaction and temperature control unit is, double tube reactor 1 is divided into internal layer and outer layer, internal layer is reaction member, being provided with in reactor thermocouple 2 is placed in catalyst and filler centre, outer layer is temperature control unit, being divided into heating, constant temperature, cooling three sections, every section is provided with conduction oil entrance 3 and conduction oil outlet 4, circulating heat conduction oil respectively above-mentioned three sections of heat supplies or heat-obtaining ensures the properly functioning of light ends fractionation hydrogenation and removing alkynes, alkene test.
The number of described double tube reactor 1 is 1-5, can adopt connection in series or in parallel between reactor, and the low temperature hydrogenation parallel test of the light-end products generally parallel waies adopting two reactors connect more.
Described thermostatic bath 5 temperature adjusting ranges for-250 DEG C～250 DEG C, reaction temperature energy stability contorting in the process evaluation experiment process, and temperature fluctuation range is ± 0.5 DEG C；Constant temperature zone bath and cooling section bath can be merged use when adopting single reactor by described thermostatic bath 5, at least need 2 baths, at least need 3 baths when adopting two reactor parallel connections.
(3) gas-liquid separation unit described in includes, condenser 15, system back pressure valve 16, knockout drum 18, liquid level shaker 19, liquid level pneumatic control valve 20.
The particular content of gas-liquid separation unit is, the material outlet of double tube reactor is sequentially connected with condenser 15, knockout drum 18, material is divided into gas circuit and oil circuit after knockout drum, and gas circuit is controlled by system back pressure valve 16, and oil circuit is jointly controlled by liquid level pneumatic control valve 20 and liquid level shaker 19.
(4) the product sampling described in includes with recovery unit, fast sampling mouth 21, product storage tank 22, wet gas flow meter 17；
Wet gas flow meter 17, the emptying after wet gas flow meter 17 measures of test tail gas it is connected to after described system back pressure valve 16；
The particular content of product sampling and recovery unit is be connected to product storage tank 22 after described liquid level pneumatic control valve 20, and product storage tank 23 is provided with atmospheric valve, is provided with snap joint sample tap 21 before material enters product storage tank 22.
A kind of light ends fractionation hydrogenation test apparatus is connected with computer aided control system, computer aided control system hydrogen quality effusion meter, system back pressure valve, liquid level pneumatic control valve are controlled.
Described whole system pressure hydrogen quality effusion meter 7 and system back pressure valve 16 control；
Described reaction temperature thermostatic bath 5 controls；
Described feed volume air speed air-actuated feeding pump 14 controls；
Mol ratio hydrogen quality effusion meter 7 and the pneumatic feed pump 14 of described hydrogen and alkynes control.
Light ends fractionation hydrogenation test apparatus of the present invention includes feed unit, reaction and temperature control unit, gas-liquid separation unit, product sampling and recovery unit successively, and its specific implementation process is such that
In feed unit, hydrogen is measured press-in double tube reactor 1 by mass flowmenter 7 after air relief valve 6 reduces pressure.Light ends fractionation raw oil storage tank 12 Raw is measured by electronic scale 11, air-actuated feeding pump 14 squeeze into double tube reactor 1, and air-actuated feeding pump is to be driven by 0.2～0.5Mpa air.Double tube reactor 1 is divided into internal layer and outer layer, internal layer is used for loading catalyst and filler and is provided with the interior thermocouple 2 of multiple mensuration bed temperature, outer layer is divided into preheating, constant temperature, cooling three sections, adopts circulating heat conduction oil respectively above-mentioned three sections of heat supplies or heat-obtaining from thermostatic bath 5 to ensure the stability contorting of catalyst bed reaction temperature in hydrogenation process.Product by double tube reactor 1 out after condense through condenser 15, and enter knockout drum 18 and separate, isolated gas is reduced pressure by system back pressure valve 16, and emptying after wet gas flow meter 17 measures.Liquid level shaker 19 is combined liquid level pneumatic control valve 20 and is regulated the level of condensate in knockout drum 18.The product liquid discharged by liquid level pneumatic control valve 20 enters product storage tank 22, and can be sampled by fast sampling mouth 21.In process of the test, control whole system pressure with mass-flow gas meter 7 and system back pressure valve 16, control the ratio of the alkene in hydrogen and reaction oil or reaction oil and/or alkynes with mass-flow gas meter 7 and pneumatic feed pump 14.
