CN203513598U - Light hydrocarbon fraction hydrogenation test device - Google Patents
Light hydrocarbon fraction hydrogenation test device Download PDFInfo
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- CN203513598U CN203513598U CN201320548003.XU CN201320548003U CN203513598U CN 203513598 U CN203513598 U CN 203513598U CN 201320548003 U CN201320548003 U CN 201320548003U CN 203513598 U CN203513598 U CN 203513598U
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- 238000005984 hydrogenation reaction Methods 0.000 title claims abstract description 41
- 238000012360 testing method Methods 0.000 title claims abstract description 41
- 229930195733 hydrocarbon Natural products 0.000 title claims abstract description 12
- 150000002430 hydrocarbons Chemical class 0.000 title claims abstract description 11
- 239000004215 Carbon black (E152) Substances 0.000 title claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 41
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000000945 filler Substances 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims description 33
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 21
- 238000005194 fractionation Methods 0.000 claims description 19
- 239000007789 gas Substances 0.000 claims description 19
- 229910052739 hydrogen Inorganic materials 0.000 claims description 17
- 239000001257 hydrogen Substances 0.000 claims description 17
- 238000005070 sampling Methods 0.000 claims description 15
- 238000011084 recovery Methods 0.000 claims description 11
- 238000000926 separation method Methods 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 9
- 230000008878 coupling Effects 0.000 claims description 3
- 238000010168 coupling process Methods 0.000 claims description 3
- 238000005859 coupling reaction Methods 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 abstract description 12
- 238000000034 method Methods 0.000 abstract description 11
- 230000008569 process Effects 0.000 abstract description 11
- 150000001345 alkine derivatives Chemical class 0.000 abstract description 8
- 150000001336 alkenes Chemical class 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000011160 research Methods 0.000 abstract description 2
- -1 acetylene hydrocarbon Chemical class 0.000 abstract 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 abstract 1
- 238000003795 desorption Methods 0.000 abstract 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 abstract 1
- 239000000047 product Substances 0.000 description 22
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- 229930195735 unsaturated hydrocarbon Natural products 0.000 description 3
- 238000004517 catalytic hydrocracking Methods 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000008030 elimination Effects 0.000 description 2
- 238000003379 elimination reaction Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
A light hydrocarbon fraction hydrogenation test device belongs to the technical field of test devices with heating and heat-taking functions in the reaction process. The sleeve type reactor is divided into an inner layer and an outer layer, the inner layer is a reaction unit and is provided with a thermocouple arranged in the middle of a catalyst and a filler, the outer layer is a temperature control unit and is divided into three sections of heating, constant temperature and cooling, each section is provided with a heat conduction oil inlet and a heat conduction oil outlet, and circulating heat conduction oil supplies heat to the three sections or heats the three sections respectively to ensure the normal operation of low-temperature strong exothermic reactions such as acetylene hydrocarbon and olefin removal through hydrogenation of light hydrocarbon fractions. The utility model discloses the device adopts sleeve type reactor stable control catalyst bed reaction temperature, can be used for simulating the industrial unit actual production condition, and process conditions stable control, product nature reliable and stable, experimental data can be used to light hydrocarbon fraction hydrogenation desorption alkyne, alkene reaction process's thermodynamics and dynamics research.
Description
Technical field
The utility model relates to a kind of light ends fractionation hydrogenation test apparatus, belongs to the testing apparatus technical field that reaction process possesses heating and heat-obtaining function.
Background technology
Hydrogenation catalyst possesses oil product lighting in refining of petroleum and chemical industry, clean and increase economic efficiency, the vital role of enhancing efficiency by relying on tapping internal latent power, its exploitation need to be carried out a large amount of test evaluation work with performance test, hydropyrolysis experiment is evaluation of catalyst activity, the sole mode of selectivity and stability, the processing condition of hydrogenation, catalyzer and the requirement meeting of testing apparatus be there are differences according to the difference of stock oil character and target product, for example, according to pressure rating, can be divided into low pressure, middle pressure, high pressure and ultra-high voltage hydrogenation, according to heat, can be divided into heat absorption, heat release and strong exothermal reaction, therefore, hydrogenation unit there are differences according to technological process, in the exploitation of hydrogenation catalyst and performance evaluation, need to set up targetedly a set of reliable and stable testing apparatus according to test requirements document.
