CN106950332B - A kind of high temperature and pressure catalytic hydrogenation device - Google Patents

A kind of high temperature and pressure catalytic hydrogenation device Download PDF

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Publication number
CN106950332B
CN106950332B CN201710183337.4A CN201710183337A CN106950332B CN 106950332 B CN106950332 B CN 106950332B CN 201710183337 A CN201710183337 A CN 201710183337A CN 106950332 B CN106950332 B CN 106950332B
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reaction
reaction tube
hydrogen
catalytic hydrogenation
high temperature
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CN106950332A (en
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张向云
李军
张干
卢家烂
莫扬之
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Nanjing Shuilian Tianxia Water Treatment Technology Research Institute Co ltd
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Guangzhou Institute of Geochemistry of CAS
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/10Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using catalysis
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34Purifying; Cleaning

Abstract

A kind of high temperature and pressure catalytic hydrogenation device, including sequentially connected reaction tube, flue, reaction collecting pipe, vacuum pump;The reaction tube is sealed tube body, and the hydrogen reaction tube for being internally provided with sample cell and being arranged in below sample cell is equipped with heating furnace in the periphery of reaction tube, further includes cold-trap collector, the reaction collecting pipe is placed in cold-trap collector.Advantage is to remove steel cylinder to pressurize for hydrogen and air compressor machine, safe and reliable easy to operate, simple for structure, and easy to operate, at low cost, reaction efficiency is high.