The controllable technological parameter index of this device is:
Single reactor catalyst loadings: 20mL-200mL, dilutes with inert ceramic balls；
Air speed: 0.5-10h-1；
Bed temperature: 5-250 DEG C；
Pressure: 0.5-5.0Mpa；
Hydrogen and oil or hydrogen and wherein unsaturated hydrocarbons mol ratio: 1:1-50:1；
Owing to adopting double tube reactor reaction bed temperature precise control and almost without temperature rise, namely strong exothermal reaction carries out on hotbed waiting, adopt general isothermal bed bioreactor when device stability controls poor, bed reaction temperature rising is higher than 40 DEG C, and the stability deficiency of control causes product property fluctuation big, unreliable.Apparatus of the present invention are for C-4-fraction low temperature hydrogenation elimination alkynes and alkadienes test, and in the catalyst stability of 500h is investigated, process regulation is steady, reaction pressure 2.0Mpa, feed volume air speed 2.5h-1Hydrogen/(alkynes+alkadienes) mol ratio 2～5, bed reaction temperature 28～32 DEG C, thermostatic bath the circulating heat conduction oil temperature controlled is 25～28 DEG C, in whole process of the test, the fluctuating margin of reaction bed temperature is less than 0.5 DEG C, investigates result and sees following table:
A kind of light ends fractionation hydrogenation test apparatus, described double tube reactor 1 is divided into internal layer and outer layer, internal layer is reaction member, being provided with in reactor thermocouple 2 is placed in catalyst and filler centre, outer layer is temperature control unit, being divided into heating, constant temperature, cooling three sections, every section is provided with conduction oil entrance 3 and conduction oil outlet 4, circulating heat conduction oil respectively above-mentioned three sections of heat supplies or heat-obtaining ensures the properly functioning of the low temperature strong exothermal reactions such as light ends fractionation hydrogenation and removing alkynes, alkene.
Described circulating heat conduction oil is by thermostatic bath 5 regulating and controlling temperature, and conduction oil flows out from thermostatic bath, conduction oil entrance 3 respectively enter the bringing-up section of double tube reactor, constant temperature zone and/or cooling section, and flowed back to thermostatic bath 5 by conduction oil outlet 4.
Described thermostatic bath 5 carries circulating pump and controls circulating of conduction oil, and its temperature adjusting ranges for-50 DEG C～250 DEG C, reaction temperature energy stability contorting in the process evaluation experiment process, and temperature fluctuation range is ± 0.5 DEG C.
The number of described double tube reactor 1 is 1-5, can adopt connection in series or in parallel between reactor, and the low temperature hydrogenation parallel test of the light ends fractionation generally parallel waies adopting two reactors connect more.
When adopting single reactor to test, the constant temperature zone of double tube reactor and cooling section can be connected a public thermostatic bath 5, and assay device has only to 2 baths can stability contorting catalyst bed reaction temperature；When adopting two reactor parallel connections to carry out parallel test, a public thermostatic bath 5 of can the bringing-up section of two double tube reactors being connected, the test of reactor in-parallel at least needs 3 baths.
A kind of light ends fractionation hydrogenation test method, containing following steps；
In feed unit, hydrogen is measured press-in double tube reactor 1 by mass flowmenter 7 after air relief valve 6 reduces pressure；Light ends fractionation raw oil storage tank 12 Raw is measured by electronic scale 11, air-actuated feeding pump 14 squeeze into double tube reactor 1, and air-actuated feeding pump is to be driven by 0.2～0.5Mpa air；Double tube reactor 1 is divided into internal layer and outer layer, internal layer is used for loading catalyst and filler and is provided with the interior thermocouple 2 of multiple mensuration bed temperature, outer layer is divided into preheating, constant temperature, cooling three sections, adopts circulating heat conduction oil respectively above-mentioned three sections of heat supplies or heat-obtaining from thermostatic bath 5 to ensure the stability contorting of catalyst bed reaction temperature in hydrogenation process；Product by double tube reactor 1 out after condense through condenser 15, and enter knockout drum 18 and separate, isolated gas is reduced pressure by system back pressure valve 16, and emptying after wet gas flow meter 17 measures；Liquid level shaker 19 is combined liquid level pneumatic control valve 20 and is regulated the level of condensate in knockout drum 18；The product liquid discharged by liquid level pneumatic control valve 20 enters product storage tank 22, and can be sampled by fast sampling mouth 21；In process of the test, control whole system pressure with mass-flow gas meter 7 and system back pressure valve 16, control the ratio of the alkene in hydrogen and reaction oil or reaction oil and/or alkynes with mass-flow gas meter 7 and pneumatic feed pump 14；
The technological parameter index controlled is:
Single reactor catalyst loadings: 20mL-200mL, dilutes with inert ceramic balls；
Air speed: 0.5-10h-1；
Bed temperature: 5-250 DEG C；
Pressure: 0.5-5.0Mpa；
Hydrogen and oil or hydrogen and wherein unsaturated hydrocarbons mol ratio: 1:1-50:1；
Adopting double tube reactor reaction bed temperature to control, strong exothermal reaction carries out on hotbed waiting, removes alkynes for C-4-fraction low temperature hydrogenation and alkadienes is tested, at the catalyst stability of 500h, reaction pressure 2.0Mpa, feed volume air speed 2.5h-1, hydrogen/(alkynes+alkadienes) mol ratio 2～5, bed reaction temperature 28～32 DEG C, thermostatic bath the circulating heat conduction oil temperature controlled is 25～28 DEG C, and in whole process of the test, the fluctuating margin of reaction bed temperature is less than 0.5 DEG C.