Light ends fractionation is because being rich in one or more in monoolefine, diolefine and the alkynes of C2～C5, can not effectively fully utilize, there is larger financial loss and environmental pollution, its selective hydrogenation or full unifining process can effective elimination undesirable components wherein, the hydrogenation process of low carbon number unsaturated hydrocarbons mostly is strong exothermal reaction, the general noble metal catalyst low temperature hydrogenations such as Pd, Au, Pt that adopt, the control of catalyst bed reaction temperature is a difficult problem, therefore, be necessary to set up targetedly a set of reliable and stable testing apparatus according to test requirements document.
CN102491864A discloses a kind of hydrogenation test apparatus.This device is applicable to carbon two carbon three selective hydrogenation tests, by line compression gas distributing system, material, distribute reactive system, tail gas recycle three parts to form, because raw material is that after this device of low pressure gaseous feed adopts air actuation compressor compresses raw material, gaseous state material measures laggard system through mass-flow gas meter, device running stability is high, each reactor content forms in full accord, and device fabrication cost declines.
CN201424455Y discloses a kind of petroleum fractions hydrofining, hydrocracking testing apparatus.This device is applicable to the high temperature thermo-negative reaction such as fraction oil hydrogenation refining, hydrocracking or gasoline and diesel hydrogenation refining desulfurization, feed unit, reaction member, condensation recovery unit three parts, consist of, the gas circuit of device, oil circuit, system response temperature and pressure all can pass through microcomputer control.
CN201842823U discloses a kind of hydrogenation test apparatus.This device has installed a gas liquid mixer additional between high score gas water filling port and scrubber tower, makes the gentle fully mixing in mixing tank of water, then, by the secondary gas washing of scrubber tower, has reached the H in abundant washing high score gas
2s and NH
3deng object, thereby solved NH in device running
4salt stops up the problem of gas circuit pipeline.
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, for light ends fractionation hydrogenation, beds temperature rise is uncontrollable, the practical situation of the analoging industrial device production run that its technical process and hydrogenation process can not be approximate.
Summary of the invention
In order to overcome the deficiencies in the prior art, the utility model provides a kind of light ends fractionation hydrogenation test apparatus, be applicable to the strong exothermal reaction of light ends fractionation hydrogenation cold-starting, be specially light ends fractionation selective hydrogenation or full hydrogenation effective elimination wherein lab scale or the pilot plant of unsaturated hydro carbons undesirable components.
A kind of light ends fractionation hydrogenation test apparatus, comprise feed unit, reaction and temperature control unit, gas-liquid separation unit, product sampling and recovery unit, in feed unit, hydrogen feed system comprises reducing valve, hydrogen quality under meter, hydrogen gas buffer, check valve successively; Lighter hydrocarbons feed system comprises successively, electronic scales, light hydrocarbon feedstocks tank, strainer, air-actuated feeding pump; Reaction comprises thermopair in double tube reactor, reactor, thermal oil entrance, thermal oil outlet, thermostatic bath with temperature control unit; Reaction with the structure of temperature control unit is: double tube reactor is divided into internal layer and skin, internal layer is reaction member, be provided with thermopair in reactor and be placed in catalyzer and filler centre, skin is temperature control unit, heating, constant temperature, cooling three sections be respectively equipped with thermal oil entrance and thermal oil outlet; Gas-liquid separation unit comprises 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 connects condenser, knockout drum successively, material is divided into gas circuit and oil circuit after knockout drum, 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; Product sampling comprises fast sampling mouth, product storage tank, wet test meter with recovery unit; After system back pressure valve, be connected with wet test meter; The number of double tube reactor is 1-5, between reactor, adopt series connection or be connected in parallel, product sampling with the concrete structure of recovery unit is: liquid level pneumatic control valve is connected with product storage tank, and product storage tank is provided with blow-off valve, and the front end of product storage tank connects rapid-acting coupling thief hole.