Description

A kind of high temperature and pressure catalytic hydrogenation device
Technical field
The present invention relates to catalytic hydrogenation cracking apparatus technical field, specially a kind of high temperature and pressure catalytic hydrogenation device.
Background technique
Catalytic hydrogenation cracking technique (HyPy) is that it is real to carry out temperature programming cracking by catalysis under high pressure hydrogen stream mode It tests, to separate the different carbon component of the stability in sample.It is usually used in extracting the biology of Covalent bonding together in kerogen at present Marker compounds, and determining, palaeosedimentary environment sentences knowledge and OIL SOURCE CORRELATION etc. applied to source rock organic matter source of students.Concrete application is ground Studying carefully has: immature Covalent bonding together molecule and the comparison of free state molecule into middle high evolution stage completely serial kerogen are ground Study carefully;The comparative study of Covalent bonding together molecule and free state molecule in different evolution grade solid asphalts;Different evolution grade mirrors The comparative study of Covalent bonding together molecule and free state molecule in coal;And different experimental conditions are to discharged biological marker chemical combination The influence etc. of object.But HyPy for carbon separation black in surrounding medium research compared to less, reason may be do not set up also it is corresponding Maturation method.By taking the black carbon separation in atmospheric aerosol as an example, with conventional separation methods (such as: CTO375 method, thermophotometry etc.) Carbon coking problem can all occur in high temperature, this will lead to it14The result of C measurement is not accurate enough for source resolution.And HyPy is this High pressure hydrogen also original system reduces the possibility that organic carbon forms black carbon due to coking, reduces interference to analyze its content.Therefore Method of the HyPy for carbon separation black in surrounding medium is developed, to make it be applied to atmospheric aerosol, soil and deposit The research of black carbon in equal surrounding mediums.Such as: EC (elemental carbon) in atmosphere carbonaceous aerosol source, this high pressure are separated by HyPy Hydrogen reducing system reduces the possibility that organic carbon forms EC due to coking, reduces interference to analyze the content of EC.Make EC's14It is more acurrate that C measuring method carries out atmosphere carbonaceous aerosol source parsing result.
Summary of the invention
The purpose of the present invention is overcoming the above-mentioned prior art, a kind of simple for structure, easy to operate, cost is provided Low, high-efficient high temperature and pressure catalytic hydrogenation device.
The present invention is achieved through the following technical solutions:
A kind of high temperature and pressure catalytic hydrogenation device, including sequentially connected reaction tube, flue, reaction collecting pipe, vacuum Pump;The reaction tube forms sealed tube body by both ends construction of switch, is internally provided with sample cell and is arranged under sample cell The hydrogen reaction tube of side is equipped with heating furnace in the periphery of reaction tube, further includes cold-trap collector, the reaction collecting pipe is placed in In cold-trap collector as an improvement of the above scheme, the both ends construction of switch be by stainless steel sealing fill in split mouth into Row sealing;The opening is sized for passing through for the sample cell and hydrogen reaction tube.
As an improvement of the above scheme, the sample cell include the first quartz ampoule, inside the first quartz ampoule from up to Under be followed successively by silica wool, sample position, silica wool, the first quartz ampoule is fixed at the reaction position of reaction tube.
As an improvement of the above scheme, it is equipped with the second quartz ampoule inside the reaction collecting pipe, in the second quartz ampoule Inside is followed successively by silica wool, adsorption silica gel, silica wool from top to bottom, and the second quartz ampoule is fixed at the reaction of reaction collecting pipe Collect position.
As an improvement of the above scheme, it is reacted by excessive aluminium powder with gauge water in the hydrogen reaction tube and generates hydrogen Gas.
As an improvement of the above scheme, the heating furnace is equipped with temperature controller to control the temperature of heating furnace.
As an improvement of the above scheme, the cold-trap collector is cold nitrogen cold-trap.
As an improvement of the above scheme, the flue is stainless steel tube, which is provided with needle-like stainless valve.
High temperature and pressure catalytic hydrogenation device of the invention is run in this way:
1. being added to sample cell after sample is added catalyst, clogging both ends with silica wool (prevents example reaction process to be scattered, again Can ventilate), the adsorption silica gel of activation is added in reaction collecting pipe, clogs both ends with silica wool.
2. then sample cell to be put into the reaction position of reaction tube;Hydrogen reaction tube is put into reaction tube from the other side;By Position is collected in the reaction that two quartz ampoules are put into reaction collecting pipe.
3. vacuum pump vacuumizes whole system after tightening each interface.Inspection system gas leakage, in no gas leakage the case where side It can continue to test.After position placement liquid nitrogen cold trap is collected in reaction, experimental arrangement is set.