As it has been described above, embodiments of the invention have been explained, but as long as can have a lot of deformation essentially without the inventive point and effect that depart from the present invention, this will be readily apparent to persons skilled in the art.Therefore, such variation is also integrally incorporated within protection scope of the present invention.
Claims (6)
1. a light ends fractionation hydrogenation test method, it is characterised in that containing following steps；
In feed unit, hydrogen is pressed into double tube reactor by mass flowmenter metering after air relief valve reduces pressure；Light ends fractionation raw oil storage tank Raw is measured by electronic scale, air-actuated feeding pump squeeze into double tube reactor, and air-actuated feeding pump is to be driven by 0.2～0.5Mpa air；Double tube reactor (1) is divided into internal layer and outer layer, internal layer is used for loading catalyst and filler and is provided with the interior thermocouple of multiple mensuration bed temperature, outer layer is divided into preheating, constant temperature, cooling three sections, adopts circulating heat conduction oil respectively above-mentioned three sections of heat supplies or heat-obtaining from thermostatic bath to ensure the stability contorting of catalyst bed reaction temperature in hydrogenation process；Product by double tube reactor out after through condenser condense, and enter knockout drum separate, isolated gas is reduced pressure by system back pressure valve, and through wet gas flow meter measure after emptying；Level of condensate in liquid level shaker associating liquid level pneumatic control valve regulation knockout drum；The product liquid discharged by liquid level pneumatic control valve enters product storage tank, and can be sampled by fast sampling mouth；In process of the test, control whole system pressure with mass-flow gas meter and system back pressure valve, control the ratio of the alkene in hydrogen and reaction oil or reaction oil and/or alkynes with mass-flow gas meter and pneumatic feed pump.
2. a kind of light ends fractionation hydrogenation test method according to claim 1, it is characterised in that the technological parameter index of control is:
Single reactor catalyst loadings: 20mL-200mL, dilutes with inert ceramic balls；
Air speed: 0.5-10h-1；
Bed temperature: 5-250 DEG C；
Pressure: 0.5-5.0Mpa
Hydrogen and oil or hydrogen and wherein unsaturated hydrocarbons mol ratio: 1:1-50:1
Adopting double tube reactor reaction bed temperature to control, strong exothermal reaction carries out on hotbed waiting, removes alkynes for C-4-fraction low temperature hydrogenation and alkadienes is tested, at the catalyst stability of 500h, reaction pressure 2.0Mpa, feed volume air speed 2.5h-1, hydrogen/(alkynes+alkadienes) mol ratio 2～5, bed reaction temperature 28～32 DEG C, thermostatic bath the circulating heat conduction oil temperature controlled is 25～28 DEG C, and in whole process of the test, the fluctuating margin of reaction bed temperature is less than 0.5 DEG C.