The utility model has the advantages that the low temperature hydrogenation strong exothermal reaction for light ends fractionation, solved conventional hydrogenation unit charging poor stability with process furnace, system pressure fluctuation is large and beds cannot be stablized the problems such as control because temperature rise causes especially greatly temperature of reaction.
The utility model device adopts the stable catalyst bed reaction temperature of controlling of double tube reactor, can be for analoging industrial device practical condition, processing condition are steadily controlled, product property is reliable and stable, and testing 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 the detailed description with reference to below, can more completely understand better the utility model and easily learn wherein many advantages of following, but accompanying drawing described herein is used to provide further understanding of the present utility model, form a part of the present utility model, schematic description and description of the present utility model is used for explaining the utility model, do not form improper restriction of the present utility model, as schemed wherein:
Fig. 1 is structural representation of the present utility model.
Fig. 2 is structural representation of the present utility model.
Below in conjunction with drawings and Examples, the utility model is further illustrated.
Embodiment
Obviously, the many modifications and variations that those skilled in the art do based on aim of the present utility model belong to protection domain of the present utility model.
Embodiment 1: as shown in Figure 1 and Figure 2, and a kind of light ends fractionation hydrogenation test apparatus, double tube reactor 1; Thermopair 2 in reactor; Thermal oil entrance 3; Thermal oil outlet 4; Thermostatic bath 5; Reducing valve 6; Hydrogen quality under meter 7; Hydrogen gas buffer 8; Check valve 9; Suspended body flowmeter 10; Electronic scales 11; Light hydrocarbon feedstocks tank 12; Strainer 13; Air-actuated feeding pump 14; Condenser 15; System back pressure valve 16; Wet test meter 17; Knockout drum 18; Liquid level shaker 19; Liquid level pneumatic control valve 20; Fast sampling mouth 21; Product storage tank 22.
Light ends fractionation hydrogenation test apparatus of the present utility model is achieved in that
For light ends fractionation hydrogenation test apparatus, comprise successively feed unit, reaction and temperature control unit, gas-liquid separation unit, product sampling and a recovery unit, it is characterized in that:
(1) in described feed unit, hydrogen feed system comprises successively, reducing valve 6, hydrogen quality under meter 7, hydrogen gas buffer 8, check valve 9; Lighter hydrocarbons feed system comprises successively, electronic scales 11, light hydrocarbon feedstocks tank 12, strainer 13, air-actuated feeding pump 14.
The particular content of feed unit is that hydrogen quality under meter 7 ranges are 0～16L/h, are small-range under meter; Electronic scales 11 ranges are 0～30Kg, and precision is not less than 5g; Air-actuated feeding pump 14 needs 0.2～0.5Mpa air actuation, and range ability is 0～600g/h.
(2) described reaction and temperature control unit comprises, thermopair 2, thermal oil entrance 3, thermal oil outlet 4, thermostatic bath 5 in double tube reactor 1, reactor.
Reaction with the particular content of temperature control unit is, double tube reactor 1 is divided into internal layer and skin, internal layer is reaction member, be provided with thermopair 2 in reactor and be placed in catalyzer and filler centre, skin is temperature control unit, be divided into heating, constant temperature, cooling three sections, every section is provided with thermal oil entrance 3 and thermal oil outlet 4, by circulating heat conduction oil, is respectively the normal operation that above-mentioned three sections of heat supplies or heat-obtaining ensure light ends fractionation hydrogenation and removing alkynes, alkene test.