4. setting temperature program is that 20 DEG C 250 DEG C/min are raised to 300 DEG C, then rise to 550 degree with 8 DEG C/min, constant temperature 5min。
After reaction, etc. 5. temperature are down to 300 degree, vacuum pump connection is disconnected, needle-like valve is slowly opened, removes cold Trap.Reaction product is collected into clean sample pipe to save.
It pressurizes the invention has the following advantages: removing steel cylinder from for hydrogen and air compressor machine, safe and reliable easy to operate, knot Structure is succinct, easy to operate, at low cost, and reaction efficiency is high.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of high temperature and pressure catalytic hydrogenation device of the invention.
Description of symbols: 1, reaction tube;2, flue;3, collecting pipe is reacted;4, vacuum pump;5, sample cell;6, hydrogen Reaction tube;7, heating furnace;8, sealing-plug;9, the first quartz ampoule;10, silica wool;11, sample position;12, silica wool;13, it reacts Position;14, the second quartz ampoule;15, silica wool;16, adsorption silica gel;17, silica wool;18, silica wool;19, temperature controller;20, Cold-trap collector;21, needle-like stainless valve.
Specific embodiment
As shown in Figure 1, a kind of high temperature and pressure catalytic hydrogenation device, including sequentially connected reaction tube 1, flue 2, reaction Collecting pipe 3, vacuum pump 4;The reaction tube 1 forms sealed tube body by both ends construction of switch, is internally provided with 5 He of sample cell Hydrogen reaction tube 6 below sample cell 5 is set, is equipped with heating furnace 7 in the periphery of reaction tube 1.It opens at the both ends Closing structure is to be sealed by stainless steel sealing-plug 8 into opening;The opening be sized for the sample cell 5 with Hydrogen reaction tube 6 passes through.The sample cell 5 includes the first quartz ampoule 9, inside the first quartz ampoule 9 from top to bottom successively For silica wool 10, sample position 11, silica wool 12, the first quartz ampoule 9 is fixed at the reaction position 13 of reaction tube 1.Described is anti- It answers and is equipped with the second quartz ampoule 14 inside collecting pipe 3, be followed successively by silica wool 15, absorption from top to bottom inside the second quartz ampoule 14 Position 18 is collected in silica gel 16, silica wool 17, the reaction that the second quartz ampoule 14 is fixed at reaction collecting pipe 3.The hydrogen is anti- Generation hydrogen should be reacted with gauge water by excessive aluminium powder in pipe 6.The heating furnace 7 is equipped with temperature controller 19 to control The temperature of heating furnace 7.It further include cold-trap collector 20, the reaction collecting pipe 3 is placed in cold-trap collector 20, and described is cold Trap collector 20 is cold nitrogen cold-trap.The flue 2 is stainless steel tube, which is provided with needle-like stainless valve 21.
Principle of device:
The hydrogen source of hydrogen reaction tube is that excessive aluminium powder is reacted with gauge water, water determination and reaction volume, reactant Reaction generates hydrogen when product correlation .2Al+6H2O=2Al (OH) 3+3H2 ↑ heating 180 degree.
Device source pressure, in closed system, pressure and temperature, gas flow have following correlation:
PV=nRT
This equation has 4 variables: p refers to the pressure of perfect gas, and V is the volume of perfect gas, and n indicates gaseous matter Amount, and T then indicates the thermodynamic temperature of perfect gas;There are one constants: R is ideal gas constant.
Condition 15MPa Hydrogen Vapor Pressure at 550 degree of heating needed for testing, is kept for 5 minutes.
The given volume of reaction tube can calculate the amount of required hydrogen molecule substance, then basis according to pV=nRT 2Al+6H2O=2Al (OH) 3+3H2 ↑, required water and aluminium powder amount are calculated, aluminium powder is slightly excessive during the experiment, adds 1.1 Resulting value is calculated again.
Application test:
Sample is a- graphite and urban atmosphere aerosol, and catalyst is molybdenum sulfide.
1. being added to sample cell after sample is added catalyst, clogging both ends with silica wool (prevents example reaction process to be scattered, again Can ventilate), the adsorption silica gel of activation is added in reaction collecting pipe, clogs both ends with silica wool.
2. then sample cell to be put into the reaction position of reaction tube;Hydrogen reaction tube is put into reaction tube from the other side to tighten; Position is collected into the reaction that second quartz ampoule is put into reaction collecting pipe.
3. vacuum pump vacuumizes whole system after tightening each interface.Inspection system gas leakage, in no gas leakage the case where side It can continue to test.After position placement liquid nitrogen cold trap is collected in reaction, experimental arrangement is set.
4. setting temperature program is that 20 DEG C 250 DEG C/min are raised to 300 DEG C, then rise to 550 degree with 8 DEG C/min, constant temperature 5min。
After reaction, etc. 5. temperature are down to 300 degree, vacuum pump connection is disconnected, needle-like valve is slowly opened, removes cold Trap.Reaction product is collected into clean sample pipe to save.
Following table is above-mentioned test data:
Statistics indicate that high temperature and pressure catalytic hydrogenation device of the present invention has practicability.
Above-listed detailed description is illustrating for possible embodiments of the present invention, and the embodiment is not to limit this hair Bright the scope of the patents, all equivalence enforcements or change without departing from carried out by the present invention, is intended to be limited solely by the scope of the patents of this case.