3. a light ends fractionation hydrogenation test apparatus, it is characterised in that include feed unit, reaction and temperature control unit, gas-liquid separation unit, product sampling and recovery unit,
(1) in the feed unit described in, hydrogen feed system includes successively, air relief valve, hydrogen quality effusion meter, hydrogen gas buffer, check valve；Lighter hydrocarbons feed system includes successively, electronic scale, light hydrocarbon feedstocks tank, filter, air-actuated feeding pump；
The particular content of feed unit is, hydrogen quality effusion meter range is 0～16L/h, for small-range effusion meter；Electronic scale range is 0～30Kg, and precision is not less than 5g；Air-actuated feeding pump needs 0.2～0.5Mpa air to drive, and range ability is 0～600g/h；
(2) reaction described in and temperature control unit include thermocouple in double tube reactor, reactor, conduction oil entrance, conduction oil outlet, thermostatic bath；
The structure of reaction and temperature control unit is, double tube reactor is divided into internal layer and outer layer, internal layer is reaction member, being provided with in reactor thermocouple is placed in catalyst and filler centre, outer layer is temperature control unit, being divided into heating, constant temperature, cooling three sections, every section is provided with conduction oil entrance and conduction oil outlet；
(3) gas-liquid separation unit described in includes, condenser, system back pressure valve, knockout drum, liquid level shaker, liquid level pneumatic control valve；
The structure of gas-liquid separation unit is, the material outlet of double tube reactor is sequentially connected with condenser, knockout drum, material is divided into gas circuit and oil circuit after knockout drum, and gas circuit is controlled by system back pressure valve, and oil circuit is jointly controlled by liquid level pneumatic control valve and liquid level shaker；
(4) the product sampling described in includes with recovery unit, fast sampling mouth, product storage tank, wet gas flow meter；
Wet gas flow meter, the emptying after wet gas flow meter measures of test tail gas it is connected to after described system back pressure valve.
4. a kind of light ends fractionation hydrogenation test apparatus according to claim 3, it is characterized in that the number of described double tube reactor is 1-5, can adopting connection in series or in parallel between reactor, the low temperature hydrogenation parallel test of light-end products adopts the parallel way of two reactors to connect；
Described conduction oil is by thermostatic bath regulating and controlling temperature, and conduction oil flows out from thermostatic bath, conduction oil entrance respectively enter the bringing-up section of double tube reactor, constant temperature zone and/or cooling section, and flowed back to thermostatic bath by conduction oil outlet；
Constant temperature zone bath and cooling section bath can be merged use when adopting single reactor by described thermostatic bath, at least need 2 baths, at least need 3 baths when adopting two reactor parallel connections.
5. a kind of light ends fractionation hydrogenation test apparatus according to claim 3, it is characterized in that the concrete structure of product sampling and recovery unit is, it is connected to product storage tank after described liquid level pneumatic control valve, product storage tank is provided with atmospheric valve, is provided with snap joint sample tap before material enters product storage tank.
6. a kind of light ends fractionation hydrogenation test apparatus according to claim 3, it is characterised in that hydrogen quality effusion meter, system back pressure valve, liquid level pneumatic control valve are controlled by computer aided control system；
Pressure hydrogen quality effusion meter and system back pressure valve control；
Described reaction temperature thermostatic bath control；
Described feed volume air speed air-actuated feeding pump controls；
The mol ratio hydrogen quality effusion meter of described hydrogen and alkynes and pneumatic feed pump control.
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| CN107488460A (en) * | 2016-06-12 | 2017-12-19 | 中国石油化工股份有限公司 | A kind of light ends fractionation hydrogenation plant |
| CN109107497A (en) * | 2017-06-23 | 2019-01-01 | 中国石油化工股份有限公司 | A kind of hydrogenation reaction of unsaturated hydrocarbon device |
| CN107674703B (en) * | 2017-11-07 | 2019-10-22 | 河北新启元能源技术开发股份有限公司 | Reaction feed temperature control equipment in a kind of coal tar hydrogenating |
| CN107741468B (en) * | 2017-11-09 | 2021-01-22 | 中国科学院电工研究所 | Magneto-optic thermal synergistic catalyst evaluation device |
| CN108440281B (en) * | 2018-03-16 | 2021-03-02 | 上海载正化工科技发展有限公司 | Chemical reaction device and application thereof |
| CN109404718B (en) * | 2018-12-13 | 2023-12-19 | 国能龙源环保有限公司 | System and method for reducing VOCs emission and sealed nitrogen consumption of oil storage tank |
| CN110849023B (en) * | 2019-11-01 | 2021-02-02 | 西安交通大学 | Combined cooling, heating and power system and method for compressed air and thermochemical coupling energy storage |
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| CN201842823U (en) * | 2010-11-05 | 2011-05-25 | 中国石油化工股份有限公司 | Hydrogenation test device |
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