The number of described double tube reactor 1 is 1-5, can adopt series connection or be connected in parallel between reactor, and the general parallel waies of two reactors that adopt of low temperature hydrogenation parallel test of light-end products connect more.
Described thermostatic bath 5 temperature adjusting scopes are-250 ℃～250 ℃, and in the process evaluation experiment process, temperature of reaction can be stablized control, and temperature fluctuation range is ± 0.5 ℃; Described thermostatic bath 5 can merge use by constant temperature zone bath and cooling section bath when adopting single reactor, at least needs 2 baths, at least needs 3 baths when adopting two reactors in parallel.
(3) described gas-liquid separation unit comprises, 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 connects condenser 15, knockout drum 18 successively, material is divided into gas circuit and oil circuit after knockout drum, 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) described product sampling comprises with recovery unit, fast sampling mouth 21, product storage tank 22, wet test meter 17;
After described system back pressure valve 16, be connected with wet test meter 17, test tail gas is emptying after wet test meter 17 meterings;
Product samples with the particular content of recovery unit, after described liquid level pneumatic control valve 20, is connected with product storage tank 22, and product storage tank 23 is provided with blow-off valve, is provided with rapid-acting coupling thief hole 21 before material enters product storage tank 22.
A kind of light ends fractionation hydrogenation test apparatus is connected with computer aided control system, by computer aided control system, hydrogen quality under meter, system back pressure valve, liquid level pneumatic control valve is controlled.
Described whole system pressure is controlled with hydrogen quality under meter 7 and system back pressure valve 16;
Described temperature of reaction is controlled with thermostatic bath 5;
Described feed volume air speed is controlled with air-actuated feeding pump 14;
Described hydrogen and the mol ratio of alkynes are controlled with hydrogen quality under meter 7 and pneumatic fresh feed pump 14.
The utility model light ends fractionation hydrogenation test apparatus comprises feed unit, reaction and temperature control unit, gas-liquid separation unit, product sampling and recovery unit successively, and its specific implementation process is such:
In feed unit, hydrogen is pressed into double tube reactor 1 by mass flowmeter 7 meterings after reducing valve 6 decompressions.Light ends fractionation stock oil storage tank 12 Raws are measured by electronic scales 11, by air-actuated feeding pump 14, squeeze into double tube reactor 1, and air-actuated feeding pump is by 0.2～0.5Mpa air actuation.Double tube reactor 1 is divided into internal layer and skin, internal layer is used for loading catalyst and filler and is provided with the interior thermopair 2 of a plurality of mensuration bed temperatures, skin is divided into preheating, constant temperature, cooling three sections, adopts circulating heat conduction oil from thermostatic bath 5 to be respectively the stable control that above-mentioned three sections of heat supplies or heat-obtaining ensure catalyst bed reaction temperature in hydrogenation process.Reaction product out by condenser 15 condensations, and enters knockout drum 18 separation by double tube reactor 1, and isolated gas is by 16 decompressions of system back pressure valve, and emptying after wet test meter 17 meterings.The level of condensate that liquid level shaker 19 associating liquid level pneumatic control valves 20 regulate in knockout drum 18.The product liquid of being discharged by liquid level pneumatic control valve 20 enters product storage tank 22, and can be by 21 samplings of fast sampling mouth.In process of the test, with mass-flow gas meter 7 and system back pressure valve 16, control whole system pressure, by the alkene in mass-flow gas meter 7 and pneumatic fresh feed pump 14 control hydrogen and reaction oil or reaction oil and/or the ratio of alkynes.