Claims (9)

1. a kind of high temperature and pressure catalytic hydrogenation device, which is characterized in that received including sequentially connected reaction tube, flue, reaction Collector, vacuum pump;The reaction tube forms sealed tube body by both ends construction of switch, is internally provided with sample cell and setting exists Hydrogen reaction tube below sample cell is equipped with heating furnace in the periphery of reaction tube, further includes cold-trap collector, the reaction is received Collector is placed in cold-trap collector, is reacted by excessive aluminium powder with gauge water in the hydrogen reaction tube and is generated hydrogen, described Flue be stainless steel tube, which is provided with needle-like stainless valve.
2. a kind of high temperature and pressure catalytic hydrogenation device according to claim 1, which is characterized in that the two end switch knots Structure is to fill in split mouth by stainless steel sealing to be sealed;The opening to be sized for the sample cell and hydrogen anti- Should pipe pass through.
3. a kind of high temperature and pressure catalytic hydrogenation device according to claim 1, which is characterized in that the sample cell includes First quartz ampoule, is followed successively by silica wool, sample position, silica wool from top to bottom inside the first quartz ampoule, and the first quartz ampoule is fixed The reaction position of reaction tube is set.
4. a kind of high temperature and pressure catalytic hydrogenation device according to claim 1, which is characterized in that the reaction collecting pipe Inside is equipped with the second quartz ampoule, is being followed successively by silica wool, adsorption silica gel, silica wool from top to bottom inside the second quartz ampoule, the Position is collected in the reaction that two quartz ampoules are fixed at reaction collecting pipe.
5. a kind of high temperature and pressure catalytic hydrogenation device according to claim 1, which is characterized in that set on the heating furnace There is temperature controller to control the temperature of heating furnace.
6. a kind of high temperature and pressure catalytic hydrogenation device according to claim 1, which is characterized in that the cold-trap collector For cold nitrogen cold-trap.
7. a kind of application method comprising any one of claim 1 to 6 high temperature and pressure catalytic hydrogenation device, which is characterized in that tool Steps are as follows for body:
Step 1 is added to sample cell after sample is added catalyst;
Sample cell is put into the reaction position of reaction tube by step 2;By be calculated test needed for water and aluminium powder amount and by its It is packed into hydrogen reaction tube, hydrogen reaction tube is put into reaction tube from the other side and is tightened;Second quartz ampoule is put into reaction collecting pipe Reaction collect position;
After step 3 tightens each interface, vacuum pump vacuumizes whole system;
Step 4 setting temperature program is 20 DEG C and starts to be raised to 300 DEG C with 250 DEG C/min, then rises to 550 degree with 8 DEG C/min, constant temperature 5min;
Step 5 after reaction, etc. temperature be down to 300 degree, disconnect vacuum pump connection, slowly open needle-like valve, remove cold-trap, Reaction product is collected into clean sample pipe to save.
8. the method according to the description of claim 7 is characterized in that be calculated described in step 2 test needed for water and Aluminium powder amount, specific reaction equation are as follows:
2Al+6H2O=2Al (OH)3+3H2↑ (1)
When heating 180 degree, reaction generates hydrogen;Device source pressure, in closed system, pressure and temperature, gas flow has following It is related:
PV=nRT (2)
This equation has 4 variables: p refers to the pressure of perfect gas, and V is the volume of perfect gas, and n indicates gaseous matter Amount, and T then indicates the thermodynamic temperature of perfect gas;There are one constants: R is ideal gas constant;The volume one of reaction tube It is fixed, according to formula (2), the amount of required hydrogen molecule substance can be calculated, then according to formula (1), calculate required water and Aluminium powder amount.
9. according to the method described in claim 8, it is characterized in that, the aluminium powder in an experiment the amount of use for calculated value 1.1 again.
CN201710183337.4A 2017-03-24 2017-03-24 A kind of high temperature and pressure catalytic hydrogenation device Active CN106950332B (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102139193A (en) * 2011-01-19 2011-08-03 中国科学院广州地球化学研究所 Full automatic high-pressure hydrogenation thermal cracking device for geochemistry research
CN204017807U (en) * 2014-03-05 2014-12-17 华东理工大学 Catalyzed chemical reaction device and for the air supply part of this device
CN104785171A (en) * 2014-01-21 2015-07-22 北京金菲特能源科技有限公司 Universal heavy raw material hydrogenation lightening device
CN105859499A (en) * 2016-06-08 2016-08-17 北京神雾环境能源科技集团股份有限公司 Reaction system and method for preparing ethylene through hydrogenation of acetylene
CN106483245A (en) * 2016-11-16 2017-03-08 中国科学院广州地球化学研究所 A kind of catalytic hydrogenation example reaction and reactant collection device
CN206638638U (en) * 2017-03-24 2017-11-14 中国科学院广州地球化学研究所 A kind of HTHP catalytic hydrogenation device

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102139193A (en) * 2011-01-19 2011-08-03 中国科学院广州地球化学研究所 Full automatic high-pressure hydrogenation thermal cracking device for geochemistry research
CN104785171A (en) * 2014-01-21 2015-07-22 北京金菲特能源科技有限公司 Universal heavy raw material hydrogenation lightening device
CN204017807U (en) * 2014-03-05 2014-12-17 华东理工大学 Catalyzed chemical reaction device and for the air supply part of this device
CN105859499A (en) * 2016-06-08 2016-08-17 北京神雾环境能源科技集团股份有限公司 Reaction system and method for preparing ethylene through hydrogenation of acetylene
CN106483245A (en) * 2016-11-16 2017-03-08 中国科学院广州地球化学研究所 A kind of catalytic hydrogenation example reaction and reactant collection device
CN206638638U (en) * 2017-03-24 2017-11-14 中国科学院广州地球化学研究所 A kind of HTHP catalytic hydrogenation device

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