This installs controllable processing parameter index:
Single reactor catalyst loadings: 20mL-200mL, dilutes with inert ceramic balls;
Air speed: 0.5-10h
-1;
Bed temperature: 5-250 ℃;
Pressure: 0.5-5.0Mpa;
Hydrogen and oil or hydrogen and wherein unsaturated hydrocarbons mol ratio: 1:1-50:1;
Due to employing double tube reactor reaction bed temperature precise control and almost without temperature rise, being strong exothermal reaction carries out waiting on hotbed, adopt general isothermal bed bioreactor to control poor in the situation that at device stability, bed reaction temperature rising is higher than 40 ℃, and the stability deficiency of control causes product property fluctuation large, unreliable.The utility model device removes alkynes and diolefine test for C-4-fraction low temperature hydrogenation, and in the catalyst stability of 500h is investigated, process regulation is steady, reaction pressure 2.0Mpa, feed volume air speed 2.5h
-1, hydrogen/(alkynes+diolefine) mol ratio 2～5,28～32 ℃ of bed temperature of reaction, the circulating heat conduction oil temperature of being controlled by thermostatic bath is 25～28 ℃, in whole process of the test, the fluctuating range of reaction bed temperature is no more than 0.5 ℃, investigates and the results are shown in following table:
As mentioned above, embodiment of the present utility model is explained, but as long as not departing from fact inventive point of the present utility model and effect can have a lot of distortion, this will be readily apparent to persons skilled in the art.Therefore, within such variation is also all included in protection domain of the present utility model.
Claims (1)
1. a light ends fractionation hydrogenation test apparatus, it is characterized in that comprising feed unit, reaction and temperature control unit, gas-liquid separation unit, product sampling and recovery unit, in feed unit, hydrogen feed system comprises reducing valve, hydrogen quality under meter, hydrogen gas buffer, check valve successively; Lighter hydrocarbons feed system comprises successively, electronic scales, light hydrocarbon feedstocks tank, strainer, air-actuated feeding pump; Reaction comprises thermopair in double tube reactor, reactor, thermal oil entrance, thermal oil outlet, thermostatic bath with temperature control unit; Reaction with the structure of temperature control unit is: double tube reactor is divided into internal layer and skin, internal layer is reaction member, be provided with thermopair in reactor and be placed in catalyzer and filler centre, skin is temperature control unit, heating, constant temperature, cooling three sections be respectively equipped with thermal oil entrance and thermal oil outlet; Gas-liquid separation unit comprises 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 connects condenser, knockout drum successively, material is divided into gas circuit and oil circuit after knockout drum, 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; Product sampling comprises fast sampling mouth, product storage tank, wet test meter with recovery unit; After system back pressure valve, be connected with wet test meter; The number of double tube reactor is 1-5, between reactor, adopt series connection or be connected in parallel, product sampling with the concrete structure of recovery unit is: liquid level pneumatic control valve is connected with product storage tank, and product storage tank is provided with blow-off valve, and the front end of product storage tank connects rapid-acting coupling thief hole.
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| CN201320548003.XU CN203513598U (en) | 2013-09-04 | 2013-09-04 | Light hydrocarbon fraction hydrogenation test device |
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|---|---|---|---|
| CN201320548003.XU CN203513598U (en) | 2013-09-04 | 2013-09-04 | Light hydrocarbon fraction hydrogenation test device |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106475020A (en) * | 2016-10-20 | 2017-03-08 | 中国石油化工股份有限公司 | A kind of Oscillatory Flow Reactor for isopropylbenzene catalysis oxidation cumyl hydroperoxide and method |
| 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 |
-
2013
- 2013-09-04 CN CN201320548003.XU patent/CN203513598U/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106475020A (en) * | 2016-10-20 | 2017-03-08 | 中国石油化工股份有限公司 | A kind of Oscillatory Flow Reactor for isopropylbenzene catalysis oxidation cumyl hydroperoxide and method |
| CN106475020B (en) * | 2016-10-20 | 2019-01-29 | 中国石油化工股份有限公司 | A kind of Oscillatory Flow Reactor and method for isopropylbenzene catalysis oxidation cumyl hydroperoxide |
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Granted publication date: 20140402 Termination date: 20210904 |
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